DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:17:42 2018) ID: 2932; threads 39; handles 878; mem 517952.00 (1237728.00)kB; time: 1w 5d 21h 23m 12s MEMORY INFO: Memory PF:0.0, Ph:155.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.8,peak PF: 708.5, WS: 269.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:155.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.6,peak PF: 708.5, WS: 271.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:17:42 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000063 0.000087 0.000102 ) 0.087412 -0.166882 0.063604 ( 0.000057 0.000079 0.000093 ) 0.055227 -0.024260 0.122680 ( 0.000081 0.000112 0.000132 ) 5.91535 ( 0.00411 ) 5.92288 ( 0.00426 ) 5.91286 ( 0.00636 ) 59.95509 ( 0.09288 ) 89.89521 ( 0.07016 ) 59.99590 ( 0.07399 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 12:17:42 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000063 0.000087 0.000102 ) 0.087412 -0.166882 0.063604 ( 0.000057 0.000079 0.000093 ) 0.055227 -0.024260 0.122680 ( 0.000081 0.000112 0.000132 ) M - matrix: 0.021540 -0.014330 0.007148 ( 0.000019 0.000016 0.000019 ) -0.014330 0.028673 -0.014354 ( 0.000016 0.000027 0.000022 ) 0.007148 -0.014354 0.021576 ( 0.000019 0.000022 0.000036 ) unit cell: 5.915(4) 5.923(4) 5.913(6) 59.96(9) 89.90(7) 60.00(7) V = 146.5(2) 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\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb PROFFITPEAK info: 302 peaks in the peak location table UB fit with 131 obs out of 138 (total:138,skipped:0) (94.93%) UB - matrix: -0.104252 -0.015123 0.050240 ( 0.000098 0.000126 0.000162 ) 0.087054 -0.166697 0.063594 ( 0.000158 0.000204 0.000261 ) 0.055416 -0.024381 0.122081 ( 0.000149 0.000193 0.000247 ) M - matrix: 0.021518 -0.014286 0.007064 ( 0.000038 0.000036 0.000038 ) -0.014286 0.028611 -0.014337 ( 0.000036 0.000069 0.000052 ) 0.007064 -0.014337 0.021472 ( 0.000038 0.000052 0.000071 ) unit cell: 5.914(7) 5.938(9) 5.934(12) 59.73(19) 89.62(12) 59.96(14) V = 147.2(4) UB fit with 131 obs out of 138 (total:138,skipped:0) (94.93%) UB - matrix: -0.104252 -0.015123 0.050240 ( 0.000098 0.000126 0.000162 ) 0.087054 -0.166697 0.063594 ( 0.000158 0.000204 0.000261 ) 0.055416 -0.024381 0.122081 ( 0.000149 0.000193 0.000247 ) M - matrix: 0.021518 -0.014286 0.007064 ( 0.000038 0.000036 0.000038 ) -0.014286 0.028611 -0.014337 ( 0.000036 0.000069 0.000052 ) 0.007064 -0.014337 0.021472 ( 0.000038 0.000052 0.000071 ) unit cell: 5.914(7) 5.938(9) 5.934(12) 59.73(19) 89.62(12) 59.96(14) V = 147.2(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB fit with 132 obs out of 138 (total:138,skipped:0) (95.65%) UB - matrix: -0.104234 -0.015133 0.050325 ( 0.000103 0.000133 0.000172 ) 0.087048 -0.166701 0.063513 ( 0.000146 0.000189 0.000244 ) 0.055423 -0.024403 0.122017 ( 0.000152 0.000196 0.000253 ) M - matrix: 0.021514 -0.014286 0.007046 ( 0.000037 0.000035 0.000038 ) -0.014286 0.028614 -0.014327 ( 0.000035 0.000064 0.000050 ) 0.007046 -0.014327 0.021455 ( 0.000038 0.000050 0.000071 ) unit cell: 5.915(7) 5.939(9) 5.936(12) 59.72(19) 89.57(13) 59.93(14) V = 147.2(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 138 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Run 1 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104233 -0.015134 0.050326 ( 0.000103 0.000133 0.000172 ) 0.087047 -0.166700 0.063512 ( 0.000147 0.000189 0.000244 ) 0.055422 -0.024402 0.122016 ( 0.000152 0.000196 0.000253 ) M - matrix: 0.021513 -0.014286 0.007045 ( 0.000037 0.000035 0.000038 ) -0.014286 0.028614 -0.014327 ( 0.000035 0.000064 0.000050 ) 0.007045 -0.014327 0.021454 ( 0.000038 0.000050 0.000071 ) UB fit with 132 obs out of 138 (total:138,skipped:0) (95.65%) unit cell: 5.915(7) 5.939(9) 5.936(12) 59.72(19) 89.57(13) 59.93(14) V = 147.2(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 132 obs out of 138 (total:138,skipped:0) (95.65%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb 2 of 99 peaks identified as outliers and rejected 97 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 97 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 97 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.38 | 10 | 1.008 ( 0.114) | 1.346 ( 0.537) | 1.390 ( 0.975) | 1.32- 1.09 | 10 | 1.112 ( 0.087) | 1.150 ( 0.132) | 1.109 ( 0.303) | 1.09- 0.96 | 10 | 1.173 ( 0.096) | 1.326 ( 0.403) | 1.382 ( 0.646) | 0.96- 0.84 | 10 | 1.177 ( 0.063) | 1.204 ( 0.149) | 1.174 ( 0.407) | 0.84- 0.81 | 10 | 1.186 ( 0.085) | 1.196 ( 0.152) | 1.163 ( 0.415) | 0.81- 0.73 | 10 | 1.226 ( 0.027) | 1.247 ( 0.066) | 1.410 ( 0.461) | 0.73- 0.71 | 10 | 1.219 ( 0.035) | 1.193 ( 0.165) | 1.276 ( 0.449) | 0.70- 0.64 | 10 | 1.226 ( 0.037) | 1.262 ( 0.119) | 1.181 ( 0.410) | 0.64- 0.61 | 10 | 1.261 ( 0.070) | 1.290 ( 0.160) | 1.141 ( 0.440) | 0.61- 0.59 | 7 | 1.217 ( 0.056) | 1.401 ( 0.212) | 0.990 ( 0.302) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 97 | 1.179 ( 0.101) | 1.257 ( 0.262) | 1.229 ( 0.537) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) UB - matrix: -0.104232 -0.015109 0.049570 ( 0.000046 0.000058 0.000078 ) 0.087383 -0.167102 0.063498 ( 0.000056 0.000070 0.000095 ) 0.055265 -0.024315 0.122500 ( 0.000063 0.000079 0.000106 ) M - matrix: 0.021554 -0.014371 0.007152 ( 0.000015 0.000014 0.000016 ) -0.014371 0.028742 -0.014338 ( 0.000014 0.000024 0.000019 ) 0.007152 -0.014338 0.021495 ( 0.000016 0.000019 0.000030 ) unit cell: 5.917(3) 5.917(4) 5.923(5) 60.00(8) 89.93(5) 59.96(6) V = 146.62(16) OTKP changes: 97 1 1 1 UB - matrix: -0.104182 -0.015182 0.049746 ( 0.000048 0.000059 0.000080 ) 0.087372 -0.167059 0.063317 ( 0.000054 0.000067 0.000091 ) 0.055454 -0.024451 0.122477 ( 0.000062 0.000077 0.000104 ) M - matrix: 0.021563 -0.014371 0.007141 ( 0.000015 0.000013 0.000016 ) -0.014371 0.028737 -0.014328 ( 0.000013 0.000023 0.000019 ) 0.007141 -0.014328 0.021484 ( 0.000016 0.000019 0.000029 ) UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) unit cell: 5.916(3) 5.917(3) 5.923(5) 60.01(7) 89.91(5) 59.95(6) V = 146.60(16) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.001) HKL list info: 268 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb 2 of 100 peaks identified as outliers and rejected 98 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 98 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 98 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.06- 1.38 | 10 | 1.022 ( 0.119) | 1.375 ( 0.613) | 1.444 ( 1.035) | 1.32- 1.09 | 10 | 1.113 ( 0.088) | 1.153 ( 0.135) | 1.099 ( 0.291) | 1.09- 0.96 | 10 | 1.174 ( 0.097) | 1.327 ( 0.403) | 1.387 ( 0.660) | 0.96- 0.84 | 10 | 1.177 ( 0.064) | 1.207 ( 0.140) | 1.181 ( 0.436) | 0.84- 0.81 | 10 | 1.178 ( 0.087) | 1.194 ( 0.151) | 1.160 ( 0.406) | 0.81- 0.73 | 10 | 1.224 ( 0.028) | 1.245 ( 0.069) | 1.446 ( 0.488) | 0.73- 0.71 | 10 | 1.223 ( 0.034) | 1.230 ( 0.131) | 1.311 ( 0.460) | 0.70- 0.64 | 10 | 1.230 ( 0.043) | 1.285 ( 0.138) | 1.100 ( 0.283) | 0.64- 0.61 | 10 | 1.259 ( 0.057) | 1.250 ( 0.146) | 1.219 ( 0.527) | 0.61- 0.59 | 8 | 1.216 ( 0.049) | 1.411 ( 0.196) | 0.994 ( 0.274) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.06- 0.59 | 98 | 1.181 ( 0.098) | 1.265 ( 0.276) | 1.239 ( 0.555) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.7 | 10 | 1.179 ( 0.053) | 1.345 ( 0.374) | 1.497 ( 0.675) | 13.5-19.9 | 10 | 1.199 ( 0.038) | 1.288 ( 0.068) | 1.095 ( 0.420) | 20.2-24.1 | 10 | 1.198 ( 0.069) | 1.256 ( 0.102) | 1.208 ( 0.522) | 24.5-27.9 | 10 | 1.138 ( 0.122) | 1.131 ( 0.137) | 1.409 ( 0.437) | 28.0-31.1 | 10 | 1.177 ( 0.092) | 1.466 ( 0.525) | 1.375 ( 0.655) | 31.4-33.5 | 10 | 1.151 ( 0.082) | 1.159 ( 0.121) | 1.219 ( 0.230) | 33.8-36.5 | 10 | 1.153 ( 0.111) | 1.187 ( 0.197) | 1.067 ( 0.219) | 37.5-39.8 | 10 | 1.210 ( 0.052) | 1.165 ( 0.139) | 1.069 ( 0.480) | 40.2-44.1 | 10 | 1.204 ( 0.088) | 1.378 ( 0.205) | 1.314 ( 0.906) | 44.6-49.8 | 8 | 1.204 ( 0.183) | 1.277 ( 0.313) | 1.111 ( 0.409) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 98 | 1.181 ( 0.098) | 1.265 ( 0.276) | 1.239 ( 0.555) | Fitted profile normalization line parameters e1 dimension: a=0.0011 b=0.98 e2 dimension: a=0.0028 b=0.91 e3 dimension: a=-0.0007 b=0.99 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6425 lp-corr: 5348 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 609776 Maximum peak integral for reflections I/sig<= 10000 - raw: 5209173 lp-corr: 2194691 PROFFITPEAK - Finished at Wed Mar 28 12:17:44 2018 PROFFITMAIN - Started at Wed Mar 28 12:17:44 2018 OTKP changes: 98 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 98 1 1 1 UB - matrix: -0.104181 -0.015186 0.049730 ( 0.000047 0.000059 0.000079 ) 0.087354 -0.167065 0.063318 ( 0.000055 0.000069 0.000092 ) 0.055491 -0.024472 0.122511 ( 0.000063 0.000078 0.000104 ) M - matrix: 0.021564 -0.014370 0.007148 ( 0.000015 0.000013 0.000016 ) -0.014370 0.028740 -0.014332 ( 0.000013 0.000023 0.000019 ) 0.007148 -0.014332 0.021491 ( 0.000016 0.000019 0.000029 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 5.915(3) 5.916(3) 5.922(5) 60.01(7) 89.93(5) 59.96(6) V = 146.57(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 264 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.104181 -0.015186 0.049730 ( 0.000047 0.000059 0.000079 ) 0.087354 -0.167065 0.063318 ( 0.000055 0.000069 0.000092 ) 0.055491 -0.024472 0.122511 ( 0.000063 0.000078 0.000104 ) M - matrix: 0.021564 -0.014370 0.007148 ( 0.000015 0.000013 0.000016 ) -0.014370 0.028740 -0.014332 ( 0.000013 0.000023 0.000019 ) 0.007148 -0.014332 0.021491 ( 0.000016 0.000019 0.000029 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 5.915(3) 5.916(3) 5.922(5) 60.01(7) 89.93(5) 59.96(6) V = 146.57(16) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104181 -0.015186 0.049730 ( 0.000047 0.000059 0.000079 ) 0.087354 -0.167065 0.063318 ( 0.000055 0.000069 0.000092 ) 0.055491 -0.024472 0.122511 ( 0.000063 0.000078 0.000104 ) M - matrix: 0.021564 -0.014370 0.007148 ( 0.000015 0.000013 0.000016 ) -0.014370 0.028740 -0.014332 ( 0.000013 0.000023 0.000019 ) 0.007148 -0.014332 0.021491 ( 0.000016 0.000019 0.000029 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 5.915(3) 5.916(3) 5.922(5) 60.01(7) 89.93(5) 59.96(6) V = 146.57(16) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 7 reflections under beam stop or inside a detector rejection region 1 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof 129 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:17:45 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 1bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) PROFFIT INFO: signal sum: min=971.0000 max=4617601.0000 PROFFIT INFO: signal sum lp corr: min=1011.0900 max=1882468.4838 PROFFIT INFO: background sum: min=1115.0000 max=4591.0000 PROFFIT INFO: background sum sig2: min=651.0000 max=4349.0000 PROFFIT INFO: num of signal pixels: min=61 max=397 PROFFIT INFO: Inet: min=2206.0146 max=4107204.0000 PROFFIT INFO: sig(Inet): min=249.8297 max=56764.6133 PROFFIT INFO: Inet/sig(Inet): min=1.97 max=200.42 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 1 10 18 27 30 50 85 116 129 Percent 0.0 0.0 0.8 7.8 14.0 20.9 23.3 38.8 65.9 89.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 129 100.00 (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 129 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4107204- 1717799 12 2511571.25 134.84 100.00 1649783- 1254396 12 1455666.19 117.90 100.00 1220931- 398009 12 803060.77 95.20 100.00 376469- 222959 12 284288.05 77.71 100.00 220142- 193813 12 208650.62 47.75 100.00 192563- 160117 12 173257.41 40.10 100.00 158942- 130940 12 149790.01 33.82 100.00 126207- 88844 12 107722.02 26.75 100.00 88655- 5751 12 19729.12 11.68 100.00 5514- 2206 21 3805.55 3.53 52.38 ------------------------------------------------------------------------------------ 4107204- 2206 129 532129.78 55.06 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.41 12 895111.46 75.54 100.00 1.39- 1.12 12 735006.27 65.72 100.00 1.12- 0.96 12 808667.88 90.69 100.00 0.96- 0.85 12 636000.42 68.01 100.00 0.84- 0.81 12 610348.69 63.41 100.00 0.81- 0.75 12 229070.50 34.21 83.33 0.75- 0.71 12 448536.81 50.92 83.33 0.71- 0.67 12 639378.35 57.93 100.00 0.67- 0.64 12 361066.12 39.56 75.00 0.64- 0.59 21 204119.22 26.26 85.71 ------------------------------------------------------------------------------------ 4.17- 0.59 129 532129.78 55.06 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:17:45 2018 Sorting 129 observations 0 unique observations with > 7.00 F2/sig(F2) 129 observations in 1 runs Run # start # end # total # 1 1 24 24 Total number of frames 24 Maximum number of 0 frame scales suggested for reliable scaling Can't fit requested scale/empirical absorption model (pTmpToScale3AbspackHKL) ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 0, Friedel: 1 Min/max for: run:1/1 frame:2/25 129 reflections read from tmp file 129 reflections are rejected (0 as outliers, 129 as groups of 1 refl) ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4107204- 1717799 12 2511571.25 134.84 100.00 1649783- 1254396 12 1455666.19 117.90 100.00 1220931- 398009 12 803060.77 95.20 100.00 376469- 222959 12 284288.05 77.71 100.00 220142- 193813 12 208650.62 47.75 100.00 192563- 160117 12 173257.41 40.10 100.00 158942- 130940 12 149790.01 33.82 100.00 126207- 88844 12 107722.02 26.75 100.00 88655- 5751 12 19729.12 11.68 100.00 5514- 2206 21 3805.55 3.53 52.38 ------------------------------------------------------------------------------------ 4107204- 2206 129 532129.78 55.06 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.41 12 895111.46 75.54 100.00 1.39- 1.12 12 735006.27 65.72 100.00 1.12- 0.96 12 808667.88 90.69 100.00 0.96- 0.85 12 636000.42 68.01 100.00 0.84- 0.81 12 610348.69 63.41 100.00 0.81- 0.75 12 229070.50 34.21 83.33 0.75- 0.71 12 448536.81 50.92 83.33 0.71- 0.67 12 639378.35 57.93 100.00 0.67- 0.64 12 361066.12 39.56 75.00 0.64- 0.59 21 204119.22 26.26 85.71 ------------------------------------------------------------------------------------ 4.17- 0.59 129 532129.78 55.06 92.25 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.41 12 895111.46 75.54 100.00 4.17- 1.12 24 815058.87 70.63 100.00 4.17- 0.96 36 812928.54 77.31 100.00 4.17- 0.85 48 768696.51 74.99 100.00 4.17- 0.81 60 737026.94 72.67 100.00 4.17- 0.75 72 652367.54 66.26 97.22 4.17- 0.71 84 623248.86 64.07 95.24 4.17- 0.67 96 625265.05 63.30 95.83 4.17- 0.64 108 595909.61 60.67 93.52 4.17- 0.59 129 532129.78 55.06 92.25 ------------------------------------------------------------------------------------ 4.17- 0.59 129 532129.78 55.06 92.25 Scale applied to data: s=0.243474 (maximum obs:4107204.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.000; Rsigma 0.012: data 129 -> merged 129 With outlier rejection... Rint 0.000; Rsigma 0.012: data 129 -> merged 129 Rejected total: 0, method kkm 0, method Blessing 0 Completeness direct cell (a, b, c) = (5.915, 5.916, 5.922), (alpha, beta, gamma) = (60.012, 89.932, 59.964) wavelength: 0.709300 dmin, dmax value (Ang): 0.587354, 4.182654 completeness table (Laue group: P1, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.32 14 137 1.00 10.22 14 1.32 - 1.02 14 137 1.00 10.22 14 1.02 - 0.91 15 137 1.00 10.95 15 0.91 - 0.82 12 137 1.00 8.76 12 0.82 - 0.76 15 137 1.00 10.95 15 0.76 - 0.72 11 137 1.00 8.03 11 0.72 - 0.68 11 137 1.00 8.03 11 0.68 - 0.65 9 137 1.00 6.57 9 0.65 - 0.63 10 137 1.00 7.30 10 0.63 - 0.60 13 141 1.00 9.22 13 --------------------------------------------------------------- 5.92 - 0.60 124 1374 1.00 9.02 124 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:17:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915157 5.915574 5.922243 60.0122 89.9318 59.9640 129 Reflections read from file xs1715a.hkl; mean (I/sigma) = 55.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 66 66 66 67 99 91 88 129 N (int>3sigma) = 0 61 66 61 60 94 86 82 119 Mean intensity = 0.0 12.5 4.9 12.6 10.9 10.0 13.3 13.1 13.0 Mean int/sigma = 0.0 51.0 49.3 53.9 53.3 51.4 52.8 56.6 55.1 Lattice type: P chosen Volume: 146.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.912 5.915 5.920 119.93 90.02 119.98 Niggli form: a.a = 34.953 b.b = 34.989 c.c = 35.046 b.c = -17.473 a.c = -0.011 a.b = -17.474 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.066 CUBIC F-lattice R(int) = 0.044 [ 36] Vol = 586.3 Cell: 8.365 8.375 8.368 90.08 89.92 90.07 Volume: 586.27 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.032 RHOMBOHEDRAL R-lattice R(int) = 0.099 [ 3] Vol = 439.7 Cell: 5.915 5.912 14.515 89.98 90.06 119.98 Volume: 439.70 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.032 RHOMBOHEDRAL R-lattice R(int) = 0.000 [ 0] Vol = 439.7 Trigonal Cell: 5.915 5.912 14.515 89.98 90.06 119.98 Volume: 439.70 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.159 TETRAGONAL I-lattice R(int) = 0.073 [ 7] Vol = 293.1 Cell: 5.916 5.924 8.365 89.90 89.99 90.05 Volume: 293.13 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.127 TETRAGONAL I-lattice R(int) = 0.073 [ 7] Vol = 293.1 Cell: 5.916 5.924 8.365 89.90 89.99 90.05 Volume: 293.13 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.108 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 32] Vol = 293.1 Cell: 5.916 8.365 5.924 89.90 89.95 90.01 Volume: 293.13 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 293.1 Cell: 8.365 5.916 5.924 90.05 90.10 90.01 Volume: 293.13 Matrix:-1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.011 MONOCLINIC I-lattice R(int) = 0.014 [ 11] Vol = 293.1 Cell: 5.920 5.912 8.375 90.01 90.10 89.98 Volume: 293.13 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.090 MONOCLINIC C-lattice R(int) = 0.064 [ 3] Vol = 293.1 Cell: 8.365 8.375 5.912 90.01 134.95 90.07 Volume: 293.13 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.6 Cell: 5.912 5.915 5.920 119.93 90.02 119.98 Volume: 146.57 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 66 0 86 87 129 N (int>3sigma) = 0 0 0 0 66 0 80 78 119 Mean intensity = 0.0 0.0 0.0 0.0 4.9 0.0 9.3 12.0 13.0 Mean int/sigma = 0.0 0.0 0.0 0.0 49.3 0.0 50.0 49.6 55.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.468 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 10 26 N I>3s 1 1 10 26 0.2 0.2 0.1 5.3 14.9 14.9 7.5 56.3 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 0.044 34 Fd-3m 1 1 227 C N N N N 37 2284 0.042 51 0kl, 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365324 8.375287 8.367865 90.0779 89.9239 90.0686 ZERR 1.00 0.009598 0.001769 0.017995 0.0665 0.0224 0.0175 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4107204- 1220931 25 25 25 1.0 1953111.21 125.27 0.000 0.000 1198363- 218333 25 25 25 1.0 490629.19 82.52 0.000 0.000 216252- 157195 25 25 25 1.0 184724.66 42.51 0.000 0.000 157062- 8081 25 25 25 1.0 112009.07 28.29 0.000 0.000 7848- 2206 29 29 29 1.0 4582.36 4.77 0.000 0.000 ------------------------------------------------------------------------------------------- 4107204- 2206 129 129 129 1.0 532129.78 55.06 0.000 0.000 Statistics vs resolution - point group symmetry: P-1 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 25 25 25 1.0 889475.66 75.82 0.000 0.000 0.011 1.09-0.84 25 25 25 1.0 601518.36 71.48 0.000 0.000 0.009 0.84-0.73 25 25 25 1.0 464981.86 51.83 0.000 0.000 0.012 0.73-0.65 25 25 25 1.0 464421.98 47.91 0.000 0.000 0.014 0.65-0.59 29 29 29 1.0 280510.17 31.97 0.000 0.000 0.018 ------------------------------------------------------------------------------------------------------ inf-0.59 129 129 129 1.0 532129.78 55.06 0.000 0.000 0.012 inf-0.60 124 124 124 1.0 550217.88 56.47 0.000 0.000 0.012 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-1.12 25 223 25 11.2 1.0 889475.66 75.82 0.000 0.000 1.09-0.84 25 268 25 9.3 1.0 601518.36 71.48 0.000 0.000 0.84-0.73 25 251 25 10.0 1.0 464981.86 51.83 0.000 0.000 0.73-0.65 25 324 25 7.7 1.0 464421.98 47.91 0.000 0.000 0.65-0.59 29 419 29 6.9 1.0 280510.17 31.97 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.59 129 1513 129 8.5 1.0 532129.78 55.06 0.000 0.000 inf-0.60 124 1369 124 9.1 1.0 550217.88 56.47 0.000 0.000 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 1.0 -1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 1.0 -1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.076955 0.034819 0.007593 ( 0.000049 0.000050 0.000030 ) -0.012018 0.008196 0.083533 ( 0.000057 0.000058 0.000034 ) 0.033510 -0.076765 0.012236 ( 0.000065 0.000065 0.000039 ) M - matrix: 0.007189 0.000009 -0.000010 ( 0.000009 0.000007 0.000006 ) 0.000009 0.007172 0.000010 ( 0.000007 0.000011 0.000006 ) -0.000010 0.000010 0.007185 ( 0.000006 0.000006 0.000006 ) Constraint UB - matrix: 0.076955 0.034819 0.007593 ( 0.000049 0.000050 0.000030 ) -0.012018 0.008196 0.083533 ( 0.000057 0.000058 0.000034 ) 0.033510 -0.076765 0.012236 ( 0.000065 0.000065 0.000039 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000001 ) unit cell: 8.365(5) 8.375(6) 8.368(4) 90.08(5) 89.92(4) 90.07(5) V = 586.3(6) unit cell: 8.3695(8) 8.3695(8) 8.3695(8) 90.0 90.0 90.0 V = 586.27(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: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) PROFFIT INFO: signal sum: min=971.0000 max=4617601.0000 PROFFIT INFO: signal sum lp corr: min=1011.0900 max=1882468.4838 PROFFIT INFO: background sum: min=1115.0000 max=4591.0000 PROFFIT INFO: background sum sig2: min=651.0000 max=4349.0000 PROFFIT INFO: num of signal pixels: min=61 max=397 PROFFIT INFO: Inet: min=2206.0146 max=4107204.0000 PROFFIT INFO: sig(Inet): min=249.8297 max=56764.6133 PROFFIT INFO: Inet/sig(Inet): min=1.97 max=200.42 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 2 20 36 54 60 100 170 232 258 Percent 0.0 0.0 0.8 7.8 14.0 20.9 23.3 38.8 65.9 89.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 129 100.00 (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 129 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4107204- 1717799 12 2511571.25 134.84 100.00 1649783- 1254396 12 1455666.19 117.90 100.00 1220931- 398009 12 803060.77 95.20 100.00 376469- 222959 12 284288.05 77.71 100.00 220142- 193813 12 208650.62 47.75 100.00 192563- 160117 12 173257.41 40.10 100.00 158942- 130940 12 149790.01 33.82 100.00 126207- 88844 12 107722.02 26.75 100.00 88655- 5751 12 19729.12 11.68 100.00 5514- 2206 21 3805.55 3.53 52.38 ------------------------------------------------------------------------------------ 4107204- 2206 129 532129.78 55.06 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.18- 1.41 12 895111.46 75.54 100.00 1.39- 1.12 12 746477.73 66.75 100.00 1.12- 0.96 12 803669.58 91.83 100.00 0.96- 0.85 12 629527.27 65.83 100.00 0.84- 0.81 12 606377.17 62.66 100.00 0.81- 0.75 12 233588.36 35.08 83.33 0.75- 0.71 12 449543.83 51.16 83.33 0.71- 0.67 12 637824.98 57.57 100.00 0.67- 0.64 12 361066.12 39.56 75.00 0.64- 0.59 21 204119.22 26.26 85.71 ------------------------------------------------------------------------------------ 4.18- 0.59 129 532129.78 55.06 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:17:45 2018 Sorting 129 observations 25 unique observations with > 7.00 F2/sig(F2) 129 observations in 1 runs Run # start # end # total # 1 1 24 24 Total number of frames 24 Maximum number of 25 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 129 observations in 1 runs Run # start # end # total # 1 1 24 24 Total number of frames 24 Frame #8 of 24 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 106 observations > 7.00 F2/sig(F2) 106 observations in 1 runs Run # start # end # total # 1 1 24 24 Total number of frames 24 Frame #8 of 24 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: 2.7 (Out of 106 removed 36 = 70, unique = 26) 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 70 observations in 1 runs Run # start # end # total # 1 1 24 24 Total number of frames 24 Frame #8 of 24 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 26 unique data precomputed (should be 26) 26 unique data with 70 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.7 (Out of 70 removed 0 = 70, unique = 26) 26 unique data precomputed (should be 26) 26 unique data with 70 observations RMS deviation of equivalent data = 0.05935 Rint = 0.04207 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.04207, wR= 0.05955 Trying model 1 (ne=2, no=0)... Results: Rint= 0.02165, wR= 0.02370, Acormin=0.884, Acormax=1.185, Acor_av=0.976 F test: Probability=1.000, F= 3.346 Trying model 2 (ne=2, no=1)... Results: Rint= 0.01748, wR= 0.02077, Acormin=0.880, Acormax=1.200, Acor_av=0.989 F test: Probability=0.853, F= 1.416 Final absorption model (ne=2, no=0): Rint= 0.02165, Acormin=0.884, Acormax=1.185, Acor_av=0.976 Combined refinement in use Rint: 0.04239 There are 23 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 27 pars with 378 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.05935 Using Levenberg-Marquardt: 0.00010 New wR= 0.01506 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.04207 with corrections 0.01150 Rint for all data: 0.04239 with corrections 0.01186 0 observations identified as outliers and rejected Cycle 2 wR= 0.01506 Using Levenberg-Marquardt: 0.00001 New wR= 0.01494 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.04207 with corrections 0.01122 Rint for all data: 0.04239 with corrections 0.01158 0 observations identified as outliers and rejected Cycle 3 wR= 0.01494 Using Levenberg-Marquardt: 0.00000 New wR= 0.01506 Using Levenberg-Marquardt: 0.00001 New wR= 0.01506 Using Levenberg-Marquardt: 0.00010 New wR= 0.01505 Using Levenberg-Marquardt: 0.00100 New wR= 0.01504 Using Levenberg-Marquardt: 0.01000 New wR= 0.01497 Using Levenberg-Marquardt: 0.10000 New wR= 0.01481 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.04207 with corrections 0.01093 Rint for all data: 0.04239 with corrections 0.01130 0 observations identified as outliers and rejected Cycle 4 wR= 0.01481 Using Levenberg-Marquardt: 0.01000 New wR= 0.01503 Using Levenberg-Marquardt: 0.10000 New wR= 0.01481 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.04207 with corrections 0.01081 Rint for all data: 0.04239 with corrections 0.01117 Final wR= 0.01481 Final frame scales: Min= 0.9757 Max= 1.0861 Final absorption correction factors: Amin= 0.8747 Amax= 1.0615 PROFFIT INFO: Inet (after scale3 abspack): min=2355.0979 max=4287867.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=288.4205 max=59261.5195 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:2/25 129 reflections read from tmp file 41 reflections are rejected (1 as outliers, 40 as groups of 1 refl) Redundancy: 1 2 3 4 5+ Number of groups: 0 16 13 3 1 Initial Chi^2= 0.27664 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.38361 Current error model SIG(F2)^2 = 219.05*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 84.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 84.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4287868- 1714650 12 2495902.97 148.29 100.00 1696774- 1287481 12 1449645.95 84.72 100.00 1261759- 387094 12 807127.36 66.96 100.00 379358- 226495 12 285064.77 57.15 100.00 226019- 205963 12 214509.97 34.76 100.00 195218- 157115 12 168597.32 28.18 100.00 156192- 121588 12 147119.46 25.43 100.00 118239- 92816 12 106859.17 19.96 100.00 87309- 6052 12 19821.09 9.53 100.00 5920- 2355 21 3802.90 4.61 100.00 ------------------------------------------------------------------------------------ 4287868- 2355 129 530353.78 44.93 100.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.18- 1.41 12 899259.03 80.91 100.00 1.39- 1.12 12 743232.64 74.74 100.00 1.12- 0.96 12 815736.80 65.96 100.00 0.96- 0.85 12 630230.65 47.70 100.00 0.84- 0.81 12 611187.61 45.45 100.00 0.81- 0.75 12 234014.35 26.01 100.00 0.75- 0.71 12 444401.21 37.11 100.00 0.71- 0.67 12 621114.18 41.63 100.00 0.67- 0.64 12 353317.08 29.00 100.00 0.64- 0.59 21 199319.76 19.74 100.00 ------------------------------------------------------------------------------------ 4.18- 0.59 129 530353.78 44.93 100.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.18- 1.41 12 899259.03 80.91 100.00 4.18- 1.12 24 821245.83 77.83 100.00 4.18- 0.96 36 819409.49 73.87 100.00 4.18- 0.85 48 772114.78 67.33 100.00 4.18- 0.81 60 739929.35 62.95 100.00 4.18- 0.75 72 655610.18 56.79 100.00 4.18- 0.71 84 625437.47 53.98 100.00 4.18- 0.67 96 624897.06 52.44 100.00 4.18- 0.64 108 594721.51 49.83 100.00 4.18- 0.59 129 530353.78 44.93 100.00 ------------------------------------------------------------------------------------ 4.18- 0.59 129 530353.78 44.93 100.00 Scale applied to data: s=0.233216 (maximum obs:4287867.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.011; Rsigma 0.014: data 129 -> merged 73 With outlier rejection... Rint 0.011; Rsigma 0.014: data 127 -> merged 73 Rejected total: 2, method kkm 2, method Blessing 0 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.587423, 4.184742 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 6 10 1.33 60.00 8 1.61 - 1.21 7 10 1.43 70.00 10 1.17 - 1.01 6 10 2.17 60.00 13 0.99 - 0.89 9 10 1.78 90.00 16 0.88 - 0.81 8 10 1.88 80.00 15 0.81 - 0.74 7 10 1.86 70.00 13 0.73 - 0.71 8 10 1.63 80.00 13 0.70 - 0.66 6 10 1.83 60.00 11 0.66 - 0.64 6 10 1.83 60.00 11 0.63 - 0.60 8 10 1.75 80.00 14 --------------------------------------------------------------- 5.92 - 0.60 71 100 1.75 71.00 124 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:17:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915157 5.915574 5.922243 60.0122 89.9318 59.9640 129 Reflections read from file xs1715a.hkl; mean (I/sigma) = 55.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 66 66 66 67 99 91 88 129 N (int>3sigma) = 0 61 66 61 60 94 86 82 119 Mean intensity = 0.0 12.5 4.9 12.6 10.9 10.0 13.3 13.1 13.0 Mean int/sigma = 0.0 51.0 49.3 53.9 53.3 51.4 52.8 56.6 55.1 Lattice type: P chosen Volume: 146.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.912 5.915 5.920 119.93 90.02 119.98 Niggli form: a.a = 34.953 b.b = 34.989 c.c = 35.046 b.c = -17.473 a.c = -0.011 a.b = -17.474 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.066 CUBIC F-lattice R(int) = 0.044 [ 36] Vol = 586.3 Cell: 8.365 8.375 8.368 90.08 89.92 90.07 Volume: 586.27 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.032 RHOMBOHEDRAL R-lattice R(int) = 0.099 [ 3] Vol = 439.7 Cell: 5.915 5.912 14.515 89.98 90.06 119.98 Volume: 439.70 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.032 RHOMBOHEDRAL R-lattice R(int) = 0.000 [ 0] Vol = 439.7 Trigonal Cell: 5.915 5.912 14.515 89.98 90.06 119.98 Volume: 439.70 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.159 TETRAGONAL I-lattice R(int) = 0.073 [ 7] Vol = 293.1 Cell: 5.916 5.924 8.365 89.90 89.99 90.05 Volume: 293.13 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.127 TETRAGONAL I-lattice R(int) = 0.073 [ 7] Vol = 293.1 Cell: 5.916 5.924 8.365 89.90 89.99 90.05 Volume: 293.13 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.108 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 32] Vol = 293.1 Cell: 5.916 8.365 5.924 89.90 89.95 90.01 Volume: 293.13 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 293.1 Cell: 8.365 5.916 5.924 90.05 90.10 90.01 Volume: 293.13 Matrix:-1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.011 MONOCLINIC I-lattice R(int) = 0.014 [ 11] Vol = 293.1 Cell: 5.920 5.912 8.375 90.01 90.10 89.98 Volume: 293.13 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.090 MONOCLINIC C-lattice R(int) = 0.064 [ 3] Vol = 293.1 Cell: 8.365 8.375 5.912 90.01 134.95 90.07 Volume: 293.13 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.6 Cell: 5.912 5.915 5.920 119.93 90.02 119.98 Volume: 146.57 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 66 0 86 87 129 N (int>3sigma) = 0 0 0 0 66 0 80 78 119 Mean intensity = 0.0 0.0 0.0 0.0 4.9 0.0 9.3 12.0 13.0 Mean int/sigma = 0.0 0.0 0.0 0.0 49.3 0.0 50.0 49.6 55.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.468 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 10 26 N I>3s 1 1 10 26 0.2 0.2 0.1 5.3 14.9 14.9 7.5 56.3 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 0.044 34 Fd-3m 1 1 227 C N N N N 37 2284 0.042 51 0kl, 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365324 8.375287 8.367865 90.0779 89.9239 90.0686 ZERR 1.00 0.009598 0.001769 0.017995 0.0665 0.0224 0.0175 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4287868- 200749 61 61 36 1.7 1036430.00 77.67 0.009 0.010 186244- 2355 68 66 37 1.8 76205.64 15.57 0.019 0.019 ------------------------------------------------------------------------------------------- 4287868- 2355 129 127 73 1.7 537415.77 45.40 0.011 0.011 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-0.81 63 62 36 1.7 725492.28 62.33 0.010 0.010 0.010 0.78-0.59 66 65 37 1.8 358019.71 29.25 0.012 0.012 0.021 ------------------------------------------------------------------------------------------------------ inf-0.59 129 127 73 1.7 537415.77 45.40 0.011 0.011 0.014 inf-0.60 124 122 70 1.7 556164.07 46.63 0.010 0.011 0.014 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-0.81 62 50 36 72.0 1.7 725492.28 86.29 0.010 0.008 0.78-0.59 65 56 37 66.1 1.8 358019.71 41.09 0.012 0.014 -------------------------------------------------------------------------------------------- inf-0.59 127 108 73 67.6 1.7 537415.77 63.15 0.011 0.010 inf-0.60 122 99 70 70.7 1.7 556164.07 64.79 0.010 0.010 ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:23:03 2018) ID: 2932; threads 39; handles 878; mem 518476.00 (1237724.00)kB; time: 1w 5d 21h 28m 33s MEMORY INFO: Memory PF:0.0, Ph:161.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.4,peak PF: 708.5, WS: 270.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:161.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.2,peak PF: 708.5, WS: 272.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:23:03 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000047 0.000059 0.000079 ) 0.087412 -0.166882 0.063604 ( 0.000055 0.000069 0.000092 ) 0.055227 -0.024260 0.122680 ( 0.000063 0.000078 0.000104 ) 5.91535 ( 0.00311 ) 5.92288 ( 0.00355 ) 5.91286 ( 0.00492 ) 59.95509 ( 0.07479 ) 89.89521 ( 0.05359 ) 59.99590 ( 0.05888 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 12:23:03 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000047 0.000059 0.000079 ) 0.087412 -0.166882 0.063604 ( 0.000055 0.000069 0.000092 ) 0.055227 -0.024260 0.122680 ( 0.000063 0.000078 0.000104 ) M - matrix: 0.021564 -0.014370 0.007148 ( 0.000015 0.000013 0.000016 ) -0.014370 0.028740 -0.014332 ( 0.000013 0.000023 0.000019 ) 0.007148 -0.014332 0.021491 ( 0.000016 0.000019 0.000029 ) unit cell: 5.915(3) 5.923(3) 5.913(5) 59.96(7) 89.90(5) 60.00(6) V = 146.51(16) 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\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb PROFFITPEAK info: 591 peaks in the peak location table UB fit with 258 obs out of 274 (total:274,skipped:0) (94.16%) UB - matrix: -0.104208 -0.015260 0.049988 ( 0.000074 0.000072 0.000105 ) 0.087099 -0.166772 0.063658 ( 0.000094 0.000091 0.000133 ) 0.055312 -0.024098 0.122481 ( 0.000102 0.000099 0.000144 ) M - matrix: 0.021505 -0.014268 0.007110 ( 0.000025 0.000020 0.000023 ) -0.014268 0.028627 -0.014331 ( 0.000020 0.000031 0.000027 ) 0.007110 -0.014331 0.021553 ( 0.000023 0.000027 0.000041 ) unit cell: 5.912(4) 5.922(5) 5.915(7) 59.92(10) 89.87(8) 60.08(8) V = 146.6(2) UB fit with 258 obs out of 274 (total:274,skipped:0) (94.16%) UB - matrix: -0.104208 -0.015260 0.049988 ( 0.000074 0.000072 0.000105 ) 0.087099 -0.166772 0.063658 ( 0.000094 0.000091 0.000133 ) 0.055312 -0.024098 0.122481 ( 0.000102 0.000099 0.000144 ) M - matrix: 0.021505 -0.014268 0.007110 ( 0.000025 0.000020 0.000023 ) -0.014268 0.028627 -0.014331 ( 0.000020 0.000031 0.000027 ) 0.007110 -0.014331 0.021553 ( 0.000023 0.000027 0.000041 ) unit cell: 5.912(4) 5.922(5) 5.915(7) 59.92(10) 89.87(8) 60.08(8) V = 146.6(2) OTKP changes: 50 1 1 1 UB - matrix: -0.104032 -0.015147 0.049635 ( 0.000073 0.000071 0.000103 ) 0.087139 -0.166598 0.063513 ( 0.000086 0.000084 0.000123 ) 0.055262 -0.024268 0.122377 ( 0.000101 0.000098 0.000143 ) M - matrix: 0.021470 -0.014283 0.007134 ( 0.000024 0.000019 0.000022 ) -0.014283 0.028573 -0.014303 ( 0.000019 0.000028 0.000025 ) 0.007134 -0.014303 0.021474 ( 0.000022 0.000025 0.000040 ) UB fit with 258 obs out of 274 (total:274,skipped:0) (94.16%) unit cell: 5.925(4) 5.933(5) 5.929(7) 59.95(10) 89.94(7) 60.02(8) V = 147.4(2) UB fit with 258 obs out of 274 (total:274,skipped:0) (94.16%) UB - matrix: -0.104032 -0.015147 0.049635 ( 0.000073 0.000071 0.000103 ) 0.087139 -0.166598 0.063513 ( 0.000086 0.000084 0.000123 ) 0.055262 -0.024268 0.122377 ( 0.000101 0.000098 0.000143 ) M - matrix: 0.021470 -0.014283 0.007134 ( 0.000024 0.000019 0.000022 ) -0.014283 0.028573 -0.014303 ( 0.000019 0.000028 0.000025 ) 0.007134 -0.014303 0.021474 ( 0.000022 0.000025 0.000040 ) unit cell: 5.925(4) 5.933(5) 5.929(7) 59.95(10) 89.94(7) 60.02(8) V = 147.4(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.104042 -0.015117 0.049624 ( 0.000073 0.000071 0.000104 ) 0.087134 -0.166630 0.063544 ( 0.000087 0.000084 0.000124 ) 0.055227 -0.024260 0.122390 ( 0.000101 0.000098 0.000144 ) M - matrix: 0.021467 -0.014286 0.007133 ( 0.000024 0.000019 0.000022 ) -0.014286 0.028583 -0.014308 ( 0.000019 0.000029 0.000025 ) 0.007133 -0.014308 0.021480 ( 0.000022 0.000025 0.000040 ) UB fit with 257 obs out of 274 (total:274,skipped:0) (93.80%) unit cell: 5.926(4) 5.933(5) 5.928(7) 59.95(10) 89.93(7) 60.01(8) V = 147.4(2) 274 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Run 1 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.031) HKL list info: 427 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104041 -0.015117 0.049624 ( 0.000073 0.000071 0.000104 ) 0.087134 -0.166630 0.063544 ( 0.000087 0.000084 0.000124 ) 0.055227 -0.024260 0.122390 ( 0.000101 0.000098 0.000144 ) M - matrix: 0.021467 -0.014286 0.007133 ( 0.000024 0.000019 0.000022 ) -0.014286 0.028583 -0.014308 ( 0.000019 0.000029 0.000025 ) 0.007133 -0.014308 0.021480 ( 0.000022 0.000025 0.000040 ) UB fit with 257 obs out of 274 (total:274,skipped:0) (93.80%) unit cell: 5.926(4) 5.933(5) 5.928(7) 59.95(10) 89.93(7) 60.01(8) V = 147.4(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 258 obs out of 274 (total:274,skipped:0) (94.16%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb 4 of 204 peaks identified as outliers and rejected 200 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 200 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 200 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 1.32 | 20 | 0.991 ( 0.128) | 1.197 ( 0.493) | 1.375 ( 0.818) | 1.28- 1.09 | 20 | 1.123 ( 0.079) | 1.188 ( 0.106) | 1.217 ( 0.548) | 1.09- 0.97 | 20 | 1.139 ( 0.092) | 1.224 ( 0.310) | 1.157 ( 0.442) | 0.96- 0.84 | 20 | 1.174 ( 0.049) | 1.199 ( 0.135) | 1.228 ( 0.397) | 0.84- 0.81 | 20 | 1.188 ( 0.057) | 1.224 ( 0.128) | 1.122 ( 0.393) | 0.81- 0.73 | 20 | 1.198 ( 0.046) | 1.205 ( 0.130) | 1.336 ( 0.384) | 0.73- 0.70 | 20 | 1.207 ( 0.041) | 1.202 ( 0.186) | 1.342 ( 0.432) | 0.69- 0.66 | 20 | 1.209 ( 0.046) | 1.212 ( 0.136) | 1.274 ( 0.396) | 0.65- 0.62 | 20 | 1.215 ( 0.082) | 1.289 ( 0.127) | 1.118 ( 0.427) | 0.62- 0.59 | 20 | 1.230 ( 0.072) | 1.270 ( 0.214) | 1.146 ( 0.413) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 0.59 | 200 | 1.167 ( 0.100) | 1.221 ( 0.230) | 1.232 ( 0.490) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) UB - matrix: -0.104179 -0.014831 0.049198 ( 0.000041 0.000039 0.000054 ) 0.087394 -0.166942 0.063466 ( 0.000031 0.000029 0.000040 ) 0.055138 -0.024388 0.122584 ( 0.000040 0.000038 0.000052 ) M - matrix: 0.021531 -0.014389 0.007180 ( 0.000011 0.000007 0.000009 ) -0.014389 0.028684 -0.014314 ( 0.000007 0.000010 0.000009 ) 0.007180 -0.014314 0.021475 ( 0.000009 0.000009 0.000015 ) unit cell: 5.929(2) 5.9268(18) 5.925(3) 60.07(4) 90.00(3) 59.88(4) V = 147.11(9) OTKP changes: 200 1 1 1 UB - matrix: -0.104323 -0.015044 0.049746 ( 0.000030 0.000028 0.000039 ) 0.087369 -0.167139 0.063574 ( 0.000028 0.000027 0.000037 ) 0.055351 -0.024253 0.122727 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021580 -0.014376 0.007158 ( 0.000009 0.000006 0.000008 ) -0.014376 0.028750 -0.014350 ( 0.000006 0.000009 0.000008 ) 0.007158 -0.014350 0.021578 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9125(17) 5.9125(16) 5.908(2) 60.04(3) 89.93(3) 59.96(3) V = 146.12(8) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.934) HKL list info: 424 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104323 -0.015044 0.049746 ( 0.000030 0.000028 0.000039 ) 0.087369 -0.167139 0.063574 ( 0.000028 0.000027 0.000037 ) 0.055351 -0.024253 0.122727 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021580 -0.014376 0.007158 ( 0.000009 0.000006 0.000008 ) -0.014376 0.028750 -0.014350 ( 0.000006 0.000009 0.000008 ) 0.007158 -0.014350 0.021578 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9125(17) 5.9125(16) 5.908(2) 60.04(3) 89.93(3) 59.96(3) V = 146.12(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb 3 of 203 peaks identified as outliers and rejected 200 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 200 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 200 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.04- 1.32 | 20 | 0.991 ( 0.128) | 1.177 ( 0.494) | 1.365 ( 0.809) | 1.27- 1.09 | 20 | 1.117 ( 0.075) | 1.177 ( 0.107) | 1.224 ( 0.669) | 1.09- 0.96 | 20 | 1.147 ( 0.087) | 1.225 ( 0.323) | 1.376 ( 0.590) | 0.96- 0.84 | 20 | 1.176 ( 0.049) | 1.200 ( 0.128) | 1.238 ( 0.417) | 0.84- 0.81 | 20 | 1.187 ( 0.058) | 1.220 ( 0.128) | 1.118 ( 0.418) | 0.81- 0.73 | 20 | 1.194 ( 0.050) | 1.188 ( 0.121) | 1.256 ( 0.444) | 0.73- 0.70 | 20 | 1.211 ( 0.039) | 1.202 ( 0.145) | 1.390 ( 0.409) | 0.70- 0.67 | 20 | 1.205 ( 0.047) | 1.233 ( 0.160) | 1.281 ( 0.387) | 0.66- 0.62 | 20 | 1.216 ( 0.089) | 1.283 ( 0.122) | 1.255 ( 0.500) | 0.62- 0.59 | 20 | 1.224 ( 0.064) | 1.247 ( 0.219) | 1.204 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.04- 0.59 | 200 | 1.167 ( 0.099) | 1.215 ( 0.230) | 1.271 ( 0.530) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 20 | 1.162 ( 0.049) | 1.285 ( 0.275) | 1.496 ( 0.644) | 13.0-19.3 | 20 | 1.159 ( 0.056) | 1.237 ( 0.095) | 1.185 ( 0.483) | 19.5-23.6 | 20 | 1.189 ( 0.058) | 1.264 ( 0.083) | 1.321 ( 0.654) | 24.1-28.0 | 20 | 1.126 ( 0.106) | 1.127 ( 0.126) | 1.285 ( 0.419) | 28.0-31.2 | 20 | 1.172 ( 0.073) | 1.366 ( 0.400) | 1.292 ( 0.535) | 31.3-34.6 | 20 | 1.137 ( 0.075) | 1.171 ( 0.147) | 1.160 ( 0.275) | 34.8-37.6 | 20 | 1.186 ( 0.071) | 1.193 ( 0.171) | 1.295 ( 0.411) | 37.7-40.0 | 20 | 1.148 ( 0.125) | 1.116 ( 0.146) | 1.204 ( 0.531) | 40.2-43.6 | 20 | 1.160 ( 0.126) | 1.177 ( 0.246) | 1.175 ( 0.671) | 43.7-49.8 | 20 | 1.227 ( 0.150) | 1.216 ( 0.274) | 1.294 ( 0.459) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 200 | 1.167 ( 0.099) | 1.215 ( 0.230) | 1.271 ( 0.530) | Fitted profile normalization line parameters e1 dimension: a=0.0013 b=0.98 e2 dimension: a=0.0005 b=1.00 e3 dimension: a=-0.0036 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6425 lp-corr: 5352 Maximum peak integral for reflections I/sig<= 100 - raw: 464319 lp-corr: 640702 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2283883 PROFFITPEAK - Finished at Wed Mar 28 12:23:07 2018 PROFFITMAIN - Started at Wed Mar 28 12:23:07 2018 OTKP changes: 200 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 200 1 1 1 UB - matrix: -0.104337 -0.015044 0.049761 ( 0.000029 0.000028 0.000039 ) 0.087380 -0.167175 0.063581 ( 0.000029 0.000028 0.000039 ) 0.055372 -0.024252 0.122757 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021587 -0.014381 0.007161 ( 0.000009 0.000007 0.000008 ) -0.014381 0.028762 -0.014355 ( 0.000007 0.000009 0.000008 ) 0.007161 -0.014355 0.021588 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9115(17) 5.9108(16) 5.906(2) 60.05(3) 89.93(3) 59.96(3) V = 146.02(8) *** 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= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.921) HKL list info: 421 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104337 -0.015044 0.049761 ( 0.000029 0.000028 0.000039 ) 0.087380 -0.167175 0.063581 ( 0.000029 0.000028 0.000039 ) 0.055372 -0.024252 0.122757 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021587 -0.014381 0.007161 ( 0.000009 0.000007 0.000008 ) -0.014381 0.028762 -0.014355 ( 0.000007 0.000009 0.000008 ) 0.007161 -0.014355 0.021588 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9115(17) 5.9108(16) 5.906(2) 60.05(3) 89.93(3) 59.96(3) V = 146.02(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! 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: -0.104337 -0.015044 0.049761 ( 0.000029 0.000028 0.000039 ) 0.087380 -0.167175 0.063581 ( 0.000029 0.000028 0.000039 ) 0.055372 -0.024252 0.122757 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021587 -0.014381 0.007161 ( 0.000009 0.000007 0.000008 ) -0.014381 0.028762 -0.014355 ( 0.000007 0.000009 0.000008 ) 0.007161 -0.014355 0.021588 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9115(17) 5.9108(16) 5.906(2) 60.05(3) 89.93(3) 59.96(3) V = 146.02(8) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104337 -0.015044 0.049761 ( 0.000029 0.000028 0.000039 ) 0.087380 -0.167175 0.063581 ( 0.000029 0.000028 0.000039 ) 0.055372 -0.024252 0.122757 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021587 -0.014381 0.007161 ( 0.000009 0.000007 0.000008 ) -0.014381 0.028762 -0.014355 ( 0.000007 0.000009 0.000008 ) 0.007161 -0.014355 0.021588 ( 0.000008 0.000008 0.000014 ) UB fit with 200 obs out of 200 (total:200,skipped:0) (100.00%) unit cell: 5.9115(17) 5.9108(16) 5.906(2) 60.05(3) 89.93(3) 59.96(3) V = 146.02(8) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 14 reflections under beam stop or inside a detector rejection region 3 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof 270 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:23:08 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.921) PROFFIT INFO: signal sum: min=524.0000 max=19734144.0000 PROFFIT INFO: signal sum lp corr: min=691.9651 max=2247941.6347 PROFFIT INFO: background sum: min=872.0000 max=15463.0000 PROFFIT INFO: background sum sig2: min=740.0000 max=8870.0000 PROFFIT INFO: num of signal pixels: min=68 max=519 PROFFIT INFO: Inet: min=1509.7421 max=4904600.5000 PROFFIT INFO: sig(Inet): min=247.9734 max=63802.9531 PROFFIT INFO: Inet/sig(Inet): min=1.37 max=228.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 2 21 34 59 63 104 174 242 270 Percent 0.0 0.0 0.7 7.8 12.6 21.9 23.3 38.5 64.4 89.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 270 100.00 (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 270 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4904601- 1708197 27 2653146.43 143.81 100.00 1699683- 1154647 27 1408079.19 110.13 100.00 1150972- 367360 27 585785.83 93.87 100.00 365089- 228495 27 270884.58 70.16 100.00 227802- 184614 27 209367.41 52.15 100.00 177893- 150345 27 162376.49 35.37 100.00 149332- 107216 27 125643.91 29.78 100.00 107195- 6315 27 59877.10 20.64 100.00 6147- 3990 27 5043.28 4.92 85.19 3962- 1510 27 3246.18 3.44 37.04 ------------------------------------------------------------------------------------ 4904601- 1510 270 548345.04 56.43 92.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 3.72- 1.27 27 975682.76 90.45 100.00 1.27- 1.01 27 660186.46 74.21 96.30 0.98- 0.85 27 707830.17 66.63 100.00 0.85- 0.74 27 469665.67 56.74 96.30 0.74- 0.67 27 653325.65 63.28 88.89 0.67- 0.61 27 411350.43 47.65 92.59 0.61- 0.57 27 583418.84 54.15 96.30 0.56- 0.52 27 388812.39 40.76 77.78 0.52- 0.48 27 330733.33 37.63 85.19 0.48- 0.40 27 302444.70 32.78 88.89 ------------------------------------------------------------------------------------ 3.72- 0.40 270 548345.04 56.43 92.22 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:23:08 2018 Sorting 270 observations 52 unique observations with > 7.00 F2/sig(F2) 270 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Maximum number of 52 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 270 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 219 observations > 7.00 F2/sig(F2) 219 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 219 removed 125 = 94, 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): 2/m3bar 94 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Frame #6 of 49 skipped from refinement Frame #8 of 49 skipped from refinement Frame #28 of 49 skipped from refinement Frame #33 of 49 skipped from refinement Frame #40 of 49 skipped from refinement Frame #42 of 49 skipped from refinement Frame #45 of 49 skipped from refinement Frame #48 of 49 skipped from refinement 8 frames need to be skipped from refinement, because of missing redundant and/or observable data 45 unique data precomputed (should be 45) 45 unique data with 94 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 94 removed 0 = 94, unique = 45) 45 unique data precomputed (should be 45) 45 unique data with 94 observations RMS deviation of equivalent data = 0.64588 Rint = 0.56050 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.56050, wR= 6.29358 Trying model 1 (ne=2, no=0)... Results: Rint= 0.49223, wR= 3.92131, Acormin=-0.270, Acormax=1.054, Acor_av=0.249 F test: Probability=0.695, F= 1.164 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84563, wR= 5.59923, Acormin=-0.146, Acormax=0.302, Acor_av=0.026 F test: Probability=0.000, F= 0.368 Trying model 3 (ne=4, no=0)... Results: Rint= 0.39474, wR= 2.46122, Acormin=-0.209, Acormax=0.592, Acor_av=0.073 F test: Probability=0.870, F= 1.440 Trying model 4 (ne=4, no=1)... Results: Rint= 0.25255, wR= 2.39818, Acormin=-0.610, Acormax=0.297, Acor_av=0.061 F test: Probability=1.000, F= 3.217 Trying model 5 (ne=4, no=3)... Results: Rint= 0.21491, wR= 1.21839, Acormin=-0.105, Acormax=1.002, Acor_av=0.028 F test: Probability=0.999, F= 3.470 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: 0.70774 There are 41 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 45 pars with 1035 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.64588 Using Levenberg-Marquardt: 0.00010 New wR= 0.60912 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56050 with corrections 0.58369 Rint for all data: 0.70774 with corrections 0.71739 4 observations identified as outliers and rejected Cycle 2 wR= 0.58868 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= 0.74766 Using Levenberg-Marquardt: 0.10000 New wR= 0.63816 Using Levenberg-Marquardt: 1.00000 New wR= 0.56034 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.64183 Rint for all data: 0.70774 with corrections 0.74175 0 observations identified as outliers and rejected Cycle 3 wR= 0.56034 Using Levenberg-Marquardt: 0.10000 New wR= 0.52938 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.67360 Rint for all data: 0.70774 with corrections 0.73648 0 observations identified as outliers and rejected Cycle 4 wR= 0.52938 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.51132 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.71420 Rint for all data: 0.70774 with corrections 0.77187 0 observations identified as outliers and rejected Cycle 5 wR= 0.51132 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.50044 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.59609 Rint for all data: 0.70774 with corrections 0.75801 0 observations identified as outliers and rejected Final wR= 0.50044 Final frame scales: Min= 1.0000 Max= 16.4481 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time with different frame scales initialization There are 41 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 40 pars with 820 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.11014 Using Levenberg-Marquardt: 0.00010 New wR= 0.56988 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.54529 Rint for all data: 0.70774 with corrections 0.70963 0 observations identified as outliers and rejected Cycle 2 wR= 0.56988 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= 0.55331 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.54030 Rint for all data: 0.70774 with corrections 0.70159 0 observations identified as outliers and rejected Cycle 3 wR= 0.55331 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= 0.53311 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.51924 Rint for all data: 0.70774 with corrections 0.68962 0 observations identified as outliers and rejected Cycle 4 wR= 0.53311 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.52032 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.50794 Rint for all data: 0.70774 with corrections 0.68422 0 observations identified as outliers and rejected Cycle 5 wR= 0.52032 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.51224 There are 8 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56902 with corrections 0.50252 Rint for all data: 0.70774 with corrections 0.68290 0 observations identified as outliers and rejected Final wR= 0.51224 Final frame scales: Min= 1.0000 Max= 28.6421 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 14 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 13 pars with 91 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.88217 Using Levenberg-Marquardt: 0.00010 New wR= 0.69730 There are 6 clusters with unrefined scales (size 1-13) Rint for refined data: 0.56902 with corrections 0.60232 Rint for all data: 0.70774 with corrections 0.73698 0 observations identified as outliers and rejected Cycle 2 wR= 0.62094 Using Levenberg-Marquardt: 0.00001 New wR= 0.60354 There are 6 clusters with unrefined scales (size 1-13) Rint for refined data: 0.56902 with corrections 0.91741 Rint for all data: 0.70774 with corrections 0.95310 0 observations identified as outliers and rejected Cycle 3 wR= 0.85604 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.83424 There are 6 clusters with unrefined scales (size 1-13) Rint for refined data: 0.56902 with corrections 0.95079 Rint for all data: 0.70774 with corrections 0.98394 0 observations identified as outliers and rejected Cycle 4 wR= 0.80336 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.79218 There are 6 clusters with unrefined scales (size 1-13) Rint for refined data: 0.56902 with corrections 0.99489 Rint for all data: 0.70774 with corrections 1.01287 0 observations identified as outliers and rejected Cycle 5 wR= 0.75371 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1000.00000 New wR= 0.75348 There are 6 clusters with unrefined scales (size 1-13) Rint for refined data: 0.56902 with corrections 0.99611 Rint for all data: 0.70774 with corrections 1.01361 Final wR= 0.75348 Frame scales out of range! Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 13 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 12 pars with 78 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 5.68110 Using Levenberg-Marquardt: 0.00010 New wR= 0.61538 There are 5 clusters with unrefined scales (size 1-18) Rint for refined data: 0.56902 with corrections 0.54028 Rint for all data: 0.70774 with corrections 0.68580 0 observations identified as outliers and rejected Cycle 2 wR= 0.61739 Using Levenberg-Marquardt: 0.00001 New wR= 0.61288 There are 5 clusters with unrefined scales (size 1-18) Rint for refined data: 0.56902 with corrections 0.54535 Rint for all data: 0.70774 with corrections 0.69171 0 observations identified as outliers and rejected Cycle 3 wR= 0.61736 Using Levenberg-Marquardt: 0.00000 New wR= 0.61146 There are 5 clusters with unrefined scales (size 1-18) Rint for refined data: 0.56902 with corrections 0.54613 Rint for all data: 0.70774 with corrections 0.69080 0 observations identified as outliers and rejected Cycle 4 wR= 0.61953 Using Levenberg-Marquardt: 0.00000 New wR= 0.61723 There are 5 clusters with unrefined scales (size 1-18) Rint for refined data: 0.56902 with corrections 0.54501 Rint for all data: 0.70774 with corrections 0.69050 0 observations identified as outliers and rejected Cycle 5 wR= 0.61873 Using Levenberg-Marquardt: 0.00000 New wR= 0.61531 There are 5 clusters with unrefined scales (size 1-18) Rint for refined data: 0.56902 with corrections 0.55100 Rint for all data: 0.70774 with corrections 0.69386 0 observations identified as outliers and rejected Final wR= 0.61531 Final frame scales: Min= 0.3050 Max= 1.9342 PROFFIT INFO: Inet (after scale3 abspack): min=1125.6979 max=4808790.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=450.3861 max=58726.3477 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:2/50 270 reflections read from tmp file 240 reflections are rejected (96 as outliers, 144 as groups of 1 refl) Redundancy: 1 2+ Number of groups: 0 15 Initial Chi^2= 0.71529 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.47990 Current error model SIG(F2)^2 = 955.74*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 458.66*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 458.66*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4808790- 1758082 27 2737842.24 66.05 100.00 1718999- 973846 27 1331442.05 33.88 100.00 941865- 337166 27 505508.70 26.49 100.00 332287- 222940 27 260460.05 20.44 100.00 222113- 168982 27 188525.70 17.19 100.00 168541- 127573 27 147217.35 12.86 100.00 126534- 91127 27 112965.86 9.75 100.00 90113- 8073 27 49569.93 7.34 81.48 7300- 3825 27 5269.83 2.39 25.93 3772- 1126 27 2999.04 1.72 0.00 ------------------------------------------------------------------------------------ 4808790- 1126 270 534180.07 19.81 80.74 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 3.72- 1.27 27 940089.05 43.06 100.00 1.27- 1.01 27 711981.80 25.96 81.48 0.98- 0.85 27 639435.17 25.08 85.19 0.85- 0.74 27 461321.73 17.67 77.78 0.74- 0.67 27 673225.84 19.63 81.48 0.67- 0.61 27 414026.27 14.88 85.19 0.61- 0.57 27 641147.21 16.82 77.78 0.56- 0.52 27 353470.72 12.79 70.37 0.52- 0.48 27 264895.27 11.84 77.78 0.48- 0.40 27 242207.68 10.39 70.37 ------------------------------------------------------------------------------------ 3.72- 0.40 270 534180.07 19.81 80.74 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 3.72- 1.27 27 940089.05 43.06 100.00 3.72- 1.01 54 826035.43 34.51 90.74 3.72- 0.85 81 763835.34 31.37 88.89 3.72- 0.74 108 688206.94 27.94 86.11 3.72- 0.67 135 685210.72 26.28 85.19 3.72- 0.61 162 640013.31 24.38 85.19 3.72- 0.57 189 640175.30 23.30 84.13 3.72- 0.52 216 604337.22 21.99 82.41 3.72- 0.48 243 566621.45 20.86 81.89 3.72- 0.40 270 534180.07 19.81 80.74 ------------------------------------------------------------------------------------ 3.72- 0.40 270 534180.07 19.81 80.74 Scale applied to data: s=0.207952 (maximum obs:4808790.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.694; Rsigma 0.032: data 270 -> merged 199 With outlier rejection... Rint 0.679; Rsigma 0.032: data 264 -> merged 199 Rejected total: 6, method kkm 6, method Blessing 0 Completeness direct cell (a, b, c) = (5.266, 5.266, 5.266), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.403874, 3.723535 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 11 15 1.36 73.33 15 1.46 - 1.12 14 15 1.64 93.33 23 1.07 - 0.96 14 15 1.36 93.33 19 0.96 - 0.85 14 15 1.36 93.33 19 0.85 - 0.78 12 15 1.33 80.00 16 0.78 - 0.73 11 15 1.36 73.33 15 0.73 - 0.69 11 15 1.27 73.33 14 0.69 - 0.65 12 15 1.42 80.00 17 0.65 - 0.63 5 15 1.80 33.33 9 0.63 - 0.60 13 21 1.31 61.90 17 --------------------------------------------------------------- 5.91 - 0.60 117 156 1.40 75.00 164 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:23:08 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.911464 5.910752 5.906027 60.0487 89.9347 59.9584 264 Reflections read from file xs1715a.hkl; mean (I/sigma) = 20.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 129 137 130 134 198 185 184 264 N (int>3sigma) = 0 102 137 103 103 171 153 149 215 Mean intensity = 0.0 10.9 4.1 10.9 9.3 8.6 11.6 11.4 11.3 Mean int/sigma = 0.0 18.8 15.6 19.2 16.6 17.9 19.8 20.5 20.1 Lattice type: P chosen Volume: 146.02 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 Unitcell: 5.906 5.907 5.911 60.03 60.05 60.11 Niggli form: a.a = 34.881 b.b = 34.897 c.c = 34.937 b.c = 17.444 a.c = 17.429 a.b = 17.389 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.079 CUBIC F-lattice R(int) = 0.175 [ 138] Vol = 584.1 Cell: 8.361 8.351 8.365 90.05 90.05 90.05 Volume: 584.08 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.154 [ 40] Vol = 438.1 Cell: 5.916 5.913 14.465 90.07 89.98 120.03 Volume: 438.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 8] Vol = 438.1 Trigonal Cell: 5.916 5.913 14.465 90.07 89.98 120.03 Volume: 438.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 126] Vol = 438.1 Cell: 5.906 5.916 14.483 89.98 89.99 120.04 Volume: 438.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.139 [ 30] Vol = 438.1 Trigonal Cell: 5.906 5.916 14.483 89.98 89.99 120.04 Volume: 438.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.159 [ 83] Vol = 292.0 Cell: 5.906 5.911 8.365 90.00 89.93 90.07 Volume: 292.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.112 ORTHORHOMBIC I-lattice R(int) = 0.124 [ 90] Vol = 292.0 Cell: 5.911 8.351 5.916 90.00 89.97 90.07 Volume: 292.04 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.021 MONOCLINIC I-lattice R(int) = 0.124 [ 86] Vol = 292.0 Cell: 5.911 5.916 8.351 90.00 90.07 90.03 Volume: 292.04 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.052 MONOCLINIC I-lattice R(int) = 0.098 [ 21] Vol = 292.0 Cell: 5.906 5.911 8.365 90.00 90.07 90.07 Volume: 292.04 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.145 MONOCLINIC I-lattice R(int) = 0.193 [ 53] Vol = 292.0 Cell: 5.913 5.907 8.361 89.93 90.00 89.91 Volume: 292.04 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.089 [ 1] Vol = 146.0 Cell: 5.906 5.907 5.911 60.03 60.05 60.11 Volume: 146.02 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 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 0 137 0 179 185 264 N (int>3sigma) = 0 0 0 0 137 0 143 153 215 Mean intensity = 0.0 0.0 0.0 0.0 4.1 0.0 11.1 11.6 11.3 Mean int/sigma = 0.0 0.0 0.0 0.0 15.6 0.0 19.9 19.8 20.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.259 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 13 60 N I>3s 0 0 7 60 0.0 0.0 0.1 4.6 1.5 1.5 2.6 18.0 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 0.175 135 Fd-3m 1 1 227 C N N N N 37 2284 0.178 167 0kl, h0l, 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.360989 8.351466 8.364719 90.0519 90.0519 90.0527 ZERR 1.00 0.000884 0.004937 0.008380 0.0082 0.0325 0.0067 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4808790- 1236429 38 38 28 1.4 2020973.18 48.94 0.649 0.649 1234709- 605273 42 42 28 1.5 892996.03 26.28 0.986 0.986 528899- 227507 44 42 28 1.5 335723.84 22.29 0.400 0.400 227148- 158960 43 41 28 1.5 189359.49 15.11 0.162 0.162 151780- 113309 35 34 28 1.2 133736.88 11.29 0.269 0.269 112187- 8473 34 33 28 1.2 83355.63 9.93 0.135 0.135 7244- 1126 34 34 31 1.1 4060.07 1.90 0.242 0.242 ------------------------------------------------------------------------------------------- 4808790- 1126 270 264 199 1.3 543949.95 20.06 0.679 0.679 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-1.05 48 43 29 1.5 812053.87 36.95 0.794 0.794 0.017 1.03-0.82 40 39 29 1.3 700459.94 25.14 0.770 0.770 0.025 0.82-0.69 39 39 29 1.3 655448.66 20.19 0.552 0.552 0.031 0.69-0.61 40 40 28 1.4 475506.17 15.42 0.663 0.663 0.039 0.60-0.53 40 40 28 1.4 479278.26 14.86 0.508 0.508 0.041 0.53-0.49 34 34 28 1.2 285777.25 12.03 0.556 0.556 0.052 0.48-0.40 29 29 28 1.0 272283.83 10.98 0.982 0.982 0.054 ------------------------------------------------------------------------------------------------------ inf-0.40 270 264 199 1.3 543949.95 20.06 0.679 0.679 0.032 inf-0.60 170 164 117 1.4 671611.18 24.76 0.674 0.674 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.05 43 34 29 85.3 1.5 812053.87 52.68 0.794 0.015 1.03-0.82 39 33 29 87.9 1.3 700459.94 32.44 0.770 0.022 0.82-0.69 39 38 29 76.3 1.3 655448.66 26.71 0.552 0.023 0.69-0.61 40 46 28 60.9 1.4 475506.17 21.66 0.663 0.030 0.60-0.53 40 60 28 46.7 1.4 479278.26 19.83 0.508 0.034 0.53-0.49 34 66 28 42.4 1.2 285777.25 13.86 0.556 0.053 0.48-0.40 29 181 28 15.5 1.0 272283.83 11.96 0.982 0.033 -------------------------------------------------------------------------------------------- inf-0.40 264 458 199 43.4 1.3 543949.95 26.71 0.679 0.025 inf-0.60 164 155 117 75.5 1.4 671611.18 33.87 0.674 0.021 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.034810 -0.077049 0.007522 ( 0.000020 0.000024 0.000014 ) 0.008107 0.011899 0.083587 ( 0.000019 0.000023 0.000014 ) -0.076938 -0.033692 0.012126 ( 0.000025 0.000030 0.000018 ) M - matrix: 0.007197 0.000007 0.000007 ( 0.000004 0.000003 0.000002 ) 0.000007 0.007213 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000007 0.000007 0.007190 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.034810 -0.077049 0.007522 ( 0.000020 0.000024 0.000014 ) 0.008107 0.011899 0.083587 ( 0.000019 0.000023 0.000014 ) -0.076938 -0.033692 0.012126 ( 0.000025 0.000030 0.000018 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) unit cell: 8.361(2) 8.351(2) 8.3647(14) 90.052(18) 90.052(18) 90.05(2) V = 584.1(3) unit cell: 8.3591(5) 8.3591(5) 8.3591(5) 90.0 90.0 90.0 V = 584.08(6) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.921) PROFFIT INFO: signal sum: min=524.0000 max=19734144.0000 PROFFIT INFO: signal sum lp corr: min=691.9651 max=2247941.6347 PROFFIT INFO: background sum: min=872.0000 max=15463.0000 PROFFIT INFO: background sum sig2: min=740.0000 max=8870.0000 PROFFIT INFO: num of signal pixels: min=68 max=519 PROFFIT INFO: Inet: min=1509.7421 max=4904600.5000 PROFFIT INFO: sig(Inet): min=247.9734 max=63802.9531 PROFFIT INFO: Inet/sig(Inet): min=1.37 max=228.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 42 68 118 126 208 348 484 540 Percent 0.0 0.0 0.7 7.8 12.6 21.9 23.3 38.5 64.4 89.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 270 100.00 (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 270 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4904601- 1708197 27 2653146.43 143.81 100.00 1699683- 1154647 27 1408079.19 110.13 100.00 1150972- 367360 27 585785.83 93.87 100.00 365089- 228495 27 270884.58 70.16 100.00 227802- 184614 27 209367.41 52.15 100.00 177893- 150345 27 162376.49 35.37 100.00 149332- 107216 27 125643.91 29.78 100.00 107195- 6315 27 59877.10 20.64 100.00 6147- 3990 27 5043.28 4.92 85.19 3962- 1510 27 3246.18 3.44 37.04 ------------------------------------------------------------------------------------ 4904601- 1510 270 548345.04 56.43 92.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.32 27 1042035.17 82.35 100.00 1.27- 1.09 27 817320.30 82.26 100.00 1.09- 0.93 27 689427.47 80.75 100.00 0.92- 0.84 27 607804.04 64.02 96.30 0.84- 0.78 27 531291.29 59.24 96.30 0.78- 0.73 27 323853.36 40.86 92.59 0.73- 0.69 27 453358.19 45.18 92.59 0.69- 0.65 27 434471.25 43.26 77.78 0.64- 0.62 27 363718.33 38.31 81.48 0.62- 0.59 27 220171.00 28.04 85.19 ------------------------------------------------------------------------------------ 4.17- 0.59 270 548345.04 56.43 92.22 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:23:09 2018 Sorting 270 observations 61 unique observations with > 7.00 F2/sig(F2) 270 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Maximum number of 61 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 270 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 219 observations > 7.00 F2/sig(F2) 219 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Removing 'redundancy=1' reflections Average redundancy: 3.3 (Out of 219 removed 17 = 202, unique = 61) 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 202 observations in 1 runs Run # start # end # total # 1 1 49 49 Total number of frames 49 Frame #40 of 49 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 61 unique data precomputed (should be 61) 61 unique data with 202 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.3 (Out of 202 removed 0 = 202, unique = 61) 61 unique data precomputed (should be 61) 61 unique data with 202 observations RMS deviation of equivalent data = 0.08955 Rint = 0.06753 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.06753, wR= 0.09486 Trying model 1 (ne=2, no=0)... Results: Rint= 0.03025, wR= 0.03856, Acormin=0.717, Acormax=1.086, Acor_av=0.880 F test: Probability=1.000, F= 4.807 Trying model 2 (ne=2, no=1)... Results: Rint= 0.02722, wR= 0.03474, Acormin=0.731, Acormax=1.194, Acor_av=0.891 F test: Probability=0.862, F= 1.208 Trying model 3 (ne=4, no=0)... Results: Rint= 0.01902, wR= 0.02471, Acormin=0.723, Acormax=1.275, Acor_av=0.950 F test: Probability=1.000, F= 2.363 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01614, wR= 0.02252, Acormin=0.740, Acormax=1.397, Acor_av=0.954 F test: Probability=0.955, F= 1.355 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01376, wR= 0.01901, Acormin=0.776, Acormax=1.387, Acor_av=0.972 F test: Probability=0.923, F= 1.300 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01320, wR= 0.01922, Acormin=0.774, Acormax=1.371, Acor_av=0.971 F test: Probability=0.958, F= 1.376 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01304, wR= 0.01848, Acormin=0.782, Acormax=1.381, Acor_av=0.972 F test: Probability=0.000, F= 0.996 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01112, wR= 0.01520, Acormin=0.800, Acormax=1.396, Acor_av=0.979 F test: Probability=0.902, F= 1.284 Trying model 9 (ne=6, no=5)... Results: Rint= 0.00985, wR= 0.01363, Acormin=0.750, Acormax=1.419, Acor_av=0.981 F test: Probability=0.971, F= 1.464 Final absorption model (ne=6, no=5): Rint= 0.00985, Acormin=0.750, Acormax=1.419, Acor_av=0.981 Combined refinement in use Rint: 0.06771 There are 48 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 95 pars with 4560 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.08955 Using Levenberg-Marquardt: 0.00010 New wR= 0.01485 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.06753 with corrections 0.01019 Rint for all data: 0.06771 with corrections 0.01045 0 observations identified as outliers and rejected Cycle 2 wR= 0.01485 Using Levenberg-Marquardt: 0.00001 New wR= 0.01103 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.06753 with corrections 0.00800 Rint for all data: 0.06771 with corrections 0.00827 0 observations identified as outliers and rejected Cycle 3 wR= 0.01103 Using Levenberg-Marquardt: 0.00000 New wR= 0.01057 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.06753 with corrections 0.00759 Rint for all data: 0.06771 with corrections 0.00786 0 observations identified as outliers and rejected Cycle 4 wR= 0.01057 Using Levenberg-Marquardt: 0.00000 New wR= 0.01018 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.06753 with corrections 0.00722 Rint for all data: 0.06771 with corrections 0.00749 0 observations identified as outliers and rejected Cycle 5 wR= 0.01018 Using Levenberg-Marquardt: 0.00000 New wR= 0.01011 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.06753 with corrections 0.00708 Rint for all data: 0.06771 with corrections 0.00735 0 observations identified as outliers and rejected Final wR= 0.01011 Final frame scales: Min= 0.9627 Max= 1.0962 Final absorption correction factors: Amin= 0.7065 Amax= 2.3143 PROFFIT INFO: Inet (after scale3 abspack): min=1609.5217 max=4425945.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=187.6747 max=60619.0625 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:2/50 270 reflections read from tmp file 20 reflections are rejected (1 as outliers, 19 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 21 29 9 6 8 1 Initial Chi^2= 0.23497 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.52566 Current error model SIG(F2)^2 = 171.36*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 90.08*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 90.08*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4425945- 1693064 27 2604853.42 151.03 100.00 1688678- 1117720 27 1408929.19 75.06 100.00 1117552- 334928 27 589915.12 64.63 100.00 330391- 230497 27 264597.46 50.51 100.00 229649- 174557 27 212058.32 34.95 100.00 167815- 141320 27 159988.62 24.57 100.00 140940- 113924 27 125459.92 22.04 100.00 113452- 6592 27 61802.25 15.12 100.00 6452- 4041 27 4917.74 4.66 100.00 3985- 1610 27 3226.63 4.51 88.89 ------------------------------------------------------------------------------------ 4425945- 1610 270 543574.87 44.71 98.89 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.32 27 1047135.07 98.53 100.00 1.27- 1.09 27 771949.25 67.28 100.00 1.09- 0.93 27 712501.41 56.23 100.00 0.92- 0.84 27 586328.74 44.82 100.00 0.84- 0.78 27 536462.25 41.49 100.00 0.78- 0.73 27 317441.43 28.98 100.00 0.73- 0.69 27 450708.79 31.93 100.00 0.69- 0.65 27 438342.65 30.53 92.59 0.64- 0.62 27 355036.14 27.14 100.00 0.62- 0.59 27 219842.94 20.13 96.30 ------------------------------------------------------------------------------------ 4.17- 0.59 270 543574.87 44.71 98.89 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.17- 1.32 27 1047135.07 98.53 100.00 4.17- 1.09 54 909542.16 82.90 100.00 4.17- 0.93 81 843861.91 74.01 100.00 4.17- 0.84 108 779478.62 66.71 100.00 4.17- 0.78 135 730875.34 61.67 100.00 4.17- 0.73 162 661969.69 56.22 100.00 4.17- 0.69 189 631789.56 52.75 100.00 4.17- 0.65 216 607608.70 49.97 99.07 4.17- 0.62 243 579545.08 47.44 99.18 4.17- 0.59 270 543574.87 44.71 98.89 ------------------------------------------------------------------------------------ 4.17- 0.59 270 543574.87 44.71 98.89 Scale applied to data: s=0.225940 (maximum obs:4425945.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.007; Rsigma 0.014: data 270 -> merged 93 With outlier rejection... Rint 0.007; Rsigma 0.014: data 268 -> merged 93 Rejected total: 2, method kkm 2, method Blessing 0 Completeness direct cell (a, b, c) = (8.359, 8.359, 8.359), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586691, 4.179527 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 7 10 1.71 70.00 12 1.61 - 1.21 8 10 2.88 80.00 23 1.17 - 1.01 10 10 3.10 100.00 31 0.99 - 0.89 10 10 3.20 100.00 32 0.88 - 0.81 10 10 2.90 100.00 29 0.81 - 0.74 10 10 2.80 100.00 28 0.73 - 0.71 10 10 2.90 100.00 29 0.70 - 0.66 9 10 2.89 90.00 26 0.65 - 0.64 7 10 3.00 70.00 21 0.63 - 0.60 9 10 2.78 90.00 25 --------------------------------------------------------------- 5.91 - 0.60 90 100 2.84 90.00 256 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:23:08 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.911464 5.910752 5.906027 60.0487 89.9347 59.9584 264 Reflections read from file xs1715a.hkl; mean (I/sigma) = 20.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 129 137 130 134 198 185 184 264 N (int>3sigma) = 0 102 137 103 103 171 153 149 215 Mean intensity = 0.0 10.9 4.1 10.9 9.3 8.6 11.6 11.4 11.3 Mean int/sigma = 0.0 18.8 15.6 19.2 16.6 17.9 19.8 20.5 20.1 Lattice type: P chosen Volume: 146.02 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 Unitcell: 5.906 5.907 5.911 60.03 60.05 60.11 Niggli form: a.a = 34.881 b.b = 34.897 c.c = 34.937 b.c = 17.444 a.c = 17.429 a.b = 17.389 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.079 CUBIC F-lattice R(int) = 0.175 [ 138] Vol = 584.1 Cell: 8.361 8.351 8.365 90.05 90.05 90.05 Volume: 584.08 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.154 [ 40] Vol = 438.1 Cell: 5.916 5.913 14.465 90.07 89.98 120.03 Volume: 438.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 8] Vol = 438.1 Trigonal Cell: 5.916 5.913 14.465 90.07 89.98 120.03 Volume: 438.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 126] Vol = 438.1 Cell: 5.906 5.916 14.483 89.98 89.99 120.04 Volume: 438.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.139 [ 30] Vol = 438.1 Trigonal Cell: 5.906 5.916 14.483 89.98 89.99 120.04 Volume: 438.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.159 [ 83] Vol = 292.0 Cell: 5.906 5.911 8.365 90.00 89.93 90.07 Volume: 292.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.112 ORTHORHOMBIC I-lattice R(int) = 0.124 [ 90] Vol = 292.0 Cell: 5.911 8.351 5.916 90.00 89.97 90.07 Volume: 292.04 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.021 MONOCLINIC I-lattice R(int) = 0.124 [ 86] Vol = 292.0 Cell: 5.911 5.916 8.351 90.00 90.07 90.03 Volume: 292.04 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.052 MONOCLINIC I-lattice R(int) = 0.098 [ 21] Vol = 292.0 Cell: 5.906 5.911 8.365 90.00 90.07 90.07 Volume: 292.04 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.145 MONOCLINIC I-lattice R(int) = 0.193 [ 53] Vol = 292.0 Cell: 5.913 5.907 8.361 89.93 90.00 89.91 Volume: 292.04 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.089 [ 1] Vol = 146.0 Cell: 5.906 5.907 5.911 60.03 60.05 60.11 Volume: 146.02 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 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 0 137 0 179 185 264 N (int>3sigma) = 0 0 0 0 137 0 143 153 215 Mean intensity = 0.0 0.0 0.0 0.0 4.1 0.0 11.1 11.6 11.3 Mean int/sigma = 0.0 0.0 0.0 0.0 15.6 0.0 19.9 19.8 20.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.259 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 13 60 N I>3s 0 0 7 60 0.0 0.0 0.1 4.6 1.5 1.5 2.6 18.0 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 0.175 135 Fd-3m 1 1 227 C N N N N 37 2284 0.178 167 0kl, h0l, 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.360989 8.351466 8.364719 90.0519 90.0519 90.0527 ZERR 1.00 0.000884 0.004937 0.008380 0.0082 0.0325 0.0067 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4377124- 334793 81 80 31 2.6 1498343.98 95.55 0.005 0.005 330895- 120372 101 101 31 3.3 195483.06 33.75 0.015 0.015 118629- 1988 88 87 31 2.8 31279.98 9.27 0.043 0.045 ------------------------------------------------------------------------------------------- 4377124- 1988 270 268 93 2.9 531092.04 44.25 0.007 0.007 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-0.92 89 87 32 2.7 756095.10 70.03 0.007 0.007 0.009 0.91-0.71 92 92 31 3.0 483628.60 36.79 0.007 0.007 0.016 0.71-0.59 89 89 30 3.0 360208.56 26.76 0.009 0.010 0.022 ------------------------------------------------------------------------------------------------------ inf-0.59 270 268 93 2.9 531092.04 44.25 0.007 0.007 0.014 inf-0.60 256 254 89 2.9 555881.48 45.91 0.007 0.007 0.014 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-0.92 87 37 32 86.5 2.7 756095.10 117.22 0.007 0.005 0.91-0.71 92 31 31 100.0 3.0 483628.60 67.24 0.007 0.009 0.71-0.59 89 40 30 75.0 3.0 360208.56 50.76 0.009 0.013 -------------------------------------------------------------------------------------------- inf-0.59 268 108 93 86.1 2.9 531092.04 77.99 0.007 0.008 inf-0.60 254 99 89 89.9 2.9 555881.48 80.81 0.007 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:28:50 2018) ID: 2932; threads 39; handles 878; mem 519060.00 (1237724.00)kB; time: 1w 5d 21h 34m 20s MEMORY INFO: Memory PF:0.0, Ph:165.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.9,peak PF: 708.5, WS: 271.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:165.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.7,peak PF: 708.5, WS: 272.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:28:50 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000029 0.000028 0.000039 ) 0.087412 -0.166882 0.063604 ( 0.000029 0.000028 0.000039 ) 0.055227 -0.024260 0.122680 ( 0.000038 0.000036 0.000050 ) 5.91535 ( 0.00171 ) 5.92288 ( 0.00161 ) 5.91286 ( 0.00241 ) 59.95509 ( 0.03520 ) 89.89521 ( 0.02785 ) 59.99590 ( 0.02944 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 12:28:50 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000029 0.000028 0.000039 ) 0.087412 -0.166882 0.063604 ( 0.000029 0.000028 0.000039 ) 0.055227 -0.024260 0.122680 ( 0.000038 0.000036 0.000050 ) M - matrix: 0.021587 -0.014381 0.007161 ( 0.000009 0.000007 0.000008 ) -0.014381 0.028762 -0.014355 ( 0.000007 0.000009 0.000008 ) 0.007161 -0.014355 0.021588 ( 0.000008 0.000008 0.000014 ) unit cell: 5.9154(17) 5.9229(16) 5.913(2) 59.96(3) 89.90(3) 60.00(3) V = 146.51(8) 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\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb PROFFITPEAK info: 922 peaks in the peak location table UB fit with 392 obs out of 421 (total:421,skipped:0) (93.11%) UB - matrix: -0.104177 -0.015273 0.049963 ( 0.000067 0.000063 0.000081 ) 0.087128 -0.166801 0.063633 ( 0.000074 0.000069 0.000090 ) 0.055313 -0.024043 0.122617 ( 0.000080 0.000075 0.000097 ) M - matrix: 0.021504 -0.014272 0.007122 ( 0.000021 0.000016 0.000017 ) -0.014272 0.028634 -0.014325 ( 0.000016 0.000024 0.000019 ) 0.007122 -0.014325 0.021580 ( 0.000017 0.000019 0.000028 ) unit cell: 5.913(4) 5.917(4) 5.908(5) 59.99(7) 89.93(6) 60.09(6) V = 146.43(17) UB fit with 392 obs out of 421 (total:421,skipped:0) (93.11%) UB - matrix: -0.104177 -0.015273 0.049963 ( 0.000067 0.000063 0.000081 ) 0.087128 -0.166801 0.063633 ( 0.000074 0.000069 0.000090 ) 0.055313 -0.024043 0.122617 ( 0.000080 0.000075 0.000097 ) M - matrix: 0.021504 -0.014272 0.007122 ( 0.000021 0.000016 0.000017 ) -0.014272 0.028634 -0.014325 ( 0.000016 0.000024 0.000019 ) 0.007122 -0.014325 0.021580 ( 0.000017 0.000019 0.000028 ) unit cell: 5.913(4) 5.917(4) 5.908(5) 59.99(7) 89.93(6) 60.09(6) V = 146.43(17) OTKP changes: 75 1 1 1 UB - matrix: -0.104141 -0.015068 0.049640 ( 0.000064 0.000060 0.000078 ) 0.087247 -0.166754 0.063602 ( 0.000070 0.000065 0.000085 ) 0.055290 -0.024198 0.122506 ( 0.000079 0.000074 0.000096 ) M - matrix: 0.021514 -0.014318 0.007153 ( 0.000020 0.000015 0.000016 ) -0.014318 0.028620 -0.014318 ( 0.000015 0.000022 0.000018 ) 0.007153 -0.014318 0.021517 ( 0.000016 0.000018 0.000027 ) UB fit with 390 obs out of 421 (total:421,skipped:0) (92.64%) unit cell: 5.921(4) 5.928(3) 5.920(5) 60.00(7) 89.96(6) 60.00(6) V = 146.97(16) UB fit with 390 obs out of 421 (total:421,skipped:0) (92.64%) UB - matrix: -0.104141 -0.015068 0.049640 ( 0.000064 0.000060 0.000078 ) 0.087247 -0.166754 0.063602 ( 0.000070 0.000065 0.000085 ) 0.055290 -0.024198 0.122506 ( 0.000079 0.000074 0.000096 ) M - matrix: 0.021514 -0.014318 0.007153 ( 0.000020 0.000015 0.000016 ) -0.014318 0.028620 -0.014318 ( 0.000015 0.000022 0.000018 ) 0.007153 -0.014318 0.021517 ( 0.000016 0.000018 0.000027 ) unit cell: 5.921(4) 5.928(3) 5.920(5) 60.00(7) 89.96(6) 60.00(6) V = 146.97(16) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 421 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Run 1 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.983) HKL list info: 585 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104141 -0.015068 0.049640 ( 0.000064 0.000060 0.000078 ) 0.087247 -0.166754 0.063602 ( 0.000070 0.000065 0.000085 ) 0.055290 -0.024198 0.122506 ( 0.000079 0.000074 0.000096 ) M - matrix: 0.021514 -0.014318 0.007153 ( 0.000020 0.000015 0.000016 ) -0.014318 0.028620 -0.014318 ( 0.000015 0.000022 0.000018 ) 0.007153 -0.014318 0.021517 ( 0.000016 0.000018 0.000027 ) UB fit with 390 obs out of 421 (total:421,skipped:0) (92.64%) unit cell: 5.921(4) 5.928(3) 5.920(5) 60.00(7) 89.96(6) 60.00(6) V = 146.97(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 393 obs out of 421 (total:421,skipped:0) (93.35%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb 7 of 312 peaks identified as outliers and rejected 305 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 305 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 305 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.42 | 31 | 0.980 ( 0.157) | 1.185 ( 0.607) | 1.316 ( 0.748) | 1.42- 1.12 | 31 | 1.093 ( 0.076) | 1.195 ( 0.182) | 1.137 ( 0.493) | 1.09- 0.97 | 31 | 1.139 ( 0.079) | 1.226 ( 0.267) | 1.222 ( 0.471) | 0.97- 0.85 | 31 | 1.150 ( 0.053) | 1.167 ( 0.120) | 1.209 ( 0.431) | 0.84- 0.81 | 31 | 1.178 ( 0.051) | 1.205 ( 0.146) | 1.181 ( 0.400) | 0.81- 0.73 | 31 | 1.182 ( 0.047) | 1.156 ( 0.144) | 1.336 ( 0.409) | 0.73- 0.70 | 31 | 1.199 ( 0.047) | 1.198 ( 0.176) | 1.344 ( 0.449) | 0.69- 0.65 | 31 | 1.209 ( 0.056) | 1.198 ( 0.151) | 1.342 ( 0.442) | 0.64- 0.62 | 31 | 1.197 ( 0.083) | 1.228 ( 0.153) | 1.147 ( 0.420) | 0.62- 0.59 | 26 | 1.211 ( 0.065) | 1.226 ( 0.220) | 1.309 ( 0.494) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 305 | 1.153 ( 0.103) | 1.198 ( 0.258) | 1.253 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 305 obs out of 305 (total:305,skipped:0) (100.00%) UB - matrix: -0.104252 -0.014808 0.049363 ( 0.000033 0.000031 0.000036 ) 0.087422 -0.166978 0.063576 ( 0.000024 0.000022 0.000026 ) 0.055231 -0.024396 0.122608 ( 0.000031 0.000028 0.000033 ) M - matrix: 0.021562 -0.014401 0.007184 ( 0.000009 0.000006 0.000006 ) -0.014401 0.028696 -0.014338 ( 0.000006 0.000008 0.000006 ) 0.007184 -0.014338 0.021511 ( 0.000006 0.000006 0.000009 ) unit cell: 5.9244(17) 5.9280(12) 5.9216(18) 60.03(3) 89.95(2) 59.87(3) V = 146.89(6) OTKP changes: 305 1 1 1 UB - matrix: -0.104335 -0.015025 0.049777 ( 0.000027 0.000025 0.000029 ) 0.087404 -0.167200 0.063698 ( 0.000021 0.000020 0.000023 ) 0.055402 -0.024274 0.122791 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021595 -0.014391 0.007177 ( 0.000007 0.000005 0.000006 ) -0.014391 0.028771 -0.014379 ( 0.000005 0.000007 0.000006 ) 0.007177 -0.014379 0.021613 ( 0.000006 0.000006 0.000009 ) UB fit with 305 obs out of 305 (total:305,skipped:0) (100.00%) unit cell: 5.9116(14) 5.9126(11) 5.9054(16) 60.02(2) 89.94(2) 59.96(2) V = 145.98(6) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.895) HKL list info: 581 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104335 -0.015025 0.049777 ( 0.000027 0.000025 0.000029 ) 0.087404 -0.167200 0.063698 ( 0.000021 0.000020 0.000023 ) 0.055402 -0.024274 0.122791 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021595 -0.014391 0.007177 ( 0.000007 0.000005 0.000006 ) -0.014391 0.028771 -0.014379 ( 0.000005 0.000007 0.000006 ) 0.007177 -0.014379 0.021613 ( 0.000006 0.000006 0.000009 ) UB fit with 305 obs out of 305 (total:305,skipped:0) (100.00%) unit cell: 5.9116(14) 5.9126(11) 5.9054(16) 60.02(2) 89.94(2) 59.96(2) V = 145.98(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 305 obs out of 305 (total:305,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb 4 of 307 peaks identified as outliers and rejected 303 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 303 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 303 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 30 | 1.012 ( 0.224) | 1.283 ( 0.765) | 1.503 ( 1.132) | 1.41- 1.12 | 30 | 1.103 ( 0.070) | 1.187 ( 0.096) | 1.214 ( 0.636) | 1.12- 0.96 | 30 | 1.133 ( 0.082) | 1.196 ( 0.281) | 1.298 ( 0.540) | 0.96- 0.85 | 30 | 1.148 ( 0.054) | 1.159 ( 0.120) | 1.218 ( 0.435) | 0.85- 0.81 | 30 | 1.180 ( 0.052) | 1.195 ( 0.146) | 1.194 ( 0.402) | 0.81- 0.75 | 30 | 1.180 ( 0.048) | 1.157 ( 0.146) | 1.300 ( 0.442) | 0.74- 0.71 | 30 | 1.194 ( 0.043) | 1.203 ( 0.131) | 1.346 ( 0.444) | 0.71- 0.66 | 30 | 1.209 ( 0.045) | 1.204 ( 0.167) | 1.258 ( 0.363) | 0.66- 0.62 | 30 | 1.205 ( 0.087) | 1.231 ( 0.174) | 1.314 ( 0.523) | 0.62- 0.59 | 33 | 1.200 ( 0.069) | 1.222 ( 0.200) | 1.277 ( 0.454) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 303 | 1.157 ( 0.109) | 1.204 ( 0.292) | 1.292 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 30 | 1.150 ( 0.049) | 1.267 ( 0.228) | 1.428 ( 0.633) | 13.1-19.2 | 30 | 1.160 ( 0.162) | 1.304 ( 0.511) | 1.364 ( 1.011) | 19.3-23.2 | 30 | 1.178 ( 0.069) | 1.329 ( 0.400) | 1.262 ( 0.620) | 23.4-27.5 | 30 | 1.121 ( 0.101) | 1.154 ( 0.113) | 1.341 ( 0.477) | 27.5-30.6 | 30 | 1.128 ( 0.105) | 1.194 ( 0.160) | 1.206 ( 0.387) | 30.7-33.6 | 30 | 1.155 ( 0.070) | 1.200 ( 0.335) | 1.251 ( 0.435) | 33.8-36.7 | 30 | 1.154 ( 0.080) | 1.177 ( 0.176) | 1.257 ( 0.419) | 36.7-39.8 | 30 | 1.138 ( 0.123) | 1.133 ( 0.185) | 1.263 ( 0.489) | 39.9-43.3 | 30 | 1.162 ( 0.104) | 1.148 ( 0.236) | 1.229 ( 0.568) | 43.5-49.9 | 33 | 1.216 ( 0.141) | 1.138 ( 0.256) | 1.318 ( 0.495) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 303 | 1.157 ( 0.109) | 1.204 ( 0.292) | 1.292 ( 0.582) | Fitted profile normalization line parameters e1 dimension: a=0.0015 b=0.97 e2 dimension: a=-0.0013 b=1.04 e3 dimension: a=-0.0003 b=1.02 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6425 lp-corr: 5353 Maximum peak integral for reflections I/sig<= 100 - raw: 464319 lp-corr: 640871 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2289399 PROFFITPEAK - Finished at Wed Mar 28 12:28:55 2018 PROFFITMAIN - Started at Wed Mar 28 12:28:55 2018 OTKP changes: 303 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 303 1 1 1 UB - matrix: -0.104387 -0.014982 0.049779 ( 0.000032 0.000030 0.000035 ) 0.087420 -0.167253 0.063732 ( 0.000021 0.000020 0.000023 ) 0.055405 -0.024268 0.122809 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021609 -0.014402 0.007179 ( 0.000008 0.000005 0.000006 ) -0.014402 0.028787 -0.014386 ( 0.000005 0.000007 0.000006 ) 0.007179 -0.014386 0.021622 ( 0.000006 0.000006 0.000009 ) UB fit with 303 obs out of 303 (total:303,skipped:0) (100.00%) unit cell: 5.9101(17) 5.9115(12) 5.9041(17) 60.02(2) 89.93(2) 59.95(2) V = 145.88(6) *** 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= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.871) HKL list info: 581 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104387 -0.014982 0.049779 ( 0.000032 0.000030 0.000035 ) 0.087420 -0.167253 0.063732 ( 0.000021 0.000020 0.000023 ) 0.055405 -0.024268 0.122809 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021609 -0.014402 0.007179 ( 0.000008 0.000005 0.000006 ) -0.014402 0.028787 -0.014386 ( 0.000005 0.000007 0.000006 ) 0.007179 -0.014386 0.021622 ( 0.000006 0.000006 0.000009 ) UB fit with 303 obs out of 303 (total:303,skipped:0) (100.00%) unit cell: 5.9101(17) 5.9115(12) 5.9041(17) 60.02(2) 89.93(2) 59.95(2) V = 145.88(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 303 obs out of 303 (total:303,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! 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: -0.104387 -0.014982 0.049779 ( 0.000032 0.000030 0.000035 ) 0.087420 -0.167253 0.063732 ( 0.000021 0.000020 0.000023 ) 0.055405 -0.024268 0.122809 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021609 -0.014402 0.007179 ( 0.000008 0.000005 0.000006 ) -0.014402 0.028787 -0.014386 ( 0.000005 0.000007 0.000006 ) 0.007179 -0.014386 0.021622 ( 0.000006 0.000006 0.000009 ) UB fit with 303 obs out of 303 (total:303,skipped:0) (100.00%) unit cell: 5.9101(17) 5.9115(12) 5.9041(17) 60.02(2) 89.93(2) 59.95(2) V = 145.88(6) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104387 -0.014982 0.049779 ( 0.000032 0.000030 0.000035 ) 0.087420 -0.167253 0.063732 ( 0.000021 0.000020 0.000023 ) 0.055405 -0.024268 0.122809 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021609 -0.014402 0.007179 ( 0.000008 0.000005 0.000006 ) -0.014402 0.028787 -0.014386 ( 0.000005 0.000007 0.000006 ) 0.007179 -0.014386 0.021622 ( 0.000006 0.000006 0.000009 ) UB fit with 303 obs out of 303 (total:303,skipped:0) (100.00%) unit cell: 5.9101(17) 5.9115(12) 5.9041(17) 60.02(2) 89.93(2) 59.95(2) V = 145.88(6) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 19 reflections under beam stop or inside a detector rejection region 6 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof 414 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:28:56 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.871) PROFFIT INFO: signal sum: min=506.0000 max=19744344.0000 PROFFIT INFO: signal sum lp corr: min=715.8997 max=2235181.8372 PROFFIT INFO: background sum: min=957.0000 max=16421.0000 PROFFIT INFO: background sum sig2: min=676.0000 max=9278.0000 PROFFIT INFO: num of signal pixels: min=68 max=541 PROFFIT INFO: Inet: min=1561.9629 max=4876760.5000 PROFFIT INFO: sig(Inet): min=248.5124 max=63967.4102 PROFFIT INFO: Inet/sig(Inet): min=1.22 max=252.92 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 30 51 89 95 156 271 367 414 Percent 0.0 0.0 1.0 7.2 12.3 21.5 22.9 37.7 65.5 88.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 414 100.00 (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 414 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4876761- 1796122 41 2616038.27 145.82 100.00 1772680- 1098202 41 1414688.45 110.92 100.00 1056410- 369249 41 607845.17 97.32 100.00 368236- 232078 41 278210.65 69.62 100.00 231707- 185668 41 212379.57 53.63 100.00 185605- 153718 41 166682.54 37.05 100.00 153357- 107815 41 130532.89 30.84 100.00 107585- 6644 41 65324.79 22.67 100.00 6563- 4203 41 5168.18 5.16 87.80 4182- 1562 45 3279.10 3.47 44.44 ------------------------------------------------------------------------------------ 4876761- 1562 414 544732.49 57.13 92.75 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.25- 1.27 41 757923.15 90.18 100.00 1.27- 0.98 41 826612.03 75.56 97.56 0.98- 0.82 41 586927.27 59.57 97.56 0.82- 0.73 41 684113.49 70.15 95.12 0.73- 0.65 41 542734.75 60.14 92.68 0.65- 0.60 41 547821.99 54.34 92.68 0.60- 0.55 41 432532.44 46.96 95.12 0.55- 0.51 41 445865.67 45.41 82.93 0.51- 0.48 41 325934.33 35.96 85.37 0.47- 0.40 45 318892.90 35.14 88.89 ------------------------------------------------------------------------------------ 5.25- 0.40 414 544732.49 57.13 92.75 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:28:56 2018 Sorting 414 observations 94 unique observations with > 7.00 F2/sig(F2) 414 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Maximum number of 94 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 414 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Frame #8 of 74 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 334 observations > 7.00 F2/sig(F2) 334 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Frame #8 of 74 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: 2.3 (Out of 334 removed 156 = 178, unique = 77) 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 178 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Frame #8 of 74 skipped from refinement Frame #28 of 74 skipped from refinement Frame #33 of 74 skipped from refinement Frame #40 of 74 skipped from refinement Frame #42 of 74 skipped from refinement Frame #45 of 74 skipped from refinement Frame #48 of 74 skipped from refinement Frame #52 of 74 skipped from refinement Frame #55 of 74 skipped from refinement Frame #56 of 74 skipped from refinement Frame #64 of 74 skipped from refinement Frame #71 of 74 skipped from refinement 12 frames need to be skipped from refinement, because of missing redundant and/or observable data 77 unique data precomputed (should be 77) 77 unique data with 178 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.3 (Out of 178 removed 0 = 178, unique = 77) 77 unique data precomputed (should be 77) 77 unique data with 178 observations RMS deviation of equivalent data = 0.62411 Rint = 0.60335 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.60335, wR= 5.08423 Trying model 1 (ne=2, no=0)... Results: Rint= 0.82238, wR= 4.71223, Acormin=-0.582, Acormax=1.296, Acor_av=0.198 F test: Probability=0.000, F= 0.512 Trying model 2 (ne=2, no=1)... Results: Rint= 0.87671, wR= 6.59691, Acormin=-0.657, Acormax=0.965, Acor_av=-0.032 F test: Probability=0.000, F= 0.436 Trying model 3 (ne=4, no=0)... Results: Rint= 0.87421, wR= 2.81815, Acormin=-0.245, Acormax=0.788, Acor_av=0.024 F test: Probability=0.000, F= 0.410 Trying model 4 (ne=4, no=1)... Results: Rint= 0.57539, wR= 4.23322, Acormin=-0.803, Acormax=0.364, Acor_av=-0.057 F test: Probability=0.000, F= 0.914 Trying model 5 (ne=4, no=3)... Results: Rint= 0.75486, wR= 6.38928, Acormin=-0.209, Acormax=1.496, Acor_av=-0.002 F test: Probability=0.000, F= 0.487 Trying model 6 (ne=6, no=0)... Results: Rint= 0.78263, wR= 3.85790, Acormin=-0.185, Acormax=0.438, Acor_av=0.003 F test: Probability=0.000, F= 0.435 Trying model 7 (ne=6, no=1)... Results: Rint= 0.63562, wR= 4.60162, Acormin=-0.189, Acormax=0.369, Acor_av=-0.012 F test: Probability=0.000, F= 0.633 Trying model 8 (ne=6, no=3)... Results: Rint= 0.83227, wR= 4.85533, Acormin=-0.078, Acormax=1.354, Acor_av=0.013 F test: Probability=0.000, F= 0.333 Trying model 9 (ne=6, no=5)... Results: Rint= 0.24317, wR= 0.87190, Acormin=-0.027, Acormax=0.515, Acor_av=0.012 F test: Probability=1.000, F= 3.231 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: 0.74363 There are 62 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 66 pars with 2211 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.62411 Using Levenberg-Marquardt: 0.00010 New wR= 0.55632 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.55619 Rint for all data: 0.74363 with corrections 0.71691 0 observations identified as outliers and rejected Cycle 2 wR= 0.55632 Using Levenberg-Marquardt: 0.00001 New wR= 0.60376 Using Levenberg-Marquardt: 0.00010 New wR= 0.60025 Using Levenberg-Marquardt: 0.00100 New wR= 0.57230 Using Levenberg-Marquardt: 0.01000 New wR= 0.52957 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.76076 Rint for all data: 0.74363 with corrections 0.82636 0 observations identified as outliers and rejected Cycle 3 wR= 0.52957 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.54247 Using Levenberg-Marquardt: 0.10000 New wR= 0.51368 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.66741 Rint for all data: 0.74363 with corrections 0.77223 0 observations identified as outliers and rejected Cycle 4 wR= 0.51368 Using Levenberg-Marquardt: 0.01000 New wR= 0.57123 Using Levenberg-Marquardt: 0.10000 New wR= 0.50550 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.63724 Rint for all data: 0.74363 with corrections 0.75858 0 observations identified as outliers and rejected Cycle 5 wR= 0.50550 Using Levenberg-Marquardt: 0.01000 New wR= 0.67888 Using Levenberg-Marquardt: 0.10000 New wR= 0.50102 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.60687 Rint for all data: 0.74363 with corrections 0.74196 0 observations identified as outliers and rejected Final wR= 0.50102 Final frame scales: Min= 1.0000 Max= 15.0208 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time with different frame scales initialization There are 62 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 61 pars with 1891 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 2.21705 Using Levenberg-Marquardt: 0.00010 New wR= 0.55709 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.54470 Rint for all data: 0.74363 with corrections 0.71928 0 observations identified as outliers and rejected Cycle 2 wR= 0.55709 Using Levenberg-Marquardt: 0.00001 New wR= 0.52986 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.53950 Rint for all data: 0.74363 with corrections 0.72528 0 observations identified as outliers and rejected Cycle 3 wR= 0.52986 Using Levenberg-Marquardt: 0.00000 New wR= 0.52173 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.54064 Rint for all data: 0.74363 with corrections 0.74366 0 observations identified as outliers and rejected Cycle 4 wR= 0.52173 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.50448 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.53626 Rint for all data: 0.74363 with corrections 0.73794 0 observations identified as outliers and rejected Cycle 5 wR= 0.50448 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.49755 There are 11 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60335 with corrections 0.54143 Rint for all data: 0.74363 with corrections 0.74693 0 observations identified as outliers and rejected Final wR= 0.49755 Final frame scales: Min= 1.0000 Max= 52.8474 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 18 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 17 pars with 153 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.88391 Using Levenberg-Marquardt: 0.00010 New wR= 0.66998 There are 12 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.59922 Rint for all data: 0.74363 with corrections 0.75007 0 observations identified as outliers and rejected Cycle 2 wR= 0.62371 Using Levenberg-Marquardt: 0.00001 New wR= 0.58312 There are 12 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.64833 Rint for all data: 0.74363 with corrections 0.78004 0 observations identified as outliers and rejected Cycle 3 wR= 0.61336 Using Levenberg-Marquardt: 0.00000 New wR= 0.60136 There are 12 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.95024 Rint for all data: 0.74363 with corrections 0.95932 0 observations identified as outliers and rejected Cycle 4 wR= 0.61657 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 New wR= 0.62811 Using Levenberg-Marquardt: 1000.00000 New wR= 0.61661 There are 12 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.95773 Rint for all data: 0.74363 with corrections 0.96520 Final wR= 0.61661 Frame scales out of range! Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 16 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 15 pars with 120 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.82687 Using Levenberg-Marquardt: 0.00010 New wR= 0.62156 There are 11 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.58195 Rint for all data: 0.74363 with corrections 0.73153 0 observations identified as outliers and rejected Cycle 2 wR= 0.61075 Using Levenberg-Marquardt: 0.00001 New wR= 0.58815 There are 11 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.56665 Rint for all data: 0.74363 with corrections 0.72410 0 observations identified as outliers and rejected Cycle 3 wR= 0.59139 Using Levenberg-Marquardt: 0.00000 New wR= 0.57982 There are 11 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.57569 Rint for all data: 0.74363 with corrections 0.72721 0 observations identified as outliers and rejected Cycle 4 wR= 0.58799 Using Levenberg-Marquardt: 0.00000 New wR= 0.58040 There are 11 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.57857 Rint for all data: 0.74363 with corrections 0.72566 0 observations identified as outliers and rejected Cycle 5 wR= 0.58679 Using Levenberg-Marquardt: 0.00000 New wR= 0.58114 There are 11 clusters with unrefined scales (size 1-17) Rint for refined data: 0.60335 with corrections 0.59628 Rint for all data: 0.74363 with corrections 0.73856 0 observations identified as outliers and rejected Final wR= 0.58114 Final frame scales: Min= 0.2005 Max= 1.5027 PROFFIT INFO: Inet (after scale3 abspack): min=743.1957 max=7878627.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=151.1000 max=89021.1328 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:2/75 414 reflections read from tmp file 368 reflections are rejected (185 as outliers, 183 as groups of 1 refl) Redundancy: 1 2+ Number of groups: 0 23 Initial Chi^2= 1.03983 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.75117 Current error model SIG(F2)^2 = 492.67*I_RAW + 0.00*I_BACK+(0.02991*)^2 Cycle 2, Chi^2= 1.00176 Current error model SIG(F2)^2 = 402.02*I_RAW + 0.00*I_BACK+(0.01639*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 3, Chi^2= 0.98222 Current error model SIG(F2)^2 = 434.41*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 426.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 426.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7878628- 1769802 41 3074635.93 59.43 100.00 1744805- 705375 41 1190945.57 41.99 100.00 666015- 348772 41 478672.77 29.91 100.00 340164- 245559 41 285694.47 18.64 100.00 245158- 180533 41 212130.00 19.11 100.00 180135- 114632 41 147074.27 12.75 100.00 113642- 72420 41 89245.03 16.60 100.00 71960- 8776 41 39887.41 7.75 87.80 8524- 4193 41 5983.38 2.36 12.20 4079- 743 45 2340.79 2.11 11.11 ------------------------------------------------------------------------------------ 7878628- 743 414 547343.86 20.88 80.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.25- 1.27 41 875989.75 42.78 100.00 1.27- 0.98 41 776629.60 31.12 80.49 0.98- 0.82 41 644538.24 23.31 87.80 0.82- 0.73 41 673842.45 22.53 73.17 0.73- 0.65 41 579419.75 19.33 87.80 0.65- 0.60 41 578907.69 17.55 73.17 0.60- 0.55 41 385604.80 15.19 80.49 0.55- 0.51 41 439929.15 14.69 75.61 0.51- 0.48 41 281191.48 11.76 70.73 0.47- 0.40 45 264937.52 11.48 75.56 ------------------------------------------------------------------------------------ 5.25- 0.40 414 547343.86 20.88 80.43 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.25- 1.27 41 875989.75 42.78 100.00 5.25- 0.98 82 826309.68 36.95 90.24 5.25- 0.82 123 765719.20 32.40 89.43 5.25- 0.73 164 742750.01 29.94 85.37 5.25- 0.65 205 710083.96 27.81 85.85 5.25- 0.60 246 688221.25 26.10 83.74 5.25- 0.55 287 644990.33 24.54 83.28 5.25- 0.51 328 619357.68 23.31 82.32 5.25- 0.48 369 581783.66 22.03 81.03 5.25- 0.40 414 547343.86 20.88 80.43 ------------------------------------------------------------------------------------ 5.25- 0.40 414 547343.86 20.88 80.43 Scale applied to data: s=0.126926 (maximum obs:7878627.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.739; Rsigma 0.030: data 414 -> merged 274 With outlier rejection... Rint 0.655; Rsigma 0.031: data 386 -> merged 274 Rejected total: 28, method kkm 28, method Blessing 0 Completeness direct cell (a, b, c) = (5.264, 5.264, 5.264), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.403741, 5.264139 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 14 15 1.71 93.33 24 1.46 - 1.12 14 15 1.93 93.33 27 1.07 - 0.96 15 15 1.53 100.00 23 0.96 - 0.85 14 15 1.64 93.33 23 0.85 - 0.78 15 15 1.60 100.00 24 0.78 - 0.73 11 15 1.73 73.33 19 0.73 - 0.69 14 15 1.43 93.33 20 0.69 - 0.65 14 15 1.64 93.33 23 0.65 - 0.63 8 15 1.75 53.33 14 0.63 - 0.60 16 17 1.38 94.12 22 --------------------------------------------------------------- 5.91 - 0.60 135 152 1.62 88.82 219 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:28:56 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.910129 5.911499 5.904089 60.0193 89.9301 59.9480 386 Reflections read from file xs1715a.hkl; mean (I/sigma) = 19.73 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 191 201 188 196 290 266 261 386 N (int>3sigma) = 0 146 201 143 148 245 212 206 308 Mean intensity = 0.0 55.2 26.0 55.8 57.9 45.3 64.4 65.0 65.4 Mean int/sigma = 0.0 18.0 17.1 17.8 18.5 17.6 18.6 19.7 19.7 Lattice type: P chosen Volume: 145.88 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.904 5.906 5.910 90.08 119.95 119.93 Niggli form: a.a = 34.858 b.b = 34.883 c.c = 34.922 b.c = -0.051 a.c = -17.417 a.b = -17.398 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.105 CUBIC F-lattice R(int) = 0.298 [ 242] Vol = 583.5 Cell: 8.361 8.359 8.349 90.06 89.97 90.00 Volume: 583.50 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.103 RHOMBOHEDRAL R-lattice R(int) = 0.266 [ 191] Vol = 437.6 Cell: 5.911 5.906 14.481 90.05 90.00 120.05 Volume: 437.63 Matrix: 1.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.103 RHOMBOHEDRAL R-lattice R(int) = 0.357 [ 48] Vol = 437.6 Trigonal Cell: 5.911 5.906 14.481 90.05 90.00 120.05 Volume: 437.63 Matrix: 1.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.317 [ 92] Vol = 291.8 Cell: 5.911 5.911 8.349 89.98 89.94 90.01 Volume: 291.75 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.074 TETRAGONAL I-lattice R(int) = 0.317 [ 92] Vol = 291.8 Cell: 5.911 5.911 8.349 90.06 90.02 90.01 Volume: 291.75 Matrix: 1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.231 [ 180] Vol = 291.8 Cell: 5.911 5.911 8.349 89.94 89.98 90.01 Volume: 291.75 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.164 [ 115] Vol = 291.8 Cell: 5.904 8.361 5.910 89.98 89.93 90.02 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.184 [ 137] Vol = 291.8 Cell: 5.911 5.911 8.349 90.02 90.06 90.01 Volume: 291.75 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.072 MONOCLINIC I-lattice R(int) = 0.078 [ 23] Vol = 291.8 Cell: 5.904 5.910 8.361 90.02 90.02 90.07 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.175 [ 28] Vol = 291.8 Cell: 5.904 8.361 5.910 89.98 90.07 89.98 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.033 MONOCLINIC I-lattice R(int) = 0.191 [ 88] Vol = 291.8 Cell: 5.910 5.904 8.361 89.98 90.02 89.93 Volume: 291.75 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.096 MONOCLINIC C-lattice R(int) = 0.299 [ 85] Vol = 291.8 Cell: 10.233 5.906 5.910 90.08 125.23 89.92 Volume: 291.75 Matrix: 1.0000 -1.0000 2.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.047 [ 2] Vol = 145.9 Cell: 5.904 5.906 5.910 90.08 119.95 119.93 Volume: 145.88 Matrix: 0.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 Option [19] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 198 201 191 0 295 256 261 386 N (int>3sigma) = 0 153 201 146 0 250 205 206 308 Mean intensity = 0.0 55.6 26.0 57.1 0.0 46.0 71.0 65.0 65.4 Mean int/sigma = 0.0 18.1 17.1 18.7 0.0 17.9 20.5 19.7 19.7 Crystal system ORTHORHOMBIC and Lattice type I selected Mean |E*E-1| = 1.199 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: b-- c-- -a- -c- --a --b N 32 32 9 9 9 9 N I>3s 32 32 6 6 9 9 36.5 36.5 0.6 0.6 37.1 37.1 23.7 23.7 3.1 3.1 24.9 24.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Ima2 (abc ) 46 A N ? Y Y 27 67 0.166 106 Ima2 (-cba) 46 A N ? Y Y 27 67 0.119 27 Imma (a-cb) 74 C N N N N 21 207 0.166 107 Imma (cab ) 74 C N N N N 21 207 0.165 112 Imma mmm Orthorhombic (1) x, y, z (2) -x,-y+1/2, z+1/2 (3) -x, y+1/2,-z (4) x,-y,-z+1/2 (5) -x,-y,-z (6) x, y+1/2,-z+1/2 (7) x,-y+1/2, z (8) -x, y, z+1/2 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Imma REM Imma (#74, found as Imcm in cab setting) CELL 0.71073 5.910129 5.904089 8.361086 90.0223 89.9763 89.9301 ZERR 1.00 0.001674 0.001692 0.006249 0.0179 0.0176 0.0232 LATT 2 SYMM -x,-y+1/2, z+1/2 SYMM -x, y+1/2,-z SYMM x,-y,-z+1/2 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 7878628- 1542519 38 37 27 1.4 2508166.18 49.07 0.677 0.677 1474994- 888184 46 42 27 1.6 1019748.27 27.93 0.866 0.866 853368- 471939 47 43 27 1.6 551392.75 27.17 0.823 0.810 468892- 286279 55 49 27 1.8 329510.96 24.24 0.278 0.255 279222- 203711 49 43 27 1.6 224011.09 16.89 0.186 0.186 202396- 156393 42 39 27 1.4 169079.54 15.28 0.476 0.476 155847- 100618 35 34 27 1.3 128937.55 11.67 0.346 0.346 99069- 47428 34 32 27 1.2 68080.25 10.68 0.268 0.268 44948- 4802 35 34 27 1.3 16412.75 4.23 0.399 0.399 4646- 1003 33 33 31 1.1 2932.53 2.02 0.079 0.079 ------------------------------------------------------------------------------------------- 7878628- 1003 414 386 274 1.4 515366.15 19.73 0.655 0.653 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 58 49 27 1.8 808464.56 38.55 0.751 0.763 0.015 1.12-0.87 56 44 28 1.6 677045.81 24.95 0.763 0.763 0.024 0.85-0.74 49 46 27 1.7 586833.57 21.46 0.713 0.699 0.030 0.73-0.65 40 40 27 1.5 649898.50 19.98 0.468 0.468 0.030 0.65-0.60 45 43 29 1.5 517940.90 17.24 0.499 0.499 0.036 0.60-0.55 42 42 29 1.4 397941.98 14.48 0.662 0.662 0.042 0.55-0.52 37 36 27 1.3 433295.29 14.32 0.759 0.759 0.044 0.51-0.49 29 29 27 1.1 197913.74 11.56 0.535 0.535 0.060 0.49-0.45 32 31 28 1.1 306311.70 11.55 0.420 0.420 0.050 0.45-0.40 26 26 25 1.0 258363.66 10.97 0.445 0.445 0.053 ------------------------------------------------------------------------------------------------------ inf-0.40 414 386 274 1.4 515366.15 19.73 0.655 0.653 0.031 inf-0.60 245 219 135 1.6 655477.57 24.82 0.648 0.646 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 49 29 27 93.1 1.8 808464.56 57.82 0.751 0.014 1.12-0.87 44 29 28 96.6 1.6 677045.81 35.13 0.763 0.020 0.85-0.74 46 31 27 87.1 1.7 586833.57 31.35 0.713 0.025 0.73-0.65 40 29 27 93.1 1.5 649898.50 27.30 0.468 0.023 0.65-0.60 43 37 29 78.4 1.5 517940.90 23.54 0.499 0.028 0.60-0.55 42 40 29 72.5 1.4 397941.98 19.19 0.662 0.041 0.55-0.52 36 38 27 71.1 1.3 433295.29 18.36 0.759 0.037 0.51-0.49 29 42 27 64.3 1.1 197913.74 12.88 0.535 0.053 0.49-0.45 31 59 28 47.5 1.1 306311.70 12.10 0.420 0.102 0.45-0.40 26 128 25 19.5 1.0 258363.66 11.24 0.445 0.070 -------------------------------------------------------------------------------------------- inf-0.40 386 464 274 59.1 1.4 515366.15 27.03 0.655 0.025 inf-0.60 219 152 135 88.8 1.6 655477.57 35.82 0.648 0.022 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 0.0 0.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.111878 -0.042288 0.007491 ( 0.000021 0.000030 0.000015 ) -0.003794 0.019894 0.083626 ( 0.000014 0.000020 0.000010 ) -0.043271 -0.110675 0.012134 ( 0.000019 0.000028 0.000014 ) M - matrix: 0.014403 -0.000018 -0.000004 ( 0.000005 0.000004 0.000002 ) -0.000018 0.014433 0.000004 ( 0.000004 0.000007 0.000002 ) -0.000004 0.000004 0.007197 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.111878 -0.042288 0.007491 ( 0.000021 0.000030 0.000015 ) -0.003794 0.019894 0.083626 ( 0.000014 0.000020 0.000010 ) -0.043271 -0.110675 0.012134 ( 0.000019 0.000028 0.000014 ) M - matrix: 0.014400 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.014396 0.000000 ( 0.000000 0.000007 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000002 ) unit cell: 5.9101(11) 5.9041(13) 8.3611(10) 90.022(13) 89.976(13) 89.930(17) V = 291.75(9) unit cell: 5.9081(6) 5.9090(15) 8.3570(9) 90.0 90.0 90.0 V = 291.75(9) Laue class changed... Laue class: 2/m2/m2/m - Friedel mate is equivalent Point group: mmm Lattice type: I-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.871) PROFFIT INFO: signal sum: min=506.0000 max=19744344.0000 PROFFIT INFO: signal sum lp corr: min=715.8997 max=2235181.8372 PROFFIT INFO: background sum: min=957.0000 max=16421.0000 PROFFIT INFO: background sum sig2: min=676.0000 max=9278.0000 PROFFIT INFO: num of signal pixels: min=68 max=541 PROFFIT INFO: Inet: min=1561.9629 max=4876760.5000 PROFFIT INFO: sig(Inet): min=248.5124 max=63967.4102 PROFFIT INFO: Inet/sig(Inet): min=1.22 max=252.92 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 60 102 178 190 312 542 734 828 Percent 0.0 0.0 1.0 7.2 12.3 21.5 22.9 37.7 65.5 88.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 414 100.00 (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 414 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4876761- 1796122 41 2616038.27 145.82 100.00 1772680- 1098202 41 1414688.45 110.92 100.00 1056410- 369249 41 607845.17 97.32 100.00 368236- 232078 41 278210.65 69.62 100.00 231707- 185668 41 212379.57 53.63 100.00 185605- 153718 41 166682.54 37.05 100.00 153357- 107815 41 130532.89 30.84 100.00 107585- 6644 41 65324.79 22.67 100.00 6563- 4203 41 5168.18 5.16 87.80 4182- 1562 45 3279.10 3.47 44.44 ------------------------------------------------------------------------------------ 4876761- 1562 414 544732.49 57.13 92.75 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.81- 1.39 41 801437.58 87.23 100.00 1.39- 1.09 41 971864.79 74.59 100.00 1.09- 0.96 41 619077.85 78.90 100.00 0.96- 0.85 41 664119.74 70.29 97.56 0.85- 0.81 41 662592.00 67.66 97.56 0.81- 0.73 41 374606.27 44.27 92.68 0.73- 0.70 41 295376.97 36.36 90.24 0.70- 0.65 41 557654.37 52.91 90.24 0.65- 0.62 41 310852.87 34.43 80.49 0.62- 0.59 45 221297.11 27.51 80.00 ------------------------------------------------------------------------------------ 4.81- 0.59 414 544732.49 57.13 92.75 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:28:57 2018 Sorting 414 observations 99 unique observations with > 7.00 F2/sig(F2) 414 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Maximum number of 99 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 414 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Frame #8 of 74 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 334 observations > 7.00 F2/sig(F2) 334 observations in 1 runs Run # start # end # total # 1 1 74 74 Total number of frames 74 Frame #8 of 74 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: 2.2 (Out of 334 removed 122 = 212, unique = 98) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m2/m2/m 212 observations in 1 runs Run # start # end # total # 1 1 73 73 Total number of frames 73 Frame #8 of 73 skipped from refinement Frame #28 of 73 skipped from refinement Frame #40 of 73 skipped from refinement Frame #48 of 73 skipped from refinement Frame #55 of 73 skipped from refinement Frame #56 of 73 skipped from refinement Frame #64 of 73 skipped from refinement Frame #71 of 73 skipped from refinement 8 frames need to be skipped from refinement, because of missing redundant and/or observable data 98 unique data precomputed (should be 98) 98 unique data with 212 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.2 (Out of 212 removed 0 = 212, unique = 98) 98 unique data precomputed (should be 98) 98 unique data with 212 observations RMS deviation of equivalent data = 0.06265 Rint = 0.04620 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.04620, wR= 0.06800 Trying model 1 (ne=2, no=0)... Results: Rint= 0.02644, wR= 0.03817, Acormin=0.785, Acormax=1.065, Acor_av=0.910 F test: Probability=1.000, F= 2.920 Trying model 2 (ne=2, no=1)... Results: Rint= 0.02496, wR= 0.03650, Acormin=0.769, Acormax=1.132, Acor_av=0.909 F test: Probability=0.674, F= 1.091 Trying model 3 (ne=4, no=0)... Results: Rint= 0.01517, wR= 0.02104, Acormin=0.777, Acormax=1.270, Acor_av=0.971 F test: Probability=1.000, F= 2.787 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01280, wR= 0.01919, Acormin=0.850, Acormax=1.411, Acor_av=0.979 F test: Probability=0.936, F= 1.362 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01188, wR= 0.01702, Acormin=0.871, Acormax=1.316, Acor_av=0.986 F test: Probability=0.968, F= 1.467 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01119, wR= 0.01628, Acormin=0.872, Acormax=1.326, Acor_av=0.987 F test: Probability=0.656, F= 1.089 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01086, wR= 0.01593, Acormin=0.864, Acormax=1.357, Acor_av=0.987 F test: Probability=0.695, F= 1.117 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01030, wR= 0.01411, Acormin=0.858, Acormax=1.395, Acor_av=0.988 F test: Probability=0.718, F= 1.137 Trying model 9 (ne=6, no=5)... Results: Rint= 0.00823, wR= 0.01207, Acormin=0.883, Acormax=1.294, Acor_av=0.991 F test: Probability=0.965, F= 1.529 Trying model 10 (ne=8, no=0)... Results: Rint= 0.00838, wR= 0.01281, Acormin=0.880, Acormax=1.284, Acor_av=0.990 F test: Probability=0.538, F= 1.023 Trying model 11 (ne=8, no=1)... Results: Rint= 0.00854, wR= 0.01261, Acormin=0.879, Acormax=1.289, Acor_av=0.991 F test: Probability=0.000, F= 0.941 Trying model 12 (ne=8, no=3)... Results: Rint= 0.00804, wR= 0.01149, Acormin=0.887, Acormax=1.283, Acor_av=0.991 F test: Probability=0.000, F= 0.952 Trying model 13 (ne=8, no=5)... Results: Rint= 0.00656, wR= 0.01058, Acormin=0.889, Acormax=1.270, Acor_av=0.992 F test: Probability=0.712, F= 1.167 Trying model 14 (ne=8, no=7)... Results: Rint= 0.00574, wR= 0.01006, Acormin=0.866, Acormax=1.273, Acor_av=0.993 F test: Probability=0.563, F= 1.059 Final absorption model (ne=6, no=5): Rint= 0.00823, Acormin=0.883, Acormax=1.294, Acor_av=0.991 Combined refinement in use Rint: 0.04632 There are 65 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 112 pars with 6328 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.06265 Using Levenberg-Marquardt: 0.00010 New wR= 0.01054 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00630 Rint for all data: 0.04632 with corrections 0.00649 0 observations identified as outliers and rejected Cycle 2 wR= 0.01054 Using Levenberg-Marquardt: 0.00001 New wR= 0.00948 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00601 Rint for all data: 0.04632 with corrections 0.00620 0 observations identified as outliers and rejected Cycle 3 wR= 0.00948 Using Levenberg-Marquardt: 0.00000 New wR= 0.00925 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00613 Rint for all data: 0.04632 with corrections 0.00632 0 observations identified as outliers and rejected Cycle 4 wR= 0.00925 Using Levenberg-Marquardt: 0.00000 New wR= 0.00924 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00634 Rint for all data: 0.04632 with corrections 0.00653 0 observations identified as outliers and rejected Cycle 5 wR= 0.00924 Using Levenberg-Marquardt: 0.00000 New wR= 0.00923 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00638 Rint for all data: 0.04632 with corrections 0.00657 0 observations identified as outliers and rejected Final wR= 0.00923 Final frame scales: Min= 0.9486 Max= 1.0991 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 65 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 101 pars with 5151 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.08993 Using Levenberg-Marquardt: 0.00010 New wR= 0.01963 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.01346 Rint for all data: 0.04632 with corrections 0.01363 0 observations identified as outliers and rejected Cycle 2 wR= 0.01963 Using Levenberg-Marquardt: 0.00001 New wR= 0.01052 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00653 Rint for all data: 0.04632 with corrections 0.00672 0 observations identified as outliers and rejected Cycle 3 wR= 0.01052 Using Levenberg-Marquardt: 0.00000 New wR= 0.00947 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00614 Rint for all data: 0.04632 with corrections 0.00633 0 observations identified as outliers and rejected Cycle 4 wR= 0.00947 Using Levenberg-Marquardt: 0.00000 New wR= 0.00947 There are 8 clusters with unrefined scales (size 1-2) Rint for refined data: 0.04620 with corrections 0.00607 Rint for all data: 0.04632 with corrections 0.00626 Final wR= 0.00947 Final frame scales: Min= 0.9676 Max= 1.1598 Final absorption correction factors: Amin= 0.7002 Amax= 2.0842 PROFFIT INFO: Inet (after scale3 abspack): min=972.1647 max=4795065.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=305.9123 max=62468.8867 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 4, Friedel: 1 Min/max for: run:1/1 frame:2/75 414 reflections read from tmp file 153 reflections are rejected (1 as outliers, 152 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 106 15 1 Initial Chi^2= 0.30118 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.38917 Current error model SIG(F2)^2 = 219.11*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 85.27*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 85.27*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4795065- 1848029 41 2611871.13 151.34 100.00 1847028- 1121992 41 1437086.22 78.25 100.00 1111091- 355481 41 591347.05 77.92 100.00 353046- 233836 41 277831.49 48.47 100.00 231231- 195112 41 215958.03 39.71 100.00 185888- 152772 41 168147.21 25.97 100.00 152769- 110243 41 131536.01 22.74 100.00 108514- 7106 41 59721.84 17.30 100.00 6778- 4312 41 5121.92 5.33 100.00 4299- 972 45 3260.09 4.23 91.11 ------------------------------------------------------------------------------------ 4795065- 972 414 544903.77 46.71 99.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.81- 1.39 41 812248.37 95.06 100.00 1.39- 1.09 41 961988.94 76.88 100.00 1.09- 0.96 41 623392.82 56.43 100.00 0.96- 0.85 41 665151.54 50.43 100.00 0.85- 0.81 41 666798.39 48.49 100.00 0.81- 0.73 41 375662.16 32.19 100.00 0.73- 0.70 41 295921.08 26.64 100.00 0.70- 0.65 41 556404.96 38.01 95.12 0.65- 0.62 41 299225.46 25.22 100.00 0.62- 0.59 45 223591.52 20.34 95.56 ------------------------------------------------------------------------------------ 4.81- 0.59 414 544903.77 46.71 99.03 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.81- 1.39 41 812248.37 95.06 100.00 4.81- 1.09 82 887118.66 85.97 100.00 4.81- 0.96 123 799210.04 76.12 100.00 4.81- 0.85 164 765695.42 69.70 100.00 4.81- 0.81 205 745916.01 65.46 100.00 4.81- 0.73 246 684207.04 59.91 100.00 4.81- 0.70 287 628737.61 55.16 100.00 4.81- 0.65 328 619696.03 53.01 99.39 4.81- 0.62 369 584088.19 49.93 99.46 4.81- 0.59 414 544903.77 46.71 99.03 ------------------------------------------------------------------------------------ 4.81- 0.59 414 544903.77 46.71 99.03 Scale applied to data: s=0.208548 (maximum obs:4795065.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.006; Rsigma 0.014: data 414 -> merged 274 With outlier rejection... Rint 0.006; Rsigma 0.014: data 412 -> merged 274 Rejected total: 2, method kkm 2, method Blessing 0 Completeness direct cell (a, b, c) = (5.908, 5.909, 8.357), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586465, 4.824281 completeness table (Laue group: Immm, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.41 20 41 1.60 48.78 32 1.41 - 1.09 24 41 2.04 58.54 49 1.09 - 0.96 23 41 1.91 56.10 44 0.96 - 0.84 25 41 1.72 60.98 43 0.84 - 0.78 30 41 1.50 73.17 45 0.78 - 0.73 27 41 1.44 65.85 39 0.73 - 0.70 28 41 1.36 68.29 38 0.70 - 0.65 26 41 1.31 63.41 34 0.65 - 0.64 26 41 1.23 63.41 32 0.64 - 0.60 31 50 1.26 62.00 39 --------------------------------------------------------------- 5.91 - 0.60 260 419 1.52 62.05 395 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:28:56 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.910129 5.911499 5.904089 60.0193 89.9301 59.9480 386 Reflections read from file xs1715a.hkl; mean (I/sigma) = 19.73 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 191 201 188 196 290 266 261 386 N (int>3sigma) = 0 146 201 143 148 245 212 206 308 Mean intensity = 0.0 55.2 26.0 55.8 57.9 45.3 64.4 65.0 65.4 Mean int/sigma = 0.0 18.0 17.1 17.8 18.5 17.6 18.6 19.7 19.7 Lattice type: P chosen Volume: 145.88 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.904 5.906 5.910 90.08 119.95 119.93 Niggli form: a.a = 34.858 b.b = 34.883 c.c = 34.922 b.c = -0.051 a.c = -17.417 a.b = -17.398 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.105 CUBIC F-lattice R(int) = 0.298 [ 242] Vol = 583.5 Cell: 8.361 8.359 8.349 90.06 89.97 90.00 Volume: 583.50 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.103 RHOMBOHEDRAL R-lattice R(int) = 0.266 [ 191] Vol = 437.6 Cell: 5.911 5.906 14.481 90.05 90.00 120.05 Volume: 437.63 Matrix: 1.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.103 RHOMBOHEDRAL R-lattice R(int) = 0.357 [ 48] Vol = 437.6 Trigonal Cell: 5.911 5.906 14.481 90.05 90.00 120.05 Volume: 437.63 Matrix: 1.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.317 [ 92] Vol = 291.8 Cell: 5.911 5.911 8.349 89.98 89.94 90.01 Volume: 291.75 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.074 TETRAGONAL I-lattice R(int) = 0.317 [ 92] Vol = 291.8 Cell: 5.911 5.911 8.349 90.06 90.02 90.01 Volume: 291.75 Matrix: 1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.231 [ 180] Vol = 291.8 Cell: 5.911 5.911 8.349 89.94 89.98 90.01 Volume: 291.75 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.164 [ 115] Vol = 291.8 Cell: 5.904 8.361 5.910 89.98 89.93 90.02 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.184 [ 137] Vol = 291.8 Cell: 5.911 5.911 8.349 90.02 90.06 90.01 Volume: 291.75 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.072 MONOCLINIC I-lattice R(int) = 0.078 [ 23] Vol = 291.8 Cell: 5.904 5.910 8.361 90.02 90.02 90.07 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.175 [ 28] Vol = 291.8 Cell: 5.904 8.361 5.910 89.98 90.07 89.98 Volume: 291.75 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.033 MONOCLINIC I-lattice R(int) = 0.191 [ 88] Vol = 291.8 Cell: 5.910 5.904 8.361 89.98 90.02 89.93 Volume: 291.75 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.096 MONOCLINIC C-lattice R(int) = 0.299 [ 85] Vol = 291.8 Cell: 10.233 5.906 5.910 90.08 125.23 89.92 Volume: 291.75 Matrix: 1.0000 -1.0000 2.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.047 [ 2] Vol = 145.9 Cell: 5.904 5.906 5.910 90.08 119.95 119.93 Volume: 145.88 Matrix: 0.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 Option [19] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 198 201 191 0 295 256 261 386 N (int>3sigma) = 0 153 201 146 0 250 205 206 308 Mean intensity = 0.0 55.6 26.0 57.1 0.0 46.0 71.0 65.0 65.4 Mean int/sigma = 0.0 18.1 17.1 18.7 0.0 17.9 20.5 19.7 19.7 Crystal system ORTHORHOMBIC and Lattice type I selected Mean |E*E-1| = 1.199 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: b-- c-- -a- -c- --a --b N 32 32 9 9 9 9 N I>3s 32 32 6 6 9 9 36.5 36.5 0.6 0.6 37.1 37.1 23.7 23.7 3.1 3.1 24.9 24.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Ima2 (abc ) 46 A N ? Y Y 27 67 0.166 106 Ima2 (-cba) 46 A N ? Y Y 27 67 0.119 27 Imma (a-cb) 74 C N N N N 21 207 0.166 107 Imma (cab ) 74 C N N N N 21 207 0.165 112 Imma mmm Orthorhombic (1) x, y, z (2) -x,-y+1/2, z+1/2 (3) -x, y+1/2,-z (4) x,-y,-z+1/2 (5) -x,-y,-z (6) x, y+1/2,-z+1/2 (7) x,-y+1/2, z (8) -x, y, z+1/2 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Imma REM Imma (#74, found as Imcm in cab setting) CELL 0.71073 5.910129 5.904089 8.361086 90.0223 89.9763 89.9301 ZERR 1.00 0.001674 0.001692 0.006249 0.0179 0.0176 0.0232 LATT 2 SYMM -x,-y+1/2, z+1/2 SYMM -x, y+1/2,-z SYMM x,-y,-z+1/2 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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: Immm # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4795065- 1770913 45 44 27 1.6 2535114.11 144.97 0.004 0.004 1743504- 1111091 38 38 27 1.4 1391227.09 75.75 0.003 0.003 1089385- 350372 44 44 27 1.6 557775.50 76.37 0.006 0.006 350060- 225311 52 52 27 1.9 257346.82 45.38 0.014 0.015 224369- 169198 44 44 27 1.6 195800.46 34.27 0.017 0.018 168764- 139154 36 36 27 1.3 156863.09 25.31 0.012 0.012 139148- 104949 33 33 27 1.2 121649.35 21.33 0.025 0.025 102440- 6350 36 36 27 1.3 53115.39 16.65 0.020 0.021 6114- 4178 41 41 27 1.5 5021.99 5.37 0.130 0.130 4164- 972 45 44 31 1.4 3358.11 4.18 0.135 0.137 ------------------------------------------------------------------------------------------- 4795065- 972 414 412 274 1.5 540966.84 46.37 0.006 0.006 Statistics vs resolution - point group symmetry: Immm resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.27 50 48 27 1.8 906348.14 98.13 0.004 0.004 0.007 1.26-1.01 54 54 27 2.0 605322.45 55.37 0.007 0.007 0.010 1.01-0.89 49 49 27 1.8 780463.04 58.19 0.005 0.005 0.011 0.89-0.82 42 42 27 1.6 802493.12 55.08 0.006 0.006 0.012 0.81-0.75 40 40 27 1.5 324640.20 30.66 0.010 0.010 0.019 0.75-0.72 35 35 27 1.3 344044.49 31.03 0.010 0.010 0.021 0.72-0.68 35 35 27 1.3 453863.82 33.48 0.003 0.003 0.018 0.68-0.64 36 36 27 1.3 454846.71 31.51 0.007 0.007 0.019 0.64-0.62 33 33 27 1.2 235522.29 23.41 0.006 0.006 0.028 0.62-0.59 40 40 31 1.3 241992.51 21.21 0.013 0.013 0.027 ------------------------------------------------------------------------------------------------------ inf-0.59 414 412 274 1.5 540966.84 46.37 0.006 0.006 0.014 inf-0.60 395 393 259 1.5 560284.71 47.79 0.006 0.006 0.013 Statistics vs resolution (taking redundancy into account) - point group symmetry: Immm resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.27 48 56 27 48.2 1.8 906348.14 129.41 0.004 0.004 1.26-1.01 54 46 27 58.7 2.0 605322.45 78.88 0.007 0.007 1.01-0.89 49 43 27 62.8 1.8 780463.04 80.07 0.005 0.008 0.89-0.82 42 39 27 69.2 1.6 802493.12 72.27 0.006 0.009 0.81-0.75 40 40 27 67.5 1.5 324640.20 39.20 0.010 0.014 0.75-0.72 35 37 27 73.0 1.3 344044.49 36.71 0.010 0.017 0.72-0.68 35 42 27 64.3 1.3 453863.82 41.00 0.003 0.012 0.68-0.64 36 42 27 64.3 1.3 454846.71 38.37 0.007 0.014 0.64-0.62 33 45 27 60.0 1.2 235522.29 27.20 0.006 0.018 0.62-0.59 40 67 31 46.3 1.3 241992.51 24.21 0.013 0.024 -------------------------------------------------------------------------------------------- inf-0.59 412 461 274 59.4 1.5 540966.84 60.59 0.006 0.009 inf-0.60 393 418 259 62.0 1.5 560284.71 62.58 0.006 0.009 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:34:11 2018) ID: 2932; threads 39; handles 876; mem 518728.00 (1237724.00)kB; time: 1w 5d 21h 39m 42s MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.6,peak PF: 708.5, WS: 270.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:169.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.4,peak PF: 708.5, WS: 272.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:34:11 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000032 0.000030 0.000035 ) 0.087412 -0.166882 0.063604 ( 0.000021 0.000020 0.000023 ) 0.055227 -0.024260 0.122680 ( 0.000029 0.000027 0.000032 ) 5.91535 ( 0.00168 ) 5.92288 ( 0.00116 ) 5.91286 ( 0.00170 ) 59.95509 ( 0.02507 ) 89.89521 ( 0.02323 ) 59.99590 ( 0.02489 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 12:34:11 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000032 0.000030 0.000035 ) 0.087412 -0.166882 0.063604 ( 0.000021 0.000020 0.000023 ) 0.055227 -0.024260 0.122680 ( 0.000029 0.000027 0.000032 ) M - matrix: 0.021609 -0.014402 0.007179 ( 0.000008 0.000005 0.000006 ) -0.014402 0.028787 -0.014386 ( 0.000005 0.000007 0.000006 ) 0.007179 -0.014386 0.021622 ( 0.000006 0.000006 0.000009 ) unit cell: 5.9154(17) 5.9229(12) 5.9129(17) 59.96(2) 89.90(2) 60.00(2) V = 146.51(6) 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\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb PROFFITPEAK info: 1172 peaks in the peak location table UB fit with 514 obs out of 549 (total:549,skipped:0) (93.62%) UB - matrix: -0.104101 -0.015326 0.049887 ( 0.000059 0.000058 0.000064 ) 0.087125 -0.166792 0.063600 ( 0.000064 0.000062 0.000069 ) 0.055263 -0.023985 0.122566 ( 0.000067 0.000065 0.000072 ) M - matrix: 0.021482 -0.014262 0.007121 ( 0.000018 0.000014 0.000014 ) -0.014262 0.028630 -0.014312 ( 0.000014 0.000021 0.000015 ) 0.007121 -0.014312 0.021556 ( 0.000014 0.000015 0.000021 ) unit cell: 5.916(3) 5.916(3) 5.911(4) 60.02(6) 89.97(5) 60.11(5) V = 146.57(14) UB fit with 514 obs out of 549 (total:549,skipped:0) (93.62%) UB - matrix: -0.104101 -0.015326 0.049887 ( 0.000059 0.000058 0.000064 ) 0.087125 -0.166792 0.063600 ( 0.000064 0.000062 0.000069 ) 0.055263 -0.023985 0.122566 ( 0.000067 0.000065 0.000072 ) M - matrix: 0.021482 -0.014262 0.007121 ( 0.000018 0.000014 0.000014 ) -0.014262 0.028630 -0.014312 ( 0.000014 0.000021 0.000015 ) 0.007121 -0.014312 0.021556 ( 0.000014 0.000015 0.000021 ) unit cell: 5.916(3) 5.916(3) 5.911(4) 60.02(6) 89.97(5) 60.11(5) V = 146.57(14) OTKP changes: 100 1 1 1 UB - matrix: -0.104093 -0.015073 0.049617 ( 0.000058 0.000056 0.000063 ) 0.087200 -0.166806 0.063586 ( 0.000061 0.000059 0.000066 ) 0.055241 -0.024187 0.122472 ( 0.000065 0.000063 0.000071 ) M - matrix: 0.021491 -0.014313 0.007145 ( 0.000018 0.000013 0.000013 ) -0.014313 0.028636 -0.014317 ( 0.000013 0.000020 0.000014 ) 0.007145 -0.014317 0.021504 ( 0.000013 0.000014 0.000020 ) UB fit with 511 obs out of 549 (total:549,skipped:0) (93.08%) unit cell: 5.924(3) 5.926(3) 5.922(4) 60.00(6) 89.96(5) 60.00(5) V = 147.03(13) UB fit with 511 obs out of 549 (total:549,skipped:0) (93.08%) UB - matrix: -0.104093 -0.015073 0.049617 ( 0.000058 0.000056 0.000063 ) 0.087200 -0.166806 0.063586 ( 0.000061 0.000059 0.000066 ) 0.055241 -0.024187 0.122472 ( 0.000065 0.000063 0.000071 ) M - matrix: 0.021491 -0.014313 0.007145 ( 0.000018 0.000013 0.000013 ) -0.014313 0.028636 -0.014317 ( 0.000013 0.000020 0.000014 ) 0.007145 -0.014317 0.021504 ( 0.000013 0.000014 0.000020 ) unit cell: 5.924(3) 5.926(3) 5.922(4) 60.00(6) 89.96(5) 60.00(5) V = 147.03(13) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104093 -0.015074 0.049619 ( 0.000058 0.000056 0.000063 ) 0.087199 -0.166807 0.063587 ( 0.000061 0.000059 0.000066 ) 0.055240 -0.024185 0.122473 ( 0.000065 0.000063 0.000071 ) M - matrix: 0.021491 -0.014312 0.007145 ( 0.000018 0.000013 0.000013 ) -0.014312 0.028637 -0.014317 ( 0.000013 0.000020 0.000014 ) 0.007145 -0.014317 0.021505 ( 0.000013 0.000014 0.000020 ) UB fit with 511 obs out of 549 (total:549,skipped:0) (93.08%) unit cell: 5.924(3) 5.925(3) 5.922(4) 60.00(6) 89.96(5) 60.00(5) V = 147.03(13) 549 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Run 1 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.979) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104093 -0.015074 0.049619 ( 0.000058 0.000056 0.000063 ) 0.087199 -0.166807 0.063587 ( 0.000061 0.000059 0.000066 ) 0.055240 -0.024185 0.122473 ( 0.000065 0.000063 0.000071 ) M - matrix: 0.021491 -0.014312 0.007145 ( 0.000018 0.000013 0.000013 ) -0.014312 0.028637 -0.014317 ( 0.000013 0.000020 0.000014 ) 0.007145 -0.014317 0.021505 ( 0.000013 0.000014 0.000020 ) UB fit with 511 obs out of 549 (total:549,skipped:0) (93.08%) unit cell: 5.924(3) 5.925(3) 5.922(4) 60.00(6) 89.96(5) 60.00(5) V = 147.03(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 549 (total:549,skipped:0) (93.62%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb 8 of 412 peaks identified as outliers and rejected 404 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 404 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 404 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 40 | 1.004 ( 0.148) | 1.228 ( 0.569) | 1.347 ( 0.887) | 1.33- 1.12 | 40 | 1.081 ( 0.078) | 1.140 ( 0.130) | 1.200 ( 0.539) | 1.09- 0.97 | 40 | 1.147 ( 0.125) | 1.301 ( 0.507) | 1.141 ( 0.522) | 0.97- 0.88 | 40 | 1.134 ( 0.055) | 1.147 ( 0.125) | 1.194 ( 0.432) | 0.88- 0.81 | 40 | 1.168 ( 0.053) | 1.214 ( 0.137) | 1.179 ( 0.400) | 0.81- 0.75 | 40 | 1.175 ( 0.053) | 1.138 ( 0.152) | 1.330 ( 0.389) | 0.75- 0.71 | 40 | 1.183 ( 0.046) | 1.172 ( 0.155) | 1.328 ( 0.457) | 0.70- 0.67 | 40 | 1.199 ( 0.053) | 1.199 ( 0.174) | 1.220 ( 0.382) | 0.67- 0.62 | 40 | 1.200 ( 0.085) | 1.216 ( 0.166) | 1.202 ( 0.477) | 0.62- 0.59 | 44 | 1.194 ( 0.071) | 1.204 ( 0.197) | 1.316 ( 0.503) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 404 | 1.149 ( 0.102) | 1.196 ( 0.282) | 1.246 ( 0.523) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) UB - matrix: -0.104310 -0.014721 0.049279 ( 0.000030 0.000029 0.000029 ) 0.087346 -0.167010 0.063573 ( 0.000021 0.000020 0.000020 ) 0.055269 -0.024462 0.122580 ( 0.000029 0.000028 0.000029 ) M - matrix: 0.021565 -0.014404 0.007187 ( 0.000008 0.000005 0.000006 ) -0.014404 0.028707 -0.014341 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014341 0.021496 ( 0.000006 0.000005 0.000008 ) unit cell: 5.9238(16) 5.9272(11) 5.9250(16) 60.02(2) 89.97(2) 59.88(2) V = 146.93(6) OTKP changes: 404 1 1 1 UB - matrix: -0.104312 -0.014970 0.049606 ( 0.000026 0.000025 0.000026 ) 0.087343 -0.167138 0.063661 ( 0.000019 0.000018 0.000019 ) 0.055385 -0.024325 0.122725 ( 0.000028 0.000027 0.000027 ) M - matrix: 0.021577 -0.014384 0.007183 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028751 -0.014368 ( 0.000005 0.000006 0.000005 ) 0.007183 -0.014368 0.021575 ( 0.000005 0.000005 0.000008 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9147(14) 5.9153(10) 5.9119(15) 60.02(2) 89.98(2) 59.97(2) V = 146.27(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.931) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104312 -0.014970 0.049606 ( 0.000026 0.000025 0.000026 ) 0.087343 -0.167138 0.063661 ( 0.000019 0.000018 0.000019 ) 0.055385 -0.024325 0.122725 ( 0.000028 0.000027 0.000027 ) M - matrix: 0.021577 -0.014384 0.007183 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028751 -0.014368 ( 0.000005 0.000006 0.000005 ) 0.007183 -0.014368 0.021575 ( 0.000005 0.000005 0.000008 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9147(14) 5.9153(10) 5.9119(15) 60.02(2) 89.98(2) 59.97(2) V = 146.27(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb 9 of 414 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 405 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 405 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 41 | 1.024 ( 0.199) | 1.278 ( 0.676) | 1.465 ( 1.140) | 1.32- 1.12 | 41 | 1.083 ( 0.074) | 1.162 ( 0.188) | 1.329 ( 0.663) | 1.11- 0.96 | 41 | 1.115 ( 0.088) | 1.175 ( 0.255) | 1.234 ( 0.528) | 0.96- 0.85 | 41 | 1.136 ( 0.059) | 1.139 ( 0.125) | 1.238 ( 0.478) | 0.85- 0.81 | 41 | 1.171 ( 0.049) | 1.212 ( 0.134) | 1.162 ( 0.386) | 0.81- 0.73 | 41 | 1.172 ( 0.052) | 1.137 ( 0.158) | 1.307 ( 0.443) | 0.73- 0.70 | 41 | 1.189 ( 0.049) | 1.181 ( 0.165) | 1.254 ( 0.422) | 0.69- 0.65 | 41 | 1.191 ( 0.057) | 1.190 ( 0.149) | 1.217 ( 0.414) | 0.65- 0.62 | 41 | 1.189 ( 0.083) | 1.206 ( 0.161) | 1.241 ( 0.493) | 0.62- 0.59 | 36 | 1.204 ( 0.066) | 1.222 ( 0.210) | 1.311 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 405 | 1.147 ( 0.104) | 1.190 ( 0.275) | 1.275 ( 0.591) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 41 | 1.136 ( 0.049) | 1.247 ( 0.200) | 1.442 ( 0.629) | 13.0-19.4 | 41 | 1.151 ( 0.141) | 1.276 ( 0.440) | 1.430 ( 0.910) | 19.5-24.2 | 41 | 1.169 ( 0.069) | 1.307 ( 0.354) | 1.301 ( 0.628) | 24.2-27.9 | 41 | 1.110 ( 0.096) | 1.135 ( 0.115) | 1.281 ( 0.482) | 28.0-31.3 | 41 | 1.133 ( 0.095) | 1.237 ( 0.323) | 1.171 ( 0.460) | 31.4-34.5 | 41 | 1.129 ( 0.083) | 1.137 ( 0.159) | 1.147 ( 0.327) | 34.5-37.5 | 41 | 1.148 ( 0.084) | 1.163 ( 0.186) | 1.227 ( 0.425) | 37.5-40.0 | 41 | 1.127 ( 0.119) | 1.117 ( 0.237) | 1.221 ( 0.660) | 40.1-43.6 | 41 | 1.158 ( 0.100) | 1.123 ( 0.223) | 1.240 ( 0.598) | 43.6-49.8 | 36 | 1.214 ( 0.140) | 1.152 ( 0.260) | 1.294 ( 0.501) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 405 | 1.147 ( 0.104) | 1.190 ( 0.275) | 1.275 ( 0.591) | Fitted profile normalization line parameters e1 dimension: a=0.0016 b=0.97 e2 dimension: a=-0.0017 b=1.05 e3 dimension: a=-0.0027 b=1.09 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6425 lp-corr: 5349 Maximum peak integral for reflections I/sig<= 100 - raw: 464319 lp-corr: 678322 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2290400 PROFFITPEAK - Finished at Wed Mar 28 12:34:18 2018 PROFFITMAIN - Started at Wed Mar 28 12:34:18 2018 OTKP changes: 405 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 405 1 1 1 UB - matrix: -0.104346 -0.014963 0.049635 ( 0.000028 0.000027 0.000027 ) 0.087370 -0.167197 0.063700 ( 0.000018 0.000018 0.000018 ) 0.055377 -0.024292 0.122726 ( 0.000023 0.000022 0.000023 ) M - matrix: 0.021588 -0.014392 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014392 0.028769 -0.014375 ( 0.000005 0.000006 0.000004 ) 0.007182 -0.014375 0.021583 ( 0.000005 0.000004 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9132(14) 5.9136(9) 5.9107(13) 60.02(2) 89.966(19) 59.97(2) V = 146.16(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= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.908) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014963 0.049635 ( 0.000028 0.000027 0.000027 ) 0.087370 -0.167197 0.063700 ( 0.000018 0.000018 0.000018 ) 0.055377 -0.024292 0.122726 ( 0.000023 0.000022 0.000023 ) M - matrix: 0.021588 -0.014392 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014392 0.028769 -0.014375 ( 0.000005 0.000006 0.000004 ) 0.007182 -0.014375 0.021583 ( 0.000005 0.000004 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9132(14) 5.9136(9) 5.9107(13) 60.02(2) 89.966(19) 59.97(2) V = 146.16(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.146925 -0.097950 0.048924 ( 0.000019 0.000019 0.000019 ) -0.000000 0.138486 -0.069144 ( 0.000024 0.000023 0.000024 ) 0.000024 -0.000003 0.119903 ( 0.000026 0.000025 0.000026 ) M - matrix: 0.021587 -0.014391 0.007191 ( 0.000006 0.000005 0.000005 ) -0.014391 0.028772 -0.014368 ( 0.000005 0.000007 0.000005 ) 0.007191 -0.014368 0.021551 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9132(9) 5.9122(13) 5.9157(14) 60.03(2) 90.018(16) 59.993(19) V = 146.27(5) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104357 -0.014972 0.049664 ( 0.000028 0.000027 0.000027 ) 0.087381 -0.167177 0.063650 ( 0.000019 0.000018 0.000018 ) 0.055400 -0.024292 0.122699 ( 0.000023 0.000022 0.000023 ) M - matrix: 0.021595 -0.014391 0.007177 ( 0.000007 0.000005 0.000005 ) -0.014391 0.028762 -0.014365 ( 0.000005 0.000006 0.000004 ) 0.007177 -0.014365 0.021573 ( 0.000005 0.000004 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9120(14) 5.9137(9) 5.9111(13) 60.03(2) 89.956(19) 59.96(2) V = 146.16(5) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 26 reflections under beam stop or inside a detector rejection region 7 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof 556 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:34:19 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m2/m2/m - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.908) PROFFIT INFO: signal sum: min=488.0000 max=19711404.0000 PROFFIT INFO: signal sum lp corr: min=691.5840 max=2242846.6075 PROFFIT INFO: background sum: min=885.0000 max=16754.0000 PROFFIT INFO: background sum sig2: min=674.0000 max=10584.0000 PROFFIT INFO: num of signal pixels: min=68 max=821 PROFFIT INFO: Inet: min=1508.9105 max=4893483.5000 PROFFIT INFO: sig(Inet): min=248.5227 max=63787.0664 PROFFIT INFO: Inet/sig(Inet): min=1.30 max=252.61 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 7 42 72 122 131 218 368 499 556 Percent 0.0 0.0 1.3 7.6 12.9 21.9 23.6 39.2 66.2 89.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 556 100.00 (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 556 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4893484- 1731533 55 2559862.19 140.09 100.00 1707466- 1089842 55 1377149.71 108.97 100.00 1077394- 363545 55 609841.82 94.29 100.00 354969- 229121 55 269929.36 68.21 100.00 228869- 171697 55 202303.04 51.58 100.00 171292- 146833 55 160454.80 36.22 100.00 146162- 106300 55 123978.43 29.74 100.00 105840- 6378 55 58422.15 21.35 100.00 6309- 4028 55 4937.65 5.02 81.82 4014- 1509 61 3186.84 3.49 47.54 ------------------------------------------------------------------------------------ 4893484- 1509 556 531245.95 55.33 92.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.78- 1.17 55 832879.76 84.52 100.00 1.17- 0.94 55 715485.52 72.96 98.18 0.93- 0.78 55 651071.07 65.03 96.36 0.78- 0.69 55 645604.19 65.20 100.00 0.68- 0.62 55 468034.50 53.89 90.91 0.62- 0.57 55 593584.50 58.79 100.00 0.57- 0.53 55 372151.79 41.87 87.27 0.53- 0.49 55 400036.35 41.67 83.64 0.49- 0.46 55 379474.41 39.45 85.45 0.46- 0.39 61 281394.03 32.43 83.61 ------------------------------------------------------------------------------------ 4.78- 0.39 556 531245.95 55.33 92.45 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:34:19 2018 Sorting 556 observations 103 unique observations with > 7.00 F2/sig(F2) 556 observations in 1 runs Run # start # end # total # 1 1 99 99 Total number of frames 99 Maximum number of 103 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 556 observations in 1 runs Run # start # end # total # 1 1 99 99 Total number of frames 99 Frame #8 of 99 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 446 observations > 7.00 F2/sig(F2) 446 observations in 1 runs Run # start # end # total # 1 1 99 99 Total number of frames 99 Frame #8 of 99 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: 2.1 (Out of 446 removed 272 = 174, unique = 84) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m2/m2/m 174 observations in 1 runs Run # start # end # total # 1 1 99 99 Total number of frames 99 Frame #8 of 99 skipped from refinement Frame #28 of 99 skipped from refinement Frame #40 of 99 skipped from refinement Frame #41 of 99 skipped from refinement Frame #42 of 99 skipped from refinement Frame #45 of 99 skipped from refinement Frame #48 of 99 skipped from refinement Frame #52 of 99 skipped from refinement Frame #55 of 99 skipped from refinement Frame #56 of 99 skipped from refinement Frame #64 of 99 skipped from refinement Frame #65 of 99 skipped from refinement Frame #71 of 99 skipped from refinement Frame #75 of 99 skipped from refinement Frame #76 of 99 skipped from refinement Frame #79 of 99 skipped from refinement Frame #80 of 99 skipped from refinement Frame #83 of 99 skipped from refinement Frame #98 of 99 skipped from refinement 19 frames need to be skipped from refinement, because of missing redundant and/or observable data 84 unique data precomputed (should be 84) 84 unique data with 174 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 174 removed 0 = 174, unique = 84) 84 unique data precomputed (should be 84) 84 unique data with 174 observations RMS deviation of equivalent data = 0.32956 Rint = 0.34646 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.32462, wR= 3.65020 Trying model 1 (ne=2, no=0)... Results: Rint= 0.41856, wR= 5.00708, Acormin=-0.019, Acormax=1.034, Acor_av=0.440 F test: Probability=0.000, F= 0.568 Trying model 2 (ne=2, no=1)... Results: Rint= 0.38954, wR= 6.65789, Acormin=-0.606, Acormax=0.982, Acor_av=-0.038 F test: Probability=0.000, F= 0.632 Trying model 3 (ne=4, no=0)... Results: Rint= 0.38666, wR= 3.59182, Acormin=-0.282, Acormax=0.812, Acor_av=0.084 F test: Probability=0.000, F= 0.594 Trying model 4 (ne=4, no=1)... Results: Rint= 0.27501, wR= 2.11156, Acormin=-0.648, Acormax=0.500, Acor_av=0.026 F test: Probability=0.700, F= 1.127 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23356, wR= 1.73458, Acormin=-0.050, Acormax=0.711, Acor_av=0.096 F test: Probability=0.928, F= 1.411 Trying model 6 (ne=6, no=0)... Results: Rint= 0.14819, wR= 0.61576, Acormin=-0.014, Acormax=0.841, Acor_av=0.197 F test: Probability=1.000, F= 3.343 Trying model 7 (ne=6, no=1)... Results: Rint= 0.12423, wR= 0.51669, Acormin=-0.130, Acormax=0.970, Acor_av=0.185 F test: Probability=1.000, F= 4.526 Trying model 8 (ne=6, no=3)... Results: Rint= 0.11276, wR= 0.54922, Acormin=0.001, Acormax=1.270, Acor_av=0.194 F test: Probability=1.000, F= 4.842 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05436, wR= 0.32933, Acormin=-0.827, Acormax=0.793, Acor_av=0.271 F test: Probability=1.000, F= 3.393 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06239, wR= 0.47557, Acormin=-0.310, Acormax=0.859, Acor_av=0.260 F test: Probability=1.000, F= 2.826 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05186, wR= 0.25625, Acormin=-0.458, Acormax=0.915, Acor_av=0.314 F test: Probability=1.000, F= 3.818 Trying model 12 (ne=8, no=3)... Results: Rint= 0.03209, wR= 0.17663, Acormin=-0.496, Acormax=1.530, Acor_av=0.383 F test: Probability=1.000, F= 8.311 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02324, wR= 0.09256, Acormin=-0.199, Acormax=2.342, Acor_av=0.442 F test: Probability=1.000, F= 10.866 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01733, wR= 0.03722, Acormin=-0.107, Acormax=2.253, Acor_av=0.541 F test: Probability=0.998, F= 7.330 Final absorption model (ne=6, no=3): Rint= 0.11276, Acormin=0.001, Acormax=1.270, Acor_av=0.194 Combined refinement in use Rint: 0.63620 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 116 pars with 6786 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.32956 Using Levenberg-Marquardt: 0.00010 New wR= 0.29053 There are 13 clusters with unrefined scales (size 1-3) Rint for refined data: 0.34646 with corrections 0.27216 Rint for all data: 0.63620 with corrections 0.56989 6 observations identified as outliers and rejected Cycle 2 wR= 0.27593 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= 0.25645 There are 13 clusters with unrefined scales (size 1-3) Rint for refined data: 0.31425 with corrections 0.15574 Rint for all data: 0.63620 with corrections 0.54697 0 observations identified as outliers and rejected Cycle 3 wR= 0.25645 Using Levenberg-Marquardt: 0.00100 New wR= 0.60773 Using Levenberg-Marquardt: 0.01000 New wR= 0.25308 There are 13 clusters with unrefined scales (size 1-3) Rint for refined data: 0.31425 with corrections 0.12706 Rint for all data: 0.63620 with corrections 0.53500 0 observations identified as outliers and rejected Cycle 4 wR= 0.25308 Using Levenberg-Marquardt: 0.00100 New wR= 0.64009 Using Levenberg-Marquardt: 0.01000 New wR= 0.25303 There are 13 clusters with unrefined scales (size 1-3) Rint for refined data: 0.31425 with corrections 0.12591 Rint for all data: 0.63620 with corrections 0.53722 Final wR= 0.25303 Final frame scales: Min= 0.8633 Max= 1.2191 Final absorption correction factors: Amin= 0.2843 Amax= 5.0300 PROFFIT INFO: Inet (after scale3 abspack): min=886.9302 max=17142004.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=271.3532 max=128377.1875 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 4, Friedel: 1 Min/max for: run:1/1 frame:2/100 556 reflections read from tmp file 418 reflections are rejected (109 as outliers, 309 as groups of 1 refl) Redundancy: 1 2+ Number of groups: 0 69 Initial Chi^2= 0.31051 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.75242 Current error model SIG(F2)^2 = 184.29*I_RAW + 0.00*I_BACK+(0.02547*)^2 Cycle 2, Chi^2= 1.02865 Current error model SIG(F2)^2 = 184.59*I_RAW + 0.00*I_BACK+(0.01400*)^2 Cycle 3, Chi^2= 0.99632 Current error model SIG(F2)^2 = 171.76*I_RAW + 0.00*I_BACK+(0.01686*)^2 Cycle 4, Chi^2= 1.00411 Current error model SIG(F2)^2 = 180.35*I_RAW + 0.00*I_BACK+(0.01536*)^2 Cycle 5, Chi^2= 0.99845 Current error model SIG(F2)^2 = 176.25*I_RAW + 0.00*I_BACK+(0.01613*)^2 Cycle 6, Chi^2= 1.00097 Current error model SIG(F2)^2 = 178.50*I_RAW + 0.00*I_BACK+(0.01573*)^2 Cycle 7, Chi^2= 0.99953 Current error model SIG(F2)^2 = 177.35*I_RAW + 0.00*I_BACK+(0.01594*)^2 Cycle 8, Chi^2= 1.00026 Current error model SIG(F2)^2 = 177.96*I_RAW + 0.00*I_BACK+(0.01583*)^2 Cycle 9, Chi^2= 0.99987 Current error model SIG(F2)^2 = 177.64*I_RAW + 0.00*I_BACK+(0.01588*)^2 Final Chi^2= 0.99987 Final error model SIG(F2)^2 = 177.64*I_RAW + 0.00*I_BACK+(0.01588*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 17142004- 1622340 55 3600260.40 71.42 100.00 1610004- 707981 55 1059313.80 46.98 100.00 704490- 407122 55 555418.98 37.78 100.00 403089- 250346 55 312766.59 27.57 100.00 248153- 148299 55 200454.11 22.54 100.00 147372- 86708 55 113265.77 17.87 100.00 85825- 57660 55 71099.82 16.01 100.00 57297- 8236 55 34010.36 11.44 100.00 7871- 3291 55 5065.10 3.72 69.09 3162- 887 61 2037.45 2.75 26.23 ------------------------------------------------------------------------------------ 17142004- 887 556 588966.38 25.56 88.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.78- 1.17 55 1545097.41 42.88 100.00 1.17- 0.94 55 1026467.54 37.00 98.18 0.93- 0.78 55 862269.54 31.82 94.55 0.78- 0.69 55 726174.34 27.01 100.00 0.68- 0.62 55 428353.66 23.97 87.27 0.62- 0.57 55 511707.92 24.29 92.73 0.57- 0.53 55 271018.57 18.81 83.64 0.53- 0.49 55 250105.13 18.45 76.36 0.49- 0.46 55 200202.85 17.55 81.82 0.46- 0.39 61 119483.19 14.96 75.41 ------------------------------------------------------------------------------------ 4.78- 0.39 556 588966.38 25.56 88.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.78- 1.17 55 1545097.41 42.88 100.00 4.78- 0.94 110 1285782.48 39.94 99.09 4.78- 0.78 165 1144611.50 37.24 97.58 4.78- 0.69 220 1040002.21 34.68 98.18 4.78- 0.62 275 917672.50 32.54 96.00 4.78- 0.57 330 850011.73 31.16 95.45 4.78- 0.53 385 767298.42 29.40 93.77 4.78- 0.49 440 702649.26 28.03 91.59 4.78- 0.46 495 646821.88 26.87 90.51 4.78- 0.39 556 588966.38 25.56 88.85 ------------------------------------------------------------------------------------ 4.78- 0.39 556 588966.38 25.56 88.85 Scale applied to data: s=0.058336 (maximum obs:17142004.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.537; Rsigma 0.022: data 556 -> merged 423 With outlier rejection... Rint 0.454; Rsigma 0.022: data 551 -> merged 423 Rejected total: 5, method kkm 5, method Blessing 0 Completeness direct cell (a, b, c) = (5.524, 4.787, 5.527), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.393734, 4.786776 completeness table (Laue group: Pmmm, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 22 44 1.45 50.00 32 1.41 - 1.10 23 44 1.52 52.27 35 1.10 - 0.94 22 44 1.68 50.00 37 0.94 - 0.85 18 44 1.61 40.91 29 0.85 - 0.78 19 44 1.47 43.18 28 0.78 - 0.73 18 44 1.44 40.91 26 0.73 - 0.69 20 44 1.50 45.45 30 0.69 - 0.66 15 44 1.40 34.09 21 0.66 - 0.63 20 44 1.40 45.45 28 0.63 - 0.60 19 46 1.26 41.30 24 --------------------------------------------------------------- 5.92 - 0.60 196 442 1.48 44.34 290 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:34:20 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.912045 5.913651 5.911136 60.0259 89.9561 59.9603 551 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 272 281 277 275 415 375 373 551 N (int>3sigma) = 0 236 281 241 237 379 333 335 489 Mean intensity = 0.0 31.1 13.4 30.9 27.7 25.1 32.2 35.4 34.0 Mean int/sigma = 0.0 24.6 22.6 24.6 23.9 23.9 25.2 25.3 25.0 Lattice type: P chosen Volume: 146.16 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 Unitcell: 5.909 5.911 5.912 90.04 119.97 119.95 Niggli form: a.a = 34.920 b.b = 34.942 c.c = 34.952 b.c = -0.027 a.c = -17.450 a.b = -17.438 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.088 CUBIC F-lattice R(int) = 0.374 [ 404] Vol = 584.6 Cell: 8.363 8.365 8.357 90.05 89.99 89.99 Volume: 584.63 Matrix: 1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.326 [ 247] Vol = 438.5 Cell: 5.915 5.911 14.487 90.01 90.02 120.04 Volume: 438.48 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.292 [ 61] Vol = 438.5 Trigonal Cell: 5.915 5.911 14.487 90.01 90.02 120.04 Volume: 438.48 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.040 TETRAGONAL I-lattice R(int) = 0.287 [ 236] Vol = 292.3 Cell: 5.914 5.915 8.357 89.97 89.96 89.99 Volume: 292.32 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.051 TETRAGONAL I-lattice R(int) = 0.287 [ 236] Vol = 292.3 Cell: 5.915 5.914 8.357 90.04 90.03 89.99 Volume: 292.32 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.042 ORTHORHOMBIC I-lattice R(int) = 0.197 [ 321] Vol = 292.3 Cell: 5.915 5.914 8.357 89.96 89.97 89.99 Volume: 292.32 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.026 ORTHORHOMBIC I-lattice R(int) = 0.355 [ 177] Vol = 292.3 Cell: 5.909 8.363 5.915 90.00 89.95 90.01 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.197 [ 198] Vol = 292.3 Cell: 5.914 5.915 8.357 90.03 90.04 89.99 Volume: 292.32 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.040 MONOCLINIC I-lattice R(int) = 0.177 [ 60] Vol = 292.3 Cell: 5.909 5.915 8.363 90.00 90.01 90.05 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.015 MONOCLINIC I-lattice R(int) = 0.461 [ 47] Vol = 292.3 Cell: 5.909 8.363 5.915 90.00 90.05 89.99 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.071 MONOCLINIC C-lattice R(int) = 0.263 [ 109] Vol = 292.3 Cell: 10.241 5.911 5.912 90.04 125.23 89.94 Volume: 292.32 Matrix: 2.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.007 [ 3] Vol = 146.2 Cell: 5.909 5.911 5.912 90.04 119.97 119.95 Volume: 146.16 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 281 0 369 375 551 N (int>3sigma) = 0 0 0 0 281 0 325 333 489 Mean intensity = 0.0 0.0 0.0 0.0 13.4 0.0 29.0 32.2 34.0 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 24.5 25.2 25.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.251 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 45 121 N I>3s 5 5 34 121 0.5 0.5 0.3 16.1 8.0 8.0 4.7 25.1 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 0.374 378 Fd-3m 1 1 227 C N N N N 37 2284 0.371 415 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363454 8.364625 8.357048 90.0524 89.9912 89.9880 ZERR 1.00 0.000553 0.005110 0.003266 0.0019 0.0015 0.0203 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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: Pmmm # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 17142004- 1323336 62 61 42 1.5 3019653.51 54.72 0.463 0.478 1303663- 710419 61 60 42 1.4 921446.07 38.14 0.716 0.716 704490- 455610 66 64 42 1.5 540610.68 33.48 0.391 0.391 455418- 263294 65 64 42 1.5 341907.43 28.08 0.261 0.261 259427- 148299 63 63 42 1.5 209544.87 23.42 0.054 0.054 147701- 88606 52 52 42 1.2 115690.58 18.20 0.053 0.053 88518- 63262 48 48 42 1.1 74955.49 16.17 0.068 0.068 63226- 34861 43 43 42 1.0 51284.08 14.17 0.169 0.169 33311- 3026 51 51 42 1.2 8707.04 5.65 0.222 0.226 2775- 887 45 45 45 1.0 1825.40 2.69 0.000 0.000 ------------------------------------------------------------------------------------------- 17142004- 887 556 551 423 1.3 583508.72 25.01 0.454 0.463 Statistics vs resolution - point group symmetry: Pmmm resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.11 66 63 42 1.5 1416636.29 40.89 0.210 0.210 0.016 1.11-0.86 71 69 42 1.6 1027521.63 32.35 0.481 0.512 0.019 0.85-0.72 62 62 42 1.5 716157.93 29.22 0.612 0.612 0.021 0.72-0.64 59 59 42 1.4 595359.34 24.94 0.470 0.470 0.024 0.64-0.58 57 57 42 1.4 502808.81 25.32 0.375 0.375 0.027 0.58-0.55 54 54 42 1.3 332854.01 19.68 0.729 0.729 0.032 0.54-0.50 52 52 42 1.2 270629.99 19.75 0.836 0.836 0.030 0.50-0.48 47 47 42 1.1 191152.23 16.71 0.374 0.374 0.038 0.48-0.45 43 43 42 1.0 156477.82 15.91 0.994 0.994 0.037 0.45-0.39 45 45 45 1.0 120412.32 15.30 0.000 0.000 0.040 ------------------------------------------------------------------------------------------------------ inf-0.39 556 551 423 1.3 583508.72 25.01 0.454 0.463 0.022 inf-0.60 295 290 196 1.5 871370.92 30.68 0.451 0.461 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pmmm resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.11 63 82 42 51.2 1.5 1416636.29 54.78 0.210 0.010 1.11-0.86 69 91 42 46.2 1.6 1027521.63 47.41 0.481 0.014 0.85-0.72 62 98 42 42.9 1.5 716157.93 42.88 0.612 0.016 0.72-0.64 59 103 42 40.8 1.4 595359.34 33.96 0.470 0.018 0.64-0.58 57 116 42 36.2 1.4 502808.81 33.02 0.375 0.021 0.58-0.55 54 99 42 42.4 1.3 332854.01 24.75 0.729 0.027 0.54-0.50 52 134 42 31.3 1.2 270629.99 25.44 0.836 0.023 0.50-0.48 47 129 42 32.6 1.1 191152.23 18.98 0.374 0.027 0.48-0.45 43 153 42 27.5 1.0 156477.82 16.71 0.994 0.028 0.45-0.39 45 456 45 9.9 1.0 120412.32 15.30 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.39 551 1472 423 28.7 1.3 583508.72 33.08 0.454 0.016 inf-0.60 290 441 196 44.4 1.5 871370.92 43.07 0.451 0.014 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 -1.0 No constraint UB - matrix: -0.034829 0.007489 -0.077005 ( 0.000011 0.000012 0.000014 ) -0.008073 0.083589 0.011865 ( 0.000008 0.000009 0.000010 ) 0.076901 0.012144 -0.033649 ( 0.000010 0.000010 0.000012 ) M - matrix: 0.007192 -0.000002 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000006 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.034829 0.007489 -0.077005 ( 0.000011 0.000012 0.000014 ) -0.008073 0.083589 0.011865 ( 0.000008 0.000009 0.000010 ) 0.076901 0.012144 -0.033649 ( 0.000010 0.000010 0.000012 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3639(10) 8.3646(9) 8.3576(12) 90.051(10) 89.988(11) 89.986(9) V = 584.70(13) unit cell: 8.3620(3) 8.3620(3) 8.3620(3) 90.0 90.0 90.0 V = 584.70(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.908) PROFFIT INFO: signal sum: min=488.0000 max=19711404.0000 PROFFIT INFO: signal sum lp corr: min=691.5840 max=2242846.6075 PROFFIT INFO: background sum: min=885.0000 max=16754.0000 PROFFIT INFO: background sum sig2: min=674.0000 max=10584.0000 PROFFIT INFO: num of signal pixels: min=68 max=821 PROFFIT INFO: Inet: min=1508.9105 max=4893483.5000 PROFFIT INFO: sig(Inet): min=248.5227 max=63787.0664 PROFFIT INFO: Inet/sig(Inet): min=1.30 max=252.61 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 14 84 144 244 262 436 736 998 1112 Percent 0.0 0.0 1.3 7.6 12.9 21.9 23.6 39.2 66.2 89.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 556 100.00 (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 556 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4893484- 1731533 55 2559862.19 140.09 100.00 1707466- 1089842 55 1377149.71 108.97 100.00 1077394- 363545 55 609841.82 94.29 100.00 354969- 229121 55 269929.36 68.21 100.00 228869- 171697 55 202303.04 51.58 100.00 171292- 146833 55 160454.80 36.22 100.00 146162- 106300 55 123978.43 29.74 100.00 105840- 6378 55 58422.15 21.35 100.00 6309- 4028 55 4937.65 5.02 81.82 4014- 1509 61 3186.84 3.49 47.54 ------------------------------------------------------------------------------------ 4893484- 1509 556 531245.95 55.33 92.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 55 829759.09 79.56 100.00 1.32- 1.09 55 949088.68 78.46 100.00 1.09- 0.96 55 575726.85 70.27 100.00 0.96- 0.85 55 623820.97 68.80 98.18 0.85- 0.80 55 600697.25 63.67 98.18 0.80- 0.73 55 385565.70 43.96 92.73 0.73- 0.70 55 312198.36 37.60 90.91 0.70- 0.65 55 550299.73 54.12 96.36 0.65- 0.62 55 263591.08 30.02 70.91 0.62- 0.59 61 252157.83 29.65 78.69 ------------------------------------------------------------------------------------ 4.82- 0.59 556 531245.95 55.33 92.45 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:34:20 2018 Sorting 556 observations 76 unique observations with > 7.00 F2/sig(F2) 556 observations in 1 runs Run # start # end # total # 1 1 99 99 Total number of frames 99 Maximum number of 76 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 556 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 446 observations > 7.00 F2/sig(F2) 446 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Removing 'redundancy=1' reflections Average redundancy: 5.7 (Out of 446 removed 8 = 438, unique = 77) 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 438 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 77 unique data precomputed (should be 77) 77 unique data with 438 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.7 (Out of 438 removed 0 = 438, unique = 77) 77 unique data precomputed (should be 77) 77 unique data with 438 observations RMS deviation of equivalent data = 0.14046 Rint = 0.10971 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10971, wR= 0.14550 Trying model 1 (ne=2, no=0)... Results: Rint= 0.03988, wR= 0.05086, Acormin=0.609, Acormax=1.056, Acor_av=0.805 F test: Probability=1.000, F= 7.461 Trying model 2 (ne=2, no=1)... Results: Rint= 0.03128, wR= 0.04107, Acormin=0.603, Acormax=1.170, Acor_av=0.816 F test: Probability=1.000, F= 1.612 Trying model 3 (ne=4, no=0)... Results: Rint= 0.02473, wR= 0.03210, Acormin=0.655, Acormax=1.172, Acor_av=0.866 F test: Probability=1.000, F= 1.572 Trying model 4 (ne=4, no=1)... Results: Rint= 0.02410, wR= 0.03180, Acormin=0.656, Acormax=1.177, Acor_av=0.870 F test: Probability=0.654, F= 1.044 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01849, wR= 0.02553, Acormin=0.708, Acormax=1.272, Acor_av=0.903 F test: Probability=1.000, F= 1.737 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01680, wR= 0.02409, Acormin=0.718, Acormax=1.315, Acor_av=0.917 F test: Probability=0.953, F= 1.201 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01664, wR= 0.02364, Acormin=0.702, Acormax=1.330, Acor_av=0.919 F test: Probability=0.534, F= 1.009 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01533, wR= 0.02181, Acormin=0.727, Acormax=1.358, Acor_av=0.927 F test: Probability=0.916, F= 1.165 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01459, wR= 0.02012, Acormin=0.740, Acormax=1.706, Acor_av=0.935 F test: Probability=0.974, F= 1.241 Final absorption model (ne=6, no=5): Rint= 0.01459, Acormin=0.740, Acormax=1.706, Acor_av=0.935 Combined refinement in use Rint: 0.10982 There are 50 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 97 pars with 4753 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14046 Using Levenberg-Marquardt: 0.00010 New wR= 0.01867 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10971 with corrections 0.01259 Rint for all data: 0.10982 with corrections 0.01282 0 observations identified as outliers and rejected Cycle 2 wR= 0.01867 Using Levenberg-Marquardt: 0.00001 New wR= 0.01755 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10971 with corrections 0.01193 Rint for all data: 0.10982 with corrections 0.01215 0 observations identified as outliers and rejected Cycle 3 wR= 0.01755 Using Levenberg-Marquardt: 0.00000 New wR= 0.01719 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10971 with corrections 0.01189 Rint for all data: 0.10982 with corrections 0.01211 0 observations identified as outliers and rejected Cycle 4 wR= 0.01719 Using Levenberg-Marquardt: 0.00000 New wR= 0.01711 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10971 with corrections 0.01197 Rint for all data: 0.10982 with corrections 0.01220 0 observations identified as outliers and rejected Cycle 5 wR= 0.01711 Using Levenberg-Marquardt: 0.00000 New wR= 0.01710 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10971 with corrections 0.01199 Rint for all data: 0.10982 with corrections 0.01222 Final wR= 0.01710 Final frame scales: Min= 0.9629 Max= 1.0720 Final absorption correction factors: Amin= 0.4252 Amax= 1.3031 PROFFIT INFO: Inet (after scale3 abspack): min=1715.8340 max=4467976.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=296.7238 max=61455.6602 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:2/100 556 reflections read from tmp file 16 reflections are rejected (8 as outliers, 8 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 11 11 10 17 14 11 5 4 11 Initial Chi^2= 0.23795 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.05746 Current error model SIG(F2)^2 = 112.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 118.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 118.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4467976- 1670323 55 2500008.15 129.97 100.00 1670123- 1105761 55 1354241.90 64.90 100.00 1099485- 324360 55 614237.08 63.56 100.00 321258- 227247 55 260567.57 40.43 100.00 222486- 178364 55 205809.10 30.75 100.00 173698- 138411 55 150351.46 21.00 100.00 138116- 112833 55 125495.09 19.53 100.00 112044- 6406 55 59408.95 13.82 100.00 6273- 3996 55 4866.56 4.33 100.00 3955- 1716 61 3194.34 3.57 75.41 ------------------------------------------------------------------------------------ 4467976- 1716 556 522156.61 38.80 97.30 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 55 800023.58 75.96 100.00 1.32- 1.09 55 957078.19 68.89 100.00 1.09- 0.96 55 572933.57 44.55 100.00 0.96- 0.85 55 619797.04 41.77 100.00 0.85- 0.80 55 581291.13 38.69 100.00 0.80- 0.73 55 377037.31 27.06 100.00 0.73- 0.70 55 320420.42 23.26 98.18 0.70- 0.65 55 518068.69 32.83 100.00 0.65- 0.62 55 255195.31 18.75 80.00 0.62- 0.59 61 249468.66 18.47 95.08 ------------------------------------------------------------------------------------ 4.82- 0.59 556 522156.61 38.80 97.30 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 55 800023.58 75.96 100.00 4.82- 1.09 110 878550.89 72.43 100.00 4.82- 0.96 165 776678.45 63.14 100.00 4.82- 0.85 220 737458.09 57.79 100.00 4.82- 0.80 275 706224.70 53.97 100.00 4.82- 0.73 330 651360.14 49.49 100.00 4.82- 0.70 385 604083.03 45.74 99.74 4.82- 0.65 440 593331.24 44.13 99.77 4.82- 0.62 495 555760.58 41.31 97.58 4.82- 0.59 556 522156.61 38.80 97.30 ------------------------------------------------------------------------------------ 4.82- 0.59 556 522156.61 38.80 97.30 Scale applied to data: s=0.223815 (maximum obs:4467976.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.012; Rsigma 0.016: data 556 -> merged 102 With outlier rejection... Rint 0.012; Rsigma 0.017: data 552 -> merged 102 Rejected total: 4, method kkm 3, method Blessing 1 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586899, 4.827816 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 3.00 80.00 24 1.61 - 1.21 10 10 4.70 100.00 47 1.17 - 1.01 10 10 6.90 100.00 69 0.99 - 0.89 10 10 6.20 100.00 62 0.88 - 0.81 10 10 6.30 100.00 63 0.81 - 0.74 10 10 5.90 100.00 59 0.73 - 0.71 10 10 5.70 100.00 57 0.70 - 0.66 10 10 5.40 100.00 54 0.65 - 0.64 10 10 4.40 100.00 44 0.63 - 0.60 10 10 5.00 100.00 50 --------------------------------------------------------------- 5.92 - 0.60 98 100 5.40 98.00 529 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:34:20 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.912045 5.913651 5.911136 60.0259 89.9561 59.9603 551 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 272 281 277 275 415 375 373 551 N (int>3sigma) = 0 236 281 241 237 379 333 335 489 Mean intensity = 0.0 31.1 13.4 30.9 27.7 25.1 32.2 35.4 34.0 Mean int/sigma = 0.0 24.6 22.6 24.6 23.9 23.9 25.2 25.3 25.0 Lattice type: P chosen Volume: 146.16 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 Unitcell: 5.909 5.911 5.912 90.04 119.97 119.95 Niggli form: a.a = 34.920 b.b = 34.942 c.c = 34.952 b.c = -0.027 a.c = -17.450 a.b = -17.438 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.088 CUBIC F-lattice R(int) = 0.374 [ 404] Vol = 584.6 Cell: 8.363 8.365 8.357 90.05 89.99 89.99 Volume: 584.63 Matrix: 1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.326 [ 247] Vol = 438.5 Cell: 5.915 5.911 14.487 90.01 90.02 120.04 Volume: 438.48 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.292 [ 61] Vol = 438.5 Trigonal Cell: 5.915 5.911 14.487 90.01 90.02 120.04 Volume: 438.48 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.040 TETRAGONAL I-lattice R(int) = 0.287 [ 236] Vol = 292.3 Cell: 5.914 5.915 8.357 89.97 89.96 89.99 Volume: 292.32 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.051 TETRAGONAL I-lattice R(int) = 0.287 [ 236] Vol = 292.3 Cell: 5.915 5.914 8.357 90.04 90.03 89.99 Volume: 292.32 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.042 ORTHORHOMBIC I-lattice R(int) = 0.197 [ 321] Vol = 292.3 Cell: 5.915 5.914 8.357 89.96 89.97 89.99 Volume: 292.32 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.026 ORTHORHOMBIC I-lattice R(int) = 0.355 [ 177] Vol = 292.3 Cell: 5.909 8.363 5.915 90.00 89.95 90.01 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.197 [ 198] Vol = 292.3 Cell: 5.914 5.915 8.357 90.03 90.04 89.99 Volume: 292.32 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.040 MONOCLINIC I-lattice R(int) = 0.177 [ 60] Vol = 292.3 Cell: 5.909 5.915 8.363 90.00 90.01 90.05 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.015 MONOCLINIC I-lattice R(int) = 0.461 [ 47] Vol = 292.3 Cell: 5.909 8.363 5.915 90.00 90.05 89.99 Volume: 292.32 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.071 MONOCLINIC C-lattice R(int) = 0.263 [ 109] Vol = 292.3 Cell: 10.241 5.911 5.912 90.04 125.23 89.94 Volume: 292.32 Matrix: 2.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.007 [ 3] Vol = 146.2 Cell: 5.909 5.911 5.912 90.04 119.97 119.95 Volume: 146.16 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 281 0 369 375 551 N (int>3sigma) = 0 0 0 0 281 0 325 333 489 Mean intensity = 0.0 0.0 0.0 0.0 13.4 0.0 29.0 32.2 34.0 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 24.5 25.2 25.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.251 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 45 121 N I>3s 5 5 34 121 0.5 0.5 0.3 16.1 8.0 8.0 4.7 25.1 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 0.374 378 Fd-3m 1 1 227 C N N N N 37 2284 0.371 415 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363454 8.364625 8.357048 90.0524 89.9912 89.9880 ZERR 1.00 0.000553 0.005110 0.003266 0.0019 0.0015 0.0203 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4380843- 1012163 118 116 25 4.6 1837228.98 91.08 0.010 0.012 979219- 182157 158 158 25 6.3 323527.19 44.43 0.015 0.016 166068- 94128 135 135 25 5.4 130162.19 19.30 0.023 0.028 61975- 2148 145 143 27 5.3 7931.62 5.46 0.091 0.106 ------------------------------------------------------------------------------------------- 4380843- 2148 556 552 102 5.4 512576.04 37.99 0.012 0.014 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 130 126 25 5.0 784659.52 66.07 0.012 0.015 0.010 1.01-0.80 149 149 25 6.0 590654.64 39.87 0.009 0.010 0.015 0.78-0.67 155 155 26 6.0 405688.79 27.91 0.012 0.013 0.022 0.66-0.59 122 122 26 4.7 272012.88 19.51 0.017 0.018 0.029 ------------------------------------------------------------------------------------------------------ inf-0.59 556 552 102 5.4 512576.04 37.99 0.012 0.014 0.017 inf-0.60 531 527 97 5.4 528334.74 39.03 0.012 0.014 0.016 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 126 27 25 92.6 5.0 784659.52 159.24 0.012 0.004 1.01-0.80 149 25 25 100.0 6.0 590654.64 101.69 0.009 0.006 0.78-0.67 155 26 26 100.0 6.0 405688.79 72.29 0.012 0.010 0.66-0.59 122 29 26 89.7 4.7 272012.88 43.22 0.017 0.014 -------------------------------------------------------------------------------------------- inf-0.59 552 107 102 95.3 5.4 512576.04 93.65 0.012 0.007 inf-0.60 527 99 97 98.0 5.4 528334.74 96.47 0.012 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:36:34 2018) ID: 2932; threads 38; handles 877; mem 518200.00 (1229532.00)kB; time: 1w 5d 21h 42m 5s MEMORY INFO: Memory PF:0.0, Ph:170.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:506.1,peak PF: 708.5, WS: 270.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:170.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:507.8,peak PF: 708.5, WS: 272.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:36:34 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000028 0.000027 0.000027 ) 0.087412 -0.166882 0.063604 ( 0.000019 0.000018 0.000018 ) 0.055227 -0.024260 0.122680 ( 0.000023 0.000022 0.000023 ) 5.91535 ( 0.00143 ) 5.92288 ( 0.00096 ) 5.91286 ( 0.00127 ) 59.95509 ( 0.01961 ) 89.89521 ( 0.01861 ) 59.99590 ( 0.02089 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 12:36:35 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000028 0.000027 0.000027 ) 0.087412 -0.166882 0.063604 ( 0.000019 0.000018 0.000018 ) 0.055227 -0.024260 0.122680 ( 0.000023 0.000022 0.000023 ) M - matrix: 0.021595 -0.014391 0.007177 ( 0.000007 0.000005 0.000005 ) -0.014391 0.028762 -0.014365 ( 0.000005 0.000006 0.000004 ) 0.007177 -0.014365 0.021573 ( 0.000005 0.000004 0.000007 ) unit cell: 5.9154(14) 5.9229(10) 5.9129(13) 59.96(2) 89.895(19) 60.00(2) V = 146.51(5) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb PROFFITPEAK info: 1279 peaks in the peak location table UB fit with 559 obs out of 600 (total:600,skipped:0) (93.17%) UB - matrix: -0.104100 -0.015309 0.049810 ( 0.000058 0.000057 0.000060 ) 0.087112 -0.166781 0.063585 ( 0.000060 0.000058 0.000061 ) 0.055247 -0.023972 0.122559 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021478 -0.014259 0.007125 ( 0.000017 0.000013 0.000013 ) -0.014259 0.028625 -0.014305 ( 0.000013 0.000020 0.000014 ) 0.007125 -0.014305 0.021545 ( 0.000013 0.000014 0.000019 ) unit cell: 5.916(3) 5.915(3) 5.912(3) 60.03(6) 89.99(4) 60.12(5) V = 146.62(13) UB fit with 559 obs out of 600 (total:600,skipped:0) (93.17%) UB - matrix: -0.104100 -0.015309 0.049810 ( 0.000058 0.000057 0.000060 ) 0.087112 -0.166781 0.063585 ( 0.000060 0.000058 0.000061 ) 0.055247 -0.023972 0.122559 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021478 -0.014259 0.007125 ( 0.000017 0.000013 0.000013 ) -0.014259 0.028625 -0.014305 ( 0.000013 0.000020 0.000014 ) 0.007125 -0.014305 0.021545 ( 0.000013 0.000014 0.000019 ) unit cell: 5.916(3) 5.915(3) 5.912(3) 60.03(6) 89.99(4) 60.12(5) V = 146.62(13) OTKP changes: 109 1 1 1 UB - matrix: -0.104072 -0.015081 0.049572 ( 0.000056 0.000055 0.000058 ) 0.087182 -0.166792 0.063572 ( 0.000059 0.000058 0.000061 ) 0.055233 -0.024180 0.122474 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021482 -0.014307 0.007148 ( 0.000017 0.000013 0.000013 ) -0.014307 0.028632 -0.014312 ( 0.000013 0.000020 0.000014 ) 0.007148 -0.014312 0.021499 ( 0.000013 0.000014 0.000019 ) UB fit with 556 obs out of 600 (total:600,skipped:0) (92.67%) unit cell: 5.925(3) 5.925(3) 5.922(3) 60.01(6) 89.98(4) 60.01(5) V = 147.08(13) UB fit with 556 obs out of 600 (total:600,skipped:0) (92.67%) UB - matrix: -0.104072 -0.015081 0.049572 ( 0.000056 0.000055 0.000058 ) 0.087182 -0.166792 0.063572 ( 0.000059 0.000058 0.000061 ) 0.055233 -0.024180 0.122474 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021482 -0.014307 0.007148 ( 0.000017 0.000013 0.000013 ) -0.014307 0.028632 -0.014312 ( 0.000013 0.000020 0.000014 ) 0.007148 -0.014312 0.021499 ( 0.000013 0.000014 0.000019 ) unit cell: 5.925(3) 5.925(3) 5.922(3) 60.01(6) 89.98(4) 60.01(5) V = 147.08(13) OTKP changes: 109 1 1 1 OTKP changes: 109 1 1 1 OTKP changes: 109 1 1 1 UB - matrix: -0.104090 -0.015047 0.049558 ( 0.000056 0.000055 0.000058 ) 0.087178 -0.166817 0.063576 ( 0.000059 0.000058 0.000061 ) 0.055216 -0.024187 0.122468 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021483 -0.014312 0.007146 ( 0.000017 0.000013 0.000013 ) -0.014312 0.028639 -0.014313 ( 0.000013 0.000020 0.000014 ) 0.007146 -0.014313 0.021496 ( 0.000013 0.000014 0.000019 ) UB fit with 556 obs out of 600 (total:600,skipped:0) (92.67%) unit cell: 5.925(3) 5.925(3) 5.923(3) 60.01(6) 89.97(4) 60.00(5) V = 147.08(13) 600 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.985) HKL list info: 802 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104090 -0.015047 0.049558 ( 0.000056 0.000055 0.000058 ) 0.087178 -0.166817 0.063576 ( 0.000059 0.000058 0.000061 ) 0.055216 -0.024187 0.122468 ( 0.000064 0.000063 0.000066 ) M - matrix: 0.021483 -0.014312 0.007146 ( 0.000017 0.000013 0.000013 ) -0.014312 0.028639 -0.014313 ( 0.000013 0.000020 0.000014 ) 0.007146 -0.014313 0.021496 ( 0.000013 0.000014 0.000019 ) UB fit with 556 obs out of 600 (total:600,skipped:0) (92.67%) unit cell: 5.925(3) 5.925(3) 5.923(3) 60.01(6) 89.97(4) 60.00(5) V = 147.08(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 558 obs out of 600 (total:600,skipped:0) (93.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 0.992 ( 0.141) | 1.234 ( 0.538) | 1.355 ( 0.852) | 1.33- 1.09 | 45 | 1.086 ( 0.076) | 1.149 ( 0.127) | 1.216 ( 0.535) | 1.09- 0.96 | 45 | 1.127 ( 0.080) | 1.241 ( 0.459) | 1.148 ( 0.477) | 0.96- 0.85 | 45 | 1.143 ( 0.051) | 1.154 ( 0.124) | 1.276 ( 0.482) | 0.85- 0.81 | 45 | 1.163 ( 0.055) | 1.202 ( 0.131) | 1.137 ( 0.388) | 0.81- 0.74 | 45 | 1.171 ( 0.050) | 1.138 ( 0.156) | 1.322 ( 0.408) | 0.73- 0.70 | 45 | 1.186 ( 0.047) | 1.193 ( 0.148) | 1.280 ( 0.441) | 0.70- 0.66 | 45 | 1.190 ( 0.061) | 1.193 ( 0.165) | 1.235 ( 0.409) | 0.66- 0.62 | 45 | 1.197 ( 0.083) | 1.232 ( 0.171) | 1.185 ( 0.447) | 0.62- 0.59 | 42 | 1.202 ( 0.070) | 1.212 ( 0.199) | 1.327 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 447 | 1.145 ( 0.098) | 1.195 ( 0.266) | 1.247 ( 0.516) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) UB - matrix: -0.104312 -0.014699 0.049249 ( 0.000029 0.000028 0.000027 ) 0.087321 -0.167021 0.063578 ( 0.000020 0.000019 0.000019 ) 0.055280 -0.024491 0.122573 ( 0.000028 0.000027 0.000026 ) M - matrix: 0.021562 -0.014405 0.007190 ( 0.000008 0.000005 0.000005 ) -0.014405 0.028712 -0.014345 ( 0.000005 0.000007 0.000005 ) 0.007190 -0.014345 0.021492 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9243(15) 5.9272(11) 5.9263(15) 60.02(2) 89.97(2) 59.89(2) V = 146.97(5) OTKP changes: 447 1 1 1 OTKP changes: 447 1 1 1 OTKP changes: 447 1 1 1 UB - matrix: -0.104290 -0.014938 0.049492 ( 0.000026 0.000025 0.000024 ) 0.087286 -0.167041 0.063615 ( 0.000019 0.000019 0.000018 ) 0.055317 -0.024325 0.122666 ( 0.000026 0.000026 0.000025 ) M - matrix: 0.021555 -0.014368 0.007177 ( 0.000007 0.000005 0.000005 ) -0.014368 0.028717 -0.014349 ( 0.000005 0.000006 0.000005 ) 0.007177 -0.014349 0.021543 ( 0.000005 0.000005 0.000007 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 5.9177(13) 5.9184(10) 5.9164(14) 60.03(2) 89.989(19) 59.98(2) V = 146.54(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.985) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104290 -0.014938 0.049492 ( 0.000026 0.000025 0.000024 ) 0.087286 -0.167041 0.063615 ( 0.000019 0.000019 0.000018 ) 0.055317 -0.024325 0.122666 ( 0.000026 0.000026 0.000025 ) M - matrix: 0.021555 -0.014368 0.007177 ( 0.000007 0.000005 0.000005 ) -0.014368 0.028717 -0.014349 ( 0.000005 0.000006 0.000005 ) 0.007177 -0.014349 0.021543 ( 0.000005 0.000005 0.000007 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 5.9177(13) 5.9184(10) 5.9164(14) 60.03(2) 89.989(19) 59.98(2) V = 146.54(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 8 of 457 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 45 | 1.135 ( 0.048) | 1.248 ( 0.191) | 1.401 ( 0.627) | 13.1-19.4 | 45 | 1.151 ( 0.135) | 1.265 ( 0.420) | 1.452 ( 0.892) | 19.5-24.1 | 45 | 1.168 ( 0.086) | 1.306 ( 0.393) | 1.280 ( 0.632) | 24.2-27.9 | 45 | 1.114 ( 0.091) | 1.146 ( 0.113) | 1.279 ( 0.484) | 27.9-30.9 | 45 | 1.129 ( 0.093) | 1.250 ( 0.341) | 1.215 ( 0.464) | 30.9-34.3 | 45 | 1.138 ( 0.073) | 1.151 ( 0.150) | 1.107 ( 0.329) | 34.3-37.3 | 45 | 1.142 ( 0.082) | 1.150 ( 0.175) | 1.190 ( 0.402) | 37.3-39.7 | 45 | 1.136 ( 0.118) | 1.136 ( 0.238) | 1.218 ( 0.646) | 39.7-43.1 | 45 | 1.145 ( 0.115) | 1.132 ( 0.213) | 1.218 ( 0.597) | 43.3-49.8 | 44 | 1.207 ( 0.144) | 1.143 ( 0.260) | 1.298 ( 0.492) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Fitted profile normalization line parameters e1 dimension: a=0.0016 b=0.97 e2 dimension: a=-0.0017 b=1.04 e3 dimension: a=-0.0030 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6425 lp-corr: 5345 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 677772 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2286282 PROFFITPEAK - Finished at Wed Mar 28 12:36:41 2018 PROFFITMAIN - Started at Wed Mar 28 12:36:41 2018 OTKP changes: 449 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104294 -0.014949 0.049472 ( 0.000026 0.000026 0.000025 ) 0.087280 -0.166989 0.063603 ( 0.000018 0.000017 0.000017 ) 0.055268 -0.024273 0.122625 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021550 -0.014357 0.007169 ( 0.000007 0.000004 0.000005 ) -0.014357 0.028698 -0.014337 ( 0.000004 0.000006 0.000004 ) 0.007169 -0.014337 0.021530 ( 0.000005 0.000004 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9176(13) 5.9195(9) 5.9176(12) 60.029(19) 89.985(17) 59.98(2) V = 146.62(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= -30.94 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104303 -0.014901 0.049477 ( 0.000026 0.000025 0.000025 ) 0.087286 -0.167072 0.063620 ( 0.000018 0.000017 0.000017 ) 0.055275 -0.024322 0.122635 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021553 -0.014373 0.007171 ( 0.000007 0.000004 0.000005 ) -0.014373 0.028727 -0.014349 ( 0.000004 0.000006 0.000004 ) 0.007171 -0.014349 0.021535 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9187(13) 5.9187(9) 5.9176(12) 60.020(19) 89.967(17) 59.96(2) V = 146.57(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104294 -0.014949 0.049472 ( 0.000026 0.000026 0.000025 ) 0.087280 -0.166989 0.063603 ( 0.000018 0.000017 0.000017 ) 0.055268 -0.024273 0.122625 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021550 -0.014357 0.007169 ( 0.000007 0.000004 0.000005 ) -0.014357 0.028698 -0.014337 ( 0.000004 0.000006 0.000004 ) 0.007169 -0.014337 0.021530 ( 0.000005 0.000004 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9176(13) 5.9195(9) 5.9176(12) 60.029(19) 89.985(17) 59.98(2) V = 146.62(5) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104294 -0.014949 0.049472 ( 0.000026 0.000026 0.000025 ) 0.087280 -0.166989 0.063603 ( 0.000018 0.000017 0.000017 ) 0.055268 -0.024273 0.122625 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021550 -0.014357 0.007169 ( 0.000007 0.000004 0.000005 ) -0.014357 0.028698 -0.014337 ( 0.000004 0.000006 0.000004 ) 0.007169 -0.014337 0.021530 ( 0.000005 0.000004 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9176(13) 5.9195(9) 5.9176(12) 60.029(19) 89.985(17) 59.98(2) V = 146.62(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.146783 -0.097824 0.048897 ( 0.000018 0.000018 0.000017 ) 0.000019 0.138341 -0.069123 ( 0.000023 0.000023 0.000022 ) 0.000012 0.000002 0.119802 ( 0.000024 0.000024 0.000023 ) M - matrix: 0.021545 -0.014356 0.007177 ( 0.000005 0.000004 0.000004 ) -0.014356 0.028708 -0.014346 ( 0.000004 0.000007 0.000005 ) 0.007177 -0.014346 0.021521 ( 0.000004 0.000005 0.000007 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9178(9) 5.9188(12) 5.9205(13) 60.02(2) 90.014(15) 60.008(18) V = 146.67(5) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104307 -0.014956 0.049499 ( 0.000026 0.000026 0.000025 ) 0.087289 -0.166966 0.063553 ( 0.000018 0.000018 0.000017 ) 0.055294 -0.024274 0.122594 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021557 -0.014356 0.007163 ( 0.000007 0.000005 0.000005 ) -0.014356 0.028690 -0.014327 ( 0.000005 0.000006 0.000004 ) 0.007163 -0.014327 0.021518 ( 0.000005 0.000004 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9197(9) 5.9183(12) 60.035(19) 89.976(17) 59.98(2) V = 146.63(5) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 30 reflections under beam stop or inside a detector rejection region 7 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof 606 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:36:43 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=486.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=827 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 43 75 130 142 236 403 545 606 Percent 0.0 0.0 1.3 7.1 12.4 21.5 23.4 38.9 66.5 89.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 606 100.00 (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 606 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1738382 60 2561482.50 138.32 100.00 1703940- 1100203 60 1391808.96 110.75 100.00 1089803- 365258 60 639111.63 95.91 100.00 363943- 230390 60 270143.89 68.07 100.00 230127- 172385 60 201921.11 51.11 100.00 171706- 145419 60 159740.63 36.01 100.00 144792- 106108 60 123572.83 30.36 100.00 105652- 6841 60 61785.11 21.77 100.00 6629- 4104 60 5057.78 5.14 83.33 4036- 1484 66 3205.90 3.51 50.00 ------------------------------------------------------------------------------------ 4887974- 1484 606 536450.59 55.57 92.90 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 60 733039.82 84.86 100.00 1.21- 0.96 60 875146.53 78.19 98.33 0.96- 0.81 60 533967.94 52.36 98.33 0.81- 0.72 60 699243.16 70.41 96.67 0.72- 0.65 60 500305.87 55.33 91.67 0.65- 0.59 60 601232.24 60.13 96.67 0.58- 0.55 60 378715.91 42.95 95.00 0.55- 0.51 60 413550.67 42.47 83.33 0.51- 0.48 60 325912.50 35.87 85.00 0.48- 0.40 66 324578.45 35.19 84.85 ------------------------------------------------------------------------------------ 5.26- 0.40 606 536450.59 55.57 92.90 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:36:43 2018 Sorting 606 observations 155 unique observations with > 7.00 F2/sig(F2) 606 observations in 1 runs Run # start # end # total # 1 1 107 107 Total number of frames 107 Maximum number of 155 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 606 observations in 1 runs Run # start # end # total # 1 1 107 107 Total number of frames 107 Frame #8 of 107 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 489 observations > 7.00 F2/sig(F2) 489 observations in 1 runs Run # start # end # total # 1 1 107 107 Total number of frames 107 Frame #8 of 107 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: 2.7 (Out of 489 removed 107 = 382, unique = 144) 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 382 observations in 1 runs Run # start # end # total # 1 1 107 107 Total number of frames 107 Frame #8 of 107 skipped from refinement Frame #45 of 107 skipped from refinement Frame #48 of 107 skipped from refinement 3 frames need to be skipped from refinement, because of missing redundant and/or observable data 144 unique data precomputed (should be 144) 144 unique data with 382 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.7 (Out of 382 removed 0 = 382, unique = 144) 144 unique data precomputed (should be 144) 144 unique data with 382 observations RMS deviation of equivalent data = 0.67148 Rint = 0.62067 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.60633, wR= 4.84092 Trying model 1 (ne=2, no=0)... Results: Rint= 0.85959, wR= 2.80213, Acormin=-0.583, Acormax=1.110, Acor_av=0.195 F test: Probability=0.000, F= 0.487 Trying model 2 (ne=2, no=1)... Results: Rint= 1.00118, wR= 4.56347, Acormin=-0.389, Acormax=0.926, Acor_av=0.037 F test: Probability=0.000, F= 0.354 Trying model 3 (ne=4, no=0)... Results: Rint= 0.92773, wR= 2.92108, Acormin=-0.346, Acormax=0.856, Acor_av=0.037 F test: Probability=0.000, F= 0.402 Trying model 4 (ne=4, no=1)... Results: Rint= 0.79974, wR= 2.77697, Acormin=-0.390, Acormax=0.523, Acor_av=0.008 F test: Probability=0.000, F= 0.534 Trying model 5 (ne=4, no=3)... Results: Rint= 0.88836, wR= 7.42037, Acormin=-0.149, Acormax=0.689, Acor_av=0.009 F test: Probability=0.000, F= 0.419 Trying model 6 (ne=6, no=0)... Results: Rint= 0.82534, wR= 2.40893, Acormin=-0.111, Acormax=0.388, Acor_av=0.009 F test: Probability=0.000, F= 0.478 Trying model 7 (ne=6, no=1)... Results: Rint= 0.84201, wR= 2.69652, Acormin=-0.102, Acormax=0.374, Acor_av=0.006 F test: Probability=0.000, F= 0.453 Trying model 8 (ne=6, no=3)... Results: Rint= 0.85669, wR= 4.53974, Acormin=-0.124, Acormax=0.318, Acor_av=0.007 F test: Probability=0.000, F= 0.423 Trying model 9 (ne=6, no=5)... Results: Rint= 0.86957, wR= 5.41296, Acormin=-0.021, Acormax=0.337, Acor_av=0.002 F test: Probability=0.000, F= 0.388 Trying model 10 (ne=8, no=0)... Results: Rint= 0.79444, wR= 1.64903, Acormin=-0.090, Acormax=0.285, Acor_av=0.004 F test: Probability=0.000, F= 0.474 Trying model 11 (ne=8, no=1)... Results: Rint= 0.77180, wR= 1.65259, Acormin=-0.095, Acormax=0.265, Acor_av=0.003 F test: Probability=0.000, F= 0.495 Trying model 12 (ne=8, no=3)... Results: Rint= 0.80163, wR= 1.51205, Acormin=-0.027, Acormax=0.073, Acor_av=0.002 F test: Probability=0.000, F= 0.442 Trying model 13 (ne=8, no=5)... Results: Rint= 0.74671, wR= 3.31456, Acormin=-0.017, Acormax=0.272, Acor_av=0.002 F test: Probability=0.000, F= 0.479 Trying model 14 (ne=8, no=7)... Results: Rint= 0.48239, wR= 0.52887, Acormin=-0.003, Acormax=0.617, Acor_av=0.004 F test: Probability=0.619, F= 1.047 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: 0.77186 There are 104 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 108 pars with 5886 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.67148 Using Levenberg-Marquardt: 0.00010 New wR= 0.63079 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.62067 with corrections 0.57351 Rint for all data: 0.77186 with corrections 0.73662 1 observations identified as outliers and rejected Cycle 2 wR= 0.62627 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= 0.61426 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.56636 Rint for all data: 0.77186 with corrections 0.75491 0 observations identified as outliers and rejected Cycle 3 wR= 0.61426 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= 0.59013 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.56100 Rint for all data: 0.77186 with corrections 0.75522 0 observations identified as outliers and rejected Cycle 4 wR= 0.59013 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58090 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.56472 Rint for all data: 0.77186 with corrections 0.75970 0 observations identified as outliers and rejected Cycle 5 wR= 0.58090 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57610 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.56978 Rint for all data: 0.77186 with corrections 0.76656 0 observations identified as outliers and rejected Final wR= 0.57610 Final frame scales: Min= 0.7124 Max= 17.5214 Final absorption correction factors: Amin= 0.1300 Amax= 1.1058 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 104 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 108 pars with 5886 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.80334 Using Levenberg-Marquardt: 0.00010 New wR= 0.66811 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.99225 Rint for all data: 0.77186 with corrections 1.05076 0 observations identified as outliers and rejected Cycle 2 wR= 0.66811 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= 0.62732 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.72118 Rint for all data: 0.77186 with corrections 0.84563 0 observations identified as outliers and rejected Cycle 3 wR= 0.62732 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= 0.61208 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.73263 Rint for all data: 0.77186 with corrections 0.85961 0 observations identified as outliers and rejected Cycle 4 wR= 0.61208 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60390 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.70755 Rint for all data: 0.77186 with corrections 0.84008 0 observations identified as outliers and rejected Cycle 5 wR= 0.60390 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59654 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60633 with corrections 0.70803 Rint for all data: 0.77186 with corrections 0.83943 0 observations identified as outliers and rejected Final wR= 0.59654 Final frame scales: Min= 0.5995 Max= 22.1769 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 44 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 43 pars with 946 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.13163 Using Levenberg-Marquardt: 0.00010 New wR= 0.69320 There are 7 clusters with unrefined scales (size 1-21) Rint for refined data: 0.60633 with corrections 0.65991 Rint for all data: 0.77186 with corrections 0.80724 0 observations identified as outliers and rejected Cycle 2 wR= 0.67627 Using Levenberg-Marquardt: 0.00001 New wR= 0.63961 There are 7 clusters with unrefined scales (size 1-21) Rint for refined data: 0.60633 with corrections 0.67421 Rint for all data: 0.77186 with corrections 0.82278 0 observations identified as outliers and rejected Cycle 3 wR= 0.65775 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.64986 There are 7 clusters with unrefined scales (size 1-21) Rint for refined data: 0.60633 with corrections 0.63194 Rint for all data: 0.77186 with corrections 0.78494 0 observations identified as outliers and rejected Cycle 4 wR= 0.65002 Using Levenberg-Marquardt: 0.01000 New wR= 0.63905 There are 7 clusters with unrefined scales (size 1-21) Rint for refined data: 0.60633 with corrections 0.65146 Rint for all data: 0.77186 with corrections 0.79760 0 observations identified as outliers and rejected Cycle 5 wR= 0.64535 Using Levenberg-Marquardt: 0.00100 New wR= 0.64405 There are 7 clusters with unrefined scales (size 1-21) Rint for refined data: 0.60633 with corrections 0.63900 Rint for all data: 0.77186 with corrections 0.78862 0 observations identified as outliers and rejected Final wR= 0.64405 Final frame scales: Min= 0.2770 Max= 1.3381 PROFFIT INFO: Inet (after scale3 abspack): min=931.4454 max=7007747.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=130.8777 max=78840.4844 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:2/108 606 reflections read from tmp file 543 reflections are rejected (393 as outliers, 150 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 30 1 Initial Chi^2= 1.50461 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.86305 Current error model SIG(F2)^2 = 1073.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 926.20*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 926.20*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7007747- 1683551 60 2755102.01 42.20 100.00 1671566- 818343 60 1226900.92 27.75 100.00 807531- 348911 60 539727.12 19.42 100.00 344911- 231390 60 284610.52 16.00 100.00 231324- 172425 60 200192.61 10.09 100.00 171114- 123377 60 149322.41 9.24 100.00 123132- 81576 60 102458.41 8.63 100.00 79471- 7815 60 44599.29 5.25 75.00 7764- 3764 60 5365.01 1.59 6.67 3760- 931 66 2584.89 1.43 1.52 ------------------------------------------------------------------------------------ 7007747- 931 606 525853.63 14.03 77.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 60 764025.54 28.89 85.00 1.21- 0.96 60 863054.34 21.83 86.67 0.96- 0.81 60 545918.74 14.57 76.67 0.81- 0.72 60 667290.95 15.92 80.00 0.72- 0.65 60 474572.25 12.11 73.33 0.65- 0.59 60 581095.72 13.09 80.00 0.58- 0.55 60 366028.79 9.46 75.00 0.55- 0.51 60 406469.58 9.35 73.33 0.51- 0.48 60 333043.19 7.95 71.67 0.48- 0.40 66 281475.07 7.80 74.24 ------------------------------------------------------------------------------------ 5.26- 0.40 606 525853.63 14.03 77.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 60 764025.54 28.89 85.00 5.26- 0.96 120 813539.94 25.36 85.83 5.26- 0.81 180 724332.87 21.76 82.78 5.26- 0.72 240 710072.39 20.30 82.08 5.26- 0.65 300 662972.36 18.67 80.33 5.26- 0.59 360 649326.26 17.74 80.28 5.26- 0.55 420 608855.19 16.55 79.52 5.26- 0.51 480 583556.99 15.65 78.75 5.26- 0.48 540 555722.12 14.80 77.96 5.26- 0.40 606 525853.63 14.03 77.56 ------------------------------------------------------------------------------------ 5.26- 0.40 606 525853.63 14.03 77.56 Scale applied to data: s=0.142699 (maximum obs:7007747.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.789; Rsigma 0.046: data 606 -> merged 280 With outlier rejection... Rint 0.559; Rsigma 0.051: data 496 -> merged 280 Rejected total: 110, method kkm 109, method Blessing 1 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404434, 5.273180 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 14 15 1.79 93.33 25 1.46 - 1.12 14 15 2.29 93.33 32 1.08 - 0.96 15 15 2.00 100.00 30 0.96 - 0.86 14 15 2.50 93.33 35 0.86 - 0.79 15 15 1.73 100.00 26 0.79 - 0.73 12 15 1.83 80.00 22 0.73 - 0.69 14 15 1.79 93.33 25 0.69 - 0.65 14 15 2.07 93.33 29 0.65 - 0.63 8 15 1.88 53.33 15 0.63 - 0.60 20 21 1.60 95.24 32 --------------------------------------------------------------- 5.92 - 0.60 140 156 1.94 89.74 271 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:36:44 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916409 5.919681 5.918314 60.0348 89.9755 59.9783 496 Reflections read from file xs1715a.hkl; mean (I/sigma) = 12.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 228 271 235 252 367 336 335 496 N (int>3sigma) = 0 170 271 177 188 309 260 259 384 Mean intensity = 0.0 49.5 28.3 48.1 59.4 41.3 61.7 63.9 62.2 Mean int/sigma = 0.0 10.7 11.0 10.9 11.9 10.8 12.2 12.8 12.7 Lattice type: P chosen Volume: 146.63 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.916 5.916 5.918 90.02 119.96 119.96 Niggli form: a.a = 35.000 b.b = 35.004 c.c = 35.026 b.c = -0.015 a.c = -17.484 a.b = -17.481 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.063 CUBIC F-lattice R(int) = 0.286 [ 353] Vol = 586.5 Cell: 8.370 8.375 8.367 90.06 89.98 90.01 Volume: 586.51 Matrix: 1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.061 RHOMBOHEDRAL R-lattice R(int) = 0.244 [ 184] Vol = 439.9 Cell: 5.920 5.916 14.506 90.00 90.04 120.02 Volume: 439.89 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.061 RHOMBOHEDRAL R-lattice R(int) = 0.304 [ 42] Vol = 439.9 Trigonal Cell: 5.920 5.916 14.506 90.00 90.04 120.02 Volume: 439.89 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.030 TETRAGONAL I-lattice R(int) = 0.242 [ 207] Vol = 293.3 Cell: 5.921 5.920 8.367 89.97 89.95 89.97 Volume: 293.26 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.080 TETRAGONAL I-lattice R(int) = 0.242 [ 207] Vol = 293.3 Cell: 5.920 5.921 8.367 90.05 90.03 89.97 Volume: 293.26 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.038 ORTHORHOMBIC I-lattice R(int) = 0.217 [ 276] Vol = 293.3 Cell: 5.920 5.921 8.367 89.95 89.97 89.97 Volume: 293.26 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.034 ORTHORHOMBIC I-lattice R(int) = 0.323 [ 144] Vol = 293.3 Cell: 5.916 8.370 5.922 89.98 89.94 90.00 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.021 MONOCLINIC I-lattice R(int) = 0.197 [ 167] Vol = 293.3 Cell: 5.921 5.920 8.367 90.03 90.05 89.97 Volume: 293.26 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.062 MONOCLINIC I-lattice R(int) = 0.252 [ 61] Vol = 293.3 Cell: 5.916 5.922 8.370 90.02 90.00 90.06 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.023 MONOCLINIC I-lattice R(int) = 0.359 [ 36] Vol = 293.3 Cell: 5.916 8.370 5.922 89.98 90.06 90.00 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.025 MONOCLINIC I-lattice R(int) = 0.319 [ 79] Vol = 293.3 Cell: 5.922 5.916 8.370 90.00 90.02 89.94 Volume: 293.26 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.045 MONOCLINIC C-lattice R(int) = 0.187 [ 47] Vol = 293.3 Cell: 10.251 5.916 5.918 90.02 125.21 89.96 Volume: 293.26 Matrix:-1.0000 2.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.045 [ 3] Vol = 146.6 Cell: 5.916 5.916 5.918 90.02 119.96 119.96 Volume: 146.63 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 271 0 332 332 496 N (int>3sigma) = 0 0 0 0 271 0 256 254 384 Mean intensity = 0.0 0.0 0.0 0.0 28.3 0.0 61.3 59.1 62.2 Mean int/sigma = 0.0 0.0 0.0 0.0 11.0 0.0 12.3 12.5 12.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.068 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 4 4 36 117 N I>3s 2 2 4 117 0.7 0.7 0.6 32.5 3.8 3.8 2.0 12.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.286 335 Fd-3m 1 1 227 C N N N N 37 2284 0.291 370 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370202 8.375141 8.366624 90.0581 89.9816 90.0134 ZERR 1.00 0.000521 0.004890 0.003077 0.0016 0.0013 0.0193 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5172827- 1148107 62 52 28 1.9 1765556.17 31.60 0.619 0.610 1130427- 823680 78 61 28 2.2 761428.12 16.50 0.632 0.613 818343- 606892 69 53 28 1.9 478161.89 15.93 0.592 0.586 603717- 344917 75 58 28 2.1 312218.60 12.08 0.507 0.502 332948- 210013 78 53 28 1.9 256427.36 15.01 0.245 0.236 204497- 155294 58 50 28 1.8 176738.92 7.98 0.212 0.210 154862- 105911 58 49 28 1.8 138874.23 8.59 0.295 0.283 104489- 73120 48 42 28 1.5 79196.62 5.89 0.549 0.507 72986- 6803 46 45 28 1.6 37935.97 4.12 0.776 0.824 6027- 1244 34 33 28 1.2 3301.64 1.38 0.308 0.308 ------------------------------------------------------------------------------------------- 5172827- 1244 606 496 280 1.8 435649.31 12.68 0.559 0.548 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 79 57 28 2.0 614385.06 25.39 0.647 0.648 0.024 1.08-0.86 76 61 28 2.2 693916.19 17.87 0.561 0.534 0.034 0.86-0.73 70 52 28 1.9 474009.11 14.30 0.570 0.547 0.046 0.73-0.65 69 56 29 1.9 410378.70 11.00 0.516 0.510 0.054 0.65-0.60 64 49 29 1.7 415499.25 11.30 0.417 0.422 0.058 0.59-0.55 62 49 28 1.8 337692.85 9.55 0.460 0.464 0.071 0.55-0.51 58 52 29 1.8 366706.15 8.29 0.816 0.820 0.069 0.51-0.48 55 48 29 1.7 322590.77 7.87 0.553 0.553 0.073 0.48-0.45 44 43 29 1.5 271205.51 7.95 0.281 0.281 0.083 0.45-0.40 29 29 23 1.3 275248.80 7.54 0.543 0.543 0.081 ------------------------------------------------------------------------------------------------------ inf-0.40 606 496 280 1.8 435649.31 12.68 0.559 0.548 0.051 inf-0.60 352 271 140 1.9 534687.19 16.32 0.555 0.543 0.040 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 57 30 28 93.3 2.0 614385.06 39.17 0.647 0.018 1.08-0.86 61 29 28 96.6 2.2 693916.19 30.35 0.561 0.024 0.86-0.73 52 31 28 90.3 1.9 474009.11 22.09 0.570 0.039 0.73-0.65 56 33 29 87.9 1.9 410378.70 16.76 0.516 0.039 0.65-0.60 49 35 29 82.9 1.7 415499.25 16.09 0.417 0.041 0.59-0.55 49 41 28 68.3 1.8 337692.85 12.91 0.460 0.056 0.55-0.51 52 42 29 69.0 1.8 366706.15 13.54 0.816 0.052 0.51-0.48 48 43 29 67.4 1.7 322590.77 11.09 0.553 0.058 0.48-0.45 43 62 29 46.8 1.5 271205.51 10.49 0.281 0.060 0.45-0.40 29 117 23 19.7 1.3 275248.80 9.32 0.543 0.061 -------------------------------------------------------------------------------------------- inf-0.40 496 464 280 60.3 1.8 435649.31 19.25 0.559 0.039 inf-0.60 271 156 140 89.7 1.9 534687.19 25.53 0.555 0.030 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 -1.0 2.0 -1.0 -1.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 -1.0 2.0 -1.0 -1.0 0.0 1.0 No constraint UB - matrix: -0.034881 -0.007479 0.076898 ( 0.000011 0.000012 0.000013 ) -0.008063 -0.083482 -0.011868 ( 0.000008 0.000009 0.000009 ) 0.076808 -0.012138 0.033648 ( 0.000010 0.000011 0.000012 ) M - matrix: 0.007181 0.000002 -0.000002 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007173 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007186 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.034881 -0.007479 0.076898 ( 0.000011 0.000012 0.000013 ) -0.008063 -0.083482 -0.011868 ( 0.000008 0.000009 0.000009 ) 0.076808 -0.012138 0.033648 ( 0.000010 0.000011 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3702(10) 8.3752(9) 8.3671(12) 90.058(10) 89.983(11) 90.014(9) V = 586.54(13) unit cell: 8.3708(3) 8.3708(3) 8.3708(3) 90.0 90.0 90.0 V = 586.54(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=486.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=827 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 16 86 150 260 284 472 806 1090 1212 Percent 0.0 0.0 1.3 7.1 12.4 21.5 23.4 38.9 66.5 89.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 606 100.00 (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 606 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1738382 60 2561482.50 138.32 100.00 1703940- 1100203 60 1391808.96 110.75 100.00 1089803- 365258 60 639111.63 95.91 100.00 363943- 230390 60 270143.89 68.07 100.00 230127- 172385 60 201921.11 51.11 100.00 171706- 145419 60 159740.63 36.01 100.00 144792- 106108 60 123572.83 30.36 100.00 105652- 6841 60 61785.11 21.77 100.00 6629- 4104 60 5057.78 5.14 83.33 4036- 1484 66 3205.90 3.51 50.00 ------------------------------------------------------------------------------------ 4887974- 1484 606 536450.59 55.57 92.90 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 60 871855.08 80.88 100.00 1.32- 1.09 60 925225.64 77.00 100.00 1.09- 0.96 60 595561.50 71.04 100.00 0.96- 0.85 60 694642.44 72.69 96.67 0.84- 0.80 60 560053.68 62.59 98.33 0.80- 0.73 60 360827.23 42.29 93.33 0.73- 0.70 60 335551.00 39.13 93.33 0.70- 0.65 60 543519.74 53.33 95.00 0.65- 0.62 60 269503.88 30.87 75.00 0.62- 0.59 66 237646.12 28.60 78.79 ------------------------------------------------------------------------------------ 4.82- 0.59 606 536450.59 55.57 92.90 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:36:44 2018 Sorting 606 observations 77 unique observations with > 7.00 F2/sig(F2) 606 observations in 1 runs Run # start # end # total # 1 1 107 107 Total number of frames 107 Maximum number of 77 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 606 observations in 1 runs Run # start # end # total # 1 0 53 54 Total number of frames 54 489 observations > 7.00 F2/sig(F2) 489 observations in 1 runs Run # start # end # total # 1 0 53 54 Total number of frames 54 Removing 'redundancy=1' reflections Average redundancy: 6.2 (Out of 489 removed 8 = 481, unique = 78) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 481 observations in 1 runs Run # start # end # total # 1 0 53 54 Total number of frames 54 78 unique data precomputed (should be 78) 78 unique data with 481 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.2 (Out of 481 removed 0 = 481, unique = 78) 78 unique data precomputed (should be 78) 78 unique data with 481 observations RMS deviation of equivalent data = 0.14425 Rint = 0.11621 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11621, wR= 0.14875 Trying model 1 (ne=2, no=0)... Results: Rint= 0.04315, wR= 0.05559, Acormin=0.614, Acormax=1.122, Acor_av=0.809 F test: Probability=1.000, F= 7.164 Trying model 2 (ne=2, no=1)... Results: Rint= 0.03548, wR= 0.04597, Acormin=0.553, Acormax=1.223, Acor_av=0.824 F test: Probability=1.000, F= 1.468 Trying model 3 (ne=4, no=0)... Results: Rint= 0.02896, wR= 0.03707, Acormin=0.637, Acormax=1.153, Acor_av=0.844 F test: Probability=1.000, F= 1.478 Trying model 4 (ne=4, no=1)... Results: Rint= 0.02819, wR= 0.03604, Acormin=0.589, Acormax=1.129, Acor_av=0.848 F test: Probability=0.676, F= 1.048 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02055, wR= 0.02730, Acormin=0.681, Acormax=1.240, Acor_av=0.884 F test: Probability=1.000, F= 1.935 Trying model 6 (ne=6, no=0)... Results: Rint= 0.02048, wR= 0.02746, Acormin=0.698, Acormax=1.284, Acor_av=0.895 F test: Probability=0.000, F= 0.999 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01982, wR= 0.02655, Acormin=0.692, Acormax=1.294, Acor_av=0.901 F test: Probability=0.708, F= 1.058 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01532, wR= 0.02130, Acormin=0.718, Acormax=1.360, Acor_av=0.925 F test: Probability=1.000, F= 1.737 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01462, wR= 0.01991, Acormin=0.730, Acormax=1.629, Acor_av=0.931 F test: Probability=0.728, F= 1.066 Final absorption model (ne=6, no=3): Rint= 0.01532, Acormin=0.718, Acormax=1.360, Acor_av=0.925 Combined refinement in use Rint: 0.11633 There are 54 active scales (one needs to be fixed) Refinement control: frame scale #31 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= 0.14425 Using Levenberg-Marquardt: 0.00010 New wR= 0.01876 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11621 with corrections 0.01218 Rint for all data: 0.11633 with corrections 0.01241 0 observations identified as outliers and rejected Cycle 2 wR= 0.01876 Using Levenberg-Marquardt: 0.00001 New wR= 0.01823 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11621 with corrections 0.01174 Rint for all data: 0.11633 with corrections 0.01198 0 observations identified as outliers and rejected Cycle 3 wR= 0.01823 Using Levenberg-Marquardt: 0.00000 New wR= 0.01822 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11621 with corrections 0.01172 Rint for all data: 0.11633 with corrections 0.01195 Final wR= 0.01822 Final frame scales: Min= 0.9610 Max= 1.0560 Final absorption correction factors: Amin= 0.6662 Amax= 1.2886 PROFFIT INFO: Inet (after scale3 abspack): min=1528.7201 max=4367454.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=285.0477 max=64135.1523 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:2/108 606 reflections read from tmp file 18 reflections are rejected (12 as outliers, 6 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 11 12 6 13 18 10 7 4 15 Initial Chi^2= 0.24673 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.95698 Current error model SIG(F2)^2 = 118.21*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 113.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 113.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4367455- 1685234 60 2515082.22 134.56 100.00 1679891- 1134966 60 1378576.34 68.38 100.00 1132742- 323402 60 646400.55 65.42 100.00 320763- 226151 60 261981.10 40.90 100.00 225071- 177750 60 204612.63 31.63 100.00 172732- 139626 60 151170.92 21.75 100.00 139383- 113006 60 125898.62 20.09 100.00 111887- 6649 60 62564.60 14.18 100.00 6585- 4033 60 4949.49 4.64 100.00 4018- 1529 66 3184.02 3.68 77.27 ------------------------------------------------------------------------------------ 4367455- 1529 606 530172.17 40.16 97.52 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 60 849628.46 81.50 100.00 1.32- 1.09 60 940695.88 69.42 100.00 1.09- 0.96 60 593590.59 45.99 100.00 0.96- 0.85 60 694999.18 45.20 98.33 0.84- 0.80 60 543277.19 38.95 100.00 0.80- 0.73 60 353475.61 26.72 100.00 0.73- 0.70 60 340609.70 24.77 98.33 0.70- 0.65 60 519565.14 33.18 98.33 0.65- 0.62 60 259249.78 19.72 86.67 0.62- 0.59 66 236043.05 18.31 93.94 ------------------------------------------------------------------------------------ 4.82- 0.59 606 530172.17 40.16 97.52 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 60 849628.46 81.50 100.00 4.82- 1.09 120 895162.17 75.46 100.00 4.82- 0.96 180 794638.31 65.64 100.00 4.82- 0.85 240 769728.53 60.53 99.58 4.82- 0.80 300 724438.26 56.21 99.67 4.82- 0.73 360 662611.15 51.30 99.72 4.82- 0.70 420 616610.94 47.51 99.52 4.82- 0.65 480 604480.22 45.72 99.38 4.82- 0.62 540 566121.28 42.83 97.96 4.82- 0.59 606 530172.17 40.16 97.52 ------------------------------------------------------------------------------------ 4.82- 0.59 606 530172.17 40.16 97.52 Scale applied to data: s=0.228966 (maximum obs:4367454.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.012; Rsigma 0.016: data 606 -> merged 102 With outlier rejection... Rint 0.011; Rsigma 0.016: data 599 -> merged 102 Rejected total: 7, method kkm 7, method Blessing 0 Completeness direct cell (a, b, c) = (8.371, 8.371, 8.371), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.587515, 4.832882 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 3.25 80.00 26 1.61 - 1.21 10 10 5.10 100.00 51 1.17 - 1.02 10 10 7.10 100.00 71 0.99 - 0.89 10 10 7.10 100.00 71 0.88 - 0.81 10 10 7.00 100.00 70 0.81 - 0.74 10 10 6.10 100.00 61 0.73 - 0.71 10 10 6.40 100.00 64 0.70 - 0.66 10 10 5.70 100.00 57 0.66 - 0.64 10 10 4.90 100.00 49 0.63 - 0.60 10 10 5.20 100.00 52 --------------------------------------------------------------- 5.92 - 0.60 98 100 5.84 98.00 572 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:36:44 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916409 5.919681 5.918314 60.0348 89.9755 59.9783 496 Reflections read from file xs1715a.hkl; mean (I/sigma) = 12.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 228 271 235 252 367 336 335 496 N (int>3sigma) = 0 170 271 177 188 309 260 259 384 Mean intensity = 0.0 49.5 28.3 48.1 59.4 41.3 61.7 63.9 62.2 Mean int/sigma = 0.0 10.7 11.0 10.9 11.9 10.8 12.2 12.8 12.7 Lattice type: P chosen Volume: 146.63 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.916 5.916 5.918 90.02 119.96 119.96 Niggli form: a.a = 35.000 b.b = 35.004 c.c = 35.026 b.c = -0.015 a.c = -17.484 a.b = -17.481 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.063 CUBIC F-lattice R(int) = 0.286 [ 353] Vol = 586.5 Cell: 8.370 8.375 8.367 90.06 89.98 90.01 Volume: 586.51 Matrix: 1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.061 RHOMBOHEDRAL R-lattice R(int) = 0.244 [ 184] Vol = 439.9 Cell: 5.920 5.916 14.506 90.00 90.04 120.02 Volume: 439.89 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.061 RHOMBOHEDRAL R-lattice R(int) = 0.304 [ 42] Vol = 439.9 Trigonal Cell: 5.920 5.916 14.506 90.00 90.04 120.02 Volume: 439.89 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.030 TETRAGONAL I-lattice R(int) = 0.242 [ 207] Vol = 293.3 Cell: 5.921 5.920 8.367 89.97 89.95 89.97 Volume: 293.26 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.080 TETRAGONAL I-lattice R(int) = 0.242 [ 207] Vol = 293.3 Cell: 5.920 5.921 8.367 90.05 90.03 89.97 Volume: 293.26 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.038 ORTHORHOMBIC I-lattice R(int) = 0.217 [ 276] Vol = 293.3 Cell: 5.920 5.921 8.367 89.95 89.97 89.97 Volume: 293.26 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.034 ORTHORHOMBIC I-lattice R(int) = 0.323 [ 144] Vol = 293.3 Cell: 5.916 8.370 5.922 89.98 89.94 90.00 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.021 MONOCLINIC I-lattice R(int) = 0.197 [ 167] Vol = 293.3 Cell: 5.921 5.920 8.367 90.03 90.05 89.97 Volume: 293.26 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.062 MONOCLINIC I-lattice R(int) = 0.252 [ 61] Vol = 293.3 Cell: 5.916 5.922 8.370 90.02 90.00 90.06 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.023 MONOCLINIC I-lattice R(int) = 0.359 [ 36] Vol = 293.3 Cell: 5.916 8.370 5.922 89.98 90.06 90.00 Volume: 293.26 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.025 MONOCLINIC I-lattice R(int) = 0.319 [ 79] Vol = 293.3 Cell: 5.922 5.916 8.370 90.00 90.02 89.94 Volume: 293.26 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.045 MONOCLINIC C-lattice R(int) = 0.187 [ 47] Vol = 293.3 Cell: 10.251 5.916 5.918 90.02 125.21 89.96 Volume: 293.26 Matrix:-1.0000 2.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.045 [ 3] Vol = 146.6 Cell: 5.916 5.916 5.918 90.02 119.96 119.96 Volume: 146.63 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 271 0 332 332 496 N (int>3sigma) = 0 0 0 0 271 0 256 254 384 Mean intensity = 0.0 0.0 0.0 0.0 28.3 0.0 61.3 59.1 62.2 Mean int/sigma = 0.0 0.0 0.0 0.0 11.0 0.0 12.3 12.5 12.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.068 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 4 4 36 117 N I>3s 2 2 4 117 0.7 0.7 0.6 32.5 3.8 3.8 2.0 12.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.286 335 Fd-3m 1 1 227 C N N N N 37 2284 0.291 370 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370202 8.375141 8.366624 90.0581 89.9816 90.0134 ZERR 1.00 0.000521 0.004890 0.003077 0.0016 0.0013 0.0193 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4304976- 1010850 132 127 25 5.1 1830399.43 92.62 0.008 0.009 984008- 181552 169 169 25 6.8 319813.69 45.37 0.017 0.019 165100- 94680 150 150 25 6.0 129985.60 19.80 0.024 0.030 61620- 2116 155 153 27 5.7 7793.77 5.57 0.097 0.110 ------------------------------------------------------------------------------------------- 4304976- 2116 606 599 102 5.9 512853.97 38.82 0.011 0.012 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 139 134 25 5.4 789391.07 67.66 0.010 0.010 0.010 1.02-0.81 166 165 25 6.6 597399.61 41.24 0.010 0.011 0.015 0.78-0.67 159 159 25 6.4 427004.32 29.32 0.012 0.012 0.021 0.67-0.59 142 141 27 5.2 247918.45 19.29 0.018 0.019 0.030 ------------------------------------------------------------------------------------------------------ inf-0.59 606 599 102 5.9 512853.97 38.82 0.011 0.012 0.016 inf-0.60 577 570 97 5.9 530454.86 39.99 0.011 0.012 0.016 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 134 27 25 92.6 5.4 789391.07 171.17 0.010 0.004 1.02-0.81 165 25 25 100.0 6.6 597399.61 110.14 0.010 0.006 0.78-0.67 159 25 25 100.0 6.4 427004.32 78.91 0.012 0.009 0.67-0.59 141 31 27 87.1 5.2 247918.45 45.62 0.018 0.014 -------------------------------------------------------------------------------------------- inf-0.59 599 108 102 94.4 5.9 512853.97 100.32 0.011 0.007 inf-0.60 570 99 97 98.0 5.9 530454.86 103.52 0.011 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:41:39 2018) ID: 2932; threads 39; handles 878; mem 518348.00 (1237724.00)kB; time: 1w 5d 21h 47m 9s MEMORY INFO: Memory PF:1.0, Ph:171.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.2,peak PF: 708.5, WS: 270.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:3.0, Ph:171.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 708.5, WS: 272.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:41:39 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000026 0.000026 0.000025 ) 0.087412 -0.166882 0.063604 ( 0.000018 0.000018 0.000017 ) 0.055227 -0.024260 0.122680 ( 0.000022 0.000022 0.000021 ) 5.91535 ( 0.00134 ) 5.92288 ( 0.00092 ) 5.91286 ( 0.00120 ) 59.95509 ( 0.01868 ) 89.89521 ( 0.01748 ) 59.99590 ( 0.01978 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 31 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 12:41:39 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000026 0.000026 0.000025 ) 0.087412 -0.166882 0.063604 ( 0.000018 0.000018 0.000017 ) 0.055227 -0.024260 0.122680 ( 0.000022 0.000022 0.000021 ) M - matrix: 0.021557 -0.014356 0.007163 ( 0.000007 0.000005 0.000005 ) -0.014356 0.028690 -0.014327 ( 0.000005 0.000006 0.000004 ) 0.007163 -0.014327 0.021518 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9154(13) 5.9229(9) 5.9129(12) 59.955(19) 89.895(17) 60.00(2) V = 146.51(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb PROFFITPEAK info: 323 peaks in the peak location table UB fit with 134 obs out of 146 (total:146,skipped:0) (91.78%) UB - matrix: -0.104134 -0.015063 0.050186 ( 0.000083 0.000161 0.000162 ) 0.087378 -0.166830 0.063677 ( 0.000084 0.000163 0.000164 ) 0.055301 -0.024020 0.122007 ( 0.000110 0.000214 0.000216 ) M - matrix: 0.021537 -0.014337 0.007085 ( 0.000026 0.000029 0.000029 ) -0.014337 0.028636 -0.014310 ( 0.000029 0.000055 0.000041 ) 0.007085 -0.014310 0.021459 ( 0.000029 0.000041 0.000059 ) unit cell: 5.919(6) 5.935(8) 5.930(11) 59.87(16) 89.68(11) 59.86(12) V = 147.1(4) UB fit with 134 obs out of 146 (total:146,skipped:0) (91.78%) UB - matrix: -0.104134 -0.015063 0.050186 ( 0.000083 0.000161 0.000162 ) 0.087378 -0.166830 0.063677 ( 0.000084 0.000163 0.000164 ) 0.055301 -0.024020 0.122007 ( 0.000110 0.000214 0.000216 ) M - matrix: 0.021537 -0.014337 0.007085 ( 0.000026 0.000029 0.000029 ) -0.014337 0.028636 -0.014310 ( 0.000029 0.000055 0.000041 ) 0.007085 -0.014310 0.021459 ( 0.000029 0.000041 0.000059 ) unit cell: 5.919(6) 5.935(8) 5.930(11) 59.87(16) 89.68(11) 59.86(12) V = 147.1(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.103993 -0.014840 0.050159 ( 0.000088 0.000173 0.000172 ) 0.087314 -0.166874 0.063792 ( 0.000094 0.000184 0.000183 ) 0.055036 -0.023901 0.121626 ( 0.000116 0.000227 0.000226 ) M - matrix: 0.021467 -0.014343 0.007047 ( 0.000028 0.000032 0.000031 ) -0.014343 0.028638 -0.014297 ( 0.000032 0.000063 0.000044 ) 0.007047 -0.014297 0.021378 ( 0.000031 0.000044 0.000062 ) UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) unit cell: 5.935(7) 5.945(8) 5.944(11) 59.80(17) 89.55(12) 59.74(13) V = 147.9(4) UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) UB - matrix: -0.103993 -0.014840 0.050160 ( 0.000088 0.000173 0.000172 ) 0.087314 -0.166874 0.063792 ( 0.000094 0.000184 0.000183 ) 0.055036 -0.023900 0.121627 ( 0.000116 0.000227 0.000226 ) M - matrix: 0.021467 -0.014343 0.007048 ( 0.000028 0.000032 0.000031 ) -0.014343 0.028638 -0.014297 ( 0.000032 0.000063 0.000044 ) 0.007048 -0.014297 0.021379 ( 0.000031 0.000044 0.000062 ) unit cell: 5.935(7) 5.945(8) 5.944(11) 59.80(17) 89.55(12) 59.74(13) V = 147.9(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.103992 -0.014842 0.050155 ( 0.000088 0.000172 0.000171 ) 0.087315 -0.166875 0.063786 ( 0.000094 0.000185 0.000183 ) 0.055037 -0.023906 0.121619 ( 0.000116 0.000228 0.000226 ) M - matrix: 0.021467 -0.014343 0.007047 ( 0.000028 0.000032 0.000031 ) -0.014343 0.028639 -0.014296 ( 0.000032 0.000063 0.000044 ) 0.007047 -0.014296 0.021375 ( 0.000031 0.000044 0.000062 ) UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) unit cell: 5.935(7) 5.945(8) 5.944(11) 59.80(17) 89.55(12) 59.74(13) V = 147.9(4) 146 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Run 2 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) HKL list info: 276 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103992 -0.014841 0.050158 ( 0.000088 0.000173 0.000172 ) 0.087315 -0.166874 0.063790 ( 0.000094 0.000184 0.000183 ) 0.055037 -0.023902 0.121626 ( 0.000116 0.000227 0.000226 ) M - matrix: 0.021467 -0.014343 0.007048 ( 0.000028 0.000032 0.000031 ) -0.014343 0.028638 -0.014296 ( 0.000032 0.000063 0.000044 ) 0.007048 -0.014296 0.021378 ( 0.000031 0.000044 0.000062 ) UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) unit cell: 5.935(7) 5.945(8) 5.944(11) 59.80(17) 89.55(12) 59.74(13) V = 147.9(4) 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb 0 of 93 peaks identified as outliers and rejected 93 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 93 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 93 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.00- 1.61 | 9 | 0.949 ( 0.133) | 1.050 ( 0.255) | 1.403 ( 1.091) | 1.60- 1.17 | 9 | 1.081 ( 0.119) | 1.104 ( 0.144) | 1.060 ( 0.160) | 1.16- 0.99 | 9 | 1.136 ( 0.108) | 1.127 ( 0.134) | 1.058 ( 0.306) | 0.99- 0.89 | 9 | 1.137 ( 0.082) | 1.109 ( 0.094) | 1.416 ( 0.437) | 0.88- 0.82 | 9 | 1.196 ( 0.072) | 1.167 ( 0.116) | 1.087 ( 0.283) | 0.82- 0.76 | 9 | 1.249 ( 0.041) | 1.203 ( 0.088) | 1.141 ( 0.388) | 0.76- 0.71 | 9 | 1.230 ( 0.054) | 1.234 ( 0.147) | 1.229 ( 0.323) | 0.71- 0.67 | 9 | 1.235 ( 0.035) | 1.245 ( 0.155) | 1.152 ( 0.446) | 0.66- 0.64 | 9 | 1.260 ( 0.025) | 1.230 ( 0.092) | 1.126 ( 0.353) | 0.63- 0.59 | 12 | 1.290 ( 0.061) | 1.418 ( 0.251) | 1.100 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.00- 0.59 | 93 | 1.180 ( 0.127) | 1.196 ( 0.193) | 1.175 ( 0.503) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) UB - matrix: -0.103904 -0.015285 0.049369 ( 0.000043 0.000090 0.000088 ) 0.087414 -0.167162 0.064002 ( 0.000032 0.000067 0.000066 ) 0.055056 -0.023877 0.122236 ( 0.000042 0.000088 0.000087 ) M - matrix: 0.021468 -0.014339 0.007195 ( 0.000012 0.000013 0.000013 ) -0.014339 0.028747 -0.014372 ( 0.000013 0.000023 0.000017 ) 0.007195 -0.014372 0.021475 ( 0.000013 0.000017 0.000024 ) unit cell: 5.928(3) 5.917(3) 5.934(4) 59.97(7) 90.11(5) 60.08(6) V = 147.15(15) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB - matrix: -0.104138 -0.015086 0.049850 ( 0.000026 0.000055 0.000054 ) 0.087389 -0.167126 0.063672 ( 0.000027 0.000056 0.000055 ) 0.055300 -0.023978 0.122238 ( 0.000040 0.000083 0.000082 ) M - matrix: 0.021540 -0.014360 0.007133 ( 0.000008 0.000010 0.000010 ) -0.014360 0.028734 -0.014324 ( 0.000010 0.000019 0.000015 ) 0.007133 -0.014324 0.021481 ( 0.000010 0.000015 0.000022 ) UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) unit cell: 5.918(2) 5.917(3) 5.923(4) 60.00(6) 89.90(4) 59.95(4) V = 146.69(13) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb 0 of 93 peaks identified as outliers and rejected 93 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 93 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 93 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.03- 1.61 | 9 | 0.920 ( 0.124) | 1.009 ( 0.271) | 1.443 ( 1.070) | 1.60- 1.17 | 9 | 1.112 ( 0.078) | 1.144 ( 0.068) | 1.120 ( 0.261) | 1.16- 0.98 | 9 | 1.122 ( 0.104) | 1.136 ( 0.133) | 0.975 ( 0.099) | 0.98- 0.88 | 9 | 1.153 ( 0.082) | 1.123 ( 0.109) | 1.413 ( 0.490) | 0.88- 0.82 | 9 | 1.172 ( 0.082) | 1.129 ( 0.109) | 1.133 ( 0.333) | 0.82- 0.76 | 9 | 1.235 ( 0.050) | 1.205 ( 0.091) | 1.175 ( 0.357) | 0.76- 0.71 | 9 | 1.230 ( 0.053) | 1.217 ( 0.150) | 1.198 ( 0.363) | 0.71- 0.67 | 9 | 1.242 ( 0.035) | 1.229 ( 0.159) | 1.242 ( 0.423) | 0.66- 0.64 | 9 | 1.259 ( 0.026) | 1.228 ( 0.092) | 1.128 ( 0.354) | 0.63- 0.59 | 12 | 1.287 ( 0.060) | 1.429 ( 0.246) | 1.092 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.03- 0.59 | 93 | 1.177 ( 0.126) | 1.193 ( 0.194) | 1.189 ( 0.503) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 54 | 1.143 ( 0.051) | 1.241 ( 0.176) | 1.327 ( 0.597) | 13.1-19.4 | 54 | 1.148 ( 0.129) | 1.242 ( 0.388) | 1.411 ( 0.844) | 19.4-23.7 | 54 | 1.176 ( 0.089) | 1.285 ( 0.363) | 1.317 ( 0.609) | 23.8-27.6 | 54 | 1.130 ( 0.092) | 1.156 ( 0.103) | 1.242 ( 0.465) | 27.9-30.8 | 54 | 1.129 ( 0.108) | 1.201 ( 0.236) | 1.154 ( 0.388) | 30.8-34.0 | 54 | 1.142 ( 0.076) | 1.196 ( 0.275) | 1.167 ( 0.401) | 34.3-37.4 | 54 | 1.150 ( 0.087) | 1.151 ( 0.171) | 1.205 ( 0.402) | 37.4-39.7 | 54 | 1.139 ( 0.127) | 1.126 ( 0.228) | 1.202 ( 0.594) | 39.7-43.0 | 54 | 1.141 ( 0.124) | 1.135 ( 0.224) | 1.275 ( 0.706) | 43.1-49.8 | 56 | 1.216 ( 0.145) | 1.195 ( 0.287) | 1.226 ( 0.487) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 542 | 1.152 ( 0.110) | 1.193 ( 0.264) | 1.253 ( 0.572) | Fitted profile normalization line parameters e1 dimension: a=0.0015 b=0.98 e2 dimension: a=-0.0008 b=1.02 e3 dimension: a=-0.0037 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 3679 lp-corr: 2195 Maximum peak integral for reflections I/sig<= 100 - raw: 427004 lp-corr: 681858 Maximum peak integral for reflections I/sig<= 10000 - raw: 4883952 lp-corr: 1873353 PROFFITPEAK - Finished at Wed Mar 28 12:41:41 2018 PROFFITMAIN - Started at Wed Mar 28 12:41:41 2018 OTKP changes: 542 1 1 2 OTKP changes: 542 1 1 2 OTKP changes: 542 1 1 2 OTKP changes: 542 1 1 2 UB - matrix: -0.104229 -0.015017 0.049513 ( 0.000021 0.000023 0.000022 ) 0.087313 -0.167009 0.063622 ( 0.000014 0.000016 0.000015 ) 0.055344 -0.024249 0.122565 ( 0.000020 0.000022 0.000022 ) M - matrix: 0.021550 -0.014359 0.007178 ( 0.000005 0.000004 0.000004 ) -0.014359 0.028705 -0.014341 ( 0.000004 0.000005 0.000004 ) 0.007178 -0.014341 0.021521 ( 0.000004 0.000004 0.000006 ) UB fit with 542 obs out of 542 (total:542,skipped:0) (100.00%) unit cell: 5.9175(11) 5.9186(8) 5.9197(12) 60.030(18) 90.016(16) 60.001(17) V = 146.65(4) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) UB - matrix: -0.104067 -0.015177 0.049693 ( 0.000028 0.000060 0.000058 ) 0.087417 -0.167151 0.063718 ( 0.000027 0.000058 0.000055 ) 0.055287 -0.023964 0.122309 ( 0.000041 0.000086 0.000083 ) M - matrix: 0.021528 -0.014357 0.007161 ( 0.000009 0.000010 0.000010 ) -0.014357 0.028744 -0.014336 ( 0.000010 0.000020 0.000015 ) 0.007161 -0.014336 0.021489 ( 0.000010 0.000015 0.000022 ) unit cell: 5.920(2) 5.914(3) 5.923(4) 60.03(6) 90.00(4) 60.00(4) V = 146.70(13) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB - matrix: -0.104146 -0.015108 0.049821 ( 0.000027 0.000057 0.000055 ) 0.087394 -0.167144 0.063679 ( 0.000027 0.000058 0.000056 ) 0.055316 -0.023949 0.122311 ( 0.000040 0.000086 0.000082 ) M - matrix: 0.021544 -0.014359 0.007142 ( 0.000009 0.000010 0.000010 ) -0.014359 0.028739 -0.014326 ( 0.000010 0.000020 0.000015 ) 0.007142 -0.014326 0.021497 ( 0.000010 0.000015 0.000022 ) UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) unit cell: 5.917(2) 5.914(3) 5.920(4) 60.03(6) 89.94(4) 59.97(4) V = 146.56(13) Run 2 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) HKL list info: 268 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104146 -0.015108 0.049821 ( 0.000027 0.000057 0.000055 ) 0.087394 -0.167144 0.063679 ( 0.000027 0.000058 0.000056 ) 0.055316 -0.023949 0.122311 ( 0.000040 0.000086 0.000082 ) M - matrix: 0.021544 -0.014359 0.007142 ( 0.000009 0.000010 0.000010 ) -0.014359 0.028739 -0.014326 ( 0.000010 0.000020 0.000015 ) 0.007142 -0.014326 0.021497 ( 0.000010 0.000015 0.000022 ) UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) unit cell: 5.917(2) 5.914(3) 5.920(4) 60.03(6) 89.94(4) 59.97(4) V = 146.56(13) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104281 -0.014991 0.049534 ( 0.000021 0.000023 0.000022 ) 0.087304 -0.166988 0.063575 ( 0.000015 0.000016 0.000016 ) 0.055367 -0.024264 0.122527 ( 0.000020 0.000022 0.000022 ) M - matrix: 0.021562 -0.014359 0.007169 ( 0.000006 0.000004 0.000004 ) -0.014359 0.028698 -0.014332 ( 0.000004 0.000005 0.000004 ) 0.007169 -0.014332 0.021508 ( 0.000004 0.000004 0.000006 ) UB fit with 542 obs out of 542 (total:542,skipped:0) (100.00%) unit cell: 5.9154(11) 5.9191(8) 5.9209(12) 60.026(18) 89.992(16) 59.994(17) V = 146.65(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 7 reflections under beam stop or inside a detector rejection region 1 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof 736 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:41:42 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=486.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=827 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 9 51 89 155 171 282 484 657 736 Percent 0.0 0.0 1.2 6.9 12.1 21.1 23.2 38.3 65.8 89.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 736 100.00 (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 736 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1770048 73 2551028.22 137.85 100.00 1738382- 1156475 73 1432193.45 113.23 100.00 1151211- 354106 73 664965.32 96.42 100.00 349356- 234113 73 275139.94 73.52 100.00 232815- 177442 73 208894.37 53.50 100.00 175601- 149289 73 163145.47 38.33 100.00 148819- 108047 73 128036.96 30.49 100.00 107715- 6968 73 65116.03 22.12 100.00 6956- 4139 73 5221.08 5.10 84.93 4110- 1484 79 3243.51 3.51 49.37 ------------------------------------------------------------------------------------ 4887974- 1484 736 545243.64 56.97 93.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 73 705985.94 92.92 100.00 1.28- 0.98 73 900523.36 76.64 97.26 0.98- 0.82 73 601973.48 58.36 98.63 0.82- 0.72 73 700699.68 70.20 97.26 0.72- 0.65 73 526600.75 58.68 95.89 0.65- 0.60 73 486962.47 50.54 93.15 0.60- 0.56 73 464673.39 49.14 98.63 0.56- 0.52 73 428767.98 44.35 82.19 0.52- 0.48 73 358920.83 37.42 83.56 0.48- 0.40 79 297676.50 33.37 84.81 ------------------------------------------------------------------------------------ 5.26- 0.40 736 545243.64 56.97 93.07 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:41:42 2018 Sorting 736 observations 194 unique observations with > 7.00 F2/sig(F2) 736 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 24 131 Total number of frames 131 Maximum number of 194 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 736 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 24 131 Total number of frames 131 Frame #8 of 131 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 595 observations > 7.00 F2/sig(F2) 595 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 24 131 Total number of frames 131 Frame #8 of 131 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: 2.8 (Out of 595 removed 92 = 503, unique = 179) 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 503 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 24 131 Total number of frames 131 Frame #8 of 131 skipped from refinement Frame #119 of 131 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 179 unique data precomputed (should be 179) 179 unique data with 503 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.8 (Out of 503 removed 0 = 503, unique = 179) 179 unique data precomputed (should be 179) 179 unique data with 503 observations RMS deviation of equivalent data = 0.66845 Rint = 0.61935 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.59831, wR= 3.16217 Trying model 1 (ne=2, no=0)... Results: Rint= 0.86886, wR= 2.79198, Acormin=-0.264, Acormax=1.857, Acor_av=0.205 F test: Probability=0.000, F= 0.467 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84046, wR= 3.17020, Acormin=-0.757, Acormax=1.212, Acor_av=0.034 F test: Probability=0.000, F= 0.494 Trying model 3 (ne=4, no=0)... Results: Rint= 0.92853, wR= 1.76948, Acormin=-0.275, Acormax=1.960, Acor_av=0.067 F test: Probability=0.000, F= 0.397 Trying model 4 (ne=4, no=1)... Results: Rint= 0.82262, wR= 1.90427, Acormin=-0.463, Acormax=1.332, Acor_av=0.020 F test: Probability=0.000, F= 0.501 Trying model 5 (ne=4, no=3)... Results: Rint= 0.80475, wR= 2.84591, Acormin=-0.241, Acormax=0.720, Acor_av=0.017 F test: Probability=0.000, F= 0.512 Trying model 6 (ne=6, no=0)... Results: Rint= 0.87611, wR= 1.51222, Acormin=-0.199, Acormax=0.928, Acor_av=0.019 F test: Probability=0.000, F= 0.427 Trying model 7 (ne=6, no=1)... Results: Rint= 0.85540, wR= 1.39952, Acormin=-0.188, Acormax=0.907, Acor_av=0.011 F test: Probability=0.000, F= 0.444 Trying model 8 (ne=6, no=3)... Results: Rint= 0.86042, wR= 1.48749, Acormin=-0.201, Acormax=0.632, Acor_av=0.004 F test: Probability=0.000, F= 0.428 Trying model 9 (ne=6, no=5)... Results: Rint= 0.89271, wR= 2.55424, Acormin=-0.087, Acormax=0.180, Acor_av=0.002 F test: Probability=0.000, F= 0.382 Trying model 10 (ne=8, no=0)... Results: Rint= 0.85006, wR= 1.89746, Acormin=-0.131, Acormax=0.380, Acor_av=0.009 F test: Probability=0.000, F= 0.428 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87628, wR= 1.73190, Acormin=-0.119, Acormax=0.372, Acor_av=0.007 F test: Probability=0.000, F= 0.398 Trying model 12 (ne=8, no=3)... Results: Rint= 0.83655, wR= 1.56292, Acormin=-0.040, Acormax=0.018, Acor_av=0.001 F test: Probability=0.000, F= 0.426 Trying model 13 (ne=8, no=5)... Results: Rint= 0.86589, wR= 1.92415, Acormin=-0.040, Acormax=0.042, Acor_av=0.001 F test: Probability=0.000, F= 0.381 Trying model 14 (ne=8, no=7)... Results: Rint= 0.62456, wR= 1.30052, Acormin=-0.011, Acormax=0.069, Acor_av=0.002 F test: Probability=0.000, F= 0.690 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: 0.76991 There are 129 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 133 pars with 8911 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.66845 Using Levenberg-Marquardt: 0.00010 New wR= 0.62509 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.61935 with corrections 0.57719 Rint for all data: 0.76991 with corrections 0.73827 1 observations identified as outliers and rejected Cycle 2 wR= 0.62319 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= 0.60308 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60896 with corrections 0.57616 Rint for all data: 0.76991 with corrections 0.73937 1 observations identified as outliers and rejected Cycle 3 wR= 0.59992 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58385 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.58127 Rint for all data: 0.76991 with corrections 0.74831 0 observations identified as outliers and rejected Cycle 4 wR= 0.58385 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57575 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.59071 Rint for all data: 0.76991 with corrections 0.75768 0 observations identified as outliers and rejected Cycle 5 wR= 0.57575 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57353 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.60577 Rint for all data: 0.76991 with corrections 0.77210 0 observations identified as outliers and rejected Final wR= 0.57353 Final frame scales: Min= 0.8295 Max= 7.9085 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time with different frame scales initialization There are 129 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.84982 Using Levenberg-Marquardt: 0.00010 New wR= 0.62730 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.58813 Rint for all data: 0.76991 with corrections 0.76117 0 observations identified as outliers and rejected Cycle 2 wR= 0.62730 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= 0.60608 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.57990 Rint for all data: 0.76991 with corrections 0.75711 0 observations identified as outliers and rejected Cycle 3 wR= 0.60608 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59481 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.58429 Rint for all data: 0.76991 with corrections 0.76097 0 observations identified as outliers and rejected Cycle 4 wR= 0.59481 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59006 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.59596 Rint for all data: 0.76991 with corrections 0.77077 0 observations identified as outliers and rejected Cycle 5 wR= 0.59006 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58896 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59831 with corrections 0.61021 Rint for all data: 0.76991 with corrections 0.78421 0 observations identified as outliers and rejected Final wR= 0.58896 Final frame scales: Min= 1.0000 Max= 16.4502 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 89 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 88 pars with 3916 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.85279 Using Levenberg-Marquardt: 0.00010 New wR= 0.69573 There are 12 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59831 with corrections 0.60117 Rint for all data: 0.76991 with corrections 0.77225 1 observations identified as outliers and rejected Cycle 2 wR= 0.63649 Using Levenberg-Marquardt: 0.00001 New wR= 0.58835 There are 12 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.62808 Rint for all data: 0.76991 with corrections 0.80096 0 observations identified as outliers and rejected Cycle 3 wR= 0.63223 Using Levenberg-Marquardt: 0.00000 New wR= 0.62899 There are 12 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.60919 Rint for all data: 0.76991 with corrections 0.78365 0 observations identified as outliers and rejected Cycle 4 wR= 0.62780 Using Levenberg-Marquardt: 0.00000 New wR= 0.61627 There are 12 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.85185 Rint for all data: 0.76991 with corrections 0.97894 0 observations identified as outliers and rejected Cycle 5 wR= 0.65095 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.65542 Using Levenberg-Marquardt: 100.00000 New wR= 0.65086 There are 12 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.87688 Rint for all data: 0.76991 with corrections 0.99949 Final wR= 0.65086 Frame scales out of range! Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 86 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 85 pars with 3655 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.88207 Using Levenberg-Marquardt: 0.00010 New wR= 0.65038 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.58553 Rint for all data: 0.76991 with corrections 0.76865 0 observations identified as outliers and rejected Cycle 2 wR= 0.64256 Using Levenberg-Marquardt: 0.00001 New wR= 0.61688 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.59130 Rint for all data: 0.76991 with corrections 0.76622 0 observations identified as outliers and rejected Cycle 3 wR= 0.63275 Using Levenberg-Marquardt: 0.00000 New wR= 0.62407 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.60211 Rint for all data: 0.76991 with corrections 0.77529 0 observations identified as outliers and rejected Cycle 4 wR= 0.63379 Using Levenberg-Marquardt: 0.00000 New wR= 0.62626 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.62188 Rint for all data: 0.76991 with corrections 0.78471 0 observations identified as outliers and rejected Cycle 5 wR= 0.63291 Using Levenberg-Marquardt: 0.00000 New wR= 0.62848 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.62338 Rint for all data: 0.76991 with corrections 0.78631 0 observations identified as outliers and rejected Final wR= 0.62848 Final frame scales: Min= 0.1894 Max= 1.0134 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 85 active scales (one needs to be fixed) Refinement control: frame scale #100 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 84 pars with 3570 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.08694 Using Levenberg-Marquardt: 0.00010 New wR= 0.64883 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.58208 Rint for all data: 0.76991 with corrections 0.76411 0 observations identified as outliers and rejected Cycle 2 wR= 0.64257 Using Levenberg-Marquardt: 0.00001 New wR= 0.61781 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.58625 Rint for all data: 0.76991 with corrections 0.76347 0 observations identified as outliers and rejected Cycle 3 wR= 0.63195 Using Levenberg-Marquardt: 0.00000 New wR= 0.62642 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.59390 Rint for all data: 0.76991 with corrections 0.76841 0 observations identified as outliers and rejected Cycle 4 wR= 0.63200 Using Levenberg-Marquardt: 0.00000 New wR= 0.62603 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.59961 Rint for all data: 0.76991 with corrections 0.76978 0 observations identified as outliers and rejected Cycle 5 wR= 0.63080 Using Levenberg-Marquardt: 0.00000 New wR= 0.62822 There are 13 clusters with unrefined scales (size 1-9) Rint for refined data: 0.59061 with corrections 0.60278 Rint for all data: 0.76991 with corrections 0.77172 0 observations identified as outliers and rejected Final wR= 0.62822 Final frame scales: Min= 0.2987 Max= 1.0795 PROFFIT INFO: Inet (after scale3 abspack): min=807.7871 max=5402479.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=137.6380 max=79920.7266 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:2/108 736 reflections read from tmp file 634 reflections are rejected (496 as outliers, 138 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 45 4 Initial Chi^2= 1.64515 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.76538 Current error model SIG(F2)^2 = 518.51*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 396.86*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 396.86*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5402479- 1672522 73 2656661.92 65.20 100.00 1654748- 992206 73 1291655.36 41.30 100.00 991273- 358038 73 605058.93 32.59 100.00 355707- 240125 73 287933.19 23.57 100.00 237913- 180999 73 206381.63 18.72 100.00 180224- 138578 73 160135.11 13.74 100.00 137914- 92320 73 116499.14 11.16 100.00 91738- 8580 73 54208.94 8.05 84.93 8442- 3870 73 5407.95 2.56 21.92 3837- 808 79 2829.52 2.04 10.13 ------------------------------------------------------------------------------------ 5402479- 808 736 534308.84 21.73 81.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 73 634793.40 44.96 100.00 1.28- 0.98 73 927383.74 33.89 86.30 0.98- 0.82 73 642322.22 23.37 84.93 0.82- 0.72 73 645585.13 24.12 78.08 0.72- 0.65 73 531919.26 19.56 84.93 0.65- 0.60 73 498740.10 16.95 73.97 0.60- 0.56 73 422925.03 16.45 82.19 0.56- 0.52 73 427962.60 14.88 78.08 0.52- 0.48 73 365262.00 12.65 69.86 0.48- 0.40 79 268077.04 11.33 73.42 ------------------------------------------------------------------------------------ 5.26- 0.40 736 534308.84 21.73 81.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 73 634793.40 44.96 100.00 5.26- 0.98 146 781088.57 39.43 93.15 5.26- 0.82 219 734833.12 34.07 90.41 5.26- 0.72 292 712521.12 31.59 87.33 5.26- 0.65 365 676400.75 29.18 86.85 5.26- 0.60 438 646790.64 27.14 84.70 5.26- 0.56 511 614809.84 25.62 84.34 5.26- 0.52 584 591453.93 24.27 83.56 5.26- 0.48 657 566321.50 22.98 82.04 5.26- 0.40 736 534308.84 21.73 81.11 ------------------------------------------------------------------------------------ 5.26- 0.40 736 534308.84 21.73 81.11 Scale applied to data: s=0.185100 (maximum obs:5402479.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.772; Rsigma 0.030: data 736 -> merged 298 With outlier rejection... Rint 0.490; Rsigma 0.033: data 593 -> merged 298 Rejected total: 143, method kkm 141, method Blessing 2 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404452, 5.273412 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 2.47 100.00 37 1.46 - 1.12 15 15 2.73 100.00 41 1.08 - 0.96 15 15 2.40 100.00 36 0.96 - 0.86 15 15 3.00 100.00 45 0.86 - 0.79 15 15 2.20 100.00 33 0.79 - 0.73 13 15 2.31 86.67 30 0.73 - 0.69 15 15 1.80 100.00 27 0.69 - 0.65 14 15 2.57 93.33 36 0.65 - 0.63 12 15 1.67 80.00 20 0.63 - 0.60 21 21 1.95 100.00 41 --------------------------------------------------------------- 5.92 - 0.60 150 156 2.31 96.15 346 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:41:43 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915415 5.919113 5.920917 60.0259 89.9925 59.9940 593 Reflections read from file xs1715a.hkl; mean (I/sigma) = 19.80 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 272 324 282 296 439 406 394 593 N (int>3sigma) = 0 208 324 218 231 375 331 317 478 Mean intensity = 0.0 62.8 38.6 60.8 84.9 53.3 86.5 82.6 82.0 Mean int/sigma = 0.0 16.6 17.6 16.4 20.1 16.9 19.8 20.0 19.8 Lattice type: P chosen Volume: 146.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.915 5.917 5.921 60.02 60.05 60.03 Niggli form: a.a = 34.992 b.b = 35.008 c.c = 35.055 b.c = 17.503 a.c = 17.487 a.b = 17.482 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.067 CUBIC F-lattice R(int) = 0.219 [ 445] Vol = 586.6 Cell: 8.370 8.369 8.374 90.05 89.98 90.05 Volume: 586.59 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.068 RHOMBOHEDRAL R-lattice R(int) = 0.201 [ 253] Vol = 439.9 Cell: 5.919 5.922 14.491 90.06 89.98 120.00 Volume: 439.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.068 RHOMBOHEDRAL R-lattice R(int) = 0.175 [ 63] Vol = 439.9 Trigonal Cell: 5.919 5.922 14.491 90.06 89.98 120.00 Volume: 439.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.024 RHOMBOHEDRAL R-lattice R(int) = 0.207 [ 269] Vol = 439.9 Cell: 5.915 5.919 14.509 89.98 90.01 120.01 Volume: 439.94 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.024 RHOMBOHEDRAL R-lattice R(int) = 0.220 [ 68] Vol = 439.9 Trigonal Cell: 5.915 5.919 14.509 89.98 90.01 120.01 Volume: 439.94 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.203 [ 221] Vol = 293.3 Cell: 5.915 5.921 8.374 89.95 89.97 90.01 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.115 ORTHORHOMBIC I-lattice R(int) = 0.157 [ 310] Vol = 293.3 Cell: 5.921 8.369 5.919 90.00 89.97 90.08 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.021 MONOCLINIC I-lattice R(int) = 0.135 [ 184] Vol = 293.3 Cell: 5.921 5.919 8.369 90.00 90.08 90.03 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.051 MONOCLINIC I-lattice R(int) = 0.176 [ 129] Vol = 293.3 Cell: 5.915 5.921 8.374 90.05 90.03 90.01 Volume: 293.30 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.017 MONOCLINIC I-lattice R(int) = 0.175 [ 108] Vol = 293.3 Cell: 5.921 5.915 8.374 90.03 90.05 90.01 Volume: 293.30 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.077 MONOCLINIC I-lattice R(int) = 0.175 [ 108] Vol = 293.3 Cell: 8.374 5.915 5.921 90.01 90.05 90.03 Volume: 293.30 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 30] Vol = 146.6 Cell: 5.915 5.917 5.921 60.02 60.05 60.03 Volume: 146.65 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 324 0 397 398 593 N (int>3sigma) = 0 0 0 0 324 0 321 316 478 Mean intensity = 0.0 0.0 0.0 0.0 38.6 0.0 80.3 80.7 82.0 Mean int/sigma = 0.0 0.0 0.0 0.0 17.6 0.0 19.3 19.8 19.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.106 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 45 146 N I>3s 5 5 16 146 1.3 1.3 1.0 43.9 5.3 5.3 3.1 21.6 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 0.218 419 Fd-3m 1 1 227 C N N N N 37 2284 0.228 455 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370099 8.369004 8.373958 90.0542 89.9844 90.0533 ZERR 1.00 0.000476 0.002770 0.004498 0.0007 0.0176 0.0006 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4963163- 1205600 64 54 29 1.9 1920458.40 52.46 0.394 0.389 1190850- 916299 85 63 29 2.2 719417.71 25.85 0.546 0.440 862736- 645070 81 64 29 2.2 616533.78 24.11 0.656 0.562 635373- 461759 101 74 29 2.6 331524.62 17.36 0.709 0.685 457038- 261995 90 69 29 2.4 275624.85 25.74 0.411 0.439 256381- 177145 69 55 29 1.9 211781.38 16.08 0.281 0.296 176774- 131094 74 55 29 1.9 145708.62 12.24 0.206 0.198 130985- 95562 59 53 29 1.8 122306.91 10.47 0.405 0.380 94597- 56187 59 53 29 1.8 71992.23 7.24 0.669 0.651 54413- 1209 54 53 37 1.4 14658.92 3.38 0.793 0.774 ------------------------------------------------------------------------------------------- 4963163- 1209 736 593 298 2.0 443126.30 19.80 0.490 0.450 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 96 71 29 2.4 647536.82 42.90 0.361 0.362 0.016 1.12-0.87 104 83 29 2.9 623405.72 24.85 0.624 0.531 0.024 0.86-0.74 87 66 29 2.3 455430.07 19.92 0.486 0.406 0.031 0.73-0.65 86 67 31 2.2 388110.18 16.97 0.634 0.573 0.035 0.65-0.60 75 59 32 1.8 505640.10 17.68 0.388 0.394 0.037 0.60-0.56 68 52 29 1.8 264888.82 13.56 0.282 0.282 0.051 0.56-0.52 65 56 29 1.9 426199.91 14.49 0.621 0.605 0.041 0.52-0.49 63 53 29 1.8 295001.80 11.01 0.433 0.437 0.049 0.49-0.46 50 44 29 1.5 296482.89 12.09 0.360 0.360 0.051 0.46-0.40 42 42 32 1.3 305709.92 12.06 0.340 0.340 0.053 ------------------------------------------------------------------------------------------------------ inf-0.40 736 593 298 2.0 443126.30 19.80 0.490 0.450 0.033 inf-0.60 448 346 150 2.3 530671.45 24.86 0.504 0.452 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 71 29 29 100.0 2.4 647536.82 73.82 0.361 0.011 1.12-0.87 83 29 29 100.0 2.9 623405.72 51.10 0.624 0.017 0.86-0.74 66 31 29 93.5 2.3 455430.07 36.25 0.486 0.022 0.73-0.65 67 34 31 91.2 2.2 388110.18 29.57 0.634 0.028 0.65-0.60 59 33 32 97.0 1.8 505640.10 27.72 0.388 0.028 0.60-0.56 52 37 29 78.4 1.8 264888.82 18.59 0.282 0.039 0.56-0.52 56 34 29 85.3 1.9 426199.91 23.29 0.621 0.032 0.52-0.49 53 43 29 67.4 1.8 295001.80 15.51 0.433 0.043 0.49-0.46 44 55 29 52.7 1.5 296482.89 16.63 0.360 0.033 0.46-0.40 42 138 32 23.2 1.3 305709.92 14.74 0.340 0.048 -------------------------------------------------------------------------------------------- inf-0.40 593 464 298 64.2 2.0 443126.30 33.62 0.490 0.025 inf-0.60 346 156 150 96.2 2.3 530671.45 44.77 0.504 0.020 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.034868 0.076905 -0.007496 ( 0.000009 0.000010 0.000010 ) 0.008055 -0.011864 -0.083494 ( 0.000007 0.000007 0.000008 ) -0.076815 0.033579 -0.012132 ( 0.000010 0.000010 0.000011 ) M - matrix: 0.007181 0.000007 -0.000002 ( 0.000002 0.000001 0.000001 ) 0.000007 0.007183 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007175 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.034868 0.076905 -0.007496 ( 0.000009 0.000010 0.000010 ) 0.008055 -0.011864 -0.083494 ( 0.000007 0.000007 0.000008 ) -0.076815 0.033579 -0.012132 ( 0.000010 0.000010 0.000011 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3701(10) 8.3693(10) 8.3740(8) 90.053(9) 89.984(9) 90.052(9) V = 586.61(11) unit cell: 8.3711(3) 8.3711(3) 8.3711(3) 90.0 90.0 90.0 V = 586.61(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -82.000,25 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=486.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=827 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 18 102 178 310 342 564 968 1314 1472 Percent 0.0 0.0 1.2 6.9 12.1 21.1 23.2 38.3 65.8 89.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 736 100.00 (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 736 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1770048 73 2551028.22 137.85 100.00 1738382- 1156475 73 1432193.45 113.23 100.00 1151211- 354106 73 664965.32 96.42 100.00 349356- 234113 73 275139.94 73.52 100.00 232815- 177442 73 208894.37 53.50 100.00 175601- 149289 73 163145.47 38.33 100.00 148819- 108047 73 128036.96 30.49 100.00 107715- 6968 73 65116.03 22.12 100.00 6956- 4139 73 5221.08 5.10 84.93 4110- 1484 79 3243.51 3.51 49.37 ------------------------------------------------------------------------------------ 4887974- 1484 736 545243.64 56.97 93.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 73 803324.19 85.43 98.63 1.32- 1.09 73 950747.98 78.16 100.00 1.09- 0.96 73 608150.66 72.90 100.00 0.96- 0.85 73 707119.88 73.74 97.26 0.85- 0.80 73 585208.20 64.13 98.63 0.80- 0.73 73 399635.01 44.16 94.52 0.73- 0.70 73 299834.86 36.35 93.15 0.70- 0.65 73 570380.69 54.83 95.89 0.65- 0.62 73 302253.76 33.27 76.71 0.62- 0.58 79 250044.14 29.00 77.22 ------------------------------------------------------------------------------------ 4.82- 0.58 736 545243.64 56.97 93.07 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:41:44 2018 Sorting 736 observations 79 unique observations with > 7.00 F2/sig(F2) 736 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 24 131 Total number of frames 131 Maximum number of 79 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 736 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 12 67 Total number of frames 67 595 observations > 7.00 F2/sig(F2) 595 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 12 67 Total number of frames 67 Removing 'redundancy=1' reflections Average redundancy: 7.3 (Out of 595 removed 7 = 588, unique = 80) 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 588 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 12 67 Total number of frames 67 80 unique data precomputed (should be 80) 80 unique data with 588 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.3 (Out of 588 removed 0 = 588, unique = 80) 80 unique data precomputed (should be 80) 80 unique data with 588 observations RMS deviation of equivalent data = 0.14471 Rint = 0.10851 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10655, wR= 0.14688 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05026, wR= 0.06968, Acormin=0.622, Acormax=1.127, Acor_av=0.795 F test: Probability=1.000, F= 4.450 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04152, wR= 0.05642, Acormin=0.564, Acormax=1.214, Acor_av=0.842 F test: Probability=1.000, F= 1.457 Trying model 3 (ne=4, no=0)... Results: Rint= 0.03819, wR= 0.05524, Acormin=0.576, Acormax=1.083, Acor_av=0.751 F test: Probability=0.958, F= 1.168 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03491, wR= 0.04923, Acormin=0.545, Acormax=1.139, Acor_av=0.816 F test: Probability=0.973, F= 1.189 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02704, wR= 0.03482, Acormin=0.675, Acormax=1.192, Acor_av=0.852 F test: Probability=1.000, F= 1.642 Trying model 6 (ne=6, no=0)... Results: Rint= 0.02878, wR= 0.03985, Acormin=0.640, Acormax=1.140, Acor_av=0.829 F test: Probability=0.000, F= 0.878 Trying model 7 (ne=6, no=1)... Results: Rint= 0.02806, wR= 0.03868, Acormin=0.649, Acormax=1.127, Acor_av=0.835 F test: Probability=0.000, F= 0.917 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02343, wR= 0.03082, Acormin=0.680, Acormax=1.268, Acor_av=0.877 F test: Probability=0.998, F= 1.297 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02209, wR= 0.02877, Acormin=0.679, Acormax=1.314, Acor_av=0.885 F test: Probability=0.842, F= 1.098 Final absorption model (ne=6, no=3): Rint= 0.02343, Acormin=0.680, Acormax=1.268, Acor_av=0.877 Combined refinement in use Rint: 0.10864 There are 67 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 103 pars with 5356 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14471 Using Levenberg-Marquardt: 0.00010 New wR= 0.02861 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10851 with corrections 0.01736 Rint for all data: 0.10864 with corrections 0.01759 0 observations identified as outliers and rejected Cycle 2 wR= 0.02861 Using Levenberg-Marquardt: 0.00001 New wR= 0.02049 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10851 with corrections 0.01426 Rint for all data: 0.10864 with corrections 0.01449 0 observations identified as outliers and rejected Cycle 3 wR= 0.02049 Using Levenberg-Marquardt: 0.00000 New wR= 0.02065 Using Levenberg-Marquardt: 0.00001 New wR= 0.02064 Using Levenberg-Marquardt: 0.00010 New wR= 0.02061 Using Levenberg-Marquardt: 0.00100 New wR= 0.02056 Using Levenberg-Marquardt: 0.01000 New wR= 0.02049 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10851 with corrections 0.01426 Rint for all data: 0.10864 with corrections 0.01449 Final wR= 0.02049 Final frame scales: Min= 0.9138 Max= 1.2657 Final absorption correction factors: Amin= 0.5228 Amax= 1.3001 PROFFIT INFO: Inet (after scale3 abspack): min=1516.2721 max=4485504.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=294.6111 max=66891.1094 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:2/108 736 reflections read from tmp file 25 reflections are rejected (20 as outliers, 5 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 8 14 6 6 14 10 8 9 24 Initial Chi^2= 0.25418 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.99654 Current error model SIG(F2)^2 = 120.45*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 120.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 120.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4485504- 1683199 73 2538444.03 128.60 100.00 1677810- 1126413 73 1390151.00 67.05 100.00 1118851- 386563 73 675882.40 64.99 100.00 341768- 230856 73 272338.33 42.05 100.00 230261- 191191 73 211272.69 31.32 100.00 190506- 141023 73 157207.00 22.55 100.00 140767- 112556 73 126002.78 19.55 100.00 112172- 7199 73 64728.96 13.93 100.00 6933- 4051 73 5090.09 4.53 100.00 4029- 1516 79 3214.75 3.53 68.35 ------------------------------------------------------------------------------------ 4485504- 1516 736 540021.10 39.51 96.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 73 820242.71 77.55 100.00 1.32- 1.09 73 979839.17 69.42 100.00 1.09- 0.96 73 610956.18 45.43 100.00 0.96- 0.85 73 706534.71 44.51 98.63 0.85- 0.80 73 565846.88 38.74 100.00 0.80- 0.73 73 381809.26 27.09 100.00 0.73- 0.70 73 295619.16 22.46 95.89 0.70- 0.65 73 542662.10 33.12 98.63 0.65- 0.62 73 282882.34 20.55 83.56 0.62- 0.58 79 238593.35 18.03 89.87 ------------------------------------------------------------------------------------ 4.82- 0.58 736 540021.10 39.51 96.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 73 820242.71 77.55 100.00 4.82- 1.09 146 900040.94 73.48 100.00 4.82- 0.96 219 803679.35 64.13 100.00 4.82- 0.85 292 779393.19 59.23 99.66 4.82- 0.80 365 736683.93 55.13 99.73 4.82- 0.73 438 677538.15 50.46 99.77 4.82- 0.70 511 622978.29 46.46 99.22 4.82- 0.65 584 612938.77 44.79 99.14 4.82- 0.62 657 576265.83 42.10 97.41 4.82- 0.58 736 540021.10 39.51 96.60 ------------------------------------------------------------------------------------ 4.82- 0.58 736 540021.10 39.51 96.60 Scale applied to data: s=0.222940 (maximum obs:4485504.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.016: data 736 -> merged 104 With outlier rejection... Rint 0.013; Rsigma 0.017: data 726 -> merged 104 Rejected total: 10, method kkm 10, method Blessing 0 Completeness direct cell (a, b, c) = (8.371, 8.371, 8.371), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586096, 4.833068 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 4.00 80.00 32 1.61 - 1.21 10 10 5.90 100.00 59 1.17 - 1.02 10 10 8.70 100.00 87 0.99 - 0.89 10 10 8.70 100.00 87 0.88 - 0.81 10 10 8.60 100.00 86 0.81 - 0.74 10 10 7.50 100.00 75 0.73 - 0.71 10 10 7.70 100.00 77 0.70 - 0.66 10 10 6.70 100.00 67 0.66 - 0.64 10 10 6.00 100.00 60 0.63 - 0.60 10 10 6.20 100.00 62 --------------------------------------------------------------- 5.92 - 0.60 98 100 7.06 98.00 692 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:41:43 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915415 5.919113 5.920917 60.0259 89.9925 59.9940 593 Reflections read from file xs1715a.hkl; mean (I/sigma) = 19.80 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 272 324 282 296 439 406 394 593 N (int>3sigma) = 0 208 324 218 231 375 331 317 478 Mean intensity = 0.0 62.8 38.6 60.8 84.9 53.3 86.5 82.6 82.0 Mean int/sigma = 0.0 16.6 17.6 16.4 20.1 16.9 19.8 20.0 19.8 Lattice type: P chosen Volume: 146.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.915 5.917 5.921 60.02 60.05 60.03 Niggli form: a.a = 34.992 b.b = 35.008 c.c = 35.055 b.c = 17.503 a.c = 17.487 a.b = 17.482 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.067 CUBIC F-lattice R(int) = 0.219 [ 445] Vol = 586.6 Cell: 8.370 8.369 8.374 90.05 89.98 90.05 Volume: 586.59 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.068 RHOMBOHEDRAL R-lattice R(int) = 0.201 [ 253] Vol = 439.9 Cell: 5.919 5.922 14.491 90.06 89.98 120.00 Volume: 439.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.068 RHOMBOHEDRAL R-lattice R(int) = 0.175 [ 63] Vol = 439.9 Trigonal Cell: 5.919 5.922 14.491 90.06 89.98 120.00 Volume: 439.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.024 RHOMBOHEDRAL R-lattice R(int) = 0.207 [ 269] Vol = 439.9 Cell: 5.915 5.919 14.509 89.98 90.01 120.01 Volume: 439.94 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.024 RHOMBOHEDRAL R-lattice R(int) = 0.220 [ 68] Vol = 439.9 Trigonal Cell: 5.915 5.919 14.509 89.98 90.01 120.01 Volume: 439.94 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.203 [ 221] Vol = 293.3 Cell: 5.915 5.921 8.374 89.95 89.97 90.01 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.115 ORTHORHOMBIC I-lattice R(int) = 0.157 [ 310] Vol = 293.3 Cell: 5.921 8.369 5.919 90.00 89.97 90.08 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.021 MONOCLINIC I-lattice R(int) = 0.135 [ 184] Vol = 293.3 Cell: 5.921 5.919 8.369 90.00 90.08 90.03 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.051 MONOCLINIC I-lattice R(int) = 0.176 [ 129] Vol = 293.3 Cell: 5.915 5.921 8.374 90.05 90.03 90.01 Volume: 293.30 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.017 MONOCLINIC I-lattice R(int) = 0.175 [ 108] Vol = 293.3 Cell: 5.921 5.915 8.374 90.03 90.05 90.01 Volume: 293.30 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.077 MONOCLINIC I-lattice R(int) = 0.175 [ 108] Vol = 293.3 Cell: 8.374 5.915 5.921 90.01 90.05 90.03 Volume: 293.30 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 30] Vol = 146.6 Cell: 5.915 5.917 5.921 60.02 60.05 60.03 Volume: 146.65 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 324 0 397 398 593 N (int>3sigma) = 0 0 0 0 324 0 321 316 478 Mean intensity = 0.0 0.0 0.0 0.0 38.6 0.0 80.3 80.7 82.0 Mean int/sigma = 0.0 0.0 0.0 0.0 17.6 0.0 19.3 19.8 19.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.106 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 45 146 N I>3s 5 5 16 146 1.3 1.3 1.0 43.9 5.3 5.3 3.1 21.6 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 0.218 419 Fd-3m 1 1 227 C N N N N 37 2284 0.228 455 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370099 8.369004 8.373958 90.0542 89.9844 90.0533 ZERR 1.00 0.000476 0.002770 0.004498 0.0007 0.0176 0.0006 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4410843- 977442 171 165 26 6.3 1782345.46 86.98 0.010 0.011 904416- 156689 222 220 26 8.5 284428.72 42.76 0.019 0.022 156252- 24621 171 171 26 6.6 119642.80 18.70 0.027 0.035 11687- 1952 172 170 26 6.5 4663.51 4.33 0.146 0.154 ------------------------------------------------------------------------------------------- 4410843- 1952 736 726 104 7.0 520541.37 38.14 0.013 0.014 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 185 176 27 6.5 701098.94 59.98 0.010 0.008 0.010 0.99-0.78 220 220 26 8.5 590239.40 39.55 0.013 0.016 0.015 0.76-0.65 193 193 28 6.9 446887.00 29.06 0.014 0.017 0.021 0.65-0.59 138 137 23 6.0 280421.62 20.63 0.020 0.022 0.030 ------------------------------------------------------------------------------------------------------ inf-0.59 736 726 104 7.0 520541.37 38.14 0.013 0.014 0.017 inf-0.60 700 690 97 7.1 538904.34 39.32 0.012 0.013 0.016 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 176 29 27 93.1 6.5 701098.94 164.63 0.010 0.004 0.99-0.78 220 26 26 100.0 8.5 590239.40 118.35 0.013 0.005 0.76-0.65 193 28 28 100.0 6.9 446887.00 83.88 0.014 0.009 0.65-0.59 137 27 23 85.2 6.0 280421.62 55.97 0.020 0.013 -------------------------------------------------------------------------------------------- inf-0.59 726 110 104 94.5 7.0 520541.37 108.64 0.013 0.007 inf-0.60 690 99 97 98.0 7.1 538904.34 112.24 0.012 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:47:01 2018) ID: 2932; threads 39; handles 878; mem 518708.00 (1237724.00)kB; time: 1w 5d 21h 52m 31s MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 708.5, WS: 270.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:169.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.3,peak PF: 708.5, WS: 272.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:47:01 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000021 0.000023 0.000022 ) 0.087412 -0.166882 0.063604 ( 0.000015 0.000016 0.000016 ) 0.055227 -0.024260 0.122680 ( 0.000020 0.000022 0.000022 ) 5.91535 ( 0.00111 ) 5.92288 ( 0.00085 ) 5.91286 ( 0.00118 ) 59.95509 ( 0.01782 ) 89.89521 ( 0.01573 ) 59.99590 ( 0.01730 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 12:47:01 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000021 0.000023 0.000022 ) 0.087412 -0.166882 0.063604 ( 0.000015 0.000016 0.000016 ) 0.055227 -0.024260 0.122680 ( 0.000020 0.000022 0.000022 ) M - matrix: 0.021562 -0.014359 0.007169 ( 0.000006 0.000004 0.000004 ) -0.014359 0.028698 -0.014332 ( 0.000004 0.000005 0.000004 ) 0.007169 -0.014332 0.021508 ( 0.000004 0.000004 0.000006 ) unit cell: 5.9154(11) 5.9229(8) 5.9129(12) 59.955(18) 89.895(16) 59.996(17) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb PROFFITPEAK info: 612 peaks in the peak location table UB fit with 270 obs out of 290 (total:290,skipped:0) (93.10%) UB - matrix: -0.104205 -0.015001 0.050158 ( 0.000066 0.000100 0.000096 ) 0.087216 -0.166682 0.063439 ( 0.000077 0.000117 0.000111 ) 0.055305 -0.023797 0.122231 ( 0.000078 0.000118 0.000113 ) M - matrix: 0.021524 -0.014290 0.007066 ( 0.000021 0.000021 0.000019 ) -0.014290 0.028574 -0.014235 ( 0.000021 0.000039 0.000025 ) 0.007066 -0.014235 0.021481 ( 0.000019 0.000025 0.000033 ) unit cell: 5.916(4) 5.925(5) 5.913(6) 60.06(10) 89.79(7) 59.92(8) V = 146.8(2) UB fit with 270 obs out of 290 (total:290,skipped:0) (93.10%) UB - matrix: -0.104205 -0.015001 0.050158 ( 0.000066 0.000100 0.000096 ) 0.087216 -0.166682 0.063439 ( 0.000077 0.000117 0.000111 ) 0.055305 -0.023797 0.122231 ( 0.000078 0.000118 0.000113 ) M - matrix: 0.021524 -0.014290 0.007066 ( 0.000021 0.000021 0.000019 ) -0.014290 0.028574 -0.014235 ( 0.000021 0.000039 0.000025 ) 0.007066 -0.014235 0.021481 ( 0.000019 0.000025 0.000033 ) unit cell: 5.916(4) 5.925(5) 5.913(6) 60.06(10) 89.79(7) 59.92(8) V = 146.8(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.104076 -0.014904 0.050063 ( 0.000068 0.000103 0.000099 ) 0.087247 -0.166674 0.063538 ( 0.000078 0.000117 0.000112 ) 0.055201 -0.023815 0.122039 ( 0.000081 0.000121 0.000117 ) M - matrix: 0.021491 -0.014305 0.007070 ( 0.000022 0.000021 0.000019 ) -0.014305 0.028569 -0.014243 ( 0.000021 0.000040 0.000026 ) 0.007070 -0.014243 0.021437 ( 0.000019 0.000026 0.000033 ) UB fit with 273 obs out of 290 (total:290,skipped:0) (94.14%) unit cell: 5.926(4) 5.934(5) 5.924(6) 60.01(10) 89.75(7) 59.86(8) V = 147.3(2) UB fit with 273 obs out of 290 (total:290,skipped:0) (94.14%) UB - matrix: -0.104076 -0.014904 0.050063 ( 0.000068 0.000103 0.000099 ) 0.087247 -0.166674 0.063538 ( 0.000078 0.000117 0.000112 ) 0.055201 -0.023815 0.122039 ( 0.000081 0.000121 0.000117 ) M - matrix: 0.021491 -0.014305 0.007070 ( 0.000022 0.000021 0.000019 ) -0.014305 0.028569 -0.014243 ( 0.000021 0.000040 0.000026 ) 0.007070 -0.014243 0.021437 ( 0.000019 0.000026 0.000033 ) unit cell: 5.926(4) 5.934(5) 5.924(6) 60.01(10) 89.75(7) 59.86(8) V = 147.3(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.104083 -0.014904 0.050069 ( 0.000068 0.000103 0.000099 ) 0.087244 -0.166675 0.063537 ( 0.000078 0.000117 0.000112 ) 0.055202 -0.023811 0.122040 ( 0.000081 0.000121 0.000117 ) M - matrix: 0.021492 -0.014305 0.007069 ( 0.000022 0.000021 0.000019 ) -0.014305 0.028570 -0.014242 ( 0.000021 0.000040 0.000026 ) 0.007069 -0.014242 0.021438 ( 0.000019 0.000026 0.000033 ) UB fit with 273 obs out of 290 (total:290,skipped:0) (94.14%) unit cell: 5.925(4) 5.934(5) 5.924(6) 60.01(10) 89.75(7) 59.86(8) V = 147.3(2) 290 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Run 2 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.000) HKL list info: 438 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104083 -0.014904 0.050069 ( 0.000068 0.000103 0.000099 ) 0.087244 -0.166675 0.063537 ( 0.000078 0.000117 0.000112 ) 0.055202 -0.023811 0.122040 ( 0.000081 0.000121 0.000117 ) M - matrix: 0.021492 -0.014305 0.007069 ( 0.000022 0.000021 0.000019 ) -0.014305 0.028570 -0.014242 ( 0.000021 0.000040 0.000026 ) 0.007069 -0.014242 0.021438 ( 0.000019 0.000026 0.000033 ) UB fit with 273 obs out of 290 (total:290,skipped:0) (94.14%) unit cell: 5.925(4) 5.934(5) 5.924(6) 60.01(10) 89.75(7) 59.86(8) V = 147.3(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 274 obs out of 290 (total:290,skipped:0) (94.48%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb 2 of 204 peaks identified as outliers and rejected 202 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 202 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 202 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 20 | 0.969 ( 0.158) | 1.128 ( 0.561) | 1.253 ( 0.840) | 1.42- 1.12 | 20 | 1.094 ( 0.086) | 1.174 ( 0.192) | 1.121 ( 0.501) | 1.12- 0.99 | 20 | 1.139 ( 0.092) | 1.158 ( 0.120) | 1.205 ( 0.419) | 0.97- 0.88 | 20 | 1.173 ( 0.083) | 1.189 ( 0.124) | 1.100 ( 0.428) | 0.88- 0.81 | 20 | 1.190 ( 0.082) | 1.165 ( 0.133) | 1.129 ( 0.321) | 0.81- 0.75 | 20 | 1.215 ( 0.053) | 1.189 ( 0.107) | 1.132 ( 0.324) | 0.74- 0.71 | 20 | 1.226 ( 0.083) | 1.284 ( 0.111) | 1.147 ( 0.356) | 0.71- 0.67 | 20 | 1.230 ( 0.036) | 1.319 ( 0.148) | 1.105 ( 0.343) | 0.67- 0.63 | 20 | 1.272 ( 0.039) | 1.266 ( 0.107) | 1.133 ( 0.345) | 0.63- 0.59 | 22 | 1.272 ( 0.064) | 1.336 ( 0.233) | 1.152 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 202 | 1.179 ( 0.121) | 1.222 ( 0.237) | 1.148 ( 0.465) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) UB - matrix: -0.103931 -0.015164 0.049504 ( 0.000029 0.000045 0.000044 ) 0.087451 -0.167104 0.063859 ( 0.000026 0.000039 0.000039 ) 0.055207 -0.024095 0.122289 ( 0.000031 0.000048 0.000047 ) M - matrix: 0.021497 -0.014368 0.007191 ( 0.000008 0.000008 0.000008 ) -0.014368 0.028734 -0.014368 ( 0.000008 0.000013 0.000009 ) 0.007191 -0.014368 0.021483 ( 0.000008 0.000009 0.000013 ) unit cell: 5.9288(18) 5.9235(19) 5.932(2) 59.97(4) 90.03(3) 59.98(3) V = 147.16(9) OTKP changes: 202 1 1 1 UB - matrix: -0.104119 -0.015169 0.049789 ( 0.000024 0.000036 0.000036 ) 0.087385 -0.167087 0.063710 ( 0.000025 0.000039 0.000038 ) 0.055376 -0.024099 0.122391 ( 0.000028 0.000043 0.000043 ) M - matrix: 0.021543 -0.014356 0.007161 ( 0.000007 0.000007 0.000007 ) -0.014356 0.028729 -0.014350 ( 0.000007 0.000013 0.000009 ) 0.007161 -0.014350 0.021517 ( 0.000007 0.000009 0.000012 ) UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) unit cell: 5.9171(15) 5.9173(17) 5.921(2) 59.99(3) 89.96(2) 60.00(3) V = 146.62(8) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.982) HKL list info: 438 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104119 -0.015169 0.049789 ( 0.000024 0.000036 0.000036 ) 0.087385 -0.167087 0.063710 ( 0.000025 0.000039 0.000038 ) 0.055376 -0.024099 0.122391 ( 0.000028 0.000043 0.000043 ) M - matrix: 0.021543 -0.014356 0.007161 ( 0.000007 0.000007 0.000007 ) -0.014356 0.028729 -0.014350 ( 0.000007 0.000013 0.000009 ) 0.007161 -0.014350 0.021517 ( 0.000007 0.000009 0.000012 ) UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) unit cell: 5.9171(15) 5.9173(17) 5.921(2) 59.99(3) 89.96(2) 60.00(3) V = 146.62(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb 1 of 205 peaks identified as outliers and rejected 204 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 204 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 204 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 20 | 0.962 ( 0.152) | 1.120 ( 0.553) | 1.173 ( 0.796) | 1.41- 1.12 | 20 | 1.114 ( 0.084) | 1.268 ( 0.384) | 1.346 ( 0.577) | 1.12- 0.98 | 20 | 1.147 ( 0.081) | 1.165 ( 0.112) | 1.171 ( 0.384) | 0.96- 0.88 | 20 | 1.160 ( 0.081) | 1.163 ( 0.129) | 1.201 ( 0.511) | 0.88- 0.82 | 20 | 1.192 ( 0.082) | 1.170 ( 0.125) | 1.104 ( 0.345) | 0.82- 0.76 | 20 | 1.217 ( 0.053) | 1.173 ( 0.100) | 1.167 ( 0.384) | 0.75- 0.71 | 20 | 1.220 ( 0.084) | 1.280 ( 0.126) | 1.146 ( 0.342) | 0.71- 0.67 | 20 | 1.230 ( 0.036) | 1.266 ( 0.160) | 1.177 ( 0.338) | 0.67- 0.64 | 20 | 1.261 ( 0.040) | 1.301 ( 0.133) | 1.061 ( 0.301) | 0.63- 0.59 | 24 | 1.274 ( 0.063) | 1.341 ( 0.220) | 1.175 ( 0.487) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 204 | 1.179 ( 0.119) | 1.227 ( 0.258) | 1.172 ( 0.475) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 65 | 1.150 ( 0.052) | 1.235 ( 0.162) | 1.342 ( 0.607) | 13.1-19.4 | 65 | 1.152 ( 0.121) | 1.256 ( 0.387) | 1.390 ( 0.805) | 19.4-23.6 | 65 | 1.178 ( 0.093) | 1.269 ( 0.329) | 1.270 ( 0.544) | 23.7-27.5 | 65 | 1.136 ( 0.090) | 1.200 ( 0.295) | 1.234 ( 0.515) | 27.6-30.8 | 65 | 1.145 ( 0.108) | 1.207 ( 0.219) | 1.173 ( 0.397) | 30.8-33.8 | 65 | 1.148 ( 0.088) | 1.229 ( 0.296) | 1.157 ( 0.381) | 34.0-37.3 | 65 | 1.144 ( 0.104) | 1.140 ( 0.177) | 1.145 ( 0.386) | 37.3-39.7 | 65 | 1.150 ( 0.126) | 1.168 ( 0.230) | 1.197 ( 0.558) | 39.7-43.0 | 65 | 1.147 ( 0.119) | 1.151 ( 0.229) | 1.234 ( 0.651) | 43.0-49.8 | 68 | 1.214 ( 0.150) | 1.182 ( 0.268) | 1.222 ( 0.503) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 653 | 1.157 ( 0.111) | 1.203 ( 0.271) | 1.237 ( 0.554) | Fitted profile normalization line parameters e1 dimension: a=0.0015 b=0.98 e2 dimension: a=-0.0007 b=1.01 e3 dimension: a=-0.0035 b=1.13 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4988 lp-corr: 4270 Maximum peak integral for reflections I/sig<= 100 - raw: 436199 lp-corr: 681646 Maximum peak integral for reflections I/sig<= 10000 - raw: 8155742 lp-corr: 2571399 PROFFITPEAK - Finished at Wed Mar 28 12:47:05 2018 PROFFITMAIN - Started at Wed Mar 28 12:47:05 2018 OTKP changes: 653 1 1 2 OTKP changes: 653 1 1 2 OTKP changes: 653 1 1 2 OTKP changes: 653 1 1 2 UB - matrix: -0.104193 -0.015041 0.049530 ( 0.000019 0.000022 0.000022 ) 0.087358 -0.167028 0.063639 ( 0.000014 0.000016 0.000016 ) 0.055354 -0.024236 0.122548 ( 0.000018 0.000021 0.000020 ) M - matrix: 0.021552 -0.014366 0.007182 ( 0.000005 0.000004 0.000004 ) -0.014366 0.028712 -0.014345 ( 0.000004 0.000006 0.000004 ) 0.007182 -0.014345 0.021521 ( 0.000004 0.000004 0.000006 ) UB fit with 653 obs out of 653 (total:653,skipped:0) (100.00%) unit cell: 5.9183(11) 5.9189(8) 5.9202(11) 60.030(17) 90.020(15) 59.993(17) V = 146.67(4) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 204 obs out of 204 (total:204,skipped:0) (100.00%) UB - matrix: -0.104094 -0.015128 0.049693 ( 0.000033 0.000051 0.000049 ) 0.087373 -0.167139 0.063825 ( 0.000028 0.000044 0.000042 ) 0.055289 -0.024090 0.122407 ( 0.000031 0.000048 0.000046 ) M - matrix: 0.021527 -0.014361 0.007171 ( 0.000009 0.000009 0.000008 ) -0.014361 0.028745 -0.014368 ( 0.000009 0.000015 0.000010 ) 0.007171 -0.014368 0.021526 ( 0.000008 0.000010 0.000013 ) unit cell: 5.921(2) 5.918(2) 5.922(2) 59.97(4) 89.97(3) 60.00(4) V = 146.69(9) OTKP changes: 204 1 1 1 UB - matrix: -0.104117 -0.015147 0.049756 ( 0.000033 0.000051 0.000049 ) 0.087386 -0.167104 0.063752 ( 0.000028 0.000044 0.000042 ) 0.055365 -0.024117 0.122426 ( 0.000030 0.000047 0.000045 ) M - matrix: 0.021542 -0.014361 0.007169 ( 0.000009 0.000009 0.000008 ) -0.014361 0.028735 -0.014360 ( 0.000009 0.000015 0.000010 ) 0.007169 -0.014360 0.021528 ( 0.000008 0.000010 0.000013 ) UB fit with 204 obs out of 204 (total:204,skipped:0) (100.00%) unit cell: 5.918(2) 5.918(2) 5.921(2) 59.98(4) 89.97(3) 60.00(4) V = 146.61(9) Run 2 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.983) HKL list info: 433 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104117 -0.015147 0.049756 ( 0.000033 0.000051 0.000049 ) 0.087386 -0.167104 0.063752 ( 0.000028 0.000044 0.000042 ) 0.055365 -0.024117 0.122426 ( 0.000030 0.000047 0.000045 ) M - matrix: 0.021542 -0.014361 0.007169 ( 0.000009 0.000009 0.000008 ) -0.014361 0.028735 -0.014360 ( 0.000009 0.000015 0.000010 ) 0.007169 -0.014360 0.021528 ( 0.000008 0.000010 0.000013 ) UB fit with 204 obs out of 204 (total:204,skipped:0) (100.00%) unit cell: 5.918(2) 5.918(2) 5.921(2) 59.98(4) 89.97(3) 60.00(4) V = 146.61(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 204 (total:204,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104117 -0.015147 0.049756 ( 0.000033 0.000051 0.000049 ) 0.087386 -0.167104 0.063752 ( 0.000028 0.000044 0.000042 ) 0.055365 -0.024117 0.122426 ( 0.000030 0.000047 0.000045 ) M - matrix: 0.021542 -0.014361 0.007169 ( 0.000009 0.000009 0.000008 ) -0.014361 0.028735 -0.014360 ( 0.000009 0.000015 0.000010 ) 0.007169 -0.014360 0.021528 ( 0.000008 0.000010 0.000013 ) UB fit with 204 obs out of 204 (total:204,skipped:0) (100.00%) unit cell: 5.918(2) 5.918(2) 5.921(2) 59.98(4) 89.97(3) 60.00(4) V = 146.61(9) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104228 -0.015028 0.049559 ( 0.000019 0.000022 0.000022 ) 0.087320 -0.167011 0.063602 ( 0.000014 0.000016 0.000016 ) 0.055379 -0.024262 0.122532 ( 0.000018 0.000020 0.000020 ) M - matrix: 0.021555 -0.014361 0.007174 ( 0.000005 0.000004 0.000004 ) -0.014361 0.028707 -0.014340 ( 0.000004 0.000006 0.000004 ) 0.007174 -0.014340 0.021516 ( 0.000004 0.000004 0.000006 ) UB fit with 653 obs out of 653 (total:653,skipped:0) (100.00%) unit cell: 5.9168(11) 5.9188(8) 5.9206(11) 60.022(17) 90.002(15) 59.996(17) V = 146.65(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 13 reflections under beam stop or inside a detector rejection region 2 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof 885 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:47:06 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.983) PROFFIT INFO: signal sum: min=388.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=887 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 11 58 105 187 206 337 582 791 885 Percent 0.0 0.0 1.2 6.6 11.9 21.1 23.3 38.1 65.8 89.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 885 100.00 (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 885 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1738382 88 2524240.47 138.69 100.00 1735534- 1143495 88 1426385.04 112.63 100.00 1142803- 343267 88 640833.45 93.21 100.00 341333- 231847 88 272965.14 75.95 100.00 231041- 175601 88 205641.93 52.45 100.00 175528- 150220 88 162950.17 37.71 100.00 149731- 108770 88 129325.96 30.85 100.00 108182- 6956 88 63267.65 21.34 100.00 6841- 4159 88 5167.47 4.87 85.23 4146- 1484 93 3218.69 3.63 51.61 ------------------------------------------------------------------------------------ 4887974- 1484 885 540347.73 56.83 93.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 88 690057.43 91.21 100.00 1.24- 0.98 88 885765.01 75.44 97.73 0.98- 0.82 88 603229.45 60.47 98.86 0.82- 0.72 88 664520.87 68.91 96.59 0.72- 0.65 88 554895.47 59.79 96.59 0.65- 0.60 88 465413.85 49.64 94.32 0.60- 0.56 88 474693.31 49.54 97.73 0.56- 0.52 88 433308.55 44.87 82.95 0.52- 0.48 88 347642.85 36.26 84.09 0.48- 0.40 93 297735.27 33.49 86.02 ------------------------------------------------------------------------------------ 5.26- 0.40 885 540347.73 56.83 93.45 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:47:06 2018 Sorting 885 observations 215 unique observations with > 7.00 F2/sig(F2) 885 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 49 156 Total number of frames 156 Maximum number of 215 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 885 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 49 156 Total number of frames 156 Frame #8 of 156 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 713 observations > 7.00 F2/sig(F2) 713 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 49 156 Total number of frames 156 Frame #8 of 156 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.2 (Out of 713 removed 74 = 639, unique = 201) 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 2 runs Run # start # end # total # 1 1 107 107 2 1 49 156 Total number of frames 156 Frame #8 of 156 skipped from refinement Frame #119 of 156 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 201 unique data precomputed (should be 201) 201 unique data with 639 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.2 (Out of 639 removed 0 = 639, unique = 201) 201 unique data precomputed (should be 201) 201 unique data with 639 observations RMS deviation of equivalent data = 0.66425 Rint = 0.57968 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.55537, wR= 2.80193 Trying model 1 (ne=2, no=0)... Results: Rint= 0.80941, wR= 2.52555, Acormin=-0.218, Acormax=1.791, Acor_av=0.252 F test: Probability=0.000, F= 0.465 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84747, wR= 3.16721, Acormin=-0.789, Acormax=1.172, Acor_av=0.036 F test: Probability=0.000, F= 0.422 Trying model 3 (ne=4, no=0)... Results: Rint= 0.93563, wR= 1.82348, Acormin=-0.273, Acormax=2.072, Acor_av=0.075 F test: Probability=0.000, F= 0.341 Trying model 4 (ne=4, no=1)... Results: Rint= 0.82801, wR= 2.06853, Acormin=-0.554, Acormax=1.364, Acor_av=0.016 F test: Probability=0.000, F= 0.432 Trying model 5 (ne=4, no=3)... Results: Rint= 0.85261, wR= 2.97071, Acormin=-0.259, Acormax=0.672, Acor_av=0.017 F test: Probability=0.000, F= 0.401 Trying model 6 (ne=6, no=0)... Results: Rint= 0.87898, wR= 1.58373, Acormin=-0.246, Acormax=1.323, Acor_av=0.027 F test: Probability=0.000, F= 0.374 Trying model 7 (ne=6, no=1)... Results: Rint= 0.85055, wR= 1.69169, Acormin=-0.232, Acormax=1.198, Acor_av=0.013 F test: Probability=0.000, F= 0.397 Trying model 8 (ne=6, no=3)... Results: Rint= 0.88153, wR= 1.62337, Acormin=-0.261, Acormax=0.669, Acor_av=0.005 F test: Probability=0.000, F= 0.363 Trying model 9 (ne=6, no=5)... Results: Rint= 0.90193, wR= 2.91266, Acormin=-0.099, Acormax=0.230, Acor_av=0.001 F test: Probability=0.000, F= 0.337 Trying model 10 (ne=8, no=0)... Results: Rint= 0.89117, wR= 1.45255, Acormin=-0.214, Acormax=0.520, Acor_av=0.010 F test: Probability=0.000, F= 0.349 Trying model 11 (ne=8, no=1)... Results: Rint= 0.93323, wR= 1.47070, Acormin=-0.203, Acormax=0.504, Acor_av=0.006 F test: Probability=0.000, F= 0.316 Trying model 12 (ne=8, no=3)... Results: Rint= 0.87150, wR= 1.77698, Acormin=-0.044, Acormax=0.021, Acor_av=0.001 F test: Probability=0.000, F= 0.356 Trying model 13 (ne=8, no=5)... Results: Rint= 0.84317, wR= 1.92240, Acormin=-0.031, Acormax=0.042, Acor_av=0.001 F test: Probability=0.000, F= 0.369 Trying model 14 (ne=8, no=7)... Results: Rint= 0.61718, wR= 1.43736, Acormin=-0.012, Acormax=0.047, Acor_av=0.002 F test: Probability=0.000, F= 0.661 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: 0.74624 There are 154 active scales (one needs to be fixed) Refinement control: frame scale #149 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.66425 Using Levenberg-Marquardt: 0.00010 New wR= 0.62574 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.57968 with corrections 0.54571 Rint for all data: 0.74624 with corrections 0.71687 2 observations identified as outliers and rejected Cycle 2 wR= 0.62056 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= 0.66624 Using Levenberg-Marquardt: 0.10000 New wR= 0.60293 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56245 with corrections 0.54832 Rint for all data: 0.74624 with corrections 0.72142 1 observations identified as outliers and rejected Cycle 3 wR= 0.58595 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57218 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55537 with corrections 0.56154 Rint for all data: 0.74624 with corrections 0.73339 0 observations identified as outliers and rejected Cycle 4 wR= 0.57218 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56320 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55537 with corrections 0.58213 Rint for all data: 0.74624 with corrections 0.74945 0 observations identified as outliers and rejected Cycle 5 wR= 0.56320 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.55874 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55537 with corrections 0.59829 Rint for all data: 0.74624 with corrections 0.76385 0 observations identified as outliers and rejected Final wR= 0.55874 Final frame scales: Min= 0.6450 Max= 4.0943 Final absorption correction factors: Amin= 0.0801 Amax= 1.7525 PROFFIT INFO: Inet (after scale3 abspack): min=746.3881 max=6366182.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=131.8391 max=128193.7734 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:2/108 885 reflections read from tmp file 737 reflections are rejected (600 as outliers, 137 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 52 12 2 Initial Chi^2= 1.18799 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.76144 Current error model SIG(F2)^2 = 339.33*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 258.38*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 258.38*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6366182- 1390057 88 2466165.07 75.51 100.00 1371972- 765336 88 1059533.74 53.98 100.00 760148- 352990 88 523704.59 38.95 100.00 348589- 232034 88 286511.86 29.00 100.00 231311- 155815 88 190808.81 22.19 100.00 155103- 111981 88 133049.31 18.05 100.00 111807- 79207 88 95462.31 16.31 100.00 78640- 7960 88 44868.39 10.76 85.23 7938- 3259 88 5008.72 3.17 44.32 3233- 746 93 2230.85 2.69 26.88 ------------------------------------------------------------------------------------ 6366182- 746 885 478030.96 26.92 85.31 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 88 752440.55 56.18 100.00 1.24- 0.98 88 729298.84 41.65 94.32 0.98- 0.82 88 575476.88 29.02 92.05 0.82- 0.72 88 581280.16 29.21 93.18 0.72- 0.65 88 417252.74 24.71 82.95 0.65- 0.60 88 355236.17 20.65 79.55 0.60- 0.56 88 356141.06 20.56 86.36 0.56- 0.52 88 376074.94 18.65 79.55 0.52- 0.48 88 316265.83 15.24 71.59 0.48- 0.40 93 329293.38 14.09 74.19 ------------------------------------------------------------------------------------ 5.26- 0.40 885 478030.96 26.92 85.31 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 88 752440.55 56.18 100.00 5.26- 0.98 176 740869.69 48.92 97.16 5.26- 0.82 264 685738.76 42.28 95.45 5.26- 0.72 352 659624.11 39.01 94.89 5.26- 0.65 440 611149.83 36.15 92.50 5.26- 0.60 528 568497.56 33.57 90.34 5.26- 0.56 616 538160.91 31.71 89.77 5.26- 0.52 704 517900.17 30.08 88.49 5.26- 0.48 792 495496.35 28.43 86.62 5.26- 0.40 885 478030.96 26.92 85.31 ------------------------------------------------------------------------------------ 5.26- 0.40 885 478030.96 26.92 85.31 Scale applied to data: s=0.157080 (maximum obs:6366182.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.764; Rsigma 0.025: data 885 -> merged 299 With outlier rejection... Rint 0.501; Rsigma 0.027: data 712 -> merged 299 Rejected total: 173, method kkm 173, method Blessing 0 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404456, 5.273461 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 3.00 100.00 45 1.46 - 1.12 15 15 4.20 100.00 63 1.08 - 0.96 15 15 3.40 100.00 51 0.96 - 0.86 15 15 3.33 100.00 50 0.86 - 0.79 15 15 2.67 100.00 40 0.79 - 0.73 13 15 2.31 86.67 30 0.73 - 0.69 15 15 2.47 100.00 37 0.69 - 0.65 14 15 2.86 93.33 40 0.65 - 0.63 12 15 1.92 80.00 23 0.63 - 0.60 21 21 2.19 100.00 46 --------------------------------------------------------------- 5.92 - 0.60 150 156 2.83 96.15 425 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:47:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916773 5.918795 5.920638 60.0225 90.0022 59.9964 712 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.92 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 350 389 343 359 541 496 464 712 N (int>3sigma) = 0 291 389 284 293 482 430 399 604 Mean intensity = 0.0 50.4 31.2 50.2 60.5 43.4 62.0 59.5 60.5 Mean int/sigma = 0.0 23.1 22.4 23.1 24.3 22.9 25.2 25.2 24.9 Lattice type: P chosen Volume: 146.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.917 5.917 5.920 60.02 60.04 60.02 Niggli form: a.a = 35.008 b.b = 35.016 c.c = 35.048 b.c = 17.505 a.c = 17.495 a.b = 17.496 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.313 [ 564] Vol = 586.6 Cell: 8.370 8.370 8.373 90.04 89.99 90.04 Volume: 586.61 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.043 RHOMBOHEDRAL R-lattice R(int) = 0.241 [ 351] Vol = 440.0 Cell: 5.919 5.922 14.494 90.03 89.99 120.00 Volume: 439.96 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.043 RHOMBOHEDRAL R-lattice R(int) = 0.244 [ 97] Vol = 440.0 Trigonal Cell: 5.919 5.922 14.494 90.03 89.99 120.00 Volume: 439.96 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.015 RHOMBOHEDRAL R-lattice R(int) = 0.274 [ 386] Vol = 440.0 Cell: 5.917 5.919 14.507 89.98 90.01 120.00 Volume: 439.96 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.015 RHOMBOHEDRAL R-lattice R(int) = 0.240 [ 110] Vol = 440.0 Trigonal Cell: 5.917 5.919 14.507 89.98 90.01 120.00 Volume: 439.96 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.213 [ 361] Vol = 293.3 Cell: 5.917 5.921 8.373 89.96 89.98 90.00 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.083 ORTHORHOMBIC I-lattice R(int) = 0.260 [ 396] Vol = 293.3 Cell: 5.920 8.370 5.919 90.00 89.98 90.06 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.012 MONOCLINIC I-lattice R(int) = 0.196 [ 255] Vol = 293.3 Cell: 5.920 5.919 8.370 90.00 90.06 90.02 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.035 MONOCLINIC I-lattice R(int) = 0.162 [ 251] Vol = 293.3 Cell: 5.917 5.921 8.373 90.04 90.02 90.00 Volume: 293.30 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.012 MONOCLINIC I-lattice R(int) = 0.178 [ 233] Vol = 293.3 Cell: 5.921 5.917 8.373 90.02 90.04 90.00 Volume: 293.30 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.178 [ 233] Vol = 293.3 Cell: 8.373 5.917 5.921 90.00 90.04 90.02 Volume: 293.30 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 121] Vol = 146.7 Cell: 5.917 5.917 5.920 60.02 60.04 60.02 Volume: 146.65 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 389 0 481 477 712 N (int>3sigma) = 0 0 0 0 389 0 410 401 604 Mean intensity = 0.0 0.0 0.0 0.0 31.2 0.0 54.8 62.8 60.5 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 23.6 25.3 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.129 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 57 172 N I>3s 4 4 33 172 2.0 2.0 0.8 35.8 6.1 6.1 3.7 27.4 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 0.313 526 Fd-3m 1 1 227 C N N N N 37 2284 0.316 562 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370153 8.370475 8.372672 90.0413 89.9867 90.0374 ZERR 1.00 0.000433 0.002595 0.004312 0.0003 0.0165 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5336962- 1140558 72 59 29 2.0 1724405.85 57.79 0.433 0.373 1140412- 776315 100 75 29 2.6 689307.98 39.13 0.577 0.464 772185- 551463 99 70 29 2.4 466013.46 31.73 0.511 0.430 540668- 394682 118 91 29 3.1 324840.30 22.94 0.661 0.581 388423- 271970 105 85 29 2.9 246596.78 28.17 0.498 0.509 267539- 174112 101 93 29 3.2 196567.60 21.65 0.477 0.501 170307- 121700 76 57 29 2.0 139146.13 14.51 0.347 0.293 121683- 84317 87 70 29 2.4 103477.90 14.41 0.310 0.222 83915- 47760 64 54 29 1.9 63878.61 10.74 0.342 0.323 47248- 746 63 58 38 1.5 15832.42 4.62 0.722 0.722 ------------------------------------------------------------------------------------------- 5336962- 746 885 712 299 2.4 385398.14 24.92 0.501 0.427 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 117 99 29 3.4 610259.34 48.19 0.452 0.374 0.014 1.12-0.87 124 105 29 3.6 600668.82 34.36 0.613 0.511 0.019 0.86-0.74 104 73 29 2.5 337854.52 24.93 0.444 0.331 0.026 0.73-0.65 106 81 31 2.6 221699.43 17.82 0.370 0.307 0.039 0.65-0.60 82 61 29 2.1 328900.87 21.57 0.408 0.332 0.032 0.60-0.56 85 64 30 2.1 291155.83 18.70 0.416 0.360 0.036 0.56-0.52 80 68 30 2.3 305763.63 17.92 0.553 0.511 0.037 0.52-0.49 75 61 30 2.0 218987.35 13.19 0.471 0.421 0.040 0.49-0.46 61 52 29 1.8 338241.46 16.60 0.520 0.499 0.041 0.46-0.40 51 48 33 1.5 372102.14 14.64 0.620 0.620 0.041 ------------------------------------------------------------------------------------------------------ inf-0.40 885 712 299 2.4 385398.14 24.92 0.501 0.427 0.027 inf-0.60 539 425 150 2.8 444256.73 30.88 0.498 0.405 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 99 29 29 100.0 3.4 610259.34 94.98 0.452 0.008 1.12-0.87 105 29 29 100.0 3.6 600668.82 75.52 0.613 0.012 0.86-0.74 73 31 29 93.5 2.5 337854.52 44.82 0.444 0.019 0.73-0.65 81 34 31 91.2 2.6 221699.43 30.08 0.370 0.027 0.65-0.60 61 30 29 96.7 2.1 328900.87 38.20 0.408 0.023 0.60-0.56 64 37 30 81.1 2.1 291155.83 29.40 0.416 0.025 0.56-0.52 68 36 30 83.3 2.3 305763.63 30.22 0.553 0.027 0.52-0.49 61 43 30 69.8 2.0 218987.35 19.95 0.471 0.033 0.49-0.46 52 54 29 53.7 1.8 338241.46 25.39 0.520 0.029 0.46-0.40 48 132 33 25.0 1.5 372102.14 18.78 0.620 0.035 -------------------------------------------------------------------------------------------- inf-0.40 712 457 299 65.4 2.4 385398.14 45.99 0.501 0.019 inf-0.60 425 156 150 96.2 2.8 444256.73 60.27 0.498 0.015 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.034849 0.076891 -0.007514 ( 0.000009 0.000010 0.000010 ) 0.008045 -0.011858 -0.083505 ( 0.000007 0.000008 0.000008 ) -0.076824 0.033576 -0.012131 ( 0.000009 0.000009 0.000010 ) M - matrix: 0.007181 0.000005 -0.000002 ( 0.000002 0.000001 0.000001 ) 0.000005 0.007180 0.000005 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000005 0.007177 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.034849 0.076891 -0.007514 ( 0.000009 0.000010 0.000010 ) 0.008045 -0.011858 -0.083505 ( 0.000007 0.000008 0.000008 ) -0.076824 0.033576 -0.012131 ( 0.000009 0.000009 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3701(9) 8.3707(9) 8.3727(8) 90.041(9) 89.987(9) 90.038(9) V = 586.62(11) unit cell: 8.3712(3) 8.3712(3) 8.3712(3) 90.0 90.0 90.0 V = 586.62(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -57.000,50 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.983) PROFFIT INFO: signal sum: min=388.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=887 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 22 116 210 374 412 674 1164 1582 1770 Percent 0.0 0.0 1.2 6.6 11.9 21.1 23.3 38.1 65.8 89.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 885 100.00 (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 885 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1738382 88 2524240.47 138.69 100.00 1735534- 1143495 88 1426385.04 112.63 100.00 1142803- 343267 88 640833.45 93.21 100.00 341333- 231847 88 272965.14 75.95 100.00 231041- 175601 88 205641.93 52.45 100.00 175528- 150220 88 162950.17 37.71 100.00 149731- 108770 88 129325.96 30.85 100.00 108182- 6956 88 63267.65 21.34 100.00 6841- 4159 88 5167.47 4.87 85.23 4146- 1484 93 3218.69 3.63 51.61 ------------------------------------------------------------------------------------ 4887974- 1484 885 540347.73 56.83 93.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 88 757950.80 84.26 98.86 1.32- 1.09 88 1021650.18 82.48 100.00 1.09- 0.96 88 558217.74 69.96 100.00 0.96- 0.85 88 638952.02 69.01 96.59 0.85- 0.81 88 626697.25 66.47 98.86 0.80- 0.73 88 400579.90 44.32 95.45 0.73- 0.71 88 309188.36 37.11 93.18 0.71- 0.65 88 552701.04 53.94 96.59 0.65- 0.62 88 285173.40 31.75 76.14 0.62- 0.58 93 267849.45 30.48 79.57 ------------------------------------------------------------------------------------ 4.82- 0.58 885 540347.73 56.83 93.45 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:47:07 2018 Sorting 885 observations 80 unique observations with > 7.00 F2/sig(F2) 885 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 49 156 Total number of frames 156 Maximum number of 80 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 885 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 24 79 Total number of frames 79 713 observations > 7.00 F2/sig(F2) 713 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 24 79 Total number of frames 79 Removing 'redundancy=1' reflections Average redundancy: 8.7 (Out of 713 removed 7 = 706, unique = 81) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 706 observations in 2 runs Run # start # end # total # 1 0 53 54 2 0 24 79 Total number of frames 79 81 unique data precomputed (should be 81) 81 unique data with 706 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.7 (Out of 706 removed 0 = 706, unique = 81) 81 unique data precomputed (should be 81) 81 unique data with 706 observations RMS deviation of equivalent data = 0.14071 Rint = 0.10147 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.09955, wR= 0.14033 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05171, wR= 0.07018, Acormin=0.635, Acormax=1.121, Acor_av=0.796 F test: Probability=1.000, F= 3.676 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04613, wR= 0.06041, Acormin=0.566, Acormax=1.191, Acor_av=0.842 F test: Probability=0.997, F= 1.250 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04093, wR= 0.05727, Acormin=0.600, Acormax=1.124, Acor_av=0.777 F test: Probability=0.998, F= 1.258 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03756, wR= 0.05110, Acormin=0.573, Acormax=1.172, Acor_av=0.844 F test: Probability=0.980, F= 1.182 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02776, wR= 0.03937, Acormin=0.637, Acormax=1.125, Acor_av=0.841 F test: Probability=1.000, F= 1.809 Trying model 6 (ne=6, no=0)... Results: Rint= 0.02958, wR= 0.04065, Acormin=0.654, Acormax=1.178, Acor_av=0.849 F test: Probability=0.000, F= 0.876 Trying model 7 (ne=6, no=1)... Results: Rint= 0.02857, wR= 0.03907, Acormin=0.646, Acormax=1.179, Acor_av=0.859 F test: Probability=0.000, F= 0.935 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02534, wR= 0.03494, Acormin=0.655, Acormax=1.222, Acor_av=0.869 F test: Probability=0.974, F= 1.174 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02342, wR= 0.03050, Acormin=0.656, Acormax=1.297, Acor_av=0.886 F test: Probability=0.953, F= 1.150 Trying model 10 (ne=8, no=0)... Results: Rint= 0.02462, wR= 0.03277, Acormin=0.648, Acormax=1.249, Acor_av=0.876 F test: Probability=0.000, F= 0.911 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02440, wR= 0.03193, Acormin=0.640, Acormax=1.262, Acor_av=0.880 F test: Probability=0.000, F= 0.923 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02170, wR= 0.02926, Acormin=0.646, Acormax=1.284, Acor_av=0.894 F test: Probability=0.955, F= 1.153 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02112, wR= 0.02756, Acormin=0.655, Acormax=1.335, Acor_av=0.902 F test: Probability=0.658, F= 1.035 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01727, wR= 0.02344, Acormin=0.676, Acormax=1.524, Acor_av=0.922 F test: Probability=1.000, F= 1.506 Final absorption model (ne=8, no=7): Rint= 0.01727, Acormin=0.676, Acormax=1.524, Acor_av=0.922 Combined refinement in use Rint: 0.10161 There are 79 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14071 Using Levenberg-Marquardt: 0.00010 New wR= 0.02372 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10147 with corrections 0.01504 Rint for all data: 0.10161 with corrections 0.01528 1 observations identified as outliers and rejected Cycle 2 wR= 0.02121 Using Levenberg-Marquardt: 0.00001 New wR= 0.01779 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10133 with corrections 0.01278 Rint for all data: 0.10161 with corrections 0.01328 0 observations identified as outliers and rejected Cycle 3 wR= 0.01779 Using Levenberg-Marquardt: 0.00000 New wR= 0.01740 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10133 with corrections 0.01264 Rint for all data: 0.10161 with corrections 0.01313 0 observations identified as outliers and rejected Cycle 4 wR= 0.01740 Using Levenberg-Marquardt: 0.00000 New wR= 0.01735 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10133 with corrections 0.01273 Rint for all data: 0.10161 with corrections 0.01322 0 observations identified as outliers and rejected Cycle 5 wR= 0.01735 Using Levenberg-Marquardt: 0.00000 New wR= 0.01734 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10133 with corrections 0.01279 Rint for all data: 0.10161 with corrections 0.01328 Final wR= 0.01734 Final frame scales: Min= 0.9512 Max= 1.1225 Final absorption correction factors: Amin= 0.4649 Amax= 1.3358 PROFFIT INFO: Inet (after scale3 abspack): min=1512.7341 max=4492049.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=299.5486 max=67514.7969 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:2/108 885 reflections read from tmp file 18 reflections are rejected (14 as outliers, 4 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 12 7 6 5 7 8 16 35 Initial Chi^2= 0.25547 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.98948 Current error model SIG(F2)^2 = 108.92*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 107.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 107.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4492050- 1660301 88 2528140.09 135.13 100.00 1653569- 1102103 88 1372482.21 70.07 100.00 1096813- 342629 88 653973.36 69.84 100.00 340848- 228387 88 273239.47 44.82 100.00 228378- 189912 88 208967.24 32.06 100.00 186417- 140911 88 155312.44 23.60 100.00 140599- 111664 88 125916.89 20.69 100.00 111545- 6864 88 62081.00 14.34 100.00 6816- 4062 88 5011.31 4.70 100.00 4043- 1513 93 3210.76 3.77 81.72 ------------------------------------------------------------------------------------ 4492050- 1513 885 535807.36 41.69 98.08 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 88 794339.18 81.95 100.00 1.32- 1.09 88 1055305.22 75.84 100.00 1.09- 0.96 88 557410.94 45.87 100.00 0.96- 0.85 88 644994.47 44.05 98.86 0.85- 0.81 88 602250.66 42.35 100.00 0.80- 0.73 88 378818.68 28.70 100.00 0.73- 0.71 88 302383.29 24.18 97.73 0.71- 0.65 88 520582.06 34.43 100.00 0.65- 0.62 88 265533.32 20.79 90.91 0.62- 0.58 93 252549.94 19.94 93.55 ------------------------------------------------------------------------------------ 4.82- 0.58 885 535807.36 41.69 98.08 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 88 794339.18 81.95 100.00 4.82- 1.09 176 924822.20 78.89 100.00 4.82- 0.96 264 802351.78 67.88 100.00 4.82- 0.85 352 763012.45 61.93 99.72 4.82- 0.81 440 730860.09 58.01 99.77 4.82- 0.73 528 672186.53 53.13 99.81 4.82- 0.71 616 619357.49 48.99 99.51 4.82- 0.65 704 607010.56 47.17 99.57 4.82- 0.62 792 569068.65 44.24 98.61 4.82- 0.58 885 535807.36 41.69 98.08 ------------------------------------------------------------------------------------ 4.82- 0.58 885 535807.36 41.69 98.08 Scale applied to data: s=0.222615 (maximum obs:4492049.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.013; Rsigma 0.015: data 885 -> merged 104 With outlier rejection... Rint 0.012; Rsigma 0.016: data 876 -> merged 104 Rejected total: 9, method kkm 9, method Blessing 0 Completeness direct cell (a, b, c) = (8.371, 8.371, 8.371), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586099, 4.833099 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 4.75 80.00 38 1.61 - 1.21 10 10 7.40 100.00 74 1.17 - 1.02 10 10 10.50 100.00 105 0.99 - 0.89 10 10 10.80 100.00 108 0.88 - 0.81 10 10 10.10 100.00 101 0.81 - 0.74 10 10 8.90 100.00 89 0.73 - 0.71 10 10 9.50 100.00 95 0.70 - 0.66 10 10 7.90 100.00 79 0.66 - 0.64 10 10 7.30 100.00 73 0.63 - 0.60 10 10 7.60 100.00 76 --------------------------------------------------------------- 5.92 - 0.60 98 100 8.55 98.00 838 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:47:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916773 5.918795 5.920638 60.0225 90.0022 59.9964 712 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.92 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 350 389 343 359 541 496 464 712 N (int>3sigma) = 0 291 389 284 293 482 430 399 604 Mean intensity = 0.0 50.4 31.2 50.2 60.5 43.4 62.0 59.5 60.5 Mean int/sigma = 0.0 23.1 22.4 23.1 24.3 22.9 25.2 25.2 24.9 Lattice type: P chosen Volume: 146.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.917 5.917 5.920 60.02 60.04 60.02 Niggli form: a.a = 35.008 b.b = 35.016 c.c = 35.048 b.c = 17.505 a.c = 17.495 a.b = 17.496 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.313 [ 564] Vol = 586.6 Cell: 8.370 8.370 8.373 90.04 89.99 90.04 Volume: 586.61 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.043 RHOMBOHEDRAL R-lattice R(int) = 0.241 [ 351] Vol = 440.0 Cell: 5.919 5.922 14.494 90.03 89.99 120.00 Volume: 439.96 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.043 RHOMBOHEDRAL R-lattice R(int) = 0.244 [ 97] Vol = 440.0 Trigonal Cell: 5.919 5.922 14.494 90.03 89.99 120.00 Volume: 439.96 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.015 RHOMBOHEDRAL R-lattice R(int) = 0.274 [ 386] Vol = 440.0 Cell: 5.917 5.919 14.507 89.98 90.01 120.00 Volume: 439.96 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.015 RHOMBOHEDRAL R-lattice R(int) = 0.240 [ 110] Vol = 440.0 Trigonal Cell: 5.917 5.919 14.507 89.98 90.01 120.00 Volume: 439.96 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.213 [ 361] Vol = 293.3 Cell: 5.917 5.921 8.373 89.96 89.98 90.00 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.083 ORTHORHOMBIC I-lattice R(int) = 0.260 [ 396] Vol = 293.3 Cell: 5.920 8.370 5.919 90.00 89.98 90.06 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.012 MONOCLINIC I-lattice R(int) = 0.196 [ 255] Vol = 293.3 Cell: 5.920 5.919 8.370 90.00 90.06 90.02 Volume: 293.30 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.035 MONOCLINIC I-lattice R(int) = 0.162 [ 251] Vol = 293.3 Cell: 5.917 5.921 8.373 90.04 90.02 90.00 Volume: 293.30 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.012 MONOCLINIC I-lattice R(int) = 0.178 [ 233] Vol = 293.3 Cell: 5.921 5.917 8.373 90.02 90.04 90.00 Volume: 293.30 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.178 [ 233] Vol = 293.3 Cell: 8.373 5.917 5.921 90.00 90.04 90.02 Volume: 293.30 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 121] Vol = 146.7 Cell: 5.917 5.917 5.920 60.02 60.04 60.02 Volume: 146.65 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 389 0 481 477 712 N (int>3sigma) = 0 0 0 0 389 0 410 401 604 Mean intensity = 0.0 0.0 0.0 0.0 31.2 0.0 54.8 62.8 60.5 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 23.6 25.3 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.129 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 57 172 N I>3s 4 4 33 172 2.0 2.0 0.8 35.8 6.1 6.1 3.7 27.4 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 0.313 526 Fd-3m 1 1 227 C N N N N 37 2284 0.316 562 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370153 8.370475 8.372672 90.0413 89.9867 90.0374 ZERR 1.00 0.000433 0.002595 0.004312 0.0003 0.0165 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4415701- 969188 203 200 26 7.7 1797839.25 92.82 0.009 0.011 903818- 156179 269 267 26 10.3 285928.71 45.12 0.016 0.019 155121- 25708 207 207 26 8.0 119063.84 19.72 0.027 0.033 12016- 1960 206 202 26 7.8 4623.59 4.52 0.141 0.147 ------------------------------------------------------------------------------------------- 4415701- 1960 885 876 104 8.4 526816.20 40.65 0.012 0.013 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 223 215 27 8.0 752286.50 65.28 0.010 0.010 0.010 0.99-0.78 265 265 26 10.2 567805.71 40.74 0.011 0.013 0.015 0.76-0.65 235 234 28 8.4 438024.75 30.58 0.013 0.016 0.020 0.65-0.59 162 162 23 7.0 288784.51 22.36 0.018 0.023 0.028 ------------------------------------------------------------------------------------------------------ inf-0.59 885 876 104 8.4 526816.20 40.65 0.012 0.013 0.016 inf-0.60 845 836 97 8.6 543296.54 41.75 0.012 0.013 0.015 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 215 29 27 93.1 8.0 752286.50 196.31 0.010 0.004 0.99-0.78 265 26 26 100.0 10.2 567805.71 133.69 0.011 0.005 0.76-0.65 234 28 28 100.0 8.4 438024.75 96.77 0.013 0.008 0.65-0.59 162 27 23 85.2 7.0 288784.51 66.36 0.018 0.011 -------------------------------------------------------------------------------------------- inf-0.59 876 110 104 94.5 8.4 526816.20 126.75 0.012 0.006 inf-0.60 836 99 97 98.0 8.6 543296.54 130.53 0.012 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:52:23 2018) ID: 2932; threads 39; handles 876; mem 518596.00 (1237724.00)kB; time: 1w 5d 21h 57m 54s MEMORY INFO: Memory PF:1.0, Ph:171.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.4,peak PF: 708.5, WS: 270.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:3.0, Ph:171.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.2,peak PF: 708.5, WS: 272.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:52:23 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000019 0.000022 0.000022 ) 0.087412 -0.166882 0.063604 ( 0.000014 0.000016 0.000016 ) 0.055227 -0.024260 0.122680 ( 0.000018 0.000020 0.000020 ) 5.91535 ( 0.00106 ) 5.92288 ( 0.00083 ) 5.91286 ( 0.00108 ) 59.95509 ( 0.01681 ) 89.89521 ( 0.01476 ) 59.99590 ( 0.01659 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 12:52:23 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000019 0.000022 0.000022 ) 0.087412 -0.166882 0.063604 ( 0.000014 0.000016 0.000016 ) 0.055227 -0.024260 0.122680 ( 0.000018 0.000020 0.000020 ) M - matrix: 0.021555 -0.014361 0.007174 ( 0.000005 0.000004 0.000004 ) -0.014361 0.028707 -0.014340 ( 0.000004 0.000006 0.000004 ) 0.007174 -0.014340 0.021516 ( 0.000004 0.000004 0.000006 ) unit cell: 5.9154(11) 5.9229(8) 5.9129(11) 59.955(17) 89.895(15) 59.996(17) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb PROFFITPEAK info: 906 peaks in the peak location table UB fit with 401 obs out of 430 (total:430,skipped:0) (93.26%) UB - matrix: -0.104118 -0.015210 0.050085 ( 0.000058 0.000075 0.000072 ) 0.087233 -0.166700 0.063490 ( 0.000068 0.000088 0.000085 ) 0.055371 -0.023840 0.122346 ( 0.000064 0.000083 0.000080 ) M - matrix: 0.021516 -0.014278 0.007098 ( 0.000018 0.000017 0.000015 ) -0.014278 0.028589 -0.014262 ( 0.000017 0.000030 0.000019 ) 0.007098 -0.014262 0.021508 ( 0.000015 0.000019 0.000023 ) unit cell: 5.914(3) 5.920(4) 5.912(4) 60.06(7) 89.90(5) 60.02(6) V = 146.68(16) UB fit with 401 obs out of 430 (total:430,skipped:0) (93.26%) UB - matrix: -0.104118 -0.015210 0.050085 ( 0.000058 0.000075 0.000072 ) 0.087233 -0.166700 0.063490 ( 0.000068 0.000088 0.000085 ) 0.055371 -0.023840 0.122346 ( 0.000064 0.000083 0.000080 ) M - matrix: 0.021516 -0.014278 0.007098 ( 0.000018 0.000017 0.000015 ) -0.014278 0.028589 -0.014262 ( 0.000017 0.000030 0.000019 ) 0.007098 -0.014262 0.021508 ( 0.000015 0.000019 0.000023 ) unit cell: 5.914(3) 5.920(4) 5.912(4) 60.06(7) 89.90(5) 60.02(6) V = 146.68(16) OTKP changes: 75 1 1 1 UB - matrix: -0.103989 -0.015179 0.050000 ( 0.000058 0.000075 0.000070 ) 0.087217 -0.166758 0.063578 ( 0.000068 0.000088 0.000082 ) 0.055255 -0.023894 0.122197 ( 0.000065 0.000085 0.000079 ) M - matrix: 0.021474 -0.014286 0.007098 ( 0.000018 0.000016 0.000015 ) -0.014286 0.028610 -0.014281 ( 0.000016 0.000030 0.000019 ) 0.007098 -0.014281 0.021474 ( 0.000015 0.000019 0.000023 ) UB fit with 404 obs out of 430 (total:430,skipped:0) (93.95%) unit cell: 5.923(3) 5.926(4) 5.922(4) 60.00(7) 89.87(5) 59.98(6) V = 147.09(16) UB fit with 404 obs out of 430 (total:430,skipped:0) (93.95%) UB - matrix: -0.103989 -0.015179 0.050000 ( 0.000058 0.000075 0.000070 ) 0.087217 -0.166758 0.063578 ( 0.000068 0.000088 0.000082 ) 0.055255 -0.023894 0.122197 ( 0.000065 0.000085 0.000079 ) M - matrix: 0.021474 -0.014286 0.007098 ( 0.000018 0.000016 0.000015 ) -0.014286 0.028609 -0.014281 ( 0.000016 0.000030 0.000019 ) 0.007098 -0.014281 0.021474 ( 0.000015 0.000019 0.000023 ) unit cell: 5.923(3) 5.926(4) 5.922(4) 60.00(7) 89.87(5) 59.98(6) V = 147.09(16) OTKP changes: 75 1 1 1 UB - matrix: -0.103986 -0.015176 0.049989 ( 0.000058 0.000074 0.000070 ) 0.087214 -0.166750 0.063578 ( 0.000068 0.000088 0.000082 ) 0.055241 -0.023885 0.122185 ( 0.000066 0.000085 0.000079 ) M - matrix: 0.021471 -0.014284 0.007096 ( 0.000018 0.000016 0.000015 ) -0.014284 0.028606 -0.014279 ( 0.000016 0.000030 0.000019 ) 0.007096 -0.014279 0.021470 ( 0.000015 0.000019 0.000023 ) UB fit with 404 obs out of 430 (total:430,skipped:0) (93.95%) unit cell: 5.924(3) 5.926(4) 5.923(4) 60.00(7) 89.87(5) 59.98(6) V = 147.13(16) 430 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Run 2 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 601 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103986 -0.015176 0.049989 ( 0.000058 0.000074 0.000070 ) 0.087214 -0.166750 0.063578 ( 0.000068 0.000088 0.000082 ) 0.055241 -0.023885 0.122185 ( 0.000066 0.000085 0.000079 ) M - matrix: 0.021471 -0.014284 0.007096 ( 0.000018 0.000016 0.000015 ) -0.014284 0.028606 -0.014279 ( 0.000016 0.000030 0.000019 ) 0.007096 -0.014279 0.021470 ( 0.000015 0.000019 0.000023 ) UB fit with 404 obs out of 430 (total:430,skipped:0) (93.95%) unit cell: 5.924(3) 5.926(4) 5.923(4) 60.00(7) 89.87(5) 59.98(6) V = 147.13(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 430 (total:430,skipped:0) (94.42%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb 4 of 315 peaks identified as outliers and rejected 311 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 311 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 311 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 31 | 0.988 ( 0.145) | 1.246 ( 0.713) | 1.229 ( 0.739) | 1.33- 1.12 | 31 | 1.094 ( 0.090) | 1.169 ( 0.196) | 1.143 ( 0.518) | 1.09- 0.97 | 31 | 1.135 ( 0.087) | 1.152 ( 0.123) | 1.168 ( 0.450) | 0.97- 0.85 | 31 | 1.165 ( 0.076) | 1.170 ( 0.133) | 1.203 ( 0.467) | 0.85- 0.81 | 31 | 1.186 ( 0.073) | 1.168 ( 0.134) | 1.265 ( 0.389) | 0.81- 0.73 | 31 | 1.205 ( 0.061) | 1.159 ( 0.134) | 1.101 ( 0.334) | 0.73- 0.70 | 31 | 1.211 ( 0.070) | 1.221 ( 0.164) | 1.118 ( 0.384) | 0.70- 0.66 | 31 | 1.225 ( 0.049) | 1.233 ( 0.172) | 1.175 ( 0.399) | 0.66- 0.62 | 31 | 1.254 ( 0.068) | 1.218 ( 0.159) | 1.199 ( 0.470) | 0.62- 0.59 | 32 | 1.239 ( 0.085) | 1.253 ( 0.244) | 1.227 ( 0.516) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 311 | 1.170 ( 0.114) | 1.199 ( 0.277) | 1.183 ( 0.481) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 311 obs out of 311 (total:311,skipped:0) (100.00%) UB - matrix: -0.103951 -0.015107 0.049626 ( 0.000026 0.000034 0.000032 ) 0.087380 -0.167152 0.063845 ( 0.000022 0.000029 0.000027 ) 0.055187 -0.024104 0.122410 ( 0.000026 0.000034 0.000032 ) M - matrix: 0.021487 -0.014366 0.007176 ( 0.000007 0.000006 0.000006 ) -0.014366 0.028749 -0.014372 ( 0.000006 0.000010 0.000007 ) 0.007176 -0.014372 0.021523 ( 0.000006 0.000007 0.000009 ) unit cell: 5.9297(15) 5.9208(14) 5.9236(17) 59.98(3) 89.98(2) 59.96(2) V = 146.94(6) OTKP changes: 311 1 1 1 UB - matrix: -0.104136 -0.015145 0.049880 ( 0.000023 0.000030 0.000028 ) 0.087416 -0.167191 0.063772 ( 0.000021 0.000028 0.000026 ) 0.055400 -0.024059 0.122535 ( 0.000024 0.000032 0.000030 ) M - matrix: 0.021555 -0.014371 0.007169 ( 0.000007 0.000006 0.000005 ) -0.014371 0.028761 -0.014366 ( 0.000006 0.000010 0.000006 ) 0.007169 -0.014366 0.021570 ( 0.000005 0.000006 0.000009 ) UB fit with 311 obs out of 311 (total:311,skipped:0) (100.00%) unit cell: 5.9161(13) 5.9129(13) 5.9120(16) 60.02(2) 89.96(2) 59.98(2) V = 146.28(6) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.938) HKL list info: 601 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104136 -0.015145 0.049880 ( 0.000023 0.000030 0.000028 ) 0.087416 -0.167191 0.063772 ( 0.000021 0.000028 0.000026 ) 0.055400 -0.024059 0.122535 ( 0.000024 0.000032 0.000030 ) M - matrix: 0.021555 -0.014371 0.007169 ( 0.000007 0.000006 0.000005 ) -0.014371 0.028761 -0.014366 ( 0.000006 0.000010 0.000006 ) 0.007169 -0.014366 0.021570 ( 0.000005 0.000006 0.000009 ) UB fit with 311 obs out of 311 (total:311,skipped:0) (100.00%) unit cell: 5.9161(13) 5.9129(13) 5.9120(16) 60.02(2) 89.96(2) 59.98(2) V = 146.28(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 311 obs out of 311 (total:311,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb 3 of 319 peaks identified as outliers and rejected 316 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 316 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 316 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.36 | 32 | 0.989 ( 0.149) | 1.268 ( 0.713) | 1.273 ( 0.776) | 1.32- 1.12 | 32 | 1.099 ( 0.091) | 1.166 ( 0.191) | 1.183 ( 0.532) | 1.09- 0.96 | 32 | 1.133 ( 0.085) | 1.173 ( 0.183) | 1.152 ( 0.434) | 0.96- 0.87 | 32 | 1.145 ( 0.084) | 1.143 ( 0.137) | 1.155 ( 0.461) | 0.85- 0.81 | 32 | 1.182 ( 0.071) | 1.167 ( 0.131) | 1.267 ( 0.411) | 0.81- 0.74 | 32 | 1.205 ( 0.060) | 1.162 ( 0.130) | 1.110 ( 0.327) | 0.73- 0.70 | 32 | 1.214 ( 0.072) | 1.213 ( 0.160) | 1.175 ( 0.410) | 0.70- 0.65 | 32 | 1.232 ( 0.048) | 1.235 ( 0.169) | 1.244 ( 0.414) | 0.64- 0.62 | 32 | 1.247 ( 0.071) | 1.229 ( 0.175) | 1.174 ( 0.453) | 0.62- 0.59 | 28 | 1.248 ( 0.085) | 1.244 ( 0.244) | 1.265 ( 0.532) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 316 | 1.168 ( 0.115) | 1.199 ( 0.282) | 1.199 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 77 | 1.148 ( 0.051) | 1.260 ( 0.240) | 1.377 ( 0.620) | 13.4-19.5 | 77 | 1.152 ( 0.113) | 1.251 ( 0.357) | 1.369 ( 0.771) | 19.6-23.7 | 77 | 1.171 ( 0.092) | 1.271 ( 0.321) | 1.256 ( 0.565) | 23.7-27.9 | 77 | 1.134 ( 0.098) | 1.177 ( 0.271) | 1.222 ( 0.459) | 28.0-30.9 | 77 | 1.145 ( 0.102) | 1.221 ( 0.282) | 1.193 ( 0.431) | 31.0-34.3 | 77 | 1.155 ( 0.080) | 1.197 ( 0.320) | 1.134 ( 0.352) | 34.4-37.4 | 77 | 1.140 ( 0.109) | 1.142 ( 0.173) | 1.160 ( 0.397) | 37.5-40.2 | 77 | 1.154 ( 0.118) | 1.155 ( 0.227) | 1.236 ( 0.569) | 40.2-43.6 | 77 | 1.149 ( 0.123) | 1.115 ( 0.217) | 1.265 ( 0.644) | 43.6-49.8 | 72 | 1.210 ( 0.161) | 1.164 ( 0.275) | 1.165 ( 0.484) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 765 | 1.155 ( 0.110) | 1.196 ( 0.278) | 1.238 ( 0.549) | Fitted profile normalization line parameters e1 dimension: a=0.0015 b=0.98 e2 dimension: a=-0.0015 b=1.03 e3 dimension: a=-0.0037 b=1.15 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4255 Maximum peak integral for reflections I/sig<= 100 - raw: 439406 lp-corr: 681962 Maximum peak integral for reflections I/sig<= 10000 - raw: 17496592 lp-corr: 2571651 PROFFITPEAK - Finished at Wed Mar 28 12:52:29 2018 PROFFITMAIN - Started at Wed Mar 28 12:52:29 2018 OTKP changes: 765 1 1 2 OTKP changes: 765 1 1 2 UB - matrix: -0.104184 -0.015091 0.049739 ( 0.000018 0.000021 0.000020 ) 0.087386 -0.167239 0.063740 ( 0.000013 0.000015 0.000014 ) 0.055479 -0.024305 0.122685 ( 0.000016 0.000019 0.000018 ) M - matrix: 0.021569 -0.014391 0.007194 ( 0.000005 0.000003 0.000004 ) -0.014391 0.028787 -0.014392 ( 0.000003 0.000005 0.000004 ) 0.007194 -0.014392 0.021588 ( 0.000004 0.000004 0.000005 ) UB fit with 765 obs out of 765 (total:765,skipped:0) (100.00%) unit cell: 5.9160(10) 5.9127(7) 5.9123(10) 60.005(15) 90.000(14) 59.988(15) V = 146.22(4) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 316 obs out of 316 (total:316,skipped:0) (100.00%) UB - matrix: -0.104097 -0.015202 0.049927 ( 0.000026 0.000035 0.000033 ) 0.087475 -0.167143 0.063732 ( 0.000022 0.000029 0.000027 ) 0.055491 -0.024112 0.122582 ( 0.000025 0.000033 0.000030 ) M - matrix: 0.021567 -0.014376 0.007180 ( 0.000007 0.000006 0.000006 ) -0.014376 0.028749 -0.014367 ( 0.000006 0.000010 0.000007 ) 0.007180 -0.014367 0.021581 ( 0.000006 0.000007 0.000009 ) unit cell: 5.9153(15) 5.9143(13) 5.9106(17) 60.03(3) 89.98(2) 59.98(2) V = 146.26(6) OTKP changes: 316 1 1 1 UB - matrix: -0.104128 -0.015141 0.049867 ( 0.000026 0.000035 0.000032 ) 0.087423 -0.167198 0.063783 ( 0.000021 0.000028 0.000026 ) 0.055388 -0.024065 0.122545 ( 0.000024 0.000032 0.000030 ) M - matrix: 0.021553 -0.014373 0.007171 ( 0.000007 0.000006 0.000006 ) -0.014373 0.028764 -0.014369 ( 0.000006 0.000010 0.000006 ) 0.007171 -0.014369 0.021572 ( 0.000006 0.000006 0.000009 ) UB fit with 316 obs out of 316 (total:316,skipped:0) (100.00%) unit cell: 5.9168(15) 5.9132(13) 5.9119(16) 60.02(3) 89.96(2) 59.98(2) V = 146.29(6) Run 2 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.943) HKL list info: 595 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104128 -0.015141 0.049867 ( 0.000026 0.000035 0.000032 ) 0.087423 -0.167198 0.063783 ( 0.000021 0.000028 0.000026 ) 0.055388 -0.024065 0.122545 ( 0.000024 0.000032 0.000030 ) M - matrix: 0.021553 -0.014373 0.007171 ( 0.000007 0.000006 0.000006 ) -0.014373 0.028764 -0.014369 ( 0.000006 0.000010 0.000006 ) 0.007171 -0.014369 0.021572 ( 0.000006 0.000006 0.000009 ) UB fit with 316 obs out of 316 (total:316,skipped:0) (100.00%) unit cell: 5.9168(15) 5.9132(13) 5.9119(16) 60.02(3) 89.96(2) 59.98(2) V = 146.29(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 316 obs out of 316 (total:316,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104128 -0.015141 0.049867 ( 0.000026 0.000035 0.000032 ) 0.087423 -0.167198 0.063783 ( 0.000021 0.000028 0.000026 ) 0.055388 -0.024065 0.122545 ( 0.000024 0.000032 0.000030 ) M - matrix: 0.021553 -0.014373 0.007171 ( 0.000007 0.000006 0.000006 ) -0.014373 0.028764 -0.014369 ( 0.000006 0.000010 0.000006 ) 0.007171 -0.014369 0.021572 ( 0.000006 0.000006 0.000009 ) UB fit with 316 obs out of 316 (total:316,skipped:0) (100.00%) unit cell: 5.9168(15) 5.9132(13) 5.9119(16) 60.02(3) 89.96(2) 59.98(2) V = 146.29(6) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104194 -0.015062 0.049625 ( 0.000018 0.000021 0.000021 ) 0.087340 -0.167051 0.063642 ( 0.000013 0.000015 0.000015 ) 0.055424 -0.024257 0.122560 ( 0.000018 0.000020 0.000020 ) M - matrix: 0.021556 -0.014365 0.007181 ( 0.000005 0.000004 0.000004 ) -0.014365 0.028721 -0.014352 ( 0.000004 0.000005 0.000004 ) 0.007181 -0.014352 0.021534 ( 0.000004 0.000004 0.000006 ) UB fit with 765 obs out of 765 (total:765,skipped:0) (100.00%) unit cell: 5.9167(10) 5.9176(8) 5.9186(11) 60.020(16) 90.009(14) 60.000(16) V = 146.56(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 20 reflections under beam stop or inside a detector rejection region 3 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof 1028 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:52:30 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.943) PROFFIT INFO: signal sum: min=368.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=871 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 13 68 121 215 236 386 674 916 1028 Percent 0.0 0.0 1.3 6.6 11.8 20.9 23.0 37.5 65.6 89.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1028 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 1028 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1787953 102 2567976.29 140.60 100.00 1774700- 1178767 102 1450847.56 113.79 100.00 1171342- 349178 102 679396.04 95.07 100.00 346667- 232010 102 277534.60 74.50 100.00 231964- 181855 102 208704.12 51.89 100.00 180555- 152416 102 164372.86 38.44 100.00 151578- 109716 102 132429.70 31.47 100.00 109678- 7215 102 67386.26 22.43 100.00 7059- 4172 102 5221.98 4.88 85.29 4159- 1484 110 3266.48 3.64 51.82 ------------------------------------------------------------------------------------ 4887974- 1484 1028 551414.39 57.25 93.39 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 102 753998.55 92.57 100.00 1.24- 0.98 102 877006.18 75.99 98.04 0.98- 0.82 102 580634.84 58.66 99.02 0.82- 0.72 102 686200.49 70.56 97.06 0.72- 0.65 102 554677.83 58.22 93.14 0.65- 0.60 102 576442.77 57.86 97.06 0.60- 0.55 102 373212.45 42.94 96.08 0.55- 0.51 102 438250.62 43.66 81.37 0.51- 0.48 102 350975.81 37.23 87.25 0.48- 0.40 110 339374.91 36.44 85.45 ------------------------------------------------------------------------------------ 5.26- 0.40 1028 551414.39 57.25 93.39 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:52:30 2018 Sorting 1028 observations 232 unique observations with > 7.00 F2/sig(F2) 1028 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 74 181 Total number of frames 181 Maximum number of 232 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1028 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 74 181 Total number of frames 181 Frame #8 of 181 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 830 observations > 7.00 F2/sig(F2) 830 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 74 181 Total number of frames 181 Frame #8 of 181 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 830 removed 61 = 769, unique = 223) 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 769 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 74 181 Total number of frames 181 Frame #8 of 181 skipped from refinement Frame #119 of 181 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 223 unique data precomputed (should be 223) 223 unique data with 769 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 769 removed 0 = 769, unique = 223) 223 unique data precomputed (should be 223) 223 unique data with 769 observations RMS deviation of equivalent data = 0.65547 Rint = 0.55280 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.51774, wR= 2.62031 Trying model 1 (ne=2, no=0)... Results: Rint= 0.76259, wR= 2.16011, Acormin=-0.239, Acormax=1.784, Acor_av=0.296 F test: Probability=0.000, F= 0.457 Trying model 2 (ne=2, no=1)... Results: Rint= 0.82133, wR= 2.80068, Acormin=-0.793, Acormax=1.224, Acor_av=0.015 F test: Probability=0.000, F= 0.391 Trying model 3 (ne=4, no=0)... Results: Rint= 0.85318, wR= 1.78331, Acormin=-0.316, Acormax=2.161, Acor_av=0.105 F test: Probability=0.000, F= 0.359 Trying model 4 (ne=4, no=1)... Results: Rint= 0.81732, wR= 2.02928, Acormin=-0.667, Acormax=1.338, Acor_av=0.004 F test: Probability=0.000, F= 0.389 Trying model 5 (ne=4, no=3)... Results: Rint= 0.81148, wR= 1.88866, Acormin=-0.366, Acormax=0.692, Acor_av=0.010 F test: Probability=0.000, F= 0.389 Trying model 6 (ne=6, no=0)... Results: Rint= 0.87542, wR= 1.82614, Acormin=-0.313, Acormax=1.725, Acor_av=0.051 F test: Probability=0.000, F= 0.332 Trying model 7 (ne=6, no=1)... Results: Rint= 0.85410, wR= 1.91164, Acormin=-0.292, Acormax=1.377, Acor_av=0.012 F test: Probability=0.000, F= 0.347 Trying model 8 (ne=6, no=3)... Results: Rint= 0.86714, wR= 1.33274, Acormin=-0.318, Acormax=0.719, Acor_av=0.005 F test: Probability=0.000, F= 0.332 Trying model 9 (ne=6, no=5)... Results: Rint= 0.86936, wR= 1.65300, Acormin=-0.270, Acormax=0.254, Acor_av=0.002 F test: Probability=0.000, F= 0.323 Trying model 10 (ne=8, no=0)... Results: Rint= 0.82197, wR= 1.33702, Acormin=-0.267, Acormax=1.165, Acor_av=0.018 F test: Probability=0.000, F= 0.364 Trying model 11 (ne=8, no=1)... Results: Rint= 0.82845, wR= 1.30607, Acormin=-0.234, Acormax=1.023, Acor_av=0.008 F test: Probability=0.000, F= 0.357 Trying model 12 (ne=8, no=3)... Results: Rint= 0.82830, wR= 1.67540, Acormin=-0.134, Acormax=0.034, Acor_av=0.001 F test: Probability=0.000, F= 0.352 Trying model 13 (ne=8, no=5)... Results: Rint= 0.84112, wR= 1.61587, Acormin=-0.036, Acormax=0.066, Acor_av=0.002 F test: Probability=0.000, F= 0.333 Trying model 14 (ne=8, no=7)... Results: Rint= 0.71444, wR= 1.55171, Acormin=-0.008, Acormax=0.051, Acor_av=0.002 F test: Probability=0.000, F= 0.448 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: 0.72688 There are 179 active scales (one needs to be fixed) Refinement control: frame scale #149 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 183 pars with 16836 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.65547 Using Levenberg-Marquardt: 0.00010 New wR= 0.61255 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55280 with corrections 0.53208 Rint for all data: 0.72688 with corrections 0.70962 4 observations identified as outliers and rejected Cycle 2 wR= 0.59273 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= 0.57993 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52894 with corrections 0.53143 Rint for all data: 0.72688 with corrections 0.72037 2 observations identified as outliers and rejected Cycle 3 wR= 0.57360 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56369 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51481 with corrections 0.55053 Rint for all data: 0.72688 with corrections 0.74089 1 observations identified as outliers and rejected Cycle 4 wR= 0.56357 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.55574 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51407 with corrections 0.58070 Rint for all data: 0.72688 with corrections 0.76428 1 observations identified as outliers and rejected Cycle 5 wR= 0.55195 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.54452 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51186 with corrections 0.60985 Rint for all data: 0.72688 with corrections 0.78736 1 observations identified as outliers and rejected Final wR= 0.54452 Final frame scales: Min= 0.4761 Max= 2.3810 Final absorption correction factors: Amin= 0.0793 Amax= 2.0488 1 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=833.8163 max=5977433.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=157.9387 max=119751.6016 PROFFIT INFO: 4 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:2/108 1024 reflections read from tmp file 791 reflections are rejected (669 as outliers, 122 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 87 17 2 Initial Chi^2= 1.05904 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.72375 Current error model SIG(F2)^2 = 322.53*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 233.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 233.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5977434- 1349616 102 2499097.96 82.78 100.00 1342144- 815166 102 1055782.11 56.64 100.00 813569- 366301 102 567053.26 41.78 100.00 361547- 223467 102 281510.19 29.60 100.00 222434- 149522 102 181612.82 24.44 100.00 149469- 112767 102 128210.29 19.56 100.00 112489- 82351 102 98239.18 16.25 100.00 81514- 8397 102 48312.42 11.50 87.25 8116- 3237 102 4860.10 3.29 48.04 3233- 834 106 2230.44 2.84 33.02 ------------------------------------------------------------------------------------ 5977434- 834 1024 484798.45 28.77 86.62 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 102 892958.50 62.31 100.00 1.24- 0.98 102 725090.85 43.27 96.08 0.98- 0.82 102 469685.27 29.91 96.08 0.82- 0.72 102 559253.54 31.42 93.14 0.72- 0.65 102 389684.05 25.42 82.35 0.65- 0.60 102 415161.58 25.17 87.25 0.60- 0.55 102 324555.49 18.80 85.29 0.55- 0.51 102 364709.53 19.38 75.49 0.51- 0.48 102 357084.34 16.64 74.51 0.47- 0.40 106 354895.61 15.86 76.42 ------------------------------------------------------------------------------------ 5.26- 0.40 1024 484798.45 28.77 86.62 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 102 892958.50 62.31 100.00 5.26- 0.98 204 809024.67 52.79 98.04 5.26- 0.82 306 695911.54 45.16 97.39 5.26- 0.72 408 661747.04 41.73 96.32 5.26- 0.65 510 607334.44 38.47 93.53 5.26- 0.60 612 575305.63 36.25 92.48 5.26- 0.55 714 539484.18 33.76 91.46 5.26- 0.51 816 517637.35 31.96 89.46 5.26- 0.48 918 499798.13 30.26 87.80 5.26- 0.40 1024 484798.45 28.77 86.62 ------------------------------------------------------------------------------------ 5.26- 0.40 1024 484798.45 28.77 86.62 Scale applied to data: s=0.167296 (maximum obs:5977433.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.785; Rsigma 0.024: data 1024 -> merged 304 With outlier rejection... Rint 0.497; Rsigma 0.026: data 805 -> merged 304 Rejected total: 219, method kkm 217, method Blessing 2 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404374, 5.272389 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 3.60 100.00 54 1.46 - 1.12 15 15 4.00 100.00 60 1.08 - 0.96 15 15 3.87 100.00 58 0.96 - 0.86 15 15 3.93 100.00 59 0.86 - 0.79 15 15 3.20 100.00 48 0.79 - 0.73 13 15 3.00 86.67 39 0.73 - 0.69 15 15 2.40 100.00 36 0.69 - 0.65 14 15 3.43 93.33 48 0.65 - 0.63 12 15 2.33 80.00 28 0.63 - 0.60 21 21 2.38 100.00 50 --------------------------------------------------------------- 5.92 - 0.60 150 156 3.20 96.15 480 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:52:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916697 5.917598 5.918557 60.0203 90.0092 59.9998 805 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 390 430 388 402 604 546 532 805 N (int>3sigma) = 0 331 430 329 334 545 486 464 697 Mean intensity = 0.0 48.5 32.5 47.9 61.3 42.6 59.2 58.5 59.1 Mean int/sigma = 0.0 23.8 24.2 24.0 26.2 24.0 25.9 26.9 26.7 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.917 5.917 5.918 60.01 60.03 60.01 Niggli form: a.a = 35.007 b.b = 35.012 c.c = 35.028 b.c = 17.506 a.c = 17.495 a.b = 17.501 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.023 CUBIC F-lattice R(int) = 0.272 [ 654] Vol = 586.2 Cell: 8.368 8.369 8.371 90.03 89.99 90.02 Volume: 586.25 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.023 RHOMBOHEDRAL R-lattice R(int) = 0.212 [ 424] Vol = 439.7 Cell: 5.918 5.920 14.493 90.02 89.99 120.00 Volume: 439.69 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.023 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 120] Vol = 439.7 Trigonal Cell: 5.918 5.920 14.493 90.02 89.99 120.00 Volume: 439.69 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.010 RHOMBOHEDRAL R-lattice R(int) = 0.240 [ 484] Vol = 439.7 Cell: 5.917 5.918 14.501 89.98 90.01 120.00 Volume: 439.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.010 RHOMBOHEDRAL R-lattice R(int) = 0.255 [ 147] Vol = 439.7 Trigonal Cell: 5.917 5.918 14.501 89.98 90.01 120.00 Volume: 439.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.172 [ 469] Vol = 293.1 Cell: 5.917 5.919 8.371 89.98 89.99 89.99 Volume: 293.12 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.053 ORTHORHOMBIC I-lattice R(int) = 0.243 [ 487] Vol = 293.1 Cell: 5.918 8.369 5.918 90.01 89.98 90.03 Volume: 293.12 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.011 MONOCLINIC I-lattice R(int) = 0.188 [ 340] Vol = 293.1 Cell: 5.918 5.918 8.369 89.99 90.03 90.02 Volume: 293.12 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.019 MONOCLINIC I-lattice R(int) = 0.150 [ 358] Vol = 293.1 Cell: 5.917 5.919 8.371 90.02 90.01 89.99 Volume: 293.12 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.009 MONOCLINIC I-lattice R(int) = 0.145 [ 339] Vol = 293.1 Cell: 5.919 5.917 8.371 90.01 90.02 89.99 Volume: 293.12 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.145 [ 339] Vol = 293.1 Cell: 8.371 5.917 5.919 89.99 90.02 90.01 Volume: 293.12 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 226] Vol = 146.6 Cell: 5.917 5.917 5.918 60.01 60.03 60.01 Volume: 146.56 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 430 0 534 533 805 N (int>3sigma) = 0 0 0 0 430 0 459 461 697 Mean intensity = 0.0 0.0 0.0 0.0 32.5 0.0 55.8 60.7 59.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 25.7 27.4 26.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.116 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 64 189 N I>3s 5 5 41 189 2.6 2.6 1.0 37.2 6.3 6.3 3.9 29.5 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 0.272 609 Fd-3m 1 1 227 C N N N N 37 2284 0.281 646 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368117 8.369460 8.370619 90.0268 89.9915 90.0180 ZERR 1.00 0.000425 0.002500 0.004126 0.0006 0.0159 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4375690- 1165441 92 65 30 2.2 1139679.56 53.19 0.258 0.217 1163371- 802477 113 93 30 3.1 702145.83 44.10 0.630 0.483 789068- 562138 121 94 30 3.1 513778.43 36.19 0.540 0.395 548638- 404721 126 95 30 3.2 297185.55 24.51 0.710 0.664 397925- 296156 128 113 30 3.8 290355.31 30.24 0.609 0.627 295460- 169586 101 82 30 2.7 172926.63 19.57 0.415 0.404 168472- 124698 99 75 30 2.5 120788.21 15.61 0.240 0.196 123538- 93064 93 69 30 2.3 105213.81 14.47 0.394 0.253 91964- 54001 81 62 30 2.1 70605.27 11.71 0.236 0.207 50109- 834 70 57 34 1.7 13736.23 4.69 0.325 0.325 ------------------------------------------------------------------------------------------- 4375690- 834 1024 805 304 2.6 353262.15 26.67 0.497 0.387 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 140 114 30 3.8 468201.51 47.32 0.434 0.320 0.016 1.08-0.86 137 113 30 3.8 482656.71 35.35 0.656 0.523 0.019 0.86-0.72 127 99 32 3.1 378789.56 28.66 0.537 0.368 0.022 0.72-0.65 117 88 30 2.9 303249.94 24.12 0.497 0.390 0.028 0.64-0.60 96 71 30 2.4 284909.91 22.06 0.506 0.478 0.030 0.59-0.56 98 72 30 2.4 268757.01 18.67 0.468 0.379 0.035 0.55-0.51 97 75 31 2.4 259063.71 18.86 0.429 0.327 0.035 0.51-0.49 87 71 31 2.3 312008.37 16.95 0.466 0.440 0.037 0.48-0.45 71 55 30 1.8 307812.02 16.37 0.318 0.318 0.040 0.45-0.40 54 47 30 1.6 301777.52 14.80 0.204 0.204 0.042 ------------------------------------------------------------------------------------------------------ inf-0.40 1024 805 304 2.6 353262.15 26.67 0.497 0.387 0.026 inf-0.60 608 480 150 3.2 399458.09 32.96 0.538 0.412 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 114 30 30 100.0 3.8 468201.51 96.38 0.434 0.009 1.08-0.86 113 30 30 100.0 3.8 482656.71 80.93 0.656 0.012 0.86-0.72 99 34 32 94.1 3.1 378789.56 57.40 0.537 0.014 0.72-0.65 88 33 30 90.9 2.9 303249.94 48.41 0.497 0.019 0.64-0.60 71 31 30 96.8 2.4 284909.91 41.89 0.506 0.023 0.59-0.56 72 38 30 78.9 2.4 268757.01 33.54 0.468 0.023 0.55-0.51 75 41 31 75.6 2.4 259063.71 32.92 0.429 0.023 0.51-0.49 71 43 31 72.1 2.3 312008.37 28.23 0.466 0.026 0.48-0.45 55 60 30 50.0 1.8 307812.02 22.73 0.318 0.030 0.45-0.40 47 121 30 24.8 1.6 301777.52 19.41 0.204 0.033 -------------------------------------------------------------------------------------------- inf-0.40 805 464 304 65.5 2.6 353262.15 52.30 0.497 0.019 inf-0.60 480 156 150 96.2 3.2 399458.09 68.54 0.538 0.014 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.034815 0.076908 -0.007531 ( 0.000008 0.000010 0.000010 ) 0.008035 -0.011849 -0.083525 ( 0.000006 0.000007 0.000007 ) -0.076863 0.033568 -0.012130 ( 0.000008 0.000010 0.000010 ) M - matrix: 0.007185 0.000002 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007182 0.000003 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.034815 0.076908 -0.007531 ( 0.000008 0.000010 0.000010 ) 0.008035 -0.011849 -0.083525 ( 0.000006 0.000007 0.000007 ) -0.076863 0.033568 -0.012130 ( 0.000008 0.000010 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3681(9) 8.3697(9) 8.3707(7) 90.027(8) 89.992(8) 90.018(9) V = 586.27(10) unit cell: 8.3695(3) 8.3695(3) 8.3695(3) 90.0 90.0 90.0 V = 586.27(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -32.000,75 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.943) PROFFIT INFO: signal sum: min=368.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=871 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 26 136 242 430 472 772 1348 1832 2056 Percent 0.0 0.0 1.3 6.6 11.8 20.9 23.0 37.5 65.6 89.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1028 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 1028 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1787953 102 2567976.29 140.60 100.00 1774700- 1178767 102 1450847.56 113.79 100.00 1171342- 349178 102 679396.04 95.07 100.00 346667- 232010 102 277534.60 74.50 100.00 231964- 181855 102 208704.12 51.89 100.00 180555- 152416 102 164372.86 38.44 100.00 151578- 109716 102 132429.70 31.47 100.00 109678- 7215 102 67386.26 22.43 100.00 7059- 4172 102 5221.98 4.88 85.29 4159- 1484 110 3266.48 3.64 51.82 ------------------------------------------------------------------------------------ 4887974- 1484 1028 551414.39 57.25 93.39 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 102 816023.13 84.35 99.02 1.32- 1.09 102 987440.29 82.08 100.00 1.09- 0.96 102 583455.78 70.13 100.00 0.96- 0.85 102 664453.17 70.83 96.08 0.85- 0.80 102 640503.17 67.10 99.02 0.80- 0.73 102 403633.25 44.91 96.08 0.73- 0.71 102 281488.04 35.37 92.16 0.70- 0.65 102 579532.43 55.28 95.10 0.65- 0.62 102 293095.28 32.81 78.43 0.62- 0.58 110 285384.46 31.65 79.09 ------------------------------------------------------------------------------------ 4.82- 0.58 1028 551414.39 57.25 93.39 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:52:31 2018 Sorting 1028 observations 84 unique observations with > 7.00 F2/sig(F2) 1028 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 74 181 Total number of frames 181 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1028 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 24 61 Total number of frames 61 830 observations > 7.00 F2/sig(F2) 830 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 24 61 Total number of frames 61 Removing 'redundancy=1' reflections Average redundancy: 9.6 (Out of 830 removed 4 = 826, unique = 86) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 826 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 24 61 Total number of frames 61 86 unique data precomputed (should be 86) 86 unique data with 826 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 9.6 (Out of 826 removed 0 = 826, unique = 86) 86 unique data precomputed (should be 86) 86 unique data with 826 observations RMS deviation of equivalent data = 0.13413 Rint = 0.09411 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.09240, wR= 0.13314 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05270, wR= 0.06989, Acormin=0.641, Acormax=1.120, Acor_av=0.799 F test: Probability=1.000, F= 3.053 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04511, wR= 0.05914, Acormin=0.579, Acormax=1.201, Acor_av=0.846 F test: Probability=1.000, F= 1.359 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04280, wR= 0.05840, Acormin=0.619, Acormax=1.132, Acor_av=0.782 F test: Probability=0.904, F= 1.102 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03904, wR= 0.05236, Acormin=0.597, Acormax=1.200, Acor_av=0.850 F test: Probability=1.000, F= 1.319 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03563, wR= 0.04890, Acormin=0.570, Acormax=1.069, Acor_av=0.792 F test: Probability=0.990, F= 1.189 Trying model 6 (ne=6, no=0)... Results: Rint= 0.03485, wR= 0.04642, Acormin=0.673, Acormax=1.155, Acor_av=0.829 F test: Probability=0.705, F= 1.041 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03340, wR= 0.04425, Acormin=0.639, Acormax=1.170, Acor_av=0.840 F test: Probability=0.947, F= 1.129 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03022, wR= 0.03922, Acormin=0.647, Acormax=1.180, Acor_av=0.852 F test: Probability=1.000, F= 1.365 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02614, wR= 0.03319, Acormin=0.652, Acormax=1.290, Acor_av=0.880 F test: Probability=1.000, F= 1.316 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03165, wR= 0.03920, Acormin=0.640, Acormax=1.180, Acor_av=0.847 F test: Probability=0.000, F= 0.686 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02913, wR= 0.03536, Acormin=0.643, Acormax=1.243, Acor_av=0.866 F test: Probability=0.000, F= 0.806 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02854, wR= 0.03484, Acormin=0.627, Acormax=1.238, Acor_av=0.871 F test: Probability=0.000, F= 0.832 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02409, wR= 0.03042, Acormin=0.645, Acormax=1.327, Acor_av=0.894 F test: Probability=0.965, F= 1.149 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02185, wR= 0.02725, Acormin=0.670, Acormax=1.481, Acor_av=0.910 F test: Probability=0.987, F= 1.188 Final absorption model (ne=8, no=7): Rint= 0.02185, Acormin=0.670, Acormax=1.481, Acor_av=0.910 Combined refinement in use Rint: 0.09425 There are 61 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 140 pars with 9870 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13413 Using Levenberg-Marquardt: 0.00010 New wR= 0.02547 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09411 with corrections 0.01554 Rint for all data: 0.09425 with corrections 0.01576 0 observations identified as outliers and rejected Cycle 2 wR= 0.02547 Using Levenberg-Marquardt: 0.00001 New wR= 0.02031 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09411 with corrections 0.01438 Rint for all data: 0.09425 with corrections 0.01460 0 observations identified as outliers and rejected Cycle 3 wR= 0.02031 Using Levenberg-Marquardt: 0.00000 New wR= 0.01994 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09411 with corrections 0.01412 Rint for all data: 0.09425 with corrections 0.01434 0 observations identified as outliers and rejected Cycle 4 wR= 0.01994 Using Levenberg-Marquardt: 0.00000 New wR= 0.01985 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09411 with corrections 0.01404 Rint for all data: 0.09425 with corrections 0.01426 0 observations identified as outliers and rejected Cycle 5 wR= 0.01985 Using Levenberg-Marquardt: 0.00000 New wR= 0.01967 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09411 with corrections 0.01392 Rint for all data: 0.09425 with corrections 0.01414 0 observations identified as outliers and rejected Final wR= 0.01967 Final frame scales: Min= 0.9350 Max= 1.0878 Final absorption correction factors: Amin= 0.4055 Amax= 1.3159 PROFFIT INFO: Inet (after scale3 abspack): min=1533.7831 max=4483098.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=301.3950 max=68288.6094 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:2/108 1028 reflections read from tmp file 26 reflections are rejected (23 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 8 8 7 7 1 8 15 46 Initial Chi^2= 0.23903 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.31705 Current error model SIG(F2)^2 = 107.41*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 141.46*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 141.46*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4483098- 1704012 102 2584047.43 121.76 100.00 1700896- 1124651 102 1402339.36 62.24 100.00 1123568- 381345 102 684573.11 59.90 100.00 347471- 230997 102 277668.37 39.49 100.00 230846- 190509 102 210912.53 28.24 100.00 190066- 143337 102 157504.19 20.70 100.00 143288- 113014 102 128009.94 18.18 100.00 112981- 7134 102 67275.58 13.16 100.00 7003- 4112 102 5101.73 4.08 89.22 4079- 1534 110 3259.06 3.36 60.00 ------------------------------------------------------------------------------------ 4483098- 1534 1028 547798.23 36.85 94.65 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 102 854538.90 74.70 99.02 1.32- 1.09 102 1018911.04 64.15 100.00 1.09- 0.96 102 589425.73 41.31 100.00 0.96- 0.85 102 663187.25 39.43 99.02 0.85- 0.80 102 622526.04 37.31 99.02 0.80- 0.73 102 386174.70 25.36 96.08 0.73- 0.71 102 277450.64 20.17 92.16 0.70- 0.65 102 545572.26 30.78 98.04 0.65- 0.62 102 275928.07 18.71 78.43 0.62- 0.58 110 266342.67 18.04 85.45 ------------------------------------------------------------------------------------ 4.82- 0.58 1028 547798.23 36.85 94.65 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 102 854538.90 74.70 99.02 4.82- 1.09 204 936724.97 69.42 99.51 4.82- 0.96 306 820958.56 60.05 99.67 4.82- 0.85 408 781515.73 54.90 99.51 4.82- 0.80 510 749717.79 51.38 99.41 4.82- 0.73 612 689127.27 47.04 98.86 4.82- 0.71 714 630316.33 43.20 97.90 4.82- 0.65 816 619723.32 41.65 97.92 4.82- 0.62 918 581523.85 39.10 95.75 4.82- 0.58 1028 547798.23 36.85 94.65 ------------------------------------------------------------------------------------ 4.82- 0.58 1028 547798.23 36.85 94.65 Scale applied to data: s=0.223060 (maximum obs:4483098.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.017: data 1028 -> merged 107 With outlier rejection... Rint 0.013; Rsigma 0.018: data 1021 -> merged 107 Rejected total: 7, method kkm 6, method Blessing 1 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585982, 4.832135 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 5.63 80.00 45 1.61 - 1.21 10 10 8.90 100.00 89 1.17 - 1.01 10 10 12.00 100.00 120 0.99 - 0.89 10 10 12.30 100.00 123 0.88 - 0.81 10 10 11.60 100.00 116 0.81 - 0.74 10 10 10.50 100.00 105 0.73 - 0.71 10 10 11.10 100.00 111 0.70 - 0.66 10 10 9.20 100.00 92 0.66 - 0.64 10 10 8.60 100.00 86 0.63 - 0.60 10 10 8.70 100.00 87 --------------------------------------------------------------- 5.92 - 0.60 98 100 9.94 98.00 974 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:52:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916697 5.917598 5.918557 60.0203 90.0092 59.9998 805 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 390 430 388 402 604 546 532 805 N (int>3sigma) = 0 331 430 329 334 545 486 464 697 Mean intensity = 0.0 48.5 32.5 47.9 61.3 42.6 59.2 58.5 59.1 Mean int/sigma = 0.0 23.8 24.2 24.0 26.2 24.0 25.9 26.9 26.7 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.917 5.917 5.918 60.01 60.03 60.01 Niggli form: a.a = 35.007 b.b = 35.012 c.c = 35.028 b.c = 17.506 a.c = 17.495 a.b = 17.501 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.023 CUBIC F-lattice R(int) = 0.272 [ 654] Vol = 586.2 Cell: 8.368 8.369 8.371 90.03 89.99 90.02 Volume: 586.25 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.023 RHOMBOHEDRAL R-lattice R(int) = 0.212 [ 424] Vol = 439.7 Cell: 5.918 5.920 14.493 90.02 89.99 120.00 Volume: 439.69 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.023 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 120] Vol = 439.7 Trigonal Cell: 5.918 5.920 14.493 90.02 89.99 120.00 Volume: 439.69 Matrix: 0.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.010 RHOMBOHEDRAL R-lattice R(int) = 0.240 [ 484] Vol = 439.7 Cell: 5.917 5.918 14.501 89.98 90.01 120.00 Volume: 439.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.010 RHOMBOHEDRAL R-lattice R(int) = 0.255 [ 147] Vol = 439.7 Trigonal Cell: 5.917 5.918 14.501 89.98 90.01 120.00 Volume: 439.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.172 [ 469] Vol = 293.1 Cell: 5.917 5.919 8.371 89.98 89.99 89.99 Volume: 293.12 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.053 ORTHORHOMBIC I-lattice R(int) = 0.243 [ 487] Vol = 293.1 Cell: 5.918 8.369 5.918 90.01 89.98 90.03 Volume: 293.12 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.011 MONOCLINIC I-lattice R(int) = 0.188 [ 340] Vol = 293.1 Cell: 5.918 5.918 8.369 89.99 90.03 90.02 Volume: 293.12 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.019 MONOCLINIC I-lattice R(int) = 0.150 [ 358] Vol = 293.1 Cell: 5.917 5.919 8.371 90.02 90.01 89.99 Volume: 293.12 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.009 MONOCLINIC I-lattice R(int) = 0.145 [ 339] Vol = 293.1 Cell: 5.919 5.917 8.371 90.01 90.02 89.99 Volume: 293.12 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.145 [ 339] Vol = 293.1 Cell: 8.371 5.917 5.919 89.99 90.02 90.01 Volume: 293.12 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 226] Vol = 146.6 Cell: 5.917 5.917 5.918 60.01 60.03 60.01 Volume: 146.56 Matrix:-1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 430 0 534 533 805 N (int>3sigma) = 0 0 0 0 430 0 459 461 697 Mean intensity = 0.0 0.0 0.0 0.0 32.5 0.0 55.8 60.7 59.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 25.7 27.4 26.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.116 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 64 189 N I>3s 5 5 41 189 2.6 2.6 1.0 37.2 6.3 6.3 3.9 29.5 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 0.272 609 Fd-3m 1 1 227 C N N N N 37 2284 0.281 646 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368117 8.369460 8.370619 90.0268 89.9915 90.0180 ZERR 1.00 0.000425 0.002500 0.004126 0.0006 0.0159 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4429431- 977462 237 233 26 9.0 1835204.40 83.30 0.011 0.012 929065- 182794 284 282 26 10.8 305893.26 41.10 0.018 0.019 167147- 93740 250 250 26 9.6 131045.52 17.91 0.026 0.033 61968- 1994 257 256 29 8.8 8118.76 4.99 0.101 0.129 ------------------------------------------------------------------------------------------- 4429431- 1994 1028 1021 107 9.5 537418.52 36.00 0.013 0.015 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.01 247 241 26 9.3 804490.91 60.56 0.012 0.012 0.011 1.01-0.78 317 316 27 11.7 563345.28 35.04 0.012 0.014 0.017 0.76-0.65 273 273 28 9.8 437524.54 26.56 0.014 0.016 0.023 0.65-0.59 191 191 26 7.3 300317.75 20.07 0.018 0.021 0.031 ------------------------------------------------------------------------------------------------------ inf-0.59 1028 1021 107 9.5 537418.52 36.00 0.013 0.015 0.018 inf-0.60 979 972 97 10.0 552701.76 36.93 0.013 0.014 0.017 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.01 241 28 26 92.9 9.3 804490.91 191.91 0.012 0.004 1.01-0.78 316 27 27 100.0 11.7 563345.28 123.89 0.012 0.005 0.76-0.65 273 28 28 100.0 9.8 437524.54 89.71 0.014 0.008 0.65-0.59 191 27 26 96.3 7.3 300317.75 61.13 0.018 0.013 -------------------------------------------------------------------------------------------- inf-0.59 1021 110 107 97.3 9.5 537418.52 119.07 0.013 0.006 inf-0.60 972 99 97 98.0 10.0 552701.76 122.84 0.013 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 12:58:00 2018) ID: 2932; threads 39; handles 878; mem 518616.00 (1237724.00)kB; time: 1w 5d 22h 3m 31s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.5,peak PF: 708.5, WS: 270.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.3,peak PF: 708.5, WS: 272.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 12:58:00 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000021 ) 0.087412 -0.166882 0.063604 ( 0.000013 0.000015 0.000015 ) 0.055227 -0.024260 0.122680 ( 0.000018 0.000020 0.000020 ) 5.91535 ( 0.00101 ) 5.92288 ( 0.00079 ) 5.91286 ( 0.00106 ) 59.95509 ( 0.01627 ) 89.89521 ( 0.01423 ) 59.99590 ( 0.01583 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 12:58:01 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000021 ) 0.087412 -0.166882 0.063604 ( 0.000013 0.000015 0.000015 ) 0.055227 -0.024260 0.122680 ( 0.000018 0.000020 0.000020 ) M - matrix: 0.021556 -0.014365 0.007181 ( 0.000005 0.000004 0.000004 ) -0.014365 0.028721 -0.014352 ( 0.000004 0.000005 0.000004 ) 0.007181 -0.014352 0.021534 ( 0.000004 0.000004 0.000006 ) unit cell: 5.9154(10) 5.9229(8) 5.9129(11) 59.955(16) 89.895(14) 59.996(16) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb PROFFITPEAK info: 1164 peaks in the peak location table UB fit with 520 obs out of 555 (total:555,skipped:0) (93.69%) UB - matrix: -0.104078 -0.015259 0.050113 ( 0.000056 0.000068 0.000061 ) 0.087205 -0.166652 0.063503 ( 0.000058 0.000071 0.000064 ) 0.055421 -0.023889 0.122359 ( 0.000058 0.000070 0.000064 ) M - matrix: 0.021508 -0.014269 0.007103 ( 0.000017 0.000014 0.000012 ) -0.014269 0.028576 -0.014271 ( 0.000014 0.000024 0.000015 ) 0.007103 -0.014271 0.021516 ( 0.000012 0.000015 0.000019 ) unit cell: 5.914(3) 5.922(3) 5.913(3) 60.04(6) 89.91(4) 60.04(5) V = 146.73(13) UB fit with 520 obs out of 555 (total:555,skipped:0) (93.69%) UB - matrix: -0.104078 -0.015259 0.050113 ( 0.000056 0.000068 0.000061 ) 0.087205 -0.166652 0.063503 ( 0.000058 0.000071 0.000064 ) 0.055421 -0.023889 0.122359 ( 0.000058 0.000070 0.000064 ) M - matrix: 0.021508 -0.014269 0.007103 ( 0.000017 0.000014 0.000012 ) -0.014269 0.028576 -0.014271 ( 0.000014 0.000024 0.000015 ) 0.007103 -0.014271 0.021516 ( 0.000012 0.000015 0.000019 ) unit cell: 5.914(3) 5.922(3) 5.913(3) 60.04(6) 89.91(4) 60.04(5) V = 146.73(13) OTKP changes: 100 1 1 1 UB - matrix: -0.103977 -0.015189 0.050017 ( 0.000056 0.000068 0.000062 ) 0.087223 -0.166776 0.063584 ( 0.000058 0.000070 0.000064 ) 0.055322 -0.023973 0.122236 ( 0.000058 0.000070 0.000063 ) M - matrix: 0.021480 -0.014294 0.007108 ( 0.000017 0.000014 0.000012 ) -0.014294 0.028620 -0.014294 ( 0.000014 0.000024 0.000015 ) 0.007108 -0.014294 0.021486 ( 0.000012 0.000015 0.000019 ) UB fit with 522 obs out of 555 (total:555,skipped:0) (94.05%) unit cell: 5.923(3) 5.926(3) 5.922(3) 59.99(6) 89.87(4) 59.98(5) V = 147.06(14) UB fit with 522 obs out of 555 (total:555,skipped:0) (94.05%) UB - matrix: -0.103977 -0.015189 0.050017 ( 0.000056 0.000068 0.000062 ) 0.087223 -0.166776 0.063584 ( 0.000058 0.000070 0.000064 ) 0.055322 -0.023973 0.122236 ( 0.000058 0.000070 0.000063 ) M - matrix: 0.021480 -0.014294 0.007108 ( 0.000017 0.000014 0.000012 ) -0.014294 0.028620 -0.014294 ( 0.000014 0.000024 0.000015 ) 0.007108 -0.014294 0.021486 ( 0.000012 0.000015 0.000019 ) unit cell: 5.923(3) 5.926(3) 5.922(3) 59.99(6) 89.87(4) 59.98(5) V = 147.06(14) OTKP changes: 100 1 1 1 UB - matrix: -0.103962 -0.015186 0.049992 ( 0.000056 0.000068 0.000062 ) 0.087219 -0.166751 0.063576 ( 0.000058 0.000070 0.000064 ) 0.055299 -0.023965 0.122214 ( 0.000058 0.000070 0.000063 ) M - matrix: 0.021473 -0.014290 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014290 0.028611 -0.014289 ( 0.000014 0.000024 0.000015 ) 0.007106 -0.014289 0.021478 ( 0.000012 0.000015 0.000019 ) UB fit with 522 obs out of 555 (total:555,skipped:0) (94.05%) unit cell: 5.924(3) 5.927(3) 5.923(3) 59.99(6) 89.88(4) 59.98(5) V = 147.14(14) 555 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Run 2 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.993) HKL list info: 758 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103962 -0.015186 0.049992 ( 0.000056 0.000068 0.000062 ) 0.087219 -0.166751 0.063576 ( 0.000058 0.000070 0.000064 ) 0.055299 -0.023965 0.122214 ( 0.000058 0.000070 0.000063 ) M - matrix: 0.021473 -0.014290 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014290 0.028611 -0.014289 ( 0.000014 0.000024 0.000015 ) 0.007106 -0.014289 0.021478 ( 0.000012 0.000015 0.000019 ) UB fit with 522 obs out of 555 (total:555,skipped:0) (94.05%) unit cell: 5.924(3) 5.927(3) 5.923(3) 59.99(6) 89.88(4) 59.98(5) V = 147.14(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 519 obs out of 555 (total:555,skipped:0) (93.51%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb 5 of 417 peaks identified as outliers and rejected 412 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 412 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 412 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 41 | 0.965 ( 0.141) | 1.226 ( 0.718) | 1.179 ( 0.686) | 1.33- 1.12 | 41 | 1.091 ( 0.087) | 1.158 ( 0.180) | 1.120 ( 0.507) | 1.12- 0.97 | 41 | 1.125 ( 0.082) | 1.155 ( 0.105) | 1.269 ( 0.496) | 0.97- 0.85 | 41 | 1.149 ( 0.077) | 1.162 ( 0.121) | 1.165 ( 0.480) | 0.85- 0.81 | 41 | 1.177 ( 0.072) | 1.161 ( 0.124) | 1.329 ( 0.387) | 0.81- 0.73 | 41 | 1.189 ( 0.065) | 1.148 ( 0.130) | 1.068 ( 0.338) | 0.73- 0.70 | 41 | 1.208 ( 0.055) | 1.213 ( 0.159) | 1.192 ( 0.396) | 0.70- 0.66 | 41 | 1.216 ( 0.054) | 1.205 ( 0.173) | 1.211 ( 0.413) | 0.65- 0.62 | 41 | 1.232 ( 0.082) | 1.178 ( 0.167) | 1.173 ( 0.450) | 0.62- 0.59 | 43 | 1.222 ( 0.091) | 1.217 ( 0.231) | 1.279 ( 0.518) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 412 | 1.158 ( 0.114) | 1.182 ( 0.274) | 1.199 ( 0.482) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 411 obs out of 412 (total:412,skipped:0) (99.76%) UB - matrix: -0.103931 -0.015109 0.049614 ( 0.000024 0.000030 0.000027 ) 0.087391 -0.167159 0.063795 ( 0.000020 0.000025 0.000023 ) 0.055234 -0.024192 0.122387 ( 0.000023 0.000029 0.000026 ) M - matrix: 0.021490 -0.014374 0.007179 ( 0.000007 0.000005 0.000005 ) -0.014374 0.028756 -0.014374 ( 0.000005 0.000009 0.000006 ) 0.007179 -0.014374 0.021510 ( 0.000005 0.000006 0.000007 ) unit cell: 5.9305(13) 5.9218(12) 5.9264(14) 59.97(2) 89.973(19) 59.94(2) V = 147.01(5) OTKP changes: 411 1 1 1 UB - matrix: -0.104095 -0.015189 0.049877 ( 0.000021 0.000027 0.000024 ) 0.087434 -0.167162 0.063735 ( 0.000019 0.000024 0.000022 ) 0.055452 -0.024114 0.122532 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021555 -0.014372 0.007175 ( 0.000006 0.000005 0.000004 ) -0.014372 0.028755 -0.014366 ( 0.000005 0.000008 0.000005 ) 0.007175 -0.014366 0.021564 ( 0.000004 0.000005 0.000007 ) UB fit with 411 obs out of 412 (total:412,skipped:0) (99.76%) unit cell: 5.9165(12) 5.9140(11) 5.9136(12) 60.02(2) 89.980(17) 59.99(2) V = 146.35(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.941) HKL list info: 757 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104095 -0.015189 0.049877 ( 0.000021 0.000027 0.000024 ) 0.087434 -0.167162 0.063735 ( 0.000019 0.000024 0.000022 ) 0.055452 -0.024114 0.122532 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021555 -0.014372 0.007175 ( 0.000006 0.000005 0.000004 ) -0.014372 0.028755 -0.014366 ( 0.000005 0.000008 0.000005 ) 0.007175 -0.014366 0.021564 ( 0.000004 0.000005 0.000007 ) UB fit with 411 obs out of 412 (total:412,skipped:0) (99.76%) unit cell: 5.9165(12) 5.9140(11) 5.9136(12) 60.02(2) 89.980(17) 59.99(2) V = 146.35(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 411 obs out of 412 (total:412,skipped:0) (99.76%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb 4 of 417 peaks identified as outliers and rejected 413 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 413 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 413 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 41 | 0.980 ( 0.159) | 1.203 ( 0.662) | 1.302 ( 0.812) | 1.36- 1.12 | 41 | 1.102 ( 0.081) | 1.222 ( 0.417) | 1.192 ( 0.503) | 1.12- 0.96 | 41 | 1.126 ( 0.085) | 1.172 ( 0.136) | 1.159 ( 0.466) | 0.96- 0.88 | 41 | 1.142 ( 0.083) | 1.149 ( 0.121) | 1.220 ( 0.489) | 0.88- 0.81 | 41 | 1.166 ( 0.075) | 1.146 ( 0.132) | 1.243 ( 0.431) | 0.81- 0.74 | 41 | 1.195 ( 0.061) | 1.147 ( 0.122) | 1.154 ( 0.362) | 0.74- 0.71 | 41 | 1.198 ( 0.069) | 1.214 ( 0.142) | 1.205 ( 0.391) | 0.71- 0.65 | 41 | 1.217 ( 0.055) | 1.200 ( 0.174) | 1.207 ( 0.366) | 0.65- 0.62 | 41 | 1.229 ( 0.083) | 1.201 ( 0.167) | 1.224 ( 0.476) | 0.62- 0.59 | 44 | 1.228 ( 0.088) | 1.215 ( 0.230) | 1.326 ( 0.516) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 413 | 1.159 ( 0.114) | 1.187 ( 0.285) | 1.224 ( 0.500) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 86 | 1.144 ( 0.050) | 1.252 ( 0.229) | 1.382 ( 0.618) | 13.2-19.4 | 86 | 1.151 ( 0.109) | 1.242 ( 0.340) | 1.356 ( 0.754) | 19.4-23.6 | 86 | 1.160 ( 0.093) | 1.247 ( 0.298) | 1.250 ( 0.531) | 23.6-27.6 | 86 | 1.142 ( 0.098) | 1.215 ( 0.382) | 1.260 ( 0.546) | 27.6-30.8 | 86 | 1.138 ( 0.107) | 1.186 ( 0.205) | 1.185 ( 0.399) | 30.8-34.2 | 86 | 1.152 ( 0.077) | 1.216 ( 0.353) | 1.175 ( 0.391) | 34.2-37.2 | 86 | 1.136 ( 0.108) | 1.123 ( 0.168) | 1.136 ( 0.384) | 37.2-40.0 | 86 | 1.144 ( 0.126) | 1.156 ( 0.221) | 1.260 ( 0.548) | 40.1-43.0 | 86 | 1.153 ( 0.118) | 1.116 ( 0.220) | 1.256 ( 0.638) | 43.1-49.8 | 88 | 1.202 ( 0.159) | 1.148 ( 0.261) | 1.197 ( 0.479) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 862 | 1.152 ( 0.110) | 1.190 ( 0.280) | 1.246 ( 0.546) | Fitted profile normalization line parameters e1 dimension: a=0.0016 b=0.98 e2 dimension: a=-0.0016 b=1.04 e3 dimension: a=-0.0031 b=1.13 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4254 Maximum peak integral for reflections I/sig<= 100 - raw: 453201 lp-corr: 682501 Maximum peak integral for reflections I/sig<= 10000 - raw: 17496592 lp-corr: 2570455 PROFFITPEAK - Finished at Wed Mar 28 12:58:07 2018 PROFFITMAIN - Started at Wed Mar 28 12:58:07 2018 OTKP changes: 862 1 1 2 OTKP changes: 862 1 1 2 UB - matrix: -0.104175 -0.015098 0.049765 ( 0.000018 0.000020 0.000019 ) 0.087381 -0.167238 0.063737 ( 0.000012 0.000013 0.000013 ) 0.055476 -0.024302 0.122682 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.021565 -0.014389 0.007191 ( 0.000005 0.000003 0.000003 ) -0.014389 0.028787 -0.014392 ( 0.000003 0.000005 0.000003 ) 0.007191 -0.014392 0.021590 ( 0.000003 0.000003 0.000005 ) UB fit with 862 obs out of 862 (total:862,skipped:0) (100.00%) unit cell: 5.9163(9) 5.9127(7) 5.9119(9) 60.002(14) 89.990(13) 59.985(15) V = 146.22(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 413 obs out of 413 (total:413,skipped:0) (100.00%) UB - matrix: -0.104085 -0.015216 0.049910 ( 0.000024 0.000031 0.000027 ) 0.087458 -0.167126 0.063721 ( 0.000017 0.000022 0.000020 ) 0.055504 -0.024139 0.122569 ( 0.000021 0.000027 0.000024 ) M - matrix: 0.021563 -0.014372 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028745 -0.014368 ( 0.000005 0.000008 0.000005 ) 0.007181 -0.014368 0.021574 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9155(13) 5.9149(11) 5.9122(14) 60.02(2) 89.990(19) 59.99(2) V = 146.32(5) OTKP changes: 413 1 1 1 UB - matrix: -0.104105 -0.015178 0.049882 ( 0.000024 0.000030 0.000027 ) 0.087422 -0.167184 0.063745 ( 0.000017 0.000022 0.000020 ) 0.055457 -0.024141 0.122556 ( 0.000021 0.000027 0.000024 ) M - matrix: 0.021556 -0.014374 0.007176 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028764 -0.014373 ( 0.000005 0.000007 0.000005 ) 0.007176 -0.014373 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 413 obs out of 413 (total:413,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9136(11) 5.9129(13) 60.01(2) 89.975(18) 59.99(2) V = 146.31(5) Run 2 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.935) HKL list info: 753 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104105 -0.015178 0.049882 ( 0.000024 0.000030 0.000027 ) 0.087422 -0.167184 0.063745 ( 0.000017 0.000022 0.000020 ) 0.055457 -0.024141 0.122556 ( 0.000021 0.000027 0.000024 ) M - matrix: 0.021556 -0.014374 0.007176 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028764 -0.014373 ( 0.000005 0.000007 0.000005 ) 0.007176 -0.014373 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 413 obs out of 413 (total:413,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9136(11) 5.9129(13) 60.01(2) 89.975(18) 59.99(2) V = 146.31(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 413 obs out of 413 (total:413,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104105 -0.015178 0.049882 ( 0.000024 0.000030 0.000027 ) 0.087422 -0.167184 0.063745 ( 0.000017 0.000022 0.000020 ) 0.055457 -0.024141 0.122556 ( 0.000021 0.000027 0.000024 ) M - matrix: 0.021556 -0.014374 0.007176 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028764 -0.014373 ( 0.000005 0.000007 0.000005 ) 0.007176 -0.014373 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 413 obs out of 413 (total:413,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9136(11) 5.9129(13) 60.01(2) 89.975(18) 59.99(2) V = 146.31(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104176 -0.015081 0.049675 ( 0.000018 0.000021 0.000020 ) 0.087348 -0.167056 0.063639 ( 0.000012 0.000014 0.000013 ) 0.055449 -0.024270 0.122592 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.021557 -0.014367 0.007181 ( 0.000005 0.000003 0.000004 ) -0.014367 0.028724 -0.014356 ( 0.000003 0.000005 0.000004 ) 0.007181 -0.014356 0.021546 ( 0.000004 0.000004 0.000005 ) UB fit with 862 obs out of 862 (total:862,skipped:0) (100.00%) unit cell: 5.9167(10) 5.9174(7) 5.9166(10) 60.021(15) 90.005(14) 59.995(15) V = 146.51(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 28 reflections under beam stop or inside a detector rejection region 6 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof 1164 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 12:58:09 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.935) PROFFIT INFO: signal sum: min=394.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=869 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 13 77 142 244 267 436 764 1042 1164 Percent 0.0 0.0 1.1 6.6 12.2 21.0 22.9 37.5 65.6 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1164 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 1164 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1759129 116 2558036.74 138.55 100.00 1742565- 1168560 116 1431208.66 112.41 100.00 1160174- 348268 116 671977.39 94.50 100.00 345581- 234113 116 277115.99 73.43 100.00 232815- 183456 116 209308.72 52.81 100.00 181957- 151281 116 163931.92 37.96 100.00 150975- 110732 116 132573.83 31.49 100.00 109445- 6629 116 65230.55 21.54 100.00 6469- 4100 116 5042.25 4.76 83.62 4036- 1484 120 3140.38 3.58 51.67 ------------------------------------------------------------------------------------ 4887974- 1484 1164 549871.36 56.92 93.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 116 714905.51 88.91 99.14 1.24- 0.96 116 878884.05 76.58 98.28 0.96- 0.81 116 559416.52 56.60 99.14 0.81- 0.72 116 728248.88 72.37 97.41 0.72- 0.64 116 541999.25 57.75 93.97 0.64- 0.58 116 558148.75 56.97 96.55 0.58- 0.54 116 436378.62 46.20 95.69 0.54- 0.50 116 401449.46 40.69 81.03 0.50- 0.47 116 363633.90 38.88 87.93 0.47- 0.40 120 323456.11 35.00 85.00 ------------------------------------------------------------------------------------ 5.26- 0.40 1164 549871.36 56.92 93.38 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:58:09 2018 Sorting 1164 observations 248 unique observations with > 7.00 F2/sig(F2) 1164 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 98 205 Total number of frames 205 Maximum number of 248 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1164 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 98 205 Total number of frames 205 Frame #8 of 205 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 938 observations > 7.00 F2/sig(F2) 938 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 98 205 Total number of frames 205 Frame #8 of 205 skipped from refinement Frame #185 of 205 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.7 (Out of 938 removed 44 = 894, unique = 241) 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 894 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 98 205 Total number of frames 205 Frame #8 of 205 skipped from refinement Frame #119 of 205 skipped from refinement Frame #185 of 205 skipped from refinement 3 frames need to be skipped from refinement, because of missing redundant and/or observable data 241 unique data precomputed (should be 241) 241 unique data with 894 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.7 (Out of 894 removed 0 = 894, unique = 241) 241 unique data precomputed (should be 241) 241 unique data with 894 observations RMS deviation of equivalent data = 0.64356 Rint = 0.55931 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.52391, wR= 2.48731 Trying model 1 (ne=2, no=0)... Results: Rint= 0.76313, wR= 2.07049, Acormin=-0.203, Acormax=1.689, Acor_av=0.327 F test: Probability=0.000, F= 0.468 Trying model 2 (ne=2, no=1)... Results: Rint= 0.76498, wR= 2.67649, Acormin=-0.769, Acormax=1.196, Acor_av=0.009 F test: Probability=0.000, F= 0.463 Trying model 3 (ne=4, no=0)... Results: Rint= 0.83826, wR= 1.81521, Acormin=-0.303, Acormax=1.706, Acor_av=0.141 F test: Probability=0.000, F= 0.382 Trying model 4 (ne=4, no=1)... Results: Rint= 0.79013, wR= 2.09299, Acormin=-0.685, Acormax=1.043, Acor_av=0.001 F test: Probability=0.000, F= 0.428 Trying model 5 (ne=4, no=3)... Results: Rint= 0.82882, wR= 1.87678, Acormin=-0.573, Acormax=0.915, Acor_av=0.003 F test: Probability=0.000, F= 0.385 Trying model 6 (ne=6, no=0)... Results: Rint= 0.88317, wR= 1.60698, Acormin=-0.343, Acormax=1.473, Acor_av=0.067 F test: Probability=0.000, F= 0.337 Trying model 7 (ne=6, no=1)... Results: Rint= 0.82445, wR= 1.78158, Acormin=-0.403, Acormax=1.173, Acor_av=0.005 F test: Probability=0.000, F= 0.385 Trying model 8 (ne=6, no=3)... Results: Rint= 0.87156, wR= 1.57055, Acormin=-0.403, Acormax=0.960, Acor_av=-0.002 F test: Probability=0.000, F= 0.341 Trying model 9 (ne=6, no=5)... Results: Rint= 0.90847, wR= 1.36601, Acormin=-0.253, Acormax=0.311, Acor_av=0.003 F test: Probability=0.000, F= 0.308 Trying model 10 (ne=8, no=0)... Results: Rint= 0.87624, wR= 1.41269, Acormin=-0.295, Acormax=1.006, Acor_av=0.024 F test: Probability=0.000, F= 0.333 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87311, wR= 1.39011, Acormin=-0.261, Acormax=0.927, Acor_av=0.013 F test: Probability=0.000, F= 0.334 Trying model 12 (ne=8, no=3)... Results: Rint= 0.87462, wR= 1.64039, Acormin=-0.052, Acormax=0.059, Acor_av=0.001 F test: Probability=0.000, F= 0.329 Trying model 13 (ne=8, no=5)... Results: Rint= 0.82070, wR= 1.29134, Acormin=-0.037, Acormax=0.046, Acor_av=0.002 F test: Probability=0.000, F= 0.367 Trying model 14 (ne=8, no=7)... Results: Rint= 0.78846, wR= 1.35025, Acormin=-0.011, Acormax=0.038, Acor_av=0.002 F test: Probability=0.000, F= 0.387 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: 0.73675 There are 202 active scales (one needs to be fixed) Refinement control: frame scale #149 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 206 pars with 21321 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.64356 Using Levenberg-Marquardt: 0.00010 New wR= 0.61048 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55931 with corrections 0.53862 Rint for all data: 0.73675 with corrections 0.72110 4 observations identified as outliers and rejected Cycle 2 wR= 0.60562 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= 0.62328 Using Levenberg-Marquardt: 0.10000 New wR= 0.59410 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.53854 with corrections 0.52928 Rint for all data: 0.73675 with corrections 0.72786 2 observations identified as outliers and rejected Cycle 3 wR= 0.57889 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57229 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52391 with corrections 0.53355 Rint for all data: 0.73675 with corrections 0.73844 1 observations identified as outliers and rejected Cycle 4 wR= 0.56644 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56233 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52145 with corrections 0.54773 Rint for all data: 0.73675 with corrections 0.75107 2 observations identified as outliers and rejected Cycle 5 wR= 0.55892 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.55533 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51940 with corrections 0.56103 Rint for all data: 0.73675 with corrections 0.76266 4 observations identified as outliers and rejected Final wR= 0.55533 Final frame scales: Min= 0.6490 Max= 2.5839 Final absorption correction factors: Amin= 0.2504 Amax= 2.1895 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=1006.5714 max=6992934.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=170.3114 max=119894.8047 PROFFIT INFO: 6 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:2/108 1158 reflections read from tmp file 874 reflections are rejected (774 as outliers, 100 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 94 20 9 Initial Chi^2= 1.02302 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.66700 Current error model SIG(F2)^2 = 476.20*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 317.62*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 317.62*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6992934- 1479624 115 2469144.60 72.60 100.00 1477891- 936331 115 1202423.58 45.64 100.00 932129- 358491 115 623810.88 38.24 100.00 355081- 219611 115 274576.52 26.34 100.00 217700- 170137 115 190748.02 18.97 100.00 170112- 132571 115 150802.47 17.17 100.00 132127- 99056 115 114601.22 13.35 100.00 99023- 8621 115 61211.94 10.20 91.30 8547- 3543 115 5241.31 2.71 25.22 3530- 1007 123 2526.20 2.44 14.63 ------------------------------------------------------------------------------------ 6992934- 1007 1158 506006.21 24.61 82.64 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 115 871445.09 51.92 98.26 1.24- 0.96 115 783602.44 37.83 89.57 0.96- 0.81 115 486033.98 25.13 86.96 0.81- 0.72 115 617611.37 28.09 85.22 0.72- 0.64 115 425364.09 21.96 79.13 0.64- 0.58 115 452273.15 21.23 85.22 0.58- 0.54 115 365742.40 16.95 80.00 0.54- 0.51 115 381002.77 15.80 68.70 0.50- 0.47 115 367427.53 14.97 79.13 0.47- 0.40 123 322336.27 13.03 74.80 ------------------------------------------------------------------------------------ 5.26- 0.40 1158 506006.21 24.61 82.64 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 115 871445.09 51.92 98.26 5.26- 0.96 230 827523.76 44.88 93.91 5.26- 0.81 345 713693.83 38.29 91.59 5.26- 0.72 460 689673.22 35.74 90.00 5.26- 0.64 575 636811.39 32.99 87.83 5.26- 0.58 690 606055.02 31.03 87.39 5.26- 0.54 805 571724.65 29.02 86.34 5.26- 0.51 920 547884.41 27.36 84.13 5.26- 0.47 1035 527833.65 25.99 83.57 5.26- 0.40 1158 506006.21 24.61 82.64 ------------------------------------------------------------------------------------ 5.26- 0.40 1158 506006.21 24.61 82.64 Scale applied to data: s=0.143001 (maximum obs:6992934.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.761; Rsigma 0.027: data 1158 -> merged 304 With outlier rejection... Rint 0.574; Rsigma 0.028: data 981 -> merged 304 Rejected total: 177, method kkm 173, method Blessing 4 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404325, 5.271749 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 3.87 100.00 58 1.46 - 1.12 15 15 4.87 100.00 73 1.08 - 0.96 15 15 4.53 100.00 68 0.96 - 0.86 15 15 4.73 100.00 71 0.86 - 0.79 15 15 3.80 100.00 57 0.79 - 0.73 13 15 3.46 86.67 45 0.73 - 0.69 15 15 3.20 100.00 48 0.69 - 0.65 14 15 3.64 93.33 51 0.65 - 0.63 12 15 3.00 80.00 36 0.63 - 0.60 21 21 2.90 100.00 61 --------------------------------------------------------------- 5.92 - 0.60 150 156 3.79 96.15 568 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:58:09 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916745 5.917356 5.916641 60.0214 90.0046 59.9955 981 Reflections read from file xs1715a.hkl; mean (I/sigma) = 23.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 486 518 478 486 741 665 641 981 N (int>3sigma) = 0 386 518 378 379 641 546 524 805 Mean intensity = 0.0 52.6 28.9 53.5 62.9 44.6 61.3 61.8 62.9 Mean int/sigma = 0.0 21.6 20.4 22.0 22.9 21.3 23.2 23.9 23.8 Lattice type: P chosen Volume: 146.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 Unitcell: 5.917 5.917 5.917 60.01 90.00 60.01 Niggli form: a.a = 35.007 b.b = 35.007 c.c = 35.008 b.c = 17.500 a.c = 0.003 a.b = 17.497 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.034 CUBIC F-lattice R(int) = 0.239 [ 830] Vol = 586.0 Cell: 8.368 8.370 8.367 90.00 90.00 89.98 Volume: 586.04 Matrix: 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.021 RHOMBOHEDRAL R-lattice R(int) = 0.180 [ 659] Vol = 439.5 Cell: 5.918 5.917 14.496 89.99 90.03 120.01 Volume: 439.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.021 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 193] Vol = 439.5 Trigonal Cell: 5.918 5.917 14.496 89.99 90.03 120.01 Volume: 439.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.009 ORTHORHOMBIC I-lattice R(int) = 0.205 [ 657] Vol = 293.0 Cell: 5.918 8.368 5.917 89.98 89.98 89.99 Volume: 293.02 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.009 MONOCLINIC I-lattice R(int) = 0.133 [ 524] Vol = 293.0 Cell: 8.368 5.918 5.917 90.02 90.02 89.99 Volume: 293.02 Matrix:-1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.007 MONOCLINIC I-lattice R(int) = 0.139 [ 483] Vol = 293.0 Cell: 5.917 5.917 8.370 89.98 90.01 90.00 Volume: 293.02 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 345] Vol = 146.5 Cell: 5.917 5.917 5.917 60.01 90.00 60.01 Volume: 146.51 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 518 0 663 651 981 N (int>3sigma) = 0 0 0 0 518 0 546 534 805 Mean intensity = 0.0 0.0 0.0 0.0 28.9 0.0 59.3 60.3 62.9 Mean int/sigma = 0.0 0.0 0.0 0.0 20.4 0.0 23.1 23.3 23.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.179 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 80 220 N I>3s 5 5 32 220 1.2 1.2 0.7 33.6 5.4 5.4 3.2 25.0 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 0.238 770 Fd-3m 1 1 227 C N N N N 37 2284 0.244 806 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367803 8.370207 8.367132 90.0036 89.9990 89.9781 ZERR 1.00 0.002403 0.003872 0.000401 0.0150 0.0002 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5224989- 1162088 109 88 30 2.9 1598685.06 57.42 0.369 0.240 1150897- 838237 116 95 30 3.2 829662.30 34.95 0.682 0.569 835672- 619185 126 105 30 3.5 614427.17 30.70 0.686 0.549 617797- 459339 170 150 30 5.0 416994.29 24.86 0.877 0.868 453856- 330703 134 115 30 3.8 299525.08 24.75 0.659 0.666 319185- 171132 116 96 30 3.2 201872.94 18.73 0.391 0.308 169855- 131398 117 95 30 3.2 146428.04 15.01 0.244 0.181 128970- 100578 91 74 30 2.5 119465.81 11.52 0.271 0.187 100278- 61278 96 84 30 2.8 79103.69 9.33 0.671 0.561 57645- 1007 83 79 34 2.3 21946.36 4.34 0.795 0.767 ------------------------------------------------------------------------------------------- 5224989- 1007 1158 981 304 3.2 439878.69 23.83 0.574 0.446 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 154 131 30 4.4 712506.48 47.28 0.534 0.448 0.014 1.08-0.86 158 141 31 4.5 598845.95 30.86 0.764 0.622 0.021 0.83-0.72 124 104 30 3.5 520154.55 26.66 0.524 0.385 0.024 0.72-0.65 138 110 31 3.5 334215.83 20.14 0.571 0.419 0.034 0.64-0.60 107 90 30 3.0 360461.99 19.53 0.677 0.618 0.033 0.59-0.56 111 89 30 3.0 285243.31 16.30 0.504 0.387 0.039 0.55-0.51 106 95 30 3.2 353286.56 17.06 0.641 0.567 0.037 0.51-0.49 94 77 30 2.6 308404.62 13.88 0.397 0.278 0.042 0.49-0.46 92 79 30 2.6 320800.60 13.51 0.445 0.377 0.045 0.45-0.40 74 65 32 2.0 344687.55 13.51 0.273 0.196 0.046 ------------------------------------------------------------------------------------------------------ inf-0.40 1158 981 304 3.2 439878.69 23.83 0.574 0.446 0.028 inf-0.60 672 568 150 3.8 528114.41 30.24 0.620 0.497 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 131 30 30 100.0 4.4 712506.48 111.83 0.534 0.008 1.08-0.86 141 31 31 100.0 4.5 598845.95 84.34 0.764 0.013 0.83-0.72 104 32 30 93.8 3.5 520154.55 60.02 0.524 0.015 0.72-0.65 110 34 31 91.2 3.5 334215.83 44.22 0.571 0.021 0.64-0.60 90 31 30 96.8 3.0 360461.99 42.66 0.677 0.021 0.59-0.56 89 38 30 78.9 3.0 285243.31 33.47 0.504 0.023 0.55-0.51 95 39 30 76.9 3.2 353286.56 37.38 0.641 0.024 0.51-0.49 77 42 30 71.4 2.6 308404.62 24.80 0.397 0.027 0.49-0.46 79 57 30 52.6 2.6 320800.60 24.63 0.445 0.030 0.45-0.40 65 129 32 24.8 2.0 344687.55 21.74 0.273 0.032 -------------------------------------------------------------------------------------------- inf-0.40 981 464 304 65.5 3.2 439878.69 54.32 0.574 0.019 inf-0.60 568 156 150 96.2 3.8 528114.41 72.63 0.620 0.014 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.076924 -0.007541 -0.034790 ( 0.000010 0.000010 0.000008 ) 0.011854 -0.083528 -0.008035 ( 0.000007 0.000007 0.000006 ) -0.033571 -0.012135 0.076885 ( 0.000010 0.000010 0.000008 ) M - matrix: 0.007185 -0.000003 -0.000000 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007181 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000000 0.007186 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.076924 -0.007541 -0.034790 ( 0.000010 0.000010 0.000008 ) 0.011854 -0.083528 -0.008035 ( 0.000007 0.000007 0.000006 ) -0.033571 -0.012135 0.076885 ( 0.000010 0.000010 0.000008 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3680(9) 8.3702(7) 8.3672(8) 90.004(8) 89.999(8) 89.979(8) V = 586.05(10) unit cell: 8.3684(3) 8.3684(3) 8.3684(3) 90.0 90.0 90.0 V = 586.05(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - -7.000,100 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.935) PROFFIT INFO: signal sum: min=394.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=679.9553 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=869 PROFFIT INFO: Inet: min=1483.5388 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.41 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 26 154 284 488 534 872 1528 2084 2328 Percent 0.0 0.0 1.1 6.6 12.2 21.0 22.9 37.5 65.6 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1164 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 1164 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1759129 116 2558036.74 138.55 100.00 1742565- 1168560 116 1431208.66 112.41 100.00 1160174- 348268 116 671977.39 94.50 100.00 345581- 234113 116 277115.99 73.43 100.00 232815- 183456 116 209308.72 52.81 100.00 181957- 151281 116 163931.92 37.96 100.00 150975- 110732 116 132573.83 31.49 100.00 109445- 6629 116 65230.55 21.54 100.00 6469- 4100 116 5042.25 4.76 83.62 4036- 1484 120 3140.38 3.58 51.67 ------------------------------------------------------------------------------------ 4887974- 1484 1164 549871.36 56.92 93.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 116 795021.89 82.93 98.28 1.32- 1.09 116 979055.28 80.55 100.00 1.09- 0.96 116 589848.06 68.83 100.00 0.96- 0.85 116 675717.65 71.84 96.55 0.85- 0.80 116 596577.50 63.52 98.28 0.80- 0.73 116 419434.27 46.73 96.55 0.73- 0.70 116 345228.88 39.32 92.24 0.70- 0.65 116 518277.27 50.27 90.52 0.65- 0.62 116 299646.48 34.36 82.76 0.62- 0.58 120 288905.19 31.71 79.17 ------------------------------------------------------------------------------------ 4.82- 0.58 1164 549871.36 56.92 93.38 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 12:58:10 2018 Sorting 1164 observations 84 unique observations with > 7.00 F2/sig(F2) 1164 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 98 205 Total number of frames 205 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1164 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 32 69 Total number of frames 69 938 observations > 7.00 F2/sig(F2) 938 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 32 69 Total number of frames 69 Removing 'redundancy=1' reflections Average redundancy: 11.0 (Out of 938 removed 5 = 933, 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): 4/m3bar2/m 933 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 32 69 Total number of frames 69 85 unique data precomputed (should be 85) 85 unique data with 933 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 11.0 (Out of 933 removed 0 = 933, unique = 85) 85 unique data precomputed (should be 85) 85 unique data with 933 observations RMS deviation of equivalent data = 0.13171 Rint = 0.09112 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.08938, wR= 0.12847 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05827, wR= 0.07602, Acormin=0.667, Acormax=1.132, Acor_av=0.808 F test: Probability=1.000, F= 2.339 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04527, wR= 0.06056, Acormin=0.612, Acormax=1.232, Acor_av=0.846 F test: Probability=1.000, F= 1.651 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04624, wR= 0.06298, Acormin=0.639, Acormax=1.135, Acor_av=0.783 F test: Probability=0.000, F= 0.952 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03898, wR= 0.05432, Acormin=0.639, Acormax=1.232, Acor_av=0.851 F test: Probability=1.000, F= 1.334 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03606, wR= 0.04780, Acormin=0.601, Acormax=1.114, Acor_av=0.808 F test: Probability=0.983, F= 1.159 Trying model 6 (ne=6, no=0)... Results: Rint= 0.03841, wR= 0.05000, Acormin=0.679, Acormax=1.139, Acor_av=0.819 F test: Probability=0.000, F= 0.878 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03250, wR= 0.04471, Acormin=0.674, Acormax=1.202, Acor_av=0.846 F test: Probability=0.998, F= 1.222 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02916, wR= 0.03799, Acormin=0.658, Acormax=1.250, Acor_av=0.867 F test: Probability=0.998, F= 1.231 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02767, wR= 0.03589, Acormin=0.655, Acormax=1.258, Acor_av=0.874 F test: Probability=0.903, F= 1.096 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03369, wR= 0.04420, Acormin=0.649, Acormax=1.166, Acor_av=0.828 F test: Probability=0.000, F= 0.743 Trying model 11 (ne=8, no=1)... Results: Rint= 0.03031, wR= 0.04063, Acormin=0.675, Acormax=1.207, Acor_av=0.854 F test: Probability=0.000, F= 0.914 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02754, wR= 0.03402, Acormin=0.646, Acormax=1.274, Acor_av=0.883 F test: Probability=0.906, F= 1.098 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02554, wR= 0.03198, Acormin=0.657, Acormax=1.324, Acor_av=0.893 F test: Probability=0.999, F= 1.259 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02240, wR= 0.02838, Acormin=0.670, Acormax=1.648, Acor_av=0.911 F test: Probability=1.000, F= 1.275 Final absorption model (ne=8, no=7): Rint= 0.02240, Acormin=0.670, Acormax=1.648, Acor_av=0.911 Combined refinement in use Rint: 0.09126 There are 69 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 148 pars with 11026 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13171 Using Levenberg-Marquardt: 0.00010 New wR= 0.02287 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09112 with corrections 0.01524 Rint for all data: 0.09126 with corrections 0.01546 0 observations identified as outliers and rejected Cycle 2 wR= 0.02287 Using Levenberg-Marquardt: 0.00001 New wR= 0.02026 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09112 with corrections 0.01408 Rint for all data: 0.09126 with corrections 0.01430 0 observations identified as outliers and rejected Cycle 3 wR= 0.02026 Using Levenberg-Marquardt: 0.00000 New wR= 0.01984 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09112 with corrections 0.01371 Rint for all data: 0.09126 with corrections 0.01393 0 observations identified as outliers and rejected Cycle 4 wR= 0.01984 Using Levenberg-Marquardt: 0.00000 New wR= 0.01981 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09112 with corrections 0.01363 Rint for all data: 0.09126 with corrections 0.01385 0 observations identified as outliers and rejected Cycle 5 wR= 0.01981 Using Levenberg-Marquardt: 0.00000 New wR= 0.01982 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09112 with corrections 0.01367 Rint for all data: 0.09126 with corrections 0.01389 Final wR= 0.01982 Final frame scales: Min= 0.9326 Max= 1.0996 Final absorption correction factors: Amin= 0.4341 Amax= 1.2738 PROFFIT INFO: Inet (after scale3 abspack): min=1389.3601 max=4468112.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=295.7950 max=67554.8125 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:2/108 1164 reflections read from tmp file 29 reflections are rejected (26 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 7 7 4 5 7 3 12 57 Initial Chi^2= 0.24138 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.37172 Current error model SIG(F2)^2 = 103.57*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 142.07*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 142.07*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4468112- 1692514 116 2554424.29 119.90 100.00 1690163- 1128092 116 1393875.88 61.14 100.00 1119242- 377999 116 682806.38 60.24 100.00 342879- 232133 116 274530.61 39.17 100.00 232052- 191766 116 211764.63 28.61 100.00 190965- 144111 116 157639.52 20.46 100.00 144066- 114294 116 128679.65 18.13 100.00 113487- 6669 116 65840.83 12.70 100.00 6551- 3952 116 4958.82 4.00 87.93 3951- 1389 120 3123.23 3.32 56.67 ------------------------------------------------------------------------------------ 4468112- 1389 1164 545892.77 36.65 94.33 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 116 821205.70 73.03 99.14 1.32- 1.09 116 1000999.05 63.85 100.00 1.09- 0.96 116 591683.36 40.99 100.00 0.96- 0.85 116 674248.93 39.90 98.28 0.85- 0.80 116 580865.84 35.32 98.28 0.80- 0.73 116 405273.14 26.26 96.55 0.73- 0.70 116 341157.31 22.25 91.38 0.70- 0.65 116 491461.41 28.06 93.10 0.65- 0.62 116 286691.51 19.47 82.76 0.62- 0.58 120 274693.12 18.03 84.17 ------------------------------------------------------------------------------------ 4.82- 0.58 1164 545892.77 36.65 94.33 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 116 821205.70 73.03 99.14 4.82- 1.09 232 911102.37 68.44 99.57 4.82- 0.96 348 804629.37 59.29 99.71 4.82- 0.85 464 772034.26 54.45 99.35 4.82- 0.80 580 733800.58 50.62 99.14 4.82- 0.73 696 679046.00 46.56 98.71 4.82- 0.70 812 630776.19 43.09 97.66 4.82- 0.65 928 613361.84 41.21 97.09 4.82- 0.62 1044 577065.14 38.79 95.50 4.82- 0.58 1164 545892.77 36.65 94.33 ------------------------------------------------------------------------------------ 4.82- 0.58 1164 545892.77 36.65 94.33 Scale applied to data: s=0.223808 (maximum obs:4468112.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.017: data 1164 -> merged 107 With outlier rejection... Rint 0.013; Rsigma 0.018: data 1156 -> merged 107 Rejected total: 8, method kkm 7, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585909, 4.831526 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 6.38 80.00 51 1.61 - 1.21 10 10 9.80 100.00 98 1.17 - 1.01 10 10 13.90 100.00 139 0.99 - 0.89 10 10 13.80 100.00 138 0.88 - 0.81 10 10 13.30 100.00 133 0.81 - 0.74 10 10 11.60 100.00 116 0.73 - 0.71 10 10 12.50 100.00 125 0.70 - 0.66 10 10 10.40 100.00 104 0.66 - 0.64 10 10 9.80 100.00 98 0.63 - 0.60 10 10 10.00 100.00 100 --------------------------------------------------------------- 5.92 - 0.60 98 100 11.24 98.00 1102 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 12:58:09 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916745 5.917356 5.916641 60.0214 90.0046 59.9955 981 Reflections read from file xs1715a.hkl; mean (I/sigma) = 23.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 486 518 478 486 741 665 641 981 N (int>3sigma) = 0 386 518 378 379 641 546 524 805 Mean intensity = 0.0 52.6 28.9 53.5 62.9 44.6 61.3 61.8 62.9 Mean int/sigma = 0.0 21.6 20.4 22.0 22.9 21.3 23.2 23.9 23.8 Lattice type: P chosen Volume: 146.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 Unitcell: 5.917 5.917 5.917 60.01 90.00 60.01 Niggli form: a.a = 35.007 b.b = 35.007 c.c = 35.008 b.c = 17.500 a.c = 0.003 a.b = 17.497 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.034 CUBIC F-lattice R(int) = 0.239 [ 830] Vol = 586.0 Cell: 8.368 8.370 8.367 90.00 90.00 89.98 Volume: 586.04 Matrix: 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.021 RHOMBOHEDRAL R-lattice R(int) = 0.180 [ 659] Vol = 439.5 Cell: 5.918 5.917 14.496 89.99 90.03 120.01 Volume: 439.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.021 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 193] Vol = 439.5 Trigonal Cell: 5.918 5.917 14.496 89.99 90.03 120.01 Volume: 439.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.009 ORTHORHOMBIC I-lattice R(int) = 0.205 [ 657] Vol = 293.0 Cell: 5.918 8.368 5.917 89.98 89.98 89.99 Volume: 293.02 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.009 MONOCLINIC I-lattice R(int) = 0.133 [ 524] Vol = 293.0 Cell: 8.368 5.918 5.917 90.02 90.02 89.99 Volume: 293.02 Matrix:-1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.007 MONOCLINIC I-lattice R(int) = 0.139 [ 483] Vol = 293.0 Cell: 5.917 5.917 8.370 89.98 90.01 90.00 Volume: 293.02 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.080 [ 345] Vol = 146.5 Cell: 5.917 5.917 5.917 60.01 90.00 60.01 Volume: 146.51 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 518 0 663 651 981 N (int>3sigma) = 0 0 0 0 518 0 546 534 805 Mean intensity = 0.0 0.0 0.0 0.0 28.9 0.0 59.3 60.3 62.9 Mean int/sigma = 0.0 0.0 0.0 0.0 20.4 0.0 23.1 23.3 23.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.179 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 80 220 N I>3s 5 5 32 220 1.2 1.2 0.7 33.6 5.4 5.4 3.2 25.0 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 0.238 770 Fd-3m 1 1 227 C N N N N 37 2284 0.244 806 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367803 8.370207 8.367132 90.0036 89.9990 89.9781 ZERR 1.00 0.002403 0.003872 0.000401 0.0150 0.0002 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4417514- 986291 269 264 26 10.2 1818177.22 82.14 0.011 0.012 952997- 181832 323 321 26 12.3 305616.28 41.33 0.018 0.020 167206- 94385 284 284 26 10.9 131689.45 17.83 0.026 0.033 61423- 1820 288 287 29 9.9 7647.17 4.84 0.102 0.130 ------------------------------------------------------------------------------------------- 4417514- 1820 1164 1156 107 10.8 534339.23 35.82 0.013 0.015 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.01 283 276 26 10.6 776501.27 59.49 0.012 0.011 0.011 1.01-0.78 344 343 26 13.2 577024.72 35.81 0.013 0.015 0.017 0.78-0.66 289 289 26 11.1 481651.80 28.52 0.013 0.016 0.023 0.65-0.59 248 248 29 8.6 267197.39 17.98 0.019 0.022 0.032 ------------------------------------------------------------------------------------------------------ inf-0.59 1164 1156 107 10.8 534339.23 35.82 0.013 0.015 0.018 inf-0.60 1108 1100 97 11.3 549543.33 36.75 0.013 0.014 0.017 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.01 276 28 26 92.9 10.6 776501.27 201.98 0.012 0.003 1.01-0.78 343 26 26 100.0 13.2 577024.72 134.53 0.013 0.005 0.78-0.66 289 26 26 100.0 11.1 481651.80 102.36 0.013 0.008 0.65-0.59 248 30 29 96.7 8.6 267197.39 58.91 0.019 0.012 -------------------------------------------------------------------------------------------- inf-0.59 1156 110 107 97.3 10.8 534339.23 126.37 0.013 0.006 inf-0.60 1100 99 97 98.0 11.3 549543.33 130.34 0.013 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:00:16 2018) ID: 2932; threads 39; handles 877; mem 518988.00 (1237724.00)kB; time: 1w 5d 22h 5m 46s MEMORY INFO: Memory PF:2.0, Ph:173.0, V:1208.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:506.8,peak PF: 708.5, WS: 271.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:4.0, Ph:173.0, V:1210.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:508.6,peak PF: 708.5, WS: 272.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:00:16 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000020 ) 0.087412 -0.166882 0.063604 ( 0.000012 0.000014 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000017 0.000019 0.000018 ) 5.91535 ( 0.00098 ) 5.92288 ( 0.00074 ) 5.91286 ( 0.00100 ) 59.95509 ( 0.01525 ) 89.89521 ( 0.01366 ) 59.99590 ( 0.01515 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:00:16 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000020 ) 0.087412 -0.166882 0.063604 ( 0.000012 0.000014 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.021557 -0.014367 0.007181 ( 0.000005 0.000003 0.000004 ) -0.014367 0.028724 -0.014356 ( 0.000003 0.000005 0.000004 ) 0.007181 -0.014356 0.021546 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9154(10) 5.9229(7) 5.9129(10) 59.955(15) 89.895(14) 59.996(15) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb PROFFITPEAK info: 1256 peaks in the peak location table UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) 605 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 90 | 1.141 ( 0.051) | 1.250 ( 0.224) | 1.368 ( 0.607) | 13.2-19.3 | 90 | 1.148 ( 0.108) | 1.238 ( 0.333) | 1.378 ( 0.755) | 19.3-23.5 | 90 | 1.156 ( 0.090) | 1.244 ( 0.292) | 1.224 ( 0.523) | 23.6-27.6 | 90 | 1.144 ( 0.093) | 1.215 ( 0.372) | 1.261 ( 0.547) | 27.6-30.8 | 90 | 1.133 ( 0.110) | 1.192 ( 0.214) | 1.188 ( 0.397) | 30.9-34.3 | 90 | 1.147 ( 0.077) | 1.197 ( 0.261) | 1.159 ( 0.386) | 34.3-37.3 | 90 | 1.136 ( 0.106) | 1.126 ( 0.164) | 1.154 ( 0.394) | 37.3-40.1 | 90 | 1.143 ( 0.125) | 1.142 ( 0.221) | 1.281 ( 0.581) | 40.1-43.1 | 90 | 1.153 ( 0.116) | 1.124 ( 0.215) | 1.238 ( 0.629) | 43.2-49.8 | 88 | 1.202 ( 0.159) | 1.147 ( 0.260) | 1.184 ( 0.479) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 898 | 1.150 ( 0.108) | 1.188 ( 0.266) | 1.244 ( 0.547) | Fitted profile normalization line parameters e1 dimension: a=0.0016 b=0.98 e2 dimension: a=-0.0016 b=1.04 e3 dimension: a=-0.0036 b=1.15 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 453201 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 2567504 PROFFITPEAK - Finished at Wed Mar 28 13:00:23 2018 PROFFITMAIN - Started at Wed Mar 28 13:00:23 2018 OTKP changes: 898 1 1 2 OTKP changes: 898 1 1 2 UB - matrix: -0.104168 -0.015105 0.049741 ( 0.000018 0.000020 0.000019 ) 0.087390 -0.167228 0.063737 ( 0.000012 0.000013 0.000012 ) 0.055475 -0.024296 0.122677 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.021565 -0.014388 0.007194 ( 0.000005 0.000003 0.000003 ) -0.014388 0.028784 -0.014390 ( 0.000003 0.000005 0.000003 ) 0.007194 -0.014390 0.021586 ( 0.000003 0.000003 0.000005 ) UB fit with 898 obs out of 898 (total:898,skipped:0) (100.00%) unit cell: 5.9164(9) 5.9129(7) 5.9126(9) 60.007(14) 90.002(13) 59.990(14) V = 146.25(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104031 -0.015244 0.049808 ( 0.000025 0.000031 0.000027 ) 0.087368 -0.167038 0.063649 ( 0.000017 0.000021 0.000019 ) 0.055413 -0.024128 0.122513 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021526 -0.014345 0.007168 ( 0.000006 0.000005 0.000005 ) -0.014345 0.028716 -0.014347 ( 0.000005 0.000007 0.000005 ) 0.007168 -0.014347 0.021541 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9190(13) 5.9159(10) 5.9163(13) 60.03(2) 90.004(18) 60.02(2) V = 146.58(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104070 -0.015237 0.049879 ( 0.000024 0.000031 0.000027 ) 0.087412 -0.167221 0.063746 ( 0.000017 0.000021 0.000019 ) 0.055497 -0.024199 0.122598 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021551 -0.014374 0.007185 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028781 -0.014386 ( 0.000005 0.000007 0.000005 ) 0.007185 -0.014386 0.021582 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9166(13) 5.9118(10) 5.9128(13) 60.00(2) 89.999(18) 60.01(2) V = 146.27(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.914) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104070 -0.015237 0.049879 ( 0.000024 0.000031 0.000027 ) 0.087412 -0.167221 0.063746 ( 0.000017 0.000021 0.000019 ) 0.055497 -0.024199 0.122598 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021551 -0.014374 0.007185 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028781 -0.014386 ( 0.000005 0.000007 0.000005 ) 0.007185 -0.014386 0.021582 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9166(13) 5.9118(10) 5.9128(13) 60.00(2) 89.999(18) 60.01(2) V = 146.27(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104070 -0.015237 0.049879 ( 0.000024 0.000031 0.000027 ) 0.087412 -0.167221 0.063746 ( 0.000017 0.000021 0.000019 ) 0.055497 -0.024199 0.122598 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021551 -0.014374 0.007185 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028781 -0.014386 ( 0.000005 0.000007 0.000005 ) 0.007185 -0.014386 0.021582 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9166(13) 5.9118(10) 5.9128(13) 60.00(2) 89.999(18) 60.01(2) V = 146.27(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104165 -0.015102 0.049686 ( 0.000018 0.000021 0.000020 ) 0.087335 -0.167068 0.063640 ( 0.000013 0.000014 0.000013 ) 0.055462 -0.024289 0.122616 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.021554 -0.014365 0.007183 ( 0.000005 0.000003 0.000003 ) -0.014365 0.028730 -0.014361 ( 0.000003 0.000005 0.000003 ) 0.007183 -0.014361 0.021554 ( 0.000003 0.000003 0.000005 ) UB fit with 898 obs out of 898 (total:898,skipped:0) (100.00%) unit cell: 5.9167(10) 5.9165(7) 5.9159(10) 60.019(15) 90.010(13) 60.005(15) V = 146.48(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 28 reflections under beam stop or inside a detector rejection region 7 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof 1218 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:00:25 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.914) PROFFIT INFO: signal sum: min=168.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=589.8818 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=838 PROFFIT INFO: Inet: min=1287.0148 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.04 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 15 80 149 255 279 460 800 1089 1218 Percent 0.0 0.0 1.2 6.6 12.2 20.9 22.9 37.8 65.7 89.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1218 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 1218 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1754000 121 2539583.61 139.82 100.00 1741262- 1160174 121 1430090.49 112.63 100.00 1151211- 345581 121 657292.67 94.08 100.00 344246- 233963 121 276661.74 73.78 100.00 232815- 182204 121 208782.56 52.69 100.00 181747- 150499 121 163538.23 38.04 100.00 150233- 110629 121 131630.21 31.29 100.00 110585- 6968 121 67313.75 22.17 100.00 6956- 4104 121 5141.74 4.70 85.12 4093- 1287 129 3144.67 3.64 51.94 ------------------------------------------------------------------------------------ 4887974- 1287 1218 544737.19 56.93 93.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 121 696958.21 89.64 99.17 1.24- 0.96 121 864846.97 76.65 98.35 0.96- 0.81 121 582579.45 59.01 99.17 0.81- 0.72 121 715020.88 71.62 97.52 0.70- 0.64 121 541673.31 57.67 94.21 0.64- 0.58 121 557269.64 57.06 95.87 0.58- 0.54 121 442892.82 46.17 95.87 0.54- 0.50 121 387792.74 39.74 80.17 0.50- 0.47 121 368212.90 39.46 89.26 0.47- 0.40 129 305914.88 33.81 85.27 ------------------------------------------------------------------------------------ 5.26- 0.40 1218 544737.19 56.93 93.43 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:00:25 2018 Sorting 1218 observations 247 unique observations with > 7.00 F2/sig(F2) 1218 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 108 215 Total number of frames 215 Maximum number of 247 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1218 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 108 215 Total number of frames 215 Frame #8 of 215 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 981 observations > 7.00 F2/sig(F2) 981 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 108 215 Total number of frames 215 Frame #8 of 215 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: 3.9 (Out of 981 removed 42 = 939, unique = 243) 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 939 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 108 215 Total number of frames 215 Frame #8 of 215 skipped from refinement Frame #119 of 215 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 243 unique data precomputed (should be 243) 243 unique data with 939 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.9 (Out of 939 removed 0 = 939, unique = 243) 243 unique data precomputed (should be 243) 243 unique data with 939 observations RMS deviation of equivalent data = 0.64202 Rint = 0.56368 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.53015, wR= 2.45494 Trying model 1 (ne=2, no=0)... Results: Rint= 0.75346, wR= 2.04417, Acormin=-0.188, Acormax=1.643, Acor_av=0.342 F test: Probability=0.000, F= 0.491 Trying model 2 (ne=2, no=1)... Results: Rint= 0.74631, wR= 2.58955, Acormin=-0.735, Acormax=1.179, Acor_av=0.018 F test: Probability=0.000, F= 0.499 Trying model 3 (ne=4, no=0)... Results: Rint= 0.85577, wR= 1.80581, Acormin=-0.301, Acormax=1.573, Acor_av=0.150 F test: Probability=0.000, F= 0.376 Trying model 4 (ne=4, no=1)... Results: Rint= 0.79962, wR= 2.11294, Acormin=-0.673, Acormax=0.991, Acor_av=0.004 F test: Probability=0.000, F= 0.429 Trying model 5 (ne=4, no=3)... Results: Rint= 0.81475, wR= 1.89792, Acormin=-0.555, Acormax=1.090, Acor_av=0.007 F test: Probability=0.000, F= 0.409 Trying model 6 (ne=6, no=0)... Results: Rint= 0.90086, wR= 1.57792, Acormin=-0.369, Acormax=1.323, Acor_av=0.066 F test: Probability=0.000, F= 0.333 Trying model 7 (ne=6, no=1)... Results: Rint= 0.84781, wR= 1.74882, Acormin=-0.436, Acormax=1.123, Acor_av=0.003 F test: Probability=0.000, F= 0.374 Trying model 8 (ne=6, no=3)... Results: Rint= 0.88718, wR= 1.50560, Acormin=-0.371, Acormax=0.819, Acor_av=-0.001 F test: Probability=0.000, F= 0.338 Trying model 9 (ne=6, no=5)... Results: Rint= 0.93313, wR= 1.44641, Acormin=-0.250, Acormax=0.343, Acor_av=0.003 F test: Probability=0.000, F= 0.300 Trying model 10 (ne=8, no=0)... Results: Rint= 0.89367, wR= 1.52352, Acormin=-0.303, Acormax=1.101, Acor_av=0.022 F test: Probability=0.000, F= 0.329 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87660, wR= 1.45185, Acormin=-0.273, Acormax=1.028, Acor_av=0.012 F test: Probability=0.000, F= 0.341 Trying model 12 (ne=8, no=3)... Results: Rint= 0.90175, wR= 1.63836, Acormin=-0.054, Acormax=0.067, Acor_av=0.001 F test: Probability=0.000, F= 0.319 Trying model 13 (ne=8, no=5)... Results: Rint= 0.80933, wR= 1.21081, Acormin=-0.041, Acormax=0.050, Acor_av=0.002 F test: Probability=0.000, F= 0.389 Trying model 14 (ne=8, no=7)... Results: Rint= 0.80915, wR= 1.24723, Acormin=-0.015, Acormax=0.051, Acor_av=0.002 F test: Probability=0.000, F= 0.380 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.74365 There are 213 active scales (one needs to be fixed) Refinement control: frame scale #149 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 217 pars with 23653 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.64202 Using Levenberg-Marquardt: 0.00010 New wR= 0.60953 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.56368 with corrections 0.54325 Rint for all data: 0.74365 with corrections 0.72701 4 observations identified as outliers and rejected Cycle 2 wR= 0.60495 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= 0.59658 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.54371 with corrections 0.53130 Rint for all data: 0.74365 with corrections 0.73152 3 observations identified as outliers and rejected Cycle 3 wR= 0.57769 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57243 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52630 with corrections 0.52458 Rint for all data: 0.74365 with corrections 0.73812 2 observations identified as outliers and rejected Cycle 4 wR= 0.55375 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.55112 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52010 with corrections 0.52491 Rint for all data: 0.74365 with corrections 0.74456 3 observations identified as outliers and rejected Cycle 5 wR= 0.54129 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.53949 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51769 with corrections 0.52811 Rint for all data: 0.74365 with corrections 0.74998 1 observations identified as outliers and rejected Final wR= 0.53949 Final frame scales: Min= 0.5437 Max= 2.3700 Final absorption correction factors: Amin= 0.3949 Amax= 1.9083 PROFFIT INFO: Inet (after scale3 abspack): min=1020.6489 max=6707535.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=142.0052 max=115295.3750 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:2/109 1218 reflections read from tmp file 922 reflections are rejected (818 as outliers, 104 as groups of 1 refl) Redundancy: 1 2 3 4 5+ Number of groups: 0 84 26 10 2 Initial Chi^2= 0.85918 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.46965 Current error model SIG(F2)^2 = 457.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 214.67*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 214.67*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6707536- 1516300 121 2450012.13 91.09 100.00 1513478- 993161 121 1239574.67 51.07 100.00 991158- 345354 121 618667.23 47.60 100.00 344598- 222443 121 267936.82 32.54 100.00 222422- 174218 121 196289.03 23.88 100.00 174124- 139001 121 156534.57 17.88 100.00 138022- 106413 121 121537.53 15.83 100.00 106210- 8309 121 62443.57 12.09 95.87 8237- 3572 121 5206.26 3.31 50.41 3568- 1021 129 2635.74 2.89 34.11 ------------------------------------------------------------------------------------ 6707536- 1021 1218 508737.63 29.64 87.68 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 121 813530.68 62.03 99.17 1.24- 0.96 121 801545.91 45.37 98.35 0.96- 0.81 121 521336.10 31.28 96.69 0.81- 0.72 121 633380.88 33.55 94.21 0.70- 0.64 121 449214.97 26.21 85.95 0.64- 0.58 121 477437.21 25.87 89.26 0.58- 0.54 121 391682.14 21.09 85.95 0.54- 0.50 121 359871.95 18.27 71.90 0.50- 0.47 121 358011.69 18.09 80.17 0.47- 0.40 129 295465.36 15.59 75.97 ------------------------------------------------------------------------------------ 5.26- 0.40 1218 508737.63 29.64 87.68 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 121 813530.68 62.03 99.17 5.26- 0.96 242 807538.29 53.70 98.76 5.26- 0.81 363 712137.56 46.23 98.07 5.26- 0.72 484 692448.39 43.06 97.11 5.26- 0.64 605 643801.71 39.69 94.88 5.26- 0.58 726 616074.29 37.39 93.94 5.26- 0.54 847 584018.27 35.06 92.80 5.26- 0.50 968 555999.98 32.96 90.19 5.26- 0.47 1089 534001.28 31.31 89.07 5.26- 0.40 1218 508737.63 29.64 87.68 ------------------------------------------------------------------------------------ 5.26- 0.40 1218 508737.63 29.64 87.68 Scale applied to data: s=0.149086 (maximum obs:6707535.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.750; Rsigma 0.022: data 1218 -> merged 304 With outlier rejection... Rint 0.614; Rsigma 0.023: data 1046 -> merged 304 Rejected total: 172, method kkm 168, method Blessing 4 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404294, 5.271355 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 4.07 100.00 61 1.46 - 1.12 15 15 4.67 100.00 70 1.08 - 0.96 15 15 4.87 100.00 73 0.96 - 0.86 15 15 5.00 100.00 75 0.86 - 0.79 15 15 3.87 100.00 58 0.79 - 0.73 13 15 3.77 86.67 49 0.73 - 0.69 15 15 3.07 100.00 46 0.69 - 0.65 14 15 4.07 93.33 57 0.65 - 0.63 12 15 3.25 80.00 39 0.63 - 0.60 21 21 3.33 100.00 70 --------------------------------------------------------------- 5.92 - 0.60 150 156 3.99 96.15 598 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:00:25 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916711 5.916502 5.915935 60.0185 90.0101 60.0046 1046 Reflections read from file xs1715a.hkl; mean (I/sigma) = 28.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 515 549 512 531 788 717 690 1046 N (int>3sigma) = 0 435 549 432 450 708 628 601 909 Mean intensity = 0.0 55.3 31.0 56.5 67.1 47.2 65.0 66.3 67.0 Mean int/sigma = 0.0 25.6 24.5 26.2 27.6 25.4 27.6 28.3 28.3 Lattice type: P chosen Volume: 146.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.916 5.917 5.917 120.00 90.01 119.98 Niggli form: a.a = 34.998 b.b = 35.005 c.c = 35.007 b.c = -17.501 a.c = -0.006 a.b = -17.491 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.021 CUBIC F-lattice R(int) = 0.200 [ 894] Vol = 585.9 Cell: 8.366 8.369 8.368 89.99 89.99 90.01 Volume: 585.90 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 660] Vol = 439.4 Cell: 5.917 5.916 14.494 90.00 90.01 119.98 Volume: 439.43 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.151 [ 207] Vol = 439.4 Trigonal Cell: 5.917 5.916 14.494 90.00 90.01 119.98 Volume: 439.43 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.022 TETRAGONAL I-lattice R(int) = 0.161 [ 700] Vol = 293.0 Cell: 5.918 5.917 8.366 89.99 90.00 90.01 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.020 TETRAGONAL I-lattice R(int) = 0.161 [ 700] Vol = 293.0 Cell: 5.918 5.917 8.366 89.99 90.00 90.01 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 661] Vol = 293.0 Cell: 5.918 8.366 5.917 89.99 89.99 90.00 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.100 [ 487] Vol = 293.0 Cell: 8.366 5.918 5.917 90.01 90.01 90.00 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.013 MONOCLINIC C-lattice R(int) = 0.129 [ 514] Vol = 293.0 Cell: 8.366 8.369 5.916 89.99 134.99 90.01 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 381] Vol = 146.5 Cell: 5.916 5.917 5.917 120.00 90.01 119.98 Volume: 146.48 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 549 0 690 688 1046 N (int>3sigma) = 0 0 0 0 549 0 596 600 909 Mean intensity = 0.0 0.0 0.0 0.0 31.0 0.0 69.1 65.3 67.0 Mean int/sigma = 0.0 0.0 0.0 0.0 24.5 0.0 29.0 27.9 28.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.171 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 87 232 N I>3s 5 5 59 232 1.0 1.0 0.7 36.2 6.4 6.4 3.9 29.9 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 0.199 827 Fd-3m 1 1 227 C N N N N 37 2284 0.202 864 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366207 8.369381 8.367682 89.9917 89.9925 90.0082 ZERR 1.00 0.000399 0.003843 0.002357 0.0003 0.0002 0.0150 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 6625651- 1114727 126 111 30 3.7 1503122.47 65.99 0.469 0.329 1101474- 829868 112 91 30 3.0 844274.83 42.03 0.675 0.519 822294- 612628 136 117 30 3.9 619970.03 33.77 0.793 0.711 592651- 468985 171 150 30 5.0 405502.11 28.88 0.859 0.878 456708- 318103 141 114 30 3.8 318219.06 28.47 0.704 0.638 317847- 171185 129 105 30 3.5 211471.70 24.51 0.375 0.313 170750- 131272 121 107 30 3.6 145516.27 17.49 0.258 0.192 130979- 104321 93 81 30 2.7 115521.36 14.00 0.356 0.251 103063- 58985 101 88 30 2.9 86408.98 10.44 0.635 0.516 58498- 1179 88 82 34 2.4 24156.05 5.34 0.891 0.862 ------------------------------------------------------------------------------------------- 6625651- 1179 1218 1046 304 3.4 449360.59 28.31 0.614 0.491 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 159 131 30 4.4 683722.77 56.43 0.617 0.499 0.012 1.08-0.86 167 150 31 4.8 641422.21 37.44 0.779 0.636 0.017 0.83-0.72 141 117 32 3.7 502214.94 30.89 0.565 0.437 0.020 0.72-0.64 137 112 30 3.7 373177.23 24.88 0.607 0.494 0.026 0.64-0.59 112 97 31 3.1 480372.80 26.13 0.553 0.535 0.026 0.59-0.55 123 101 31 3.3 304955.18 18.67 0.628 0.562 0.034 0.54-0.51 114 106 31 3.4 328659.48 18.84 0.787 0.717 0.032 0.51-0.48 114 98 31 3.2 295980.42 15.73 0.508 0.355 0.037 0.48-0.45 93 82 30 2.7 320698.41 17.10 0.347 0.286 0.037 0.45-0.40 58 52 27 1.9 310716.72 16.19 0.118 0.089 0.041 ------------------------------------------------------------------------------------------------------ inf-0.40 1218 1046 304 3.4 449360.59 28.31 0.614 0.491 0.023 inf-0.60 703 598 150 4.0 548232.61 36.25 0.653 0.538 0.018 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 131 30 30 100.0 4.4 683722.77 140.10 0.617 0.007 1.08-0.86 150 31 31 100.0 4.8 641422.21 107.33 0.779 0.010 0.83-0.72 117 34 32 94.1 3.7 502214.94 72.69 0.565 0.012 0.72-0.64 112 33 30 90.9 3.7 373177.23 60.05 0.607 0.016 0.64-0.59 97 32 31 96.9 3.1 480372.80 59.47 0.553 0.016 0.59-0.55 101 40 31 77.5 3.3 304955.18 41.33 0.628 0.021 0.54-0.51 106 41 31 75.6 3.4 328659.48 45.02 0.787 0.021 0.51-0.48 98 45 31 68.9 3.2 295980.42 33.00 0.508 0.022 0.48-0.45 82 63 30 47.6 2.7 320698.41 31.45 0.347 0.024 0.45-0.40 52 114 27 23.7 1.9 310716.72 24.62 0.118 0.029 -------------------------------------------------------------------------------------------- inf-0.40 1046 463 304 65.7 3.4 449360.59 68.35 0.614 0.015 inf-0.60 598 156 150 96.2 4.0 548232.61 92.05 0.653 0.011 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 No constraint UB - matrix: 0.034790 0.007551 0.076924 ( 0.000008 0.000010 0.000010 ) 0.008047 0.083534 -0.011848 ( 0.000006 0.000007 0.000007 ) -0.076895 0.012145 0.033576 ( 0.000007 0.000009 0.000009 ) M - matrix: 0.007188 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007182 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000001 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.034790 0.007551 0.076924 ( 0.000008 0.000010 0.000010 ) 0.008047 0.083534 -0.011848 ( 0.000006 0.000007 0.000007 ) -0.076895 0.012145 0.033576 ( 0.000007 0.000009 0.000009 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3662(8) 8.3694(7) 8.3679(9) 89.992(8) 89.992(8) 90.008(7) V = 585.92(10) unit cell: 8.3678(3) 8.3678(3) 8.3678(3) 90.0 90.0 90.0 V = 585.92(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.914) PROFFIT INFO: signal sum: min=168.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=589.8818 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=838 PROFFIT INFO: Inet: min=1287.0148 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.04 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 30 160 298 510 558 920 1600 2178 2436 Percent 0.0 0.0 1.2 6.6 12.2 20.9 22.9 37.8 65.7 89.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1218 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 1218 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1754000 121 2539583.61 139.82 100.00 1741262- 1160174 121 1430090.49 112.63 100.00 1151211- 345581 121 657292.67 94.08 100.00 344246- 233963 121 276661.74 73.78 100.00 232815- 182204 121 208782.56 52.69 100.00 181747- 150499 121 163538.23 38.04 100.00 150233- 110629 121 131630.21 31.29 100.00 110585- 6968 121 67313.75 22.17 100.00 6956- 4104 121 5141.74 4.70 85.12 4093- 1287 129 3144.67 3.64 51.94 ------------------------------------------------------------------------------------ 4887974- 1287 1218 544737.19 56.93 93.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 121 753183.42 83.73 98.35 1.32- 1.09 121 1002378.91 81.55 100.00 1.09- 0.96 121 599501.17 69.49 100.00 0.96- 0.85 121 646076.00 70.89 96.69 0.85- 0.80 121 622931.84 65.33 98.35 0.80- 0.73 121 414940.25 45.92 95.87 0.73- 0.70 121 302805.16 36.47 92.56 0.70- 0.65 121 557108.05 53.37 92.56 0.65- 0.62 121 284184.63 32.49 80.17 0.62- 0.58 129 281656.25 31.73 80.62 ------------------------------------------------------------------------------------ 4.82- 0.58 1218 544737.19 56.93 93.43 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:00:26 2018 Sorting 1218 observations 83 unique observations with > 7.00 F2/sig(F2) 1218 observations in 2 runs Run # start # end # total # 1 1 107 107 2 1 108 215 Total number of frames 215 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1218 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 36 73 Total number of frames 73 981 observations > 7.00 F2/sig(F2) 981 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 36 73 Total number of frames 73 Removing 'redundancy=1' reflections Average redundancy: 11.5 (Out of 981 removed 5 = 976, 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): 4/m3bar2/m 976 observations in 2 runs Run # start # end # total # 1 0 35 36 2 0 36 73 Total number of frames 73 85 unique data precomputed (should be 85) 85 unique data with 976 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 11.5 (Out of 976 removed 0 = 976, unique = 85) 85 unique data precomputed (should be 85) 85 unique data with 976 observations RMS deviation of equivalent data = 0.13167 Rint = 0.09152 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.08988, wR= 0.12935 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06078, wR= 0.08024, Acormin=0.670, Acormax=1.140, Acor_av=0.810 F test: Probability=1.000, F= 2.175 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04554, wR= 0.06106, Acormin=0.614, Acormax=1.249, Acor_av=0.851 F test: Probability=1.000, F= 1.775 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04765, wR= 0.06476, Acormin=0.639, Acormax=1.153, Acor_av=0.787 F test: Probability=0.000, F= 0.907 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03873, wR= 0.05429, Acormin=0.645, Acormax=1.251, Acor_av=0.855 F test: Probability=1.000, F= 1.368 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03610, wR= 0.04789, Acormin=0.601, Acormax=1.132, Acor_av=0.807 F test: Probability=0.975, F= 1.142 Trying model 6 (ne=6, no=0)... Results: Rint= 0.03952, wR= 0.05204, Acormin=0.655, Acormax=1.124, Acor_av=0.805 F test: Probability=0.000, F= 0.831 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03231, wR= 0.04495, Acormin=0.675, Acormax=1.205, Acor_av=0.845 F test: Probability=0.999, F= 1.240 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02885, wR= 0.03801, Acormin=0.655, Acormax=1.248, Acor_av=0.865 F test: Probability=0.999, F= 1.243 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02777, wR= 0.03629, Acormin=0.646, Acormax=1.249, Acor_av=0.870 F test: Probability=0.822, F= 1.066 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03599, wR= 0.04807, Acormin=0.635, Acormax=1.134, Acor_av=0.823 F test: Probability=0.000, F= 0.637 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02985, wR= 0.04092, Acormin=0.663, Acormax=1.220, Acor_av=0.854 F test: Probability=0.000, F= 0.923 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02718, wR= 0.03410, Acormin=0.643, Acormax=1.272, Acor_av=0.881 F test: Probability=0.925, F= 1.104 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02518, wR= 0.03199, Acormin=0.656, Acormax=1.323, Acor_av=0.891 F test: Probability=1.000, F= 1.270 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02241, wR= 0.02882, Acormin=0.661, Acormax=1.360, Acor_av=0.907 F test: Probability=0.999, F= 1.240 Final absorption model (ne=8, no=7): Rint= 0.02241, Acormin=0.661, Acormax=1.360, Acor_av=0.907 Combined refinement in use Rint: 0.09166 There are 73 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 152 pars with 11628 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13167 Using Levenberg-Marquardt: 0.00010 New wR= 0.02291 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09152 with corrections 0.01551 Rint for all data: 0.09166 with corrections 0.01574 0 observations identified as outliers and rejected Cycle 2 wR= 0.02291 Using Levenberg-Marquardt: 0.00001 New wR= 0.02039 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09152 with corrections 0.01410 Rint for all data: 0.09166 with corrections 0.01433 0 observations identified as outliers and rejected Cycle 3 wR= 0.02039 Using Levenberg-Marquardt: 0.00000 New wR= 0.01991 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09152 with corrections 0.01367 Rint for all data: 0.09166 with corrections 0.01390 0 observations identified as outliers and rejected Cycle 4 wR= 0.01991 Using Levenberg-Marquardt: 0.00000 New wR= 0.01987 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09152 with corrections 0.01360 Rint for all data: 0.09166 with corrections 0.01383 0 observations identified as outliers and rejected Cycle 5 wR= 0.01987 Using Levenberg-Marquardt: 0.00000 New wR= 0.01987 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09152 with corrections 0.01362 Rint for all data: 0.09166 with corrections 0.01385 Final wR= 0.01987 Final frame scales: Min= 0.9245 Max= 1.1102 Final absorption correction factors: Amin= 0.4881 Amax= 1.2763 PROFFIT INFO: Inet (after scale3 abspack): min=1380.5791 max=4449170.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=294.3279 max=66997.4453 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:2/109 1218 reflections read from tmp file 30 reflections are rejected (27 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 7 9 2 5 8 0 7 65 Initial Chi^2= 0.27057 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.11208 Current error model SIG(F2)^2 = 126.10*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 140.23*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 140.23*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4449170- 1691451 121 2534596.19 119.70 100.00 1687439- 1113810 121 1387954.11 61.48 100.00 1113310- 372792 121 668561.16 60.13 100.00 338903- 231830 121 273417.20 39.82 100.00 231099- 193482 121 211173.51 28.44 100.00 190924- 143516 121 157862.08 20.72 100.00 143260- 114196 121 128339.30 18.18 100.00 113557- 6839 121 67652.48 13.11 100.00 6803- 4017 121 5051.03 4.06 89.26 4017- 1381 129 3123.79 3.32 55.81 ------------------------------------------------------------------------------------ 4449170- 1381 1218 540222.02 36.68 94.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 121 778279.94 72.00 99.17 1.32- 1.09 121 1024514.13 64.82 100.00 1.09- 0.96 121 601804.16 41.51 100.00 0.96- 0.85 121 639007.41 39.62 99.17 0.85- 0.80 121 609445.82 36.53 98.35 0.80- 0.73 121 399894.24 25.99 95.04 0.73- 0.70 121 297884.00 20.86 92.56 0.70- 0.65 121 528909.06 29.89 93.39 0.65- 0.62 121 271538.54 18.62 80.17 0.62- 0.58 129 268882.68 18.15 85.27 ------------------------------------------------------------------------------------ 4.82- 0.58 1218 540222.02 36.68 94.25 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 121 778279.94 72.00 99.17 4.82- 1.09 242 901397.03 68.41 99.59 4.82- 0.96 363 801532.74 59.44 99.72 4.82- 0.85 484 760901.41 54.49 99.59 4.82- 0.80 605 730610.29 50.89 99.34 4.82- 0.73 726 675490.95 46.74 98.62 4.82- 0.70 847 621547.10 43.05 97.76 4.82- 0.65 968 609967.34 41.40 97.21 4.82- 0.62 1089 572364.14 38.87 95.32 4.82- 0.58 1218 540222.02 36.68 94.25 ------------------------------------------------------------------------------------ 4.82- 0.58 1218 540222.02 36.68 94.25 Scale applied to data: s=0.224761 (maximum obs:4449170.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.017: data 1218 -> merged 107 With outlier rejection... Rint 0.013; Rsigma 0.018: data 1209 -> merged 107 Rejected total: 9, method kkm 9, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585864, 4.831162 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 6.50 80.00 52 1.61 - 1.21 10 10 10.30 100.00 103 1.17 - 1.01 10 10 14.40 100.00 144 0.99 - 0.89 10 10 14.40 100.00 144 0.88 - 0.81 10 10 14.00 100.00 140 0.81 - 0.74 10 10 12.30 100.00 123 0.73 - 0.71 10 10 13.20 100.00 132 0.70 - 0.66 10 10 10.90 100.00 109 0.66 - 0.64 10 10 10.30 100.00 103 0.63 - 0.60 10 10 10.30 100.00 103 --------------------------------------------------------------- 5.92 - 0.60 98 100 11.77 98.00 1153 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:00:25 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916711 5.916502 5.915935 60.0185 90.0101 60.0046 1046 Reflections read from file xs1715a.hkl; mean (I/sigma) = 28.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 515 549 512 531 788 717 690 1046 N (int>3sigma) = 0 435 549 432 450 708 628 601 909 Mean intensity = 0.0 55.3 31.0 56.5 67.1 47.2 65.0 66.3 67.0 Mean int/sigma = 0.0 25.6 24.5 26.2 27.6 25.4 27.6 28.3 28.3 Lattice type: P chosen Volume: 146.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.916 5.917 5.917 120.00 90.01 119.98 Niggli form: a.a = 34.998 b.b = 35.005 c.c = 35.007 b.c = -17.501 a.c = -0.006 a.b = -17.491 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.021 CUBIC F-lattice R(int) = 0.200 [ 894] Vol = 585.9 Cell: 8.366 8.369 8.368 89.99 89.99 90.01 Volume: 585.90 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 660] Vol = 439.4 Cell: 5.917 5.916 14.494 90.00 90.01 119.98 Volume: 439.43 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.151 [ 207] Vol = 439.4 Trigonal Cell: 5.917 5.916 14.494 90.00 90.01 119.98 Volume: 439.43 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.022 TETRAGONAL I-lattice R(int) = 0.161 [ 700] Vol = 293.0 Cell: 5.918 5.917 8.366 89.99 90.00 90.01 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.020 TETRAGONAL I-lattice R(int) = 0.161 [ 700] Vol = 293.0 Cell: 5.918 5.917 8.366 89.99 90.00 90.01 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 661] Vol = 293.0 Cell: 5.918 8.366 5.917 89.99 89.99 90.00 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.100 [ 487] Vol = 293.0 Cell: 8.366 5.918 5.917 90.01 90.01 90.00 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.013 MONOCLINIC C-lattice R(int) = 0.129 [ 514] Vol = 293.0 Cell: 8.366 8.369 5.916 89.99 134.99 90.01 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 381] Vol = 146.5 Cell: 5.916 5.917 5.917 120.00 90.01 119.98 Volume: 146.48 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 549 0 690 688 1046 N (int>3sigma) = 0 0 0 0 549 0 596 600 909 Mean intensity = 0.0 0.0 0.0 0.0 31.0 0.0 69.1 65.3 67.0 Mean int/sigma = 0.0 0.0 0.0 0.0 24.5 0.0 29.0 27.9 28.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.171 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 87 232 N I>3s 5 5 59 232 1.0 1.0 0.7 36.2 6.4 6.4 3.9 29.9 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 0.199 827 Fd-3m 1 1 227 C N N N N 37 2284 0.202 864 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366207 8.369381 8.367682 89.9917 89.9925 90.0082 ZERR 1.00 0.000399 0.003843 0.002357 0.0003 0.0002 0.0150 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4404169- 980220 278 274 26 10.5 1821632.32 83.13 0.011 0.012 952099- 181158 342 340 26 13.1 305471.74 41.40 0.018 0.020 167025- 94098 296 296 26 11.4 130886.25 17.86 0.027 0.033 61186- 1802 302 299 29 10.3 7728.91 4.89 0.100 0.122 ------------------------------------------------------------------------------------------- 4404169- 1802 1218 1209 107 11.3 532705.48 36.06 0.013 0.015 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.01 305 297 27 11.0 757600.35 58.52 0.011 0.012 0.011 0.99-0.78 361 360 26 13.8 576848.87 36.18 0.013 0.015 0.017 0.76-0.65 315 315 27 11.7 456756.50 27.44 0.014 0.017 0.023 0.65-0.59 237 237 27 8.8 284766.79 19.22 0.018 0.021 0.032 ------------------------------------------------------------------------------------------------------ inf-0.59 1218 1209 107 11.3 532705.48 36.06 0.013 0.015 0.018 inf-0.60 1160 1151 97 11.9 547227.10 36.99 0.013 0.015 0.017 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.01 297 29 27 93.1 11.0 757600.35 204.37 0.011 0.003 0.99-0.78 360 26 26 100.0 13.8 576848.87 139.53 0.013 0.005 0.76-0.65 315 27 27 100.0 11.7 456756.50 100.68 0.014 0.008 0.65-0.59 237 27 27 100.0 8.8 284766.79 63.99 0.018 0.012 -------------------------------------------------------------------------------------------- inf-0.59 1209 109 107 98.2 11.3 532705.48 130.53 0.013 0.006 inf-0.60 1151 99 97 98.0 11.9 547227.10 134.54 0.013 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:05:30 2018) ID: 2932; threads 39; handles 878; mem 518916.00 (1237724.00)kB; time: 1w 5d 22h 11m 1s MEMORY INFO: Memory PF:3.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.8,peak PF: 708.5, WS: 271.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:5.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.6,peak PF: 708.5, WS: 272.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:05:30 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000020 ) 0.087412 -0.166882 0.063604 ( 0.000013 0.000014 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000018 0.000017 ) 5.91535 ( 0.00098 ) 5.92288 ( 0.00073 ) 5.91286 ( 0.00096 ) 59.95509 ( 0.01488 ) 89.89521 ( 0.01345 ) 59.99590 ( 0.01508 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:05:30 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000018 0.000021 0.000020 ) 0.087412 -0.166882 0.063604 ( 0.000013 0.000014 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.021554 -0.014365 0.007183 ( 0.000005 0.000003 0.000003 ) -0.014365 0.028730 -0.014361 ( 0.000003 0.000005 0.000003 ) 0.007183 -0.014361 0.021554 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(10) 5.9229(7) 5.9129(10) 59.955(15) 89.895(13) 59.996(15) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_3_1.rpb PROFFITPEAK info: 261 peaks in the peak location table UB fit with 134 obs out of 136 (total:136,skipped:0) (98.53%) UB - matrix: -0.104283 -0.014751 0.049336 ( 0.000090 0.000179 0.000305 ) 0.087105 -0.167076 0.063760 ( 0.000059 0.000116 0.000198 ) 0.055510 -0.024443 0.122579 ( 0.000091 0.000181 0.000309 ) M - matrix: 0.021544 -0.014372 0.007213 ( 0.000024 0.000026 0.000042 ) -0.014372 0.028729 -0.014377 ( 0.000026 0.000040 0.000042 ) 0.007213 -0.014377 0.021525 ( 0.000042 0.000042 0.000085 ) unit cell: 5.920(9) 5.920(8) 5.925(14) 59.99(19) 90.09(16) 60.03(15) V = 146.8(4) UB fit with 134 obs out of 136 (total:136,skipped:0) (98.53%) UB - matrix: -0.104283 -0.014751 0.049336 ( 0.000090 0.000179 0.000305 ) 0.087105 -0.167076 0.063760 ( 0.000059 0.000116 0.000198 ) 0.055510 -0.024443 0.122579 ( 0.000091 0.000181 0.000309 ) M - matrix: 0.021544 -0.014372 0.007213 ( 0.000024 0.000026 0.000042 ) -0.014372 0.028729 -0.014377 ( 0.000026 0.000040 0.000042 ) 0.007213 -0.014377 0.021525 ( 0.000042 0.000042 0.000085 ) unit cell: 5.920(9) 5.920(8) 5.925(14) 59.99(19) 90.09(16) 60.03(15) V = 146.8(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.104197 -0.014746 0.048925 ( 0.000092 0.000182 0.000308 ) 0.086991 -0.166971 0.063612 ( 0.000060 0.000119 0.000201 ) 0.055263 -0.024292 0.122562 ( 0.000091 0.000180 0.000305 ) M - matrix: 0.021478 -0.014331 0.007209 ( 0.000024 0.000026 0.000042 ) -0.014331 0.028687 -0.014320 ( 0.000026 0.000041 0.000043 ) 0.007209 -0.014320 0.021462 ( 0.000042 0.000043 0.000085 ) UB fit with 135 obs out of 136 (total:136,skipped:0) (99.26%) unit cell: 5.928(9) 5.916(8) 5.929(14) 60.11(19) 90.22(16) 60.09(15) V = 147.2(4) UB fit with 135 obs out of 136 (total:136,skipped:0) (99.26%) UB - matrix: -0.104197 -0.014746 0.048925 ( 0.000092 0.000182 0.000308 ) 0.086991 -0.166971 0.063612 ( 0.000060 0.000119 0.000201 ) 0.055263 -0.024292 0.122562 ( 0.000091 0.000180 0.000305 ) M - matrix: 0.021478 -0.014331 0.007209 ( 0.000024 0.000026 0.000042 ) -0.014331 0.028687 -0.014320 ( 0.000026 0.000041 0.000043 ) 0.007209 -0.014320 0.021462 ( 0.000042 0.000043 0.000085 ) unit cell: 5.928(9) 5.916(8) 5.929(14) 60.11(19) 90.22(16) 60.09(15) V = 147.2(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.104186 -0.014777 0.048887 ( 0.000091 0.000180 0.000307 ) 0.087007 -0.166985 0.063588 ( 0.000059 0.000117 0.000200 ) 0.055198 -0.024273 0.122594 ( 0.000091 0.000180 0.000306 ) M - matrix: 0.021472 -0.014329 0.007206 ( 0.000024 0.000026 0.000042 ) -0.014329 0.028692 -0.014316 ( 0.000026 0.000041 0.000043 ) 0.007206 -0.014316 0.021463 ( 0.000042 0.000043 0.000085 ) UB fit with 135 obs out of 136 (total:136,skipped:0) (99.26%) unit cell: 5.928(9) 5.914(8) 5.928(14) 60.12(19) 90.23(16) 60.09(15) V = 147.1(4) 136 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Run 3 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.000) HKL list info: 268 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104186 -0.014777 0.048887 ( 0.000091 0.000180 0.000307 ) 0.087007 -0.166985 0.063588 ( 0.000059 0.000117 0.000200 ) 0.055198 -0.024273 0.122594 ( 0.000091 0.000180 0.000306 ) M - matrix: 0.021472 -0.014329 0.007206 ( 0.000024 0.000026 0.000042 ) -0.014329 0.028692 -0.014316 ( 0.000026 0.000041 0.000043 ) 0.007206 -0.014316 0.021463 ( 0.000042 0.000043 0.000085 ) UB fit with 135 obs out of 136 (total:136,skipped:0) (99.26%) unit cell: 5.928(9) 5.914(8) 5.928(14) 60.12(19) 90.23(16) 60.09(15) V = 147.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 135 obs out of 136 (total:136,skipped:0) (99.26%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_1.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 101 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 101 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.47 | 10 | 1.026 ( 0.123) | 1.274 ( 0.768) | 1.570 ( 1.092) | 1.41- 1.17 | 10 | 1.158 ( 0.289) | 1.160 ( 0.291) | 1.355 ( 1.052) | 1.16- 0.98 | 10 | 1.095 ( 0.092) | 1.091 ( 0.091) | 1.066 ( 0.478) | 0.96- 0.89 | 10 | 1.150 ( 0.049) | 1.149 ( 0.086) | 1.004 ( 0.305) | 0.89- 0.84 | 10 | 1.143 ( 0.088) | 1.099 ( 0.092) | 1.054 ( 0.322) | 0.82- 0.76 | 10 | 1.215 ( 0.040) | 1.157 ( 0.089) | 1.177 ( 0.384) | 0.75- 0.72 | 10 | 1.168 ( 0.057) | 1.165 ( 0.120) | 0.925 ( 0.331) | 0.71- 0.67 | 10 | 1.230 ( 0.045) | 1.128 ( 0.100) | 1.385 ( 0.470) | 0.67- 0.64 | 10 | 1.200 ( 0.087) | 1.109 ( 0.073) | 1.452 ( 0.562) | 0.63- 0.60 | 11 | 1.277 ( 0.067) | 1.095 ( 0.105) | 1.546 ( 0.598) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.60 | 101 | 1.167 ( 0.135) | 1.142 ( 0.277) | 1.256 ( 0.662) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) UB - matrix: -0.104231 -0.015129 0.049365 ( 0.000039 0.000083 0.000138 ) 0.087312 -0.167100 0.063326 ( 0.000050 0.000107 0.000176 ) 0.054999 -0.024365 0.122979 ( 0.000055 0.000117 0.000194 ) M - matrix: 0.021512 -0.014353 0.007147 ( 0.000013 0.000017 0.000025 ) -0.014353 0.028745 -0.014325 ( 0.000017 0.000036 0.000034 ) 0.007147 -0.014325 0.021571 ( 0.000025 0.000034 0.000054 ) unit cell: 5.922(4) 5.908(6) 5.904(8) 60.12(13) 89.98(8) 59.96(9) V = 146.3(3) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 UB - matrix: -0.104293 -0.014933 0.049590 ( 0.000040 0.000085 0.000141 ) 0.087058 -0.166989 0.063696 ( 0.000044 0.000094 0.000155 ) 0.055467 -0.024296 0.122482 ( 0.000040 0.000085 0.000141 ) M - matrix: 0.021533 -0.014328 0.007167 ( 0.000012 0.000015 0.000022 ) -0.014328 0.028699 -0.014353 ( 0.000015 0.000032 0.000029 ) 0.007167 -0.014353 0.021518 ( 0.000022 0.000029 0.000042 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 5.915(4) 5.918(5) 5.923(6) 59.97(10) 90.00(7) 60.07(8) V = 146.7(2) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.000) HKL list info: 265 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104293 -0.014933 0.049590 ( 0.000040 0.000085 0.000141 ) 0.087058 -0.166989 0.063696 ( 0.000044 0.000094 0.000155 ) 0.055467 -0.024296 0.122482 ( 0.000040 0.000085 0.000141 ) M - matrix: 0.021533 -0.014328 0.007167 ( 0.000012 0.000015 0.000022 ) -0.014328 0.028699 -0.014353 ( 0.000015 0.000032 0.000029 ) 0.007167 -0.014353 0.021518 ( 0.000022 0.000029 0.000042 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 5.915(4) 5.918(5) 5.923(6) 59.97(10) 90.00(7) 60.07(8) V = 146.7(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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_1.rpb 2 of 101 peaks identified as outliers and rejected 99 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 99 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 99 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 10 | 1.008 ( 0.106) | 1.020 ( 0.109) | 1.286 ( 0.593) | 1.41- 1.12 | 10 | 1.055 ( 0.116) | 1.271 ( 0.555) | 0.989 ( 0.531) | 1.09- 0.96 | 10 | 1.113 ( 0.083) | 1.096 ( 0.080) | 1.039 ( 0.336) | 0.96- 0.84 | 10 | 1.151 ( 0.072) | 1.155 ( 0.083) | 0.984 ( 0.358) | 0.84- 0.81 | 10 | 1.155 ( 0.075) | 1.117 ( 0.088) | 1.150 ( 0.389) | 0.81- 0.73 | 10 | 1.187 ( 0.067) | 1.183 ( 0.111) | 1.022 ( 0.353) | 0.73- 0.71 | 10 | 1.203 ( 0.045) | 1.164 ( 0.134) | 0.966 ( 0.303) | 0.71- 0.67 | 10 | 1.243 ( 0.059) | 1.118 ( 0.071) | 1.457 ( 0.449) | 0.67- 0.62 | 10 | 1.204 ( 0.067) | 1.096 ( 0.064) | 1.651 ( 0.454) | 0.62- 0.60 | 9 | 1.289 ( 0.067) | 1.111 ( 0.115) | 1.563 ( 0.554) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.60 | 99 | 1.159 ( 0.112) | 1.133 ( 0.209) | 1.207 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 100 | 1.142 ( 0.050) | 1.238 ( 0.216) | 1.341 ( 0.593) | 13.1-19.3 | 100 | 1.143 ( 0.105) | 1.227 ( 0.319) | 1.380 ( 0.740) | 19.3-23.4 | 100 | 1.156 ( 0.091) | 1.229 ( 0.281) | 1.224 ( 0.509) | 23.5-27.6 | 100 | 1.145 ( 0.092) | 1.208 ( 0.356) | 1.227 ( 0.537) | 27.6-30.9 | 100 | 1.134 ( 0.109) | 1.188 ( 0.206) | 1.164 ( 0.394) | 30.9-34.2 | 100 | 1.147 ( 0.088) | 1.203 ( 0.304) | 1.176 ( 0.419) | 34.3-37.4 | 100 | 1.138 ( 0.101) | 1.130 ( 0.162) | 1.166 ( 0.393) | 37.4-40.1 | 100 | 1.152 ( 0.124) | 1.139 ( 0.213) | 1.296 ( 0.584) | 40.1-43.0 | 100 | 1.148 ( 0.122) | 1.116 ( 0.208) | 1.201 ( 0.617) | 43.0-49.8 | 97 | 1.207 ( 0.155) | 1.146 ( 0.250) | 1.225 ( 0.494) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 997 | 1.151 ( 0.109) | 1.182 ( 0.262) | 1.240 ( 0.543) | Fitted profile normalization line parameters e1 dimension: a=0.0016 b=0.97 e2 dimension: a=-0.0015 b=1.04 e3 dimension: a=-0.0031 b=1.14 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 453201 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 2567504 PROFFITPEAK - Finished at Wed Mar 28 13:05:38 2018 PROFFITMAIN - Started at Wed Mar 28 13:05:38 2018 OTKP changes: 997 2 2 3 OTKP changes: 997 2 2 3 UB - matrix: -0.104182 -0.015135 0.049795 ( 0.000015 0.000017 0.000018 ) 0.087411 -0.167293 0.063755 ( 0.000010 0.000012 0.000012 ) 0.055503 -0.024288 0.122709 ( 0.000013 0.000015 0.000016 ) M - matrix: 0.021575 -0.014395 0.007196 ( 0.000004 0.000003 0.000003 ) -0.014395 0.028806 -0.014400 ( 0.000003 0.000004 0.000003 ) 0.007196 -0.014400 0.021602 ( 0.000003 0.000003 0.000005 ) UB fit with 997 obs out of 997 (total:997,skipped:0) (100.00%) unit cell: 5.9145(8) 5.9101(6) 5.9101(8) 60.007(13) 90.000(12) 59.995(13) V = 146.08(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104056 -0.015258 0.049846 ( 0.000025 0.000032 0.000028 ) 0.087365 -0.167025 0.063631 ( 0.000017 0.000021 0.000019 ) 0.055437 -0.024108 0.122530 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014341 0.007165 ( 0.000006 0.000005 0.000005 ) -0.014341 0.028711 -0.014343 ( 0.000005 0.000007 0.000005 ) 0.007165 -0.014343 0.021547 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9169(14) 5.9148(10) 5.9144(13) 60.04(2) 90.005(18) 60.03(2) V = 146.49(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104081 -0.015241 0.049903 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167254 0.063759 ( 0.000017 0.000021 0.000019 ) 0.055517 -0.024211 0.122619 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014378 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014378 0.028792 -0.014393 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014393 0.021591 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9106(10) 5.9117(13) 60.00(2) 89.997(18) 60.01(2) V = 146.19(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.897) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104081 -0.015241 0.049903 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167254 0.063759 ( 0.000017 0.000021 0.000019 ) 0.055517 -0.024211 0.122619 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014378 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014378 0.028792 -0.014393 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014393 0.021591 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9106(10) 5.9117(13) 60.00(2) 89.997(18) 60.01(2) V = 146.19(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104081 -0.015241 0.049903 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167254 0.063759 ( 0.000017 0.000021 0.000019 ) 0.055517 -0.024211 0.122619 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014378 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014378 0.028792 -0.014393 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014393 0.021591 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9106(10) 5.9117(13) 60.00(2) 89.997(18) 60.01(2) V = 146.19(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) UB - matrix: -0.104293 -0.015042 0.049924 ( 0.000036 0.000078 0.000130 ) 0.087274 -0.167144 0.063516 ( 0.000025 0.000053 0.000088 ) 0.055505 -0.024449 0.122615 ( 0.000033 0.000071 0.000119 ) M - matrix: 0.021575 -0.014376 0.007142 ( 0.000009 0.000011 0.000018 ) -0.014376 0.028761 -0.014365 ( 0.000011 0.000018 0.000018 ) 0.007142 -0.014365 0.021561 ( 0.000018 0.000018 0.000034 ) unit cell: 5.913(4) 5.916(3) 5.914(5) 59.96(8) 89.85(7) 59.94(6) V = 146.25(17) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.104222 -0.015207 0.049920 ( 0.000034 0.000072 0.000120 ) 0.087264 -0.167250 0.063673 ( 0.000023 0.000048 0.000080 ) 0.055564 -0.024356 0.122712 ( 0.000033 0.000071 0.000118 ) M - matrix: 0.021565 -0.014363 0.007172 ( 0.000009 0.000010 0.000016 ) -0.014363 0.028797 -0.014397 ( 0.000010 0.000017 0.000017 ) 0.007172 -0.014397 0.021605 ( 0.000016 0.000017 0.000033 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 5.911(3) 5.908(3) 5.909(5) 59.97(7) 89.96(6) 60.04(6) V = 146.00(16) Run 3 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.897) HKL list info: 262 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.104222 -0.015207 0.049920 ( 0.000034 0.000072 0.000120 ) 0.087264 -0.167250 0.063673 ( 0.000023 0.000048 0.000080 ) 0.055564 -0.024356 0.122712 ( 0.000033 0.000071 0.000118 ) M - matrix: 0.021565 -0.014363 0.007172 ( 0.000009 0.000010 0.000016 ) -0.014363 0.028797 -0.014397 ( 0.000010 0.000017 0.000017 ) 0.007172 -0.014397 0.021605 ( 0.000016 0.000017 0.000033 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 5.911(3) 5.908(3) 5.909(5) 59.97(7) 89.96(6) 60.04(6) V = 146.00(16) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104183 -0.015095 0.049696 ( 0.000016 0.000018 0.000019 ) 0.087350 -0.167105 0.063649 ( 0.000011 0.000013 0.000013 ) 0.055490 -0.024311 0.122635 ( 0.000014 0.000016 0.000017 ) M - matrix: 0.021563 -0.014373 0.007187 ( 0.000004 0.000003 0.000003 ) -0.014373 0.028743 -0.014368 ( 0.000003 0.000004 0.000003 ) 0.007187 -0.014368 0.021560 ( 0.000003 0.000003 0.000005 ) UB fit with 997 obs out of 997 (total:997,skipped:0) (100.00%) unit cell: 5.9158(9) 5.9156(7) 5.9153(9) 60.017(14) 90.011(12) 60.001(13) V = 146.40(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 29 reflections under beam stop or inside a detector rejection region 8 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof 1356 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:05:40 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.897) Run 3 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.897) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=587.0452 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=932 PROFFIT INFO: Inet: min=1280.8258 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=407.06 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 20 94 171 285 312 524 901 1217 1356 Percent 0.0 0.0 1.5 6.9 12.6 21.0 23.0 38.6 66.4 89.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1356 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 1356 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1681392 135 2476730.47 137.30 100.00 1678086- 1083656 135 1374753.92 112.42 100.00 1082602- 330628 135 606558.86 92.17 100.00 330220- 225188 135 263691.32 71.04 100.00 224642- 171468 135 198871.54 51.21 100.00 171187- 142871 135 157593.94 36.13 100.00 142266- 104933 135 123063.94 31.16 100.00 104915- 6629 135 60487.44 21.42 100.00 6627- 3954 135 4964.26 4.61 83.70 3915- 1281 141 3006.27 3.52 48.94 ------------------------------------------------------------------------------------ 4887974- 1281 1356 524653.76 55.87 93.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 135 692315.65 86.56 100.00 1.24- 0.98 135 826850.07 74.05 97.78 0.98- 0.82 135 548465.84 56.53 96.30 0.82- 0.74 135 633797.46 68.12 96.30 0.73- 0.65 135 559329.20 61.09 94.81 0.65- 0.60 135 473033.60 50.02 92.59 0.60- 0.55 135 405671.77 45.43 96.30 0.55- 0.51 135 446234.33 45.29 83.70 0.51- 0.48 135 332799.22 36.26 86.67 0.48- 0.40 141 336407.00 36.20 86.52 ------------------------------------------------------------------------------------ 5.26- 0.40 1356 524653.76 55.87 93.07 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:05:40 2018 Sorting 1356 observations 252 unique observations with > 7.00 F2/sig(F2) 1356 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 24 240 Total number of frames 240 Maximum number of 252 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1356 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 24 240 Total number of frames 240 Frame #8 of 240 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 1091 observations > 7.00 F2/sig(F2) 1091 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 24 240 Total number of frames 240 Frame #8 of 240 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 4.2 (Out of 1091 removed 37 = 1054, unique = 249) 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 1054 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 24 240 Total number of frames 240 Frame #8 of 240 skipped from refinement Frame #119 of 240 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 249 unique data precomputed (should be 249) 249 unique data with 1054 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.2 (Out of 1054 removed 0 = 1054, unique = 249) 249 unique data precomputed (should be 249) 249 unique data with 1054 observations RMS deviation of equivalent data = 0.67241 Rint = 0.59025 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.55674, wR= 2.77796 Trying model 1 (ne=2, no=0)... Results: Rint= 0.70228, wR= 3.66044, Acormin=-0.201, Acormax=1.830, Acor_av=0.491 F test: Probability=0.000, F= 0.625 Trying model 2 (ne=2, no=1)... Results: Rint= 0.87393, wR= 2.90937, Acormin=-0.638, Acormax=1.587, Acor_av=0.163 F test: Probability=0.000, F= 0.402 Trying model 3 (ne=4, no=0)... Results: Rint= 0.76946, wR= 2.06809, Acormin=-0.551, Acormax=2.040, Acor_av=0.292 F test: Probability=0.000, F= 0.514 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86678, wR= 2.00044, Acormin=-0.630, Acormax=1.551, Acor_av=0.138 F test: Probability=0.000, F= 0.404 Trying model 5 (ne=4, no=3)... Results: Rint= 0.91977, wR= 1.93581, Acormin=-0.534, Acormax=1.403, Acor_av=0.046 F test: Probability=0.000, F= 0.355 Trying model 6 (ne=6, no=0)... Results: Rint= 0.80947, wR= 1.45314, Acormin=-0.391, Acormax=2.069, Acor_av=0.170 F test: Probability=0.000, F= 0.457 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87364, wR= 1.80906, Acormin=-0.491, Acormax=1.618, Acor_av=0.084 F test: Probability=0.000, F= 0.391 Trying model 8 (ne=6, no=3)... Results: Rint= 0.94041, wR= 2.28340, Acormin=-0.511, Acormax=1.056, Acor_av=0.037 F test: Probability=0.000, F= 0.334 Trying model 9 (ne=6, no=5)... Results: Rint= 0.91253, wR= 1.59395, Acormin=-0.301, Acormax=0.602, Acor_av=0.004 F test: Probability=0.000, F= 0.350 Trying model 10 (ne=8, no=0)... Results: Rint= 0.89914, wR= 1.32465, Acormin=-0.354, Acormax=1.737, Acor_av=0.072 F test: Probability=0.000, F= 0.362 Trying model 11 (ne=8, no=1)... Results: Rint= 0.90889, wR= 1.65244, Acormin=-0.291, Acormax=1.454, Acor_av=0.058 F test: Probability=0.000, F= 0.353 Trying model 12 (ne=8, no=3)... Results: Rint= 0.91174, wR= 1.64493, Acormin=-0.048, Acormax=0.079, Acor_av=0.002 F test: Probability=0.000, F= 0.348 Trying model 13 (ne=8, no=5)... Results: Rint= 0.86280, wR= 2.30449, Acormin=-0.039, Acormax=0.055, Acor_av=0.002 F test: Probability=0.000, F= 0.382 Trying model 14 (ne=8, no=7)... Results: Rint= 0.86649, wR= 2.25801, Acormin=-0.050, Acormax=0.042, Acor_av=0.002 F test: Probability=0.000, F= 0.371 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: 0.77011 There are 238 active scales (one needs to be fixed) Refinement control: frame scale #149 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 242 pars with 29403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.67241 Using Levenberg-Marquardt: 0.00010 New wR= 0.63770 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.59025 with corrections 0.56551 Rint for all data: 0.77011 with corrections 0.75369 4 observations identified as outliers and rejected Cycle 2 wR= 0.63376 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= 0.77328 Using Levenberg-Marquardt: 0.10000 New wR= 0.62559 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.57177 with corrections 0.55332 Rint for all data: 0.77011 with corrections 0.75626 4 observations identified as outliers and rejected Cycle 3 wR= 0.58660 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58264 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55420 with corrections 0.54167 Rint for all data: 0.77011 with corrections 0.75961 3 observations identified as outliers and rejected Cycle 4 wR= 0.57232 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56823 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.54720 with corrections 0.54090 Rint for all data: 0.77011 with corrections 0.76318 2 observations identified as outliers and rejected Cycle 5 wR= 0.56543 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56014 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.54604 with corrections 0.55070 Rint for all data: 0.77011 with corrections 0.76915 0 observations identified as outliers and rejected Final wR= 0.56014 Final frame scales: Min= 0.4513 Max= 2.4793 Final absorption correction factors: Amin= 0.3145 Amax= 1.6098 3 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=916.9222 max=7184942.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=125.6208 max=120679.3906 PROFFIT INFO: 12 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1344 reflections read from tmp file 1028 reflections are rejected (929 as outliers, 99 as groups of 1 refl) Redundancy: 1 2 3 4 5+ Number of groups: 0 90 21 12 5 Initial Chi^2= 0.87301 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.72865 Current error model SIG(F2)^2 = 477.63*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 348.02*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 348.02*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7184942- 1504472 134 2449645.72 69.78 100.00 1497263- 858342 134 1139059.66 41.88 100.00 839899- 345143 134 562613.86 33.43 100.00 343981- 209015 134 264584.37 26.84 100.00 208318- 157005 134 183725.06 18.59 100.00 156567- 120349 134 138553.48 14.11 100.00 120218- 89725 134 105223.95 11.82 100.00 89442- 7486 134 52267.65 8.43 87.31 7414- 3288 134 4790.59 2.58 19.40 3284- 917 138 2405.03 2.19 9.42 ------------------------------------------------------------------------------------ 7184942- 917 1344 488834.91 22.90 81.40 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 134 845456.24 47.89 97.01 1.24- 0.98 134 823878.46 34.89 86.57 0.98- 0.82 134 490858.13 22.92 84.33 0.82- 0.73 134 602286.95 25.41 79.85 0.73- 0.65 134 458319.65 21.51 85.07 0.65- 0.60 134 426481.01 18.27 75.37 0.60- 0.55 134 339186.12 16.13 79.85 0.55- 0.51 134 370900.04 15.98 75.37 0.51- 0.48 134 296587.60 13.39 73.88 0.47- 0.40 138 241769.94 12.95 76.81 ------------------------------------------------------------------------------------ 5.26- 0.40 1344 488834.91 22.90 81.40 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 134 845456.24 47.89 97.01 5.26- 0.98 268 834667.35 41.39 91.79 5.26- 0.82 402 720064.28 35.23 89.30 5.26- 0.73 536 690619.95 32.78 86.94 5.26- 0.65 670 644159.89 30.52 86.57 5.26- 0.60 804 607880.08 28.48 84.70 5.26- 0.55 938 569495.22 26.72 84.01 5.26- 0.51 1072 544670.83 25.37 82.93 5.26- 0.48 1206 517106.02 24.04 81.92 5.26- 0.40 1344 488834.91 22.90 81.40 ------------------------------------------------------------------------------------ 5.26- 0.40 1344 488834.91 22.90 81.40 Scale applied to data: s=0.139180 (maximum obs:7184942.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.766; Rsigma 0.029: data 1344 -> merged 304 With outlier rejection... Rint 0.650; Rsigma 0.030: data 1188 -> merged 304 Rejected total: 156, method kkm 153, method Blessing 3 Completeness direct cell (a, b, c) = (5.270, 5.270, 5.270), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404228, 5.270493 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 4.87 100.00 73 1.46 - 1.12 15 15 5.53 100.00 83 1.08 - 0.96 15 15 6.13 100.00 92 0.96 - 0.85 15 15 6.47 100.00 97 0.85 - 0.79 15 15 5.00 100.00 75 0.79 - 0.73 13 15 4.54 86.67 59 0.73 - 0.69 15 15 3.93 100.00 59 0.69 - 0.65 14 15 4.79 93.33 67 0.65 - 0.63 12 15 3.75 80.00 45 0.63 - 0.60 21 21 3.67 100.00 77 --------------------------------------------------------------- 5.91 - 0.60 150 156 4.85 96.15 727 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:05:41 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915796 5.915617 5.915301 60.0168 90.0106 60.0014 1188 Reflections read from file xs1715a.hkl; mean (I/sigma) = 22.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 590 627 593 601 905 804 777 1188 N (int>3sigma) = 0 461 627 464 465 776 649 621 956 Mean intensity = 0.0 53.0 27.3 53.5 60.2 44.3 59.8 58.6 60.4 Mean int/sigma = 0.0 20.7 19.0 21.0 21.0 20.2 21.6 21.9 22.0 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.915 5.916 5.916 120.00 90.01 119.98 Niggli form: a.a = 34.991 b.b = 34.995 c.c = 34.997 b.c = -17.497 a.c = -0.006 a.b = -17.487 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.020 CUBIC F-lattice R(int) = 0.230 [ 1037] Vol = 585.6 Cell: 8.365 8.367 8.367 89.99 90.00 90.00 Volume: 585.62 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.186 [ 790] Vol = 439.2 Cell: 5.916 5.915 14.491 90.00 90.01 119.98 Volume: 439.21 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 250] Vol = 439.2 Trigonal Cell: 5.916 5.915 14.491 90.00 90.01 119.98 Volume: 439.21 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.013 TETRAGONAL I-lattice R(int) = 0.177 [ 827] Vol = 292.8 Cell: 5.917 5.916 8.365 89.99 90.00 90.01 Volume: 292.81 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.012 TETRAGONAL I-lattice R(int) = 0.177 [ 827] Vol = 292.8 Cell: 5.917 5.916 8.365 89.99 90.00 90.01 Volume: 292.81 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.008 ORTHORHOMBIC I-lattice R(int) = 0.150 [ 780] Vol = 292.8 Cell: 5.917 8.365 5.916 89.99 89.99 90.00 Volume: 292.81 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.004 MONOCLINIC I-lattice R(int) = 0.113 [ 561] Vol = 292.8 Cell: 8.365 5.917 5.916 90.01 90.01 90.00 Volume: 292.81 Matrix:-1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.010 MONOCLINIC C-lattice R(int) = 0.143 [ 626] Vol = 292.8 Cell: 8.365 8.367 5.915 89.99 134.99 90.00 Volume: 292.81 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 451] Vol = 146.4 Cell: 5.915 5.916 5.916 120.00 90.01 119.98 Volume: 146.40 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 627 0 775 779 1188 N (int>3sigma) = 0 0 0 0 627 0 620 624 956 Mean intensity = 0.0 0.0 0.0 0.0 27.3 0.0 58.8 60.8 60.4 Mean int/sigma = 0.0 0.0 0.0 0.0 19.0 0.0 22.1 21.9 22.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 93 276 N I>3s 5 5 32 276 0.8 0.8 0.6 31.8 5.8 5.8 3.0 23.0 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 0.230 963 Fd-3m 1 1 227 C N N N N 37 2284 0.231 1000 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365075 8.367473 8.366623 89.9891 89.9952 90.0045 ZERR 1.00 0.000352 0.003470 0.002134 0.0004 0.0003 0.0134 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5917307- 1040355 134 112 30 3.7 1511156.94 49.07 0.561 0.397 1039193- 762341 137 123 30 4.1 847671.59 32.77 0.644 0.482 759716- 559940 154 136 30 4.5 574892.37 27.91 0.794 0.671 552377- 432852 190 172 30 5.7 378952.00 22.64 0.899 0.967 428360- 305501 158 135 30 4.5 293459.40 22.91 0.654 0.611 299712- 174430 137 118 30 3.9 204612.47 17.74 0.521 0.445 166912- 119762 140 127 30 4.2 141906.00 13.79 0.277 0.251 117411- 90502 95 81 30 2.7 98717.65 10.67 0.290 0.181 90166- 55108 100 88 30 2.9 71758.64 8.06 0.635 0.514 51928- 1053 99 96 34 2.8 25440.13 4.40 0.845 0.780 ------------------------------------------------------------------------------------------- 5917307- 1053 1344 1188 304 3.9 433850.83 22.01 0.650 0.516 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 181 156 30 5.2 706757.55 42.83 0.623 0.482 0.016 1.08-0.85 208 194 31 6.3 647865.68 27.84 0.797 0.710 0.023 0.83-0.72 165 144 31 4.6 487858.83 23.16 0.627 0.483 0.030 0.72-0.65 149 133 30 4.4 347486.77 19.29 0.690 0.619 0.034 0.64-0.60 124 111 30 3.7 393397.72 17.91 0.640 0.645 0.036 0.59-0.56 124 102 30 3.4 262266.23 14.29 0.488 0.349 0.043 0.55-0.51 120 106 31 3.4 313602.22 15.49 0.717 0.614 0.040 0.51-0.49 103 91 30 3.0 273161.66 13.10 0.522 0.376 0.046 0.49-0.45 98 87 30 2.9 232029.19 12.75 0.387 0.290 0.048 0.45-0.40 72 64 31 2.1 223482.25 12.15 0.256 0.194 0.052 ------------------------------------------------------------------------------------------------------ inf-0.40 1344 1188 304 3.9 433850.83 22.01 0.650 0.516 0.030 inf-0.60 815 727 150 4.8 542813.47 27.28 0.691 0.575 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 156 30 30 100.0 5.2 706757.55 112.51 0.623 0.009 1.08-0.85 194 31 31 100.0 6.3 647865.68 86.98 0.797 0.013 0.83-0.72 144 33 31 93.9 4.6 487858.83 55.15 0.627 0.016 0.72-0.65 133 33 30 90.9 4.4 347486.77 50.45 0.690 0.020 0.64-0.60 111 31 30 96.8 3.7 393397.72 42.02 0.640 0.022 0.59-0.56 102 38 30 78.9 3.4 262266.23 31.86 0.488 0.025 0.55-0.51 106 41 31 75.6 3.4 313602.22 36.49 0.717 0.025 0.51-0.49 91 42 30 71.4 3.0 273161.66 27.37 0.522 0.027 0.49-0.45 87 59 30 50.8 2.9 232029.19 24.43 0.387 0.030 0.45-0.40 64 123 31 25.2 2.1 223482.25 19.97 0.256 0.037 -------------------------------------------------------------------------------------------- inf-0.40 1188 461 304 65.9 3.9 433850.83 56.19 0.650 0.018 inf-0.60 727 156 150 96.2 4.8 542813.47 73.44 0.691 0.013 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 No constraint UB - matrix: 0.034790 0.007547 0.076938 ( 0.000008 0.000009 0.000009 ) 0.008053 0.083553 -0.011850 ( 0.000005 0.000006 0.000007 ) -0.076907 0.012156 0.033571 ( 0.000007 0.000008 0.000009 ) M - matrix: 0.007190 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007186 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.034790 0.007547 0.076938 ( 0.000008 0.000009 0.000009 ) 0.008053 0.083553 -0.011850 ( 0.000005 0.000006 0.000007 ) -0.076907 0.012156 0.033571 ( 0.000007 0.000008 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3651(7) 8.3675(6) 8.3668(9) 89.989(7) 89.995(8) 90.004(7) V = 585.63(9) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.63(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.897) Run 3 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.897) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=587.0452 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=64 max=932 PROFFIT INFO: Inet: min=1280.8258 max=4887974.0000 PROFFIT INFO: sig(Inet): min=245.3866 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=407.06 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 40 188 342 570 624 1048 1802 2434 2712 Percent 0.0 0.0 1.5 6.9 12.6 21.0 23.0 38.6 66.4 89.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1356 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 1356 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1681392 135 2476730.47 137.30 100.00 1678086- 1083656 135 1374753.92 112.42 100.00 1082602- 330628 135 606558.86 92.17 100.00 330220- 225188 135 263691.32 71.04 100.00 224642- 171468 135 198871.54 51.21 100.00 171187- 142871 135 157593.94 36.13 100.00 142266- 104933 135 123063.94 31.16 100.00 104915- 6629 135 60487.44 21.42 100.00 6627- 3954 135 4964.26 4.61 83.70 3915- 1281 141 3006.27 3.52 48.94 ------------------------------------------------------------------------------------ 4887974- 1281 1356 524653.76 55.87 93.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 135 701125.88 80.81 98.52 1.32- 1.09 135 1010679.92 83.02 100.00 1.09- 0.96 135 574002.35 69.28 100.00 0.96- 0.85 135 653206.87 70.46 97.04 0.85- 0.80 135 550960.23 61.05 98.52 0.80- 0.73 135 388156.65 44.15 94.81 0.73- 0.70 135 312244.59 37.05 92.59 0.70- 0.65 135 516098.63 50.89 91.85 0.65- 0.62 135 277763.12 32.22 80.74 0.62- 0.58 141 273463.39 30.83 77.30 ------------------------------------------------------------------------------------ 4.82- 0.58 1356 524653.76 55.87 93.07 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:05:41 2018 Sorting 1356 observations 83 unique observations with > 7.00 F2/sig(F2) 1356 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 24 240 Total number of frames 240 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1356 observations in 3 runs Run # start # end # total # 1 0 35 36 2 0 36 73 3 0 8 82 Total number of frames 82 1091 observations > 7.00 F2/sig(F2) 1091 observations in 3 runs Run # start # end # total # 1 0 35 36 2 0 36 73 3 0 8 82 Total number of frames 82 Removing 'redundancy=1' reflections Average redundancy: 12.8 (Out of 1091 removed 6 = 1085, 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): 4/m3bar2/m 1085 observations in 3 runs Run # start # end # total # 1 0 35 36 2 0 36 73 3 0 8 82 Total number of frames 82 85 unique data precomputed (should be 85) 85 unique data with 1085 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 12.8 (Out of 1085 removed 0 = 1085, unique = 85) 85 unique data precomputed (should be 85) 85 unique data with 1085 observations RMS deviation of equivalent data = 0.19009 Rint = 0.12061 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11888, wR= 0.17421 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06434, wR= 0.08888, Acormin=0.631, Acormax=1.410, Acor_av=0.815 F test: Probability=1.000, F= 3.397 Trying model 2 (ne=2, no=1)... Results: Rint= 0.05969, wR= 0.08209, Acormin=0.570, Acormax=1.331, Acor_av=0.754 F test: Probability=0.990, F= 1.158 Trying model 3 (ne=4, no=0)... Results: Rint= 0.05045, wR= 0.07125, Acormin=0.591, Acormax=1.573, Acor_av=0.789 F test: Probability=1.000, F= 1.392 Trying model 4 (ne=4, no=1)... Results: Rint= 0.04531, wR= 0.06559, Acormin=0.524, Acormax=1.538, Acor_av=0.774 F test: Probability=1.000, F= 1.236 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03829, wR= 0.05338, Acormin=0.493, Acormax=1.372, Acor_av=0.751 F test: Probability=1.000, F= 1.390 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04370, wR= 0.05912, Acormin=0.537, Acormax=1.446, Acor_av=0.723 F test: Probability=0.000, F= 0.765 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03776, wR= 0.05283, Acormin=0.490, Acormax=1.434, Acor_av=0.725 F test: Probability=0.632, F= 1.022 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03031, wR= 0.04117, Acormin=0.525, Acormax=1.491, Acor_av=0.781 F test: Probability=1.000, F= 1.575 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02911, wR= 0.03948, Acormin=0.510, Acormax=1.420, Acor_av=0.759 F test: Probability=0.859, F= 1.072 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03998, wR= 0.05486, Acormin=0.481, Acormax=1.306, Acor_av=0.677 F test: Probability=0.000, F= 0.571 Trying model 11 (ne=8, no=1)... Results: Rint= 0.03313, wR= 0.04564, Acormin=0.494, Acormax=1.299, Acor_av=0.711 F test: Probability=0.000, F= 0.828 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02842, wR= 0.03688, Acormin=0.510, Acormax=1.436, Acor_av=0.771 F test: Probability=0.957, F= 1.118 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02622, wR= 0.03422, Acormin=0.530, Acormax=1.526, Acor_av=0.797 F test: Probability=0.989, F= 1.162 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02353, wR= 0.03147, Acormin=0.546, Acormax=1.579, Acor_av=0.820 F test: Probability=0.999, F= 1.221 Final absorption model (ne=8, no=7): Rint= 0.02353, Acormin=0.546, Acormax=1.579, Acor_av=0.820 Combined refinement in use Rint: 0.12073 There are 82 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 161 pars with 13041 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.19009 Using Levenberg-Marquardt: 0.00010 New wR= 0.03557 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.12061 with corrections 0.02033 Rint for all data: 0.12073 with corrections 0.02056 1 observations identified as outliers and rejected Cycle 2 wR= 0.02810 Using Levenberg-Marquardt: 0.00001 New wR= 0.02234 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11888 with corrections 0.01549 Rint for all data: 0.12073 with corrections 0.01806 0 observations identified as outliers and rejected Cycle 3 wR= 0.02234 Using Levenberg-Marquardt: 0.00000 New wR= 0.02162 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11888 with corrections 0.01482 Rint for all data: 0.12073 with corrections 0.01779 0 observations identified as outliers and rejected Cycle 4 wR= 0.02162 Using Levenberg-Marquardt: 0.00000 New wR= 0.02145 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11888 with corrections 0.01471 Rint for all data: 0.12073 with corrections 0.01762 0 observations identified as outliers and rejected Cycle 5 wR= 0.02145 Using Levenberg-Marquardt: 0.00000 New wR= 0.02140 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11888 with corrections 0.01467 Rint for all data: 0.12073 with corrections 0.01748 0 observations identified as outliers and rejected Final wR= 0.02140 Final frame scales: Min= 0.9048 Max= 1.1274 Final absorption correction factors: Amin= 0.4089 Amax= 1.4379 PROFFIT INFO: Inet (after scale3 abspack): min=1304.0245 max=4306663.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=287.6122 max=72308.6484 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1356 reflections read from tmp file 47 reflections are rejected (43 as outliers, 4 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 7 2 8 3 4 5 5 69 Initial Chi^2= 0.23856 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.26360 Current error model SIG(F2)^2 = 100.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 127.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 127.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4306663- 1587613 135 2440366.65 123.19 100.00 1576944- 1035512 135 1295399.87 64.21 100.00 1033648- 328971 135 617398.29 61.26 100.00 328119- 217987 135 260469.52 40.82 100.00 217756- 181461 135 199876.00 28.86 100.00 180811- 135460 135 148539.27 21.29 100.00 135020- 106661 135 120073.02 18.69 100.00 106180- 6421 135 61419.30 13.29 100.00 6355- 3772 135 4764.48 4.19 94.07 3771- 1304 141 2991.97 3.40 61.70 ------------------------------------------------------------------------------------ 4306663- 1304 1356 512863.74 37.77 95.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 135 748271.19 72.69 100.00 1.32- 1.09 135 1025051.98 69.11 100.00 1.09- 0.96 135 565627.35 43.15 100.00 0.96- 0.85 135 631683.54 41.36 99.26 0.85- 0.80 135 524696.22 35.87 98.52 0.80- 0.73 135 361338.98 26.26 96.30 0.73- 0.70 135 296097.34 22.22 94.07 0.70- 0.65 135 477542.25 29.96 94.07 0.65- 0.62 135 257545.48 19.38 85.93 0.62- 0.58 141 252360.98 18.55 86.52 ------------------------------------------------------------------------------------ 4.82- 0.58 1356 512863.74 37.77 95.43 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 135 748271.19 72.69 100.00 4.82- 1.09 270 886661.58 70.90 100.00 4.82- 0.96 405 779650.17 61.65 100.00 4.82- 0.85 540 742658.51 56.58 99.81 4.82- 0.80 675 699066.06 52.43 99.56 4.82- 0.73 810 642778.21 48.07 99.01 4.82- 0.70 945 593252.37 44.38 98.31 4.82- 0.65 1080 578788.61 42.58 97.78 4.82- 0.62 1215 543094.93 40.00 96.46 4.82- 0.58 1356 512863.74 37.77 95.43 ------------------------------------------------------------------------------------ 4.82- 0.58 1356 512863.74 37.77 95.43 Scale applied to data: s=0.232198 (maximum obs:4306663.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.017; Rsigma 0.017: data 1356 -> merged 108 With outlier rejection... Rint 0.015; Rsigma 0.017: data 1351 -> merged 108 Rejected total: 5, method kkm 5, method Blessing 0 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585768, 4.830370 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 9 10 7.00 90.00 63 1.61 - 1.21 10 10 11.80 100.00 118 1.17 - 1.01 10 10 15.90 100.00 159 0.99 - 0.89 10 10 15.90 100.00 159 0.88 - 0.81 10 10 15.50 100.00 155 0.81 - 0.74 10 10 13.60 100.00 136 0.73 - 0.71 10 10 14.80 100.00 148 0.70 - 0.66 10 10 12.20 100.00 122 0.66 - 0.64 10 10 11.30 100.00 113 0.63 - 0.60 10 10 11.60 100.00 116 --------------------------------------------------------------- 5.91 - 0.60 99 100 13.02 99.00 1289 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:05:41 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915796 5.915617 5.915301 60.0168 90.0106 60.0014 1188 Reflections read from file xs1715a.hkl; mean (I/sigma) = 22.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 590 627 593 601 905 804 777 1188 N (int>3sigma) = 0 461 627 464 465 776 649 621 956 Mean intensity = 0.0 53.0 27.3 53.5 60.2 44.3 59.8 58.6 60.4 Mean int/sigma = 0.0 20.7 19.0 21.0 21.0 20.2 21.6 21.9 22.0 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.915 5.916 5.916 120.00 90.01 119.98 Niggli form: a.a = 34.991 b.b = 34.995 c.c = 34.997 b.c = -17.497 a.c = -0.006 a.b = -17.487 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.020 CUBIC F-lattice R(int) = 0.230 [ 1037] Vol = 585.6 Cell: 8.365 8.367 8.367 89.99 90.00 90.00 Volume: 585.62 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.186 [ 790] Vol = 439.2 Cell: 5.916 5.915 14.491 90.00 90.01 119.98 Volume: 439.21 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.020 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 250] Vol = 439.2 Trigonal Cell: 5.916 5.915 14.491 90.00 90.01 119.98 Volume: 439.21 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.013 TETRAGONAL I-lattice R(int) = 0.177 [ 827] Vol = 292.8 Cell: 5.917 5.916 8.365 89.99 90.00 90.01 Volume: 292.81 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.012 TETRAGONAL I-lattice R(int) = 0.177 [ 827] Vol = 292.8 Cell: 5.917 5.916 8.365 89.99 90.00 90.01 Volume: 292.81 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.008 ORTHORHOMBIC I-lattice R(int) = 0.150 [ 780] Vol = 292.8 Cell: 5.917 8.365 5.916 89.99 89.99 90.00 Volume: 292.81 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.004 MONOCLINIC I-lattice R(int) = 0.113 [ 561] Vol = 292.8 Cell: 8.365 5.917 5.916 90.01 90.01 90.00 Volume: 292.81 Matrix:-1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.010 MONOCLINIC C-lattice R(int) = 0.143 [ 626] Vol = 292.8 Cell: 8.365 8.367 5.915 89.99 134.99 90.00 Volume: 292.81 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 451] Vol = 146.4 Cell: 5.915 5.916 5.916 120.00 90.01 119.98 Volume: 146.40 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 627 0 775 779 1188 N (int>3sigma) = 0 0 0 0 627 0 620 624 956 Mean intensity = 0.0 0.0 0.0 0.0 27.3 0.0 58.8 60.8 60.4 Mean int/sigma = 0.0 0.0 0.0 0.0 19.0 0.0 22.1 21.9 22.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 93 276 N I>3s 5 5 32 276 0.8 0.8 0.6 31.8 5.8 5.8 3.0 23.0 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 0.230 963 Fd-3m 1 1 227 C N N N N 37 2284 0.231 1000 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365075 8.367473 8.366623 89.9891 89.9952 90.0045 ZERR 1.00 0.000352 0.003470 0.002134 0.0004 0.0003 0.0134 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4263277- 917569 308 305 27 11.3 1746858.44 86.01 0.012 0.014 887738- 157312 402 401 27 14.9 283578.64 41.31 0.020 0.023 147744- 25498 336 335 27 12.4 114941.05 18.14 0.029 0.035 11426- 1751 310 310 27 11.5 4412.07 4.15 0.158 0.194 ------------------------------------------------------------------------------------------- 4263277- 1751 1356 1351 108 12.5 508053.18 37.13 0.015 0.017 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.01 342 338 28 12.1 739662.62 59.96 0.013 0.015 0.010 0.99-0.76 423 422 27 15.6 589133.70 38.90 0.014 0.017 0.016 0.75-0.65 339 339 27 12.6 346592.46 24.53 0.016 0.018 0.025 0.65-0.59 252 252 26 9.7 278827.85 20.47 0.019 0.022 0.031 ------------------------------------------------------------------------------------------------------ inf-0.59 1356 1351 108 12.5 508053.18 37.13 0.015 0.017 0.017 inf-0.60 1292 1287 98 13.1 522795.62 38.11 0.014 0.017 0.017 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.01 338 29 28 96.6 12.1 739662.62 214.84 0.013 0.003 0.99-0.76 422 27 27 100.0 15.6 589133.70 158.56 0.014 0.004 0.75-0.65 339 27 27 100.0 12.6 346592.46 91.30 0.016 0.008 0.65-0.59 252 27 26 96.3 9.7 278827.85 71.64 0.019 0.011 -------------------------------------------------------------------------------------------- inf-0.59 1351 110 108 98.2 12.5 508053.18 139.55 0.015 0.005 inf-0.60 1287 99 98 99.0 13.1 522795.62 143.92 0.014 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:10:49 2018) ID: 2932; threads 39; handles 878; mem 519388.00 (1237724.00)kB; time: 1w 5d 22h 16m 19s MEMORY INFO: Memory PF:1.0, Ph:171.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.2,peak PF: 708.5, WS: 271.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:171.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.0,peak PF: 708.5, WS: 273.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:10:49 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000016 0.000018 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000014 0.000016 0.000017 ) 5.91535 ( 0.00086 ) 5.92288 ( 0.00066 ) 5.91286 ( 0.00090 ) 59.95509 ( 0.01370 ) 89.89521 ( 0.01218 ) 59.99590 ( 0.01344 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:10:49 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000016 0.000018 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000014 0.000016 0.000017 ) M - matrix: 0.021563 -0.014373 0.007187 ( 0.000004 0.000003 0.000003 ) -0.014373 0.028743 -0.014368 ( 0.000003 0.000004 0.000003 ) 0.007187 -0.014368 0.021560 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(9) 5.9229(7) 5.9129(9) 59.955(14) 89.895(12) 59.996(13) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 454 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.163 ( 0.077) | 1.144 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.73 | 45 | 1.183 ( 0.066) | 1.150 ( 0.125) | 1.117 ( 0.367) | 0.73- 0.70 | 45 | 1.199 ( 0.068) | 1.210 ( 0.152) | 1.176 ( 0.383) | 0.70- 0.66 | 45 | 1.204 ( 0.060) | 1.197 ( 0.170) | 1.215 ( 0.426) | 0.66- 0.62 | 45 | 1.232 ( 0.079) | 1.190 ( 0.164) | 1.203 ( 0.454) | 0.62- 0.59 | 45 | 1.215 ( 0.093) | 1.220 ( 0.224) | 1.259 ( 0.505) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 450 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.202 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087376 -0.167144 0.063772 ( 0.000019 0.000024 0.000021 ) 0.055238 -0.024246 0.122371 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000007 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9296(14) 59.96(2) 89.997(19) 59.96(2) V = 147.15(5) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087385 -0.167043 0.063671 ( 0.000018 0.000023 0.000020 ) 0.055392 -0.024146 0.122475 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021531 ( 0.000004 0.000005 0.000006 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9193(12) 60.01(2) 90.008(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087385 -0.167043 0.063671 ( 0.000018 0.000023 0.000020 ) 0.055392 -0.024146 0.122475 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021531 ( 0.000004 0.000005 0.000006 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9193(12) 60.01(2) 90.008(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.060) | 1.213 ( 0.160) | 1.215 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.457) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.347 ( 0.571) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.221 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_3_26.rpb PROFFITPEAK info: 514 peaks in the peak location table UB fit with 256 obs out of 258 (total:258,skipped:0) (99.22%) UB - matrix: -0.104271 -0.014815 0.049447 ( 0.000058 0.000096 0.000120 ) 0.087164 -0.166897 0.063454 ( 0.000050 0.000082 0.000103 ) 0.055500 -0.024417 0.122472 ( 0.000063 0.000104 0.000130 ) M - matrix: 0.021550 -0.014358 0.007172 ( 0.000016 0.000016 0.000019 ) -0.014358 0.028670 -0.014313 ( 0.000016 0.000028 0.000023 ) 0.007172 -0.014313 0.021471 ( 0.000019 0.000023 0.000036 ) unit cell: 5.919(4) 5.923(4) 5.926(6) 60.04(9) 90.02(7) 59.98(8) V = 146.9(2) UB fit with 256 obs out of 258 (total:258,skipped:0) (99.22%) UB - matrix: -0.104271 -0.014815 0.049447 ( 0.000058 0.000096 0.000120 ) 0.087164 -0.166897 0.063454 ( 0.000050 0.000082 0.000103 ) 0.055500 -0.024417 0.122472 ( 0.000063 0.000104 0.000130 ) M - matrix: 0.021550 -0.014358 0.007172 ( 0.000016 0.000016 0.000019 ) -0.014358 0.028670 -0.014313 ( 0.000016 0.000028 0.000023 ) 0.007172 -0.014313 0.021471 ( 0.000019 0.000023 0.000036 ) unit cell: 5.919(4) 5.923(4) 5.926(6) 60.04(9) 90.02(7) 59.98(8) V = 146.9(2) OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 UB - matrix: -0.104208 -0.014892 0.049216 ( 0.000057 0.000094 0.000118 ) 0.087001 -0.166791 0.063357 ( 0.000051 0.000084 0.000105 ) 0.055249 -0.024239 0.122413 ( 0.000062 0.000103 0.000129 ) M - matrix: 0.021481 -0.014298 0.007147 ( 0.000016 0.000016 0.000019 ) -0.014298 0.028629 -0.014267 ( 0.000016 0.000029 0.000023 ) 0.007147 -0.014267 0.021421 ( 0.000019 0.000023 0.000036 ) UB fit with 257 obs out of 258 (total:258,skipped:0) (99.61%) unit cell: 5.923(4) 5.919(4) 5.929(6) 60.10(9) 90.08(7) 60.06(7) V = 147.2(2) UB fit with 257 obs out of 258 (total:258,skipped:0) (99.61%) UB - matrix: -0.104208 -0.014892 0.049216 ( 0.000057 0.000094 0.000118 ) 0.087001 -0.166791 0.063357 ( 0.000051 0.000084 0.000105 ) 0.055249 -0.024239 0.122413 ( 0.000062 0.000103 0.000129 ) M - matrix: 0.021481 -0.014298 0.007147 ( 0.000016 0.000016 0.000019 ) -0.014298 0.028629 -0.014267 ( 0.000016 0.000029 0.000023 ) 0.007147 -0.014267 0.021421 ( 0.000019 0.000023 0.000036 ) unit cell: 5.923(4) 5.919(4) 5.929(6) 60.10(9) 90.08(7) 60.06(7) V = 147.2(2) OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 258 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Run 3 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.000) HKL list info: 426 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104208 -0.014892 0.049216 ( 0.000057 0.000094 0.000118 ) 0.087001 -0.166791 0.063357 ( 0.000051 0.000084 0.000105 ) 0.055249 -0.024239 0.122413 ( 0.000062 0.000103 0.000129 ) M - matrix: 0.021481 -0.014298 0.007147 ( 0.000016 0.000016 0.000019 ) -0.014298 0.028629 -0.014267 ( 0.000016 0.000029 0.000023 ) 0.007147 -0.014267 0.021421 ( 0.000019 0.000023 0.000036 ) UB fit with 257 obs out of 258 (total:258,skipped:0) (99.61%) unit cell: 5.923(4) 5.919(4) 5.929(6) 60.10(9) 90.08(7) 60.06(7) V = 147.2(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 258 obs out of 258 (total:258,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_26.rpb 1 of 216 peaks identified as outliers and rejected 215 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 215 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 215 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.60 | 22 | 1.069 ( 0.230) | 1.333 ( 0.782) | 1.431 ( 1.072) | 1.47- 1.17 | 22 | 1.120 ( 0.204) | 1.123 ( 0.204) | 1.220 ( 0.835) | 1.15- 0.98 | 22 | 1.106 ( 0.086) | 1.101 ( 0.097) | 1.119 ( 0.362) | 0.98- 0.89 | 22 | 1.151 ( 0.063) | 1.121 ( 0.084) | 1.050 ( 0.340) | 0.89- 0.82 | 22 | 1.185 ( 0.083) | 1.122 ( 0.074) | 1.226 ( 0.411) | 0.82- 0.75 | 22 | 1.216 ( 0.053) | 1.139 ( 0.084) | 1.199 ( 0.389) | 0.75- 0.71 | 22 | 1.225 ( 0.059) | 1.145 ( 0.101) | 1.190 ( 0.413) | 0.71- 0.67 | 22 | 1.242 ( 0.054) | 1.160 ( 0.127) | 1.269 ( 0.466) | 0.67- 0.62 | 22 | 1.241 ( 0.061) | 1.187 ( 0.120) | 1.284 ( 0.509) | 0.62- 0.60 | 17 | 1.295 ( 0.073) | 1.159 ( 0.160) | 1.366 ( 0.543) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.60 | 215 | 1.182 ( 0.133) | 1.159 ( 0.283) | 1.232 ( 0.589) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) UB - matrix: -0.104209 -0.015125 0.049478 ( 0.000027 0.000047 0.000058 ) 0.087236 -0.167142 0.063501 ( 0.000031 0.000054 0.000066 ) 0.055086 -0.024318 0.122790 ( 0.000035 0.000060 0.000073 ) M - matrix: 0.021504 -0.014344 0.007148 ( 0.000009 0.000009 0.000010 ) -0.014344 0.028757 -0.014348 ( 0.000009 0.000018 0.000014 ) 0.007148 -0.014348 0.021558 ( 0.000010 0.000014 0.000021 ) unit cell: 5.921(2) 5.910(3) 5.911(3) 60.04(5) 89.96(4) 59.99(4) V = 146.40(11) OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 UB - matrix: -0.104242 -0.014918 0.049468 ( 0.000028 0.000047 0.000058 ) 0.087102 -0.166959 0.063598 ( 0.000029 0.000050 0.000061 ) 0.055380 -0.024308 0.122562 ( 0.000026 0.000045 0.000055 ) M - matrix: 0.021520 -0.014334 0.007170 ( 0.000008 0.000009 0.000009 ) -0.014334 0.028689 -0.014336 ( 0.000009 0.000017 0.000012 ) 0.007170 -0.014336 0.021513 ( 0.000009 0.000012 0.000017 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 5.919(2) 5.918(2) 5.921(3) 60.02(4) 90.03(3) 60.04(4) V = 146.77(10) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.000) HKL list info: 421 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104242 -0.014918 0.049468 ( 0.000028 0.000047 0.000058 ) 0.087102 -0.166959 0.063598 ( 0.000029 0.000050 0.000061 ) 0.055380 -0.024308 0.122562 ( 0.000026 0.000045 0.000055 ) M - matrix: 0.021520 -0.014334 0.007170 ( 0.000008 0.000009 0.000009 ) -0.014334 0.028689 -0.014336 ( 0.000009 0.000017 0.000012 ) 0.007170 -0.014336 0.021513 ( 0.000009 0.000012 0.000017 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 5.919(2) 5.918(2) 5.921(3) 60.02(4) 90.03(3) 60.04(4) V = 146.77(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_26.rpb 2 of 214 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 212 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 212 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.61 | 21 | 1.057 ( 0.217) | 1.236 ( 0.667) | 1.295 ( 0.899) | 1.48- 1.15 | 21 | 1.069 ( 0.094) | 1.176 ( 0.393) | 1.105 ( 0.536) | 1.12- 0.99 | 21 | 1.115 ( 0.077) | 1.112 ( 0.092) | 1.129 ( 0.355) | 0.98- 0.92 | 21 | 1.153 ( 0.067) | 1.129 ( 0.088) | 1.055 ( 0.342) | 0.89- 0.84 | 21 | 1.177 ( 0.092) | 1.133 ( 0.068) | 1.098 ( 0.358) | 0.84- 0.76 | 21 | 1.217 ( 0.050) | 1.130 ( 0.093) | 1.302 ( 0.399) | 0.75- 0.72 | 21 | 1.215 ( 0.066) | 1.154 ( 0.098) | 1.098 ( 0.423) | 0.72- 0.67 | 21 | 1.246 ( 0.048) | 1.175 ( 0.131) | 1.272 ( 0.452) | 0.67- 0.64 | 21 | 1.235 ( 0.065) | 1.193 ( 0.132) | 1.261 ( 0.458) | 0.64- 0.60 | 23 | 1.287 ( 0.068) | 1.146 ( 0.148) | 1.467 ( 0.527) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.60 | 212 | 1.178 ( 0.121) | 1.158 ( 0.265) | 1.211 ( 0.516) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 111 | 1.150 ( 0.086) | 1.257 ( 0.335) | 1.337 ( 0.609) | 13.1-19.0 | 111 | 1.143 ( 0.103) | 1.215 ( 0.305) | 1.339 ( 0.716) | 19.0-23.3 | 111 | 1.165 ( 0.089) | 1.231 ( 0.272) | 1.259 ( 0.575) | 23.3-27.5 | 111 | 1.140 ( 0.097) | 1.196 ( 0.341) | 1.236 ( 0.530) | 27.5-30.7 | 111 | 1.146 ( 0.104) | 1.185 ( 0.193) | 1.188 ( 0.397) | 30.8-34.2 | 111 | 1.146 ( 0.096) | 1.192 ( 0.292) | 1.166 ( 0.411) | 34.2-37.1 | 111 | 1.145 ( 0.105) | 1.131 ( 0.170) | 1.146 ( 0.394) | 37.1-39.7 | 111 | 1.154 ( 0.124) | 1.152 ( 0.204) | 1.250 ( 0.547) | 39.8-42.8 | 111 | 1.164 ( 0.104) | 1.130 ( 0.196) | 1.218 ( 0.615) | 42.9-49.8 | 111 | 1.202 ( 0.169) | 1.133 ( 0.256) | 1.234 ( 0.490) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1110 | 1.156 ( 0.111) | 1.182 ( 0.266) | 1.237 ( 0.541) | Fitted profile normalization line parameters e1 dimension: a=0.0017 b=0.97 e2 dimension: a=-0.0013 b=1.03 e3 dimension: a=-0.0028 b=1.13 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 453201 lp-corr: 681854 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 2567482 PROFFITPEAK - Finished at Wed Mar 28 13:10:58 2018 PROFFITMAIN - Started at Wed Mar 28 13:10:58 2018 OTKP changes: 1110 2 2 3 OTKP changes: 1110 2 2 3 UB - matrix: -0.104179 -0.015160 0.049816 ( 0.000014 0.000017 0.000018 ) 0.087423 -0.167304 0.063742 ( 0.000010 0.000012 0.000012 ) 0.055509 -0.024279 0.122727 ( 0.000012 0.000015 0.000015 ) M - matrix: 0.021577 -0.014395 0.007195 ( 0.000004 0.000003 0.000003 ) -0.014395 0.028810 -0.014399 ( 0.000003 0.000004 0.000003 ) 0.007195 -0.014399 0.021607 ( 0.000003 0.000003 0.000004 ) UB fit with 1110 obs out of 1110 (total:1110,skipped:0) (100.00%) unit cell: 5.9139(8) 5.9089(6) 5.9088(8) 60.015(12) 90.003(11) 59.997(12) V = 146.03(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104068 -0.015266 0.049867 ( 0.000025 0.000032 0.000028 ) 0.087364 -0.167018 0.063622 ( 0.000017 0.000021 0.000019 ) 0.055450 -0.024097 0.122540 ( 0.000020 0.000026 0.000023 ) M - matrix: 0.021537 -0.014339 0.007164 ( 0.000006 0.000005 0.000005 ) -0.014339 0.028709 -0.014340 ( 0.000005 0.000007 0.000005 ) 0.007164 -0.014340 0.021550 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9158(14) 5.9142(10) 5.9134(13) 60.04(2) 90.005(19) 60.03(2) V = 146.45(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104082 -0.015242 0.049906 ( 0.000024 0.000031 0.000027 ) 0.087416 -0.167258 0.063760 ( 0.000017 0.000021 0.000019 ) 0.055520 -0.024213 0.122621 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014379 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028794 -0.014394 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014394 0.021592 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9105(10) 5.9116(13) 60.00(2) 89.997(18) 60.01(2) V = 146.18(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.895) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104082 -0.015242 0.049906 ( 0.000024 0.000031 0.000027 ) 0.087416 -0.167258 0.063760 ( 0.000017 0.000021 0.000019 ) 0.055520 -0.024213 0.122621 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014379 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028794 -0.014394 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014394 0.021592 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9105(10) 5.9116(13) 60.00(2) 89.997(18) 60.01(2) V = 146.18(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104082 -0.015242 0.049906 ( 0.000024 0.000031 0.000027 ) 0.087416 -0.167258 0.063760 ( 0.000017 0.000021 0.000019 ) 0.055520 -0.024213 0.122621 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021557 -0.014379 0.007187 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028794 -0.014394 ( 0.000005 0.000007 0.000005 ) 0.007187 -0.014394 0.021592 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9105(10) 5.9116(13) 60.00(2) 89.997(18) 60.01(2) V = 146.18(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) UB - matrix: -0.104258 -0.014999 0.049835 ( 0.000031 0.000053 0.000065 ) 0.087294 -0.167148 0.063597 ( 0.000023 0.000040 0.000049 ) 0.055514 -0.024519 0.122724 ( 0.000024 0.000041 0.000051 ) M - matrix: 0.021572 -0.014388 0.007169 ( 0.000008 0.000008 0.000009 ) -0.014388 0.028765 -0.014387 ( 0.000008 0.000014 0.000010 ) 0.007169 -0.014387 0.021589 ( 0.000009 0.000010 0.000015 ) unit cell: 5.916(2) 5.918(2) 5.912(2) 59.96(4) 89.89(3) 59.93(4) V = 146.28(9) OTKP changes: 212 1 1 1 OTKP changes: 212 1 1 1 OTKP changes: 212 1 1 1 UB - matrix: -0.104181 -0.015163 0.049716 ( 0.000026 0.000044 0.000054 ) 0.087293 -0.167193 0.063623 ( 0.000022 0.000038 0.000047 ) 0.055501 -0.024380 0.122813 ( 0.000024 0.000041 0.000050 ) M - matrix: 0.021554 -0.014368 0.007191 ( 0.000007 0.000007 0.000008 ) -0.014368 0.028778 -0.014385 ( 0.000007 0.000013 0.000010 ) 0.007191 -0.014385 0.021603 ( 0.000008 0.000010 0.000015 ) UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) unit cell: 5.9149(19) 5.9091(19) 5.908(2) 60.03(4) 90.03(3) 60.03(3) V = 146.12(8) Run 3 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.895) HKL list info: 421 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104181 -0.015163 0.049716 ( 0.000026 0.000044 0.000054 ) 0.087293 -0.167193 0.063623 ( 0.000022 0.000038 0.000047 ) 0.055501 -0.024380 0.122813 ( 0.000024 0.000041 0.000050 ) M - matrix: 0.021554 -0.014368 0.007191 ( 0.000007 0.000007 0.000008 ) -0.014368 0.028778 -0.014385 ( 0.000007 0.000013 0.000010 ) 0.007191 -0.014385 0.021603 ( 0.000008 0.000010 0.000015 ) UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) unit cell: 5.9149(19) 5.9091(19) 5.908(2) 60.03(4) 90.03(3) 60.03(3) V = 146.12(8) 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! 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: -0.104181 -0.015163 0.049716 ( 0.000026 0.000044 0.000054 ) 0.087293 -0.167193 0.063623 ( 0.000022 0.000038 0.000047 ) 0.055501 -0.024380 0.122813 ( 0.000024 0.000041 0.000050 ) M - matrix: 0.021554 -0.014368 0.007191 ( 0.000007 0.000007 0.000008 ) -0.014368 0.028778 -0.014385 ( 0.000007 0.000013 0.000010 ) 0.007191 -0.014385 0.021603 ( 0.000008 0.000010 0.000015 ) UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) unit cell: 5.9149(19) 5.9091(19) 5.908(2) 60.03(4) 90.03(3) 60.03(3) V = 146.12(8) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104164 -0.015115 0.049699 ( 0.000014 0.000017 0.000018 ) 0.087353 -0.167108 0.063641 ( 0.000010 0.000012 0.000013 ) 0.055465 -0.024290 0.122641 ( 0.000013 0.000015 0.000016 ) M - matrix: 0.021557 -0.014370 0.007185 ( 0.000004 0.000003 0.000003 ) -0.014370 0.028743 -0.014365 ( 0.000003 0.000004 0.000003 ) 0.007185 -0.014365 0.021561 ( 0.000003 0.000003 0.000005 ) UB fit with 1110 obs out of 1110 (total:1110,skipped:0) (100.00%) unit cell: 5.9164(8) 5.9149(6) 5.9146(9) 60.024(13) 90.012(12) 60.002(13) V = 146.40(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 30 reflections under beam stop or inside a detector rejection region 9 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof 1501 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:11:01 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.895) Run 3 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.895) PROFFIT INFO: signal sum: min=161.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=604.9870 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=63 max=922 PROFFIT INFO: Inet: min=1319.9718 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.4040 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.06 max=412.87 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 24 110 192 315 343 589 997 1353 1501 Percent 0.0 0.0 1.6 7.3 12.8 21.0 22.9 39.2 66.4 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1501 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 1501 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1624742 150 2396352.29 135.90 100.00 1618224- 1052066 150 1323368.46 112.64 100.00 1044240- 324278 150 598411.60 92.33 100.00 320473- 220083 150 256487.02 69.02 100.00 220023- 166473 150 192173.75 49.67 100.00 166298- 135992 150 152554.03 36.22 100.00 135960- 101854 150 117567.76 31.09 100.00 101616- 6402 150 56690.57 20.62 100.00 6328- 3856 150 4788.29 4.77 82.67 3808- 1320 151 2818.26 3.32 44.37 ------------------------------------------------------------------------------------ 4887974- 1320 1501 509783.23 55.52 92.67 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 150 649673.10 84.30 100.00 1.24- 0.98 150 790638.36 72.92 97.33 0.98- 0.82 150 575201.16 61.31 96.00 0.82- 0.74 150 574367.08 65.27 95.33 0.74- 0.67 150 563759.90 60.06 93.33 0.67- 0.61 150 363326.25 44.43 94.00 0.61- 0.56 150 517927.94 52.37 96.67 0.56- 0.52 150 395311.27 42.60 82.67 0.52- 0.48 150 323779.80 34.95 84.00 0.48- 0.40 151 344946.32 37.14 87.42 ------------------------------------------------------------------------------------ 5.26- 0.40 1501 509783.23 55.52 92.67 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:11:01 2018 Sorting 1501 observations 254 unique observations with > 7.00 F2/sig(F2) 1501 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 49 265 Total number of frames 265 Maximum number of 254 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1501 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 24 134 Total number of frames 134 1206 observations > 7.00 F2/sig(F2) 1206 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 24 134 Total number of frames 134 Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 1206 removed 36 = 1170, unique = 252) 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 1170 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 24 134 Total number of frames 134 252 unique data precomputed (should be 252) 252 unique data with 1170 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 1170 removed 0 = 1170, unique = 252) 252 unique data precomputed (should be 252) 252 unique data with 1170 observations RMS deviation of equivalent data = 0.67909 Rint = 0.60997 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.58222, wR= 2.70410 Trying model 1 (ne=2, no=0)... Results: Rint= 0.65051, wR= 2.64699, Acormin=-0.073, Acormax=2.042, Acor_av=0.623 F test: Probability=0.000, F= 0.797 Trying model 2 (ne=2, no=1)... Results: Rint= 0.85604, wR= 2.14177, Acormin=-0.450, Acormax=1.734, Acor_av=0.245 F test: Probability=0.000, F= 0.459 Trying model 3 (ne=4, no=0)... Results: Rint= 0.68510, wR= 1.55070, Acormin=-0.119, Acormax=2.576, Acor_av=0.475 F test: Probability=0.000, F= 0.711 Trying model 4 (ne=4, no=1)... Results: Rint= 0.87968, wR= 1.86845, Acormin=-0.577, Acormax=2.049, Acor_av=0.215 F test: Probability=0.000, F= 0.430 Trying model 5 (ne=4, no=3)... Results: Rint= 0.91393, wR= 1.81244, Acormin=-0.508, Acormax=1.885, Acor_av=0.059 F test: Probability=0.000, F= 0.395 Trying model 6 (ne=6, no=0)... Results: Rint= 0.73659, wR= 2.94278, Acormin=-0.412, Acormax=3.052, Acor_av=0.356 F test: Probability=0.000, F= 0.606 Trying model 7 (ne=6, no=1)... Results: Rint= 0.88770, wR= 3.03172, Acormin=-0.742, Acormax=2.167, Acor_av=0.143 F test: Probability=0.000, F= 0.416 Trying model 8 (ne=6, no=3)... Results: Rint= 0.95062, wR= 1.90731, Acormin=-0.548, Acormax=1.806, Acor_av=0.054 F test: Probability=0.000, F= 0.360 Trying model 9 (ne=6, no=5)... Results: Rint= 0.90241, wR= 2.13562, Acormin=-0.317, Acormax=0.644, Acor_av=0.003 F test: Probability=0.000, F= 0.394 Trying model 10 (ne=8, no=0)... Results: Rint= 0.84496, wR= 3.24880, Acormin=-0.997, Acormax=2.684, Acor_av=0.167 F test: Probability=0.000, F= 0.452 Trying model 11 (ne=8, no=1)... Results: Rint= 0.89831, wR= 3.91228, Acormin=-0.394, Acormax=1.485, Acor_av=0.105 F test: Probability=0.000, F= 0.398 Trying model 12 (ne=8, no=3)... Results: Rint= 0.89942, wR= 1.86244, Acormin=-0.043, Acormax=0.053, Acor_av=0.002 F test: Probability=0.000, F= 0.394 Trying model 13 (ne=8, no=5)... Results: Rint= 0.87771, wR= 1.50664, Acormin=-0.060, Acormax=0.067, Acor_av=0.002 F test: Probability=0.000, F= 0.409 Trying model 14 (ne=8, no=7)... Results: Rint= 0.87304, wR= 1.31925, Acormin=-0.037, Acormax=0.089, Acor_av=0.002 F test: Probability=0.000, F= 0.406 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: 0.78672 There are 134 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: 2, max odd order: 0 (5 parameters) Refinement control: 138 pars with 9591 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.67909 Using Levenberg-Marquardt: 0.00010 New wR= 0.65214 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60997 with corrections 0.59167 Rint for all data: 0.78672 with corrections 0.78092 6 observations identified as outliers and rejected Cycle 2 wR= 0.61142 Using Levenberg-Marquardt: 0.00001 New wR= 0.60626 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.59011 with corrections 0.56471 Rint for all data: 0.78672 with corrections 0.78049 6 observations identified as outliers and rejected Cycle 3 wR= 0.59438 Using Levenberg-Marquardt: 0.00000 New wR= 0.58953 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.57337 with corrections 0.56716 Rint for all data: 0.78672 with corrections 0.79056 4 observations identified as outliers and rejected Cycle 4 wR= 0.57165 Using Levenberg-Marquardt: 0.00000 New wR= 0.57014 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56707 with corrections 0.58506 Rint for all data: 0.78672 with corrections 0.80409 0 observations identified as outliers and rejected Cycle 5 wR= 0.57014 Using Levenberg-Marquardt: 0.00000 New wR= 0.56940 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56707 with corrections 0.61454 Rint for all data: 0.78672 with corrections 0.82418 0 observations identified as outliers and rejected Final wR= 0.56940 Final frame scales: Min= 1.0000 Max= 10.3750 Final absorption correction factors: Amin= 0.1692 Amax= 1.7896 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 134 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: 2, max odd order: 0 (5 parameters) Refinement control: 138 pars with 9591 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.87588 Using Levenberg-Marquardt: 0.00010 New wR= 0.80712 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56707 with corrections 1.04468 Rint for all data: 0.78672 with corrections 1.13449 2 observations identified as outliers and rejected Cycle 2 wR= 0.79847 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= 0.73344 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56610 with corrections 1.24495 Rint for all data: 0.78672 with corrections 1.31150 0 observations identified as outliers and rejected Cycle 3 wR= 0.73344 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.85008 Using Levenberg-Marquardt: 0.10000 New wR= 0.67415 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56610 with corrections 1.38894 Rint for all data: 0.78672 with corrections 1.52687 0 observations identified as outliers and rejected Cycle 4 wR= 0.67415 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= 0.64462 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56610 with corrections 1.36010 Rint for all data: 0.78672 with corrections 1.43920 0 observations identified as outliers and rejected Cycle 5 wR= 0.64462 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.61966 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.56610 with corrections 1.14019 Rint for all data: 0.78672 with corrections 1.24082 0 observations identified as outliers and rejected Final wR= 0.61966 Final frame scales: Min= 1.0000 Max= 11.0189 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 52 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 51 pars with 1326 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.89651 Using Levenberg-Marquardt: 0.00010 New wR= 0.71425 There are 5 clusters with unrefined scales (size 1-40) Rint for refined data: 0.56610 with corrections 0.67306 Rint for all data: 0.78672 with corrections 0.84797 1 observations identified as outliers and rejected Cycle 2 wR= 0.62775 Using Levenberg-Marquardt: 0.00001 New wR= 0.60885 There are 5 clusters with unrefined scales (size 1-40) Rint for refined data: 0.56575 with corrections 0.60864 Rint for all data: 0.78672 with corrections 0.80775 0 observations identified as outliers and rejected Cycle 3 wR= 0.60320 Using Levenberg-Marquardt: 0.00000 New wR= 0.59649 There are 5 clusters with unrefined scales (size 1-40) Rint for refined data: 0.56575 with corrections 0.59170 Rint for all data: 0.78672 with corrections 0.79823 0 observations identified as outliers and rejected Cycle 4 wR= 0.59985 Using Levenberg-Marquardt: 0.00000 New wR= 0.59335 There are 5 clusters with unrefined scales (size 1-40) Rint for refined data: 0.56575 with corrections 0.56853 Rint for all data: 0.78672 with corrections 0.78749 1 observations identified as outliers and rejected Cycle 5 wR= 0.59280 Using Levenberg-Marquardt: 0.00000 New wR= 0.58726 There are 5 clusters with unrefined scales (size 1-40) Rint for refined data: 0.56547 with corrections 0.55399 Rint for all data: 0.78672 with corrections 0.78112 3 observations identified as outliers and rejected Final wR= 0.58726 Final frame scales: Min= 0.8367 Max= 2.1298 PROFFIT INFO: Inet (after scale3 abspack): min=1026.7557 max=5363064.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=207.1591 max=68471.2188 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1501 reflections read from tmp file 1189 reflections are rejected (1093 as outliers, 96 as groups of 1 refl) Redundancy: 1 2 3 4 5 6+ Number of groups: 0 76 26 14 4 1 Initial Chi^2= 0.82732 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.70340 Current error model SIG(F2)^2 = 321.32*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 226.02*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 226.02*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5363065- 1604777 150 2297303.82 88.73 100.00 1603610- 1037167 150 1282173.98 48.56 100.00 1034479- 305649 150 598589.07 43.77 100.00 304093- 211480 150 252749.82 30.89 100.00 211211- 166875 150 186266.51 21.35 100.00 165746- 133400 150 150410.71 16.60 100.00 133184- 102445 150 118122.66 14.11 100.00 102372- 6336 150 57578.84 9.73 96.67 6290- 3703 150 4736.64 3.15 38.67 3663- 1027 151 2757.52 2.56 21.19 ------------------------------------------------------------------------------------ 5363065- 1027 1501 494740.97 27.93 85.61 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 150 636755.10 56.58 98.00 1.24- 0.98 150 777565.16 41.60 94.00 0.98- 0.82 150 566190.40 30.59 90.67 0.82- 0.74 150 561149.95 29.70 89.33 0.74- 0.67 150 553881.68 26.52 87.33 0.67- 0.61 150 342544.37 19.81 82.67 0.61- 0.56 150 503972.39 23.21 86.67 0.56- 0.52 150 379154.87 18.98 76.67 0.52- 0.48 150 305012.03 15.75 72.00 0.48- 0.40 151 322333.13 16.61 78.81 ------------------------------------------------------------------------------------ 5.26- 0.40 1501 494740.97 27.93 85.61 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 150 636755.10 56.58 98.00 5.26- 0.98 300 707160.13 49.09 96.00 5.26- 0.82 450 660170.22 42.92 94.22 5.26- 0.74 600 635415.15 39.62 93.00 5.26- 0.67 750 619108.46 37.00 91.87 5.26- 0.61 900 573014.44 34.13 90.33 5.26- 0.56 1050 563151.29 32.57 89.81 5.26- 0.52 1200 540151.74 30.87 88.17 5.26- 0.48 1350 514025.10 29.19 86.37 5.26- 0.40 1501 494740.97 27.93 85.61 ------------------------------------------------------------------------------------ 5.26- 0.40 1501 494740.97 27.93 85.61 Scale applied to data: s=0.186460 (maximum obs:5363064.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.781; Rsigma 0.023: data 1501 -> merged 305 With outlier rejection... Rint 0.712; Rsigma 0.024: data 1376 -> merged 305 Rejected total: 125, method kkm 119, method Blessing 6 Completeness direct cell (a, b, c) = (5.270, 5.270, 5.270), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404225, 5.270445 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 5.07 100.00 76 1.46 - 1.12 15 15 6.60 100.00 99 1.08 - 0.96 15 15 6.67 100.00 100 0.96 - 0.85 15 15 7.60 100.00 114 0.85 - 0.79 15 15 5.93 100.00 89 0.79 - 0.73 14 15 5.79 93.33 81 0.73 - 0.69 15 15 5.07 100.00 76 0.69 - 0.65 14 15 6.14 93.33 86 0.65 - 0.63 12 15 4.25 80.00 51 0.63 - 0.60 21 21 4.33 100.00 91 --------------------------------------------------------------- 5.91 - 0.60 151 156 5.72 96.79 863 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:11:02 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916401 5.914906 5.914578 60.0240 90.0116 60.0021 1376 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.15 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 674 717 701 693 1046 934 912 1376 N (int>3sigma) = 0 558 717 585 578 930 802 778 1174 Mean intensity = 0.0 80.4 35.8 78.9 86.2 64.6 90.6 87.7 88.4 Mean int/sigma = 0.0 25.2 22.7 25.2 26.1 24.4 27.2 27.2 27.1 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.916 60.01 60.02 60.02 Niggli form: a.a = 34.982 b.b = 34.986 c.c = 34.997 b.c = 17.490 a.c = 17.486 a.b = 17.479 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.020 CUBIC F-lattice R(int) = 0.141 [ 1225] Vol = 585.6 Cell: 8.367 8.365 8.367 90.02 90.01 90.02 Volume: 585.60 Matrix:-1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.017 RHOMBOHEDRAL R-lattice R(int) = 0.129 [ 965] Vol = 439.2 Cell: 5.917 5.917 14.487 90.02 90.00 120.00 Volume: 439.20 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.017 RHOMBOHEDRAL R-lattice R(int) = 0.121 [ 293] Vol = 439.2 Trigonal Cell: 5.917 5.917 14.487 90.02 90.00 120.00 Volume: 439.20 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.013 RHOMBOHEDRAL R-lattice R(int) = 0.137 [ 966] Vol = 439.2 Cell: 5.915 5.917 14.493 90.00 90.00 120.01 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.013 RHOMBOHEDRAL R-lattice R(int) = 0.129 [ 296] Vol = 439.2 Trigonal Cell: 5.915 5.917 14.493 90.00 90.00 120.01 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.017 ORTHORHOMBIC I-lattice R(int) = 0.128 [ 969] Vol = 292.8 Cell: 5.915 5.916 8.367 90.00 89.98 90.01 Volume: 292.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.119 [ 954] Vol = 292.8 Cell: 5.916 8.365 5.917 90.00 89.99 90.02 Volume: 292.80 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.005 MONOCLINIC I-lattice R(int) = 0.117 [ 698] Vol = 292.8 Cell: 5.916 5.917 8.365 90.00 90.02 90.01 Volume: 292.80 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.013 MONOCLINIC I-lattice R(int) = 0.127 [ 799] Vol = 292.8 Cell: 5.915 5.916 8.367 90.00 90.02 90.01 Volume: 292.80 Matrix: 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.013 MONOCLINIC I-lattice R(int) = 0.122 [ 716] Vol = 292.8 Cell: 5.916 5.915 8.367 90.02 90.00 90.01 Volume: 292.80 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.122 [ 716] Vol = 292.8 Cell: 8.367 5.915 5.916 90.01 90.00 90.02 Volume: 292.80 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.119 [ 525] Vol = 146.4 Cell: 5.915 5.915 5.916 60.01 60.02 60.02 Volume: 146.40 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 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 0 717 0 934 920 1376 N (int>3sigma) = 0 0 0 0 717 0 802 784 1174 Mean intensity = 0.0 0.0 0.0 0.0 35.8 0.0 90.6 88.5 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.7 0.0 27.2 26.9 27.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.211 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 99 304 N I>3s 7 7 56 304 1.2 1.2 0.8 40.8 7.6 7.6 3.8 27.5 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 0.141 1145 Fd-3m 1 1 227 C N N N N 37 2284 0.143 1182 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366612 8.364919 8.367393 90.0167 90.0101 90.0177 ZERR 1.00 0.002012 0.000332 0.003338 0.0128 0.0007 0.0006 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3839703- 1059988 132 116 30 3.9 1577593.79 63.43 0.430 0.309 1053585- 818403 173 162 30 5.4 903700.79 39.32 0.841 0.680 799597- 613718 184 177 30 5.9 673551.31 33.63 0.942 0.926 608736- 472779 196 180 30 6.0 461037.41 29.13 0.929 0.989 463941- 296089 186 164 30 5.5 309615.36 25.49 0.828 0.845 273548- 170341 177 156 30 5.2 189039.66 22.06 0.408 0.348 164780- 130654 110 100 30 3.3 147892.59 15.56 0.218 0.183 128566- 103189 123 112 30 3.7 118817.96 14.59 0.364 0.282 102372- 69276 111 104 30 3.5 82562.39 10.03 0.724 0.600 64614- 1652 109 105 35 3.0 33229.25 5.49 0.802 0.722 ------------------------------------------------------------------------------------------- 3839703- 1652 1501 1376 305 4.5 473870.10 27.15 0.712 0.589 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 204 175 30 5.8 646765.50 52.33 0.543 0.402 0.013 1.08-0.85 232 214 30 7.1 636647.90 34.19 0.845 0.749 0.018 0.85-0.73 184 172 30 5.7 578962.30 29.43 0.722 0.624 0.021 0.72-0.65 193 183 32 5.7 421294.97 23.21 0.855 0.833 0.026 0.65-0.60 141 129 31 4.2 459363.98 22.67 0.717 0.766 0.027 0.59-0.56 136 128 30 4.3 360663.69 18.89 0.691 0.608 0.032 0.55-0.51 131 126 31 4.1 401448.30 19.19 0.861 0.816 0.031 0.51-0.49 113 103 31 3.3 302385.43 15.90 0.544 0.388 0.036 0.48-0.45 98 86 30 2.9 275902.01 15.34 0.392 0.302 0.040 0.45-0.40 69 60 30 2.0 251024.79 14.28 0.277 0.200 0.043 ------------------------------------------------------------------------------------------------------ inf-0.40 1501 1376 305 4.5 473870.10 27.15 0.712 0.589 0.024 inf-0.60 941 863 151 5.7 560572.85 33.08 0.737 0.638 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 175 30 30 100.0 5.8 646765.50 152.91 0.543 0.006 1.08-0.85 214 30 30 100.0 7.1 636647.90 120.97 0.845 0.009 0.85-0.73 172 31 30 96.8 5.7 578962.30 90.84 0.722 0.011 0.72-0.65 183 35 32 91.4 5.7 421294.97 72.37 0.855 0.014 0.65-0.60 129 32 31 96.9 4.2 459363.98 63.30 0.717 0.016 0.59-0.56 128 38 30 78.9 4.3 360663.69 48.49 0.691 0.017 0.55-0.51 126 41 31 75.6 4.1 401448.30 50.45 0.861 0.018 0.51-0.49 103 43 31 72.1 3.3 302385.43 36.18 0.544 0.021 0.48-0.45 86 61 30 49.2 2.9 275902.01 28.18 0.392 0.025 0.45-0.40 60 121 30 24.8 2.0 251024.79 22.56 0.277 0.031 -------------------------------------------------------------------------------------------- inf-0.40 1376 464 305 65.7 4.5 473870.10 79.76 0.712 0.014 inf-0.60 863 156 151 96.8 5.7 560572.85 103.42 0.737 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 1.0 1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 1.0 1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.076930 -0.034790 -0.007558 ( 0.000008 0.000007 0.000008 ) -0.011856 -0.008057 -0.083554 ( 0.000006 0.000005 0.000006 ) 0.033586 0.076908 -0.012145 ( 0.000008 0.000007 0.000008 ) M - matrix: 0.007187 0.000002 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007190 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.000002 0.007186 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.076930 -0.034790 -0.007558 ( 0.000008 0.000007 0.000008 ) -0.011856 -0.008057 -0.083554 ( 0.000006 0.000005 0.000006 ) 0.033586 0.076908 -0.012145 ( 0.000008 0.000007 0.000008 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3668(8) 8.3649(7) 8.3674(6) 90.017(6) 90.011(7) 90.017(7) V = 585.61(9) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.895) Run 3 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.895) PROFFIT INFO: signal sum: min=161.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=604.9870 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=63 max=922 PROFFIT INFO: Inet: min=1319.9718 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.4040 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=1.06 max=412.87 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 48 220 384 630 686 1178 1994 2706 3002 Percent 0.0 0.0 1.6 7.3 12.8 21.0 22.9 39.2 66.4 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1501 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 1501 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1624742 150 2396352.29 135.90 100.00 1618224- 1052066 150 1323368.46 112.64 100.00 1044240- 324278 150 598411.60 92.33 100.00 320473- 220083 150 256487.02 69.02 100.00 220023- 166473 150 192173.75 49.67 100.00 166298- 135992 150 152554.03 36.22 100.00 135960- 101854 150 117567.76 31.09 100.00 101616- 6402 150 56690.57 20.62 100.00 6328- 3856 150 4788.29 4.77 82.67 3808- 1320 151 2818.26 3.32 44.37 ------------------------------------------------------------------------------------ 4887974- 1320 1501 509783.23 55.52 92.67 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 150 672095.36 80.79 98.67 1.39- 1.09 150 975110.84 83.15 99.33 1.09- 0.96 150 543603.18 67.68 98.67 0.96- 0.85 150 580808.93 66.31 96.00 0.85- 0.80 150 600108.57 64.58 98.67 0.80- 0.73 150 373329.05 42.62 94.00 0.73- 0.70 150 290616.63 36.33 91.33 0.70- 0.65 150 526764.48 51.85 92.67 0.65- 0.62 150 269838.76 31.60 80.67 0.62- 0.58 151 267173.86 30.49 76.82 ------------------------------------------------------------------------------------ 4.82- 0.58 1501 509783.23 55.52 92.67 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:11:02 2018 Sorting 1501 observations 83 unique observations with > 7.00 F2/sig(F2) 1501 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 49 265 Total number of frames 265 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1501 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 12 68 Total number of frames 68 1206 observations > 7.00 F2/sig(F2) 1206 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 12 68 Total number of frames 68 Removing 'redundancy=1' reflections Average redundancy: 14.1 (Out of 1206 removed 6 = 1200, 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): 4/m3bar2/m 1200 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 12 68 Total number of frames 68 85 unique data precomputed (should be 85) 85 unique data with 1200 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 14.1 (Out of 1200 removed 0 = 1200, unique = 85) 85 unique data precomputed (should be 85) 85 unique data with 1200 observations RMS deviation of equivalent data = 0.21600 Rint = 0.15299 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.14888, wR= 0.21597 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06192, wR= 0.08459, Acormin=0.641, Acormax=1.452, Acor_av=0.866 F test: Probability=1.000, F= 5.755 Trying model 2 (ne=2, no=1)... Results: Rint= 0.05923, wR= 0.08046, Acormin=0.602, Acormax=1.421, Acor_av=0.815 F test: Probability=0.924, F= 1.090 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04920, wR= 0.06830, Acormin=0.651, Acormax=1.531, Acor_av=0.868 F test: Probability=1.000, F= 1.571 Trying model 4 (ne=4, no=1)... Results: Rint= 0.04494, wR= 0.06449, Acormin=0.590, Acormax=1.493, Acor_av=0.850 F test: Probability=0.998, F= 1.195 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03996, wR= 0.05483, Acormin=0.515, Acormax=1.399, Acor_av=0.807 F test: Probability=1.000, F= 1.257 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04211, wR= 0.05820, Acormin=0.639, Acormax=1.524, Acor_av=0.862 F test: Probability=0.000, F= 0.898 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03792, wR= 0.05396, Acormin=0.582, Acormax=1.508, Acor_av=0.845 F test: Probability=0.948, F= 1.104 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03256, wR= 0.04513, Acormin=0.540, Acormax=1.434, Acor_av=0.814 F test: Probability=1.000, F= 1.488 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03092, wR= 0.04191, Acormin=0.428, Acormax=1.214, Acor_av=0.671 F test: Probability=0.935, F= 1.097 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03859, wR= 0.05071, Acormin=0.598, Acormax=1.439, Acor_av=0.830 F test: Probability=0.000, F= 0.707 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02993, wR= 0.04111, Acormin=0.518, Acormax=1.418, Acor_av=0.798 F test: Probability=0.995, F= 1.172 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02935, wR= 0.03870, Acormin=0.438, Acormax=1.243, Acor_av=0.686 F test: Probability=0.704, F= 1.033 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02769, wR= 0.03614, Acormin=0.455, Acormax=1.335, Acor_av=0.715 F test: Probability=0.988, F= 1.149 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02502, wR= 0.03377, Acormin=0.468, Acormax=1.403, Acor_av=0.736 F test: Probability=0.999, F= 1.207 Final absorption model (ne=8, no=7): Rint= 0.02502, Acormin=0.468, Acormax=1.403, Acor_av=0.736 Combined refinement in use Rint: 0.15310 There are 68 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 147 pars with 10878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21600 Using Levenberg-Marquardt: 0.00010 New wR= 0.04295 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15299 with corrections 0.02838 Rint for all data: 0.15310 with corrections 0.02859 1 observations identified as outliers and rejected Cycle 2 wR= 0.03766 Using Levenberg-Marquardt: 0.00001 New wR= 0.02565 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15181 with corrections 0.01907 Rint for all data: 0.15310 with corrections 0.01937 0 observations identified as outliers and rejected Cycle 3 wR= 0.02565 Using Levenberg-Marquardt: 0.00000 New wR= 0.02502 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15181 with corrections 0.01843 Rint for all data: 0.15310 with corrections 0.01882 0 observations identified as outliers and rejected Cycle 4 wR= 0.02502 Using Levenberg-Marquardt: 0.00000 New wR= 0.02487 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15181 with corrections 0.01824 Rint for all data: 0.15310 with corrections 0.01866 0 observations identified as outliers and rejected Cycle 5 wR= 0.02487 Using Levenberg-Marquardt: 0.00000 New wR= 0.02478 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15181 with corrections 0.01815 Rint for all data: 0.15310 with corrections 0.01857 0 observations identified as outliers and rejected Final wR= 0.02478 Final frame scales: Min= 0.9009 Max= 1.1395 Final absorption correction factors: Amin= 0.4762 Amax= 1.5060 PROFFIT INFO: Inet (after scale3 abspack): min=1211.8040 max=4122895.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=265.4225 max=69346.1172 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1501 reflections read from tmp file 75 reflections are rejected (71 as outliers, 4 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 6 3 5 5 4 3 4 73 Initial Chi^2= 0.24508 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.00719 Current error model SIG(F2)^2 = 92.73*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 186.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 186.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4122896- 1523780 150 2320928.27 99.94 100.00 1523221- 1006335 150 1258654.71 51.99 100.00 1001642- 315762 150 604817.38 49.72 100.00 312351- 208271 150 249533.48 33.18 100.00 206977- 174825 150 190373.88 23.54 100.00 174126- 129632 150 143892.03 17.47 100.00 129392- 102304 150 115124.26 15.26 100.00 101644- 5954 150 57143.89 10.65 97.33 5946- 3577 150 4500.73 3.39 56.00 3572- 1212 151 2813.92 2.79 26.49 ------------------------------------------------------------------------------------ 4122896- 1212 1501 494450.50 30.78 87.94 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 150 707844.40 59.00 96.67 1.39- 1.09 150 994450.90 55.51 99.33 1.09- 0.96 150 512512.39 34.70 96.67 0.96- 0.85 150 575970.48 32.21 90.00 0.85- 0.80 150 559735.89 31.31 96.67 0.80- 0.73 150 342070.36 21.00 84.00 0.73- 0.70 150 288804.34 18.01 82.00 0.70- 0.65 150 474735.48 25.21 88.67 0.65- 0.62 150 246460.37 15.73 75.33 0.62- 0.58 151 243592.76 15.18 70.20 ------------------------------------------------------------------------------------ 4.82- 0.58 1501 494450.50 30.78 87.94 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 150 707844.40 59.00 96.67 4.82- 1.09 300 851147.65 57.26 98.00 4.82- 0.96 450 738269.23 49.74 97.56 4.82- 0.85 600 697694.54 45.35 95.67 4.82- 0.80 750 670102.81 42.55 95.87 4.82- 0.73 900 615430.74 38.95 93.89 4.82- 0.70 1050 568769.82 35.96 92.19 4.82- 0.65 1200 557015.53 34.62 91.75 4.82- 0.62 1350 522509.40 32.52 89.93 4.82- 0.58 1501 494450.50 30.78 87.94 ------------------------------------------------------------------------------------ 4.82- 0.58 1501 494450.50 30.78 87.94 Scale applied to data: s=0.242548 (maximum obs:4122895.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.019; Rsigma 0.021: data 1501 -> merged 108 With outlier rejection... Rint 0.017; Rsigma 0.021: data 1492 -> merged 108 Rejected total: 9, method kkm 6, method Blessing 3 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585763, 4.830322 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 9 10 7.89 90.00 71 1.61 - 1.21 10 10 13.20 100.00 132 1.17 - 1.01 10 10 17.70 100.00 177 0.99 - 0.89 10 10 17.60 100.00 176 0.88 - 0.81 10 10 17.00 100.00 170 0.81 - 0.74 10 10 15.10 100.00 151 0.73 - 0.71 10 10 16.40 100.00 164 0.70 - 0.66 10 10 13.40 100.00 134 0.66 - 0.64 10 10 12.60 100.00 126 0.63 - 0.60 10 10 12.60 100.00 126 --------------------------------------------------------------- 5.91 - 0.60 99 100 14.41 99.00 1427 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:11:02 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916401 5.914906 5.914578 60.0240 90.0116 60.0021 1376 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.15 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 674 717 701 693 1046 934 912 1376 N (int>3sigma) = 0 558 717 585 578 930 802 778 1174 Mean intensity = 0.0 80.4 35.8 78.9 86.2 64.6 90.6 87.7 88.4 Mean int/sigma = 0.0 25.2 22.7 25.2 26.1 24.4 27.2 27.2 27.1 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.916 60.01 60.02 60.02 Niggli form: a.a = 34.982 b.b = 34.986 c.c = 34.997 b.c = 17.490 a.c = 17.486 a.b = 17.479 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.020 CUBIC F-lattice R(int) = 0.141 [ 1225] Vol = 585.6 Cell: 8.367 8.365 8.367 90.02 90.01 90.02 Volume: 585.60 Matrix:-1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.017 RHOMBOHEDRAL R-lattice R(int) = 0.129 [ 965] Vol = 439.2 Cell: 5.917 5.917 14.487 90.02 90.00 120.00 Volume: 439.20 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.017 RHOMBOHEDRAL R-lattice R(int) = 0.121 [ 293] Vol = 439.2 Trigonal Cell: 5.917 5.917 14.487 90.02 90.00 120.00 Volume: 439.20 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.013 RHOMBOHEDRAL R-lattice R(int) = 0.137 [ 966] Vol = 439.2 Cell: 5.915 5.917 14.493 90.00 90.00 120.01 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.013 RHOMBOHEDRAL R-lattice R(int) = 0.129 [ 296] Vol = 439.2 Trigonal Cell: 5.915 5.917 14.493 90.00 90.00 120.01 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.017 ORTHORHOMBIC I-lattice R(int) = 0.128 [ 969] Vol = 292.8 Cell: 5.915 5.916 8.367 90.00 89.98 90.01 Volume: 292.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.119 [ 954] Vol = 292.8 Cell: 5.916 8.365 5.917 90.00 89.99 90.02 Volume: 292.80 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.005 MONOCLINIC I-lattice R(int) = 0.117 [ 698] Vol = 292.8 Cell: 5.916 5.917 8.365 90.00 90.02 90.01 Volume: 292.80 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.013 MONOCLINIC I-lattice R(int) = 0.127 [ 799] Vol = 292.8 Cell: 5.915 5.916 8.367 90.00 90.02 90.01 Volume: 292.80 Matrix: 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.013 MONOCLINIC I-lattice R(int) = 0.122 [ 716] Vol = 292.8 Cell: 5.916 5.915 8.367 90.02 90.00 90.01 Volume: 292.80 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.122 [ 716] Vol = 292.8 Cell: 8.367 5.915 5.916 90.01 90.00 90.02 Volume: 292.80 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.119 [ 525] Vol = 146.4 Cell: 5.915 5.915 5.916 60.01 60.02 60.02 Volume: 146.40 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 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 0 717 0 934 920 1376 N (int>3sigma) = 0 0 0 0 717 0 802 784 1174 Mean intensity = 0.0 0.0 0.0 0.0 35.8 0.0 90.6 88.5 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.7 0.0 27.2 26.9 27.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.211 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 99 304 N I>3s 7 7 56 304 1.2 1.2 0.8 40.8 7.6 7.6 3.8 27.5 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 0.141 1145 Fd-3m 1 1 227 C N N N N 37 2284 0.143 1182 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366612 8.364919 8.367393 90.0167 90.0101 90.0177 ZERR 1.00 0.002012 0.000332 0.003338 0.0128 0.0007 0.0006 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4024729- 878533 346 340 27 12.6 1656817.05 69.03 0.015 0.018 868213- 150239 447 446 27 16.5 268119.50 33.46 0.023 0.027 141885- 24109 366 366 27 13.6 110166.92 14.78 0.031 0.037 11114- 1641 342 340 27 12.6 4162.79 3.34 0.152 0.180 ------------------------------------------------------------------------------------------- 4024729- 1641 1501 1492 108 13.8 485680.65 30.12 0.017 0.021 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-1.01 371 363 27 13.4 716782.96 49.63 0.016 0.018 0.013 1.01-0.78 457 456 27 16.9 504461.05 29.30 0.016 0.020 0.020 0.76-0.65 400 400 28 14.3 401889.54 22.46 0.019 0.022 0.028 0.65-0.59 273 273 26 10.5 269792.18 16.78 0.024 0.028 0.038 ------------------------------------------------------------------------------------------------------ inf-0.59 1501 1492 108 13.8 485680.65 30.12 0.017 0.021 0.021 inf-0.60 1434 1425 98 14.5 498550.11 30.85 0.017 0.020 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.01 363 28 27 96.4 13.4 716782.96 188.85 0.016 0.004 1.01-0.78 456 27 27 100.0 16.9 504461.05 123.43 0.016 0.005 0.76-0.65 400 28 28 100.0 14.3 401889.54 91.17 0.019 0.008 0.65-0.59 273 27 26 96.3 10.5 269792.18 61.32 0.024 0.013 -------------------------------------------------------------------------------------------- inf-0.59 1492 110 108 98.2 13.8 485680.65 119.33 0.017 0.006 inf-0.60 1425 99 98 99.0 14.5 498550.11 122.84 0.017 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:16:12 2018) ID: 2932; threads 39; handles 879; mem 518868.00 (1238752.00)kB; time: 1w 5d 22h 21m 43s MEMORY INFO: Memory PF:0.0, Ph:164.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.7,peak PF: 708.5, WS: 270.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:164.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.5,peak PF: 708.5, WS: 272.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:16:12 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000017 0.000018 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000012 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000013 0.000015 0.000016 ) 5.91535 ( 0.00080 ) 5.92288 ( 0.00064 ) 5.91286 ( 0.00086 ) 59.95509 ( 0.01319 ) 89.89521 ( 0.01151 ) 59.99590 ( 0.01272 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:16:13 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000017 0.000018 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000012 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000013 0.000015 0.000016 ) M - matrix: 0.021557 -0.014370 0.007185 ( 0.000004 0.000003 0.000003 ) -0.014370 0.028743 -0.014365 ( 0.000003 0.000004 0.000003 ) 0.007185 -0.014365 0.021561 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(8) 5.9229(6) 5.9129(9) 59.955(13) 89.895(12) 59.996(13) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_3_51.rpb PROFFITPEAK info: 773 peaks in the peak location table UB fit with 379 obs out of 385 (total:385,skipped:0) (98.44%) UB - matrix: -0.104344 -0.014767 0.049319 ( 0.000046 0.000067 0.000068 ) 0.087166 -0.167048 0.063650 ( 0.000057 0.000081 0.000083 ) 0.055547 -0.024719 0.122924 ( 0.000056 0.000080 0.000082 ) M - matrix: 0.021571 -0.014393 0.007230 ( 0.000015 0.000015 0.000014 ) -0.014393 0.028734 -0.014399 ( 0.000015 0.000028 0.000018 ) 0.007230 -0.014399 0.021594 ( 0.000014 0.000018 0.000024 ) unit cell: 5.919(3) 5.922(3) 5.915(4) 60.00(7) 90.07(5) 60.00(6) V = 146.50(15) UB fit with 379 obs out of 385 (total:385,skipped:0) (98.44%) UB - matrix: -0.104344 -0.014767 0.049319 ( 0.000046 0.000067 0.000068 ) 0.087166 -0.167048 0.063650 ( 0.000057 0.000081 0.000083 ) 0.055547 -0.024719 0.122924 ( 0.000056 0.000080 0.000082 ) M - matrix: 0.021571 -0.014393 0.007230 ( 0.000015 0.000015 0.000014 ) -0.014393 0.028734 -0.014399 ( 0.000015 0.000028 0.000018 ) 0.007230 -0.014399 0.021594 ( 0.000014 0.000018 0.000024 ) unit cell: 5.919(3) 5.922(3) 5.915(4) 60.00(7) 90.07(5) 60.00(6) V = 146.50(15) OTKP changes: 74 1 1 1 UB - matrix: -0.104127 -0.014595 0.048889 ( 0.000043 0.000062 0.000063 ) 0.086746 -0.166593 0.063601 ( 0.000056 0.000080 0.000082 ) 0.055074 -0.024312 0.122503 ( 0.000054 0.000078 0.000079 ) M - matrix: 0.021400 -0.014271 0.007173 ( 0.000015 0.000014 0.000013 ) -0.014271 0.028557 -0.014287 ( 0.000014 0.000027 0.000018 ) 0.007173 -0.014287 0.021442 ( 0.000013 0.000018 0.000023 ) UB fit with 380 obs out of 385 (total:385,skipped:0) (98.70%) unit cell: 5.938(3) 5.932(3) 5.933(4) 60.05(7) 90.13(5) 60.06(5) V = 147.86(15) UB fit with 380 obs out of 385 (total:385,skipped:0) (98.70%) UB - matrix: -0.104127 -0.014595 0.048889 ( 0.000043 0.000062 0.000063 ) 0.086746 -0.166593 0.063601 ( 0.000056 0.000080 0.000082 ) 0.055074 -0.024312 0.122503 ( 0.000054 0.000078 0.000079 ) M - matrix: 0.021400 -0.014271 0.007173 ( 0.000015 0.000014 0.000013 ) -0.014271 0.028557 -0.014287 ( 0.000014 0.000027 0.000018 ) 0.007173 -0.014287 0.021442 ( 0.000013 0.000018 0.000023 ) unit cell: 5.938(3) 5.932(3) 5.933(4) 60.05(7) 90.13(5) 60.06(5) V = 147.86(15) OTKP changes: 74 1 1 1 UB - matrix: -0.104096 -0.014600 0.048876 ( 0.000043 0.000062 0.000063 ) 0.086740 -0.166578 0.063603 ( 0.000056 0.000080 0.000082 ) 0.055042 -0.024279 0.122489 ( 0.000054 0.000078 0.000080 ) M - matrix: 0.021389 -0.014266 0.007171 ( 0.000015 0.000014 0.000013 ) -0.014266 0.028551 -0.014282 ( 0.000014 0.000027 0.000018 ) 0.007171 -0.014282 0.021438 ( 0.000013 0.000018 0.000023 ) UB fit with 380 obs out of 385 (total:385,skipped:0) (98.70%) unit cell: 5.939(3) 5.932(3) 5.933(4) 60.06(7) 90.14(5) 60.07(5) V = 147.92(15) 385 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Run 3 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.243) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104096 -0.014600 0.048876 ( 0.000043 0.000062 0.000063 ) 0.086740 -0.166578 0.063603 ( 0.000056 0.000080 0.000082 ) 0.055042 -0.024279 0.122489 ( 0.000054 0.000078 0.000080 ) M - matrix: 0.021389 -0.014266 0.007171 ( 0.000015 0.000014 0.000013 ) -0.014266 0.028551 -0.014282 ( 0.000014 0.000027 0.000018 ) 0.007171 -0.014282 0.021438 ( 0.000013 0.000018 0.000023 ) UB fit with 380 obs out of 385 (total:385,skipped:0) (98.70%) unit cell: 5.939(3) 5.932(3) 5.933(4) 60.06(7) 90.14(5) 60.07(5) V = 147.92(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 380 obs out of 385 (total:385,skipped:0) (98.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_51.rpb 3 of 325 peaks identified as outliers and rejected 322 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 322 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 322 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.48 | 32 | 1.066 ( 0.234) | 1.310 ( 0.827) | 1.654 ( 2.017) | 1.47- 1.17 | 32 | 1.107 ( 0.178) | 1.081 ( 0.066) | 1.192 ( 0.727) | 1.16- 0.99 | 32 | 1.109 ( 0.084) | 1.084 ( 0.087) | 1.151 ( 0.457) | 0.98- 0.92 | 32 | 1.149 ( 0.065) | 1.108 ( 0.084) | 1.144 ( 0.395) | 0.92- 0.82 | 32 | 1.172 ( 0.076) | 1.103 ( 0.083) | 1.233 ( 0.398) | 0.82- 0.76 | 32 | 1.207 ( 0.050) | 1.095 ( 0.087) | 1.302 ( 0.400) | 0.76- 0.71 | 32 | 1.222 ( 0.060) | 1.104 ( 0.125) | 1.171 ( 0.410) | 0.71- 0.67 | 32 | 1.238 ( 0.050) | 1.143 ( 0.135) | 1.249 ( 0.509) | 0.67- 0.63 | 32 | 1.248 ( 0.082) | 1.158 ( 0.163) | 1.376 ( 0.586) | 0.63- 0.59 | 34 | 1.306 ( 0.063) | 1.128 ( 0.170) | 1.438 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 322 | 1.183 ( 0.132) | 1.131 ( 0.291) | 1.292 ( 0.808) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 322 obs out of 322 (total:322,skipped:0) (100.00%) UB - matrix: -0.104077 -0.014733 0.049049 ( 0.000027 0.000040 0.000040 ) 0.086931 -0.166856 0.063638 ( 0.000027 0.000040 0.000040 ) 0.054788 -0.024304 0.122683 ( 0.000030 0.000043 0.000044 ) M - matrix: 0.021391 -0.014303 0.007149 ( 0.000008 0.000008 0.000007 ) -0.014303 0.028649 -0.014323 ( 0.000008 0.000014 0.000009 ) 0.007149 -0.014323 0.021507 ( 0.000007 0.000009 0.000012 ) unit cell: 5.9419(17) 5.9270(18) 5.922(2) 60.03(4) 89.99(3) 59.96(3) V = 147.46(8) OTKP changes: 321 1 1 1 UB - matrix: -0.104436 -0.014910 0.049350 ( 0.000026 0.000038 0.000039 ) 0.087229 -0.167233 0.063626 ( 0.000025 0.000036 0.000036 ) 0.055464 -0.024720 0.123089 ( 0.000022 0.000032 0.000033 ) M - matrix: 0.021592 -0.014401 0.007223 ( 0.000007 0.000007 0.000006 ) -0.014401 0.028800 -0.014419 ( 0.000007 0.000012 0.000008 ) 0.007223 -0.014419 0.021635 ( 0.000006 0.000008 0.000010 ) UB fit with 322 obs out of 322 (total:322,skipped:0) (100.00%) unit cell: 5.9128(16) 5.9112(15) 5.9076(17) 60.01(3) 90.05(2) 60.02(3) V = 145.99(7) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.865) HKL list info: 575 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104436 -0.014910 0.049350 ( 0.000026 0.000038 0.000039 ) 0.087229 -0.167233 0.063626 ( 0.000025 0.000036 0.000036 ) 0.055464 -0.024720 0.123089 ( 0.000022 0.000032 0.000033 ) M - matrix: 0.021592 -0.014401 0.007223 ( 0.000007 0.000007 0.000006 ) -0.014401 0.028800 -0.014419 ( 0.000007 0.000012 0.000008 ) 0.007223 -0.014419 0.021635 ( 0.000006 0.000008 0.000010 ) UB fit with 322 obs out of 322 (total:322,skipped:0) (100.00%) unit cell: 5.9128(16) 5.9112(15) 5.9076(17) 60.01(3) 90.05(2) 60.02(3) V = 145.99(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 322 obs out of 322 (total:322,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_51.rpb 5 of 324 peaks identified as outliers and rejected 319 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 319 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 319 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.47 | 32 | 1.056 ( 0.206) | 1.250 ( 0.749) | 1.406 ( 1.044) | 1.41- 1.12 | 32 | 1.076 ( 0.079) | 1.081 ( 0.074) | 1.022 ( 0.438) | 1.12- 0.98 | 32 | 1.127 ( 0.070) | 1.097 ( 0.085) | 1.173 ( 0.438) | 0.96- 0.92 | 32 | 1.156 ( 0.071) | 1.117 ( 0.085) | 1.142 ( 0.397) | 0.89- 0.82 | 32 | 1.181 ( 0.079) | 1.124 ( 0.076) | 1.205 ( 0.384) | 0.82- 0.75 | 32 | 1.215 ( 0.050) | 1.102 ( 0.107) | 1.330 ( 0.386) | 0.75- 0.71 | 32 | 1.224 ( 0.062) | 1.121 ( 0.128) | 1.179 ( 0.426) | 0.71- 0.67 | 32 | 1.255 ( 0.050) | 1.138 ( 0.116) | 1.301 ( 0.486) | 0.67- 0.62 | 32 | 1.243 ( 0.077) | 1.161 ( 0.171) | 1.408 ( 0.548) | 0.62- 0.59 | 31 | 1.304 ( 0.066) | 1.146 ( 0.186) | 1.326 ( 0.575) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 319 | 1.183 ( 0.119) | 1.134 ( 0.267) | 1.249 ( 0.558) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.3 | 122 | 1.151 ( 0.083) | 1.248 ( 0.322) | 1.341 ( 0.616) | 13.5-19.1 | 122 | 1.145 ( 0.100) | 1.203 ( 0.293) | 1.342 ( 0.700) | 19.2-23.3 | 122 | 1.167 ( 0.093) | 1.244 ( 0.364) | 1.290 ( 0.653) | 23.3-27.6 | 122 | 1.145 ( 0.096) | 1.187 ( 0.327) | 1.217 ( 0.525) | 27.6-30.8 | 122 | 1.142 ( 0.109) | 1.165 ( 0.194) | 1.195 ( 0.401) | 30.8-34.3 | 122 | 1.155 ( 0.089) | 1.168 ( 0.235) | 1.193 ( 0.426) | 34.3-37.3 | 122 | 1.147 ( 0.107) | 1.131 ( 0.171) | 1.153 ( 0.391) | 37.3-39.9 | 122 | 1.157 ( 0.123) | 1.135 ( 0.204) | 1.282 ( 0.561) | 39.9-43.0 | 122 | 1.169 ( 0.116) | 1.108 ( 0.198) | 1.220 ( 0.603) | 43.0-49.8 | 119 | 1.214 ( 0.166) | 1.145 ( 0.252) | 1.218 ( 0.491) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1217 | 1.159 ( 0.112) | 1.174 ( 0.268) | 1.245 ( 0.550) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0012 b=1.03 e3 dimension: a=-0.0024 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4955 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 453201 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 2567504 PROFFITPEAK - Finished at Wed Mar 28 13:16:23 2018 PROFFITMAIN - Started at Wed Mar 28 13:16:23 2018 OTKP changes: 1217 2 2 3 OTKP changes: 1217 2 2 3 UB - matrix: -0.104178 -0.015144 0.049753 ( 0.000014 0.000017 0.000017 ) 0.087421 -0.167261 0.063718 ( 0.000010 0.000012 0.000012 ) 0.055475 -0.024281 0.122784 ( 0.000013 0.000016 0.000016 ) M - matrix: 0.021573 -0.014391 0.007199 ( 0.000004 0.000003 0.000003 ) -0.014391 0.028795 -0.014392 ( 0.000003 0.000004 0.000003 ) 0.007199 -0.014392 0.021611 ( 0.000003 0.000003 0.000005 ) UB fit with 1217 obs out of 1217 (total:1217,skipped:0) (100.00%) unit cell: 5.9149(8) 5.9095(6) 5.9072(9) 60.037(13) 90.022(11) 59.997(13) V = 146.05(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104069 -0.015268 0.049870 ( 0.000025 0.000032 0.000028 ) 0.087364 -0.167016 0.063621 ( 0.000017 0.000021 0.000019 ) 0.055453 -0.024096 0.122542 ( 0.000020 0.000026 0.000023 ) M - matrix: 0.021538 -0.014338 0.007164 ( 0.000006 0.000005 0.000005 ) -0.014338 0.028708 -0.014340 ( 0.000005 0.000007 0.000005 ) 0.007164 -0.014340 0.021551 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9157(14) 5.9142(10) 5.9133(13) 60.04(2) 90.006(19) 60.03(2) V = 146.44(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104074 -0.015235 0.049881 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167226 0.063749 ( 0.000017 0.000021 0.000019 ) 0.055500 -0.024199 0.122600 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021553 -0.014376 0.007186 ( 0.000006 0.000005 0.000005 ) -0.014376 0.028782 -0.014387 ( 0.000005 0.000007 0.000005 ) 0.007186 -0.014387 0.021583 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9116(10) 5.9127(13) 60.00(2) 89.999(18) 60.01(2) V = 146.25(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.911) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104074 -0.015235 0.049881 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167226 0.063749 ( 0.000017 0.000021 0.000019 ) 0.055500 -0.024199 0.122600 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021553 -0.014376 0.007186 ( 0.000006 0.000005 0.000005 ) -0.014376 0.028782 -0.014387 ( 0.000005 0.000007 0.000005 ) 0.007186 -0.014387 0.021583 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9116(10) 5.9127(13) 60.00(2) 89.999(18) 60.01(2) V = 146.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104074 -0.015235 0.049881 ( 0.000024 0.000031 0.000027 ) 0.087415 -0.167226 0.063749 ( 0.000017 0.000021 0.000019 ) 0.055500 -0.024199 0.122600 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021553 -0.014376 0.007186 ( 0.000006 0.000005 0.000005 ) -0.014376 0.028782 -0.014387 ( 0.000005 0.000007 0.000005 ) 0.007186 -0.014387 0.021583 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9116(10) 5.9127(13) 60.00(2) 89.999(18) 60.01(2) V = 146.25(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 319 obs out of 319 (total:319,skipped:0) (100.00%) UB - matrix: -0.104481 -0.014859 0.049593 ( 0.000029 0.000043 0.000043 ) 0.087373 -0.167335 0.063690 ( 0.000021 0.000031 0.000031 ) 0.055699 -0.024892 0.123133 ( 0.000022 0.000032 0.000032 ) M - matrix: 0.021653 -0.014455 0.007242 ( 0.000008 0.000007 0.000006 ) -0.014455 0.028841 -0.014460 ( 0.000007 0.000010 0.000007 ) 0.007242 -0.014460 0.021678 ( 0.000006 0.000007 0.000010 ) unit cell: 5.9091(18) 5.9148(14) 5.9050(18) 59.95(3) 89.98(2) 59.94(3) V = 145.74(7) OTKP changes: 319 1 1 1 UB - matrix: -0.104438 -0.014936 0.049391 ( 0.000024 0.000035 0.000036 ) 0.087253 -0.167286 0.063632 ( 0.000021 0.000031 0.000031 ) 0.055480 -0.024753 0.123123 ( 0.000021 0.000031 0.000031 ) M - matrix: 0.021598 -0.014410 0.007225 ( 0.000007 0.000006 0.000006 ) -0.014410 0.028820 -0.014430 ( 0.000006 0.000011 0.000007 ) 0.007225 -0.014430 0.021648 ( 0.000006 0.000007 0.000009 ) UB fit with 319 obs out of 319 (total:319,skipped:0) (100.00%) unit cell: 5.9121(15) 5.9099(14) 5.9062(17) 60.00(3) 90.04(2) 60.01(2) V = 145.89(6) Run 3 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.859) HKL list info: 572 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104438 -0.014936 0.049391 ( 0.000024 0.000035 0.000036 ) 0.087253 -0.167286 0.063632 ( 0.000021 0.000031 0.000031 ) 0.055480 -0.024753 0.123123 ( 0.000021 0.000031 0.000031 ) M - matrix: 0.021598 -0.014410 0.007225 ( 0.000007 0.000006 0.000006 ) -0.014410 0.028820 -0.014430 ( 0.000006 0.000011 0.000007 ) 0.007225 -0.014430 0.021648 ( 0.000006 0.000007 0.000009 ) UB fit with 319 obs out of 319 (total:319,skipped:0) (100.00%) unit cell: 5.9121(15) 5.9099(14) 5.9062(17) 60.00(3) 90.04(2) 60.01(2) V = 145.89(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 319 obs out of 319 (total:319,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146961 -0.098046 0.049189 ( 0.000020 0.000029 0.000030 ) -0.000014 0.138718 -0.069543 ( 0.000022 0.000033 0.000033 ) 0.000000 -0.000020 0.120119 ( 0.000021 0.000031 0.000032 ) M - matrix: 0.021598 -0.014411 0.007230 ( 0.000006 0.000006 0.000005 ) -0.014411 0.028856 -0.014472 ( 0.000006 0.000011 0.000007 ) 0.007230 -0.014472 0.021684 ( 0.000005 0.000007 0.000009 ) UB fit with 319 obs out of 319 (total:319,skipped:0) (100.00%) unit cell: 5.9107(11) 5.9091(16) 5.9054(17) 59.93(3) 90.01(2) 60.04(2) V = 145.75(6) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104216 -0.015049 0.049617 ( 0.000014 0.000018 0.000018 ) 0.087358 -0.167109 0.063625 ( 0.000011 0.000013 0.000013 ) 0.055449 -0.024335 0.122715 ( 0.000014 0.000017 0.000017 ) M - matrix: 0.021567 -0.014379 0.007192 ( 0.000004 0.000003 0.000003 ) -0.014379 0.028744 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007192 -0.014365 0.021569 ( 0.000003 0.000003 0.000005 ) UB fit with 1217 obs out of 1217 (total:1217,skipped:0) (100.00%) unit cell: 5.9163(8) 5.9151(7) 5.9129(9) 60.040(14) 90.022(12) 59.989(13) V = 146.35(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 32 reflections under beam stop or inside a detector rejection region 10 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof 1644 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:16:26 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.911) Run 3 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.859) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=241.9352 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=61 max=875 PROFFIT INFO: Inet: min=527.8586 max=4887974.0000 PROFFIT INFO: sig(Inet): min=188.5049 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 32 124 215 347 377 652 1096 1485 1644 Percent 0.0 0.1 1.9 7.5 13.1 21.1 22.9 39.7 66.7 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1644 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 1644 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1617960 164 2377710.53 135.85 100.00 1610578- 1038838 164 1310138.78 110.12 100.00 1023845- 312524 164 591960.01 93.17 100.00 312237- 218365 164 253233.40 68.06 100.00 217730- 165484 164 189732.30 48.65 100.00 165451- 135392 164 150925.97 36.76 100.00 135363- 102009 164 117611.94 31.20 100.00 101825- 6430 164 57855.81 20.64 100.00 6402- 3645 164 4726.30 4.78 81.10 3642- 528 168 2714.08 3.16 44.64 ------------------------------------------------------------------------------------ 4887974- 528 1644 504437.20 55.11 92.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 164 651238.93 83.70 99.39 1.24- 0.98 164 793788.78 74.30 97.56 0.98- 0.82 164 564496.05 59.99 96.34 0.82- 0.74 164 566786.83 63.87 95.12 0.74- 0.67 164 562071.38 60.44 94.51 0.67- 0.61 164 356003.06 43.68 92.68 0.61- 0.56 164 523306.38 52.22 93.90 0.56- 0.52 164 360033.67 40.15 82.32 0.52- 0.48 164 342275.79 37.32 87.20 0.48- 0.40 168 328658.40 35.91 85.71 ------------------------------------------------------------------------------------ 5.26- 0.40 1644 504437.20 55.11 92.46 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:16:26 2018 Sorting 1644 observations 263 unique observations with > 7.00 F2/sig(F2) 1644 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 74 290 Total number of frames 290 Maximum number of 263 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1644 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 37 147 Total number of frames 147 1317 observations > 7.00 F2/sig(F2) 1317 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 37 147 Total number of frames 147 Removing 'redundancy=1' reflections Average redundancy: 5.0 (Out of 1317 removed 30 = 1287, unique = 260) 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 1287 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 37 147 Total number of frames 147 260 unique data precomputed (should be 260) 260 unique data with 1287 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.0 (Out of 1287 removed 0 = 1287, unique = 260) 260 unique data precomputed (should be 260) 260 unique data with 1287 observations RMS deviation of equivalent data = 0.68471 Rint = 0.62560 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.60741, wR= 2.83297 Trying model 1 (ne=2, no=0)... Results: Rint= 0.66833, wR= 2.46476, Acormin=-0.141, Acormax=2.307, Acor_av=0.658 F test: Probability=0.000, F= 0.822 Trying model 2 (ne=2, no=1)... Results: Rint= 0.86512, wR= 2.20063, Acormin=-0.148, Acormax=1.801, Acor_av=0.304 F test: Probability=0.000, F= 0.489 Trying model 3 (ne=4, no=0)... Results: Rint= 0.68719, wR= 1.88305, Acormin=-0.132, Acormax=2.742, Acor_av=0.534 F test: Probability=0.000, F= 0.771 Trying model 4 (ne=4, no=1)... Results: Rint= 0.88591, wR= 2.06421, Acormin=-0.434, Acormax=1.925, Acor_av=0.273 F test: Probability=0.000, F= 0.462 Trying model 5 (ne=4, no=3)... Results: Rint= 0.91764, wR= 2.13908, Acormin=-0.507, Acormax=2.463, Acor_av=0.059 F test: Probability=0.000, F= 0.428 Trying model 6 (ne=6, no=0)... Results: Rint= 0.70366, wR= 2.22354, Acormin=-0.328, Acormax=2.823, Acor_av=0.475 F test: Probability=0.000, F= 0.725 Trying model 7 (ne=6, no=1)... Results: Rint= 0.89705, wR= 2.27236, Acormin=-0.474, Acormax=2.266, Acor_av=0.231 F test: Probability=0.000, F= 0.445 Trying model 8 (ne=6, no=3)... Results: Rint= 0.93856, wR= 2.04920, Acormin=-0.447, Acormax=2.172, Acor_av=0.054 F test: Probability=0.000, F= 0.404 Trying model 9 (ne=6, no=5)... Results: Rint= 0.95060, wR= 1.43212, Acormin=-0.670, Acormax=0.788, Acor_av=0.002 F test: Probability=0.000, F= 0.389 Trying model 10 (ne=8, no=0)... Results: Rint= 0.78237, wR= 2.43677, Acormin=-0.712, Acormax=1.275, Acor_av=0.255 F test: Probability=0.000, F= 0.577 Trying model 11 (ne=8, no=1)... Results: Rint= 0.89859, wR= 3.10456, Acormin=-0.413, Acormax=1.290, Acor_av=0.112 F test: Probability=0.000, F= 0.436 Trying model 12 (ne=8, no=3)... Results: Rint= 0.92796, wR= 2.32001, Acormin=-0.055, Acormax=0.058, Acor_av=0.002 F test: Probability=0.000, F= 0.406 Trying model 13 (ne=8, no=5)... Results: Rint= 0.92062, wR= 1.66880, Acormin=-0.061, Acormax=0.061, Acor_av=0.001 F test: Probability=0.000, F= 0.408 Trying model 14 (ne=8, no=7)... Results: Rint= 0.90591, wR= 1.63382, Acormin=-0.063, Acormax=0.109, Acor_av=0.001 F test: Probability=0.000, F= 0.414 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: 0.80744 There are 147 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: 2, max odd order: 0 (5 parameters) Refinement control: 151 pars with 11476 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.68471 Using Levenberg-Marquardt: 0.00010 New wR= 0.66084 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62560 with corrections 0.60452 Rint for all data: 0.80744 with corrections 0.79809 5 observations identified as outliers and rejected Cycle 2 wR= 0.63833 Using Levenberg-Marquardt: 0.00001 New wR= 0.63549 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.61021 with corrections 0.57987 Rint for all data: 0.80744 with corrections 0.79653 5 observations identified as outliers and rejected Cycle 3 wR= 0.61377 Using Levenberg-Marquardt: 0.00000 New wR= 0.61063 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.59546 with corrections 0.56690 Rint for all data: 0.80744 with corrections 0.79664 8 observations identified as outliers and rejected Cycle 4 wR= 0.58702 Using Levenberg-Marquardt: 0.00000 New wR= 0.58336 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.58615 with corrections 0.56593 Rint for all data: 0.80744 with corrections 0.80250 2 observations identified as outliers and rejected Cycle 5 wR= 0.56892 Using Levenberg-Marquardt: 0.00000 New wR= 0.56737 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.58272 with corrections 0.55983 Rint for all data: 0.80744 with corrections 0.80056 3 observations identified as outliers and rejected Final wR= 0.56737 Final frame scales: Min= 0.4142 Max= 2.1719 Final absorption correction factors: Amin= 0.3957 Amax= 1.4191 PROFFIT INFO: Inet (after scale3 abspack): min=408.0210 max=8597089.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=188.5748 max=145353.7188 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1644 reflections read from tmp file 1211 reflections are rejected (1130 as outliers, 81 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 85 33 29 7 1 1 Initial Chi^2= 0.48532 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.99414 Current error model SIG(F2)^2 = 205.63*I_RAW + 0.00*I_BACK+(0.00884*)^2 Cycle 2, Chi^2= 0.98900 Current error model SIG(F2)^2 = 163.70*I_RAW + 0.00*I_BACK+(0.02103*)^2 Cycle 3, Chi^2= 0.99974 Current error model SIG(F2)^2 = 161.05*I_RAW + 0.00*I_BACK+(0.02116*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 160.92*I_RAW + 0.00*I_BACK+(0.02118*)^2 Final Chi^2= 0.99997 Final error model SIG(F2)^2 = 160.92*I_RAW + 0.00*I_BACK+(0.02118*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8597089- 1471734 164 2296920.15 91.50 100.00 1468516- 893553 164 1172998.27 54.09 100.00 892265- 305575 164 543434.06 45.85 100.00 305298- 203756 164 247565.13 31.02 100.00 202832- 159968 164 178178.01 23.26 100.00 159902- 120292 164 139794.34 19.09 100.00 120143- 91762 164 105844.21 15.82 100.00 91676- 6703 164 52546.15 11.11 95.73 6667- 3216 164 4381.53 3.48 60.98 3212- 408 168 2465.59 2.75 30.36 ------------------------------------------------------------------------------------ 8597089- 408 1644 473264.45 29.73 88.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 164 760915.46 55.74 96.95 1.24- 0.98 164 785757.06 46.69 95.73 0.98- 0.82 164 555780.52 33.16 92.07 0.82- 0.74 164 538498.40 29.89 92.07 0.74- 0.67 164 538337.79 30.20 90.24 0.67- 0.61 164 302168.47 21.97 87.80 0.61- 0.56 164 458391.78 24.53 90.24 0.56- 0.52 164 299514.09 20.22 77.44 0.52- 0.48 164 266024.08 18.31 82.32 0.48- 0.40 168 233114.21 16.90 80.95 ------------------------------------------------------------------------------------ 5.26- 0.40 1644 473264.45 29.73 88.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 164 760915.46 55.74 96.95 5.26- 0.98 328 773336.26 51.21 96.34 5.26- 0.82 492 700817.68 45.20 94.92 5.26- 0.74 656 660237.86 41.37 94.21 5.26- 0.67 820 635857.85 39.14 93.41 5.26- 0.61 984 580242.95 36.28 92.48 5.26- 0.56 1148 562835.64 34.60 92.16 5.26- 0.52 1312 529920.45 32.80 90.32 5.26- 0.48 1476 500598.63 31.19 89.43 5.26- 0.40 1644 473264.45 29.73 88.56 ------------------------------------------------------------------------------------ 5.26- 0.40 1644 473264.45 29.73 88.56 Scale applied to data: s=0.116318 (maximum obs:8597089.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.801; Rsigma 0.022: data 1644 -> merged 305 With outlier rejection... Rint 0.712; Rsigma 0.023: data 1490 -> merged 305 Rejected total: 154, method kkm 147, method Blessing 7 Completeness direct cell (a, b, c) = (5.270, 5.270, 5.270), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404183, 5.269900 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 5.73 100.00 86 1.46 - 1.12 15 15 7.27 100.00 109 1.08 - 0.96 15 15 7.20 100.00 108 0.96 - 0.85 15 15 8.00 100.00 120 0.85 - 0.79 15 15 6.80 100.00 102 0.79 - 0.73 14 15 6.00 93.33 84 0.73 - 0.69 15 15 5.60 100.00 84 0.69 - 0.65 14 15 7.00 93.33 98 0.65 - 0.63 12 15 4.42 80.00 53 0.63 - 0.60 21 21 4.67 100.00 98 --------------------------------------------------------------- 5.91 - 0.60 151 156 6.24 96.79 942 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:16:26 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916259 5.915088 5.912933 60.0402 90.0218 59.9893 1490 Reflections read from file xs1715a.hkl; mean (I/sigma) = 28.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 732 785 733 749 1125 1009 985 1490 N (int>3sigma) = 0 625 785 626 653 1018 897 876 1321 Mean intensity = 0.0 43.6 21.2 43.8 50.5 35.8 51.1 49.5 50.3 Mean int/sigma = 0.0 27.5 24.5 28.1 28.3 26.7 28.9 28.6 28.8 Lattice type: P chosen Volume: 146.35 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.915 5.915 60.02 60.04 60.01 Niggli form: a.a = 34.963 b.b = 34.984 c.c = 34.988 b.c = 17.485 a.c = 17.467 a.b = 17.480 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.036 CUBIC F-lattice R(int) = 0.177 [ 1337] Vol = 585.4 Cell: 8.363 8.366 8.367 90.03 90.00 90.03 Volume: 585.42 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.036 RHOMBOHEDRAL R-lattice R(int) = 0.167 [ 1080] Vol = 439.1 Cell: 5.915 5.918 14.484 90.02 89.97 120.00 Volume: 439.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.036 RHOMBOHEDRAL R-lattice R(int) = 0.130 [ 328] Vol = 439.1 Trigonal Cell: 5.915 5.918 14.484 90.02 89.97 120.00 Volume: 439.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.026 RHOMBOHEDRAL R-lattice R(int) = 0.153 [ 1075] Vol = 439.1 Cell: 5.913 5.915 14.495 89.98 90.03 119.99 Volume: 439.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.026 RHOMBOHEDRAL R-lattice R(int) = 0.172 [ 323] Vol = 439.1 Trigonal Cell: 5.913 5.915 14.495 89.98 90.03 119.99 Volume: 439.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.154 [ 1070] Vol = 292.7 Cell: 5.913 5.916 8.367 89.98 89.98 89.98 Volume: 292.71 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.086 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 1110] Vol = 292.7 Cell: 5.915 8.366 5.915 90.00 89.97 90.04 Volume: 292.71 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.026 MONOCLINIC I-lattice R(int) = 0.126 [ 852] Vol = 292.7 Cell: 5.915 5.915 8.366 90.00 90.04 90.03 Volume: 292.71 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.015 MONOCLINIC I-lattice R(int) = 0.139 [ 893] Vol = 292.7 Cell: 5.913 5.916 8.367 90.02 90.02 89.98 Volume: 292.71 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.015 MONOCLINIC I-lattice R(int) = 0.129 [ 807] Vol = 292.7 Cell: 5.916 5.913 8.367 90.02 90.02 89.98 Volume: 292.71 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.028 MONOCLINIC I-lattice R(int) = 0.129 [ 807] Vol = 292.7 Cell: 8.367 5.913 5.916 89.98 90.02 90.02 Volume: 292.71 Matrix: 1.0000 -2.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.079 [ 574] Vol = 146.4 Cell: 5.913 5.915 5.915 60.02 60.04 60.01 Volume: 146.35 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 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 0 785 0 985 1009 1490 N (int>3sigma) = 0 0 0 0 785 0 873 897 1321 Mean intensity = 0.0 0.0 0.0 0.0 21.2 0.0 50.7 51.1 50.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.5 0.0 28.6 28.9 28.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 112 338 N I>3s 10 10 74 338 0.6 0.6 0.5 24.2 7.2 7.2 4.0 29.4 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 0.177 1245 Fd-3m 1 1 227 C N N N N 37 2284 0.175 1282 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362911 8.366093 8.367336 90.0280 89.9990 90.0322 ZERR 1.00 0.000346 0.002055 0.003464 0.0010 0.0132 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 6305569- 920364 159 137 30 4.6 1456120.26 56.62 0.525 0.365 916353- 718715 182 171 30 5.7 800302.99 42.16 0.783 0.679 712319- 553261 219 209 30 7.0 546165.53 35.10 0.916 0.872 551053- 431230 184 168 30 5.6 413340.31 32.02 0.908 0.877 430858- 316831 209 185 30 6.2 288190.35 28.27 0.805 0.894 315484- 171977 183 152 30 5.1 190915.27 23.42 0.612 0.538 171153- 113182 152 134 30 4.5 136388.79 18.45 0.368 0.314 112502- 94713 123 112 30 3.7 104382.75 15.93 0.279 0.227 94199- 60656 130 123 30 4.1 78504.50 11.88 0.620 0.509 60497- 1111 103 99 35 2.8 30823.81 7.12 0.777 0.697 ------------------------------------------------------------------------------------------- 6305569- 1111 1644 1490 305 4.9 432844.94 28.79 0.712 0.589 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 223 195 30 6.5 676902.10 52.61 0.697 0.505 0.014 1.08-0.85 258 234 31 7.5 619451.74 37.32 0.799 0.701 0.018 0.83-0.72 211 196 32 6.1 505695.99 29.17 0.678 0.612 0.023 0.72-0.65 206 191 30 6.4 382122.47 26.60 0.865 0.901 0.024 0.64-0.60 156 137 30 4.6 400862.13 22.93 0.686 0.738 0.028 0.59-0.56 158 139 30 4.6 264694.24 19.36 0.651 0.542 0.033 0.55-0.51 137 132 30 4.4 338861.43 22.05 0.809 0.784 0.029 0.51-0.49 113 103 30 3.4 221756.68 16.41 0.501 0.346 0.036 0.49-0.46 107 96 30 3.2 226302.21 16.68 0.340 0.250 0.037 0.45-0.40 75 67 32 2.1 222138.37 16.01 0.228 0.177 0.039 ------------------------------------------------------------------------------------------------------ inf-0.40 1644 1490 305 4.9 432844.94 28.79 0.712 0.589 0.023 inf-0.60 1039 942 151 6.2 533534.24 34.76 0.747 0.647 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 195 30 30 100.0 6.5 676902.10 166.73 0.697 0.009 1.08-0.85 234 31 31 100.0 7.5 619451.74 129.57 0.799 0.009 0.83-0.72 196 33 32 97.0 6.1 505695.99 86.34 0.678 0.011 0.72-0.65 191 33 30 90.9 6.4 382122.47 84.91 0.865 0.012 0.64-0.60 137 31 30 96.8 4.6 400862.13 65.17 0.686 0.015 0.59-0.56 139 38 30 78.9 4.6 264694.24 51.13 0.651 0.018 0.55-0.51 132 39 30 76.9 4.4 338861.43 60.33 0.809 0.016 0.51-0.49 103 42 30 71.4 3.4 221756.68 37.59 0.501 0.023 0.49-0.46 96 57 30 52.6 3.2 226302.21 34.65 0.340 0.022 0.45-0.40 67 127 32 25.2 2.1 222138.37 26.72 0.228 0.027 -------------------------------------------------------------------------------------------- inf-0.40 1490 464 305 65.7 4.9 432844.94 86.55 0.712 0.014 inf-0.60 942 156 151 96.8 6.2 533534.24 110.85 0.747 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.034823 -0.076915 0.007525 ( 0.000007 0.000008 0.000008 ) 0.008063 0.011868 0.083554 ( 0.000006 0.000006 0.000007 ) -0.076914 -0.033628 0.012167 ( 0.000007 0.000007 0.000008 ) M - matrix: 0.007193 0.000004 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007188 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000004 0.007186 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.034823 -0.076915 0.007525 ( 0.000007 0.000008 0.000008 ) 0.008063 0.011868 0.083554 ( 0.000006 0.000006 0.000007 ) -0.076914 -0.033628 0.012167 ( 0.000007 0.000007 0.000008 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3630(7) 8.3664(7) 8.3674(6) 90.030(7) 90.000(7) 90.030(7) V = 585.45(8) unit cell: 8.3656(2) 8.3656(2) 8.3656(2) 90.0 90.0 90.0 V = 585.45(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.911) Run 3 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.859) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=241.9352 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=15787.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=61 max=875 PROFFIT INFO: Inet: min=527.8586 max=4887974.0000 PROFFIT INFO: sig(Inet): min=188.5049 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 64 248 430 694 754 1304 2192 2970 3288 Percent 0.0 0.1 1.9 7.5 13.1 21.1 22.9 39.7 66.7 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1644 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 1644 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1617960 164 2377710.53 135.85 100.00 1610578- 1038838 164 1310138.78 110.12 100.00 1023845- 312524 164 591960.01 93.17 100.00 312237- 218365 164 253233.40 68.06 100.00 217730- 165484 164 189732.30 48.65 100.00 165451- 135392 164 150925.97 36.76 100.00 135363- 102009 164 117611.94 31.20 100.00 101825- 6430 164 57855.81 20.64 100.00 6402- 3645 164 4726.30 4.78 81.10 3642- 528 168 2714.08 3.16 44.64 ------------------------------------------------------------------------------------ 4887974- 528 1644 504437.20 55.11 92.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 164 705903.77 82.40 98.78 1.39- 1.09 164 933878.77 79.42 98.78 1.09- 0.96 164 545922.66 68.76 98.78 0.96- 0.85 164 509829.28 61.69 96.34 0.85- 0.80 164 653661.37 68.32 97.56 0.80- 0.73 164 360475.56 41.47 93.90 0.73- 0.70 164 272631.20 35.11 91.46 0.70- 0.65 164 529660.84 52.25 92.68 0.65- 0.62 164 269647.93 31.35 78.66 0.62- 0.58 168 268514.81 30.94 77.98 ------------------------------------------------------------------------------------ 4.82- 0.58 1644 504437.20 55.11 92.46 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:16:27 2018 Sorting 1644 observations 84 unique observations with > 7.00 F2/sig(F2) 1644 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 74 290 Total number of frames 290 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1644 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 18 74 Total number of frames 74 1317 observations > 7.00 F2/sig(F2) 1317 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 18 74 Total number of frames 74 Removing 'redundancy=1' reflections Average redundancy: 15.2 (Out of 1317 removed 6 = 1311, unique = 86) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1311 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 18 74 Total number of frames 74 86 unique data precomputed (should be 86) 86 unique data with 1311 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 15.2 (Out of 1311 removed 0 = 1311, unique = 86) 86 unique data precomputed (should be 86) 86 unique data with 1311 observations RMS deviation of equivalent data = 0.20842 Rint = 0.16493 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16149, wR= 0.21639 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06884, wR= 0.09106, Acormin=0.646, Acormax=1.389, Acor_av=0.902 F test: Probability=1.000, F= 5.481 Trying model 2 (ne=2, no=1)... Results: Rint= 0.06825, wR= 0.08920, Acormin=0.649, Acormax=1.361, Acor_av=0.873 F test: Probability=0.601, F= 1.015 Trying model 3 (ne=4, no=0)... Results: Rint= 0.05605, wR= 0.07667, Acormin=0.669, Acormax=1.518, Acor_av=0.888 F test: Probability=1.000, F= 1.497 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05209, wR= 0.07194, Acormin=0.650, Acormax=1.514, Acor_av=0.884 F test: Probability=0.994, F= 1.155 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04767, wR= 0.06478, Acormin=0.519, Acormax=1.362, Acor_av=0.787 F test: Probability=0.999, F= 1.187 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04738, wR= 0.06812, Acormin=0.645, Acormax=1.488, Acor_av=0.877 F test: Probability=0.565, F= 1.010 Trying model 7 (ne=6, no=1)... Results: Rint= 0.04470, wR= 0.06361, Acormin=0.604, Acormax=1.527, Acor_av=0.872 F test: Probability=0.984, F= 1.131 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04065, wR= 0.05608, Acormin=0.499, Acormax=1.366, Acor_av=0.761 F test: Probability=0.999, F= 1.202 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03996, wR= 0.05328, Acormin=0.373, Acormax=1.029, Acor_av=0.578 F test: Probability=0.666, F= 1.025 Trying model 10 (ne=8, no=0)... Results: Rint= 0.04347, wR= 0.06200, Acormin=0.617, Acormax=1.526, Acor_av=0.851 F test: Probability=0.000, F= 0.869 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04151, wR= 0.05770, Acormin=0.590, Acormax=1.547, Acor_av=0.840 F test: Probability=0.000, F= 0.951 Trying model 12 (ne=8, no=3)... Results: Rint= 0.03509, wR= 0.04698, Acormin=0.395, Acormax=1.122, Acor_av=0.604 F test: Probability=1.000, F= 1.323 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03388, wR= 0.04450, Acormin=0.410, Acormax=1.159, Acor_av=0.630 F test: Probability=0.851, F= 1.063 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03048, wR= 0.04045, Acormin=0.428, Acormax=1.252, Acor_av=0.671 F test: Probability=1.000, F= 1.296 Final absorption model (ne=8, no=7): Rint= 0.03048, Acormin=0.428, Acormax=1.252, Acor_av=0.671 Combined refinement in use Rint: 0.16505 There are 74 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20842 Using Levenberg-Marquardt: 0.00010 New wR= 0.04027 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16493 with corrections 0.03074 Rint for all data: 0.16505 with corrections 0.03095 0 observations identified as outliers and rejected Cycle 2 wR= 0.04027 Using Levenberg-Marquardt: 0.00001 New wR= 0.03375 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16493 with corrections 0.02650 Rint for all data: 0.16505 with corrections 0.02672 0 observations identified as outliers and rejected Cycle 3 wR= 0.03375 Using Levenberg-Marquardt: 0.00000 New wR= 0.03348 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16493 with corrections 0.02619 Rint for all data: 0.16505 with corrections 0.02642 0 observations identified as outliers and rejected Cycle 4 wR= 0.03348 Using Levenberg-Marquardt: 0.00000 New wR= 0.03336 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16493 with corrections 0.02614 Rint for all data: 0.16505 with corrections 0.02637 0 observations identified as outliers and rejected Cycle 5 wR= 0.03336 Using Levenberg-Marquardt: 0.00000 New wR= 0.03327 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16493 with corrections 0.02609 Rint for all data: 0.16505 with corrections 0.02631 0 observations identified as outliers and rejected Final wR= 0.03327 Final frame scales: Min= 0.8887 Max= 1.1029 Final absorption correction factors: Amin= 0.4322 Amax= 1.3362 PROFFIT INFO: Inet (after scale3 abspack): min=547.1813 max=5836959.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=259.9705 max=68408.3828 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1644 reflections read from tmp file 144 reflections are rejected (140 as outliers, 4 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 5 6 5 5 0 4 4 74 Initial Chi^2= 0.27499 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.43005 Current error model SIG(F2)^2 = 98.04*I_RAW + 0.00*I_BACK+(0.00534*)^2 Cycle 2, Chi^2= 1.13946 Current error model SIG(F2)^2 = 56.78*I_RAW + 0.00*I_BACK+(0.01859*)^2 Cycle 3, Chi^2= 1.01011 Current error model SIG(F2)^2 = 85.34*I_RAW + 0.00*I_BACK+(0.01383*)^2 Cycle 4, Chi^2= 1.00030 Current error model SIG(F2)^2 = 80.45*I_RAW + 0.00*I_BACK+(0.01519*)^2 Cycle 5, Chi^2= 1.00018 Current error model SIG(F2)^2 = 82.11*I_RAW + 0.00*I_BACK+(0.01480*)^2 Cycle 6, Chi^2= 0.99997 Current error model SIG(F2)^2 = 81.66*I_RAW + 0.00*I_BACK+(0.01491*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 81.79*I_RAW + 0.00*I_BACK+(0.01488*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 81.79*I_RAW + 0.00*I_BACK+(0.01488*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5836959- 1534622 164 2314674.32 60.20 100.00 1527499- 1005822 164 1243721.01 50.48 100.00 998669- 324823 164 594790.15 47.78 100.00 324617- 204814 164 246143.65 38.64 100.00 204579- 171647 164 187353.67 31.06 100.00 171571- 129178 164 142630.20 24.33 100.00 129143- 102682 164 115705.88 21.57 100.00 102677- 5918 164 58261.38 15.58 100.00 5867- 3513 164 4430.00 5.00 100.00 3504- 547 168 2739.03 4.13 86.31 ------------------------------------------------------------------------------------ 5836959- 547 1644 489856.84 29.81 98.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 164 765517.25 43.56 100.00 1.39- 1.09 164 940165.24 40.84 100.00 1.09- 0.96 164 520731.92 34.22 100.00 0.96- 0.85 164 502761.28 31.03 99.39 0.85- 0.80 164 607001.95 34.36 100.00 0.80- 0.73 164 329736.80 23.42 100.00 0.73- 0.70 164 260299.88 21.76 98.78 0.70- 0.65 164 485360.78 29.46 96.95 0.65- 0.62 164 245881.97 19.89 96.34 0.62- 0.58 168 247033.82 19.83 94.64 ------------------------------------------------------------------------------------ 4.82- 0.58 1644 489856.84 29.81 98.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 164 765517.25 43.56 100.00 4.82- 1.09 328 852841.24 42.20 100.00 4.82- 0.96 492 742138.13 39.54 100.00 4.82- 0.85 656 682293.92 37.41 99.85 4.82- 0.80 820 667235.53 36.80 99.88 4.82- 0.73 984 610985.74 34.57 99.90 4.82- 0.70 1148 560887.76 32.74 99.74 4.82- 0.65 1312 551446.89 32.33 99.39 4.82- 0.62 1476 517495.23 30.95 99.05 4.82- 0.58 1644 489856.84 29.81 98.60 ------------------------------------------------------------------------------------ 4.82- 0.58 1644 489856.84 29.81 98.60 Scale applied to data: s=0.171322 (maximum obs:5836959.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.026; Rsigma 0.021: data 1644 -> merged 109 With outlier rejection... Rint 0.024; Rsigma 0.021: data 1630 -> merged 109 Rejected total: 14, method kkm 13, method Blessing 1 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585708, 4.829875 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 8.10 100.00 81 1.61 - 1.21 10 10 14.40 100.00 144 1.17 - 1.01 10 10 19.60 100.00 196 0.99 - 0.89 10 10 19.50 100.00 195 0.88 - 0.81 10 10 18.40 100.00 184 0.81 - 0.74 10 10 16.30 100.00 163 0.73 - 0.71 10 10 17.70 100.00 177 0.70 - 0.66 10 10 14.60 100.00 146 0.66 - 0.64 10 10 13.60 100.00 136 0.63 - 0.60 10 10 13.90 100.00 139 --------------------------------------------------------------- 5.91 - 0.60 100 100 15.61 100.00 1561 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:16:26 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.916259 5.915088 5.912933 60.0402 90.0218 59.9893 1490 Reflections read from file xs1715a.hkl; mean (I/sigma) = 28.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 732 785 733 749 1125 1009 985 1490 N (int>3sigma) = 0 625 785 626 653 1018 897 876 1321 Mean intensity = 0.0 43.6 21.2 43.8 50.5 35.8 51.1 49.5 50.3 Mean int/sigma = 0.0 27.5 24.5 28.1 28.3 26.7 28.9 28.6 28.8 Lattice type: P chosen Volume: 146.35 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.915 5.915 60.02 60.04 60.01 Niggli form: a.a = 34.963 b.b = 34.984 c.c = 34.988 b.c = 17.485 a.c = 17.467 a.b = 17.480 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.036 CUBIC F-lattice R(int) = 0.177 [ 1337] Vol = 585.4 Cell: 8.363 8.366 8.367 90.03 90.00 90.03 Volume: 585.42 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.036 RHOMBOHEDRAL R-lattice R(int) = 0.167 [ 1080] Vol = 439.1 Cell: 5.915 5.918 14.484 90.02 89.97 120.00 Volume: 439.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.036 RHOMBOHEDRAL R-lattice R(int) = 0.130 [ 328] Vol = 439.1 Trigonal Cell: 5.915 5.918 14.484 90.02 89.97 120.00 Volume: 439.06 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.026 RHOMBOHEDRAL R-lattice R(int) = 0.153 [ 1075] Vol = 439.1 Cell: 5.913 5.915 14.495 89.98 90.03 119.99 Volume: 439.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.026 RHOMBOHEDRAL R-lattice R(int) = 0.172 [ 323] Vol = 439.1 Trigonal Cell: 5.913 5.915 14.495 89.98 90.03 119.99 Volume: 439.06 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.154 [ 1070] Vol = 292.7 Cell: 5.913 5.916 8.367 89.98 89.98 89.98 Volume: 292.71 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.086 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 1110] Vol = 292.7 Cell: 5.915 8.366 5.915 90.00 89.97 90.04 Volume: 292.71 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.026 MONOCLINIC I-lattice R(int) = 0.126 [ 852] Vol = 292.7 Cell: 5.915 5.915 8.366 90.00 90.04 90.03 Volume: 292.71 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.015 MONOCLINIC I-lattice R(int) = 0.139 [ 893] Vol = 292.7 Cell: 5.913 5.916 8.367 90.02 90.02 89.98 Volume: 292.71 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.015 MONOCLINIC I-lattice R(int) = 0.129 [ 807] Vol = 292.7 Cell: 5.916 5.913 8.367 90.02 90.02 89.98 Volume: 292.71 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.028 MONOCLINIC I-lattice R(int) = 0.129 [ 807] Vol = 292.7 Cell: 8.367 5.913 5.916 89.98 90.02 90.02 Volume: 292.71 Matrix: 1.0000 -2.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.079 [ 574] Vol = 146.4 Cell: 5.913 5.915 5.915 60.02 60.04 60.01 Volume: 146.35 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 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 0 785 0 985 1009 1490 N (int>3sigma) = 0 0 0 0 785 0 873 897 1321 Mean intensity = 0.0 0.0 0.0 0.0 21.2 0.0 50.7 51.1 50.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.5 0.0 28.6 28.9 28.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 112 338 N I>3s 10 10 74 338 0.6 0.6 0.5 24.2 7.2 7.2 4.0 29.4 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 0.177 1245 Fd-3m 1 1 227 C N N N N 37 2284 0.175 1282 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362911 8.366093 8.367336 90.0280 89.9990 90.0322 ZERR 1.00 0.000346 0.002055 0.003464 0.0010 0.0132 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5836959- 935366 358 352 27 13.0 1703154.95 54.45 0.021 0.032 882241- 162213 485 482 27 17.9 294067.09 38.33 0.027 0.034 148429- 54417 411 409 27 15.1 115324.50 21.49 0.038 0.050 23539- 1623 390 387 28 13.8 4753.12 5.21 0.143 0.173 ------------------------------------------------------------------------------------------- 5836959- 1623 1644 1630 109 15.0 484820.90 29.72 0.024 0.034 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 392 386 27 14.3 762866.72 41.39 0.024 0.039 0.018 1.01-0.78 504 503 27 18.6 494053.68 29.74 0.020 0.026 0.021 0.78-0.65 450 445 29 15.3 374727.00 24.96 0.024 0.029 0.025 0.65-0.59 298 296 26 11.4 272057.40 21.64 0.033 0.039 0.030 ------------------------------------------------------------------------------------------------------ inf-0.59 1644 1630 109 15.0 484820.90 29.72 0.024 0.034 0.021 inf-0.60 1573 1559 99 15.7 496980.88 30.19 0.023 0.033 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 386 27 27 100.0 14.3 762866.72 179.21 0.024 0.006 1.01-0.78 503 27 27 100.0 18.6 494053.68 135.84 0.020 0.005 0.78-0.65 445 29 29 100.0 15.3 374727.00 105.76 0.024 0.007 0.65-0.59 296 26 26 100.0 11.4 272057.40 82.27 0.033 0.010 -------------------------------------------------------------------------------------------- inf-0.59 1630 109 109 100.0 15.0 484820.90 128.17 0.024 0.007 inf-0.60 1559 99 99 100.0 15.7 496980.88 131.10 0.023 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:21:48 2018) ID: 2932; threads 39; handles 879; mem 518828.00 (1237724.00)kB; time: 1w 5d 22h 27m 19s MEMORY INFO: Memory PF:0.0, Ph:165.0, V:1208.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:506.7,peak PF: 708.5, WS: 270.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:165.0, V:1210.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:508.5,peak PF: 708.5, WS: 272.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:21:48 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000018 0.000018 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000014 0.000017 0.000017 ) 5.91535 ( 0.00081 ) 5.92288 ( 0.00067 ) 5.91286 ( 0.00089 ) 59.95509 ( 0.01371 ) 89.89521 ( 0.01173 ) 59.99590 ( 0.01304 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:21:48 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000018 0.000018 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000013 ) 0.055227 -0.024260 0.122680 ( 0.000014 0.000017 0.000017 ) M - matrix: 0.021567 -0.014379 0.007192 ( 0.000004 0.000003 0.000003 ) -0.014379 0.028744 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007192 -0.014365 0.021569 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(8) 5.9229(7) 5.9129(9) 59.955(14) 89.895(12) 59.996(13) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb PROFFITPEAK info: 1077 peaks in the peak location table UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 525 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 134 | 1.152 ( 0.115) | 1.267 ( 0.416) | 1.401 ( 0.739) | 13.2-19.1 | 134 | 1.149 ( 0.122) | 1.199 ( 0.290) | 1.356 ( 0.726) | 19.1-23.2 | 134 | 1.159 ( 0.095) | 1.226 ( 0.351) | 1.280 ( 0.649) | 23.3-27.4 | 134 | 1.144 ( 0.094) | 1.177 ( 0.315) | 1.235 ( 0.522) | 27.5-30.7 | 134 | 1.145 ( 0.108) | 1.159 ( 0.190) | 1.209 ( 0.450) | 30.7-34.1 | 134 | 1.155 ( 0.089) | 1.156 ( 0.229) | 1.222 ( 0.450) | 34.1-37.3 | 134 | 1.142 ( 0.114) | 1.120 ( 0.173) | 1.124 ( 0.383) | 37.3-39.9 | 134 | 1.162 ( 0.118) | 1.123 ( 0.200) | 1.302 ( 0.566) | 39.9-43.0 | 134 | 1.171 ( 0.121) | 1.106 ( 0.197) | 1.245 ( 0.607) | 43.0-49.8 | 131 | 1.210 ( 0.166) | 1.131 ( 0.249) | 1.189 ( 0.480) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1337 | 1.159 ( 0.117) | 1.167 ( 0.276) | 1.257 ( 0.575) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0015 b=1.03 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5021 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 454025 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:22:00 2018 PROFFITMAIN - Started at Wed Mar 28 13:22:00 2018 OTKP changes: 1337 2 2 3 OTKP changes: 1337 2 2 3 UB - matrix: -0.104236 -0.015019 0.049550 ( 0.000016 0.000020 0.000018 ) 0.087415 -0.167197 0.063696 ( 0.000011 0.000013 0.000012 ) 0.055451 -0.024364 0.122925 ( 0.000017 0.000020 0.000019 ) M - matrix: 0.021581 -0.014401 0.007219 ( 0.000004 0.000003 0.000003 ) -0.014401 0.028774 -0.014389 ( 0.000003 0.000005 0.000004 ) 0.007219 -0.014389 0.021623 ( 0.000003 0.000004 0.000005 ) UB fit with 1337 obs out of 1337 (total:1337,skipped:0) (100.00%) unit cell: 5.9163(9) 5.9119(7) 5.9052(10) 60.074(15) 90.071(13) 59.984(14) V = 146.09(4) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104072 -0.015246 0.049844 ( 0.000025 0.000032 0.000028 ) 0.087353 -0.167037 0.063630 ( 0.000017 0.000021 0.000019 ) 0.055427 -0.024100 0.122528 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021534 -0.014340 0.007162 ( 0.000006 0.000005 0.000005 ) -0.014340 0.028715 -0.014341 ( 0.000005 0.000007 0.000005 ) 0.007162 -0.014341 0.021546 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9166(14) 5.9141(10) 5.9142(13) 60.04(2) 90.000(18) 60.03(2) V = 146.47(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104504 -0.014334 0.049188 ( 0.000037 0.000046 0.000040 ) 0.087169 -0.167093 0.063777 ( 0.000025 0.000032 0.000028 ) 0.055307 -0.024956 0.122919 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021578 -0.014448 0.007217 ( 0.000009 0.000007 0.000006 ) -0.014448 0.028748 -0.014429 ( 0.000007 0.000011 0.000007 ) 0.007217 -0.014429 0.021596 ( 0.000006 0.000007 0.000008 ) unit cell: 5.928(2) 5.9370(14) 5.9204(16) 59.89(3) 89.86(3) 59.80(3) V = 146.81(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104463 -0.014618 0.048941 ( 0.000028 0.000035 0.000030 ) 0.087192 -0.167145 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055354 -0.024843 0.123246 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021579 -0.014422 0.007258 ( 0.000008 0.000006 0.000006 ) -0.014422 0.028768 -0.014414 ( 0.000006 0.000010 0.000006 ) 0.007258 -0.014414 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9213(15) 5.9180(13) 5.9083(15) 60.06(2) 90.13(2) 59.97(2) V = 146.30(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104463 -0.014618 0.048941 ( 0.000028 0.000035 0.000030 ) 0.087192 -0.167145 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055354 -0.024843 0.123246 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021579 -0.014422 0.007258 ( 0.000008 0.000006 0.000006 ) -0.014422 0.028768 -0.014414 ( 0.000006 0.000010 0.000006 ) 0.007258 -0.014414 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9213(15) 5.9180(13) 5.9083(15) 60.06(2) 90.13(2) 59.97(2) V = 146.30(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146822 -0.097941 0.049174 ( 0.000021 0.000026 0.000023 ) -0.000019 0.138470 -0.069298 ( 0.000023 0.000029 0.000025 ) -0.000024 0.000035 0.119967 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021557 -0.014383 0.007218 ( 0.000006 0.000005 0.000005 ) -0.014383 0.028766 -0.014408 ( 0.000005 0.000009 0.000006 ) 0.007218 -0.014408 0.021612 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9179(10) 5.9154(14) 5.9116(14) 60.00(2) 90.059(17) 60.02(2) V = 146.31(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104208 -0.014952 0.049403 ( 0.000017 0.000020 0.000019 ) 0.087312 -0.167050 0.063643 ( 0.000011 0.000013 0.000012 ) 0.055395 -0.024380 0.122848 ( 0.000016 0.000020 0.000018 ) M - matrix: 0.021551 -0.014378 0.007214 ( 0.000004 0.000003 0.000003 ) -0.014378 0.028724 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007214 -0.014365 0.021583 ( 0.000003 0.000003 0.000005 ) UB fit with 1337 obs out of 1337 (total:1337,skipped:0) (100.00%) unit cell: 5.9203(9) 5.9169(7) 5.9112(10) 60.077(15) 90.092(13) 59.997(14) V = 146.46(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 34 reflections under beam stop or inside a detector rejection region 12 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof 1794 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:22:03 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) PROFFIT INFO: signal sum: min=176.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=262.7288 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=16000.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=11449.0000 PROFFIT INFO: num of signal pixels: min=60 max=995 PROFFIT INFO: Inet: min=573.2264 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.3042 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.46 max=400.12 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 38 139 239 375 407 709 1190 1619 1793 Percent 0.0 0.1 2.1 7.8 13.3 20.9 22.7 39.5 66.4 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1794 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 1794 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1607137 179 2355128.91 135.41 100.00 1603149- 1044954 179 1303619.56 111.68 100.00 1044240- 313907 179 606729.14 93.18 100.00 313609- 217815 179 254276.65 68.79 100.00 217730- 165253 179 188596.17 48.59 100.00 165202- 133569 179 149722.93 36.68 100.00 132590- 101560 179 117120.46 31.19 100.00 101378- 6457 179 59000.58 21.16 100.00 6417- 3633 179 4691.46 4.70 80.45 3624- 573 182 2663.92 3.14 42.86 ------------------------------------------------------------------------------------ 4887974- 573 1793 503315.90 55.36 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 667499.58 83.72 99.44 1.24- 0.98 179 771880.68 73.55 97.77 0.98- 0.83 179 615058.24 63.25 96.09 0.83- 0.74 179 541901.14 64.49 94.97 0.74- 0.67 179 558447.66 60.09 93.30 0.67- 0.61 179 343858.56 43.45 93.30 0.61- 0.57 179 521930.19 52.53 91.06 0.57- 0.53 179 343105.65 39.21 83.80 0.53- 0.48 179 345410.06 37.98 86.59 0.48- 0.40 182 327021.88 35.71 86.26 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 503315.90 55.36 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:22:04 2018 Sorting 1793 observations 268 unique observations with > 7.00 F2/sig(F2) 1793 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 Total number of frames 314 Maximum number of 268 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1793 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 1440 observations > 7.00 F2/sig(F2) 1440 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1440 removed 31 = 1409, unique = 266) 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 1409 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 266 unique data precomputed (should be 266) 266 unique data with 1409 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1409 removed 0 = 1409, unique = 266) 266 unique data precomputed (should be 266) 266 unique data with 1409 observations RMS deviation of equivalent data = 0.69460 Rint = 0.64432 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.62659, wR= 2.76605 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68447, wR= 2.24210, Acormin=-0.245, Acormax=2.430, Acor_av=0.649 F test: Probability=0.000, F= 0.834 Trying model 2 (ne=2, no=1)... Results: Rint= 0.82586, wR= 2.04016, Acormin=-0.080, Acormax=2.048, Acor_av=0.369 F test: Probability=0.000, F= 0.572 Trying model 3 (ne=4, no=0)... Results: Rint= 0.69497, wR= 1.78337, Acormin=-0.218, Acormax=2.693, Acor_av=0.569 F test: Probability=0.000, F= 0.803 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86511, wR= 1.92845, Acormin=-0.207, Acormax=1.948, Acor_av=0.334 F test: Probability=0.000, F= 0.517 Trying model 5 (ne=4, no=3)... Results: Rint= 0.94089, wR= 2.07122, Acormin=-0.507, Acormax=2.660, Acor_av=0.056 F test: Probability=0.000, F= 0.434 Trying model 6 (ne=6, no=0)... Results: Rint= 0.70741, wR= 2.31018, Acormin=-0.380, Acormax=2.934, Acor_av=0.516 F test: Probability=0.000, F= 0.766 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87629, wR= 2.31017, Acormin=-0.442, Acormax=2.261, Acor_av=0.285 F test: Probability=0.000, F= 0.498 Trying model 8 (ne=6, no=3)... Results: Rint= 0.92508, wR= 2.08638, Acormin=-0.479, Acormax=2.499, Acor_av=0.049 F test: Probability=0.000, F= 0.444 Trying model 9 (ne=6, no=5)... Results: Rint= 0.94418, wR= 1.51424, Acormin=-0.427, Acormax=1.515, Acor_av=0.013 F test: Probability=0.000, F= 0.422 Trying model 10 (ne=8, no=0)... Results: Rint= 0.78887, wR= 2.06129, Acormin=-0.749, Acormax=1.499, Acor_av=0.277 F test: Probability=0.000, F= 0.606 Trying model 11 (ne=8, no=1)... Results: Rint= 0.92226, wR= 3.25160, Acormin=-0.507, Acormax=1.299, Acor_av=0.106 F test: Probability=0.000, F= 0.443 Trying model 12 (ne=8, no=3)... Results: Rint= 0.95257, wR= 2.37757, Acormin=-0.057, Acormax=0.063, Acor_av=0.002 F test: Probability=0.000, F= 0.412 Trying model 13 (ne=8, no=5)... Results: Rint= 0.94745, wR= 1.88051, Acormin=-0.047, Acormax=0.085, Acor_av=0.002 F test: Probability=0.000, F= 0.412 Trying model 14 (ne=8, no=7)... Results: Rint= 0.94737, wR= 1.69778, Acormin=-0.075, Acormax=0.123, Acor_av=0.001 F test: Probability=0.000, F= 0.407 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: 0.82697 There are 159 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: 2, max odd order: 0 (5 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.69460 Using Levenberg-Marquardt: 0.00010 New wR= 0.67097 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64432 with corrections 0.62776 Rint for all data: 0.82697 with corrections 0.82233 6 observations identified as outliers and rejected Cycle 2 wR= 0.63384 Using Levenberg-Marquardt: 0.00001 New wR= 0.62959 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62659 with corrections 0.60427 Rint for all data: 0.82697 with corrections 0.82224 10 observations identified as outliers and rejected Cycle 3 wR= 0.61161 Using Levenberg-Marquardt: 0.00000 New wR= 0.60673 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60626 with corrections 0.60351 Rint for all data: 0.82697 with corrections 0.83196 4 observations identified as outliers and rejected Cycle 4 wR= 0.60240 Using Levenberg-Marquardt: 0.00000 New wR= 0.83386 Using Levenberg-Marquardt: 0.00000 New wR= 0.83336 Using Levenberg-Marquardt: 0.00001 New wR= 0.82833 Using Levenberg-Marquardt: 0.00010 New wR= 0.78227 Using Levenberg-Marquardt: 0.00100 New wR= 0.61082 Using Levenberg-Marquardt: 0.01000 New wR= 0.59917 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60341 with corrections 0.61314 Rint for all data: 0.82697 with corrections 0.83715 2 observations identified as outliers and rejected Cycle 5 wR= 0.59241 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.59652 Using Levenberg-Marquardt: 0.10000 New wR= 0.59039 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60288 with corrections 0.61602 Rint for all data: 0.82697 with corrections 0.83881 0 observations identified as outliers and rejected Final wR= 0.59039 Final frame scales: Min= 0.8612 Max= 3.3608 Final absorption correction factors: Amin= 0.2158 Amax= 1.5426 PROFFIT INFO: Inet (after scale3 abspack): min=438.2553 max=10300120.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=178.8705 max=175079.7813 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1793 reflections read from tmp file 1335 reflections are rejected (1257 as outliers, 78 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 80 38 32 6 2 2 Initial Chi^2= 0.62252 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.66135 Current error model SIG(F2)^2 = 347.29*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 229.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 229.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 10300120- 1450632 179 2407486.63 85.65 100.00 1449943- 849010 179 1135648.43 50.18 100.00 844796- 309966 179 542457.85 41.81 100.00 309160- 198611 179 249686.35 32.25 100.00 197580- 150723 179 171929.96 21.95 100.00 150620- 115969 179 133377.48 16.85 100.00 115665- 82984 179 98740.28 14.27 100.00 82893- 6784 179 49691.08 10.32 93.85 6735- 3137 179 4331.57 3.06 37.43 3121- 438 182 2294.47 2.54 20.88 ------------------------------------------------------------------------------------ 10300120- 438 1793 478765.85 27.84 85.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 847005.47 56.88 97.77 1.24- 0.98 179 824015.49 41.89 93.85 0.98- 0.83 179 612118.83 32.12 88.83 0.83- 0.74 179 504013.85 28.97 87.71 0.74- 0.67 179 547360.02 26.33 87.15 0.67- 0.61 179 282428.92 19.24 81.56 0.61- 0.57 179 445677.56 23.07 82.12 0.57- 0.53 179 274767.84 17.40 77.09 0.53- 0.48 179 248733.25 16.87 78.21 0.48- 0.40 182 206107.03 15.88 76.92 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 478765.85 27.84 85.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 847005.47 56.88 97.77 5.26- 0.98 358 835510.48 49.38 95.81 5.26- 0.83 537 761046.60 43.63 93.48 5.26- 0.74 716 696788.41 39.97 92.04 5.26- 0.67 895 666902.73 37.24 91.06 5.26- 0.61 1074 602823.76 34.24 89.48 5.26- 0.57 1253 580374.30 32.64 88.43 5.26- 0.53 1432 542173.50 30.74 87.01 5.26- 0.48 1611 509569.02 29.20 86.03 5.26- 0.40 1793 478765.85 27.84 85.11 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 478765.85 27.84 85.11 Scale applied to data: s=0.097086 (maximum obs:10300120.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.839; Rsigma 0.023: data 1793 -> merged 310 With outlier rejection... Rint 0.746; Rsigma 0.024: data 1609 -> merged 310 Rejected total: 184, method kkm 177, method Blessing 7 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404282, 5.271194 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 5.60 100.00 84 1.46 - 1.12 15 15 7.67 100.00 115 1.08 - 0.96 15 15 8.40 100.00 126 0.96 - 0.86 15 15 8.60 100.00 129 0.86 - 0.79 15 15 7.40 100.00 111 0.79 - 0.73 14 15 6.57 93.33 92 0.73 - 0.69 15 15 5.87 100.00 88 0.69 - 0.65 14 15 8.00 93.33 112 0.65 - 0.63 12 15 5.25 80.00 63 0.63 - 0.60 21 21 5.19 100.00 109 --------------------------------------------------------------- 5.92 - 0.60 151 156 6.81 96.79 1029 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:22:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920255 5.916866 5.911206 60.0766 90.0920 59.9970 1609 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 791 855 782 821 1214 1079 1067 1609 N (int>3sigma) = 0 653 855 644 675 1076 918 903 1364 Mean intensity = 0.0 35.5 17.3 35.6 41.6 29.1 40.9 40.2 40.7 Mean int/sigma = 0.0 24.8 22.4 24.7 26.2 23.9 26.2 26.1 26.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.917 90.07 119.92 119.93 Niggli form: a.a = 34.942 b.b = 34.961 c.c = 35.009 b.c = -0.046 a.c = -17.447 a.b = -17.439 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.220 [ 1456] Vol = 585.9 Cell: 8.370 8.373 8.359 90.09 89.96 90.03 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.195 [ 1190] Vol = 439.4 Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 365] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.921 5.918 8.359 89.97 89.91 89.98 Volume: 292.93 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.918 5.921 8.359 90.09 90.03 89.98 Volume: 292.93 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.077 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1173] Vol = 292.9 Cell: 5.918 5.921 8.359 89.91 89.97 89.98 Volume: 292.93 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.202 [ 1182] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 89.91 90.01 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.134 [ 946] Vol = 292.9 Cell: 5.921 5.918 8.359 90.03 90.09 89.98 Volume: 292.93 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.106 MONOCLINIC I-lattice R(int) = 0.189 [ 973] Vol = 292.9 Cell: 5.911 5.920 8.370 90.05 90.01 90.09 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.050 MONOCLINIC I-lattice R(int) = 0.134 [ 910] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 90.09 89.99 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.161 [ 905] Vol = 292.9 Cell: 8.370 5.911 5.920 90.09 90.05 90.01 Volume: 292.93 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.092 MONOCLINIC C-lattice R(int) = 0.145 [ 954] Vol = 292.9 Cell: 10.246 5.913 5.917 90.07 125.19 89.92 Volume: 292.93 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 615] Vol = 146.5 Cell: 5.911 5.913 5.917 90.07 119.92 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 0 855 0 1065 1079 1609 N (int>3sigma) = 0 0 0 0 855 0 900 918 1364 Mean intensity = 0.0 0.0 0.0 0.0 17.3 0.0 39.8 40.9 40.7 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 26.3 26.2 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 123 368 N I>3s 8 8 62 368 0.6 0.6 0.4 20.0 6.4 6.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.220 1353 Fd-3m 1 1 227 C N N N N 37 2284 0.219 1391 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370302 8.372823 8.359389 90.0876 89.9607 90.0251 ZERR 1.00 0.003746 0.002320 0.000390 0.0007 0.0146 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 7025109- 923321 201 169 31 5.5 1366493.40 55.32 0.628 0.501 917554- 668084 214 195 31 6.3 694577.11 38.42 0.829 0.691 659760- 513069 217 206 31 6.6 535172.35 30.90 0.907 0.870 511747- 390511 207 185 31 6.0 396299.02 28.50 0.837 0.743 388022- 322825 215 183 31 5.9 242317.16 22.59 0.796 0.841 316529- 221801 198 165 31 5.3 196276.67 21.74 0.766 0.765 207111- 111056 190 178 31 5.7 142625.64 16.74 0.532 0.531 109712- 81703 123 108 31 3.5 97320.51 13.14 0.235 0.156 80967- 54466 138 133 31 4.3 73000.47 10.15 0.606 0.531 51504- 955 90 87 31 2.8 27036.66 6.03 0.757 0.678 ------------------------------------------------------------------------------------------- 7025109- 955 1793 1609 310 5.2 419285.06 26.40 0.746 0.641 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 263 214 31 6.9 731912.62 51.44 0.738 0.613 0.014 1.05-0.83 270 251 31 8.1 589819.82 32.28 0.841 0.769 0.020 0.83-0.72 241 215 32 6.7 457252.12 26.82 0.731 0.668 0.025 0.72-0.64 227 213 31 6.9 379683.70 23.41 0.849 0.888 0.028 0.64-0.59 200 177 34 5.2 357232.39 20.77 0.602 0.546 0.031 0.58-0.54 178 163 33 4.9 288433.23 18.25 0.843 0.842 0.035 0.54-0.51 142 131 32 4.1 242089.73 16.15 0.787 0.784 0.035 0.51-0.48 125 116 31 3.7 215384.99 16.03 0.565 0.417 0.039 0.48-0.44 94 82 31 2.6 196285.82 15.39 0.242 0.174 0.040 0.44-0.40 53 47 24 2.0 164577.75 15.40 0.109 0.093 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 1793 1609 310 5.2 419285.06 26.40 0.746 0.641 0.024 inf-0.60 1153 1029 151 6.8 519782.17 31.83 0.777 0.708 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 214 31 31 100.0 6.9 731912.62 149.94 0.738 0.007 1.05-0.83 251 31 31 100.0 8.1 589819.82 111.36 0.841 0.009 0.83-0.72 215 33 32 97.0 6.7 457252.12 76.72 0.731 0.012 0.72-0.64 213 35 31 88.6 6.9 379683.70 75.77 0.849 0.014 0.64-0.59 177 35 34 97.1 5.2 357232.39 58.40 0.602 0.019 0.58-0.54 163 39 33 84.6 4.9 288433.23 52.19 0.843 0.019 0.54-0.51 131 40 32 80.0 4.1 242089.73 42.80 0.787 0.020 0.51-0.48 116 47 31 66.0 3.7 215384.99 36.55 0.565 0.022 0.48-0.44 82 65 31 47.7 2.6 196285.82 27.87 0.242 0.025 0.44-0.40 47 108 24 22.2 2.0 164577.75 22.40 0.109 0.031 -------------------------------------------------------------------------------------------- inf-0.40 1609 464 310 66.8 5.2 419285.06 77.50 0.746 0.014 inf-0.60 1029 156 151 96.8 6.8 519782.17 98.37 0.777 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007478 0.076805 -0.034876 ( 0.000010 0.000008 0.000008 ) -0.083524 -0.011835 -0.008047 ( 0.000007 0.000005 0.000006 ) -0.012188 0.033724 0.076930 ( 0.000010 0.000008 0.000008 ) M - matrix: 0.007181 0.000003 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007176 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000005 0.000011 0.007199 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007478 0.076805 -0.034876 ( 0.000010 0.000008 0.000008 ) -0.083524 -0.011835 -0.008047 ( 0.000007 0.000005 0.000006 ) -0.012188 0.033724 0.076930 ( 0.000010 0.000008 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3704(7) 8.3729(8) 8.3596(8) 90.087(8) 89.963(7) 90.025(7) V = 585.88(9) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.88(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) PROFFIT INFO: signal sum: min=176.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=262.7288 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=16000.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=11449.0000 PROFFIT INFO: num of signal pixels: min=60 max=995 PROFFIT INFO: Inet: min=573.2264 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.3042 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.46 max=400.12 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 76 278 478 750 814 1418 2380 3238 3586 Percent 0.0 0.1 2.1 7.8 13.3 20.9 22.7 39.5 66.4 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1794 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 1794 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1607137 179 2355128.91 135.41 100.00 1603149- 1044954 179 1303619.56 111.68 100.00 1044240- 313907 179 606729.14 93.18 100.00 313609- 217815 179 254276.65 68.79 100.00 217730- 165253 179 188596.17 48.59 100.00 165202- 133569 179 149722.93 36.68 100.00 132590- 101560 179 117120.46 31.19 100.00 101378- 6457 179 59000.58 21.16 100.00 6417- 3633 179 4691.46 4.70 80.45 3624- 573 182 2663.92 3.14 42.86 ------------------------------------------------------------------------------------ 4887974- 573 1793 503315.90 55.36 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 741191.88 84.61 99.44 1.39- 1.09 179 928142.67 80.36 98.32 1.09- 0.96 179 530931.65 68.63 98.32 0.96- 0.88 179 491669.78 60.21 96.09 0.88- 0.81 179 653614.87 69.08 97.21 0.81- 0.73 179 371340.61 42.30 93.30 0.73- 0.71 179 257456.33 34.56 90.50 0.71- 0.65 179 533136.69 52.42 93.30 0.65- 0.62 179 265034.39 30.97 77.65 0.62- 0.58 182 264640.26 30.91 78.57 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 503315.90 55.36 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:22:05 2018 Sorting 1793 observations 84 unique observations with > 7.00 F2/sig(F2) 1793 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 Total number of frames 314 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1793 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 1440 observations > 7.00 F2/sig(F2) 1440 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 16.5 (Out of 1440 removed 5 = 1435, unique = 87) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1435 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 87 unique data precomputed (should be 87) 87 unique data with 1435 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 16.5 (Out of 1435 removed 0 = 1435, unique = 87) 87 unique data precomputed (should be 87) 87 unique data with 1435 observations RMS deviation of equivalent data = 0.21661 Rint = 0.17149 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16989, wR= 0.22140 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07216, wR= 0.09557, Acormin=0.648, Acormax=1.398, Acor_av=0.910 F test: Probability=1.000, F= 5.522 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07258, wR= 0.09416, Acormin=0.648, Acormax=1.372, Acor_av=0.885 F test: Probability=0.000, F= 0.986 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06182, wR= 0.08556, Acormin=0.658, Acormax=1.484, Acor_av=0.886 F test: Probability=1.000, F= 1.353 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05931, wR= 0.08109, Acormin=0.654, Acormax=1.467, Acor_av=0.879 F test: Probability=0.930, F= 1.084 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05581, wR= 0.07566, Acormin=0.510, Acormax=1.293, Acor_av=0.740 F test: Probability=1.000, F= 1.218 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05473, wR= 0.07720, Acormin=0.634, Acormax=1.454, Acor_av=0.878 F test: Probability=0.747, F= 1.037 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05242, wR= 0.07282, Acormin=0.591, Acormax=1.495, Acor_av=0.867 F test: Probability=0.986, F= 1.128 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04800, wR= 0.06675, Acormin=0.471, Acormax=1.297, Acor_av=0.723 F test: Probability=0.999, F= 1.186 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04413, wR= 0.05987, Acormin=0.333, Acormax=0.963, Acor_av=0.535 F test: Probability=0.998, F= 1.173 Trying model 10 (ne=8, no=0)... Results: Rint= 0.04926, wR= 0.06647, Acormin=0.498, Acormax=1.362, Acor_av=0.810 F test: Probability=0.000, F= 0.945 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04769, wR= 0.06416, Acormin=0.527, Acormax=1.416, Acor_av=0.813 F test: Probability=0.539, F= 1.005 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04090, wR= 0.05486, Acormin=0.345, Acormax=0.957, Acor_av=0.532 F test: Probability=1.000, F= 1.360 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03736, wR= 0.04872, Acormin=0.379, Acormax=1.045, Acor_av=0.585 F test: Probability=1.000, F= 1.616 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03408, wR= 0.04572, Acormin=0.392, Acormax=1.111, Acor_av=0.615 F test: Probability=0.999, F= 1.188 Final absorption model (ne=8, no=7): Rint= 0.03408, Acormin=0.392, Acormax=1.111, Acor_av=0.615 Combined refinement in use Rint: 0.17160 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21661 Using Levenberg-Marquardt: 0.00010 New wR= 0.04541 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17149 with corrections 0.03269 Rint for all data: 0.17160 with corrections 0.03290 1 observations identified as outliers and rejected Cycle 2 wR= 0.04283 Using Levenberg-Marquardt: 0.00001 New wR= 0.03742 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02905 Rint for all data: 0.17160 with corrections 0.02931 0 observations identified as outliers and rejected Cycle 3 wR= 0.03742 Using Levenberg-Marquardt: 0.00000 New wR= 0.03682 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02852 Rint for all data: 0.17160 with corrections 0.02879 0 observations identified as outliers and rejected Cycle 4 wR= 0.03682 Using Levenberg-Marquardt: 0.00000 New wR= 0.03640 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02820 Rint for all data: 0.17160 with corrections 0.02848 0 observations identified as outliers and rejected Cycle 5 wR= 0.03640 Using Levenberg-Marquardt: 0.00000 New wR= 0.03607 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02794 Rint for all data: 0.17160 with corrections 0.02823 0 observations identified as outliers and rejected Final wR= 0.03607 Final frame scales: Min= 0.8071 Max= 1.0895 Final absorption correction factors: Amin= 0.5317 Amax= 1.3111 PROFFIT INFO: Inet (after scale3 abspack): min=572.6086 max=5673901.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=249.4240 max=68147.6797 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1793 reflections read from tmp file 171 reflections are rejected (168 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 5 2 9 2 1 2 79 Initial Chi^2= 0.29340 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.01613 Current error model SIG(F2)^2 = 99.14*I_RAW + 0.00*I_BACK+(0.01595*)^2 Cycle 2, Chi^2= 1.00900 Current error model SIG(F2)^2 = 78.34*I_RAW + 0.00*I_BACK+(0.02030*)^2 Cycle 3, Chi^2= 1.00183 Current error model SIG(F2)^2 = 86.70*I_RAW + 0.00*I_BACK+(0.01858*)^2 Cycle 4, Chi^2= 0.99992 Current error model SIG(F2)^2 = 84.28*I_RAW + 0.00*I_BACK+(0.01916*)^2 Cycle 5, Chi^2= 1.00009 Current error model SIG(F2)^2 = 85.16*I_RAW + 0.00*I_BACK+(0.01896*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 84.86*I_RAW + 0.00*I_BACK+(0.01903*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 84.96*I_RAW + 0.00*I_BACK+(0.01900*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 84.96*I_RAW + 0.00*I_BACK+(0.01900*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5673902- 1571047 179 2283291.54 49.02 100.00 1556151- 1033333 179 1247304.26 43.17 100.00 1032759- 326579 179 607268.87 41.28 100.00 326443- 203027 179 245711.51 34.91 100.00 202987- 169728 179 185484.42 28.48 100.00 169533- 128540 179 142349.02 23.03 100.00 128402- 102481 179 116319.79 20.47 100.00 102433- 5901 179 60008.69 15.25 100.00 5894- 3435 179 4391.70 4.87 100.00 3431- 573 182 2700.15 4.00 82.97 ------------------------------------------------------------------------------------ 5673902- 573 1793 488668.52 26.41 98.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 780665.24 38.05 100.00 1.39- 1.09 179 934922.22 34.35 100.00 1.09- 0.96 179 507145.46 29.89 100.00 0.96- 0.88 179 475459.24 26.99 98.88 0.88- 0.81 179 619448.44 30.65 100.00 0.81- 0.73 179 345579.32 21.38 99.44 0.73- 0.71 179 246911.56 19.90 98.88 0.71- 0.65 179 491378.89 26.50 97.21 0.65- 0.62 179 245809.12 18.14 94.97 0.62- 0.58 182 243475.12 18.37 93.41 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 488668.52 26.41 98.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 780665.24 38.05 100.00 4.82- 1.09 358 857793.73 36.20 100.00 4.82- 0.96 537 740910.97 34.10 100.00 4.82- 0.88 716 674548.04 32.32 99.72 4.82- 0.81 895 663528.12 31.99 99.78 4.82- 0.73 1074 610536.65 30.22 99.72 4.82- 0.71 1253 558590.21 28.75 99.60 4.82- 0.65 1432 550188.80 28.46 99.30 4.82- 0.62 1611 516368.83 27.32 98.82 4.82- 0.58 1793 488668.52 26.41 98.27 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 488668.52 26.41 98.27 Scale applied to data: s=0.176245 (maximum obs:5673901.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.028; Rsigma 0.025: data 1793 -> merged 109 With outlier rejection... Rint 0.026; Rsigma 0.025: data 1780 -> merged 109 Rejected total: 13, method kkm 13, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585851, 4.831048 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 9.50 100.00 95 1.61 - 1.21 10 10 15.70 100.00 157 1.17 - 1.01 10 10 21.40 100.00 214 0.99 - 0.89 10 10 21.20 100.00 212 0.88 - 0.81 10 10 20.10 100.00 201 0.81 - 0.74 10 10 18.00 100.00 180 0.73 - 0.71 10 10 19.10 100.00 191 0.70 - 0.66 10 10 15.80 100.00 158 0.66 - 0.64 10 10 15.20 100.00 152 0.63 - 0.60 10 10 15.10 100.00 151 --------------------------------------------------------------- 5.92 - 0.60 100 100 17.11 100.00 1711 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:22:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920255 5.916866 5.911206 60.0766 90.0920 59.9970 1609 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 791 855 782 821 1214 1079 1067 1609 N (int>3sigma) = 0 653 855 644 675 1076 918 903 1364 Mean intensity = 0.0 35.5 17.3 35.6 41.6 29.1 40.9 40.2 40.7 Mean int/sigma = 0.0 24.8 22.4 24.7 26.2 23.9 26.2 26.1 26.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.917 90.07 119.92 119.93 Niggli form: a.a = 34.942 b.b = 34.961 c.c = 35.009 b.c = -0.046 a.c = -17.447 a.b = -17.439 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.220 [ 1456] Vol = 585.9 Cell: 8.370 8.373 8.359 90.09 89.96 90.03 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.195 [ 1190] Vol = 439.4 Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 365] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.921 5.918 8.359 89.97 89.91 89.98 Volume: 292.93 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.918 5.921 8.359 90.09 90.03 89.98 Volume: 292.93 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.077 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1173] Vol = 292.9 Cell: 5.918 5.921 8.359 89.91 89.97 89.98 Volume: 292.93 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.202 [ 1182] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 89.91 90.01 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.134 [ 946] Vol = 292.9 Cell: 5.921 5.918 8.359 90.03 90.09 89.98 Volume: 292.93 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.106 MONOCLINIC I-lattice R(int) = 0.189 [ 973] Vol = 292.9 Cell: 5.911 5.920 8.370 90.05 90.01 90.09 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.050 MONOCLINIC I-lattice R(int) = 0.134 [ 910] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 90.09 89.99 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.161 [ 905] Vol = 292.9 Cell: 8.370 5.911 5.920 90.09 90.05 90.01 Volume: 292.93 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.092 MONOCLINIC C-lattice R(int) = 0.145 [ 954] Vol = 292.9 Cell: 10.246 5.913 5.917 90.07 125.19 89.92 Volume: 292.93 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 615] Vol = 146.5 Cell: 5.911 5.913 5.917 90.07 119.92 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 0 855 0 1065 1079 1609 N (int>3sigma) = 0 0 0 0 855 0 900 918 1364 Mean intensity = 0.0 0.0 0.0 0.0 17.3 0.0 39.8 40.9 40.7 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 26.3 26.2 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 123 368 N I>3s 8 8 62 368 0.6 0.6 0.4 20.0 6.4 6.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.220 1353 Fd-3m 1 1 227 C N N N N 37 2284 0.219 1391 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370302 8.372823 8.359389 90.0876 89.9607 90.0251 ZERR 1.00 0.003746 0.002320 0.000390 0.0007 0.0146 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5673902- 917048 396 391 27 14.5 1680316.63 45.34 0.024 0.030 909588- 159403 528 524 27 19.4 287880.05 34.15 0.028 0.034 151938- 53321 449 447 27 16.6 114877.93 20.40 0.043 0.056 22849- 1570 420 418 28 14.9 4658.89 5.04 0.146 0.175 ------------------------------------------------------------------------------------------- 5673902- 1570 1793 1780 109 16.3 483792.58 26.32 0.026 0.032 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 433 428 27 15.9 757649.69 35.60 0.026 0.031 0.021 1.01-0.78 562 561 28 20.0 476097.58 25.61 0.021 0.027 0.025 0.76-0.65 478 475 28 17.0 388949.50 23.02 0.028 0.035 0.028 0.65-0.59 320 316 26 12.2 269098.00 19.96 0.035 0.041 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 1793 1780 109 16.3 483792.58 26.32 0.026 0.032 0.025 inf-0.60 1719 1709 99 17.3 495943.57 26.69 0.026 0.032 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 428 27 27 100.0 15.9 757649.69 163.16 0.026 0.008 1.01-0.78 561 28 28 100.0 20.0 476097.58 122.56 0.021 0.006 0.76-0.65 475 28 28 100.0 17.0 388949.50 102.15 0.028 0.008 0.65-0.59 316 27 26 96.3 12.2 269098.00 79.13 0.035 0.011 -------------------------------------------------------------------------------------------- inf-0.59 1780 110 109 99.1 16.3 483792.58 119.16 0.026 0.008 inf-0.60 1709 99 99 100.0 17.3 495943.57 121.79 0.026 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:23:07 2018) ID: 2932; threads 39; handles 875; mem 519000.00 (1237724.00)kB; time: 1w 5d 22h 28m 38s MEMORY INFO: Memory PF:0.0, Ph:163.0, V:1208.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:506.9,peak PF: 708.5, WS: 271.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:163.0, V:1210.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:508.7,peak PF: 708.5, WS: 272.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:23:07 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000017 0.000020 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000020 0.000018 ) 5.91535 ( 0.00092 ) 5.92288 ( 0.00071 ) 5.91286 ( 0.00100 ) 59.95509 ( 0.01499 ) 89.89521 ( 0.01319 ) 59.99590 ( 0.01445 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:23:07 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000017 0.000020 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000020 0.000018 ) M - matrix: 0.021551 -0.014378 0.007214 ( 0.000004 0.000003 0.000003 ) -0.014378 0.028724 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007214 -0.014365 0.021583 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(9) 5.9229(7) 5.9129(10) 59.955(15) 89.895(13) 59.996(14) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 134 | 1.152 ( 0.115) | 1.267 ( 0.416) | 1.401 ( 0.739) | 13.2-19.1 | 134 | 1.149 ( 0.122) | 1.199 ( 0.290) | 1.356 ( 0.726) | 19.1-23.2 | 134 | 1.159 ( 0.095) | 1.226 ( 0.351) | 1.280 ( 0.649) | 23.3-27.4 | 134 | 1.144 ( 0.094) | 1.177 ( 0.315) | 1.235 ( 0.522) | 27.5-30.7 | 134 | 1.145 ( 0.108) | 1.159 ( 0.190) | 1.209 ( 0.450) | 30.7-34.1 | 134 | 1.155 ( 0.089) | 1.156 ( 0.229) | 1.222 ( 0.450) | 34.1-37.3 | 134 | 1.142 ( 0.114) | 1.120 ( 0.173) | 1.124 ( 0.383) | 37.3-39.9 | 134 | 1.162 ( 0.118) | 1.123 ( 0.200) | 1.302 ( 0.566) | 39.9-43.0 | 134 | 1.171 ( 0.121) | 1.106 ( 0.197) | 1.245 ( 0.607) | 43.0-49.8 | 131 | 1.210 ( 0.166) | 1.131 ( 0.249) | 1.189 ( 0.480) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1337 | 1.159 ( 0.117) | 1.167 ( 0.276) | 1.257 ( 0.575) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0015 b=1.03 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5021 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 454025 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:23:18 2018 PROFFITMAIN - Started at Wed Mar 28 13:23:18 2018 OTKP changes: 1337 2 2 3 OTKP changes: 1337 2 2 3 UB - matrix: -0.104236 -0.015019 0.049550 ( 0.000016 0.000020 0.000018 ) 0.087415 -0.167197 0.063696 ( 0.000011 0.000013 0.000012 ) 0.055451 -0.024364 0.122925 ( 0.000017 0.000020 0.000019 ) M - matrix: 0.021581 -0.014401 0.007219 ( 0.000004 0.000003 0.000003 ) -0.014401 0.028774 -0.014389 ( 0.000003 0.000005 0.000004 ) 0.007219 -0.014389 0.021623 ( 0.000003 0.000004 0.000005 ) UB fit with 1337 obs out of 1337 (total:1337,skipped:0) (100.00%) unit cell: 5.9163(9) 5.9119(7) 5.9052(10) 60.074(15) 90.071(13) 59.984(14) V = 146.09(4) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104072 -0.015246 0.049844 ( 0.000025 0.000032 0.000028 ) 0.087353 -0.167037 0.063630 ( 0.000017 0.000021 0.000019 ) 0.055427 -0.024100 0.122528 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021534 -0.014340 0.007162 ( 0.000006 0.000005 0.000005 ) -0.014340 0.028715 -0.014341 ( 0.000005 0.000007 0.000005 ) 0.007162 -0.014341 0.021546 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9166(14) 5.9141(10) 5.9142(13) 60.04(2) 90.000(18) 60.03(2) V = 146.47(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104068 -0.015211 0.049828 ( 0.000024 0.000031 0.000027 ) 0.087423 -0.167172 0.063736 ( 0.000017 0.000021 0.000019 ) 0.055466 -0.024165 0.122560 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021549 -0.014372 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014372 0.028762 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9175(13) 5.9136(10) 5.9145(13) 60.01(2) 90.006(18) 60.00(2) V = 146.38(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104504 -0.014334 0.049188 ( 0.000037 0.000046 0.000040 ) 0.087169 -0.167093 0.063777 ( 0.000025 0.000032 0.000028 ) 0.055307 -0.024956 0.122919 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021578 -0.014448 0.007217 ( 0.000009 0.000007 0.000006 ) -0.014448 0.028748 -0.014429 ( 0.000007 0.000011 0.000007 ) 0.007217 -0.014429 0.021596 ( 0.000006 0.000007 0.000008 ) unit cell: 5.928(2) 5.9370(14) 5.9204(16) 59.89(3) 89.86(3) 59.80(3) V = 146.81(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104463 -0.014618 0.048941 ( 0.000028 0.000035 0.000030 ) 0.087192 -0.167145 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055354 -0.024843 0.123246 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021579 -0.014422 0.007258 ( 0.000008 0.000006 0.000006 ) -0.014422 0.028768 -0.014414 ( 0.000006 0.000010 0.000006 ) 0.007258 -0.014414 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9213(15) 5.9180(13) 5.9083(15) 60.06(2) 90.13(2) 59.97(2) V = 146.30(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104463 -0.014618 0.048941 ( 0.000028 0.000035 0.000030 ) 0.087192 -0.167145 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055354 -0.024843 0.123246 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021579 -0.014422 0.007258 ( 0.000008 0.000006 0.000006 ) -0.014422 0.028768 -0.014414 ( 0.000006 0.000010 0.000006 ) 0.007258 -0.014414 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9213(15) 5.9180(13) 5.9083(15) 60.06(2) 90.13(2) 59.97(2) V = 146.30(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146822 -0.097941 0.049174 ( 0.000021 0.000026 0.000023 ) -0.000019 0.138470 -0.069298 ( 0.000023 0.000029 0.000025 ) -0.000024 0.000035 0.119967 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021557 -0.014383 0.007218 ( 0.000006 0.000005 0.000005 ) -0.014383 0.028766 -0.014408 ( 0.000005 0.000009 0.000006 ) 0.007218 -0.014408 0.021612 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9179(10) 5.9154(14) 5.9116(14) 60.00(2) 90.059(17) 60.02(2) V = 146.31(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104208 -0.014952 0.049403 ( 0.000017 0.000020 0.000019 ) 0.087312 -0.167050 0.063643 ( 0.000011 0.000013 0.000012 ) 0.055395 -0.024380 0.122848 ( 0.000016 0.000020 0.000018 ) M - matrix: 0.021551 -0.014378 0.007214 ( 0.000004 0.000003 0.000003 ) -0.014378 0.028724 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007214 -0.014365 0.021583 ( 0.000003 0.000003 0.000005 ) UB fit with 1337 obs out of 1337 (total:1337,skipped:0) (100.00%) unit cell: 5.9203(9) 5.9169(7) 5.9112(10) 60.077(15) 90.092(13) 59.997(14) V = 146.46(4) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 34 reflections under beam stop or inside a detector rejection region 12 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof 1794 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:23:21 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) PROFFIT INFO: signal sum: min=176.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=262.7288 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=16000.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=11449.0000 PROFFIT INFO: num of signal pixels: min=60 max=995 PROFFIT INFO: Inet: min=573.2264 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.3042 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.46 max=400.12 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 38 139 239 375 407 709 1190 1619 1793 Percent 0.0 0.1 2.1 7.8 13.3 20.9 22.7 39.5 66.4 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1794 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 1794 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1607137 179 2355128.91 135.41 100.00 1603149- 1044954 179 1303619.56 111.68 100.00 1044240- 313907 179 606729.14 93.18 100.00 313609- 217815 179 254276.65 68.79 100.00 217730- 165253 179 188596.17 48.59 100.00 165202- 133569 179 149722.93 36.68 100.00 132590- 101560 179 117120.46 31.19 100.00 101378- 6457 179 59000.58 21.16 100.00 6417- 3633 179 4691.46 4.70 80.45 3624- 573 182 2663.92 3.14 42.86 ------------------------------------------------------------------------------------ 4887974- 573 1793 503315.90 55.36 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 667499.58 83.72 99.44 1.24- 0.98 179 771880.68 73.55 97.77 0.98- 0.83 179 615058.24 63.25 96.09 0.83- 0.74 179 541901.14 64.49 94.97 0.74- 0.67 179 558447.66 60.09 93.30 0.67- 0.61 179 343858.56 43.45 93.30 0.61- 0.57 179 521930.19 52.53 91.06 0.57- 0.53 179 343105.65 39.21 83.80 0.53- 0.48 179 345410.06 37.98 86.59 0.48- 0.40 182 327021.88 35.71 86.26 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 503315.90 55.36 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:23:21 2018 Sorting 1793 observations 268 unique observations with > 7.00 F2/sig(F2) 1793 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 Total number of frames 314 Maximum number of 268 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1793 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 1440 observations > 7.00 F2/sig(F2) 1440 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1440 removed 31 = 1409, unique = 266) 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 1409 observations in 3 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 Total number of frames 159 266 unique data precomputed (should be 266) 266 unique data with 1409 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1409 removed 0 = 1409, unique = 266) 266 unique data precomputed (should be 266) 266 unique data with 1409 observations RMS deviation of equivalent data = 0.69460 Rint = 0.64432 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.62659, wR= 2.76605 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68447, wR= 2.24210, Acormin=-0.245, Acormax=2.430, Acor_av=0.649 F test: Probability=0.000, F= 0.834 Trying model 2 (ne=2, no=1)... Results: Rint= 0.82586, wR= 2.04016, Acormin=-0.080, Acormax=2.048, Acor_av=0.369 F test: Probability=0.000, F= 0.572 Trying model 3 (ne=4, no=0)... Results: Rint= 0.69497, wR= 1.78337, Acormin=-0.218, Acormax=2.693, Acor_av=0.569 F test: Probability=0.000, F= 0.803 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86511, wR= 1.92845, Acormin=-0.207, Acormax=1.948, Acor_av=0.334 F test: Probability=0.000, F= 0.517 Trying model 5 (ne=4, no=3)... Results: Rint= 0.94089, wR= 2.07122, Acormin=-0.507, Acormax=2.660, Acor_av=0.056 F test: Probability=0.000, F= 0.434 Trying model 6 (ne=6, no=0)... Results: Rint= 0.70741, wR= 2.31018, Acormin=-0.380, Acormax=2.934, Acor_av=0.516 F test: Probability=0.000, F= 0.766 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87629, wR= 2.31017, Acormin=-0.442, Acormax=2.261, Acor_av=0.285 F test: Probability=0.000, F= 0.498 Trying model 8 (ne=6, no=3)... Results: Rint= 0.92508, wR= 2.08638, Acormin=-0.479, Acormax=2.499, Acor_av=0.049 F test: Probability=0.000, F= 0.444 Trying model 9 (ne=6, no=5)... Results: Rint= 0.94418, wR= 1.51424, Acormin=-0.427, Acormax=1.515, Acor_av=0.013 F test: Probability=0.000, F= 0.422 Trying model 10 (ne=8, no=0)... Results: Rint= 0.78887, wR= 2.06129, Acormin=-0.749, Acormax=1.499, Acor_av=0.277 F test: Probability=0.000, F= 0.606 Trying model 11 (ne=8, no=1)... Results: Rint= 0.92226, wR= 3.25160, Acormin=-0.507, Acormax=1.299, Acor_av=0.106 F test: Probability=0.000, F= 0.443 Trying model 12 (ne=8, no=3)... Results: Rint= 0.95257, wR= 2.37757, Acormin=-0.057, Acormax=0.063, Acor_av=0.002 F test: Probability=0.000, F= 0.412 Trying model 13 (ne=8, no=5)... Results: Rint= 0.94745, wR= 1.88051, Acormin=-0.047, Acormax=0.085, Acor_av=0.002 F test: Probability=0.000, F= 0.412 Trying model 14 (ne=8, no=7)... Results: Rint= 0.94737, wR= 1.69778, Acormin=-0.075, Acormax=0.123, Acor_av=0.001 F test: Probability=0.000, F= 0.407 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: 0.82697 There are 159 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: 2, max odd order: 0 (5 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.69460 Using Levenberg-Marquardt: 0.00010 New wR= 0.67097 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64432 with corrections 0.62776 Rint for all data: 0.82697 with corrections 0.82233 6 observations identified as outliers and rejected Cycle 2 wR= 0.63384 Using Levenberg-Marquardt: 0.00001 New wR= 0.62959 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62659 with corrections 0.60427 Rint for all data: 0.82697 with corrections 0.82224 10 observations identified as outliers and rejected Cycle 3 wR= 0.61161 Using Levenberg-Marquardt: 0.00000 New wR= 0.60673 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60626 with corrections 0.60351 Rint for all data: 0.82697 with corrections 0.83196 4 observations identified as outliers and rejected Cycle 4 wR= 0.60240 Using Levenberg-Marquardt: 0.00000 New wR= 0.83386 Using Levenberg-Marquardt: 0.00000 New wR= 0.83336 Using Levenberg-Marquardt: 0.00001 New wR= 0.82833 Using Levenberg-Marquardt: 0.00010 New wR= 0.78227 Using Levenberg-Marquardt: 0.00100 New wR= 0.61082 Using Levenberg-Marquardt: 0.01000 New wR= 0.59917 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60341 with corrections 0.61314 Rint for all data: 0.82697 with corrections 0.83715 2 observations identified as outliers and rejected Cycle 5 wR= 0.59241 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.59652 Using Levenberg-Marquardt: 0.10000 New wR= 0.59039 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60288 with corrections 0.61602 Rint for all data: 0.82697 with corrections 0.83881 0 observations identified as outliers and rejected Final wR= 0.59039 Final frame scales: Min= 0.8612 Max= 3.3608 Final absorption correction factors: Amin= 0.2158 Amax= 1.5426 PROFFIT INFO: Inet (after scale3 abspack): min=438.2553 max=10300120.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=178.8705 max=175079.7813 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1793 reflections read from tmp file 1335 reflections are rejected (1257 as outliers, 78 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 80 38 32 6 2 2 Initial Chi^2= 0.62252 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.66135 Current error model SIG(F2)^2 = 347.29*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 229.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 229.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 10300120- 1450632 179 2407486.63 85.65 100.00 1449943- 849010 179 1135648.43 50.18 100.00 844796- 309966 179 542457.85 41.81 100.00 309160- 198611 179 249686.35 32.25 100.00 197580- 150723 179 171929.96 21.95 100.00 150620- 115969 179 133377.48 16.85 100.00 115665- 82984 179 98740.28 14.27 100.00 82893- 6784 179 49691.08 10.32 93.85 6735- 3137 179 4331.57 3.06 37.43 3121- 438 182 2294.47 2.54 20.88 ------------------------------------------------------------------------------------ 10300120- 438 1793 478765.85 27.84 85.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 847005.47 56.88 97.77 1.24- 0.98 179 824015.49 41.89 93.85 0.98- 0.83 179 612118.83 32.12 88.83 0.83- 0.74 179 504013.85 28.97 87.71 0.74- 0.67 179 547360.02 26.33 87.15 0.67- 0.61 179 282428.92 19.24 81.56 0.61- 0.57 179 445677.56 23.07 82.12 0.57- 0.53 179 274767.84 17.40 77.09 0.53- 0.48 179 248733.25 16.87 78.21 0.48- 0.40 182 206107.03 15.88 76.92 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 478765.85 27.84 85.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 179 847005.47 56.88 97.77 5.26- 0.98 358 835510.48 49.38 95.81 5.26- 0.83 537 761046.60 43.63 93.48 5.26- 0.74 716 696788.41 39.97 92.04 5.26- 0.67 895 666902.73 37.24 91.06 5.26- 0.61 1074 602823.76 34.24 89.48 5.26- 0.57 1253 580374.30 32.64 88.43 5.26- 0.53 1432 542173.50 30.74 87.01 5.26- 0.48 1611 509569.02 29.20 86.03 5.26- 0.40 1793 478765.85 27.84 85.11 ------------------------------------------------------------------------------------ 5.26- 0.40 1793 478765.85 27.84 85.11 Scale applied to data: s=0.097086 (maximum obs:10300120.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.839; Rsigma 0.023: data 1793 -> merged 310 With outlier rejection... Rint 0.746; Rsigma 0.024: data 1609 -> merged 310 Rejected total: 184, method kkm 177, method Blessing 7 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404282, 5.271194 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 5.60 100.00 84 1.46 - 1.12 15 15 7.67 100.00 115 1.08 - 0.96 15 15 8.40 100.00 126 0.96 - 0.86 15 15 8.60 100.00 129 0.86 - 0.79 15 15 7.40 100.00 111 0.79 - 0.73 14 15 6.57 93.33 92 0.73 - 0.69 15 15 5.87 100.00 88 0.69 - 0.65 14 15 8.00 93.33 112 0.65 - 0.63 12 15 5.25 80.00 63 0.63 - 0.60 21 21 5.19 100.00 109 --------------------------------------------------------------- 5.92 - 0.60 151 156 6.81 96.79 1029 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:23:22 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920255 5.916866 5.911206 60.0766 90.0920 59.9970 1609 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 791 855 782 821 1214 1079 1067 1609 N (int>3sigma) = 0 653 855 644 675 1076 918 903 1364 Mean intensity = 0.0 35.5 17.3 35.6 41.6 29.1 40.9 40.2 40.7 Mean int/sigma = 0.0 24.8 22.4 24.7 26.2 23.9 26.2 26.1 26.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.917 90.07 119.92 119.93 Niggli form: a.a = 34.942 b.b = 34.961 c.c = 35.009 b.c = -0.046 a.c = -17.447 a.b = -17.439 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.220 [ 1456] Vol = 585.9 Cell: 8.370 8.373 8.359 90.09 89.96 90.03 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.195 [ 1190] Vol = 439.4 Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 365] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.921 5.918 8.359 89.97 89.91 89.98 Volume: 292.93 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.918 5.921 8.359 90.09 90.03 89.98 Volume: 292.93 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.077 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1173] Vol = 292.9 Cell: 5.918 5.921 8.359 89.91 89.97 89.98 Volume: 292.93 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.202 [ 1182] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 89.91 90.01 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.134 [ 946] Vol = 292.9 Cell: 5.921 5.918 8.359 90.03 90.09 89.98 Volume: 292.93 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.106 MONOCLINIC I-lattice R(int) = 0.189 [ 973] Vol = 292.9 Cell: 5.911 5.920 8.370 90.05 90.01 90.09 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.050 MONOCLINIC I-lattice R(int) = 0.134 [ 910] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 90.09 89.99 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.161 [ 905] Vol = 292.9 Cell: 8.370 5.911 5.920 90.09 90.05 90.01 Volume: 292.93 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.092 MONOCLINIC C-lattice R(int) = 0.145 [ 954] Vol = 292.9 Cell: 10.246 5.913 5.917 90.07 125.19 89.92 Volume: 292.93 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 615] Vol = 146.5 Cell: 5.911 5.913 5.917 90.07 119.92 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 0 855 0 1065 1079 1609 N (int>3sigma) = 0 0 0 0 855 0 900 918 1364 Mean intensity = 0.0 0.0 0.0 0.0 17.3 0.0 39.8 40.9 40.7 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 26.3 26.2 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 123 368 N I>3s 8 8 62 368 0.6 0.6 0.4 20.0 6.4 6.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.220 1353 Fd-3m 1 1 227 C N N N N 37 2284 0.219 1391 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370302 8.372823 8.359389 90.0876 89.9607 90.0251 ZERR 1.00 0.003746 0.002320 0.000390 0.0007 0.0146 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 7025109- 923321 201 169 31 5.5 1366493.40 55.32 0.628 0.501 917554- 668084 214 195 31 6.3 694577.11 38.42 0.829 0.691 659760- 513069 217 206 31 6.6 535172.35 30.90 0.907 0.870 511747- 390511 207 185 31 6.0 396299.02 28.50 0.837 0.743 388022- 322825 215 183 31 5.9 242317.16 22.59 0.796 0.841 316529- 221801 198 165 31 5.3 196276.67 21.74 0.766 0.765 207111- 111056 190 178 31 5.7 142625.64 16.74 0.532 0.531 109712- 81703 123 108 31 3.5 97320.51 13.14 0.235 0.156 80967- 54466 138 133 31 4.3 73000.47 10.15 0.606 0.531 51504- 955 90 87 31 2.8 27036.66 6.03 0.757 0.678 ------------------------------------------------------------------------------------------- 7025109- 955 1793 1609 310 5.2 419285.06 26.40 0.746 0.641 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 263 214 31 6.9 731912.62 51.44 0.738 0.613 0.014 1.05-0.83 270 251 31 8.1 589819.82 32.28 0.841 0.769 0.020 0.83-0.72 241 215 32 6.7 457252.12 26.82 0.731 0.668 0.025 0.72-0.64 227 213 31 6.9 379683.70 23.41 0.849 0.888 0.028 0.64-0.59 200 177 34 5.2 357232.39 20.77 0.602 0.546 0.031 0.58-0.54 178 163 33 4.9 288433.23 18.25 0.843 0.842 0.035 0.54-0.51 142 131 32 4.1 242089.73 16.15 0.787 0.784 0.035 0.51-0.48 125 116 31 3.7 215384.99 16.03 0.565 0.417 0.039 0.48-0.44 94 82 31 2.6 196285.82 15.39 0.242 0.174 0.040 0.44-0.40 53 47 24 2.0 164577.75 15.40 0.109 0.093 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 1793 1609 310 5.2 419285.06 26.40 0.746 0.641 0.024 inf-0.60 1153 1029 151 6.8 519782.17 31.83 0.777 0.708 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 214 31 31 100.0 6.9 731912.62 149.94 0.738 0.007 1.05-0.83 251 31 31 100.0 8.1 589819.82 111.36 0.841 0.009 0.83-0.72 215 33 32 97.0 6.7 457252.12 76.72 0.731 0.012 0.72-0.64 213 35 31 88.6 6.9 379683.70 75.77 0.849 0.014 0.64-0.59 177 35 34 97.1 5.2 357232.39 58.40 0.602 0.019 0.58-0.54 163 39 33 84.6 4.9 288433.23 52.19 0.843 0.019 0.54-0.51 131 40 32 80.0 4.1 242089.73 42.80 0.787 0.020 0.51-0.48 116 47 31 66.0 3.7 215384.99 36.55 0.565 0.022 0.48-0.44 82 65 31 47.7 2.6 196285.82 27.87 0.242 0.025 0.44-0.40 47 108 24 22.2 2.0 164577.75 22.40 0.109 0.031 -------------------------------------------------------------------------------------------- inf-0.40 1609 464 310 66.8 5.2 419285.06 77.50 0.746 0.014 inf-0.60 1029 156 151 96.8 6.8 519782.17 98.37 0.777 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007478 0.076805 -0.034876 ( 0.000010 0.000008 0.000008 ) -0.083524 -0.011835 -0.008047 ( 0.000007 0.000005 0.000006 ) -0.012188 0.033724 0.076930 ( 0.000010 0.000008 0.000008 ) M - matrix: 0.007181 0.000003 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007176 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000005 0.000011 0.007199 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007478 0.076805 -0.034876 ( 0.000010 0.000008 0.000008 ) -0.083524 -0.011835 -0.008047 ( 0.000007 0.000005 0.000006 ) -0.012188 0.033724 0.076930 ( 0.000010 0.000008 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3704(7) 8.3729(8) 8.3596(8) 90.087(8) 89.963(7) 90.025(7) V = 585.88(9) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.88(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.939) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.939) PROFFIT INFO: signal sum: min=176.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=262.7288 max=2240321.2039 PROFFIT INFO: background sum: min=846.0000 max=16000.0000 PROFFIT INFO: background sum sig2: min=626.0000 max=11449.0000 PROFFIT INFO: num of signal pixels: min=60 max=995 PROFFIT INFO: Inet: min=573.2264 max=4887974.0000 PROFFIT INFO: sig(Inet): min=190.3042 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.46 max=400.12 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 76 278 478 750 814 1418 2380 3238 3586 Percent 0.0 0.1 2.1 7.8 13.3 20.9 22.7 39.5 66.4 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1794 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 1794 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1607137 179 2355128.91 135.41 100.00 1603149- 1044954 179 1303619.56 111.68 100.00 1044240- 313907 179 606729.14 93.18 100.00 313609- 217815 179 254276.65 68.79 100.00 217730- 165253 179 188596.17 48.59 100.00 165202- 133569 179 149722.93 36.68 100.00 132590- 101560 179 117120.46 31.19 100.00 101378- 6457 179 59000.58 21.16 100.00 6417- 3633 179 4691.46 4.70 80.45 3624- 573 182 2663.92 3.14 42.86 ------------------------------------------------------------------------------------ 4887974- 573 1793 503315.90 55.36 92.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 741191.88 84.61 99.44 1.39- 1.09 179 928142.67 80.36 98.32 1.09- 0.96 179 530931.65 68.63 98.32 0.96- 0.88 179 491669.78 60.21 96.09 0.88- 0.81 179 653614.87 69.08 97.21 0.81- 0.73 179 371340.61 42.30 93.30 0.73- 0.71 179 257456.33 34.56 90.50 0.71- 0.65 179 533136.69 52.42 93.30 0.65- 0.62 179 265034.39 30.97 77.65 0.62- 0.58 182 264640.26 30.91 78.57 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 503315.90 55.36 92.25 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:23:22 2018 Sorting 1793 observations 84 unique observations with > 7.00 F2/sig(F2) 1793 observations in 3 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 Total number of frames 314 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1793 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 1440 observations > 7.00 F2/sig(F2) 1440 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 16.5 (Out of 1440 removed 5 = 1435, unique = 87) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1435 observations in 3 runs Run # start # end # total # 1 0 26 27 2 0 27 55 3 0 24 80 Total number of frames 80 87 unique data precomputed (should be 87) 87 unique data with 1435 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 16.5 (Out of 1435 removed 0 = 1435, unique = 87) 87 unique data precomputed (should be 87) 87 unique data with 1435 observations RMS deviation of equivalent data = 0.21661 Rint = 0.17149 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16989, wR= 0.22140 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07216, wR= 0.09557, Acormin=0.648, Acormax=1.398, Acor_av=0.910 F test: Probability=1.000, F= 5.522 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07258, wR= 0.09416, Acormin=0.648, Acormax=1.372, Acor_av=0.885 F test: Probability=0.000, F= 0.986 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06182, wR= 0.08556, Acormin=0.658, Acormax=1.484, Acor_av=0.886 F test: Probability=1.000, F= 1.353 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05931, wR= 0.08109, Acormin=0.654, Acormax=1.467, Acor_av=0.879 F test: Probability=0.930, F= 1.084 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05581, wR= 0.07566, Acormin=0.510, Acormax=1.293, Acor_av=0.740 F test: Probability=1.000, F= 1.218 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05473, wR= 0.07720, Acormin=0.634, Acormax=1.454, Acor_av=0.878 F test: Probability=0.747, F= 1.037 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05242, wR= 0.07282, Acormin=0.591, Acormax=1.495, Acor_av=0.867 F test: Probability=0.986, F= 1.128 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04800, wR= 0.06675, Acormin=0.471, Acormax=1.297, Acor_av=0.723 F test: Probability=0.999, F= 1.186 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04413, wR= 0.05987, Acormin=0.333, Acormax=0.963, Acor_av=0.535 F test: Probability=0.998, F= 1.173 Trying model 10 (ne=8, no=0)... Results: Rint= 0.04926, wR= 0.06647, Acormin=0.498, Acormax=1.362, Acor_av=0.810 F test: Probability=0.000, F= 0.945 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04769, wR= 0.06416, Acormin=0.527, Acormax=1.416, Acor_av=0.813 F test: Probability=0.539, F= 1.005 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04090, wR= 0.05486, Acormin=0.345, Acormax=0.957, Acor_av=0.532 F test: Probability=1.000, F= 1.360 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03736, wR= 0.04872, Acormin=0.379, Acormax=1.045, Acor_av=0.585 F test: Probability=1.000, F= 1.616 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03408, wR= 0.04572, Acormin=0.392, Acormax=1.111, Acor_av=0.615 F test: Probability=0.999, F= 1.188 Final absorption model (ne=8, no=7): Rint= 0.03408, Acormin=0.392, Acormax=1.111, Acor_av=0.615 Combined refinement in use Rint: 0.17160 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21661 Using Levenberg-Marquardt: 0.00010 New wR= 0.04541 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17149 with corrections 0.03269 Rint for all data: 0.17160 with corrections 0.03290 1 observations identified as outliers and rejected Cycle 2 wR= 0.04283 Using Levenberg-Marquardt: 0.00001 New wR= 0.03742 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02905 Rint for all data: 0.17160 with corrections 0.02931 0 observations identified as outliers and rejected Cycle 3 wR= 0.03742 Using Levenberg-Marquardt: 0.00000 New wR= 0.03682 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02852 Rint for all data: 0.17160 with corrections 0.02879 0 observations identified as outliers and rejected Cycle 4 wR= 0.03682 Using Levenberg-Marquardt: 0.00000 New wR= 0.03640 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02820 Rint for all data: 0.17160 with corrections 0.02848 0 observations identified as outliers and rejected Cycle 5 wR= 0.03640 Using Levenberg-Marquardt: 0.00000 New wR= 0.03607 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17057 with corrections 0.02794 Rint for all data: 0.17160 with corrections 0.02823 0 observations identified as outliers and rejected Final wR= 0.03607 Final frame scales: Min= 0.8071 Max= 1.0895 Final absorption correction factors: Amin= 0.5317 Amax= 1.3111 PROFFIT INFO: Inet (after scale3 abspack): min=572.6086 max=5673901.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=249.4240 max=68147.6797 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1793 reflections read from tmp file 171 reflections are rejected (168 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 5 2 9 2 1 2 79 Initial Chi^2= 0.29340 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.01613 Current error model SIG(F2)^2 = 99.14*I_RAW + 0.00*I_BACK+(0.01595*)^2 Cycle 2, Chi^2= 1.00900 Current error model SIG(F2)^2 = 78.34*I_RAW + 0.00*I_BACK+(0.02030*)^2 Cycle 3, Chi^2= 1.00183 Current error model SIG(F2)^2 = 86.70*I_RAW + 0.00*I_BACK+(0.01858*)^2 Cycle 4, Chi^2= 0.99992 Current error model SIG(F2)^2 = 84.28*I_RAW + 0.00*I_BACK+(0.01916*)^2 Cycle 5, Chi^2= 1.00009 Current error model SIG(F2)^2 = 85.16*I_RAW + 0.00*I_BACK+(0.01896*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 84.86*I_RAW + 0.00*I_BACK+(0.01903*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 84.96*I_RAW + 0.00*I_BACK+(0.01900*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 84.96*I_RAW + 0.00*I_BACK+(0.01900*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5673902- 1571047 179 2283291.54 49.02 100.00 1556151- 1033333 179 1247304.26 43.17 100.00 1032759- 326579 179 607268.87 41.28 100.00 326443- 203027 179 245711.51 34.91 100.00 202987- 169728 179 185484.42 28.48 100.00 169533- 128540 179 142349.02 23.03 100.00 128402- 102481 179 116319.79 20.47 100.00 102433- 5901 179 60008.69 15.25 100.00 5894- 3435 179 4391.70 4.87 100.00 3431- 573 182 2700.15 4.00 82.97 ------------------------------------------------------------------------------------ 5673902- 573 1793 488668.52 26.41 98.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 780665.24 38.05 100.00 1.39- 1.09 179 934922.22 34.35 100.00 1.09- 0.96 179 507145.46 29.89 100.00 0.96- 0.88 179 475459.24 26.99 98.88 0.88- 0.81 179 619448.44 30.65 100.00 0.81- 0.73 179 345579.32 21.38 99.44 0.73- 0.71 179 246911.56 19.90 98.88 0.71- 0.65 179 491378.89 26.50 97.21 0.65- 0.62 179 245809.12 18.14 94.97 0.62- 0.58 182 243475.12 18.37 93.41 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 488668.52 26.41 98.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 179 780665.24 38.05 100.00 4.82- 1.09 358 857793.73 36.20 100.00 4.82- 0.96 537 740910.97 34.10 100.00 4.82- 0.88 716 674548.04 32.32 99.72 4.82- 0.81 895 663528.12 31.99 99.78 4.82- 0.73 1074 610536.65 30.22 99.72 4.82- 0.71 1253 558590.21 28.75 99.60 4.82- 0.65 1432 550188.80 28.46 99.30 4.82- 0.62 1611 516368.83 27.32 98.82 4.82- 0.58 1793 488668.52 26.41 98.27 ------------------------------------------------------------------------------------ 4.82- 0.58 1793 488668.52 26.41 98.27 Scale applied to data: s=0.176245 (maximum obs:5673901.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.028; Rsigma 0.025: data 1793 -> merged 109 With outlier rejection... Rint 0.026; Rsigma 0.025: data 1780 -> merged 109 Rejected total: 13, method kkm 13, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585851, 4.831048 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 9.50 100.00 95 1.61 - 1.21 10 10 15.70 100.00 157 1.17 - 1.01 10 10 21.40 100.00 214 0.99 - 0.89 10 10 21.20 100.00 212 0.88 - 0.81 10 10 20.10 100.00 201 0.81 - 0.74 10 10 18.00 100.00 180 0.73 - 0.71 10 10 19.10 100.00 191 0.70 - 0.66 10 10 15.80 100.00 158 0.66 - 0.64 10 10 15.20 100.00 152 0.63 - 0.60 10 10 15.10 100.00 151 --------------------------------------------------------------- 5.92 - 0.60 100 100 17.11 100.00 1711 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:23:22 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920255 5.916866 5.911206 60.0766 90.0920 59.9970 1609 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 791 855 782 821 1214 1079 1067 1609 N (int>3sigma) = 0 653 855 644 675 1076 918 903 1364 Mean intensity = 0.0 35.5 17.3 35.6 41.6 29.1 40.9 40.2 40.7 Mean int/sigma = 0.0 24.8 22.4 24.7 26.2 23.9 26.2 26.1 26.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.917 90.07 119.92 119.93 Niggli form: a.a = 34.942 b.b = 34.961 c.c = 35.009 b.c = -0.046 a.c = -17.447 a.b = -17.439 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.220 [ 1456] Vol = 585.9 Cell: 8.370 8.373 8.359 90.09 89.96 90.03 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.195 [ 1190] Vol = 439.4 Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.109 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 365] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.506 90.04 90.03 120.05 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.070 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.921 5.918 8.359 89.97 89.91 89.98 Volume: 292.93 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.161 [ 1222] Vol = 292.9 Cell: 5.918 5.921 8.359 90.09 90.03 89.98 Volume: 292.93 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.077 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1173] Vol = 292.9 Cell: 5.918 5.921 8.359 89.91 89.97 89.98 Volume: 292.93 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.202 [ 1182] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 89.91 90.01 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.134 [ 946] Vol = 292.9 Cell: 5.921 5.918 8.359 90.03 90.09 89.98 Volume: 292.93 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.106 MONOCLINIC I-lattice R(int) = 0.189 [ 973] Vol = 292.9 Cell: 5.911 5.920 8.370 90.05 90.01 90.09 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.050 MONOCLINIC I-lattice R(int) = 0.134 [ 910] Vol = 292.9 Cell: 5.911 8.370 5.920 89.95 90.09 89.99 Volume: 292.93 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.161 [ 905] Vol = 292.9 Cell: 8.370 5.911 5.920 90.09 90.05 90.01 Volume: 292.93 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.092 MONOCLINIC C-lattice R(int) = 0.145 [ 954] Vol = 292.9 Cell: 10.246 5.913 5.917 90.07 125.19 89.92 Volume: 292.93 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 615] Vol = 146.5 Cell: 5.911 5.913 5.917 90.07 119.92 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 0 855 0 1065 1079 1609 N (int>3sigma) = 0 0 0 0 855 0 900 918 1364 Mean intensity = 0.0 0.0 0.0 0.0 17.3 0.0 39.8 40.9 40.7 Mean int/sigma = 0.0 0.0 0.0 0.0 22.4 0.0 26.3 26.2 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 123 368 N I>3s 8 8 62 368 0.6 0.6 0.4 20.0 6.4 6.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.220 1353 Fd-3m 1 1 227 C N N N N 37 2284 0.219 1391 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370302 8.372823 8.359389 90.0876 89.9607 90.0251 ZERR 1.00 0.003746 0.002320 0.000390 0.0007 0.0146 0.0008 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5673902- 917048 396 391 27 14.5 1680316.63 45.34 0.024 0.030 909588- 159403 528 524 27 19.4 287880.05 34.15 0.028 0.034 151938- 53321 449 447 27 16.6 114877.93 20.40 0.043 0.056 22849- 1570 420 418 28 14.9 4658.89 5.04 0.146 0.175 ------------------------------------------------------------------------------------------- 5673902- 1570 1793 1780 109 16.3 483792.58 26.32 0.026 0.032 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 433 428 27 15.9 757649.69 35.60 0.026 0.031 0.021 1.01-0.78 562 561 28 20.0 476097.58 25.61 0.021 0.027 0.025 0.76-0.65 478 475 28 17.0 388949.50 23.02 0.028 0.035 0.028 0.65-0.59 320 316 26 12.2 269098.00 19.96 0.035 0.041 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 1793 1780 109 16.3 483792.58 26.32 0.026 0.032 0.025 inf-0.60 1719 1709 99 17.3 495943.57 26.69 0.026 0.032 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 428 27 27 100.0 15.9 757649.69 163.16 0.026 0.008 1.01-0.78 561 28 28 100.0 20.0 476097.58 122.56 0.021 0.006 0.76-0.65 475 28 28 100.0 17.0 388949.50 102.15 0.028 0.008 0.65-0.59 316 27 26 96.3 12.2 269098.00 79.13 0.035 0.011 -------------------------------------------------------------------------------------------- inf-0.59 1780 110 109 99.1 16.3 483792.58 119.16 0.026 0.008 inf-0.60 1709 99 99 100.0 17.3 495943.57 121.79 0.026 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:27:48 2018) ID: 2932; threads 39; handles 878; mem 519592.00 (1237724.00)kB; time: 1w 5d 22h 33m 18s MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.4,peak PF: 708.5, WS: 271.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.2,peak PF: 708.5, WS: 272.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:27:48 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000017 0.000020 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000020 0.000018 ) 5.91535 ( 0.00092 ) 5.92288 ( 0.00071 ) 5.91286 ( 0.00100 ) 59.95509 ( 0.01499 ) 89.89521 ( 0.01319 ) 59.99590 ( 0.01445 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:27:48 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000017 0.000020 0.000019 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000020 0.000018 ) M - matrix: 0.021551 -0.014378 0.007214 ( 0.000004 0.000003 0.000003 ) -0.014378 0.028724 -0.014365 ( 0.000003 0.000005 0.000003 ) 0.007214 -0.014365 0.021583 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(9) 5.9229(7) 5.9129(10) 59.955(15) 89.895(13) 59.996(14) V = 146.51(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_4_1.rpb PROFFITPEAK info: 266 peaks in the peak location table UB fit with 132 obs out of 141 (total:141,skipped:0) (93.62%) UB - matrix: -0.104135 -0.015342 0.049069 ( 0.000215 0.000262 0.000087 ) 0.087828 -0.167964 0.063747 ( 0.000392 0.000476 0.000159 ) 0.055147 -0.024254 0.122957 ( 0.000336 0.000408 0.000136 ) M - matrix: 0.021599 -0.014492 0.007270 ( 0.000090 0.000086 0.000053 ) -0.014492 0.029035 -0.014442 ( 0.000086 0.000161 0.000066 ) 0.007270 -0.014442 0.021590 ( 0.000053 0.000066 0.000040 ) unit cell: 5.918(12) 5.884(16) 5.910(14) 60.2(3) 90.25(18) 60.0(3) V = 145.6(6) UB fit with 132 obs out of 141 (total:141,skipped:0) (93.62%) UB - matrix: -0.104135 -0.015342 0.049069 ( 0.000215 0.000262 0.000087 ) 0.087828 -0.167964 0.063747 ( 0.000392 0.000476 0.000159 ) 0.055147 -0.024254 0.122957 ( 0.000336 0.000408 0.000136 ) M - matrix: 0.021599 -0.014492 0.007270 ( 0.000090 0.000086 0.000053 ) -0.014492 0.029035 -0.014442 ( 0.000086 0.000161 0.000066 ) 0.007270 -0.014442 0.021590 ( 0.000053 0.000066 0.000040 ) unit cell: 5.918(12) 5.884(16) 5.910(14) 60.2(3) 90.25(18) 60.0(3) V = 145.6(6) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.103900 -0.015812 0.049340 ( 0.000226 0.000274 0.000091 ) 0.088323 -0.168441 0.064077 ( 0.000334 0.000404 0.000134 ) 0.054835 -0.023591 0.122428 ( 0.000298 0.000361 0.000120 ) M - matrix: 0.021603 -0.014528 0.007246 ( 0.000082 0.000076 0.000047 ) -0.014528 0.029179 -0.014462 ( 0.000076 0.000137 0.000058 ) 0.007246 -0.014462 0.021529 ( 0.000047 0.000058 0.000035 ) UB fit with 135 obs out of 141 (total:141,skipped:0) (95.74%) unit cell: 5.917(12) 5.871(14) 5.919(12) 60.1(2) 90.18(17) 60.0(2) V = 145.4(6) UB fit with 135 obs out of 141 (total:141,skipped:0) (95.74%) UB - matrix: -0.103900 -0.015812 0.049340 ( 0.000226 0.000274 0.000091 ) 0.088323 -0.168441 0.064077 ( 0.000334 0.000404 0.000134 ) 0.054835 -0.023591 0.122428 ( 0.000298 0.000361 0.000120 ) M - matrix: 0.021603 -0.014528 0.007246 ( 0.000082 0.000076 0.000047 ) -0.014528 0.029179 -0.014462 ( 0.000076 0.000137 0.000058 ) 0.007246 -0.014462 0.021529 ( 0.000047 0.000058 0.000035 ) unit cell: 5.917(12) 5.871(14) 5.919(12) 60.1(2) 90.18(17) 60.0(2) V = 145.4(6) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.103914 -0.015796 0.049320 ( 0.000226 0.000274 0.000091 ) 0.088310 -0.168412 0.064080 ( 0.000334 0.000404 0.000134 ) 0.054784 -0.023495 0.122361 ( 0.000297 0.000359 0.000119 ) M - matrix: 0.021598 -0.014518 0.007237 ( 0.000082 0.000075 0.000047 ) -0.014518 0.029164 -0.014446 ( 0.000075 0.000137 0.000058 ) 0.007237 -0.014446 0.021511 ( 0.000047 0.000058 0.000035 ) UB fit with 135 obs out of 141 (total:141,skipped:0) (95.74%) unit cell: 5.917(12) 5.871(14) 5.920(12) 60.1(2) 90.18(17) 60.0(2) V = 145.5(6) 141 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Run 4 Omega scan: (3.000 - 28.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103914 -0.015796 0.049320 ( 0.000226 0.000274 0.000091 ) 0.088310 -0.168412 0.064080 ( 0.000334 0.000404 0.000134 ) 0.054784 -0.023495 0.122361 ( 0.000297 0.000359 0.000119 ) M - matrix: 0.021598 -0.014518 0.007237 ( 0.000082 0.000075 0.000047 ) -0.014518 0.029164 -0.014446 ( 0.000075 0.000137 0.000058 ) 0.007237 -0.014446 0.021511 ( 0.000047 0.000058 0.000035 ) UB fit with 135 obs out of 141 (total:141,skipped:0) (95.74%) unit cell: 5.917(12) 5.871(14) 5.920(12) 60.1(2) 90.18(17) 60.0(2) V = 145.5(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 135 obs out of 141 (total:141,skipped:0) (95.74%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_1.rpb 2 of 101 peaks identified as outliers and rejected 99 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 99 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 99 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.54- 1.28 | 10 | 0.969 ( 0.126) | 1.134 ( 0.425) | 1.053 ( 0.633) | 1.27- 1.09 | 10 | 1.076 ( 0.062) | 1.102 ( 0.097) | 0.945 ( 0.352) | 1.09- 0.96 | 10 | 1.098 ( 0.102) | 1.185 ( 0.282) | 1.319 ( 0.598) | 0.96- 0.89 | 10 | 1.122 ( 0.075) | 1.145 ( 0.105) | 1.092 ( 0.329) | 0.88- 0.81 | 10 | 1.123 ( 0.068) | 1.136 ( 0.137) | 1.000 ( 0.282) | 0.81- 0.73 | 10 | 1.162 ( 0.092) | 1.078 ( 0.088) | 0.944 ( 0.315) | 0.73- 0.71 | 10 | 1.165 ( 0.062) | 1.198 ( 0.130) | 1.036 ( 0.330) | 0.70- 0.66 | 10 | 1.193 ( 0.058) | 1.127 ( 0.106) | 1.236 ( 0.469) | 0.65- 0.62 | 10 | 1.189 ( 0.080) | 1.169 ( 0.178) | 1.324 ( 0.393) | 0.62- 0.60 | 9 | 1.271 ( 0.097) | 1.144 ( 0.219) | 1.554 ( 0.420) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.54- 0.60 | 99 | 1.135 ( 0.114) | 1.142 ( 0.206) | 1.146 ( 0.467) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) UB - matrix: -0.103882 -0.016011 0.049677 ( 0.000141 0.000174 0.000054 ) 0.087717 -0.167574 0.064069 ( 0.000137 0.000169 0.000052 ) 0.054505 -0.023382 0.122286 ( 0.000098 0.000121 0.000038 ) M - matrix: 0.021457 -0.014310 0.007125 ( 0.000039 0.000034 0.000018 ) -0.014310 0.028884 -0.014391 ( 0.000034 0.000057 0.000022 ) 0.007125 -0.014391 0.021527 ( 0.000018 0.000022 0.000013 ) unit cell: 5.918(7) 5.892(6) 5.920(4) 59.95(9) 89.98(8) 60.15(11) V = 146.2(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.104317 -0.015138 0.049113 ( 0.000110 0.000136 0.000042 ) 0.087234 -0.167313 0.063742 ( 0.000126 0.000156 0.000048 ) 0.054824 -0.023992 0.122716 ( 0.000076 0.000094 0.000029 ) M - matrix: 0.021498 -0.014332 0.007165 ( 0.000033 0.000029 0.000015 ) -0.014332 0.028799 -0.014353 ( 0.000029 0.000052 0.000019 ) 0.007165 -0.014353 0.021534 ( 0.000015 0.000019 0.000010 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 5.918(5) 5.900(5) 5.915(3) 60.07(8) 90.09(6) 60.10(9) V = 146.3(2) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 28.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 273 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! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_1.rpb 3 of 100 peaks identified as outliers and rejected 97 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 97 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 97 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.27 | 10 | 0.973 ( 0.124) | 1.092 ( 0.306) | 0.973 ( 0.508) | 1.27- 1.09 | 10 | 1.093 ( 0.063) | 1.117 ( 0.096) | 1.074 ( 0.463) | 1.09- 0.96 | 10 | 1.063 ( 0.094) | 1.080 ( 0.148) | 0.957 ( 0.457) | 0.96- 0.85 | 10 | 1.130 ( 0.071) | 1.162 ( 0.096) | 1.110 ( 0.399) | 0.84- 0.81 | 10 | 1.162 ( 0.079) | 1.163 ( 0.103) | 1.167 ( 0.282) | 0.80- 0.73 | 10 | 1.158 ( 0.078) | 1.203 ( 0.253) | 1.024 ( 0.454) | 0.73- 0.69 | 10 | 1.159 ( 0.081) | 1.188 ( 0.129) | 1.025 ( 0.316) | 0.69- 0.64 | 10 | 1.175 ( 0.063) | 1.119 ( 0.076) | 1.336 ( 0.426) | 0.64- 0.62 | 10 | 1.239 ( 0.093) | 1.185 ( 0.192) | 1.417 ( 0.440) | 0.62- 0.60 | 7 | 1.262 ( 0.104) | 1.128 ( 0.241) | 1.505 ( 0.469) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.60 | 97 | 1.138 ( 0.116) | 1.144 ( 0.183) | 1.148 ( 0.460) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 143 | 1.151 ( 0.112) | 1.262 ( 0.403) | 1.394 ( 0.727) | 13.3-19.1 | 143 | 1.149 ( 0.119) | 1.196 ( 0.281) | 1.346 ( 0.714) | 19.1-23.2 | 143 | 1.157 ( 0.097) | 1.223 ( 0.341) | 1.256 ( 0.640) | 23.2-27.4 | 143 | 1.141 ( 0.095) | 1.178 ( 0.311) | 1.208 ( 0.513) | 27.4-30.6 | 143 | 1.142 ( 0.107) | 1.167 ( 0.196) | 1.213 ( 0.459) | 30.6-34.0 | 143 | 1.156 ( 0.091) | 1.154 ( 0.223) | 1.224 ( 0.451) | 34.0-37.2 | 143 | 1.141 ( 0.112) | 1.116 ( 0.171) | 1.127 ( 0.393) | 37.2-39.7 | 143 | 1.159 ( 0.119) | 1.121 ( 0.195) | 1.287 ( 0.556) | 39.8-42.8 | 143 | 1.176 ( 0.108) | 1.119 ( 0.195) | 1.247 ( 0.597) | 42.8-49.8 | 147 | 1.201 ( 0.177) | 1.118 ( 0.252) | 1.191 ( 0.482) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1434 | 1.157 ( 0.118) | 1.165 ( 0.271) | 1.249 ( 0.568) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0014 b=1.03 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5343 lp-corr: 4248 Maximum peak integral for reflections I/sig<= 100 - raw: 454025 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 17500780 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:28:01 2018 PROFFITMAIN - Started at Wed Mar 28 13:28:01 2018 OTKP changes: 1434 2 3 4 OTKP changes: 1434 2 3 4 UB - matrix: -0.104249 -0.014980 0.049487 ( 0.000016 0.000019 0.000017 ) 0.087387 -0.167222 0.063710 ( 0.000011 0.000013 0.000011 ) 0.055397 -0.024373 0.122940 ( 0.000017 0.000019 0.000017 ) M - matrix: 0.021573 -0.014401 0.007219 ( 0.000004 0.000003 0.000003 ) -0.014401 0.028782 -0.014391 ( 0.000003 0.000004 0.000003 ) 0.007219 -0.014391 0.021622 ( 0.000003 0.000003 0.000005 ) UB fit with 1434 obs out of 1434 (total:1434,skipped:0) (100.00%) unit cell: 5.9176(9) 5.9115(7) 5.9055(9) 60.073(14) 90.071(13) 59.982(14) V = 146.11(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104095 -0.015212 0.049818 ( 0.000025 0.000032 0.000028 ) 0.087330 -0.167070 0.063638 ( 0.000017 0.000022 0.000019 ) 0.055393 -0.024093 0.122513 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021531 -0.014341 0.007158 ( 0.000006 0.000005 0.000005 ) -0.014341 0.028724 -0.014342 ( 0.000005 0.000007 0.000005 ) 0.007158 -0.014342 0.021541 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9169(14) 5.9132(10) 5.9148(13) 60.03(2) 89.991(18) 60.02(2) V = 146.47(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104056 -0.015212 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087417 -0.167147 0.063725 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024160 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021544 -0.014368 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014368 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9145(10) 5.9153(13) 60.01(2) 90.007(18) 60.00(2) V = 146.44(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104056 -0.015212 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087417 -0.167147 0.063725 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024160 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021544 -0.014368 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014368 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9145(10) 5.9153(13) 60.01(2) 90.007(18) 60.00(2) V = 146.44(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104056 -0.015212 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087417 -0.167147 0.063725 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024160 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021544 -0.014368 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014368 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9145(10) 5.9153(13) 60.01(2) 90.007(18) 60.00(2) V = 146.44(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104491 -0.014351 0.049158 ( 0.000036 0.000045 0.000039 ) 0.087153 -0.167097 0.063763 ( 0.000025 0.000032 0.000028 ) 0.055265 -0.024940 0.122935 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021568 -0.014442 0.007215 ( 0.000009 0.000007 0.000006 ) -0.014442 0.028749 -0.014426 ( 0.000007 0.000011 0.000007 ) 0.007215 -0.014426 0.021595 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9286(19) 5.9357(14) 5.9198(16) 59.90(3) 89.87(2) 59.81(3) V = 146.82(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104457 -0.014604 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087175 -0.167125 0.063638 ( 0.000023 0.000028 0.000025 ) 0.055340 -0.024832 0.123224 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021573 -0.014418 0.007256 ( 0.000008 0.000006 0.000006 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014410 0.021628 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9221(15) 5.9189(13) 5.9091(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104457 -0.014604 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087175 -0.167125 0.063638 ( 0.000023 0.000028 0.000025 ) 0.055340 -0.024832 0.123224 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021573 -0.014418 0.007256 ( 0.000008 0.000006 0.000006 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014410 0.021628 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9221(15) 5.9189(13) 5.9091(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146803 -0.097926 0.049162 ( 0.000021 0.000026 0.000023 ) -0.000020 0.138450 -0.069287 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000033 0.119950 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021551 -0.014379 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028758 -0.014403 ( 0.000005 0.000009 0.000006 ) 0.007216 -0.014403 0.021605 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9187(10) 5.9163(14) 5.9125(14) 60.00(2) 90.057(17) 60.02(2) V = 146.37(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) UB - matrix: -0.104225 -0.015277 0.049255 ( 0.000107 0.000132 0.000041 ) 0.087332 -0.167471 0.063757 ( 0.000134 0.000165 0.000051 ) 0.054991 -0.024356 0.122956 ( 0.000089 0.000110 0.000034 ) M - matrix: 0.021514 -0.014373 0.007196 ( 0.000034 0.000031 0.000016 ) -0.014373 0.028873 -0.014425 ( 0.000031 0.000056 0.000020 ) 0.007196 -0.014425 0.021609 ( 0.000016 0.000020 0.000011 ) unit cell: 5.919(5) 5.900(5) 5.910(4) 60.00(8) 90.06(6) 60.07(9) V = 146.0(2) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: -0.104390 -0.015122 0.049177 ( 0.000108 0.000133 0.000042 ) 0.087238 -0.167421 0.063716 ( 0.000130 0.000160 0.000050 ) 0.054922 -0.024125 0.122801 ( 0.000082 0.000100 0.000031 ) M - matrix: 0.021524 -0.014352 0.007169 ( 0.000033 0.000030 0.000015 ) -0.014352 0.028840 -0.014374 ( 0.000030 0.000054 0.000019 ) 0.007169 -0.014374 0.021558 ( 0.000015 0.000019 0.000011 ) UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) unit cell: 5.914(5) 5.896(5) 5.912(4) 60.06(8) 90.07(6) 60.09(9) V = 146.0(2) Run 4 Omega scan: (3.000 - 28.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) HKL list info: 264 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104390 -0.015122 0.049177 ( 0.000108 0.000133 0.000042 ) 0.087238 -0.167421 0.063716 ( 0.000130 0.000160 0.000050 ) 0.054922 -0.024125 0.122801 ( 0.000082 0.000100 0.000031 ) M - matrix: 0.021524 -0.014352 0.007169 ( 0.000033 0.000030 0.000015 ) -0.014352 0.028840 -0.014374 ( 0.000030 0.000054 0.000019 ) 0.007169 -0.014374 0.021558 ( 0.000015 0.000019 0.000011 ) UB fit with 97 obs out of 97 (total:97,skipped:0) (100.00%) unit cell: 5.914(5) 5.896(5) 5.912(4) 60.06(8) 90.07(6) 60.09(9) V = 146.0(2) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104221 -0.014929 0.049364 ( 0.000016 0.000019 0.000017 ) 0.087302 -0.167057 0.063669 ( 0.000011 0.000013 0.000012 ) 0.055384 -0.024394 0.122862 ( 0.000016 0.000018 0.000016 ) M - matrix: 0.021551 -0.014380 0.007218 ( 0.000004 0.000003 0.000003 ) -0.014380 0.028726 -0.014370 ( 0.000003 0.000005 0.000003 ) 0.007218 -0.014370 0.021585 ( 0.000003 0.000003 0.000005 ) UB fit with 1434 obs out of 1434 (total:1434,skipped:0) (100.00%) unit cell: 5.9205(9) 5.9171(7) 5.9115(9) 60.072(14) 90.099(12) 60.000(14) V = 146.47(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 35 reflections under beam stop or inside a detector rejection region 15 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof 1926 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:28:05 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 28.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=241.7853 max=2240321.2039 PROFFIT INFO: background sum: min=672.0000 max=15968.0000 PROFFIT INFO: background sum sig2: min=621.0000 max=11531.0000 PROFFIT INFO: num of signal pixels: min=60 max=1002 PROFFIT INFO: Inet: min=527.5316 max=4887974.0000 PROFFIT INFO: sig(Inet): min=191.4384 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=398.61 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 40 146 254 400 437 769 1277 1739 1925 Percent 0.0 0.1 2.1 7.6 13.2 20.8 22.7 39.9 66.3 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1926 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 1926 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1584462 192 2351657.86 134.74 100.00 1577417- 1017252 192 1286655.38 110.06 100.00 1015397- 315224 192 588507.89 93.25 100.00 313937- 219179 192 255937.00 69.80 100.00 217730- 164849 192 187676.35 48.16 100.00 164524- 131964 192 148745.29 36.55 100.00 131944- 99394 192 116250.67 31.02 100.00 99186- 6501 192 57647.64 21.06 100.00 6457- 3694 192 4720.75 4.78 81.77 3648- 528 197 2673.42 3.12 43.65 ------------------------------------------------------------------------------------ 4887974- 528 1925 498755.35 55.12 92.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 192 704690.93 84.66 100.00 1.24- 0.98 192 739408.02 72.76 97.40 0.98- 0.85 192 624636.02 63.95 96.35 0.85- 0.74 192 526884.79 62.75 95.31 0.74- 0.67 192 521237.05 57.58 92.19 0.67- 0.62 192 391566.48 48.06 95.83 0.62- 0.57 192 473438.38 49.05 87.50 0.57- 0.53 192 330694.52 39.49 91.67 0.53- 0.49 192 335276.75 36.31 80.73 0.49- 0.40 197 343756.94 37.05 87.31 ------------------------------------------------------------------------------------ 5.26- 0.40 1925 498755.35 55.12 92.42 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:28:05 2018 Sorting 1925 observations 279 unique observations with > 7.00 F2/sig(F2) 1925 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 23 338 Total number of frames 338 Maximum number of 279 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1925 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 11 171 Total number of frames 171 1548 observations > 7.00 F2/sig(F2) 1548 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 11 171 Total number of frames 171 Removing 'redundancy=1' reflections Average redundancy: 5.5 (Out of 1548 removed 24 = 1524, unique = 275) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1524 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 11 171 Total number of frames 171 275 unique data precomputed (should be 275) 275 unique data with 1524 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.5 (Out of 1524 removed 0 = 1524, unique = 275) 275 unique data precomputed (should be 275) 275 unique data with 1524 observations RMS deviation of equivalent data = 0.69862 Rint = 0.64532 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.62714, wR= 2.66328 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68495, wR= 2.12774, Acormin=-0.309, Acormax=2.483, Acor_av=0.643 F test: Probability=0.000, F= 0.835 Trying model 2 (ne=2, no=1)... Results: Rint= 0.77508, wR= 1.90642, Acormin=-0.114, Acormax=2.065, Acor_av=0.424 F test: Probability=0.000, F= 0.650 Trying model 3 (ne=4, no=0)... Results: Rint= 0.70516, wR= 1.73219, Acormin=-0.245, Acormax=2.709, Acor_av=0.570 F test: Probability=0.000, F= 0.782 Trying model 4 (ne=4, no=1)... Results: Rint= 0.80277, wR= 1.80816, Acormin=-0.290, Acormax=1.841, Acor_av=0.388 F test: Probability=0.000, F= 0.602 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96451, wR= 1.62031, Acormin=-0.555, Acormax=2.884, Acor_av=0.087 F test: Probability=0.000, F= 0.415 Trying model 6 (ne=6, no=0)... Results: Rint= 0.71316, wR= 2.21624, Acormin=-0.434, Acormax=2.937, Acor_av=0.516 F test: Probability=0.000, F= 0.756 Trying model 7 (ne=6, no=1)... Results: Rint= 0.82095, wR= 2.07190, Acormin=-0.727, Acormax=2.338, Acor_av=0.336 F test: Probability=0.000, F= 0.569 Trying model 8 (ne=6, no=3)... Results: Rint= 0.95862, wR= 1.63015, Acormin=-0.619, Acormax=2.859, Acor_av=0.083 F test: Probability=0.000, F= 0.415 Trying model 9 (ne=6, no=5)... Results: Rint= 0.98084, wR= 1.63710, Acormin=-0.391, Acormax=1.877, Acor_av=0.029 F test: Probability=0.000, F= 0.393 Trying model 10 (ne=8, no=0)... Results: Rint= 0.80500, wR= 1.91492, Acormin=-0.725, Acormax=1.589, Acor_av=0.273 F test: Probability=0.000, F= 0.585 Trying model 11 (ne=8, no=1)... Results: Rint= 0.86491, wR= 2.30714, Acormin=-0.534, Acormax=1.366, Acor_av=0.171 F test: Probability=0.000, F= 0.506 Trying model 12 (ne=8, no=3)... Results: Rint= 0.95238, wR= 2.22271, Acormin=-0.056, Acormax=0.065, Acor_av=0.002 F test: Probability=0.000, F= 0.415 Trying model 13 (ne=8, no=5)... Results: Rint= 0.95399, wR= 1.98224, Acormin=-0.061, Acormax=0.060, Acor_av=0.001 F test: Probability=0.000, F= 0.410 Trying model 14 (ne=8, no=7)... Results: Rint= 0.96675, wR= 1.74181, Acormin=-0.095, Acormax=0.105, Acor_av=0.000 F test: Probability=0.000, F= 0.394 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.82772 There are 171 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: 2, max odd order: 0 (5 parameters) Refinement control: 175 pars with 15400 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.69862 Using Levenberg-Marquardt: 0.00010 New wR= 0.67522 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64532 with corrections 0.62373 Rint for all data: 0.82772 with corrections 0.81829 7 observations identified as outliers and rejected Cycle 2 wR= 0.63996 Using Levenberg-Marquardt: 0.00001 New wR= 0.63662 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62714 with corrections 0.60655 Rint for all data: 0.82772 with corrections 0.82187 11 observations identified as outliers and rejected Cycle 3 wR= 0.61821 Using Levenberg-Marquardt: 0.00000 New wR= 0.61385 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60856 with corrections 0.60448 Rint for all data: 0.82772 with corrections 0.82961 5 observations identified as outliers and rejected Cycle 4 wR= 0.60238 Using Levenberg-Marquardt: 0.00000 New wR= 0.60110 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60353 with corrections 0.62507 Rint for all data: 0.82772 with corrections 0.84078 2 observations identified as outliers and rejected Cycle 5 wR= 0.59640 Using Levenberg-Marquardt: 0.00000 New wR= 0.91216 Using Levenberg-Marquardt: 0.00000 New wR= 0.91214 Using Levenberg-Marquardt: 0.00000 New wR= 0.91185 Using Levenberg-Marquardt: 0.00001 New wR= 0.90889 Using Levenberg-Marquardt: 0.00010 New wR= 0.86906 Using Levenberg-Marquardt: 0.00100 New wR= 0.62273 Using Levenberg-Marquardt: 0.01000 New wR= 0.59183 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.60293 with corrections 0.61288 Rint for all data: 0.82772 with corrections 0.83528 1 observations identified as outliers and rejected Final wR= 0.59183 Final frame scales: Min= 1.0000 Max= 4.2992 Final absorption correction factors: Amin= 0.2979 Amax= 1.4704 PROFFIT INFO: Inet (after scale3 abspack): min=438.0765 max=12819811.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=179.1951 max=129748.4844 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 1925 reflections read from tmp file 1421 reflections are rejected (1353 as outliers, 68 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 85 38 25 14 3 1 2 1 Initial Chi^2= 0.64279 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.62729 Current error model SIG(F2)^2 = 375.51*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 235.55*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 235.55*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 12819811- 1485481 192 2382487.24 83.75 100.00 1481876- 821577 192 1153100.82 49.42 100.00 819902- 308550 192 527386.86 41.76 100.00 308508- 202617 192 251776.22 31.12 100.00 201641- 156542 192 177944.29 21.31 100.00 156533- 117782 192 137387.31 17.26 100.00 117619- 83323 192 100140.82 13.98 100.00 83283- 6767 192 49956.04 10.24 93.75 6701- 3254 192 4448.83 3.04 37.50 3249- 438 197 2353.88 2.51 19.29 ------------------------------------------------------------------------------------ 12819811- 438 1925 477460.97 27.38 84.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 192 824539.87 57.13 98.44 1.24- 0.98 192 773819.87 39.99 93.23 0.98- 0.85 192 626598.77 32.45 89.58 0.85- 0.74 192 489285.05 27.84 85.94 0.74- 0.67 192 528557.32 24.93 84.90 0.67- 0.62 192 345489.16 20.90 83.85 0.62- 0.57 192 424923.37 21.31 79.69 0.57- 0.53 192 291605.04 17.28 83.85 0.53- 0.49 192 249274.70 15.98 70.83 0.49- 0.40 197 227038.02 16.24 78.68 ------------------------------------------------------------------------------------ 5.26- 0.40 1925 477460.97 27.38 84.88 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.24 192 824539.87 57.13 98.44 5.26- 0.98 384 799179.87 48.56 95.83 5.26- 0.85 576 741652.83 43.19 93.75 5.26- 0.74 768 678560.89 39.35 91.80 5.26- 0.67 960 648560.17 36.47 90.42 5.26- 0.62 1152 598048.34 33.87 89.32 5.26- 0.57 1344 573316.20 32.08 87.95 5.26- 0.53 1536 538102.31 30.23 87.43 5.26- 0.49 1728 506010.35 28.65 85.59 5.26- 0.40 1925 477460.97 27.38 84.88 ------------------------------------------------------------------------------------ 5.26- 0.40 1925 477460.97 27.38 84.88 Scale applied to data: s=0.078004 (maximum obs:12819811.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.835; Rsigma 0.024: data 1925 -> merged 313 With outlier rejection... Rint 0.736; Rsigma 0.025: data 1743 -> merged 313 Rejected total: 182, method kkm 172, method Blessing 10 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404289, 5.271289 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 6.93 100.00 104 1.46 - 1.12 15 15 8.93 100.00 134 1.08 - 0.96 15 15 9.13 100.00 137 0.96 - 0.86 15 15 9.07 100.00 136 0.86 - 0.79 15 15 8.53 100.00 128 0.79 - 0.73 14 15 7.71 93.33 108 0.73 - 0.69 15 15 6.80 100.00 102 0.69 - 0.65 14 15 8.36 93.33 117 0.65 - 0.63 13 15 5.46 86.67 71 0.63 - 0.60 21 21 5.57 100.00 117 --------------------------------------------------------------- 5.91 - 0.60 152 156 7.59 97.44 1154 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:28:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920520 5.917122 5.911526 60.0717 90.0989 60.0000 1743 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.12 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 849 938 843 885 1315 1170 1147 1743 N (int>3sigma) = 0 696 938 690 725 1162 996 970 1473 Mean intensity = 0.0 27.7 14.3 27.8 33.5 22.9 33.4 31.8 32.4 Mean int/sigma = 0.0 24.3 22.5 24.1 26.0 23.6 26.0 25.8 26.1 Lattice type: P chosen Volume: 146.47 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.912 5.917 90.07 119.93 119.92 Niggli form: a.a = 34.946 b.b = 34.954 c.c = 35.012 b.c = -0.044 a.c = -17.452 a.b = -17.434 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.112 CUBIC F-lattice R(int) = 0.204 [ 1589] Vol = 585.9 Cell: 8.370 8.374 8.359 90.09 89.95 90.02 Volume: 585.88 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.110 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 1321] Vol = 439.4 Cell: 5.919 5.912 14.506 90.03 90.04 120.04 Volume: 439.41 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.110 RHOMBOHEDRAL R-lattice R(int) = 0.165 [ 407] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.506 90.03 90.04 120.04 Volume: 439.41 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.069 TETRAGONAL I-lattice R(int) = 0.151 [ 1357] Vol = 292.9 Cell: 5.921 5.919 8.359 89.97 89.90 89.97 Volume: 292.94 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.131 TETRAGONAL I-lattice R(int) = 0.151 [ 1357] Vol = 292.9 Cell: 5.919 5.921 8.359 90.10 90.03 89.97 Volume: 292.94 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.076 ORTHORHOMBIC I-lattice R(int) = 0.139 [ 1307] Vol = 292.9 Cell: 5.919 5.921 8.359 89.90 89.97 89.97 Volume: 292.94 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.073 ORTHORHOMBIC I-lattice R(int) = 0.180 [ 1314] Vol = 292.9 Cell: 5.912 8.370 5.921 89.95 89.90 90.02 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.125 [ 1038] Vol = 292.9 Cell: 5.921 5.919 8.359 90.03 90.10 89.97 Volume: 292.94 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.112 MONOCLINIC I-lattice R(int) = 0.170 [ 1072] Vol = 292.9 Cell: 5.912 5.921 8.370 90.05 90.02 90.10 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.060 MONOCLINIC I-lattice R(int) = 0.124 [ 1036] Vol = 292.9 Cell: 5.912 8.370 5.921 89.95 90.10 89.98 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.045 MONOCLINIC I-lattice R(int) = 0.150 [ 1035] Vol = 292.9 Cell: 5.921 5.912 8.370 89.98 90.05 89.90 Volume: 292.94 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.094 MONOCLINIC C-lattice R(int) = 0.152 [ 1076] Vol = 292.9 Cell: 10.247 5.912 5.917 90.07 125.20 89.92 Volume: 292.94 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.102 [ 701] Vol = 146.5 Cell: 5.912 5.912 5.917 90.07 119.93 119.92 Volume: 146.47 Matrix: 0.0000 0.0000 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 0 938 0 1153 1170 1743 N (int>3sigma) = 0 0 0 0 938 0 974 996 1473 Mean intensity = 0.0 0.0 0.0 0.0 14.3 0.0 31.8 33.4 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.5 0.0 26.1 26.0 26.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 128 409 N I>3s 9 9 60 409 0.5 0.5 0.3 16.6 7.2 7.2 3.6 27.6 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 0.204 1481 Fd-3m 1 1 227 C N N N N 37 2284 0.205 1519 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.369921 8.373740 8.359298 90.0871 89.9525 90.0185 ZERR 1.00 0.003535 0.002161 0.000363 0.0002 0.0137 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5109482- 888915 226 197 31 6.4 1314222.43 54.37 0.615 0.491 887316- 671875 210 191 31 6.2 645764.05 35.66 0.837 0.712 670067- 539421 236 218 31 7.0 548870.66 30.74 0.938 0.825 520065- 411280 228 208 31 6.7 392546.78 28.13 0.824 0.768 410407- 330484 215 188 31 6.1 252706.94 23.50 0.752 0.806 329114- 220339 222 188 31 6.1 211229.63 22.32 0.708 0.728 211035- 122175 183 174 31 5.6 148470.00 16.67 0.592 0.568 121862- 83764 174 163 31 5.3 102886.85 12.95 0.367 0.277 83104- 59062 128 118 31 3.8 73748.77 10.52 0.474 0.347 55982- 930 103 98 34 2.9 28744.40 6.02 0.762 0.683 ------------------------------------------------------------------------------------------- 5109482- 930 1925 1743 313 5.6 415886.41 26.12 0.736 0.633 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 286 255 31 8.2 681715.50 50.76 0.687 0.580 0.014 1.05-0.83 298 271 31 8.7 573884.87 31.46 0.869 0.800 0.021 0.83-0.72 260 247 31 8.0 477685.88 26.13 0.768 0.758 0.025 0.72-0.64 247 230 31 7.4 377597.32 22.35 0.804 0.844 0.029 0.64-0.59 195 169 31 5.5 355124.81 19.95 0.637 0.572 0.032 0.59-0.56 185 164 32 5.1 219176.27 15.03 0.706 0.601 0.043 0.55-0.52 151 136 31 4.4 316330.49 18.91 0.756 0.683 0.033 0.51-0.49 115 103 31 3.3 177822.92 14.14 0.498 0.336 0.042 0.49-0.46 109 98 31 3.2 219513.62 15.90 0.448 0.325 0.039 0.46-0.40 79 70 33 2.1 169770.21 14.96 0.235 0.175 0.043 ------------------------------------------------------------------------------------------------------ inf-0.40 1925 1743 313 5.6 415886.41 26.12 0.736 0.633 0.025 inf-0.60 1263 1154 152 7.6 509052.53 31.23 0.766 0.711 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 255 31 31 100.0 8.2 681715.50 158.73 0.687 0.006 1.05-0.83 271 31 31 100.0 8.7 573884.87 114.10 0.869 0.009 0.83-0.72 247 32 31 96.9 8.0 477685.88 82.59 0.768 0.013 0.72-0.64 230 34 31 91.2 7.4 377597.32 74.84 0.804 0.015 0.64-0.59 169 31 31 100.0 5.5 355124.81 58.78 0.637 0.019 0.59-0.56 164 37 32 86.5 5.1 219176.27 41.52 0.706 0.023 0.55-0.52 136 37 31 83.8 4.4 316330.49 50.59 0.756 0.020 0.51-0.49 103 43 31 72.1 3.3 177822.92 30.73 0.498 0.024 0.49-0.46 98 57 31 54.4 3.2 219513.62 32.96 0.448 0.024 0.46-0.40 70 126 33 26.2 2.1 169770.21 24.21 0.235 0.029 -------------------------------------------------------------------------------------------- inf-0.40 1743 459 313 68.2 5.6 415886.41 80.74 0.736 0.014 inf-0.60 1154 156 152 97.4 7.6 509052.53 102.22 0.766 0.011 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007464 0.076790 -0.034893 ( 0.000009 0.000007 0.000008 ) -0.083528 -0.011817 -0.008044 ( 0.000007 0.000005 0.000006 ) -0.012196 0.033738 0.076925 ( 0.000009 0.000007 0.000008 ) M - matrix: 0.007181 0.000002 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007175 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000006 0.000011 0.007200 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007464 0.076790 -0.034893 ( 0.000009 0.000007 0.000008 ) -0.083528 -0.011817 -0.008044 ( 0.000007 0.000005 0.000006 ) -0.012196 0.033738 0.076925 ( 0.000009 0.000007 0.000008 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3700(7) 8.3740(7) 8.3594(7) 90.087(7) 89.954(7) 90.019(7) V = 585.91(9) unit cell: 8.3678(2) 8.3678(2) 8.3678(2) 90.0 90.0 90.0 V = 585.91(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 28.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=19682688.0000 PROFFIT INFO: signal sum lp corr: min=241.7853 max=2240321.2039 PROFFIT INFO: background sum: min=672.0000 max=15968.0000 PROFFIT INFO: background sum sig2: min=621.0000 max=11531.0000 PROFFIT INFO: num of signal pixels: min=60 max=1002 PROFFIT INFO: Inet: min=527.5316 max=4887974.0000 PROFFIT INFO: sig(Inet): min=191.4384 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=398.61 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 80 292 508 800 874 1538 2554 3478 3850 Percent 0.0 0.1 2.1 7.6 13.2 20.8 22.7 39.9 66.3 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1926 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 1926 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4887974- 1584462 192 2351657.86 134.74 100.00 1577417- 1017252 192 1286655.38 110.06 100.00 1015397- 315224 192 588507.89 93.25 100.00 313937- 219179 192 255937.00 69.80 100.00 217730- 164849 192 187676.35 48.16 100.00 164524- 131964 192 148745.29 36.55 100.00 131944- 99394 192 116250.67 31.02 100.00 99186- 6501 192 57647.64 21.06 100.00 6457- 3694 192 4720.75 4.78 81.77 3648- 528 197 2673.42 3.12 43.65 ------------------------------------------------------------------------------------ 4887974- 528 1925 498755.35 55.12 92.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 192 755513.86 86.13 99.48 1.39- 1.09 192 926860.37 80.04 98.44 1.09- 0.96 192 512955.25 67.17 98.44 0.96- 0.88 192 489564.83 59.80 95.83 0.88- 0.81 192 650852.31 69.11 97.40 0.81- 0.73 192 362079.66 42.09 93.23 0.73- 0.71 192 256923.98 34.77 90.10 0.71- 0.65 192 521148.18 51.71 94.79 0.65- 0.62 192 261435.72 30.41 77.08 0.62- 0.58 197 256527.31 30.59 79.70 ------------------------------------------------------------------------------------ 4.82- 0.58 1925 498755.35 55.12 92.42 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:28:06 2018 Sorting 1925 observations 84 unique observations with > 7.00 F2/sig(F2) 1925 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 23 338 Total number of frames 338 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 1925 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 4 69 Total number of frames 69 1548 observations > 7.00 F2/sig(F2) 1548 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 4 69 Total number of frames 69 Removing 'redundancy=1' reflections Average redundancy: 17.5 (Out of 1548 removed 4 = 1544, unique = 88) 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 1544 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 4 69 Total number of frames 69 88 unique data precomputed (should be 88) 88 unique data with 1544 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 17.5 (Out of 1544 removed 0 = 1544, unique = 88) 88 unique data precomputed (should be 88) 88 unique data with 1544 observations RMS deviation of equivalent data = 0.22058 Rint = 0.17484 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17341, wR= 0.22576 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08056, wR= 0.10896, Acormin=0.652, Acormax=1.412, Acor_av=0.919 F test: Probability=1.000, F= 4.617 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08139, wR= 0.10149, Acormin=0.610, Acormax=1.352, Acor_av=0.886 F test: Probability=0.000, F= 0.978 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06829, wR= 0.09594, Acormin=0.662, Acormax=1.504, Acor_av=0.893 F test: Probability=1.000, F= 1.383 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06397, wR= 0.08580, Acormin=0.618, Acormax=1.462, Acor_av=0.881 F test: Probability=0.993, F= 1.137 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05970, wR= 0.08044, Acormin=0.519, Acormax=1.350, Acor_av=0.811 F test: Probability=0.994, F= 1.143 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06231, wR= 0.08780, Acormin=0.625, Acormax=1.477, Acor_av=0.886 F test: Probability=0.000, F= 0.916 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05842, wR= 0.07909, Acormin=0.579, Acormax=1.488, Acor_av=0.869 F test: Probability=0.769, F= 1.040 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05442, wR= 0.07287, Acormin=0.511, Acormax=1.387, Acor_av=0.800 F test: Probability=1.000, F= 1.193 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04429, wR= 0.06366, Acormin=0.432, Acormax=1.265, Acor_av=0.708 F test: Probability=1.000, F= 1.498 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05640, wR= 0.07469, Acormin=0.435, Acormax=1.329, Acor_av=0.791 F test: Probability=0.000, F= 0.619 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05374, wR= 0.06921, Acormin=0.519, Acormax=1.424, Acor_av=0.821 F test: Probability=0.000, F= 0.680 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04552, wR= 0.05900, Acormin=0.310, Acormax=0.874, Acor_av=0.492 F test: Probability=0.000, F= 0.943 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03776, wR= 0.05034, Acormin=0.346, Acormax=0.999, Acor_av=0.561 F test: Probability=1.000, F= 1.359 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03575, wR= 0.04740, Acormin=0.360, Acormax=1.070, Acor_av=0.592 F test: Probability=1.000, F= 1.500 Final absorption model (ne=8, no=7): Rint= 0.03575, Acormin=0.360, Acormax=1.070, Acor_av=0.592 Combined refinement in use Rint: 0.17496 There are 69 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: 8, max odd order: 7 (80 parameters) Refinement control: 148 pars with 11026 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22058 Using Levenberg-Marquardt: 0.00010 New wR= 0.04349 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17484 with corrections 0.03303 Rint for all data: 0.17496 with corrections 0.03325 0 observations identified as outliers and rejected Cycle 2 wR= 0.04349 Using Levenberg-Marquardt: 0.00001 New wR= 0.03981 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17484 with corrections 0.03079 Rint for all data: 0.17496 with corrections 0.03101 0 observations identified as outliers and rejected Cycle 3 wR= 0.03981 Using Levenberg-Marquardt: 0.00000 New wR= 0.03939 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17484 with corrections 0.03037 Rint for all data: 0.17496 with corrections 0.03059 0 observations identified as outliers and rejected Cycle 4 wR= 0.03939 Using Levenberg-Marquardt: 0.00000 New wR= 0.03911 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17484 with corrections 0.03015 Rint for all data: 0.17496 with corrections 0.03037 0 observations identified as outliers and rejected Cycle 5 wR= 0.03911 Using Levenberg-Marquardt: 0.00000 New wR= 0.03891 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17484 with corrections 0.02999 Rint for all data: 0.17496 with corrections 0.03021 0 observations identified as outliers and rejected Final wR= 0.03891 Final frame scales: Min= 0.8082 Max= 1.0744 Final absorption correction factors: Amin= 0.4603 Amax= 1.3671 PROFFIT INFO: Inet (after scale3 abspack): min=535.4872 max=5692145.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=206.6831 max=67772.8828 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 1925 reflections read from tmp file 203 reflections are rejected (200 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 2 6 2 5 5 2 2 79 Initial Chi^2= 0.31094 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.03730 Current error model SIG(F2)^2 = 107.26*I_RAW + 0.00*I_BACK+(0.01358*)^2 Cycle 2, Chi^2= 1.00788 Current error model SIG(F2)^2 = 86.81*I_RAW + 0.00*I_BACK+(0.01845*)^2 Cycle 3, Chi^2= 1.00096 Current error model SIG(F2)^2 = 93.86*I_RAW + 0.00*I_BACK+(0.01702*)^2 Cycle 4, Chi^2= 0.99994 Current error model SIG(F2)^2 = 92.41*I_RAW + 0.00*I_BACK+(0.01737*)^2 Cycle 5, Chi^2= 1.00003 Current error model SIG(F2)^2 = 92.79*I_RAW + 0.00*I_BACK+(0.01729*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 92.70*I_RAW + 0.00*I_BACK+(0.01731*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 92.70*I_RAW + 0.00*I_BACK+(0.01731*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5692145- 1550154 192 2269707.72 52.65 100.00 1524039- 1013223 192 1229120.25 44.91 100.00 1010655- 315742 192 592630.81 43.01 100.00 314646- 201066 192 243457.65 35.57 100.00 200824- 169841 192 183804.60 28.31 100.00 169528- 127487 192 141088.27 22.51 100.00 127481- 102012 192 115405.74 19.74 100.00 101758- 5880 192 59924.82 14.90 100.00 5871- 3487 192 4426.04 4.70 100.00 3476- 535 197 2695.23 3.85 80.20 ------------------------------------------------------------------------------------ 5692145- 535 1925 482975.38 26.95 97.97 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 192 786426.64 40.56 100.00 1.39- 1.09 192 923769.01 35.93 100.00 1.09- 0.96 192 488519.13 30.27 100.00 0.96- 0.88 192 471622.54 27.40 98.44 0.88- 0.81 192 618440.85 31.44 99.48 0.81- 0.73 192 338812.41 21.64 98.96 0.73- 0.71 192 246289.20 20.00 98.96 0.71- 0.65 192 482062.15 26.62 97.92 0.65- 0.62 192 242709.05 17.72 92.19 0.62- 0.58 197 237495.55 18.18 93.91 ------------------------------------------------------------------------------------ 4.82- 0.58 1925 482975.38 26.95 97.97 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 192 786426.64 40.56 100.00 4.82- 1.09 384 855097.82 38.24 100.00 4.82- 0.96 576 732904.93 35.59 100.00 4.82- 0.88 768 667584.33 33.54 99.61 4.82- 0.81 960 657755.63 33.12 99.58 4.82- 0.73 1152 604598.43 31.21 99.48 4.82- 0.71 1344 553411.40 29.61 99.40 4.82- 0.65 1536 544492.74 29.23 99.22 4.82- 0.62 1728 510961.22 27.95 98.44 4.82- 0.58 1925 482975.38 26.95 97.97 ------------------------------------------------------------------------------------ 4.82- 0.58 1925 482975.38 26.95 97.97 Scale applied to data: s=0.175681 (maximum obs:5692145.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.024: data 1925 -> merged 109 With outlier rejection... Rint 0.028; Rsigma 0.024: data 1912 -> merged 109 Rejected total: 13, method kkm 13, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585862, 4.831144 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 9 10 11.33 90.00 102 1.61 - 1.21 10 10 16.90 100.00 169 1.17 - 1.01 10 10 23.00 100.00 230 0.99 - 0.89 10 10 22.90 100.00 229 0.88 - 0.81 10 10 21.40 100.00 214 0.81 - 0.74 10 10 19.40 100.00 194 0.73 - 0.71 10 10 20.70 100.00 207 0.70 - 0.66 10 10 16.90 100.00 169 0.66 - 0.64 10 10 16.20 100.00 162 0.63 - 0.60 10 10 16.40 100.00 164 --------------------------------------------------------------- 5.91 - 0.60 99 100 18.59 99.00 1840 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:28:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920520 5.917122 5.911526 60.0717 90.0989 60.0000 1743 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.12 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 849 938 843 885 1315 1170 1147 1743 N (int>3sigma) = 0 696 938 690 725 1162 996 970 1473 Mean intensity = 0.0 27.7 14.3 27.8 33.5 22.9 33.4 31.8 32.4 Mean int/sigma = 0.0 24.3 22.5 24.1 26.0 23.6 26.0 25.8 26.1 Lattice type: P chosen Volume: 146.47 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.912 5.917 90.07 119.93 119.92 Niggli form: a.a = 34.946 b.b = 34.954 c.c = 35.012 b.c = -0.044 a.c = -17.452 a.b = -17.434 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.112 CUBIC F-lattice R(int) = 0.204 [ 1589] Vol = 585.9 Cell: 8.370 8.374 8.359 90.09 89.95 90.02 Volume: 585.88 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.110 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 1321] Vol = 439.4 Cell: 5.919 5.912 14.506 90.03 90.04 120.04 Volume: 439.41 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.110 RHOMBOHEDRAL R-lattice R(int) = 0.165 [ 407] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.506 90.03 90.04 120.04 Volume: 439.41 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.069 TETRAGONAL I-lattice R(int) = 0.151 [ 1357] Vol = 292.9 Cell: 5.921 5.919 8.359 89.97 89.90 89.97 Volume: 292.94 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.131 TETRAGONAL I-lattice R(int) = 0.151 [ 1357] Vol = 292.9 Cell: 5.919 5.921 8.359 90.10 90.03 89.97 Volume: 292.94 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.076 ORTHORHOMBIC I-lattice R(int) = 0.139 [ 1307] Vol = 292.9 Cell: 5.919 5.921 8.359 89.90 89.97 89.97 Volume: 292.94 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.073 ORTHORHOMBIC I-lattice R(int) = 0.180 [ 1314] Vol = 292.9 Cell: 5.912 8.370 5.921 89.95 89.90 90.02 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.125 [ 1038] Vol = 292.9 Cell: 5.921 5.919 8.359 90.03 90.10 89.97 Volume: 292.94 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.112 MONOCLINIC I-lattice R(int) = 0.170 [ 1072] Vol = 292.9 Cell: 5.912 5.921 8.370 90.05 90.02 90.10 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.060 MONOCLINIC I-lattice R(int) = 0.124 [ 1036] Vol = 292.9 Cell: 5.912 8.370 5.921 89.95 90.10 89.98 Volume: 292.94 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.045 MONOCLINIC I-lattice R(int) = 0.150 [ 1035] Vol = 292.9 Cell: 5.921 5.912 8.370 89.98 90.05 89.90 Volume: 292.94 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.094 MONOCLINIC C-lattice R(int) = 0.152 [ 1076] Vol = 292.9 Cell: 10.247 5.912 5.917 90.07 125.20 89.92 Volume: 292.94 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.102 [ 701] Vol = 146.5 Cell: 5.912 5.912 5.917 90.07 119.93 119.92 Volume: 146.47 Matrix: 0.0000 0.0000 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 0 938 0 1153 1170 1743 N (int>3sigma) = 0 0 0 0 938 0 974 996 1473 Mean intensity = 0.0 0.0 0.0 0.0 14.3 0.0 31.8 33.4 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.5 0.0 26.1 26.0 26.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 128 409 N I>3s 9 9 60 409 0.5 0.5 0.3 16.6 7.2 7.2 3.6 27.6 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 0.204 1481 Fd-3m 1 1 227 C N N N N 37 2284 0.205 1519 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.369921 8.373740 8.359298 90.0871 89.9525 90.0185 ZERR 1.00 0.003535 0.002161 0.000363 0.0002 0.0137 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5692145- 904762 422 417 27 15.4 1669257.89 47.91 0.026 0.035 900514- 158825 569 565 27 20.9 286469.95 34.83 0.029 0.035 150464- 53382 482 480 27 17.8 113960.09 19.79 0.045 0.059 22680- 1567 452 450 28 16.1 4689.79 4.90 0.147 0.179 ------------------------------------------------------------------------------------------- 5692145- 1567 1925 1912 109 17.5 478424.33 26.86 0.028 0.037 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 465 460 27 17.0 753677.97 37.34 0.028 0.039 0.020 1.01-0.78 607 606 28 21.6 467904.40 26.03 0.022 0.029 0.024 0.76-0.65 485 482 27 17.9 403263.20 24.15 0.031 0.039 0.027 0.65-0.59 368 364 27 13.5 247616.81 18.59 0.037 0.043 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 1925 1912 109 17.5 478424.33 26.86 0.028 0.037 0.024 inf-0.60 1849 1839 99 18.6 490011.99 27.25 0.028 0.037 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 460 27 27 100.0 17.0 753677.97 174.91 0.028 0.007 1.01-0.78 606 28 28 100.0 21.6 467904.40 128.86 0.022 0.005 0.76-0.65 482 27 27 100.0 17.9 403263.20 110.75 0.031 0.008 0.65-0.59 364 28 27 96.4 13.5 247616.81 76.76 0.037 0.011 -------------------------------------------------------------------------------------------- inf-0.59 1912 110 109 99.1 17.5 478424.33 125.45 0.028 0.007 inf-0.60 1839 99 99 100.0 18.6 490011.99 128.22 0.028 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:33:26 2018) ID: 2932; threads 39; handles 876; mem 519816.00 (1237724.00)kB; time: 1w 5d 22h 38m 56s MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.6,peak PF: 708.5, WS: 271.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:509.4,peak PF: 708.5, WS: 273.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:33:26 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000016 0.000019 0.000017 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000018 0.000016 ) 5.91535 ( 0.00088 ) 5.92288 ( 0.00068 ) 5.91286 ( 0.00090 ) 59.95509 ( 0.01389 ) 89.89521 ( 0.01227 ) 59.99590 ( 0.01373 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 13:33:26 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000016 0.000019 0.000017 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000013 0.000012 ) 0.055227 -0.024260 0.122680 ( 0.000016 0.000018 0.000016 ) M - matrix: 0.021551 -0.014380 0.007218 ( 0.000004 0.000003 0.000003 ) -0.014380 0.028726 -0.014370 ( 0.000003 0.000005 0.000003 ) 0.007218 -0.014370 0.021585 ( 0.000003 0.000003 0.000005 ) unit cell: 5.9154(9) 5.9229(7) 5.9129(9) 59.955(14) 89.895(12) 59.996(14) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_4_26.rpb PROFFITPEAK info: 591 peaks in the peak location table UB fit with 275 obs out of 291 (total:291,skipped:0) (94.50%) UB - matrix: -0.104326 -0.015013 0.049036 ( 0.000116 0.000125 0.000043 ) 0.087361 -0.167253 0.063541 ( 0.000185 0.000199 0.000068 ) 0.055195 -0.024254 0.122944 ( 0.000144 0.000155 0.000053 ) M - matrix: 0.021562 -0.014384 0.007221 ( 0.000043 0.000039 0.000023 ) -0.014384 0.028787 -0.014346 ( 0.000039 0.000067 0.000026 ) 0.007221 -0.014346 0.021557 ( 0.000023 0.000026 0.000016 ) unit cell: 5.916(6) 5.901(7) 5.909(6) 60.19(11) 90.21(8) 60.06(12) V = 146.1(3) UB fit with 275 obs out of 291 (total:291,skipped:0) (94.50%) UB - matrix: -0.104326 -0.015013 0.049036 ( 0.000116 0.000125 0.000043 ) 0.087361 -0.167253 0.063541 ( 0.000185 0.000199 0.000068 ) 0.055195 -0.024254 0.122944 ( 0.000144 0.000155 0.000053 ) M - matrix: 0.021562 -0.014384 0.007221 ( 0.000043 0.000039 0.000023 ) -0.014384 0.028787 -0.014346 ( 0.000039 0.000067 0.000026 ) 0.007221 -0.014346 0.021557 ( 0.000023 0.000026 0.000016 ) unit cell: 5.916(6) 5.901(7) 5.909(6) 60.19(11) 90.21(8) 60.06(12) V = 146.1(3) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB fit with 277 obs out of 291 (total:291,skipped:0) (95.19%) UB - matrix: -0.104298 -0.015069 0.049012 ( 0.000124 0.000134 0.000046 ) 0.087300 -0.167239 0.063543 ( 0.000169 0.000183 0.000062 ) 0.055163 -0.024221 0.122949 ( 0.000144 0.000156 0.000053 ) M - matrix: 0.021542 -0.014364 0.007218 ( 0.000042 0.000037 0.000023 ) -0.014364 0.028783 -0.014343 ( 0.000037 0.000062 0.000026 ) 0.007218 -0.014343 0.021556 ( 0.000023 0.000026 0.000016 ) unit cell: 5.916(6) 5.899(6) 5.909(6) 60.19(11) 90.24(8) 60.10(11) V = 146.2(3) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 291 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Run 4 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104299 -0.015069 0.049012 ( 0.000124 0.000134 0.000046 ) 0.087300 -0.167241 0.063543 ( 0.000168 0.000182 0.000062 ) 0.055163 -0.024221 0.122949 ( 0.000144 0.000156 0.000053 ) M - matrix: 0.021542 -0.014365 0.007218 ( 0.000042 0.000036 0.000023 ) -0.014365 0.028783 -0.014344 ( 0.000036 0.000062 0.000026 ) 0.007218 -0.014344 0.021556 ( 0.000023 0.000026 0.000016 ) UB fit with 277 obs out of 291 (total:291,skipped:0) (95.19%) unit cell: 5.916(6) 5.899(6) 5.909(6) 60.19(11) 90.24(8) 60.10(11) V = 146.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 279 obs out of 291 (total:291,skipped:0) (95.88%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_26.rpb 5 of 219 peaks identified as outliers and rejected 214 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 214 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 214 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 1.41 | 21 | 1.048 ( 0.295) | 1.086 ( 0.332) | 1.148 ( 0.615) | 1.40- 1.11 | 21 | 1.083 ( 0.100) | 1.353 ( 0.685) | 0.948 ( 0.412) | 1.11- 1.00 | 21 | 1.082 ( 0.094) | 1.207 ( 0.280) | 1.174 ( 0.536) | 0.98- 0.92 | 21 | 1.129 ( 0.072) | 1.155 ( 0.091) | 1.100 ( 0.410) | 0.91- 0.82 | 21 | 1.133 ( 0.067) | 1.170 ( 0.102) | 1.137 ( 0.342) | 0.82- 0.76 | 21 | 1.154 ( 0.086) | 1.136 ( 0.116) | 1.087 ( 0.348) | 0.76- 0.71 | 21 | 1.164 ( 0.070) | 1.183 ( 0.116) | 1.085 ( 0.331) | 0.71- 0.67 | 21 | 1.157 ( 0.057) | 1.147 ( 0.123) | 1.307 ( 0.442) | 0.67- 0.64 | 21 | 1.213 ( 0.079) | 1.216 ( 0.123) | 1.298 ( 0.418) | 0.64- 0.59 | 25 | 1.234 ( 0.096) | 1.171 ( 0.211) | 1.260 ( 0.489) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 0.59 | 214 | 1.141 ( 0.133) | 1.182 ( 0.286) | 1.156 ( 0.456) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) UB - matrix: -0.104236 -0.015275 0.049380 ( 0.000055 0.000057 0.000020 ) 0.087397 -0.167430 0.063797 ( 0.000068 0.000072 0.000025 ) 0.055054 -0.024318 0.122931 ( 0.000045 0.000048 0.000017 ) M - matrix: 0.021534 -0.014380 0.007196 ( 0.000017 0.000015 0.000008 ) -0.014380 0.028858 -0.014425 ( 0.000015 0.000024 0.000009 ) 0.007196 -0.014425 0.021620 ( 0.000008 0.000009 0.000006 ) unit cell: 5.917(3) 5.903(2) 5.9089(18) 59.99(4) 90.03(3) 60.05(5) V = 145.99(10) OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 UB - matrix: -0.104310 -0.015098 0.049144 ( 0.000050 0.000052 0.000018 ) 0.087097 -0.167072 0.063696 ( 0.000062 0.000065 0.000023 ) 0.054952 -0.024053 0.122724 ( 0.000040 0.000042 0.000015 ) M - matrix: 0.021486 -0.014298 0.007165 ( 0.000016 0.000013 0.000007 ) -0.014298 0.028720 -0.014336 ( 0.000013 0.000022 0.000008 ) 0.007165 -0.014336 0.021533 ( 0.000007 0.000008 0.000005 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.918(2) 5.906(2) 5.9155(16) 60.07(3) 90.11(3) 60.14(4) V = 146.51(9) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104310 -0.015098 0.049144 ( 0.000050 0.000052 0.000018 ) 0.087097 -0.167072 0.063696 ( 0.000062 0.000065 0.000023 ) 0.054952 -0.024053 0.122724 ( 0.000040 0.000042 0.000015 ) M - matrix: 0.021486 -0.014298 0.007165 ( 0.000016 0.000013 0.000007 ) -0.014298 0.028720 -0.014336 ( 0.000013 0.000022 0.000008 ) 0.007165 -0.014336 0.021533 ( 0.000007 0.000008 0.000005 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.918(2) 5.906(2) 5.9155(16) 60.07(3) 90.11(3) 60.14(4) V = 146.51(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_26.rpb 5 of 215 peaks identified as outliers and rejected 210 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 210 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 210 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.41 | 21 | 1.068 ( 0.293) | 1.180 ( 0.566) | 1.191 ( 0.582) | 1.41- 1.12 | 21 | 1.063 ( 0.080) | 1.214 ( 0.462) | 0.998 ( 0.487) | 1.12- 0.98 | 21 | 1.082 ( 0.089) | 1.134 ( 0.113) | 1.076 ( 0.362) | 0.98- 0.89 | 21 | 1.122 ( 0.069) | 1.153 ( 0.090) | 1.151 ( 0.501) | 0.89- 0.82 | 21 | 1.142 ( 0.070) | 1.171 ( 0.112) | 1.109 ( 0.353) | 0.82- 0.75 | 21 | 1.152 ( 0.087) | 1.152 ( 0.185) | 1.061 ( 0.344) | 0.75- 0.71 | 21 | 1.168 ( 0.066) | 1.206 ( 0.118) | 1.211 ( 0.400) | 0.71- 0.67 | 21 | 1.161 ( 0.058) | 1.154 ( 0.122) | 1.290 ( 0.464) | 0.67- 0.64 | 21 | 1.211 ( 0.081) | 1.227 ( 0.138) | 1.320 ( 0.440) | 0.63- 0.59 | 21 | 1.236 ( 0.097) | 1.150 ( 0.201) | 1.221 ( 0.456) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.59 | 210 | 1.140 ( 0.131) | 1.174 ( 0.264) | 1.163 ( 0.455) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 155 | 1.156 ( 0.140) | 1.257 ( 0.390) | 1.382 ( 0.719) | 13.2-19.0 | 155 | 1.146 ( 0.116) | 1.193 ( 0.271) | 1.335 ( 0.697) | 19.0-23.1 | 155 | 1.153 ( 0.096) | 1.220 ( 0.328) | 1.245 ( 0.633) | 23.2-27.4 | 155 | 1.141 ( 0.096) | 1.189 ( 0.356) | 1.212 ( 0.517) | 27.4-30.6 | 155 | 1.142 ( 0.107) | 1.171 ( 0.192) | 1.206 ( 0.455) | 30.6-34.0 | 155 | 1.155 ( 0.088) | 1.154 ( 0.215) | 1.229 ( 0.441) | 34.0-37.3 | 155 | 1.139 ( 0.111) | 1.116 ( 0.169) | 1.137 ( 0.403) | 37.3-39.9 | 155 | 1.158 ( 0.117) | 1.140 ( 0.249) | 1.272 ( 0.543) | 39.9-43.0 | 155 | 1.172 ( 0.123) | 1.111 ( 0.197) | 1.251 ( 0.584) | 43.0-49.8 | 152 | 1.200 ( 0.169) | 1.125 ( 0.246) | 1.169 ( 0.474) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1547 | 1.156 ( 0.120) | 1.168 ( 0.275) | 1.244 ( 0.561) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.96 e2 dimension: a=-0.0014 b=1.03 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6354 lp-corr: 4295 Maximum peak integral for reflections I/sig<= 100 - raw: 458459 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 27221198 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:33:41 2018 PROFFITMAIN - Started at Wed Mar 28 13:33:41 2018 OTKP changes: 1547 2 3 4 OTKP changes: 1547 2 3 4 UB - matrix: -0.104260 -0.014981 0.049484 ( 0.000015 0.000017 0.000015 ) 0.087387 -0.167241 0.063725 ( 0.000011 0.000012 0.000010 ) 0.055395 -0.024364 0.122933 ( 0.000016 0.000017 0.000015 ) M - matrix: 0.021575 -0.014402 0.007219 ( 0.000004 0.000003 0.000003 ) -0.014402 0.028787 -0.014394 ( 0.000003 0.000004 0.000003 ) 0.007219 -0.014394 0.021622 ( 0.000003 0.000003 0.000004 ) UB fit with 1547 obs out of 1547 (total:1547,skipped:0) (100.00%) unit cell: 5.9171(8) 5.9108(6) 5.9057(8) 60.070(13) 90.072(11) 59.987(13) V = 146.09(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104106 -0.015206 0.049820 ( 0.000025 0.000032 0.000028 ) 0.087324 -0.167076 0.063636 ( 0.000017 0.000022 0.000019 ) 0.055389 -0.024087 0.122512 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021531 -0.014341 0.007156 ( 0.000006 0.000005 0.000005 ) -0.014341 0.028726 -0.014341 ( 0.000005 0.000007 0.000005 ) 0.007156 -0.014341 0.021541 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9166(14) 5.9128(10) 5.9146(13) 60.03(2) 89.988(18) 60.02(2) V = 146.45(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104060 -0.015209 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087421 -0.167151 0.063728 ( 0.000017 0.000021 0.000019 ) 0.055453 -0.024158 0.122547 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021546 -0.014370 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014370 0.028754 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9180(13) 5.9144(10) 5.9152(13) 60.02(2) 90.008(18) 60.00(2) V = 146.43(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104060 -0.015209 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087421 -0.167151 0.063728 ( 0.000017 0.000021 0.000019 ) 0.055453 -0.024158 0.122547 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021546 -0.014370 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014370 0.028754 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9180(13) 5.9144(10) 5.9152(13) 60.02(2) 90.008(18) 60.00(2) V = 146.43(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104060 -0.015209 0.049813 ( 0.000024 0.000031 0.000027 ) 0.087421 -0.167151 0.063728 ( 0.000017 0.000021 0.000019 ) 0.055453 -0.024158 0.122547 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021546 -0.014370 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014370 0.028754 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9180(13) 5.9144(10) 5.9152(13) 60.02(2) 90.008(18) 60.00(2) V = 146.43(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104489 -0.014350 0.049145 ( 0.000035 0.000044 0.000039 ) 0.087143 -0.167087 0.063759 ( 0.000025 0.000032 0.000027 ) 0.055259 -0.024933 0.122931 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021566 -0.014439 0.007214 ( 0.000009 0.000007 0.000006 ) -0.014439 0.028746 -0.014424 ( 0.000007 0.000011 0.000007 ) 0.007214 -0.014424 0.021592 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9288(19) 5.9357(14) 5.9201(16) 59.90(3) 89.88(2) 59.82(3) V = 146.84(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104461 -0.014605 0.048932 ( 0.000028 0.000035 0.000030 ) 0.087175 -0.167128 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055343 -0.024835 0.123226 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007256 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028762 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014411 0.021629 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9218(15) 5.9187(13) 5.9091(15) 60.06(2) 90.13(2) 59.97(2) V = 146.35(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104461 -0.014605 0.048932 ( 0.000028 0.000035 0.000030 ) 0.087175 -0.167128 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055343 -0.024835 0.123226 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007256 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028762 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014411 0.021629 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9218(15) 5.9187(13) 5.9091(15) 60.06(2) 90.13(2) 59.97(2) V = 146.35(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146807 -0.097928 0.049162 ( 0.000021 0.000026 0.000023 ) -0.000020 0.138453 -0.069290 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000033 0.119951 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021552 -0.014379 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028759 -0.014404 ( 0.000005 0.000009 0.000006 ) 0.007216 -0.014404 0.021606 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9185(10) 5.9162(14) 5.9124(14) 60.00(2) 90.057(17) 60.02(2) V = 146.36(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 210 obs out of 210 (total:210,skipped:0) (100.00%) UB - matrix: -0.104275 -0.015130 0.049253 ( 0.000046 0.000048 0.000017 ) 0.087277 -0.167322 0.063726 ( 0.000064 0.000068 0.000023 ) 0.055092 -0.024356 0.122957 ( 0.000053 0.000056 0.000019 ) M - matrix: 0.021526 -0.014368 0.007200 ( 0.000016 0.000014 0.000008 ) -0.014368 0.028819 -0.014403 ( 0.000014 0.000023 0.000009 ) 0.007200 -0.014403 0.021605 ( 0.000008 0.000009 0.000006 ) unit cell: 5.919(2) 5.904(2) 5.909(2) 60.03(4) 90.08(3) 60.06(4) V = 146.13(10) OTKP changes: 210 1 1 1 OTKP changes: 210 1 1 1 OTKP changes: 210 1 1 1 UB - matrix: -0.104316 -0.015181 0.049263 ( 0.000046 0.000049 0.000017 ) 0.087181 -0.167215 0.063705 ( 0.000061 0.000065 0.000023 ) 0.055029 -0.024096 0.122765 ( 0.000047 0.000050 0.000017 ) M - matrix: 0.021511 -0.014320 0.007171 ( 0.000015 0.000013 0.000008 ) -0.014320 0.028772 -0.014358 ( 0.000013 0.000022 0.000009 ) 0.007171 -0.014358 0.021556 ( 0.000008 0.000009 0.000005 ) UB fit with 210 obs out of 210 (total:210,skipped:0) (100.00%) unit cell: 5.914(2) 5.902(2) 5.9127(19) 60.06(4) 90.10(3) 60.14(4) V = 146.23(9) Run 4 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) HKL list info: 422 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104316 -0.015181 0.049263 ( 0.000046 0.000049 0.000017 ) 0.087181 -0.167215 0.063705 ( 0.000061 0.000065 0.000023 ) 0.055029 -0.024096 0.122765 ( 0.000047 0.000050 0.000017 ) M - matrix: 0.021511 -0.014320 0.007171 ( 0.000015 0.000013 0.000008 ) -0.014320 0.028772 -0.014358 ( 0.000013 0.000022 0.000009 ) 0.007171 -0.014358 0.021556 ( 0.000008 0.000009 0.000005 ) UB fit with 210 obs out of 210 (total:210,skipped:0) (100.00%) unit cell: 5.914(2) 5.902(2) 5.9127(19) 60.06(4) 90.10(3) 60.14(4) V = 146.23(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 210 obs out of 210 (total:210,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! 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: -0.104316 -0.015181 0.049263 ( 0.000046 0.000049 0.000017 ) 0.087181 -0.167215 0.063705 ( 0.000061 0.000065 0.000023 ) 0.055029 -0.024096 0.122765 ( 0.000047 0.000050 0.000017 ) M - matrix: 0.021511 -0.014320 0.007171 ( 0.000015 0.000013 0.000008 ) -0.014320 0.028772 -0.014358 ( 0.000013 0.000022 0.000009 ) 0.007171 -0.014358 0.021556 ( 0.000008 0.000009 0.000005 ) UB fit with 210 obs out of 210 (total:210,skipped:0) (100.00%) unit cell: 5.914(2) 5.902(2) 5.9127(19) 60.06(4) 90.10(3) 60.14(4) V = 146.23(9) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104225 -0.014943 0.049378 ( 0.000015 0.000017 0.000015 ) 0.087313 -0.167081 0.063690 ( 0.000011 0.000012 0.000011 ) 0.055369 -0.024360 0.122825 ( 0.000015 0.000016 0.000014 ) M - matrix: 0.021552 -0.014380 0.007215 ( 0.000004 0.000003 0.000003 ) -0.014380 0.028733 -0.014371 ( 0.000003 0.000004 0.000003 ) 0.007215 -0.014371 0.021580 ( 0.000003 0.000003 0.000004 ) UB fit with 1547 obs out of 1547 (total:1547,skipped:0) (100.00%) unit cell: 5.9200(8) 5.9165(6) 5.9124(8) 60.064(13) 90.091(11) 60.002(13) V = 146.46(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 37 reflections under beam stop or inside a detector rejection region 16 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof 2074 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:33:45 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) Run 4 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) PROFFIT INFO: signal sum: min=162.0000 max=22164944.0000 PROFFIT INFO: signal sum lp corr: min=241.7914 max=2358045.1195 PROFFIT INFO: background sum: min=762.0000 max=15918.0000 PROFFIT INFO: background sum sig2: min=602.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=60 max=886 PROFFIT INFO: Inet: min=527.5448 max=5144825.5000 PROFFIT INFO: sig(Inet): min=190.6887 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 45 154 273 431 471 822 1370 1872 2073 Percent 0.0 0.1 2.2 7.4 13.2 20.8 22.7 39.7 66.1 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2074 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 2074 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5144826- 1608612 207 2415872.46 134.03 100.00 1608361- 1023524 207 1300143.94 109.64 100.00 1019977- 324827 207 598935.03 93.73 100.00 324428- 220661 207 259849.03 70.72 100.00 220537- 165418 207 190306.49 48.57 100.00 165394- 132128 207 149376.66 36.50 100.00 132045- 99394 207 116396.17 30.93 100.00 99140- 6329 207 56364.40 20.77 100.00 6302- 3646 207 4687.45 4.83 83.09 3645- 528 210 2674.53 3.13 43.33 ------------------------------------------------------------------------------------ 5144826- 528 2073 508727.21 55.21 92.57 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 207 779014.50 85.01 100.00 1.28- 0.98 207 706140.53 69.23 97.58 0.98- 0.85 207 681838.33 66.81 96.62 0.85- 0.78 207 540218.87 65.22 96.62 0.78- 0.70 207 437905.92 50.38 93.72 0.70- 0.63 207 446380.42 51.05 91.79 0.63- 0.58 207 452551.74 49.57 88.89 0.58- 0.54 207 362134.16 41.04 91.79 0.54- 0.49 207 314641.44 35.57 81.16 0.49- 0.40 210 368478.73 38.46 87.62 ------------------------------------------------------------------------------------ 5.26- 0.40 2073 508727.21 55.21 92.57 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:33:45 2018 Sorting 2073 observations 278 unique observations with > 7.00 F2/sig(F2) 2073 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 49 364 Total number of frames 364 Maximum number of 278 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2073 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 24 184 Total number of frames 184 1666 observations > 7.00 F2/sig(F2) 1666 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 24 184 Total number of frames 184 Removing 'redundancy=1' reflections Average redundancy: 6.0 (Out of 1666 removed 29 = 1637, unique = 275) 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 1637 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 24 184 Total number of frames 184 275 unique data precomputed (should be 275) 275 unique data with 1637 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.0 (Out of 1637 removed 0 = 1637, unique = 275) 275 unique data precomputed (should be 275) 275 unique data with 1637 observations RMS deviation of equivalent data = 0.71181 Rint = 0.66668 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.64807, wR= 2.59739 Trying model 1 (ne=2, no=0)... Results: Rint= 0.70280, wR= 2.08017, Acormin=-0.326, Acormax=2.448, Acor_av=0.630 F test: Probability=0.000, F= 0.847 Trying model 2 (ne=2, no=1)... Results: Rint= 0.76966, wR= 1.96678, Acormin=-0.216, Acormax=2.192, Acor_av=0.437 F test: Probability=0.000, F= 0.705 Trying model 3 (ne=4, no=0)... Results: Rint= 0.72424, wR= 1.80878, Acormin=-0.265, Acormax=2.698, Acor_av=0.560 F test: Probability=0.000, F= 0.792 Trying model 4 (ne=4, no=1)... Results: Rint= 0.80541, wR= 1.85887, Acormin=-0.258, Acormax=1.760, Acor_av=0.406 F test: Probability=0.000, F= 0.639 Trying model 5 (ne=4, no=3)... Results: Rint= 0.93576, wR= 1.56582, Acormin=-0.579, Acormax=3.097, Acor_av=0.120 F test: Probability=0.000, F= 0.471 Trying model 6 (ne=6, no=0)... Results: Rint= 0.71293, wR= 1.84510, Acormin=-0.421, Acormax=2.951, Acor_av=0.514 F test: Probability=0.000, F= 0.810 Trying model 7 (ne=6, no=1)... Results: Rint= 0.80550, wR= 1.76877, Acormin=-0.425, Acormax=2.273, Acor_av=0.364 F test: Probability=0.000, F= 0.633 Trying model 8 (ne=6, no=3)... Results: Rint= 0.92631, wR= 1.50736, Acormin=-0.672, Acormax=3.052, Acor_av=0.114 F test: Probability=0.000, F= 0.476 Trying model 9 (ne=6, no=5)... Results: Rint= 0.98098, wR= 1.40206, Acormin=-0.388, Acormax=2.501, Acor_av=0.054 F test: Probability=0.000, F= 0.421 Trying model 10 (ne=8, no=0)... Results: Rint= 0.81317, wR= 1.65135, Acormin=-0.710, Acormax=1.669, Acor_av=0.282 F test: Probability=0.000, F= 0.615 Trying model 11 (ne=8, no=1)... Results: Rint= 0.84616, wR= 1.87490, Acormin=-0.502, Acormax=1.292, Acor_av=0.194 F test: Probability=0.000, F= 0.566 Trying model 12 (ne=8, no=3)... Results: Rint= 0.96663, wR= 2.03791, Acormin=-0.062, Acormax=0.069, Acor_av=0.002 F test: Probability=0.000, F= 0.432 Trying model 13 (ne=8, no=5)... Results: Rint= 0.97743, wR= 1.91969, Acormin=-0.062, Acormax=0.059, Acor_av=0.001 F test: Probability=0.000, F= 0.419 Trying model 14 (ne=8, no=7)... Results: Rint= 0.96091, wR= 1.60814, Acormin=-0.105, Acormax=0.101, Acor_av=0.001 F test: Probability=0.000, F= 0.428 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: 0.84632 There are 184 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: 2, max odd order: 0 (5 parameters) Refinement control: 188 pars with 17766 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71181 Using Levenberg-Marquardt: 0.00010 New wR= 0.69105 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66668 with corrections 0.64641 Rint for all data: 0.84632 with corrections 0.83690 8 observations identified as outliers and rejected Cycle 2 wR= 0.64227 Using Levenberg-Marquardt: 0.00001 New wR= 0.63917 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64807 with corrections 0.62568 Rint for all data: 0.84632 with corrections 0.83661 9 observations identified as outliers and rejected Cycle 3 wR= 0.62057 Using Levenberg-Marquardt: 0.00000 New wR= 0.61645 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63762 with corrections 0.62879 Rint for all data: 0.84632 with corrections 0.84235 8 observations identified as outliers and rejected Cycle 4 wR= 0.60577 Using Levenberg-Marquardt: 0.00000 New wR= 0.60257 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62816 with corrections 0.63141 Rint for all data: 0.84632 with corrections 0.84498 3 observations identified as outliers and rejected Cycle 5 wR= 0.59824 Using Levenberg-Marquardt: 0.00000 New wR= 0.59683 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62134 with corrections 0.64392 Rint for all data: 0.84632 with corrections 0.85284 1 observations identified as outliers and rejected Final wR= 0.59683 Final frame scales: Min= 1.0000 Max= 8.4753 Final absorption correction factors: Amin= 0.4275 Amax= 1.6232 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 184 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: 2, max odd order: 0 (5 parameters) Refinement control: 188 pars with 17766 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.87793 Using Levenberg-Marquardt: 0.00010 New wR= 0.74437 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62101 with corrections 1.22853 Rint for all data: 0.84632 with corrections 1.31990 1 observations identified as outliers and rejected Cycle 2 wR= 0.74431 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= 0.65300 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62080 with corrections 1.20651 Rint for all data: 0.84632 with corrections 1.32464 0 observations identified as outliers and rejected Cycle 3 wR= 0.65300 Using Levenberg-Marquardt: 0.01000 New wR= 0.60160 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62080 with corrections 0.73008 Rint for all data: 0.84632 with corrections 0.91051 0 observations identified as outliers and rejected Cycle 4 wR= 0.60160 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.60415 Using Levenberg-Marquardt: 0.10000 New wR= 0.59286 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62080 with corrections 0.66789 Rint for all data: 0.84632 with corrections 0.86887 0 observations identified as outliers and rejected Cycle 5 wR= 0.59286 Using Levenberg-Marquardt: 0.01000 New wR= 0.58971 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62080 with corrections 0.66813 Rint for all data: 0.84632 with corrections 0.87052 0 observations identified as outliers and rejected Final wR= 0.58971 Final frame scales: Min= 1.0000 Max= 15.8542 Final absorption correction factors: Amin= 0.2426 Amax= 1.5746 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 19 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: 2, max odd order: 0 (5 parameters) Refinement control: 23 pars with 276 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.90422 Using Levenberg-Marquardt: 0.00010 New wR= 0.70630 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.62080 with corrections 1.10449 Rint for all data: 0.84632 with corrections 1.20358 3 observations identified as outliers and rejected Cycle 2 wR= 0.75751 Using Levenberg-Marquardt: 0.00001 New wR= 0.86672 Using Levenberg-Marquardt: 0.00010 New wR= 0.85834 Using Levenberg-Marquardt: 0.00100 New wR= 0.77610 Using Levenberg-Marquardt: 0.01000 New wR= 0.72045 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.62041 with corrections 1.23558 Rint for all data: 0.84632 with corrections 1.31817 2 observations identified as outliers and rejected Cycle 3 wR= 0.73393 Using Levenberg-Marquardt: 0.00100 New wR= 0.70401 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61961 with corrections 1.25758 Rint for all data: 0.84632 with corrections 1.30124 1 observations identified as outliers and rejected Cycle 4 wR= 0.69931 Using Levenberg-Marquardt: 0.00010 New wR= 0.69079 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61852 with corrections 0.78044 Rint for all data: 0.84632 with corrections 0.90415 2 observations identified as outliers and rejected Cycle 5 wR= 0.67947 Using Levenberg-Marquardt: 0.00001 New wR= 0.66609 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61680 with corrections 0.93621 Rint for all data: 0.84632 with corrections 0.97420 2 observations identified as outliers and rejected Final wR= 0.66609 Final frame scales: Min= 1.0000 Max= 2.0907 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 19 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 18 pars with 171 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.62479 Using Levenberg-Marquardt: 0.00010 New wR= 0.63320 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61633 with corrections 0.68926 Rint for all data: 0.84632 with corrections 0.88086 3 observations identified as outliers and rejected Cycle 2 wR= 0.61676 Using Levenberg-Marquardt: 0.00001 New wR= 0.61453 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61438 with corrections 0.64653 Rint for all data: 0.84632 with corrections 0.85975 0 observations identified as outliers and rejected Cycle 3 wR= 0.59953 Using Levenberg-Marquardt: 0.00000 New wR= 0.59833 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61438 with corrections 0.62149 Rint for all data: 0.84632 with corrections 0.84930 1 observations identified as outliers and rejected Cycle 4 wR= 0.58847 Using Levenberg-Marquardt: 0.00000 New wR= 0.58755 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61421 with corrections 0.60888 Rint for all data: 0.84632 with corrections 0.84449 1 observations identified as outliers and rejected Cycle 5 wR= 0.57634 Using Levenberg-Marquardt: 0.00000 New wR= 0.57567 There are 6 clusters with unrefined scales (size 2-53) Rint for refined data: 0.61389 with corrections 0.60220 Rint for all data: 0.84632 with corrections 0.84215 0 observations identified as outliers and rejected Final wR= 0.57567 Final frame scales: Min= 0.9052 Max= 1.5868 PROFFIT INFO: Inet (after scale3 abspack): min=452.2856 max=4803753.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=224.3274 max=62604.6328 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2073 reflections read from tmp file 1573 reflections are rejected (1498 as outliers, 75 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 89 52 23 6 3 0 2 0 1 Initial Chi^2= 0.63099 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88553 Current error model SIG(F2)^2 = 222.21*I_RAW + 0.00*I_BACK+(0.02589*)^2 Cycle 2, Chi^2= 1.00119 Current error model SIG(F2)^2 = 221.45*I_RAW + 0.00*I_BACK+(0.01573*)^2 Cycle 3, Chi^2= 1.00087 Current error model SIG(F2)^2 = 228.38*I_RAW + 0.00*I_BACK+(0.01299*)^2 Cycle 4, Chi^2= 1.00027 Current error model SIG(F2)^2 = 230.31*I_RAW + 0.00*I_BACK+(0.01223*)^2 Cycle 5, Chi^2= 1.00006 Current error model SIG(F2)^2 = 230.76*I_RAW + 0.00*I_BACK+(0.01206*)^2 Cycle 6, Chi^2= 1.00001 Current error model SIG(F2)^2 = 230.85*I_RAW + 0.00*I_BACK+(0.01202*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 230.85*I_RAW + 0.00*I_BACK+(0.01202*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4803754- 1610350 207 2351687.97 87.21 100.00 1608375- 1021124 207 1292487.96 45.24 100.00 1015902- 313138 207 603677.05 43.40 100.00 312884- 214622 207 254228.87 29.84 100.00 214589- 164335 207 186425.59 20.55 100.00 164309- 132352 207 147613.34 16.00 100.00 132252- 100466 207 118150.58 13.26 100.00 100339- 6054 207 57570.15 9.43 97.58 6027- 3585 207 4572.64 2.99 35.27 3583- 452 210 2699.01 2.37 13.81 ------------------------------------------------------------------------------------ 4803754- 452 2073 501188.87 26.99 84.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 207 782683.56 54.14 97.10 1.28- 0.98 207 703644.14 38.21 91.79 0.98- 0.85 207 680213.95 34.68 88.89 0.85- 0.78 207 536169.76 27.43 88.89 0.78- 0.70 207 437854.83 22.47 84.54 0.70- 0.63 207 435516.20 22.20 78.74 0.63- 0.58 207 445606.05 21.01 82.61 0.58- 0.54 207 350728.23 17.98 82.13 0.54- 0.49 207 299852.67 15.50 73.43 0.49- 0.40 210 341927.41 16.46 77.62 ------------------------------------------------------------------------------------ 5.26- 0.40 2073 501188.87 26.99 84.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 207 782683.56 54.14 97.10 5.26- 0.98 414 743163.85 46.17 94.44 5.26- 0.85 621 722180.55 42.34 92.59 5.26- 0.78 828 675677.85 38.62 91.67 5.26- 0.70 1035 628113.25 35.39 90.24 5.26- 0.63 1242 596013.74 33.19 88.33 5.26- 0.58 1449 574526.93 31.45 87.51 5.26- 0.54 1656 546552.09 29.76 86.84 5.26- 0.49 1863 519141.04 28.18 85.35 5.26- 0.40 2073 501188.87 26.99 84.56 ------------------------------------------------------------------------------------ 5.26- 0.40 2073 501188.87 26.99 84.56 Scale applied to data: s=0.208170 (maximum obs:4803753.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.842; Rsigma 0.024: data 2073 -> merged 317 With outlier rejection... Rint 0.781; Rsigma 0.024: data 1944 -> merged 317 Rejected total: 129, method kkm 118, method Blessing 11 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404281, 5.271182 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 8.20 100.00 123 1.46 - 1.12 15 15 11.07 100.00 166 1.08 - 0.96 15 15 10.33 100.00 155 0.96 - 0.86 15 15 11.20 100.00 168 0.86 - 0.79 15 15 9.47 100.00 142 0.79 - 0.73 15 15 8.27 100.00 124 0.73 - 0.69 15 15 7.67 100.00 115 0.69 - 0.65 15 15 8.60 100.00 129 0.65 - 0.63 15 15 5.27 100.00 79 0.63 - 0.60 21 21 6.19 100.00 130 --------------------------------------------------------------- 5.91 - 0.60 156 156 8.53 100.00 1331 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:33:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919979 5.916472 5.912397 60.0644 90.0913 60.0024 1944 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 958 1024 952 968 1467 1301 1294 1944 N (int>3sigma) = 0 787 1024 781 796 1296 1111 1095 1647 Mean intensity = 0.0 9.1 4.0 9.2 9.9 7.4 10.1 10.0 10.1 Mean int/sigma = 0.0 25.6 22.2 25.6 26.4 24.4 26.4 26.5 26.7 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.913 5.916 90.06 119.94 119.93 Niggli form: a.a = 34.956 b.b = 34.960 c.c = 35.005 b.c = -0.037 a.c = -17.456 a.b = -17.444 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.097 CUBIC F-lattice R(int) = 0.127 [ 1789] Vol = 585.8 Cell: 8.369 8.373 8.360 90.07 89.96 90.02 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.121 [ 1517] Vol = 439.4 Cell: 5.918 5.913 14.504 90.03 90.04 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.118 [ 476] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.504 90.03 90.04 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.051 TETRAGONAL I-lattice R(int) = 0.116 [ 1552] Vol = 292.9 Cell: 5.920 5.918 8.360 89.97 89.92 89.97 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.110 TETRAGONAL I-lattice R(int) = 0.116 [ 1552] Vol = 292.9 Cell: 5.918 5.920 8.360 90.08 90.03 89.97 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.059 ORTHORHOMBIC I-lattice R(int) = 0.103 [ 1500] Vol = 292.9 Cell: 5.918 5.920 8.360 89.92 89.97 89.97 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.118 [ 1506] Vol = 292.9 Cell: 5.912 8.369 5.920 89.96 89.91 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.102 [ 1197] Vol = 292.9 Cell: 5.920 5.918 8.360 90.03 90.08 89.97 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.099 MONOCLINIC I-lattice R(int) = 0.106 [ 1210] Vol = 292.9 Cell: 5.912 5.920 8.369 90.04 90.01 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.046 MONOCLINIC I-lattice R(int) = 0.106 [ 1218] Vol = 292.9 Cell: 5.912 8.369 5.920 89.96 90.09 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.112 [ 1220] Vol = 292.9 Cell: 8.369 5.912 5.920 90.09 90.04 90.01 Volume: 292.92 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.078 MONOCLINIC C-lattice R(int) = 0.099 [ 1232] Vol = 292.9 Cell: 10.247 5.913 5.916 90.06 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.093 [ 800] Vol = 146.5 Cell: 5.912 5.913 5.916 90.06 119.94 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 1024 0 1297 1301 1944 N (int>3sigma) = 0 0 0 0 1024 0 1102 1111 1647 Mean intensity = 0.0 0.0 0.0 0.0 4.0 0.0 10.2 10.1 10.1 Mean int/sigma = 0.0 0.0 0.0 0.0 22.2 0.0 27.1 26.4 26.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 138 450 N I>3s 10 10 64 450 0.1 0.1 0.1 4.6 7.4 7.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.127 1671 Fd-3m 1 1 227 C N N N N 37 2284 0.127 1709 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368936 8.373419 8.360086 90.0734 89.9638 90.0169 ZERR 1.00 0.003237 0.001955 0.000332 0.0000 0.0125 0.0001 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3933537- 996027 193 176 31 5.7 1521883.58 56.39 0.479 0.349 966204- 725449 253 242 31 7.8 848562.75 39.32 0.937 0.864 720247- 594482 240 233 31 7.5 644717.17 34.04 0.959 0.929 591333- 464413 255 248 31 8.0 514925.42 26.43 1.050 1.073 462464- 350754 241 221 31 7.1 346541.52 25.70 0.917 1.002 346721- 247386 239 206 31 6.6 213441.80 19.96 0.643 0.686 243903- 140364 196 187 31 6.0 168814.96 18.36 0.549 0.459 140016- 109194 164 155 31 5.0 127438.79 14.86 0.412 0.316 106944- 77975 158 149 31 4.8 94321.66 10.94 0.539 0.416 75891- 2050 134 127 38 3.3 49708.45 6.81 0.699 0.644 ------------------------------------------------------------------------------------------- 3933537- 2050 2073 1944 317 6.1 485271.24 26.72 0.781 0.694 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 331 307 31 9.9 760373.56 49.61 0.764 0.676 0.014 1.05-0.83 333 321 31 10.4 613795.05 32.71 0.892 0.895 0.020 0.83-0.72 277 265 31 8.5 515815.72 25.52 0.778 0.807 0.024 0.72-0.65 258 248 31 8.0 402471.97 21.73 0.868 0.952 0.028 0.65-0.60 206 190 32 5.9 443335.53 21.14 0.786 0.828 0.029 0.60-0.56 191 176 31 5.7 312833.74 16.99 0.751 0.718 0.036 0.56-0.52 152 140 32 4.4 389111.83 19.19 0.801 0.726 0.033 0.52-0.49 128 115 31 3.7 250674.17 13.74 0.589 0.391 0.039 0.49-0.46 111 102 32 3.2 310871.81 15.95 0.483 0.354 0.039 0.46-0.40 86 80 35 2.3 276194.88 14.59 0.197 0.157 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 2073 1944 317 6.1 485271.24 26.72 0.781 0.694 0.024 inf-0.60 1405 1331 156 8.5 564388.32 31.48 0.817 0.807 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 307 31 31 100.0 9.9 760373.56 192.66 0.764 0.006 1.05-0.83 321 31 31 100.0 10.4 613795.05 136.97 0.892 0.008 0.83-0.72 265 31 31 100.0 8.5 515815.72 97.89 0.778 0.011 0.72-0.65 248 31 31 100.0 8.0 402471.97 82.44 0.868 0.012 0.65-0.60 190 32 32 100.0 5.9 443335.53 72.88 0.786 0.016 0.60-0.56 176 36 31 86.1 5.7 312833.74 51.65 0.751 0.019 0.56-0.52 140 35 32 91.4 4.4 389111.83 51.34 0.801 0.019 0.52-0.49 115 43 31 72.1 3.7 250674.17 34.39 0.589 0.022 0.49-0.46 102 56 32 57.1 3.2 310871.81 33.70 0.483 0.024 0.46-0.40 80 135 35 25.9 2.3 276194.88 24.95 0.197 0.029 -------------------------------------------------------------------------------------------- inf-0.40 1944 464 317 68.3 6.1 485271.24 97.23 0.781 0.014 inf-0.60 1331 156 156 100.0 8.5 564388.32 122.72 0.817 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007472 0.076799 -0.034894 ( 0.000008 0.000007 0.000007 ) -0.083539 -0.011812 -0.008040 ( 0.000006 0.000005 0.000005 ) -0.012181 0.033727 0.076918 ( 0.000008 0.000007 0.000007 ) M - matrix: 0.007183 0.000002 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007175 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000005 0.000009 0.007199 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007472 0.076799 -0.034894 ( 0.000008 0.000007 0.000007 ) -0.083539 -0.011812 -0.008040 ( 0.000006 0.000005 0.000005 ) -0.012181 0.033727 0.076918 ( 0.000008 0.000007 0.000007 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3691(6) 8.3736(7) 8.3600(7) 90.075(7) 89.964(7) 90.016(7) V = 585.87(8) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.87(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) Run 4 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) PROFFIT INFO: signal sum: min=162.0000 max=22164944.0000 PROFFIT INFO: signal sum lp corr: min=241.7914 max=2358045.1195 PROFFIT INFO: background sum: min=762.0000 max=15918.0000 PROFFIT INFO: background sum sig2: min=602.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=60 max=886 PROFFIT INFO: Inet: min=527.5448 max=5144825.5000 PROFFIT INFO: sig(Inet): min=190.6887 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=252.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 90 308 546 862 942 1644 2740 3744 4146 Percent 0.0 0.1 2.2 7.4 13.2 20.8 22.7 39.7 66.1 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2074 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 2074 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5144826- 1608612 207 2415872.46 134.03 100.00 1608361- 1023524 207 1300143.94 109.64 100.00 1019977- 324827 207 598935.03 93.73 100.00 324428- 220661 207 259849.03 70.72 100.00 220537- 165418 207 190306.49 48.57 100.00 165394- 132128 207 149376.66 36.50 100.00 132045- 99394 207 116396.17 30.93 100.00 99140- 6329 207 56364.40 20.77 100.00 6302- 3646 207 4687.45 4.83 83.09 3645- 528 210 2674.53 3.13 43.33 ------------------------------------------------------------------------------------ 5144826- 528 2073 508727.21 55.21 92.57 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 207 786132.27 87.23 100.00 1.39- 1.12 207 975141.87 77.70 98.07 1.09- 0.96 207 514152.93 68.07 98.55 0.96- 0.88 207 489739.62 59.43 96.14 0.88- 0.81 207 658836.17 69.71 97.58 0.81- 0.73 207 356936.13 41.86 93.72 0.73- 0.71 207 262034.37 34.95 89.86 0.71- 0.65 207 532544.79 52.76 95.65 0.65- 0.62 207 259064.35 30.10 76.81 0.62- 0.58 210 256347.22 30.65 79.52 ------------------------------------------------------------------------------------ 4.82- 0.58 2073 508727.21 55.21 92.57 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:33:47 2018 Sorting 2073 observations 84 unique observations with > 7.00 F2/sig(F2) 2073 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 49 364 Total number of frames 364 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2073 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 9 74 Total number of frames 74 1666 observations > 7.00 F2/sig(F2) 1666 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 9 74 Total number of frames 74 Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 1666 removed 5 = 1661, unique = 88) 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 1661 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 9 74 Total number of frames 74 88 unique data precomputed (should be 88) 88 unique data with 1661 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 1661 removed 0 = 1661, unique = 88) 88 unique data precomputed (should be 88) 88 unique data with 1661 observations RMS deviation of equivalent data = 0.21662 Rint = 0.17339 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17084, wR= 0.22569 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08419, wR= 0.11247, Acormin=0.652, Acormax=1.420, Acor_av=0.921 F test: Probability=1.000, F= 4.105 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08398, wR= 0.10307, Acormin=0.606, Acormax=1.359, Acor_av=0.884 F test: Probability=0.524, F= 1.003 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06984, wR= 0.09804, Acormin=0.645, Acormax=1.518, Acor_av=0.886 F test: Probability=1.000, F= 1.445 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06546, wR= 0.08714, Acormin=0.601, Acormax=1.472, Acor_av=0.876 F test: Probability=0.994, F= 1.136 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06011, wR= 0.08058, Acormin=0.519, Acormax=1.336, Acor_av=0.800 F test: Probability=0.999, F= 1.181 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06466, wR= 0.08974, Acormin=0.622, Acormax=1.480, Acor_av=0.878 F test: Probability=0.000, F= 0.862 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06075, wR= 0.08049, Acormin=0.571, Acormax=1.491, Acor_av=0.862 F test: Probability=0.000, F= 0.975 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05571, wR= 0.07366, Acormin=0.503, Acormax=1.371, Acor_av=0.790 F test: Probability=0.998, F= 1.154 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04635, wR= 0.06476, Acormin=0.415, Acormax=1.249, Acor_av=0.691 F test: Probability=1.000, F= 1.434 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05853, wR= 0.07631, Acormin=0.435, Acormax=1.321, Acor_av=0.781 F test: Probability=0.000, F= 0.629 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05555, wR= 0.07084, Acormin=0.513, Acormax=1.420, Acor_av=0.812 F test: Probability=0.000, F= 0.697 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04673, wR= 0.05997, Acormin=0.301, Acormax=0.862, Acor_av=0.480 F test: Probability=0.000, F= 0.980 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04014, wR= 0.05258, Acormin=0.328, Acormax=0.968, Acor_av=0.536 F test: Probability=1.000, F= 1.319 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03772, wR= 0.04932, Acormin=0.342, Acormax=1.041, Acor_av=0.570 F test: Probability=1.000, F= 1.478 Final absorption model (ne=8, no=7): Rint= 0.03772, Acormin=0.342, Acormax=1.041, Acor_av=0.570 Combined refinement in use Rint: 0.17350 There are 74 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: 8, max odd order: 7 (80 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21662 Using Levenberg-Marquardt: 0.00010 New wR= 0.04241 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17339 with corrections 0.03178 Rint for all data: 0.17350 with corrections 0.03200 0 observations identified as outliers and rejected Cycle 2 wR= 0.04241 Using Levenberg-Marquardt: 0.00001 New wR= 0.03967 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17339 with corrections 0.03025 Rint for all data: 0.17350 with corrections 0.03047 2 observations identified as outliers and rejected Cycle 3 wR= 0.03811 Using Levenberg-Marquardt: 0.00000 New wR= 0.03720 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17352 with corrections 0.02912 Rint for all data: 0.17350 with corrections 0.02958 0 observations identified as outliers and rejected Cycle 4 wR= 0.03720 Using Levenberg-Marquardt: 0.00000 New wR= 0.03693 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17352 with corrections 0.02890 Rint for all data: 0.17350 with corrections 0.02936 0 observations identified as outliers and rejected Cycle 5 wR= 0.03693 Using Levenberg-Marquardt: 0.00000 New wR= 0.03674 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17352 with corrections 0.02876 Rint for all data: 0.17350 with corrections 0.02922 0 observations identified as outliers and rejected Final wR= 0.03674 Final frame scales: Min= 0.8481 Max= 1.0931 Final absorption correction factors: Amin= 0.4369 Amax= 1.3751 PROFFIT INFO: Inet (after scale3 abspack): min=546.3385 max=5789425.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=167.4634 max=68300.7344 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2073 reflections read from tmp file 213 reflections are rejected (211 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 2 4 4 5 2 1 81 Initial Chi^2= 0.30208 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.12392 Current error model SIG(F2)^2 = 106.08*I_RAW + 0.00*I_BACK+(0.01156*)^2 Cycle 2, Chi^2= 1.03773 Current error model SIG(F2)^2 = 73.21*I_RAW + 0.00*I_BACK+(0.02012*)^2 Cycle 3, Chi^2= 1.00374 Current error model SIG(F2)^2 = 88.84*I_RAW + 0.00*I_BACK+(0.01716*)^2 Cycle 4, Chi^2= 0.99992 Current error model SIG(F2)^2 = 85.84*I_RAW + 0.00*I_BACK+(0.01794*)^2 Cycle 5, Chi^2= 1.00009 Current error model SIG(F2)^2 = 86.76*I_RAW + 0.00*I_BACK+(0.01772*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 86.51*I_RAW + 0.00*I_BACK+(0.01778*)^2 Final Chi^2= 0.99998 Final error model SIG(F2)^2 = 86.51*I_RAW + 0.00*I_BACK+(0.01778*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5789425- 1572152 207 2312403.17 51.84 100.00 1563098- 1024114 207 1238213.43 44.84 100.00 1023049- 333094 207 605698.66 42.94 100.00 330910- 201468 207 247205.24 36.16 100.00 201449- 171849 207 185415.70 28.90 100.00 170915- 128516 207 141976.63 23.00 100.00 128512- 102493 207 116079.59 20.35 100.00 102259- 5821 207 58826.84 15.13 100.00 5811- 3499 207 4408.28 4.91 100.00 3493- 546 210 2699.80 3.98 81.43 ------------------------------------------------------------------------------------ 5789425- 546 2073 490585.65 27.17 98.12 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 207 809909.85 40.55 100.00 1.39- 1.12 207 956127.09 35.50 100.00 1.09- 0.96 207 487815.55 30.71 100.00 0.96- 0.88 207 472908.03 27.39 98.55 0.88- 0.81 207 623084.14 31.77 100.00 0.81- 0.73 207 334545.10 21.90 99.03 0.73- 0.71 207 250962.86 20.35 98.07 0.71- 0.65 207 491449.41 27.27 99.03 0.65- 0.62 207 245704.46 17.84 92.75 0.62- 0.58 210 237024.83 18.57 93.81 ------------------------------------------------------------------------------------ 4.82- 0.58 2073 490585.65 27.17 98.12 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 207 809909.85 40.55 100.00 4.82- 1.12 414 883018.47 38.02 100.00 4.82- 0.96 621 751284.17 35.59 100.00 4.82- 0.88 828 681690.13 33.54 99.64 4.82- 0.81 1035 669968.93 33.18 99.71 4.82- 0.73 1242 614064.96 31.30 99.60 4.82- 0.71 1449 562193.23 29.74 99.38 4.82- 0.65 1656 553350.25 29.43 99.34 4.82- 0.62 1863 519167.39 28.14 98.60 4.82- 0.58 2073 490585.65 27.17 98.12 ------------------------------------------------------------------------------------ 4.82- 0.58 2073 490585.65 27.17 98.12 Scale applied to data: s=0.172729 (maximum obs:5789425.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.029; Rsigma 0.024: data 2073 -> merged 109 With outlier rejection... Rint 0.027; Rsigma 0.024: data 2060 -> merged 109 Rejected total: 13, method kkm 13, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585848, 4.831023 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 9 10 12.44 90.00 112 1.61 - 1.21 10 10 18.60 100.00 186 1.17 - 1.01 10 10 24.40 100.00 244 0.99 - 0.89 10 10 24.80 100.00 248 0.88 - 0.81 10 10 22.80 100.00 228 0.81 - 0.74 10 10 20.90 100.00 209 0.73 - 0.71 10 10 22.30 100.00 223 0.70 - 0.66 10 10 18.20 100.00 182 0.66 - 0.64 10 10 17.90 100.00 179 0.63 - 0.60 10 10 17.40 100.00 174 --------------------------------------------------------------- 5.91 - 0.60 99 100 20.05 99.00 1985 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:33:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919979 5.916472 5.912397 60.0644 90.0913 60.0024 1944 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 958 1024 952 968 1467 1301 1294 1944 N (int>3sigma) = 0 787 1024 781 796 1296 1111 1095 1647 Mean intensity = 0.0 9.1 4.0 9.2 9.9 7.4 10.1 10.0 10.1 Mean int/sigma = 0.0 25.6 22.2 25.6 26.4 24.4 26.4 26.5 26.7 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.913 5.916 90.06 119.94 119.93 Niggli form: a.a = 34.956 b.b = 34.960 c.c = 35.005 b.c = -0.037 a.c = -17.456 a.b = -17.444 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.097 CUBIC F-lattice R(int) = 0.127 [ 1789] Vol = 585.8 Cell: 8.369 8.373 8.360 90.07 89.96 90.02 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.121 [ 1517] Vol = 439.4 Cell: 5.918 5.913 14.504 90.03 90.04 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.118 [ 476] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.504 90.03 90.04 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.051 TETRAGONAL I-lattice R(int) = 0.116 [ 1552] Vol = 292.9 Cell: 5.920 5.918 8.360 89.97 89.92 89.97 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.110 TETRAGONAL I-lattice R(int) = 0.116 [ 1552] Vol = 292.9 Cell: 5.918 5.920 8.360 90.08 90.03 89.97 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.059 ORTHORHOMBIC I-lattice R(int) = 0.103 [ 1500] Vol = 292.9 Cell: 5.918 5.920 8.360 89.92 89.97 89.97 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.118 [ 1506] Vol = 292.9 Cell: 5.912 8.369 5.920 89.96 89.91 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.102 [ 1197] Vol = 292.9 Cell: 5.920 5.918 8.360 90.03 90.08 89.97 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.099 MONOCLINIC I-lattice R(int) = 0.106 [ 1210] Vol = 292.9 Cell: 5.912 5.920 8.369 90.04 90.01 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.046 MONOCLINIC I-lattice R(int) = 0.106 [ 1218] Vol = 292.9 Cell: 5.912 8.369 5.920 89.96 90.09 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.112 [ 1220] Vol = 292.9 Cell: 8.369 5.912 5.920 90.09 90.04 90.01 Volume: 292.92 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.078 MONOCLINIC C-lattice R(int) = 0.099 [ 1232] Vol = 292.9 Cell: 10.247 5.913 5.916 90.06 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.093 [ 800] Vol = 146.5 Cell: 5.912 5.913 5.916 90.06 119.94 119.93 Volume: 146.46 Matrix: 0.0000 0.0000 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 1024 0 1297 1301 1944 N (int>3sigma) = 0 0 0 0 1024 0 1102 1111 1647 Mean intensity = 0.0 0.0 0.0 0.0 4.0 0.0 10.2 10.1 10.1 Mean int/sigma = 0.0 0.0 0.0 0.0 22.2 0.0 27.1 26.4 26.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 138 450 N I>3s 10 10 64 450 0.1 0.1 0.1 4.6 7.4 7.4 3.6 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.127 1671 Fd-3m 1 1 227 C N N N N 37 2284 0.127 1709 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368936 8.373419 8.360086 90.0734 89.9638 90.0169 ZERR 1.00 0.003237 0.001955 0.000332 0.0000 0.0125 0.0001 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5789425- 922864 459 454 27 16.8 1687338.79 47.46 0.025 0.035 887218- 160483 610 606 27 22.4 287858.79 35.18 0.028 0.034 149363- 53915 516 514 27 19.0 114585.51 20.33 0.044 0.058 22791- 1646 488 486 28 17.4 4732.11 5.10 0.146 0.176 ------------------------------------------------------------------------------------------- 5789425- 1646 2073 2060 109 18.9 486257.77 27.09 0.027 0.037 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 504 499 27 18.5 773552.31 37.25 0.026 0.039 0.020 1.01-0.78 652 651 28 23.3 471137.90 26.24 0.022 0.029 0.024 0.76-0.65 552 549 28 19.6 385619.88 23.42 0.030 0.037 0.027 0.65-0.59 365 361 26 13.9 269452.37 20.14 0.036 0.043 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 2073 2060 109 18.9 486257.77 27.09 0.027 0.037 0.024 inf-0.60 1994 1984 99 20.0 497514.39 27.45 0.027 0.037 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 499 27 27 100.0 18.5 773552.31 182.66 0.026 0.007 1.01-0.78 651 28 28 100.0 23.3 471137.90 135.03 0.022 0.005 0.76-0.65 549 28 28 100.0 19.6 385619.88 111.81 0.030 0.007 0.65-0.59 361 27 26 96.3 13.9 269452.37 85.86 0.036 0.010 -------------------------------------------------------------------------------------------- inf-0.59 2060 110 109 99.1 18.9 486257.77 131.76 0.027 0.007 inf-0.60 1984 99 99 100.0 20.0 497514.39 134.60 0.027 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:39:03 2018) ID: 2932; threads 39; handles 876; mem 519952.00 (1237724.00)kB; time: 1w 5d 22h 44m 34s MEMORY INFO: Memory PF:2.0, Ph:170.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.8,peak PF: 708.5, WS: 271.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:4.0, Ph:170.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:509.6,peak PF: 708.5, WS: 273.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:39:03 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000015 0.000017 0.000015 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000012 0.000011 ) 0.055227 -0.024260 0.122680 ( 0.000015 0.000016 0.000014 ) 5.91535 ( 0.00081 ) 5.92288 ( 0.00062 ) 5.91286 ( 0.00081 ) 59.95509 ( 0.01254 ) 89.89521 ( 0.01110 ) 59.99590 ( 0.01257 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 13:39:03 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000015 0.000017 0.000015 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000012 0.000011 ) 0.055227 -0.024260 0.122680 ( 0.000015 0.000016 0.000014 ) M - matrix: 0.021552 -0.014380 0.007215 ( 0.000004 0.000003 0.000003 ) -0.014380 0.028733 -0.014371 ( 0.000003 0.000004 0.000003 ) 0.007215 -0.014371 0.021580 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9154(8) 5.9229(6) 5.9129(8) 59.955(13) 89.895(11) 59.996(13) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_4_51.rpb PROFFITPEAK info: 907 peaks in the peak location table UB fit with 411 obs out of 437 (total:437,skipped:0) (94.05%) UB - matrix: -0.104309 -0.014957 0.049065 ( 0.000076 0.000071 0.000038 ) 0.087240 -0.167072 0.063522 ( 0.000107 0.000100 0.000054 ) 0.055370 -0.024385 0.122990 ( 0.000087 0.000082 0.000044 ) M - matrix: 0.021557 -0.014365 0.007234 ( 0.000026 0.000022 0.000015 ) -0.014365 0.028731 -0.014346 ( 0.000022 0.000034 0.000015 ) 0.007234 -0.014346 0.021569 ( 0.000015 0.000015 0.000013 ) unit cell: 5.916(4) 5.907(4) 5.910(3) 60.17(6) 90.24(5) 60.09(7) V = 146.30(16) UB fit with 411 obs out of 437 (total:437,skipped:0) (94.05%) UB - matrix: -0.104309 -0.014957 0.049065 ( 0.000076 0.000071 0.000038 ) 0.087240 -0.167072 0.063522 ( 0.000107 0.000100 0.000054 ) 0.055370 -0.024385 0.122990 ( 0.000087 0.000082 0.000044 ) M - matrix: 0.021557 -0.014365 0.007234 ( 0.000026 0.000022 0.000015 ) -0.014365 0.028731 -0.014346 ( 0.000022 0.000034 0.000015 ) 0.007234 -0.014346 0.021569 ( 0.000015 0.000015 0.000013 ) unit cell: 5.916(4) 5.907(4) 5.910(3) 60.17(6) 90.24(5) 60.09(7) V = 146.30(16) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB fit with 416 obs out of 437 (total:437,skipped:0) (95.19%) UB - matrix: -0.104369 -0.014927 0.049022 ( 0.000078 0.000073 0.000040 ) 0.087256 -0.167096 0.063549 ( 0.000098 0.000092 0.000050 ) 0.055368 -0.024358 0.123010 ( 0.000089 0.000083 0.000046 ) M - matrix: 0.021572 -0.014371 0.007240 ( 0.000026 0.000020 0.000015 ) -0.014371 0.028737 -0.014347 ( 0.000020 0.000031 0.000015 ) 0.007240 -0.014347 0.021573 ( 0.000015 0.000015 0.000014 ) unit cell: 5.914(4) 5.906(4) 5.909(3) 60.18(6) 90.26(5) 60.10(7) V = 146.21(15) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 437 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Run 4 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 586 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104385 -0.014918 0.049017 ( 0.000079 0.000074 0.000041 ) 0.087269 -0.167105 0.063552 ( 0.000099 0.000092 0.000051 ) 0.055379 -0.024368 0.123013 ( 0.000090 0.000084 0.000046 ) M - matrix: 0.021579 -0.014375 0.007242 ( 0.000026 0.000021 0.000015 ) -0.014375 0.028740 -0.014349 ( 0.000021 0.000031 0.000015 ) 0.007242 -0.014349 0.021574 ( 0.000015 0.000015 0.000014 ) UB fit with 417 obs out of 437 (total:437,skipped:0) (95.42%) unit cell: 5.913(4) 5.906(4) 5.909(3) 60.18(6) 90.26(5) 60.09(7) V = 146.19(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 437 (total:437,skipped:0) (95.42%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_51.rpb 7 of 341 peaks identified as outliers and rejected 334 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 334 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 334 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 33 | 1.041 ( 0.257) | 1.151 ( 0.498) | 1.209 ( 0.808) | 1.41- 1.15 | 33 | 1.082 ( 0.071) | 1.208 ( 0.360) | 1.169 ( 0.596) | 1.15- 1.01 | 33 | 1.075 ( 0.095) | 1.182 ( 0.414) | 1.124 ( 0.577) | 1.01- 0.92 | 33 | 1.113 ( 0.091) | 1.179 ( 0.228) | 1.132 ( 0.446) | 0.92- 0.82 | 33 | 1.119 ( 0.070) | 1.144 ( 0.115) | 1.054 ( 0.282) | 0.82- 0.76 | 33 | 1.165 ( 0.084) | 1.153 ( 0.152) | 1.132 ( 0.370) | 0.76- 0.71 | 33 | 1.166 ( 0.069) | 1.176 ( 0.125) | 1.089 ( 0.382) | 0.71- 0.67 | 33 | 1.174 ( 0.061) | 1.135 ( 0.114) | 1.305 ( 0.442) | 0.67- 0.64 | 33 | 1.202 ( 0.070) | 1.185 ( 0.135) | 1.261 ( 0.428) | 0.63- 0.59 | 37 | 1.236 ( 0.086) | 1.160 ( 0.207) | 1.269 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 334 | 1.138 ( 0.125) | 1.167 ( 0.270) | 1.175 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 334 obs out of 334 (total:334,skipped:0) (100.00%) UB - matrix: -0.104329 -0.015139 0.049373 ( 0.000035 0.000032 0.000019 ) 0.087381 -0.167423 0.063780 ( 0.000046 0.000041 0.000024 ) 0.055146 -0.024388 0.122949 ( 0.000026 0.000023 0.000014 ) M - matrix: 0.021561 -0.014395 0.007202 ( 0.000011 0.000009 0.000006 ) -0.014395 0.028855 -0.014424 ( 0.000009 0.000014 0.000006 ) 0.007202 -0.014424 0.021622 ( 0.000006 0.000006 0.000005 ) unit cell: 5.9150(17) 5.9042(15) 5.9085(11) 60.00(2) 90.025(18) 60.03(3) V = 145.93(6) OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 UB - matrix: -0.104336 -0.015016 0.049133 ( 0.000033 0.000030 0.000018 ) 0.087070 -0.167049 0.063679 ( 0.000039 0.000035 0.000021 ) 0.055109 -0.024195 0.122766 ( 0.000024 0.000022 0.000013 ) M - matrix: 0.021504 -0.014312 0.007184 ( 0.000010 0.000008 0.000005 ) -0.014312 0.028716 -0.014346 ( 0.000008 0.000012 0.000005 ) 0.007184 -0.014346 0.021541 ( 0.000005 0.000005 0.000004 ) UB fit with 334 obs out of 334 (total:334,skipped:0) (100.00%) unit cell: 5.9167(15) 5.9084(13) 5.9162(10) 60.06(2) 90.136(17) 60.14(3) V = 146.52(6) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 587 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104336 -0.015016 0.049133 ( 0.000033 0.000030 0.000018 ) 0.087070 -0.167049 0.063679 ( 0.000039 0.000035 0.000021 ) 0.055109 -0.024195 0.122766 ( 0.000024 0.000022 0.000013 ) M - matrix: 0.021504 -0.014312 0.007184 ( 0.000010 0.000008 0.000005 ) -0.014312 0.028716 -0.014346 ( 0.000008 0.000012 0.000005 ) 0.007184 -0.014346 0.021541 ( 0.000005 0.000005 0.000004 ) UB fit with 334 obs out of 334 (total:334,skipped:0) (100.00%) unit cell: 5.9167(15) 5.9084(13) 5.9162(10) 60.06(2) 90.136(17) 60.14(3) V = 146.52(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 334 obs out of 334 (total:334,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= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_51.rpb 8 of 338 peaks identified as outliers and rejected 330 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 330 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 330 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 33 | 1.067 ( 0.262) | 1.221 ( 0.575) | 1.207 ( 0.762) | 1.41- 1.15 | 33 | 1.073 ( 0.078) | 1.237 ( 0.433) | 1.116 ( 0.544) | 1.15- 1.00 | 33 | 1.072 ( 0.093) | 1.181 ( 0.339) | 1.097 ( 0.516) | 0.99- 0.92 | 33 | 1.127 ( 0.073) | 1.142 ( 0.095) | 1.147 ( 0.459) | 0.92- 0.82 | 33 | 1.131 ( 0.070) | 1.154 ( 0.113) | 1.112 ( 0.350) | 0.82- 0.76 | 33 | 1.161 ( 0.086) | 1.145 ( 0.157) | 1.145 ( 0.389) | 0.76- 0.71 | 33 | 1.168 ( 0.068) | 1.185 ( 0.121) | 1.151 ( 0.404) | 0.71- 0.67 | 33 | 1.176 ( 0.060) | 1.140 ( 0.122) | 1.270 ( 0.463) | 0.67- 0.63 | 33 | 1.209 ( 0.074) | 1.185 ( 0.136) | 1.279 ( 0.419) | 0.63- 0.59 | 33 | 1.228 ( 0.086) | 1.153 ( 0.205) | 1.234 ( 0.444) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 330 | 1.141 ( 0.123) | 1.174 ( 0.279) | 1.176 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 167 | 1.154 ( 0.136) | 1.250 ( 0.380) | 1.379 ( 0.714) | 13.1-19.0 | 167 | 1.146 ( 0.116) | 1.202 ( 0.307) | 1.334 ( 0.686) | 19.0-23.1 | 167 | 1.156 ( 0.095) | 1.219 ( 0.319) | 1.250 ( 0.668) | 23.1-27.4 | 167 | 1.135 ( 0.098) | 1.177 ( 0.317) | 1.211 ( 0.510) | 27.4-30.6 | 167 | 1.143 ( 0.104) | 1.177 ( 0.214) | 1.199 ( 0.457) | 30.6-34.0 | 167 | 1.155 ( 0.091) | 1.156 ( 0.218) | 1.229 ( 0.446) | 34.0-37.2 | 167 | 1.137 ( 0.111) | 1.111 ( 0.169) | 1.127 ( 0.393) | 37.2-39.9 | 167 | 1.156 ( 0.119) | 1.133 ( 0.246) | 1.260 ( 0.538) | 39.9-42.9 | 167 | 1.167 ( 0.117) | 1.115 ( 0.191) | 1.229 ( 0.575) | 42.9-49.8 | 164 | 1.205 ( 0.168) | 1.140 ( 0.296) | 1.187 ( 0.468) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 1667 | 1.155 ( 0.119) | 1.168 ( 0.277) | 1.241 ( 0.560) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0024 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6354 lp-corr: 4382 Maximum peak integral for reflections I/sig<= 100 - raw: 458459 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 20148380 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:39:20 2018 PROFFITMAIN - Started at Wed Mar 28 13:39:20 2018 OTKP changes: 1667 2 3 4 OTKP changes: 1667 2 3 4 UB - matrix: -0.104261 -0.014991 0.049485 ( 0.000014 0.000015 0.000013 ) 0.087381 -0.167249 0.063729 ( 0.000011 0.000011 0.000010 ) 0.055388 -0.024351 0.122923 ( 0.000014 0.000015 0.000013 ) M - matrix: 0.021574 -0.014400 0.007218 ( 0.000004 0.000003 0.000003 ) -0.014400 0.028790 -0.014394 ( 0.000003 0.000004 0.000003 ) 0.007218 -0.014394 0.021620 ( 0.000003 0.000003 0.000004 ) UB fit with 1667 obs out of 1667 (total:1667,skipped:0) (100.00%) unit cell: 5.9168(7) 5.9102(6) 5.9059(8) 60.069(12) 90.073(10) 59.993(12) V = 146.08(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104113 -0.015206 0.049827 ( 0.000025 0.000032 0.000028 ) 0.087321 -0.167075 0.063633 ( 0.000017 0.000022 0.000019 ) 0.055393 -0.024082 0.122515 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014340 0.007155 ( 0.000006 0.000005 0.000005 ) -0.014340 0.028725 -0.014340 ( 0.000005 0.000007 0.000005 ) 0.007155 -0.014340 0.021542 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9161(14) 5.9125(10) 5.9142(13) 60.04(2) 89.988(19) 60.02(2) V = 146.43(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104058 -0.015210 0.049812 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024159 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104058 -0.015210 0.049812 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024159 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104058 -0.015210 0.049812 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024159 0.122546 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104490 -0.014345 0.049138 ( 0.000035 0.000044 0.000038 ) 0.087135 -0.167075 0.063758 ( 0.000025 0.000031 0.000027 ) 0.055262 -0.024927 0.122922 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021564 -0.014437 0.007214 ( 0.000009 0.000007 0.000006 ) -0.014437 0.028741 -0.014421 ( 0.000007 0.000011 0.000007 ) 0.007214 -0.014421 0.021589 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9288(19) 5.9359(14) 5.9204(16) 59.90(3) 89.88(2) 59.82(3) V = 146.86(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007256 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007256 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007256 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146804 -0.097926 0.049161 ( 0.000021 0.000026 0.000023 ) -0.000020 0.138450 -0.069287 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000033 0.119949 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021551 -0.014379 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028758 -0.014403 ( 0.000005 0.000009 0.000006 ) 0.007216 -0.014403 0.021605 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9186(10) 5.9163(14) 5.9125(14) 60.00(2) 90.057(17) 60.02(2) V = 146.37(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) UB - matrix: -0.104340 -0.015016 0.049244 ( 0.000031 0.000027 0.000016 ) 0.087236 -0.167284 0.063708 ( 0.000041 0.000037 0.000022 ) 0.055157 -0.024391 0.122970 ( 0.000029 0.000026 0.000015 ) M - matrix: 0.021539 -0.014372 0.007202 ( 0.000010 0.000008 0.000005 ) -0.014372 0.028804 -0.014396 ( 0.000008 0.000012 0.000006 ) 0.007202 -0.014396 0.021605 ( 0.000005 0.000006 0.000005 ) unit cell: 5.9173(15) 5.9060(14) 5.9087(12) 60.04(2) 90.077(18) 60.05(3) V = 146.12(6) OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 UB - matrix: -0.104334 -0.015122 0.049261 ( 0.000031 0.000027 0.000016 ) 0.087144 -0.167181 0.063692 ( 0.000039 0.000035 0.000021 ) 0.055128 -0.024176 0.122798 ( 0.000027 0.000024 0.000014 ) M - matrix: 0.021519 -0.014324 0.007180 ( 0.000010 0.000008 0.000005 ) -0.014324 0.028763 -0.014362 ( 0.000008 0.000012 0.000005 ) 0.007180 -0.014362 0.021563 ( 0.000005 0.000005 0.000005 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9138(15) 5.9031(13) 5.9126(11) 60.06(2) 90.112(17) 60.14(2) V = 146.24(6) Run 4 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104334 -0.015122 0.049261 ( 0.000031 0.000027 0.000016 ) 0.087144 -0.167181 0.063692 ( 0.000039 0.000035 0.000021 ) 0.055128 -0.024176 0.122798 ( 0.000027 0.000024 0.000014 ) M - matrix: 0.021519 -0.014324 0.007180 ( 0.000010 0.000008 0.000005 ) -0.014324 0.028763 -0.014362 ( 0.000008 0.000012 0.000005 ) 0.007180 -0.014362 0.021563 ( 0.000005 0.000005 0.000005 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9138(15) 5.9031(13) 5.9126(11) 60.06(2) 90.112(17) 60.14(2) V = 146.24(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104334 -0.015122 0.049261 ( 0.000031 0.000027 0.000016 ) 0.087144 -0.167181 0.063692 ( 0.000039 0.000035 0.000021 ) 0.055128 -0.024176 0.122798 ( 0.000027 0.000024 0.000014 ) M - matrix: 0.021519 -0.014324 0.007180 ( 0.000010 0.000008 0.000005 ) -0.014324 0.028763 -0.014362 ( 0.000008 0.000012 0.000005 ) 0.007180 -0.014362 0.021563 ( 0.000005 0.000005 0.000005 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9138(15) 5.9031(13) 5.9126(11) 60.06(2) 90.112(17) 60.14(2) V = 146.24(6) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104222 -0.014955 0.049381 ( 0.000014 0.000015 0.000013 ) 0.087311 -0.167091 0.063694 ( 0.000011 0.000012 0.000010 ) 0.055352 -0.024338 0.122808 ( 0.000013 0.000014 0.000013 ) M - matrix: 0.021549 -0.014377 0.007212 ( 0.000004 0.000003 0.000003 ) -0.014377 0.028735 -0.014370 ( 0.000003 0.000004 0.000003 ) 0.007212 -0.014370 0.021577 ( 0.000003 0.000003 0.000004 ) UB fit with 1667 obs out of 1667 (total:1667,skipped:0) (100.00%) unit cell: 5.9199(7) 5.9159(6) 5.9127(7) 60.063(11) 90.089(10) 60.006(12) V = 146.46(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 39 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof 2221 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:39:24 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22335936.0000 PROFFIT INFO: signal sum lp corr: min=241.7852 max=3281048.1253 PROFFIT INFO: background sum: min=763.0000 max=15918.0000 PROFFIT INFO: background sum sig2: min=602.0000 max=11374.0000 PROFFIT INFO: num of signal pixels: min=60 max=989 PROFFIT INFO: Inet: min=527.5313 max=7158651.0000 PROFFIT INFO: sig(Inet): min=190.6897 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=400.16 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 46 164 289 458 505 881 1466 2001 2220 Percent 0.0 0.1 2.1 7.4 13.0 20.6 22.7 39.7 66.0 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2221 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 2221 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7158651- 1613231 222 2447841.34 135.91 100.00 1613142- 1027314 222 1301502.63 110.53 100.00 1023524- 328909 222 600158.29 94.75 100.00 328469- 223081 222 263387.98 70.89 100.00 222487- 166290 222 193385.04 49.75 100.00 166253- 132210 222 149989.31 36.24 100.00 132179- 101206 222 117013.51 30.87 100.00 101091- 6080 222 55223.58 20.34 100.00 6075- 3651 222 4673.09 5.08 84.68 3645- 528 222 2683.46 3.11 41.44 ------------------------------------------------------------------------------------ 7158651- 528 2220 513585.82 55.75 92.61 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 222 824501.47 86.07 99.55 1.28- 1.03 222 639223.92 64.21 96.85 1.03- 0.89 222 691488.94 70.07 96.40 0.89- 0.78 222 528801.42 61.55 95.05 0.78- 0.72 222 480637.46 56.54 95.05 0.72- 0.65 222 440574.96 51.42 90.99 0.65- 0.60 222 480592.15 51.06 90.54 0.60- 0.55 222 335944.53 40.30 92.79 0.55- 0.49 222 347858.58 37.85 81.53 0.49- 0.40 222 366234.79 38.40 87.39 ------------------------------------------------------------------------------------ 5.26- 0.40 2220 513585.82 55.75 92.61 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:39:24 2018 Sorting 2220 observations 278 unique observations with > 7.00 F2/sig(F2) 2220 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 74 389 Total number of frames 389 Maximum number of 278 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2220 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 37 197 Total number of frames 197 1789 observations > 7.00 F2/sig(F2) 1789 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 36 196 Total number of frames 196 Removing 'redundancy=1' reflections Average redundancy: 6.4 (Out of 1789 removed 29 = 1760, unique = 275) 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 1760 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 36 196 Total number of frames 196 275 unique data precomputed (should be 275) 275 unique data with 1760 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.4 (Out of 1760 removed 0 = 1760, unique = 275) 275 unique data precomputed (should be 275) 275 unique data with 1760 observations RMS deviation of equivalent data = 0.72946 Rint = 0.68311 10 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66231, wR= 3.09548 Trying model 1 (ne=2, no=0)... Results: Rint= 0.72828, wR= 2.13957, Acormin=-0.351, Acormax=2.543, Acor_av=0.593 F test: Probability=0.000, F= 0.824 Trying model 2 (ne=2, no=1)... Results: Rint= 0.77994, wR= 2.16235, Acormin=-0.311, Acormax=2.408, Acor_av=0.433 F test: Probability=0.000, F= 0.717 Trying model 3 (ne=4, no=0)... Results: Rint= 0.74102, wR= 1.83207, Acormin=-0.207, Acormax=2.716, Acor_av=0.536 F test: Probability=0.000, F= 0.791 Trying model 4 (ne=4, no=1)... Results: Rint= 0.81700, wR= 2.04169, Acormin=-0.323, Acormax=2.036, Acor_av=0.406 F test: Probability=0.000, F= 0.650 Trying model 5 (ne=4, no=3)... Results: Rint= 0.90038, wR= 1.61644, Acormin=-0.486, Acormax=3.351, Acor_av=0.147 F test: Probability=0.000, F= 0.532 Trying model 6 (ne=6, no=0)... Results: Rint= 0.73479, wR= 2.09664, Acormin=-0.473, Acormax=2.950, Acor_av=0.497 F test: Probability=0.000, F= 0.798 Trying model 7 (ne=6, no=1)... Results: Rint= 0.81786, wR= 2.06033, Acormin=-0.452, Acormax=2.585, Acor_av=0.372 F test: Probability=0.000, F= 0.642 Trying model 8 (ne=6, no=3)... Results: Rint= 0.91983, wR= 1.51971, Acormin=-0.789, Acormax=3.387, Acor_av=0.128 F test: Probability=0.000, F= 0.505 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96551, wR= 1.43978, Acormin=-0.568, Acormax=2.962, Acor_av=0.076 F test: Probability=0.000, F= 0.455 Trying model 10 (ne=8, no=0)... Results: Rint= 0.84049, wR= 1.79069, Acormin=-0.752, Acormax=1.715, Acor_av=0.261 F test: Probability=0.000, F= 0.602 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87183, wR= 1.97724, Acormin=-0.569, Acormax=1.346, Acor_av=0.190 F test: Probability=0.000, F= 0.559 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97675, wR= 2.12385, Acormin=-0.061, Acormax=0.072, Acor_av=0.002 F test: Probability=0.000, F= 0.443 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99251, wR= 2.06343, Acormin=-0.060, Acormax=0.059, Acor_av=0.002 F test: Probability=0.000, F= 0.426 Trying model 14 (ne=8, no=7)... Results: Rint= 0.99314, wR= 1.68602, Acormin=-0.082, Acormax=0.068, Acor_av=0.000 F test: Probability=0.000, F= 0.421 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: 0.86101 There are 196 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 200 pars with 20100 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.72946 Using Levenberg-Marquardt: 0.00010 New wR= 0.70825 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.68311 with corrections 0.67113 Rint for all data: 0.86101 with corrections 0.85898 8 observations identified as outliers and rejected Cycle 2 wR= 0.68224 Using Levenberg-Marquardt: 0.00001 New wR= 0.68225 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.66548 with corrections 0.64545 Rint for all data: 0.86101 with corrections 0.85188 Final wR= 0.68225 Final frame scales: Min= 0.9710 Max= 2.6126 Final absorption correction factors: Amin= 0.5466 Amax= 1.7357 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=512.2889 max=7762641.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=161.9304 max=79266.9063 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2219 reflections read from tmp file 1659 reflections are rejected (1583 as outliers, 76 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 86 44 27 16 5 3 1 1 Initial Chi^2= 0.59691 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.87466 Current error model SIG(F2)^2 = 271.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 237.62*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 237.62*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7762642- 1514959 221 2309758.04 88.74 100.00 1514804- 1024169 221 1241531.83 48.35 100.00 1021284- 306210 221 613292.15 42.66 100.00 306196- 208834 221 251497.09 31.49 100.00 208062- 159876 221 183640.27 21.61 100.00 159567- 130820 221 145372.61 16.45 100.00 130757- 104392 221 117922.71 13.81 100.00 104362- 6524 221 59790.51 9.78 96.83 6483- 3518 221 4616.20 3.19 37.10 3515- 512 230 2644.34 2.47 18.26 ------------------------------------------------------------------------------------ 7762642- 512 2219 491017.72 27.75 84.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 221 875147.73 57.69 98.64 1.28- 1.03 221 596992.67 36.69 90.50 1.03- 0.89 221 682398.01 36.40 90.95 0.89- 0.79 221 489958.87 26.70 84.16 0.79- 0.72 221 472083.41 25.27 90.05 0.72- 0.65 221 407234.90 22.42 77.83 0.65- 0.60 221 430780.39 21.88 81.90 0.60- 0.55 221 310734.66 17.38 83.26 0.55- 0.49 221 314260.89 16.85 75.11 0.49- 0.40 230 336863.49 16.70 77.39 ------------------------------------------------------------------------------------ 5.26- 0.40 2219 491017.72 27.75 84.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 221 875147.73 57.69 98.64 5.26- 1.03 442 736070.20 47.19 94.57 5.26- 0.89 663 718179.47 43.59 93.36 5.26- 0.79 884 661124.32 39.37 91.06 5.26- 0.72 1105 623316.14 36.55 90.86 5.26- 0.65 1326 587302.60 34.20 88.69 5.26- 0.60 1547 564942.28 32.44 87.72 5.26- 0.55 1768 533166.33 30.55 87.16 5.26- 0.49 1989 508843.50 29.03 85.82 5.26- 0.40 2219 491017.72 27.75 84.95 ------------------------------------------------------------------------------------ 5.26- 0.40 2219 491017.72 27.75 84.95 Scale applied to data: s=0.128822 (maximum obs:7762641.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.852; Rsigma 0.024: data 2219 -> merged 317 With outlier rejection... Rint 0.781; Rsigma 0.024: data 2087 -> merged 317 Rejected total: 132, method kkm 123, method Blessing 9 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404281, 5.271178 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 10.07 100.00 151 1.46 - 1.12 15 15 13.07 100.00 196 1.08 - 0.96 15 15 12.40 100.00 186 0.96 - 0.86 15 15 12.53 100.00 188 0.86 - 0.79 15 15 10.27 100.00 154 0.79 - 0.73 15 15 8.80 100.00 132 0.73 - 0.69 15 15 7.87 100.00 118 0.69 - 0.65 15 15 9.07 100.00 136 0.65 - 0.63 15 15 5.47 100.00 82 0.63 - 0.60 21 21 6.24 100.00 131 --------------------------------------------------------------- 5.91 - 0.60 156 156 9.45 100.00 1474 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:39:25 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919940 5.915868 5.912670 60.0634 90.0888 60.0060 2087 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1029 1100 1019 1058 1574 1400 1382 2087 N (int>3sigma) = 0 850 1100 840 873 1395 1202 1172 1774 Mean intensity = 0.0 52.7 24.9 53.3 59.1 43.2 61.0 59.6 60.2 Mean int/sigma = 0.0 25.5 22.8 25.7 26.8 24.6 27.2 27.2 27.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.913 5.916 90.06 119.94 119.94 Niggli form: a.a = 34.960 b.b = 34.968 c.c = 34.997 b.c = -0.034 a.c = -17.456 a.b = -17.450 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.155 [ 1932] Vol = 585.8 Cell: 8.369 8.373 8.360 90.07 89.98 90.01 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.093 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 1661] Vol = 439.4 Cell: 5.918 5.913 14.502 90.02 90.05 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.093 RHOMBOHEDRAL R-lattice R(int) = 0.143 [ 521] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.502 90.02 90.05 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.041 TETRAGONAL I-lattice R(int) = 0.136 [ 1692] Vol = 292.9 Cell: 5.920 5.918 8.360 89.97 89.93 89.97 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.095 TETRAGONAL I-lattice R(int) = 0.136 [ 1692] Vol = 292.9 Cell: 5.918 5.920 8.360 90.07 90.03 89.97 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.050 ORTHORHOMBIC I-lattice R(int) = 0.136 [ 1639] Vol = 292.9 Cell: 5.918 5.920 8.360 89.93 89.97 89.97 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.049 ORTHORHOMBIC I-lattice R(int) = 0.135 [ 1643] Vol = 292.9 Cell: 5.913 8.369 5.920 89.97 89.91 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.130 [ 1331] Vol = 292.9 Cell: 5.920 5.918 8.360 90.03 90.07 89.97 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.090 MONOCLINIC I-lattice R(int) = 0.127 [ 1330] Vol = 292.9 Cell: 5.913 5.920 8.369 90.03 90.01 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.031 MONOCLINIC I-lattice R(int) = 0.122 [ 1351] Vol = 292.9 Cell: 5.913 8.369 5.920 89.97 90.09 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.039 MONOCLINIC I-lattice R(int) = 0.124 [ 1350] Vol = 292.9 Cell: 5.920 5.913 8.369 89.99 90.03 89.91 Volume: 292.92 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.130 [ 1336] Vol = 292.9 Cell: 10.247 5.913 5.916 90.06 125.20 89.94 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 874] Vol = 146.5 Cell: 5.913 5.913 5.916 90.06 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1100 0 1390 1400 2087 N (int>3sigma) = 0 0 0 0 1100 0 1184 1202 1774 Mean intensity = 0.0 0.0 0.0 0.0 24.9 0.0 60.2 61.0 60.2 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 27.6 27.2 27.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.177 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 162 489 N I>3s 12 12 80 489 0.7 0.7 0.5 29.2 6.4 6.4 3.7 27.9 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 0.155 1790 Fd-3m 1 1 227 C N N N N 37 2284 0.155 1828 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368593 8.373402 8.360434 90.0704 89.9755 90.0145 ZERR 1.00 0.002974 0.001780 0.000303 0.0002 0.0115 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3635658- 962567 193 177 31 5.7 1496529.85 63.88 0.472 0.381 954021- 714001 280 276 31 8.9 793015.18 36.87 0.974 0.931 712252- 584686 256 244 31 7.9 605110.08 32.89 0.902 0.840 581165- 460213 324 314 31 10.1 478017.07 30.05 0.985 1.060 456205- 362219 216 196 31 6.3 351030.90 26.89 0.941 1.012 358530- 246713 283 251 31 8.1 225308.05 19.04 0.747 0.859 245252- 133561 188 174 31 5.6 149876.73 17.60 0.486 0.402 131570- 109129 181 176 31 5.7 121029.58 14.33 0.412 0.304 107751- 76000 162 148 31 4.8 95256.34 11.03 0.513 0.375 75846- 1153 136 131 38 3.4 47866.42 6.83 0.708 0.668 ------------------------------------------------------------------------------------------- 3635658- 1153 2219 2087 317 6.6 466988.39 27.36 0.781 0.711 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 387 367 31 11.8 724396.27 49.26 0.762 0.767 0.014 1.05-0.83 388 378 32 11.8 579434.58 31.41 0.930 0.997 0.020 0.82-0.72 309 293 31 9.5 459141.96 26.12 0.752 0.766 0.025 0.72-0.65 255 241 31 7.8 366448.79 21.34 0.855 0.905 0.029 0.65-0.60 210 195 31 6.3 426318.23 21.74 0.777 0.821 0.029 0.60-0.56 216 193 35 5.5 285530.46 16.92 0.765 0.683 0.037 0.55-0.52 151 141 31 4.5 372796.47 18.96 0.784 0.734 0.033 0.51-0.49 115 107 31 3.5 230569.18 13.95 0.479 0.326 0.042 0.49-0.46 113 103 32 3.2 298289.19 15.80 0.416 0.322 0.040 0.45-0.40 75 69 32 2.2 299766.46 15.33 0.183 0.135 0.041 ------------------------------------------------------------------------------------------------------ inf-0.40 2219 2087 317 6.6 466988.39 27.36 0.781 0.711 0.024 inf-0.60 1549 1474 156 9.4 536536.30 31.88 0.819 0.847 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 367 31 31 100.0 11.8 724396.27 187.60 0.762 0.005 1.05-0.83 378 32 32 100.0 11.8 579434.58 135.38 0.930 0.008 0.82-0.72 293 31 31 100.0 9.5 459141.96 95.66 0.752 0.011 0.72-0.65 241 31 31 100.0 7.8 366448.79 79.45 0.855 0.014 0.65-0.60 195 31 31 100.0 6.3 426318.23 74.44 0.777 0.016 0.60-0.56 193 40 35 87.5 5.5 285530.46 50.13 0.765 0.019 0.55-0.52 141 37 31 83.8 4.5 372796.47 51.74 0.784 0.019 0.51-0.49 107 43 31 72.1 3.5 230569.18 30.63 0.479 0.023 0.49-0.46 103 59 32 54.2 3.2 298289.19 32.90 0.416 0.024 0.45-0.40 69 122 32 26.2 2.2 299766.46 25.60 0.183 0.028 -------------------------------------------------------------------------------------------- inf-0.40 2087 458 317 69.2 6.6 466988.39 99.24 0.781 0.014 inf-0.60 1474 156 156 100.0 9.4 536536.30 123.28 0.819 0.009 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007477 0.076800 -0.034897 ( 0.000007 0.000007 0.000007 ) -0.083543 -0.011808 -0.008043 ( 0.000006 0.000005 0.000005 ) -0.012169 0.033727 0.076912 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007184 0.000002 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007175 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000009 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007477 0.076800 -0.034897 ( 0.000007 0.000007 0.000007 ) -0.083543 -0.011808 -0.008043 ( 0.000006 0.000005 0.000005 ) -0.012169 0.033727 0.076912 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3688(5) 8.3736(7) 8.3604(7) 90.071(6) 89.975(6) 90.014(6) V = 585.87(8) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.87(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22335936.0000 PROFFIT INFO: signal sum lp corr: min=241.7852 max=3281048.1253 PROFFIT INFO: background sum: min=763.0000 max=15918.0000 PROFFIT INFO: background sum sig2: min=602.0000 max=11374.0000 PROFFIT INFO: num of signal pixels: min=60 max=989 PROFFIT INFO: Inet: min=527.5313 max=7158651.0000 PROFFIT INFO: sig(Inet): min=190.6897 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=400.16 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 92 328 578 916 1010 1762 2932 4002 4440 Percent 0.0 0.1 2.1 7.4 13.0 20.6 22.7 39.7 66.0 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2221 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 2221 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7158651- 1613231 222 2447841.34 135.91 100.00 1613142- 1027314 222 1301502.63 110.53 100.00 1023524- 328909 222 600158.29 94.75 100.00 328469- 223081 222 263387.98 70.89 100.00 222487- 166290 222 193385.04 49.75 100.00 166253- 132210 222 149989.31 36.24 100.00 132179- 101206 222 117013.51 30.87 100.00 101091- 6080 222 55223.58 20.34 100.00 6075- 3651 222 4673.09 5.08 84.68 3645- 528 222 2683.46 3.11 41.44 ------------------------------------------------------------------------------------ 7158651- 528 2220 513585.82 55.75 92.61 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 222 808462.20 89.27 100.00 1.39- 1.12 222 916732.42 75.48 98.20 1.12- 0.96 222 575996.66 70.59 98.65 0.96- 0.88 222 500373.74 61.03 95.50 0.88- 0.81 222 655805.64 69.64 97.30 0.81- 0.73 222 368504.89 42.90 93.24 0.73- 0.71 222 258988.71 34.96 90.54 0.71- 0.65 222 531262.73 52.56 95.05 0.65- 0.62 222 261724.90 30.35 77.03 0.62- 0.58 222 258006.35 30.69 80.63 ------------------------------------------------------------------------------------ 4.82- 0.58 2220 513585.82 55.75 92.61 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:39:25 2018 Sorting 2220 observations 85 unique observations with > 7.00 F2/sig(F2) 2220 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 74 389 Total number of frames 389 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2220 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 14 79 Total number of frames 79 1789 observations > 7.00 F2/sig(F2) 1789 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 14 79 Total number of frames 79 Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 1789 removed 5 = 1784, unique = 89) 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 1784 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 14 79 Total number of frames 79 89 unique data precomputed (should be 89) 89 unique data with 1784 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 1784 removed 0 = 1784, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 1784 observations RMS deviation of equivalent data = 0.22453 Rint = 0.17218 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16959, wR= 0.22671 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08624, wR= 0.11431, Acormin=0.641, Acormax=1.425, Acor_av=0.913 F test: Probability=1.000, F= 3.855 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08524, wR= 0.10507, Acormin=0.601, Acormax=1.369, Acor_av=0.876 F test: Probability=0.671, F= 1.022 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07075, wR= 0.09879, Acormin=0.635, Acormax=1.519, Acor_av=0.875 F test: Probability=1.000, F= 1.478 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06587, wR= 0.08671, Acormin=0.598, Acormax=1.485, Acor_av=0.868 F test: Probability=0.998, F= 1.152 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06088, wR= 0.08164, Acormin=0.505, Acormax=1.338, Acor_av=0.788 F test: Probability=0.999, F= 1.166 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06495, wR= 0.09061, Acormin=0.629, Acormax=1.498, Acor_av=0.867 F test: Probability=0.000, F= 0.877 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06050, wR= 0.08047, Acormin=0.582, Acormax=1.522, Acor_av=0.855 F test: Probability=0.574, F= 1.009 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05615, wR= 0.07421, Acormin=0.494, Acormax=1.390, Acor_av=0.778 F test: Probability=0.999, F= 1.167 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04539, wR= 0.06325, Acormin=0.415, Acormax=1.272, Acor_av=0.690 F test: Probability=1.000, F= 1.520 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06007, wR= 0.07778, Acormin=0.436, Acormax=1.340, Acor_av=0.776 F test: Probability=0.000, F= 0.572 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05637, wR= 0.07173, Acormin=0.520, Acormax=1.450, Acor_av=0.809 F test: Probability=0.000, F= 0.649 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04781, wR= 0.06170, Acormin=0.288, Acormax=0.839, Acor_av=0.459 F test: Probability=0.000, F= 0.898 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04039, wR= 0.05236, Acormin=0.322, Acormax=0.975, Acor_av=0.531 F test: Probability=1.000, F= 1.250 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03847, wR= 0.04992, Acormin=0.331, Acormax=1.024, Acor_av=0.556 F test: Probability=1.000, F= 1.366 Final absorption model (ne=8, no=7): Rint= 0.03847, Acormin=0.331, Acormax=1.024, Acor_av=0.556 Combined refinement in use Rint: 0.17229 There are 79 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: 8, max odd order: 7 (80 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22453 Using Levenberg-Marquardt: 0.00010 New wR= 0.04397 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17218 with corrections 0.03269 Rint for all data: 0.17229 with corrections 0.03290 0 observations identified as outliers and rejected Cycle 2 wR= 0.04397 Using Levenberg-Marquardt: 0.00001 New wR= 0.03901 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17218 with corrections 0.02994 Rint for all data: 0.17229 with corrections 0.03015 1 observations identified as outliers and rejected Cycle 3 wR= 0.03902 Using Levenberg-Marquardt: 0.00000 New wR= 0.03868 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17232 with corrections 0.02962 Rint for all data: 0.17229 with corrections 0.02985 0 observations identified as outliers and rejected Cycle 4 wR= 0.03868 Using Levenberg-Marquardt: 0.00000 New wR= 0.03849 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17232 with corrections 0.02950 Rint for all data: 0.17229 with corrections 0.02973 0 observations identified as outliers and rejected Cycle 5 wR= 0.03849 Using Levenberg-Marquardt: 0.00000 New wR= 0.03837 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17232 with corrections 0.02942 Rint for all data: 0.17229 with corrections 0.02965 0 observations identified as outliers and rejected Final wR= 0.03837 Final frame scales: Min= 0.9431 Max= 1.1086 Final absorption correction factors: Amin= 0.4348 Amax= 1.4079 PROFFIT INFO: Inet (after scale3 abspack): min=548.6063 max=5833655.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=166.1111 max=69791.4688 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2220 reflections read from tmp file 235 reflections are rejected (234 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 1 2 4 6 3 4 2 81 Initial Chi^2= 0.29804 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.52901 Current error model SIG(F2)^2 = 110.94*I_RAW + 0.00*I_BACK+(0.00615*)^2 Cycle 2, Chi^2= 1.10858 Current error model SIG(F2)^2 = 61.50*I_RAW + 0.00*I_BACK+(0.02103*)^2 Cycle 3, Chi^2= 1.00740 Current error model SIG(F2)^2 = 87.42*I_RAW + 0.00*I_BACK+(0.01689*)^2 Cycle 4, Chi^2= 1.00018 Current error model SIG(F2)^2 = 82.93*I_RAW + 0.00*I_BACK+(0.01806*)^2 Cycle 5, Chi^2= 1.00010 Current error model SIG(F2)^2 = 84.29*I_RAW + 0.00*I_BACK+(0.01775*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 83.94*I_RAW + 0.00*I_BACK+(0.01783*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 84.04*I_RAW + 0.00*I_BACK+(0.01781*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 84.04*I_RAW + 0.00*I_BACK+(0.01781*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5833656- 1579185 222 2339647.07 51.97 100.00 1566370- 1018534 222 1244896.94 44.97 100.00 1017974- 332313 222 606716.91 43.31 100.00 328022- 204461 222 249531.39 36.46 100.00 204325- 173370 222 187984.84 29.52 100.00 173128- 129672 222 143655.77 23.48 100.00 129650- 102868 222 116525.68 20.50 100.00 102760- 5686 222 57894.24 14.98 100.00 5657- 3524 222 4388.94 5.17 99.55 3512- 549 222 2706.17 4.03 82.88 ------------------------------------------------------------------------------------ 5833656- 549 2220 495394.80 27.44 98.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 222 824977.45 41.11 100.00 1.39- 1.12 222 911817.26 34.69 100.00 1.12- 0.96 222 537528.56 31.20 100.00 0.96- 0.88 222 481260.43 28.00 99.55 0.88- 0.81 222 620822.45 31.97 100.00 0.81- 0.73 222 345017.78 22.50 99.10 0.73- 0.71 222 249414.39 20.62 98.20 0.71- 0.65 222 493590.10 27.41 99.55 0.65- 0.62 222 249151.59 18.13 92.34 0.62- 0.58 222 240367.93 18.76 93.69 ------------------------------------------------------------------------------------ 4.82- 0.58 2220 495394.80 27.44 98.24 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 222 824977.45 41.11 100.00 4.82- 1.12 444 868397.36 37.90 100.00 4.82- 0.96 666 758107.76 35.67 100.00 4.82- 0.88 888 688895.93 33.75 99.89 4.82- 0.81 1110 675281.23 33.39 99.91 4.82- 0.73 1332 620237.32 31.58 99.77 4.82- 0.71 1554 567262.62 30.01 99.55 4.82- 0.65 1776 558053.55 29.69 99.55 4.82- 0.62 1998 523731.11 28.40 98.75 4.82- 0.58 2220 495394.80 27.44 98.24 ------------------------------------------------------------------------------------ 4.82- 0.58 2220 495394.80 27.44 98.24 Scale applied to data: s=0.171419 (maximum obs:5833655.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.024: data 2220 -> merged 109 With outlier rejection... Rint 0.028; Rsigma 0.024: data 2208 -> merged 109 Rejected total: 12, method kkm 12, method Blessing 0 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585849, 4.831036 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 12.30 100.00 123 1.61 - 1.21 10 10 20.10 100.00 201 1.17 - 1.01 10 10 26.70 100.00 267 0.99 - 0.89 10 10 26.20 100.00 262 0.88 - 0.81 10 10 24.70 100.00 247 0.81 - 0.74 10 10 22.10 100.00 221 0.73 - 0.71 10 10 23.70 100.00 237 0.70 - 0.66 10 10 19.50 100.00 195 0.66 - 0.64 10 10 18.90 100.00 189 0.63 - 0.60 10 10 18.90 100.00 189 --------------------------------------------------------------- 5.91 - 0.60 100 100 21.31 100.00 2131 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:39:25 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919940 5.915868 5.912670 60.0634 90.0888 60.0060 2087 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1029 1100 1019 1058 1574 1400 1382 2087 N (int>3sigma) = 0 850 1100 840 873 1395 1202 1172 1774 Mean intensity = 0.0 52.7 24.9 53.3 59.1 43.2 61.0 59.6 60.2 Mean int/sigma = 0.0 25.5 22.8 25.7 26.8 24.6 27.2 27.2 27.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.913 5.916 90.06 119.94 119.94 Niggli form: a.a = 34.960 b.b = 34.968 c.c = 34.997 b.c = -0.034 a.c = -17.456 a.b = -17.450 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.155 [ 1932] Vol = 585.8 Cell: 8.369 8.373 8.360 90.07 89.98 90.01 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.093 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 1661] Vol = 439.4 Cell: 5.918 5.913 14.502 90.02 90.05 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.093 RHOMBOHEDRAL R-lattice R(int) = 0.143 [ 521] Vol = 439.4 Trigonal Cell: 5.918 5.913 14.502 90.02 90.05 120.04 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.041 TETRAGONAL I-lattice R(int) = 0.136 [ 1692] Vol = 292.9 Cell: 5.920 5.918 8.360 89.97 89.93 89.97 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.095 TETRAGONAL I-lattice R(int) = 0.136 [ 1692] Vol = 292.9 Cell: 5.918 5.920 8.360 90.07 90.03 89.97 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.050 ORTHORHOMBIC I-lattice R(int) = 0.136 [ 1639] Vol = 292.9 Cell: 5.918 5.920 8.360 89.93 89.97 89.97 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.049 ORTHORHOMBIC I-lattice R(int) = 0.135 [ 1643] Vol = 292.9 Cell: 5.913 8.369 5.920 89.97 89.91 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.130 [ 1331] Vol = 292.9 Cell: 5.920 5.918 8.360 90.03 90.07 89.97 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.090 MONOCLINIC I-lattice R(int) = 0.127 [ 1330] Vol = 292.9 Cell: 5.913 5.920 8.369 90.03 90.01 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.031 MONOCLINIC I-lattice R(int) = 0.122 [ 1351] Vol = 292.9 Cell: 5.913 8.369 5.920 89.97 90.09 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.039 MONOCLINIC I-lattice R(int) = 0.124 [ 1350] Vol = 292.9 Cell: 5.920 5.913 8.369 89.99 90.03 89.91 Volume: 292.92 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.130 [ 1336] Vol = 292.9 Cell: 10.247 5.913 5.916 90.06 125.20 89.94 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 874] Vol = 146.5 Cell: 5.913 5.913 5.916 90.06 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1100 0 1390 1400 2087 N (int>3sigma) = 0 0 0 0 1100 0 1184 1202 1774 Mean intensity = 0.0 0.0 0.0 0.0 24.9 0.0 60.2 61.0 60.2 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 27.6 27.2 27.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.177 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 162 489 N I>3s 12 12 80 489 0.7 0.7 0.5 29.2 6.4 6.4 3.7 27.9 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 0.155 1790 Fd-3m 1 1 227 C N N N N 37 2284 0.155 1828 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368593 8.373402 8.360434 90.0704 89.9755 90.0145 ZERR 1.00 0.002974 0.001780 0.000303 0.0002 0.0115 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5778875- 932233 490 486 27 18.0 1709608.50 47.66 0.026 0.034 895279- 163089 657 653 27 24.2 292070.14 35.62 0.029 0.035 149012- 54223 549 547 27 20.3 115638.67 20.63 0.045 0.060 23069- 1760 524 522 28 18.6 4720.37 5.24 0.146 0.176 ------------------------------------------------------------------------------------------- 5778875- 1760 2220 2208 109 20.3 492441.08 27.37 0.028 0.035 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 546 542 27 20.1 781672.16 37.43 0.026 0.034 0.020 1.01-0.78 657 656 27 24.3 502175.17 27.80 0.023 0.030 0.023 0.78-0.65 629 626 29 21.6 365711.43 22.47 0.031 0.039 0.027 0.65-0.59 388 384 26 14.8 274170.13 20.44 0.037 0.044 0.032 ------------------------------------------------------------------------------------------------------ inf-0.59 2220 2208 109 20.3 492441.08 27.37 0.028 0.035 0.024 inf-0.60 2138 2129 99 21.5 503644.25 27.73 0.027 0.035 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 542 27 27 100.0 20.1 781672.16 190.70 0.026 0.008 1.01-0.78 656 27 27 100.0 24.3 502175.17 147.35 0.023 0.005 0.78-0.65 626 29 29 100.0 21.6 365711.43 111.04 0.031 0.007 0.65-0.59 384 27 26 96.3 14.8 274170.13 90.32 0.037 0.010 -------------------------------------------------------------------------------------------- inf-0.59 2208 110 109 99.1 20.3 492441.08 137.78 0.028 0.007 inf-0.60 2129 99 99 100.0 21.5 503644.25 140.65 0.027 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:44:32 2018) ID: 2932; threads 39; handles 879; mem 520476.00 (1237724.00)kB; time: 1w 5d 22h 50m 3s MEMORY INFO: Memory PF:0.0, Ph:168.0, V:1208.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:508.3,peak PF: 708.5, WS: 272.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:168.0, V:1210.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:510.1,peak PF: 708.5, WS: 273.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:44:32 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000012 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000013 0.000014 0.000013 ) 5.91535 ( 0.00075 ) 5.92288 ( 0.00057 ) 5.91286 ( 0.00073 ) 59.95509 ( 0.01140 ) 89.89521 ( 0.01010 ) 59.99590 ( 0.01157 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:44:32 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000011 0.000012 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000013 0.000014 0.000013 ) M - matrix: 0.021549 -0.014377 0.007212 ( 0.000004 0.000003 0.000003 ) -0.014377 0.028735 -0.014370 ( 0.000003 0.000004 0.000003 ) 0.007212 -0.014370 0.021577 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9154(7) 5.9229(6) 5.9129(7) 59.955(11) 89.895(10) 59.996(12) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 454 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.088 ( 0.083) | 1.214 ( 0.403) | 1.097 ( 0.492) | 1.12- 0.97 | 45 | 1.118 ( 0.084) | 1.148 ( 0.105) | 1.267 ( 0.491) | 0.97- 0.88 | 45 | 1.152 ( 0.075) | 1.173 ( 0.115) | 1.162 ( 0.451) | 0.87- 0.81 | 45 | 1.169 ( 0.076) | 1.151 ( 0.128) | 1.274 ( 0.407) | 0.81- 0.73 | 45 | 1.183 ( 0.066) | 1.150 ( 0.125) | 1.117 ( 0.367) | 0.73- 0.70 | 45 | 1.199 ( 0.068) | 1.210 ( 0.152) | 1.176 ( 0.383) | 0.70- 0.66 | 45 | 1.204 ( 0.060) | 1.197 ( 0.170) | 1.215 ( 0.426) | 0.66- 0.62 | 45 | 1.232 ( 0.079) | 1.190 ( 0.164) | 1.203 ( 0.454) | 0.62- 0.59 | 45 | 1.215 ( 0.093) | 1.220 ( 0.224) | 1.259 ( 0.505) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 450 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.201 ( 0.490) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087376 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055237 -0.024246 0.122372 ( 0.000022 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000007 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.997(19) 59.96(2) V = 147.15(5) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087385 -0.167043 0.063671 ( 0.000018 0.000023 0.000020 ) 0.055392 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021531 ( 0.000004 0.000005 0.000006 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.008(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087385 -0.167043 0.063671 ( 0.000018 0.000023 0.000020 ) 0.055392 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021531 ( 0.000004 0.000005 0.000006 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.008(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.060) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.457) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.347 ( 0.571) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb PROFFITPEAK info: 1220 peaks in the peak location table UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 1 575 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 178 | 1.155 ( 0.133) | 1.272 ( 0.432) | 1.358 ( 0.705) | 13.1-19.0 | 178 | 1.145 ( 0.113) | 1.199 ( 0.298) | 1.328 ( 0.682) | 19.0-23.1 | 178 | 1.154 ( 0.095) | 1.215 ( 0.314) | 1.258 ( 0.653) | 23.1-27.3 | 178 | 1.135 ( 0.098) | 1.173 ( 0.306) | 1.202 ( 0.505) | 27.3-30.5 | 178 | 1.145 ( 0.102) | 1.170 ( 0.205) | 1.215 ( 0.455) | 30.5-33.9 | 178 | 1.156 ( 0.092) | 1.151 ( 0.215) | 1.223 ( 0.446) | 33.9-37.2 | 178 | 1.139 ( 0.111) | 1.111 ( 0.165) | 1.156 ( 0.417) | 37.2-39.9 | 178 | 1.159 ( 0.118) | 1.124 ( 0.243) | 1.264 ( 0.535) | 39.9-42.8 | 178 | 1.171 ( 0.111) | 1.117 ( 0.192) | 1.225 ( 0.569) | 42.9-50.0 | 176 | 1.201 ( 0.168) | 1.133 ( 0.291) | 1.179 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 1778 | 1.156 ( 0.117) | 1.167 ( 0.281) | 1.241 ( 0.556) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0022 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 461776 lp-corr: 681854 Maximum peak integral for reflections I/sig<= 10000 - raw: 20148380 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:44:50 2018 PROFFITMAIN - Started at Wed Mar 28 13:44:50 2018 OTKP changes: 1778 2 3 4 OTKP changes: 1778 2 3 4 UB - matrix: -0.104246 -0.015009 0.049496 ( 0.000013 0.000014 0.000013 ) 0.087381 -0.167253 0.063728 ( 0.000010 0.000011 0.000010 ) 0.055405 -0.024364 0.122930 ( 0.000013 0.000014 0.000013 ) M - matrix: 0.021572 -0.014400 0.007220 ( 0.000004 0.000003 0.000003 ) -0.014400 0.028792 -0.014397 ( 0.000003 0.000004 0.000003 ) 0.007220 -0.014397 0.021623 ( 0.000003 0.000003 0.000004 ) UB fit with 1778 obs out of 1778 (total:1778,skipped:0) (100.00%) unit cell: 5.9169(7) 5.9099(5) 5.9058(7) 60.067(11) 90.078(10) 59.997(11) V = 146.07(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104118 -0.015206 0.049830 ( 0.000025 0.000032 0.000028 ) 0.087319 -0.167076 0.063631 ( 0.000017 0.000022 0.000019 ) 0.055393 -0.024079 0.122517 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021534 -0.014340 0.007155 ( 0.000006 0.000005 0.000005 ) -0.014340 0.028725 -0.014339 ( 0.000005 0.000007 0.000005 ) 0.007155 -0.014339 0.021542 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9159(14) 5.9122(10) 5.9140(13) 60.04(2) 89.987(19) 60.03(2) V = 146.42(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104489 -0.014343 0.049132 ( 0.000035 0.000044 0.000038 ) 0.087130 -0.167069 0.063756 ( 0.000025 0.000031 0.000027 ) 0.055261 -0.024924 0.122918 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021563 -0.014435 0.007214 ( 0.000009 0.000007 0.000006 ) -0.014435 0.028739 -0.014420 ( 0.000007 0.000011 0.000007 ) 0.007214 -0.014420 0.021588 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9289(19) 5.9360(14) 5.9206(16) 59.90(3) 89.88(2) 59.82(3) V = 146.87(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007255 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007255 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146804 -0.097925 0.049160 ( 0.000021 0.000026 0.000023 ) -0.000020 0.138450 -0.069288 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000033 0.119949 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021551 -0.014379 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028758 -0.014403 ( 0.000005 0.000009 0.000006 ) 0.007216 -0.014403 0.021605 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9186(10) 5.9163(14) 5.9125(14) 60.00(2) 90.057(17) 60.02(2) V = 146.37(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104306 -0.014976 0.049283 ( 0.000024 0.000019 0.000017 ) 0.087254 -0.167271 0.063708 ( 0.000028 0.000023 0.000020 ) 0.055329 -0.024506 0.122974 ( 0.000022 0.000018 0.000016 ) M - matrix: 0.021554 -0.014389 0.007222 ( 0.000007 0.000006 0.000004 ) -0.014389 0.028805 -0.014408 ( 0.000006 0.000008 0.000004 ) 0.007222 -0.014408 0.021610 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9177(12) 5.9089(10) 5.9102(10) 60.036(17) 90.099(14) 60.038(19) V = 146.17(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104194 -0.014998 0.049413 ( 0.000013 0.000014 0.000013 ) 0.087319 -0.167103 0.063702 ( 0.000010 0.000011 0.000010 ) 0.055345 -0.024320 0.122791 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021544 -0.014375 0.007210 ( 0.000004 0.000003 0.000002 ) -0.014375 0.028740 -0.014372 ( 0.000003 0.000004 0.000003 ) 0.007210 -0.014372 0.021577 ( 0.000002 0.000003 0.000003 ) UB fit with 1778 obs out of 1778 (total:1778,skipped:0) (100.00%) unit cell: 5.9202(7) 5.9153(5) 5.9129(7) 60.057(11) 90.085(9) 60.011(11) V = 146.46(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 41 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof 2365 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:44:55 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22689244.0000 PROFFIT INFO: signal sum lp corr: min=241.7850 max=3288195.3159 PROFFIT INFO: background sum: min=808.0000 max=15868.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=59 max=886 PROFFIT INFO: Inet: min=527.5309 max=7174244.5000 PROFFIT INFO: sig(Inet): min=190.6879 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=303.85 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 51 177 307 485 534 942 1563 2132 2364 Percent 0.0 0.1 2.2 7.5 13.0 20.5 22.6 39.8 66.1 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2365 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 2365 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7174245- 1632439 236 2463852.65 134.81 100.00 1630969- 1052456 236 1314996.50 111.15 100.00 1052066- 330111 236 609507.85 94.30 100.00 329873- 221710 236 262816.58 70.71 100.00 221552- 167049 236 193436.73 50.10 100.00 166681- 132434 236 150074.77 36.27 100.00 132403- 102464 236 117571.02 30.80 100.00 102316- 6327 236 58074.77 21.00 100.00 6302- 3651 236 4703.80 5.08 84.75 3645- 528 240 2687.30 3.10 41.25 ------------------------------------------------------------------------------------ 7174245- 528 2364 516900.65 55.64 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 879669.24 85.84 99.58 1.28- 1.03 236 640621.43 63.74 97.46 1.03- 0.90 236 618480.34 67.43 95.76 0.90- 0.81 236 468538.21 53.59 95.34 0.81- 0.72 236 614969.97 65.94 92.80 0.72- 0.67 236 475806.54 55.97 91.95 0.67- 0.61 236 329117.06 40.23 88.14 0.61- 0.55 236 424259.14 46.39 93.64 0.55- 0.49 236 368244.13 40.25 84.32 0.49- 0.40 240 352093.78 37.35 86.25 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 516900.65 55.64 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:44:55 2018 Sorting 2364 observations 278 unique observations with > 7.00 F2/sig(F2) 2364 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 Total number of frames 413 Maximum number of 278 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2364 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 1906 observations > 7.00 F2/sig(F2) 1906 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 Removing 'redundancy=1' reflections Average redundancy: 6.8 (Out of 1906 removed 27 = 1879, unique = 277) 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 1879 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 277 unique data precomputed (should be 277) 277 unique data with 1879 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.8 (Out of 1879 removed 0 = 1879, unique = 277) 277 unique data precomputed (should be 277) 277 unique data with 1879 observations RMS deviation of equivalent data = 0.73255 Rint = 0.68800 11 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66697, wR= 3.34689 Trying model 1 (ne=2, no=0)... Results: Rint= 0.74343, wR= 2.69298, Acormin=-0.363, Acormax=2.632, Acor_av=0.572 F test: Probability=0.000, F= 0.802 Trying model 2 (ne=2, no=1)... Results: Rint= 0.80038, wR= 2.19850, Acormin=-0.341, Acormax=2.478, Acor_av=0.413 F test: Probability=0.000, F= 0.691 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75496, wR= 2.07382, Acormin=-0.219, Acormax=2.865, Acor_av=0.510 F test: Probability=0.000, F= 0.774 Trying model 4 (ne=4, no=1)... Results: Rint= 0.83383, wR= 2.28638, Acormin=-0.351, Acormax=2.183, Acor_av=0.388 F test: Probability=0.000, F= 0.633 Trying model 5 (ne=4, no=3)... Results: Rint= 0.91667, wR= 2.16159, Acormin=-0.435, Acormax=3.322, Acor_av=0.140 F test: Probability=0.000, F= 0.521 Trying model 6 (ne=6, no=0)... Results: Rint= 0.74945, wR= 2.38070, Acormin=-0.468, Acormax=3.280, Acor_av=0.467 F test: Probability=0.000, F= 0.779 Trying model 7 (ne=6, no=1)... Results: Rint= 0.84185, wR= 2.37756, Acormin=-0.477, Acormax=2.770, Acor_av=0.344 F test: Probability=0.000, F= 0.616 Trying model 8 (ne=6, no=3)... Results: Rint= 0.93004, wR= 1.70474, Acormin=-0.780, Acormax=3.364, Acor_av=0.123 F test: Probability=0.000, F= 0.502 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96400, wR= 1.40772, Acormin=-0.559, Acormax=2.910, Acor_av=0.075 F test: Probability=0.000, F= 0.464 Trying model 10 (ne=8, no=0)... Results: Rint= 0.83925, wR= 1.95335, Acormin=-0.792, Acormax=1.786, Acor_av=0.262 F test: Probability=0.000, F= 0.614 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87809, wR= 2.51438, Acormin=-0.633, Acormax=1.572, Acor_av=0.186 F test: Probability=0.000, F= 0.560 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98885, wR= 2.03521, Acormin=-0.061, Acormax=0.075, Acor_av=0.002 F test: Probability=0.000, F= 0.440 Trying model 13 (ne=8, no=5)... Results: Rint= 1.00155, wR= 1.85062, Acormin=-0.057, Acormax=0.066, Acor_av=0.001 F test: Probability=0.000, F= 0.425 Trying model 14 (ne=8, no=7)... Results: Rint= 1.01183, wR= 2.04376, Acormin=-0.075, Acormax=0.079, Acor_av=0.000 F test: Probability=0.000, F= 0.413 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86731 There are 209 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 213 pars with 22791 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.73255 Using Levenberg-Marquardt: 0.00010 New wR= 0.71411 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68800 with corrections 0.68062 Rint for all data: 0.86731 with corrections 0.86845 9 observations identified as outliers and rejected Cycle 2 wR= 0.67332 Using Levenberg-Marquardt: 0.00001 New wR= 0.67167 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66949 with corrections 0.65605 Rint for all data: 0.86731 with corrections 0.86626 8 observations identified as outliers and rejected Cycle 3 wR= 0.65062 Using Levenberg-Marquardt: 0.00000 New wR= 0.64918 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65963 with corrections 0.64866 Rint for all data: 0.86731 with corrections 0.86896 13 observations identified as outliers and rejected Cycle 4 wR= 0.62718 Using Levenberg-Marquardt: 0.00000 New wR= 0.62491 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65114 with corrections 0.64287 Rint for all data: 0.86731 with corrections 0.86953 8 observations identified as outliers and rejected Cycle 5 wR= 0.59493 Using Levenberg-Marquardt: 0.00000 New wR= 0.59373 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64948 with corrections 0.63576 Rint for all data: 0.86731 with corrections 0.86405 1 observations identified as outliers and rejected Final wR= 0.59373 Final frame scales: Min= 1.0000 Max= 4.4357 Final absorption correction factors: Amin= 0.5851 Amax= 1.5160 PROFFIT INFO: Inet (after scale3 abspack): min=488.4832 max=7456964.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=188.3117 max=94621.1328 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2364 reflections read from tmp file 1750 reflections are rejected (1687 as outliers, 63 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 87 53 33 14 5 2 2 1 1 Initial Chi^2= 0.57504 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.07504 Current error model SIG(F2)^2 = 256.70*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 275.96*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 275.96*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7456965- 1528878 236 2438182.06 83.03 100.00 1528865- 990020 236 1224713.18 44.88 100.00 986992- 316552 236 608393.79 39.46 100.00 315968- 209989 236 257239.21 29.42 100.00 209979- 161154 236 182290.46 19.27 100.00 160976- 127377 236 143489.51 15.47 100.00 127281- 98073 236 113370.04 12.63 100.00 98009- 6286 236 57233.09 9.19 94.92 6223- 3405 236 4469.28 2.91 29.66 3401- 488 240 2561.17 2.28 12.50 ------------------------------------------------------------------------------------ 7456965- 488 2364 502347.08 25.81 83.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 1002837.66 54.56 96.61 1.28- 1.03 236 635693.72 33.84 89.83 1.03- 0.90 236 624434.60 31.07 87.71 0.90- 0.81 236 479606.74 23.32 82.63 0.81- 0.72 236 570864.87 26.83 85.17 0.72- 0.67 236 443635.03 22.37 82.63 0.67- 0.61 236 295522.91 16.29 74.58 0.61- 0.55 236 384698.07 18.63 83.47 0.55- 0.49 236 309271.13 16.27 77.12 0.49- 0.40 240 280663.48 15.13 76.25 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 502347.08 25.81 83.59 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 1002837.66 54.56 96.61 5.26- 1.03 472 819265.69 44.20 93.22 5.26- 0.90 708 754321.99 39.82 91.38 5.26- 0.81 944 685643.18 35.70 89.19 5.26- 0.72 1180 662687.52 33.92 88.39 5.26- 0.67 1416 626178.77 32.00 87.43 5.26- 0.61 1652 578942.22 29.75 85.59 5.26- 0.55 1888 554661.70 28.36 85.33 5.26- 0.49 2124 527396.08 27.02 84.42 5.26- 0.40 2364 502347.08 25.81 83.59 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 502347.08 25.81 83.59 Scale applied to data: s=0.134103 (maximum obs:7456964.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.864; Rsigma 0.025: data 2364 -> merged 317 With outlier rejection... Rint 0.800; Rsigma 0.025: data 2236 -> merged 317 Rejected total: 128, method kkm 118, method Blessing 10 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404281, 5.271185 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 10.87 100.00 163 1.46 - 1.12 15 15 15.13 100.00 227 1.08 - 0.96 15 15 14.13 100.00 212 0.96 - 0.86 15 15 14.20 100.00 213 0.86 - 0.79 15 15 11.40 100.00 171 0.79 - 0.73 15 15 9.20 100.00 138 0.73 - 0.69 15 15 8.67 100.00 130 0.69 - 0.65 15 15 9.20 100.00 138 0.65 - 0.63 15 15 5.67 100.00 85 0.63 - 0.60 21 21 6.76 100.00 142 --------------------------------------------------------------- 5.91 - 0.60 156 156 10.38 100.00 1619 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:44:55 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920195 5.915315 5.912900 60.0574 90.0849 60.0108 2236 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.45 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1106 1180 1100 1134 1693 1502 1489 2236 N (int>3sigma) = 0 892 1180 886 919 1479 1268 1244 1871 Mean intensity = 0.0 56.3 26.1 56.7 64.1 45.9 64.0 63.3 63.6 Mean int/sigma = 0.0 23.8 21.0 24.0 25.2 22.9 25.4 25.4 25.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.914 5.915 90.05 119.94 119.94 Niggli form: a.a = 34.962 b.b = 34.974 c.c = 34.991 b.c = -0.029 a.c = -17.458 a.b = -17.453 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.103 CUBIC F-lattice R(int) = 0.166 [ 2081] Vol = 585.8 Cell: 8.368 8.373 8.361 90.07 89.99 90.00 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1809] Vol = 439.4 Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 567] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.035 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 89.96 89.94 89.96 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.085 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 90.06 90.04 89.96 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.044 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1787] Vol = 292.9 Cell: 5.919 5.919 8.361 89.94 89.96 89.96 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 1789] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 89.92 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.131 [ 1466] Vol = 292.9 Cell: 5.919 5.919 8.361 90.04 90.06 89.96 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.076 MONOCLINIC I-lattice R(int) = 0.133 [ 1470] Vol = 292.9 Cell: 5.913 5.920 8.368 90.01 90.01 90.08 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.018 MONOCLINIC I-lattice R(int) = 0.130 [ 1493] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 90.08 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.037 MONOCLINIC I-lattice R(int) = 0.130 [ 1480] Vol = 292.9 Cell: 8.368 5.913 5.920 90.08 90.01 90.01 Volume: 292.92 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.142 [ 1474] Vol = 292.9 Cell: 10.248 5.914 5.915 90.05 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.109 [ 960] Vol = 146.5 Cell: 5.913 5.914 5.915 90.05 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1180 0 1491 1502 2236 N (int>3sigma) = 0 0 0 0 1180 0 1254 1268 1871 Mean intensity = 0.0 0.0 0.0 0.0 26.1 0.0 63.5 64.0 63.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 25.6 25.4 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 172 521 N I>3s 11 11 70 521 0.7 0.7 0.6 30.5 6.0 6.0 3.4 25.6 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 0.166 1929 Fd-3m 1 1 227 C N N N N 37 2284 0.166 1967 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367943 8.373460 8.361062 90.0706 89.9861 90.0050 ZERR 1.00 0.002752 0.001657 0.000282 0.0002 0.0106 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3965422- 951793 257 234 31 7.5 1387924.05 55.77 0.588 0.468 928567- 675666 305 300 31 9.7 786205.85 34.77 0.954 0.866 667583- 558041 254 245 31 7.9 598487.45 28.68 0.901 0.842 541045- 449522 321 314 31 10.1 473179.95 28.35 0.976 1.097 448256- 346202 252 231 31 7.5 334288.56 22.28 0.927 1.007 345590- 252350 266 236 31 7.6 226720.04 17.79 0.822 0.956 246637- 126570 215 202 31 6.5 157030.90 16.13 0.545 0.487 126312- 101272 175 170 31 5.5 115603.24 12.92 0.408 0.292 100377- 74998 179 168 31 5.4 91801.22 10.70 0.508 0.362 72575- 1115 140 136 38 3.6 47938.23 6.57 0.748 0.730 ------------------------------------------------------------------------------------------- 3965422- 1115 2364 2236 317 7.1 474009.61 25.45 0.800 0.735 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 436 414 31 13.4 790103.53 45.49 0.800 0.792 0.015 1.05-0.83 441 430 32 13.4 569209.89 28.08 0.926 1.000 0.023 0.82-0.72 331 316 32 9.9 461412.54 23.90 0.744 0.769 0.028 0.72-0.65 283 269 32 8.4 350363.70 19.65 0.871 0.946 0.032 0.64-0.60 219 205 31 6.6 392480.47 19.29 0.770 0.862 0.033 0.59-0.56 199 184 33 5.6 292160.45 15.91 0.743 0.677 0.040 0.55-0.52 152 143 31 4.6 348948.95 17.55 0.802 0.724 0.036 0.51-0.49 115 106 31 3.4 207488.24 12.95 0.477 0.319 0.045 0.49-0.46 113 100 32 3.1 245235.03 14.13 0.459 0.317 0.044 0.45-0.40 75 69 32 2.2 251234.86 14.23 0.198 0.146 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 2364 2236 317 7.1 474009.61 25.45 0.800 0.735 0.025 inf-0.60 1691 1619 156 10.4 549845.46 29.33 0.831 0.864 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 414 31 31 100.0 13.4 790103.53 184.56 0.800 0.006 1.05-0.83 430 32 32 100.0 13.4 569209.89 126.41 0.926 0.008 0.82-0.72 316 32 32 100.0 9.9 461412.54 88.76 0.744 0.012 0.72-0.65 269 32 32 100.0 8.4 350363.70 74.20 0.871 0.014 0.64-0.60 205 31 31 100.0 6.6 392480.47 64.02 0.770 0.017 0.59-0.56 184 38 33 86.8 5.6 292160.45 47.27 0.743 0.021 0.55-0.52 143 37 31 83.8 4.6 348948.95 47.69 0.802 0.021 0.51-0.49 106 41 31 75.6 3.4 207488.24 28.40 0.477 0.025 0.49-0.46 100 58 32 55.2 3.1 245235.03 28.99 0.459 0.027 0.45-0.40 69 128 32 25.0 2.2 251234.86 23.72 0.198 0.030 -------------------------------------------------------------------------------------------- inf-0.40 2236 464 317 68.3 7.1 474009.61 96.14 0.800 0.014 inf-0.60 1619 156 156 100.0 10.4 549845.46 118.16 0.831 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007499 0.076802 -0.034889 ( 0.000007 0.000007 0.000007 ) -0.083550 -0.011809 -0.008041 ( 0.000005 0.000005 0.000005 ) -0.012160 0.033722 0.076908 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007185 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007175 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000009 0.007197 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007499 0.076802 -0.034889 ( 0.000007 0.000007 0.000007 ) -0.083550 -0.011809 -0.008041 ( 0.000005 0.000005 0.000005 ) -0.012160 0.033722 0.076908 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3681(5) 8.3737(7) 8.3611(6) 90.071(6) 89.986(6) 90.005(6) V = 585.87(7) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.87(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22689244.0000 PROFFIT INFO: signal sum lp corr: min=241.7850 max=3288195.3159 PROFFIT INFO: background sum: min=808.0000 max=15868.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=59 max=886 PROFFIT INFO: Inet: min=527.5309 max=7174244.5000 PROFFIT INFO: sig(Inet): min=190.6879 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=303.85 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 102 354 614 970 1068 1884 3126 4264 4728 Percent 0.0 0.1 2.2 7.5 13.0 20.5 22.6 39.8 66.1 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2365 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 2365 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7174245- 1632439 236 2463852.65 134.81 100.00 1630969- 1052456 236 1314996.50 111.15 100.00 1052066- 330111 236 609507.85 94.30 100.00 329873- 221710 236 262816.58 70.71 100.00 221552- 167049 236 193436.73 50.10 100.00 166681- 132434 236 150074.77 36.27 100.00 132403- 102464 236 117571.02 30.80 100.00 102316- 6327 236 58074.77 21.00 100.00 6302- 3651 236 4703.80 5.08 84.75 3645- 528 240 2687.30 3.10 41.25 ------------------------------------------------------------------------------------ 7174245- 528 2364 516900.65 55.64 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 843717.59 89.08 100.00 1.39- 1.12 236 911104.73 74.81 98.31 1.12- 0.96 236 583928.45 70.61 98.73 0.96- 0.88 236 499802.30 60.66 95.34 0.88- 0.81 236 666671.38 70.63 97.46 0.81- 0.73 236 367156.64 42.53 93.22 0.73- 0.71 236 256119.25 35.16 90.68 0.71- 0.65 236 536378.96 53.03 95.34 0.65- 0.62 236 259868.90 30.14 75.00 0.62- 0.58 240 248802.32 30.22 81.25 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 516900.65 55.64 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:44:56 2018 Sorting 2364 observations 85 unique observations with > 7.00 F2/sig(F2) 2364 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 Total number of frames 413 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2364 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 1906 observations > 7.00 F2/sig(F2) 1906 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 21.4 (Out of 1906 removed 5 = 1901, unique = 89) 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 1901 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 89 unique data precomputed (should be 89) 89 unique data with 1901 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.4 (Out of 1901 removed 0 = 1901, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 1901 observations RMS deviation of equivalent data = 0.21306 Rint = 0.16697 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16422, wR= 0.22023 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08795, wR= 0.11522, Acormin=0.645, Acormax=1.413, Acor_av=0.919 F test: Probability=1.000, F= 3.477 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08403, wR= 0.10512, Acormin=0.603, Acormax=1.359, Acor_av=0.879 F test: Probability=0.971, F= 1.094 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07388, wR= 0.10094, Acormin=0.635, Acormax=1.509, Acor_av=0.877 F test: Probability=1.000, F= 1.289 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06652, wR= 0.08799, Acormin=0.595, Acormax=1.485, Acor_av=0.872 F test: Probability=1.000, F= 1.232 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06468, wR= 0.08550, Acormin=0.510, Acormax=1.343, Acor_av=0.795 F test: Probability=0.864, F= 1.053 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06798, wR= 0.09275, Acormin=0.625, Acormax=1.528, Acor_av=0.869 F test: Probability=0.000, F= 0.952 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06098, wR= 0.08182, Acormin=0.587, Acormax=1.555, Acor_av=0.859 F test: Probability=1.000, F= 1.181 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05865, wR= 0.07769, Acormin=0.492, Acormax=1.419, Acor_av=0.783 F test: Probability=0.941, F= 1.077 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04621, wR= 0.06543, Acormin=0.408, Acormax=1.306, Acor_av=0.685 F test: Probability=1.000, F= 1.724 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06373, wR= 0.08155, Acormin=0.432, Acormax=1.369, Acor_av=0.775 F test: Probability=0.000, F= 0.527 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05761, wR= 0.07427, Acormin=0.521, Acormax=1.484, Acor_av=0.810 F test: Probability=0.000, F= 0.644 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05028, wR= 0.06530, Acormin=0.277, Acormax=0.828, Acor_av=0.446 F test: Probability=0.000, F= 0.842 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04064, wR= 0.05421, Acormin=0.321, Acormax=0.985, Acor_av=0.528 F test: Probability=1.000, F= 1.280 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03840, wR= 0.05087, Acormin=0.337, Acormax=1.067, Acor_av=0.560 F test: Probability=1.000, F= 1.422 Final absorption model (ne=8, no=7): Rint= 0.03840, Acormin=0.337, Acormax=1.067, Acor_av=0.560 Combined refinement in use Rint: 0.16708 There are 84 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: 8, max odd order: 7 (80 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21306 Using Levenberg-Marquardt: 0.00010 New wR= 0.04225 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16697 with corrections 0.03151 Rint for all data: 0.16708 with corrections 0.03172 1 observations identified as outliers and rejected Cycle 2 wR= 0.04038 Using Levenberg-Marquardt: 0.00001 New wR= 0.03779 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16694 with corrections 0.02884 Rint for all data: 0.16708 with corrections 0.02931 1 observations identified as outliers and rejected Cycle 3 wR= 0.03780 Using Levenberg-Marquardt: 0.00000 New wR= 0.03726 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02842 Rint for all data: 0.16708 with corrections 0.02886 0 observations identified as outliers and rejected Cycle 4 wR= 0.03726 Using Levenberg-Marquardt: 0.00000 New wR= 0.03695 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02819 Rint for all data: 0.16708 with corrections 0.02863 0 observations identified as outliers and rejected Cycle 5 wR= 0.03695 Using Levenberg-Marquardt: 0.00000 New wR= 0.03674 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02806 Rint for all data: 0.16708 with corrections 0.02850 0 observations identified as outliers and rejected Final wR= 0.03674 Final frame scales: Min= 0.7898 Max= 1.0980 Final absorption correction factors: Amin= 0.4313 Amax= 1.4040 PROFFIT INFO: Inet (after scale3 abspack): min=552.4300 max=5920658.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=169.9829 max=68531.0625 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2364 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 3 2 2 3 4 6 1 2 84 Initial Chi^2= 0.29553 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.17615 Current error model SIG(F2)^2 = 112.97*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 245.83*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 245.83*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5920658- 1618558 236 2374094.78 90.36 100.00 1604679- 1023273 236 1254629.41 45.24 100.00 1022824- 336998 236 615189.97 44.62 100.00 335967- 204788 236 250237.05 29.80 100.00 204776- 174296 236 188583.24 20.70 100.00 173788- 129589 236 143923.39 15.22 100.00 129512- 103137 236 116663.12 13.05 100.00 103123- 5918 236 60448.34 9.55 96.61 5862- 3523 236 4434.76 3.04 39.41 3520- 552 240 2701.69 2.35 14.17 ------------------------------------------------------------------------------------ 5920658- 552 2364 500247.28 27.35 84.90 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 870968.54 59.60 99.58 1.39- 1.12 236 909386.63 45.33 93.22 1.12- 0.96 236 546627.78 31.44 92.80 0.96- 0.88 236 482843.41 25.70 83.90 0.88- 0.81 236 630606.09 29.71 94.07 0.81- 0.73 236 343260.33 18.23 77.54 0.73- 0.71 236 246902.81 15.14 76.69 0.71- 0.65 236 499312.43 22.41 91.10 0.65- 0.62 236 244886.33 13.09 66.53 0.62- 0.58 240 232221.24 13.08 73.75 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 500247.28 27.35 84.90 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 870968.54 59.60 99.58 4.82- 1.12 472 890177.58 52.46 96.40 4.82- 0.96 708 775660.98 45.45 95.20 4.82- 0.88 944 702456.59 40.52 92.37 4.82- 0.81 1180 688086.49 38.36 92.71 4.82- 0.73 1416 630615.46 35.00 90.18 4.82- 0.71 1652 575799.37 32.17 88.26 4.82- 0.65 1888 566238.50 30.95 88.61 4.82- 0.62 2124 530532.70 28.96 86.16 4.82- 0.58 2364 500247.28 27.35 84.90 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 500247.28 27.35 84.90 Scale applied to data: s=0.168900 (maximum obs:5920658.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.029; Rsigma 0.024: data 2364 -> merged 109 With outlier rejection... Rint 0.025; Rsigma 0.024: data 2351 -> merged 109 Rejected total: 13, method kkm 12, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585850, 4.831042 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 13.10 100.00 131 1.61 - 1.21 10 10 21.10 100.00 211 1.17 - 1.01 10 10 28.20 100.00 282 0.99 - 0.89 10 10 28.20 100.00 282 0.88 - 0.81 10 10 26.30 100.00 263 0.81 - 0.74 10 10 23.50 100.00 235 0.73 - 0.71 10 10 25.20 100.00 252 0.70 - 0.66 10 10 21.20 100.00 212 0.66 - 0.64 10 10 20.10 100.00 201 0.63 - 0.60 10 10 20.20 100.00 202 --------------------------------------------------------------- 5.91 - 0.60 100 100 22.71 100.00 2271 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:44:55 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920195 5.915315 5.912900 60.0574 90.0849 60.0108 2236 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.45 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1106 1180 1100 1134 1693 1502 1489 2236 N (int>3sigma) = 0 892 1180 886 919 1479 1268 1244 1871 Mean intensity = 0.0 56.3 26.1 56.7 64.1 45.9 64.0 63.3 63.6 Mean int/sigma = 0.0 23.8 21.0 24.0 25.2 22.9 25.4 25.4 25.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.914 5.915 90.05 119.94 119.94 Niggli form: a.a = 34.962 b.b = 34.974 c.c = 34.991 b.c = -0.029 a.c = -17.458 a.b = -17.453 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.103 CUBIC F-lattice R(int) = 0.166 [ 2081] Vol = 585.8 Cell: 8.368 8.373 8.361 90.07 89.99 90.00 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1809] Vol = 439.4 Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 567] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.035 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 89.96 89.94 89.96 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.085 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 90.06 90.04 89.96 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.044 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1787] Vol = 292.9 Cell: 5.919 5.919 8.361 89.94 89.96 89.96 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 1789] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 89.92 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.131 [ 1466] Vol = 292.9 Cell: 5.919 5.919 8.361 90.04 90.06 89.96 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.076 MONOCLINIC I-lattice R(int) = 0.133 [ 1470] Vol = 292.9 Cell: 5.913 5.920 8.368 90.01 90.01 90.08 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.018 MONOCLINIC I-lattice R(int) = 0.130 [ 1493] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 90.08 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.037 MONOCLINIC I-lattice R(int) = 0.130 [ 1480] Vol = 292.9 Cell: 8.368 5.913 5.920 90.08 90.01 90.01 Volume: 292.92 Matrix:-1.0000 2.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.142 [ 1474] Vol = 292.9 Cell: 10.248 5.914 5.915 90.05 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.109 [ 960] Vol = 146.5 Cell: 5.913 5.914 5.915 90.05 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1180 0 1491 1502 2236 N (int>3sigma) = 0 0 0 0 1180 0 1254 1268 1871 Mean intensity = 0.0 0.0 0.0 0.0 26.1 0.0 63.5 64.0 63.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 25.6 25.4 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 172 521 N I>3s 11 11 70 521 0.7 0.7 0.6 30.5 6.0 6.0 3.4 25.6 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 0.166 1929 Fd-3m 1 1 227 C N N N N 37 2284 0.166 1967 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367943 8.373460 8.361062 90.0706 89.9861 90.0050 ZERR 1.00 0.002752 0.001657 0.000282 0.0002 0.0106 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5853063- 934283 525 518 27 19.2 1710456.70 63.47 0.023 0.028 882475- 163327 696 691 27 25.6 290864.05 30.66 0.028 0.034 146559- 55168 588 588 27 21.8 115679.67 13.06 0.045 0.062 22841- 1776 555 554 28 19.8 4783.99 3.09 0.149 0.182 ------------------------------------------------------------------------------------------- 5853063- 1776 2364 2351 109 21.6 492417.53 26.99 0.025 0.031 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 581 573 27 21.2 783610.77 47.61 0.023 0.026 0.014 1.01-0.78 722 722 27 26.7 491259.49 25.22 0.022 0.028 0.024 0.78-0.65 652 650 29 22.4 375649.15 18.46 0.030 0.039 0.033 0.65-0.59 409 406 26 15.6 270451.57 14.68 0.036 0.043 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 2364 2351 109 21.6 492417.53 26.99 0.025 0.031 0.024 inf-0.60 2279 2269 99 22.9 503479.77 27.53 0.025 0.031 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 573 27 27 100.0 21.2 783610.77 226.34 0.023 0.004 1.01-0.78 722 27 27 100.0 26.7 491259.49 132.43 0.022 0.005 0.78-0.65 650 29 29 100.0 22.4 375649.15 92.33 0.030 0.008 0.65-0.59 406 27 26 96.3 15.6 270451.57 66.40 0.036 0.013 -------------------------------------------------------------------------------------------- inf-0.59 2351 110 109 99.1 21.6 492417.53 132.83 0.025 0.006 inf-0.60 2269 99 99 100.0 22.9 503479.77 136.17 0.025 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:45:59 2018) ID: 2932; threads 39; handles 875; mem 519796.00 (1237724.00)kB; time: 1w 5d 22h 51m 29s MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1208.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:507.6,peak PF: 708.5, WS: 271.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1210.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:509.4,peak PF: 708.5, WS: 273.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:45:59 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000011 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000013 0.000012 ) 5.91535 ( 0.00069 ) 5.92288 ( 0.00053 ) 5.91286 ( 0.00068 ) 59.95509 ( 0.01061 ) 89.89521 ( 0.00941 ) 59.99590 ( 0.01073 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:45:59 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000011 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021544 -0.014375 0.007210 ( 0.000004 0.000003 0.000002 ) -0.014375 0.028740 -0.014372 ( 0.000003 0.000004 0.000003 ) 0.007210 -0.014372 0.021577 ( 0.000002 0.000003 0.000003 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(7) 59.955(11) 89.895(9) 59.996(11) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 178 | 1.155 ( 0.133) | 1.272 ( 0.432) | 1.358 ( 0.705) | 13.1-19.0 | 178 | 1.145 ( 0.113) | 1.199 ( 0.298) | 1.328 ( 0.682) | 19.0-23.1 | 178 | 1.154 ( 0.095) | 1.215 ( 0.314) | 1.258 ( 0.653) | 23.1-27.3 | 178 | 1.135 ( 0.098) | 1.173 ( 0.306) | 1.202 ( 0.505) | 27.3-30.5 | 178 | 1.145 ( 0.102) | 1.170 ( 0.205) | 1.215 ( 0.455) | 30.5-33.9 | 178 | 1.156 ( 0.092) | 1.151 ( 0.215) | 1.223 ( 0.446) | 33.9-37.2 | 178 | 1.139 ( 0.111) | 1.111 ( 0.165) | 1.156 ( 0.417) | 37.2-39.9 | 178 | 1.159 ( 0.118) | 1.124 ( 0.243) | 1.264 ( 0.535) | 39.9-42.8 | 178 | 1.171 ( 0.111) | 1.117 ( 0.192) | 1.225 ( 0.569) | 42.9-50.0 | 176 | 1.201 ( 0.168) | 1.133 ( 0.291) | 1.179 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 1778 | 1.156 ( 0.117) | 1.167 ( 0.281) | 1.241 ( 0.556) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0022 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 461776 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 20148380 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:46:15 2018 PROFFITMAIN - Started at Wed Mar 28 13:46:15 2018 OTKP changes: 1778 2 3 4 OTKP changes: 1778 2 3 4 UB - matrix: -0.104246 -0.015009 0.049496 ( 0.000013 0.000014 0.000013 ) 0.087381 -0.167253 0.063728 ( 0.000010 0.000011 0.000010 ) 0.055405 -0.024364 0.122930 ( 0.000013 0.000014 0.000013 ) M - matrix: 0.021572 -0.014400 0.007220 ( 0.000004 0.000003 0.000003 ) -0.014400 0.028792 -0.014397 ( 0.000003 0.000004 0.000003 ) 0.007220 -0.014397 0.021623 ( 0.000003 0.000003 0.000004 ) UB fit with 1778 obs out of 1778 (total:1778,skipped:0) (100.00%) unit cell: 5.9169(7) 5.9099(5) 5.9058(7) 60.067(11) 90.078(10) 59.997(11) V = 146.07(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104118 -0.015206 0.049830 ( 0.000025 0.000032 0.000028 ) 0.087319 -0.167076 0.063631 ( 0.000017 0.000022 0.000019 ) 0.055393 -0.024079 0.122517 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021534 -0.014340 0.007155 ( 0.000006 0.000005 0.000005 ) -0.014340 0.028725 -0.014339 ( 0.000005 0.000007 0.000005 ) 0.007155 -0.014339 0.021542 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9159(14) 5.9122(10) 5.9140(13) 60.04(2) 89.987(19) 60.03(2) V = 146.42(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104058 -0.015210 0.049811 ( 0.000024 0.000031 0.000027 ) 0.087419 -0.167148 0.063726 ( 0.000017 0.000021 0.000019 ) 0.055451 -0.024158 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021545 -0.014369 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014369 0.028753 -0.014370 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014370 0.021560 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9181(13) 5.9145(10) 5.9153(13) 60.02(2) 90.008(18) 60.00(2) V = 146.44(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104489 -0.014343 0.049132 ( 0.000035 0.000044 0.000038 ) 0.087130 -0.167069 0.063756 ( 0.000025 0.000031 0.000027 ) 0.055261 -0.024924 0.122918 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021563 -0.014435 0.007214 ( 0.000009 0.000007 0.000006 ) -0.014435 0.028739 -0.014420 ( 0.000007 0.000011 0.000007 ) 0.007214 -0.014420 0.021588 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9289(19) 5.9360(14) 5.9206(16) 59.90(3) 89.88(2) 59.82(3) V = 146.87(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007255 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104459 -0.014603 0.048930 ( 0.000028 0.000035 0.000030 ) 0.087174 -0.167125 0.063637 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024833 0.123223 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021574 -0.014418 0.007255 ( 0.000008 0.000006 0.000005 ) -0.014418 0.028761 -0.014410 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014410 0.021628 ( 0.000005 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9220(15) 5.9189(13) 5.9092(15) 60.06(2) 90.13(2) 59.97(2) V = 146.36(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146804 -0.097925 0.049160 ( 0.000021 0.000026 0.000023 ) -0.000020 0.138450 -0.069288 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000033 0.119949 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021551 -0.014379 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028758 -0.014403 ( 0.000005 0.000009 0.000006 ) 0.007216 -0.014403 0.021605 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9186(10) 5.9163(14) 5.9125(14) 60.00(2) 90.057(17) 60.02(2) V = 146.37(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104306 -0.014976 0.049283 ( 0.000024 0.000019 0.000017 ) 0.087254 -0.167271 0.063708 ( 0.000028 0.000023 0.000020 ) 0.055329 -0.024506 0.122974 ( 0.000022 0.000018 0.000016 ) M - matrix: 0.021554 -0.014389 0.007222 ( 0.000007 0.000006 0.000004 ) -0.014389 0.028805 -0.014408 ( 0.000006 0.000008 0.000004 ) 0.007222 -0.014408 0.021610 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9177(12) 5.9089(10) 5.9102(10) 60.036(17) 90.099(14) 60.038(19) V = 146.17(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104265 -0.015158 0.049326 ( 0.000023 0.000019 0.000017 ) 0.087197 -0.167198 0.063714 ( 0.000027 0.000022 0.000019 ) 0.055264 -0.024249 0.122769 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021529 -0.014339 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014339 0.028773 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014377 0.021565 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9050(9) 5.9149(9) 60.040(16) 90.129(14) 60.132(18) V = 146.28(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104194 -0.014998 0.049413 ( 0.000013 0.000014 0.000013 ) 0.087319 -0.167103 0.063702 ( 0.000010 0.000011 0.000010 ) 0.055345 -0.024320 0.122791 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021544 -0.014375 0.007210 ( 0.000004 0.000003 0.000002 ) -0.014375 0.028740 -0.014372 ( 0.000003 0.000004 0.000003 ) 0.007210 -0.014372 0.021577 ( 0.000002 0.000003 0.000003 ) UB fit with 1778 obs out of 1778 (total:1778,skipped:0) (100.00%) unit cell: 5.9202(7) 5.9153(5) 5.9129(7) 60.057(11) 90.085(9) 60.011(11) V = 146.46(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 41 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof 2365 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:46:20 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22689244.0000 PROFFIT INFO: signal sum lp corr: min=241.7850 max=3288180.1082 PROFFIT INFO: background sum: min=808.0000 max=15868.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=59 max=886 PROFFIT INFO: Inet: min=527.5308 max=7174211.0000 PROFFIT INFO: sig(Inet): min=190.6879 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=303.85 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 51 177 307 485 534 942 1563 2132 2364 Percent 0.0 0.1 2.2 7.5 13.0 20.5 22.6 39.8 66.1 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2365 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 2365 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7174211- 1632433 236 2463852.98 134.81 100.00 1630964- 1052456 236 1315007.48 111.15 100.00 1052066- 330110 236 609508.22 94.30 100.00 329871- 221710 236 262816.00 70.71 100.00 221552- 167049 236 193436.31 50.10 100.00 166679- 132434 236 150074.90 36.27 100.00 132403- 102464 236 117570.77 30.80 100.00 102316- 6327 236 58074.71 21.00 100.00 6302- 3651 236 4703.76 5.08 84.75 3645- 528 240 2687.32 3.10 41.25 ------------------------------------------------------------------------------------ 7174211- 528 2364 516901.69 55.64 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 879666.34 85.84 99.58 1.28- 1.03 236 640619.66 63.74 97.46 1.03- 0.90 236 618485.22 67.43 95.76 0.90- 0.81 236 468537.00 53.59 95.34 0.81- 0.72 236 614976.99 65.94 92.80 0.72- 0.67 236 475805.46 55.97 91.95 0.67- 0.61 236 329116.41 40.23 88.14 0.61- 0.55 236 424264.12 46.39 93.64 0.55- 0.49 236 368245.37 40.25 84.32 0.49- 0.40 240 352093.74 37.35 86.25 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 516901.69 55.64 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:46:20 2018 Sorting 2364 observations 278 unique observations with > 7.00 F2/sig(F2) 2364 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 Total number of frames 413 Maximum number of 278 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2364 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 1906 observations > 7.00 F2/sig(F2) 1906 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 Removing 'redundancy=1' reflections Average redundancy: 6.8 (Out of 1906 removed 27 = 1879, unique = 277) 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 1879 observations in 4 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 Total number of frames 209 277 unique data precomputed (should be 277) 277 unique data with 1879 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.8 (Out of 1879 removed 0 = 1879, unique = 277) 277 unique data precomputed (should be 277) 277 unique data with 1879 observations RMS deviation of equivalent data = 0.73255 Rint = 0.68800 11 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66697, wR= 3.34688 Trying model 1 (ne=2, no=0)... Results: Rint= 0.74343, wR= 2.69297, Acormin=-0.363, Acormax=2.632, Acor_av=0.572 F test: Probability=0.000, F= 0.802 Trying model 2 (ne=2, no=1)... Results: Rint= 0.80038, wR= 2.19849, Acormin=-0.341, Acormax=2.478, Acor_av=0.413 F test: Probability=0.000, F= 0.691 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75496, wR= 2.07380, Acormin=-0.219, Acormax=2.865, Acor_av=0.510 F test: Probability=0.000, F= 0.774 Trying model 4 (ne=4, no=1)... Results: Rint= 0.83383, wR= 2.28638, Acormin=-0.351, Acormax=2.183, Acor_av=0.388 F test: Probability=0.000, F= 0.633 Trying model 5 (ne=4, no=3)... Results: Rint= 0.91666, wR= 2.16159, Acormin=-0.435, Acormax=3.322, Acor_av=0.140 F test: Probability=0.000, F= 0.521 Trying model 6 (ne=6, no=0)... Results: Rint= 0.74945, wR= 2.38069, Acormin=-0.468, Acormax=3.280, Acor_av=0.467 F test: Probability=0.000, F= 0.779 Trying model 7 (ne=6, no=1)... Results: Rint= 0.84185, wR= 2.37755, Acormin=-0.477, Acormax=2.770, Acor_av=0.344 F test: Probability=0.000, F= 0.616 Trying model 8 (ne=6, no=3)... Results: Rint= 0.93004, wR= 1.70472, Acormin=-0.780, Acormax=3.364, Acor_av=0.123 F test: Probability=0.000, F= 0.502 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96400, wR= 1.40772, Acormin=-0.559, Acormax=2.910, Acor_av=0.075 F test: Probability=0.000, F= 0.464 Trying model 10 (ne=8, no=0)... Results: Rint= 0.83925, wR= 1.95334, Acormin=-0.792, Acormax=1.786, Acor_av=0.262 F test: Probability=0.000, F= 0.614 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87809, wR= 2.51437, Acormin=-0.633, Acormax=1.572, Acor_av=0.186 F test: Probability=0.000, F= 0.560 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98885, wR= 2.03522, Acormin=-0.061, Acormax=0.075, Acor_av=0.002 F test: Probability=0.000, F= 0.439 Trying model 13 (ne=8, no=5)... Results: Rint= 1.00156, wR= 1.85062, Acormin=-0.057, Acormax=0.066, Acor_av=0.001 F test: Probability=0.000, F= 0.425 Trying model 14 (ne=8, no=7)... Results: Rint= 1.01182, wR= 2.04375, Acormin=-0.075, Acormax=0.079, Acor_av=0.000 F test: Probability=0.000, F= 0.413 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86731 There are 209 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 213 pars with 22791 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.73255 Using Levenberg-Marquardt: 0.00010 New wR= 0.71411 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68800 with corrections 0.68062 Rint for all data: 0.86731 with corrections 0.86845 9 observations identified as outliers and rejected Cycle 2 wR= 0.67332 Using Levenberg-Marquardt: 0.00001 New wR= 0.67167 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66949 with corrections 0.65604 Rint for all data: 0.86731 with corrections 0.86626 8 observations identified as outliers and rejected Cycle 3 wR= 0.65062 Using Levenberg-Marquardt: 0.00000 New wR= 0.64918 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65963 with corrections 0.64866 Rint for all data: 0.86731 with corrections 0.86896 13 observations identified as outliers and rejected Cycle 4 wR= 0.62718 Using Levenberg-Marquardt: 0.00000 New wR= 0.62491 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65114 with corrections 0.64286 Rint for all data: 0.86731 with corrections 0.86953 8 observations identified as outliers and rejected Cycle 5 wR= 0.59493 Using Levenberg-Marquardt: 0.00000 New wR= 0.59374 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64948 with corrections 0.63576 Rint for all data: 0.86731 with corrections 0.86404 1 observations identified as outliers and rejected Final wR= 0.59374 Final frame scales: Min= 1.0000 Max= 4.4370 Final absorption correction factors: Amin= 0.5852 Amax= 1.5162 PROFFIT INFO: Inet (after scale3 abspack): min=488.5132 max=7456367.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=188.2925 max=94618.5000 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2364 reflections read from tmp file 1750 reflections are rejected (1687 as outliers, 63 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 87 53 33 14 5 2 2 1 1 Initial Chi^2= 0.57503 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.07562 Current error model SIG(F2)^2 = 256.72*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 276.13*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 276.13*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7456368- 1529008 236 2438156.07 83.01 100.00 1528664- 990100 236 1224721.04 44.86 100.00 986914- 316533 236 608410.08 39.45 100.00 315960- 209987 236 257232.23 29.41 100.00 209967- 161150 236 182287.80 19.26 100.00 160984- 127392 236 143488.97 15.47 100.00 127274- 98066 236 113372.89 12.63 100.00 98026- 6286 236 57234.69 9.18 94.92 6222- 3405 236 4469.26 2.91 29.66 3399- 489 240 2561.18 2.28 12.50 ------------------------------------------------------------------------------------ 7456368- 489 2364 502346.33 25.80 83.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 1002823.72 54.54 96.61 1.28- 1.03 236 635681.29 33.83 89.83 1.03- 0.90 236 624429.78 31.06 87.71 0.90- 0.81 236 479597.38 23.31 82.63 0.81- 0.72 236 570857.58 26.82 85.17 0.72- 0.67 236 443630.87 22.37 82.63 0.67- 0.61 236 295523.60 16.29 74.58 0.61- 0.55 236 384705.25 18.63 83.47 0.55- 0.49 236 309280.21 16.27 77.12 0.49- 0.40 240 280690.47 15.12 76.25 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 502346.33 25.80 83.59 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 236 1002823.72 54.54 96.61 5.26- 1.03 472 819252.51 44.18 93.22 5.26- 0.90 708 754311.60 39.81 91.38 5.26- 0.81 944 685633.05 35.69 89.19 5.26- 0.72 1180 662677.95 33.91 88.39 5.26- 0.67 1416 626170.10 31.99 87.43 5.26- 0.61 1652 578934.89 29.74 85.59 5.26- 0.55 1888 554656.19 28.36 85.33 5.26- 0.49 2124 527392.19 27.01 84.42 5.26- 0.40 2364 502346.33 25.80 83.59 ------------------------------------------------------------------------------------ 5.26- 0.40 2364 502346.33 25.80 83.59 Scale applied to data: s=0.134113 (maximum obs:7456367.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.864; Rsigma 0.025: data 2364 -> merged 317 With outlier rejection... Rint 0.800; Rsigma 0.025: data 2236 -> merged 317 Rejected total: 128, method kkm 118, method Blessing 10 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404281, 5.271185 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 10.87 100.00 163 1.46 - 1.12 15 15 15.13 100.00 227 1.08 - 0.96 15 15 14.13 100.00 212 0.96 - 0.86 15 15 14.20 100.00 213 0.86 - 0.79 15 15 11.40 100.00 171 0.79 - 0.73 15 15 9.20 100.00 138 0.73 - 0.69 15 15 8.67 100.00 130 0.69 - 0.65 15 15 9.20 100.00 138 0.65 - 0.63 15 15 5.67 100.00 85 0.63 - 0.60 21 21 6.76 100.00 142 --------------------------------------------------------------- 5.91 - 0.60 156 156 10.38 100.00 1619 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:46:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920194 5.915315 5.912900 60.0574 90.0849 60.0108 2236 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1106 1180 1100 1134 1693 1502 1489 2236 N (int>3sigma) = 0 892 1180 886 919 1479 1268 1244 1871 Mean intensity = 0.0 56.3 26.1 56.7 64.1 45.9 64.0 63.3 63.6 Mean int/sigma = 0.0 23.8 21.0 24.0 25.2 22.9 25.4 25.4 25.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.914 5.915 90.05 119.94 119.94 Niggli form: a.a = 34.962 b.b = 34.974 c.c = 34.991 b.c = -0.029 a.c = -17.458 a.b = -17.453 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.103 CUBIC F-lattice R(int) = 0.166 [ 2081] Vol = 585.8 Cell: 8.368 8.373 8.361 90.07 89.99 90.00 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1809] Vol = 439.4 Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 567] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.035 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 89.96 89.94 89.96 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.085 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 90.06 90.04 89.96 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.044 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1787] Vol = 292.9 Cell: 5.919 5.919 8.361 89.94 89.96 89.96 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 1789] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 89.92 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.131 [ 1466] Vol = 292.9 Cell: 5.919 5.919 8.361 90.04 90.06 89.96 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.076 MONOCLINIC I-lattice R(int) = 0.133 [ 1470] Vol = 292.9 Cell: 5.913 5.920 8.368 90.01 90.01 90.08 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.018 MONOCLINIC I-lattice R(int) = 0.130 [ 1493] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 90.08 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.037 MONOCLINIC I-lattice R(int) = 0.130 [ 1480] Vol = 292.9 Cell: 5.920 5.913 8.368 89.99 90.01 89.92 Volume: 292.92 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.142 [ 1474] Vol = 292.9 Cell: 10.248 5.914 5.915 90.05 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.109 [ 960] Vol = 146.5 Cell: 5.913 5.914 5.915 90.05 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1180 0 1491 1502 2236 N (int>3sigma) = 0 0 0 0 1180 0 1254 1268 1871 Mean intensity = 0.0 0.0 0.0 0.0 26.1 0.0 63.5 64.0 63.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 25.6 25.4 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 172 521 N I>3s 11 11 70 521 0.7 0.7 0.6 30.5 6.0 6.0 3.4 25.6 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 0.166 1929 Fd-3m 1 1 227 C N N N N 37 2284 0.166 1967 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367943 8.373460 8.361061 90.0706 89.9861 90.0050 ZERR 1.00 0.002752 0.001657 0.000282 0.0002 0.0106 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3965272- 951877 257 234 31 7.5 1387911.55 55.75 0.588 0.468 928525- 675714 305 300 31 9.7 786205.57 34.76 0.954 0.866 667565- 558015 254 245 31 7.9 598492.54 28.67 0.901 0.842 541028- 449525 321 314 31 10.1 473177.14 28.35 0.976 1.097 448299- 346207 252 231 31 7.5 334292.34 22.27 0.927 1.007 345581- 252335 266 236 31 7.6 226718.65 17.79 0.822 0.956 246635- 126574 215 202 31 6.5 157030.14 16.13 0.545 0.487 126306- 101272 175 170 31 5.5 115605.61 12.92 0.408 0.292 100373- 75000 179 168 31 5.4 91802.50 10.70 0.508 0.362 72577- 1115 140 136 38 3.6 47939.81 6.57 0.748 0.730 ------------------------------------------------------------------------------------------- 3965272- 1115 2364 2236 317 7.1 474008.98 25.44 0.800 0.735 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 436 414 31 13.4 790086.36 45.48 0.800 0.792 0.015 1.05-0.83 433 422 31 13.6 568183.80 28.21 0.920 0.991 0.023 0.83-0.72 339 324 33 9.8 465395.67 23.80 0.760 0.790 0.028 0.72-0.65 283 269 32 8.4 350361.34 19.65 0.871 0.946 0.032 0.64-0.60 219 205 31 6.6 392490.81 19.29 0.770 0.862 0.033 0.59-0.56 199 184 33 5.6 292168.18 15.91 0.743 0.677 0.040 0.55-0.52 152 143 31 4.6 348962.10 17.54 0.802 0.724 0.036 0.51-0.49 120 111 32 3.5 225765.32 13.57 0.497 0.349 0.043 0.49-0.46 108 95 31 3.1 225901.80 13.46 0.433 0.287 0.046 0.45-0.40 75 69 32 2.2 251269.52 14.22 0.198 0.146 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 2364 2236 317 7.1 474008.98 25.44 0.800 0.735 0.025 inf-0.60 1691 1619 156 10.4 549838.96 29.32 0.831 0.864 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 414 31 31 100.0 13.4 790086.36 184.50 0.800 0.006 1.05-0.83 422 31 31 100.0 13.6 568183.80 127.26 0.920 0.008 0.83-0.72 324 33 33 100.0 9.8 465395.67 88.51 0.760 0.012 0.72-0.65 269 32 32 100.0 8.4 350361.34 74.17 0.871 0.014 0.64-0.60 205 31 31 100.0 6.6 392490.81 64.00 0.770 0.017 0.59-0.56 184 38 33 86.8 5.6 292168.18 47.25 0.743 0.021 0.55-0.52 143 37 31 83.8 4.6 348962.10 47.68 0.802 0.021 0.51-0.49 111 44 32 72.7 3.5 225765.32 30.07 0.497 0.024 0.49-0.46 95 58 31 53.4 3.1 225901.80 27.05 0.433 0.028 0.45-0.40 69 128 32 25.0 2.2 251269.52 23.72 0.198 0.030 -------------------------------------------------------------------------------------------- inf-0.40 2236 463 317 68.5 7.1 474008.98 96.10 0.800 0.014 inf-0.60 1619 156 156 100.0 10.4 549838.96 118.12 0.831 0.010 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007499 0.076802 -0.034889 ( 0.000007 0.000007 0.000007 ) -0.083550 -0.011809 -0.008041 ( 0.000005 0.000005 0.000005 ) -0.012160 0.033722 0.076908 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007185 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007175 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000009 0.007197 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007499 0.076802 -0.034889 ( 0.000007 0.000007 0.000007 ) -0.083550 -0.011809 -0.008041 ( 0.000005 0.000005 0.000005 ) -0.012160 0.033722 0.076908 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3681(5) 8.3737(7) 8.3611(6) 90.071(6) 89.986(6) 90.005(6) V = 585.87(7) unit cell: 8.3676(2) 8.3676(2) 8.3676(2) 90.0 90.0 90.0 V = 585.87(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.951) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.951) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.951) PROFFIT INFO: signal sum: min=162.0000 max=22689244.0000 PROFFIT INFO: signal sum lp corr: min=241.7850 max=3288180.1082 PROFFIT INFO: background sum: min=808.0000 max=15868.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=10642.0000 PROFFIT INFO: num of signal pixels: min=59 max=886 PROFFIT INFO: Inet: min=527.5308 max=7174211.0000 PROFFIT INFO: sig(Inet): min=190.6879 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=303.85 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 102 354 614 970 1068 1884 3126 4264 4728 Percent 0.0 0.1 2.2 7.5 13.0 20.5 22.6 39.8 66.1 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2365 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 2365 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7174211- 1632433 236 2463852.98 134.81 100.00 1630964- 1052456 236 1315007.48 111.15 100.00 1052066- 330110 236 609508.22 94.30 100.00 329871- 221710 236 262816.00 70.71 100.00 221552- 167049 236 193436.31 50.10 100.00 166679- 132434 236 150074.90 36.27 100.00 132403- 102464 236 117570.77 30.80 100.00 102316- 6327 236 58074.71 21.00 100.00 6302- 3651 236 4703.76 5.08 84.75 3645- 528 240 2687.32 3.10 41.25 ------------------------------------------------------------------------------------ 7174211- 528 2364 516901.69 55.64 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 843715.15 89.08 100.00 1.39- 1.12 236 911102.13 74.81 98.31 1.12- 0.96 236 583933.62 70.61 98.73 0.96- 0.88 236 499806.38 60.67 95.34 0.88- 0.81 236 666669.77 70.63 97.46 0.81- 0.73 236 367159.15 42.53 93.22 0.73- 0.71 236 256118.70 35.16 90.68 0.71- 0.65 236 536379.69 53.03 95.34 0.65- 0.62 236 259874.12 30.14 75.00 0.62- 0.58 240 248802.30 30.22 81.25 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 516901.69 55.64 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:46:21 2018 Sorting 2364 observations 85 unique observations with > 7.00 F2/sig(F2) 2364 observations in 4 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 Total number of frames 413 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2364 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 1906 observations > 7.00 F2/sig(F2) 1906 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 21.4 (Out of 1906 removed 5 = 1901, unique = 89) 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 1901 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 Total number of frames 84 89 unique data precomputed (should be 89) 89 unique data with 1901 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.4 (Out of 1901 removed 0 = 1901, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 1901 observations RMS deviation of equivalent data = 0.21306 Rint = 0.16697 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16422, wR= 0.22023 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08795, wR= 0.11522, Acormin=0.645, Acormax=1.413, Acor_av=0.919 F test: Probability=1.000, F= 3.477 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08403, wR= 0.10512, Acormin=0.603, Acormax=1.359, Acor_av=0.879 F test: Probability=0.971, F= 1.094 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07388, wR= 0.10094, Acormin=0.635, Acormax=1.509, Acor_av=0.877 F test: Probability=1.000, F= 1.289 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06652, wR= 0.08799, Acormin=0.595, Acormax=1.485, Acor_av=0.872 F test: Probability=1.000, F= 1.232 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06468, wR= 0.08550, Acormin=0.510, Acormax=1.343, Acor_av=0.795 F test: Probability=0.864, F= 1.053 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06798, wR= 0.09275, Acormin=0.625, Acormax=1.528, Acor_av=0.869 F test: Probability=0.000, F= 0.952 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06098, wR= 0.08182, Acormin=0.587, Acormax=1.555, Acor_av=0.859 F test: Probability=1.000, F= 1.181 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05865, wR= 0.07769, Acormin=0.492, Acormax=1.419, Acor_av=0.783 F test: Probability=0.941, F= 1.077 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04621, wR= 0.06543, Acormin=0.408, Acormax=1.306, Acor_av=0.685 F test: Probability=1.000, F= 1.724 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06373, wR= 0.08155, Acormin=0.432, Acormax=1.369, Acor_av=0.775 F test: Probability=0.000, F= 0.527 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05761, wR= 0.07427, Acormin=0.521, Acormax=1.484, Acor_av=0.810 F test: Probability=0.000, F= 0.644 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05028, wR= 0.06530, Acormin=0.277, Acormax=0.828, Acor_av=0.446 F test: Probability=0.000, F= 0.842 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04064, wR= 0.05421, Acormin=0.321, Acormax=0.985, Acor_av=0.528 F test: Probability=1.000, F= 1.280 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03840, wR= 0.05087, Acormin=0.337, Acormax=1.067, Acor_av=0.560 F test: Probability=1.000, F= 1.422 Final absorption model (ne=8, no=7): Rint= 0.03840, Acormin=0.337, Acormax=1.067, Acor_av=0.560 Combined refinement in use Rint: 0.16708 There are 84 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: 8, max odd order: 7 (80 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21306 Using Levenberg-Marquardt: 0.00010 New wR= 0.04225 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16697 with corrections 0.03151 Rint for all data: 0.16708 with corrections 0.03172 1 observations identified as outliers and rejected Cycle 2 wR= 0.04038 Using Levenberg-Marquardt: 0.00001 New wR= 0.03779 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16694 with corrections 0.02884 Rint for all data: 0.16708 with corrections 0.02931 1 observations identified as outliers and rejected Cycle 3 wR= 0.03780 Using Levenberg-Marquardt: 0.00000 New wR= 0.03726 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02843 Rint for all data: 0.16708 with corrections 0.02886 0 observations identified as outliers and rejected Cycle 4 wR= 0.03726 Using Levenberg-Marquardt: 0.00000 New wR= 0.03695 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02819 Rint for all data: 0.16708 with corrections 0.02863 0 observations identified as outliers and rejected Cycle 5 wR= 0.03695 Using Levenberg-Marquardt: 0.00000 New wR= 0.03674 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16677 with corrections 0.02806 Rint for all data: 0.16708 with corrections 0.02850 0 observations identified as outliers and rejected Final wR= 0.03674 Final frame scales: Min= 0.7899 Max= 1.0979 Final absorption correction factors: Amin= 0.4313 Amax= 1.4040 PROFFIT INFO: Inet (after scale3 abspack): min=552.4181 max=5920574.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=169.9844 max=68532.7109 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2364 reflections read from tmp file 235 reflections are rejected (233 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 2 2 3 4 6 1 2 84 Initial Chi^2= 0.29551 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.17332 Current error model SIG(F2)^2 = 113.00*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 245.58*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 245.58*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5920574- 1618569 236 2374101.55 90.40 100.00 1604693- 1023230 236 1254631.93 45.26 100.00 1022828- 337001 236 615194.63 44.64 100.00 335964- 204787 236 250236.46 29.81 100.00 204776- 174298 236 188582.43 20.71 100.00 173790- 129573 236 143923.29 15.23 100.00 129506- 103137 236 116663.47 13.05 100.00 103123- 5918 236 60448.25 9.55 96.61 5863- 3523 236 4434.72 3.04 39.41 3520- 552 240 2701.70 2.35 14.58 ------------------------------------------------------------------------------------ 5920574- 552 2364 500248.54 27.36 84.94 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 870967.51 59.63 99.58 1.39- 1.12 236 909384.30 45.35 93.64 1.12- 0.96 236 546631.49 31.45 92.80 0.96- 0.88 236 482849.79 25.71 83.90 0.88- 0.81 236 630603.21 29.73 94.07 0.81- 0.73 236 343262.07 18.24 77.54 0.73- 0.71 236 246903.31 15.15 76.69 0.71- 0.65 236 499313.86 22.42 91.10 0.65- 0.62 236 244891.23 13.10 66.53 0.62- 0.58 240 232221.49 13.09 73.75 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 500248.54 27.36 84.94 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 236 870967.51 59.63 99.58 4.82- 1.12 472 890175.91 52.49 96.61 4.82- 0.96 708 775661.10 45.48 95.34 4.82- 0.88 944 702458.27 40.54 92.48 4.82- 0.81 1180 688087.26 38.37 92.80 4.82- 0.73 1416 630616.39 35.02 90.25 4.82- 0.71 1652 575800.24 32.18 88.32 4.82- 0.65 1888 566239.44 30.96 88.67 4.82- 0.62 2124 530534.09 28.98 86.21 4.82- 0.58 2364 500248.54 27.36 84.94 ------------------------------------------------------------------------------------ 4.82- 0.58 2364 500248.54 27.36 84.94 Scale applied to data: s=0.168902 (maximum obs:5920574.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.029; Rsigma 0.024: data 2364 -> merged 109 With outlier rejection... Rint 0.025; Rsigma 0.024: data 2351 -> merged 109 Rejected total: 13, method kkm 12, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585850, 4.831042 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 13.10 100.00 131 1.61 - 1.21 10 10 21.10 100.00 211 1.17 - 1.01 10 10 28.20 100.00 282 0.99 - 0.89 10 10 28.20 100.00 282 0.88 - 0.81 10 10 26.30 100.00 263 0.81 - 0.74 10 10 23.50 100.00 235 0.73 - 0.71 10 10 25.20 100.00 252 0.70 - 0.66 10 10 21.20 100.00 212 0.66 - 0.64 10 10 20.10 100.00 201 0.63 - 0.60 10 10 20.20 100.00 202 --------------------------------------------------------------- 5.91 - 0.60 100 100 22.71 100.00 2271 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:46:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.920194 5.915315 5.912900 60.0574 90.0849 60.0108 2236 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1106 1180 1100 1134 1693 1502 1489 2236 N (int>3sigma) = 0 892 1180 886 919 1479 1268 1244 1871 Mean intensity = 0.0 56.3 26.1 56.7 64.1 45.9 64.0 63.3 63.6 Mean int/sigma = 0.0 23.8 21.0 24.0 25.2 22.9 25.4 25.4 25.4 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.913 5.914 5.915 90.05 119.94 119.94 Niggli form: a.a = 34.962 b.b = 34.974 c.c = 34.991 b.c = -0.029 a.c = -17.458 a.b = -17.453 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.103 CUBIC F-lattice R(int) = 0.166 [ 2081] Vol = 585.8 Cell: 8.368 8.373 8.361 90.07 89.99 90.00 Volume: 585.85 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1809] Vol = 439.4 Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 567] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.500 90.01 90.05 120.04 Volume: 439.39 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.035 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 89.96 89.94 89.96 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.085 TETRAGONAL I-lattice R(int) = 0.144 [ 1839] Vol = 292.9 Cell: 5.919 5.919 8.361 90.06 90.04 89.96 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.044 ORTHORHOMBIC I-lattice R(int) = 0.146 [ 1787] Vol = 292.9 Cell: 5.919 5.919 8.361 89.94 89.96 89.96 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 1789] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 89.92 90.01 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.131 [ 1466] Vol = 292.9 Cell: 5.919 5.919 8.361 90.04 90.06 89.96 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.076 MONOCLINIC I-lattice R(int) = 0.133 [ 1470] Vol = 292.9 Cell: 5.913 5.920 8.368 90.01 90.01 90.08 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.018 MONOCLINIC I-lattice R(int) = 0.130 [ 1493] Vol = 292.9 Cell: 5.913 8.368 5.920 89.99 90.08 89.99 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.037 MONOCLINIC I-lattice R(int) = 0.130 [ 1480] Vol = 292.9 Cell: 5.920 5.913 8.368 89.99 90.01 89.92 Volume: 292.92 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.074 MONOCLINIC C-lattice R(int) = 0.142 [ 1474] Vol = 292.9 Cell: 10.248 5.914 5.915 90.05 125.20 89.93 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.109 [ 960] Vol = 146.5 Cell: 5.913 5.914 5.915 90.05 119.94 119.94 Volume: 146.46 Matrix: 0.0000 0.0000 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 1180 0 1491 1502 2236 N (int>3sigma) = 0 0 0 0 1180 0 1254 1268 1871 Mean intensity = 0.0 0.0 0.0 0.0 26.1 0.0 63.5 64.0 63.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 25.6 25.4 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 172 521 N I>3s 11 11 70 521 0.7 0.7 0.6 30.5 6.0 6.0 3.4 25.6 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 0.166 1929 Fd-3m 1 1 227 C N N N N 37 2284 0.166 1967 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367943 8.373460 8.361061 90.0706 89.9861 90.0050 ZERR 1.00 0.002752 0.001657 0.000282 0.0002 0.0106 0.0002 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5853000- 934290 525 518 27 19.2 1710463.70 63.50 0.023 0.028 882490- 163327 696 691 27 25.6 290863.40 30.67 0.028 0.034 146559- 55167 588 588 27 21.8 115679.74 13.07 0.045 0.062 22841- 1776 555 554 28 19.8 4784.01 3.09 0.149 0.182 ------------------------------------------------------------------------------------------- 5853000- 1776 2364 2351 109 21.6 492418.90 27.00 0.025 0.031 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 581 573 27 21.2 783609.60 47.63 0.023 0.026 0.014 1.01-0.78 722 722 27 26.7 491262.03 25.24 0.022 0.028 0.024 0.78-0.65 652 650 29 22.4 375650.43 18.47 0.030 0.039 0.033 0.65-0.59 409 406 26 15.6 270454.60 14.69 0.036 0.043 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 2364 2351 109 21.6 492418.90 27.00 0.025 0.031 0.024 inf-0.60 2279 2269 99 22.9 503481.17 27.55 0.025 0.031 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 573 27 27 100.0 21.2 783609.60 226.45 0.023 0.004 1.01-0.78 722 27 27 100.0 26.7 491262.03 132.50 0.022 0.005 0.78-0.65 650 29 29 100.0 22.4 375650.43 92.38 0.030 0.008 0.65-0.59 406 27 26 96.3 15.6 270454.60 66.43 0.036 0.013 -------------------------------------------------------------------------------------------- inf-0.59 2351 110 109 99.1 21.6 492418.90 132.90 0.025 0.006 inf-0.60 2269 99 99 100.0 22.9 503481.17 136.23 0.025 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:50:22 2018) ID: 2932; threads 39; handles 878; mem 519796.00 (1237724.00)kB; time: 1w 5d 22h 55m 52s MEMORY INFO: Memory PF:0.0, Ph:171.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.6,peak PF: 708.5, WS: 271.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:171.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.4,peak PF: 708.5, WS: 273.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:50:22 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000011 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000013 0.000012 ) 5.91535 ( 0.00069 ) 5.92288 ( 0.00053 ) 5.91286 ( 0.00068 ) 59.95509 ( 0.01061 ) 89.89521 ( 0.00941 ) 59.99590 ( 0.01073 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.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 Mar 28 13:50:22 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000011 0.000010 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021544 -0.014375 0.007210 ( 0.000004 0.000003 0.000002 ) -0.014375 0.028740 -0.014372 ( 0.000003 0.000004 0.000003 ) 0.007210 -0.014372 0.021577 ( 0.000002 0.000003 0.000003 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(7) 59.955(11) 89.895(9) 59.996(11) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 442 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 442 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 46 | 1.232 ( 0.079) | 1.103 ( 0.193) | 1.245 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 442 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.193 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb PROFFITPEAK info: 291 peaks in the peak location table UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) UB - matrix: -0.103570 -0.015094 0.049869 ( 0.000313 0.000145 0.000186 ) 0.086920 -0.167102 0.063470 ( 0.000234 0.000109 0.000139 ) 0.056184 -0.024487 0.122434 ( 0.000220 0.000102 0.000131 ) M - matrix: 0.021438 -0.014337 0.007231 ( 0.000080 0.000044 0.000042 ) -0.014337 0.028751 -0.014357 ( 0.000044 0.000037 0.000029 ) 0.007231 -0.014357 0.021505 ( 0.000042 0.000029 0.000041 ) unit cell: 5.934(14) 5.909(7) 5.924(8) 60.12(14) 90.29(15) 60.12(18) V = 147.0(4) UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) UB - matrix: -0.103570 -0.015094 0.049869 ( 0.000313 0.000145 0.000186 ) 0.086920 -0.167102 0.063470 ( 0.000234 0.000109 0.000139 ) 0.056184 -0.024487 0.122434 ( 0.000220 0.000102 0.000131 ) M - matrix: 0.021438 -0.014337 0.007231 ( 0.000080 0.000044 0.000042 ) -0.014337 0.028751 -0.014357 ( 0.000044 0.000037 0.000029 ) 0.007231 -0.014357 0.021505 ( 0.000042 0.000029 0.000041 ) unit cell: 5.934(14) 5.909(7) 5.924(8) 60.12(14) 90.29(15) 60.12(18) V = 147.0(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.103534 -0.015069 0.049852 ( 0.000312 0.000145 0.000186 ) 0.086932 -0.167088 0.063464 ( 0.000240 0.000111 0.000143 ) 0.056266 -0.024423 0.122393 ( 0.000242 0.000112 0.000144 ) M - matrix: 0.021442 -0.014339 0.007242 ( 0.000082 0.000045 0.000044 ) -0.014339 0.028742 -0.014345 ( 0.000045 0.000038 0.000030 ) 0.007242 -0.014345 0.021493 ( 0.000044 0.000030 0.000044 ) UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) unit cell: 5.934(14) 5.908(7) 5.925(9) 60.17(15) 90.34(16) 60.13(18) V = 147.1(4) UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) UB - matrix: -0.103534 -0.015069 0.049852 ( 0.000312 0.000145 0.000186 ) 0.086932 -0.167088 0.063464 ( 0.000240 0.000111 0.000143 ) 0.056266 -0.024423 0.122393 ( 0.000242 0.000112 0.000144 ) M - matrix: 0.021442 -0.014339 0.007242 ( 0.000082 0.000045 0.000044 ) -0.014339 0.028742 -0.014345 ( 0.000045 0.000038 0.000030 ) 0.007242 -0.014345 0.021493 ( 0.000044 0.000030 0.000044 ) unit cell: 5.934(14) 5.908(7) 5.925(9) 60.17(15) 90.34(16) 60.13(18) V = 147.1(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 140 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Run 5 Omega scan: (-2.000 - 23.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 266 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103534 -0.015069 0.049852 ( 0.000312 0.000145 0.000186 ) 0.086932 -0.167088 0.063464 ( 0.000240 0.000111 0.000143 ) 0.056266 -0.024423 0.122393 ( 0.000242 0.000112 0.000144 ) M - matrix: 0.021442 -0.014339 0.007242 ( 0.000082 0.000045 0.000044 ) -0.014339 0.028742 -0.014345 ( 0.000045 0.000038 0.000030 ) 0.007242 -0.014345 0.021493 ( 0.000044 0.000030 0.000044 ) UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) unit cell: 5.934(14) 5.908(7) 5.925(9) 60.17(15) 90.34(16) 60.13(18) V = 147.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 131 obs out of 140 (total:140,skipped:0) (93.57%) 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= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb 2 of 105 peaks identified as outliers and rejected 103 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 103 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 103 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 1.41 | 10 | 1.056 ( 0.071) | 1.138 ( 0.186) | 1.776 ( 1.299) | 1.41- 1.17 | 10 | 1.059 ( 0.056) | 1.068 ( 0.090) | 1.015 ( 0.315) | 1.15- 0.98 | 10 | 1.110 ( 0.123) | 1.426 ( 0.744) | 1.363 ( 0.625) | 0.98- 0.92 | 10 | 1.146 ( 0.031) | 1.169 ( 0.072) | 1.172 ( 0.488) | 0.91- 0.82 | 10 | 1.161 ( 0.056) | 1.114 ( 0.159) | 1.134 ( 0.391) | 0.81- 0.75 | 10 | 1.175 ( 0.029) | 1.157 ( 0.171) | 1.084 ( 0.505) | 0.74- 0.71 | 10 | 1.167 ( 0.033) | 1.122 ( 0.118) | 1.021 ( 0.398) | 0.71- 0.67 | 10 | 1.175 ( 0.045) | 1.107 ( 0.103) | 1.507 ( 0.486) | 0.67- 0.64 | 10 | 1.143 ( 0.052) | 1.199 ( 0.116) | 0.946 ( 0.284) | 0.64- 0.59 | 13 | 1.189 ( 0.071) | 1.189 ( 0.119) | 1.331 ( 0.554) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 0.59 | 103 | 1.139 ( 0.077) | 1.170 ( 0.279) | 1.238 ( 0.647) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) UB - matrix: -0.104012 -0.015464 0.050330 ( 0.000117 0.000060 0.000073 ) 0.087693 -0.167183 0.063486 ( 0.000075 0.000039 0.000047 ) 0.056286 -0.024582 0.122501 ( 0.000078 0.000040 0.000049 ) M - matrix: 0.021677 -0.014436 0.007227 ( 0.000029 0.000015 0.000015 ) -0.014436 0.028793 -0.014403 ( 0.000015 0.000013 0.000010 ) 0.007227 -0.014403 0.021570 ( 0.000015 0.000010 0.000015 ) unit cell: 5.903(5) 5.915(2) 5.918(3) 59.98(5) 90.02(6) 59.99(7) V = 146.02(16) OTKP changes: 103 1 1 1 OTKP changes: 103 1 1 1 OTKP changes: 103 1 1 1 UB - matrix: -0.103899 -0.015360 0.050177 ( 0.000114 0.000059 0.000072 ) 0.087306 -0.167108 0.063452 ( 0.000058 0.000030 0.000037 ) 0.055877 -0.024440 0.122467 ( 0.000065 0.000033 0.000041 ) M - matrix: 0.021540 -0.014359 0.007170 ( 0.000027 0.000012 0.000013 ) -0.014359 0.028758 -0.014367 ( 0.000012 0.000010 0.000008 ) 0.007170 -0.014367 0.021542 ( 0.000013 0.000008 0.000013 ) UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) unit cell: 5.917(5) 5.913(2) 5.918(3) 59.99(4) 89.98(5) 60.02(6) V = 146.47(15) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 23.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 262 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103899 -0.015360 0.050177 ( 0.000114 0.000059 0.000072 ) 0.087306 -0.167108 0.063452 ( 0.000058 0.000030 0.000037 ) 0.055877 -0.024440 0.122467 ( 0.000065 0.000033 0.000041 ) M - matrix: 0.021540 -0.014359 0.007170 ( 0.000027 0.000012 0.000013 ) -0.014359 0.028758 -0.014367 ( 0.000012 0.000010 0.000008 ) 0.007170 -0.014367 0.021542 ( 0.000013 0.000008 0.000013 ) UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) unit cell: 5.917(5) 5.913(2) 5.918(3) 59.99(4) 89.98(5) 60.02(6) V = 146.47(15) 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! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb 2 of 101 peaks identified as outliers and rejected 99 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 99 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 99 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.04- 1.41 | 10 | 1.039 ( 0.077) | 1.099 ( 0.206) | 1.548 ( 1.265) | 1.41- 1.17 | 10 | 1.052 ( 0.058) | 1.204 ( 0.395) | 1.050 ( 0.298) | 1.17- 0.99 | 10 | 1.118 ( 0.081) | 1.390 ( 0.627) | 1.307 ( 0.597) | 0.97- 0.88 | 10 | 1.146 ( 0.021) | 1.143 ( 0.103) | 1.046 ( 0.403) | 0.88- 0.81 | 10 | 1.166 ( 0.056) | 1.137 ( 0.149) | 1.181 ( 0.413) | 0.81- 0.73 | 10 | 1.168 ( 0.038) | 1.132 ( 0.152) | 1.149 ( 0.505) | 0.73- 0.69 | 10 | 1.166 ( 0.031) | 1.121 ( 0.077) | 1.086 ( 0.404) | 0.69- 0.66 | 10 | 1.189 ( 0.043) | 1.125 ( 0.144) | 1.241 ( 0.400) | 0.65- 0.62 | 10 | 1.167 ( 0.065) | 1.215 ( 0.112) | 1.256 ( 0.573) | 0.62- 0.59 | 9 | 1.179 ( 0.067) | 1.163 ( 0.115) | 1.243 ( 0.431) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.04- 0.59 | 99 | 1.139 ( 0.076) | 1.173 ( 0.278) | 1.210 ( 0.607) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 188 | 1.153 ( 0.131) | 1.281 ( 0.444) | 1.362 ( 0.699) | 13.1-19.0 | 188 | 1.143 ( 0.112) | 1.202 ( 0.303) | 1.320 ( 0.674) | 19.0-23.1 | 188 | 1.153 ( 0.094) | 1.214 ( 0.307) | 1.252 ( 0.641) | 23.1-27.3 | 188 | 1.134 ( 0.097) | 1.174 ( 0.301) | 1.218 ( 0.576) | 27.3-30.5 | 188 | 1.142 ( 0.102) | 1.172 ( 0.208) | 1.215 ( 0.450) | 30.5-33.9 | 188 | 1.155 ( 0.090) | 1.144 ( 0.204) | 1.221 ( 0.447) | 33.9-37.2 | 188 | 1.140 ( 0.108) | 1.113 ( 0.165) | 1.143 ( 0.411) | 37.2-39.9 | 188 | 1.159 ( 0.117) | 1.122 ( 0.238) | 1.258 ( 0.533) | 39.9-42.9 | 188 | 1.168 ( 0.113) | 1.111 ( 0.192) | 1.226 ( 0.571) | 42.9-50.1 | 186 | 1.203 ( 0.161) | 1.136 ( 0.285) | 1.176 ( 0.467) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1878 | 1.155 ( 0.116) | 1.167 ( 0.280) | 1.239 ( 0.559) | Fitted profile normalization line parameters e1 dimension: a=0.0018 b=0.97 e2 dimension: a=-0.0013 b=1.02 e3 dimension: a=-0.0026 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 462718 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 23405112 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:50:41 2018 PROFFITMAIN - Started at Wed Mar 28 13:50:41 2018 OTKP changes: 1878 2 4 5 OTKP changes: 1878 2 4 5 UB - matrix: -0.104148 -0.015097 0.049592 ( 0.000014 0.000015 0.000013 ) 0.087365 -0.167245 0.063720 ( 0.000010 0.000010 0.000009 ) 0.055379 -0.024355 0.122906 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021546 -0.014388 0.007208 ( 0.000004 0.000003 0.000002 ) -0.014388 0.028792 -0.014399 ( 0.000003 0.000003 0.000002 ) 0.007208 -0.014399 0.021626 ( 0.000002 0.000002 0.000003 ) UB fit with 1878 obs out of 1878 (total:1878,skipped:0) (100.00%) unit cell: 5.9198(7) 5.9104(5) 5.9058(7) 60.049(10) 90.052(10) 59.996(11) V = 146.14(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104108 -0.015221 0.049840 ( 0.000025 0.000032 0.000028 ) 0.087330 -0.167061 0.063628 ( 0.000017 0.000022 0.000019 ) 0.055408 -0.024082 0.122523 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021535 -0.014339 0.007157 ( 0.000006 0.000005 0.000005 ) -0.014339 0.028721 -0.014339 ( 0.000005 0.000007 0.000005 ) 0.007157 -0.014339 0.021544 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9158(14) 5.9127(10) 5.9138(13) 60.04(2) 89.991(19) 60.03(2) V = 146.42(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104028 -0.015231 0.049809 ( 0.000024 0.000031 0.000027 ) 0.087395 -0.167117 0.063703 ( 0.000017 0.000021 0.000019 ) 0.055434 -0.024169 0.122535 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028744 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014366 0.021554 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9194(13) 5.9153(10) 5.9162(13) 60.01(2) 90.004(18) 60.01(2) V = 146.51(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104028 -0.015231 0.049809 ( 0.000024 0.000031 0.000027 ) 0.087395 -0.167117 0.063703 ( 0.000017 0.000021 0.000019 ) 0.055434 -0.024169 0.122535 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028744 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014366 0.021554 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9194(13) 5.9153(10) 5.9162(13) 60.01(2) 90.004(18) 60.01(2) V = 146.51(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104028 -0.015231 0.049809 ( 0.000024 0.000031 0.000027 ) 0.087395 -0.167117 0.063703 ( 0.000017 0.000021 0.000019 ) 0.055434 -0.024169 0.122535 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028744 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014366 0.021554 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9194(13) 5.9153(10) 5.9162(13) 60.01(2) 90.004(18) 60.01(2) V = 146.51(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104495 -0.014336 0.049146 ( 0.000036 0.000045 0.000039 ) 0.087137 -0.167068 0.063763 ( 0.000025 0.000031 0.000027 ) 0.055280 -0.024931 0.122911 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021568 -0.014438 0.007215 ( 0.000009 0.000007 0.000006 ) -0.014438 0.028739 -0.014422 ( 0.000007 0.000011 0.000007 ) 0.007215 -0.014422 0.021588 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9285(19) 5.9365(14) 5.9209(16) 59.90(3) 89.88(2) 59.82(3) V = 146.87(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104432 -0.014593 0.048915 ( 0.000028 0.000035 0.000031 ) 0.087166 -0.167099 0.063643 ( 0.000023 0.000028 0.000025 ) 0.055320 -0.024807 0.123206 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021564 -0.014414 0.007255 ( 0.000008 0.000006 0.000006 ) -0.014414 0.028750 -0.014405 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014405 0.021623 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9236(15) 5.9199(13) 5.9098(15) 60.07(2) 90.13(2) 59.97(2) V = 146.44(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104432 -0.014593 0.048915 ( 0.000028 0.000035 0.000031 ) 0.087166 -0.167099 0.063643 ( 0.000023 0.000028 0.000025 ) 0.055320 -0.024807 0.123206 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021564 -0.014414 0.007255 ( 0.000008 0.000006 0.000006 ) -0.014414 0.028750 -0.014405 ( 0.000006 0.000010 0.000006 ) 0.007255 -0.014405 0.021623 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9236(15) 5.9199(13) 5.9098(15) 60.07(2) 90.13(2) 59.97(2) V = 146.44(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146770 -0.097910 0.049156 ( 0.000021 0.000027 0.000023 ) -0.000024 0.138428 -0.069267 ( 0.000023 0.000029 0.000025 ) -0.000022 0.000029 0.119936 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021542 -0.014374 0.007214 ( 0.000006 0.000005 0.000005 ) -0.014374 0.028749 -0.014398 ( 0.000005 0.000009 0.000006 ) 0.007214 -0.014398 0.021599 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9201(11) 5.9172(14) 5.9133(14) 60.00(2) 90.060(17) 60.02(2) V = 146.45(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.104310 -0.014953 0.049271 ( 0.000024 0.000019 0.000017 ) 0.087244 -0.167268 0.063701 ( 0.000028 0.000023 0.000020 ) 0.055345 -0.024530 0.122993 ( 0.000022 0.000018 0.000016 ) M - matrix: 0.021555 -0.014391 0.007225 ( 0.000007 0.000006 0.000004 ) -0.014391 0.028804 -0.014409 ( 0.000006 0.000008 0.000004 ) 0.007225 -0.014409 0.021613 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9180(12) 5.9091(10) 5.9099(10) 60.040(18) 90.104(15) 60.035(19) V = 146.17(4) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.104242 -0.015153 0.049327 ( 0.000023 0.000019 0.000017 ) 0.087172 -0.167180 0.063717 ( 0.000027 0.000022 0.000019 ) 0.055242 -0.024216 0.122730 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021517 -0.014331 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014331 0.028765 -0.014372 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014372 0.021556 ( 0.000004 0.000004 0.000005 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9157(11) 5.9055(9) 5.9159(9) 60.040(16) 90.127(14) 60.134(18) V = 146.36(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.968) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104242 -0.015153 0.049327 ( 0.000023 0.000019 0.000017 ) 0.087172 -0.167180 0.063717 ( 0.000027 0.000022 0.000019 ) 0.055242 -0.024216 0.122730 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021517 -0.014331 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014331 0.028765 -0.014372 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014372 0.021556 ( 0.000004 0.000004 0.000005 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9157(11) 5.9055(9) 5.9159(9) 60.040(16) 90.127(14) 60.134(18) V = 146.36(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104242 -0.015153 0.049327 ( 0.000023 0.000019 0.000017 ) 0.087172 -0.167180 0.063717 ( 0.000027 0.000022 0.000019 ) 0.055242 -0.024216 0.122730 ( 0.000020 0.000016 0.000014 ) M - matrix: 0.021517 -0.014331 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014331 0.028765 -0.014372 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014372 0.021556 ( 0.000004 0.000004 0.000005 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9157(11) 5.9055(9) 5.9159(9) 60.040(16) 90.127(14) 60.134(18) V = 146.36(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) UB - matrix: -0.104038 -0.015352 0.050288 ( 0.000120 0.000062 0.000075 ) 0.087413 -0.167088 0.063428 ( 0.000058 0.000030 0.000036 ) 0.056292 -0.024553 0.122480 ( 0.000086 0.000044 0.000053 ) M - matrix: 0.021634 -0.014391 0.007207 ( 0.000029 0.000012 0.000015 ) -0.014391 0.028757 -0.014377 ( 0.000012 0.000010 0.000009 ) 0.007207 -0.014377 0.021553 ( 0.000015 0.000009 0.000016 ) unit cell: 5.904(5) 5.913(2) 5.918(3) 60.00(5) 90.05(6) 60.05(6) V = 146.15(16) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.103985 -0.015336 0.050255 ( 0.000119 0.000061 0.000074 ) 0.087456 -0.167217 0.063513 ( 0.000057 0.000030 0.000036 ) 0.055966 -0.024403 0.122425 ( 0.000075 0.000039 0.000046 ) M - matrix: 0.021594 -0.014395 0.007180 ( 0.000028 0.000012 0.000014 ) -0.014395 0.028792 -0.014379 ( 0.000012 0.000010 0.000009 ) 0.007180 -0.014379 0.021547 ( 0.000014 0.000009 0.000014 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 5.912(5) 5.912(2) 5.918(3) 59.99(5) 89.97(5) 59.99(6) V = 146.23(16) Run 5 Omega scan: (-2.000 - 23.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) HKL list info: 260 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.103985 -0.015336 0.050255 ( 0.000119 0.000061 0.000074 ) 0.087456 -0.167217 0.063513 ( 0.000057 0.000030 0.000036 ) 0.055966 -0.024403 0.122425 ( 0.000075 0.000039 0.000046 ) M - matrix: 0.021594 -0.014395 0.007180 ( 0.000028 0.000012 0.000014 ) -0.014395 0.028792 -0.014379 ( 0.000012 0.000010 0.000009 ) 0.007180 -0.014379 0.021547 ( 0.000014 0.000009 0.000014 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 5.912(5) 5.912(2) 5.918(3) 59.99(5) 89.97(5) 59.99(6) V = 146.23(16) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104100 -0.015081 0.049505 ( 0.000014 0.000015 0.000013 ) 0.087296 -0.167082 0.063689 ( 0.000010 0.000010 0.000009 ) 0.055326 -0.024305 0.122766 ( 0.000012 0.000012 0.000011 ) M - matrix: 0.021518 -0.014360 0.007198 ( 0.000004 0.000003 0.000002 ) -0.014360 0.028735 -0.014372 ( 0.000003 0.000003 0.000002 ) 0.007198 -0.014372 0.021579 ( 0.000002 0.000002 0.000003 ) UB fit with 1878 obs out of 1878 (total:1878,skipped:0) (100.00%) unit cell: 5.9229(7) 5.9158(5) 5.9128(6) 60.044(10) 90.064(9) 60.013(11) V = 146.54(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 42 reflections under beam stop or inside a detector rejection region 19 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof 2509 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:50:46 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.968) Run 5 Omega scan: (-2.000 - 23.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=162.0000 max=22697200.0000 PROFFIT INFO: signal sum lp corr: min=241.7356 max=3279627.5737 PROFFIT INFO: background sum: min=808.0000 max=16676.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=11486.0000 PROFFIT INFO: num of signal pixels: min=60 max=996 PROFFIT INFO: Inet: min=527.4231 max=7155551.0000 PROFFIT INFO: sig(Inet): min=191.4736 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=399.27 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 53 182 319 517 567 996 1655 2260 2508 Percent 0.0 0.1 2.1 7.3 12.7 20.6 22.6 39.7 66.0 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2509 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 2509 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7155551- 1631595 250 2475522.22 134.57 100.00 1630880- 1054386 250 1319925.33 112.51 100.00 1054104- 332081 250 619903.73 95.33 100.00 331887- 224926 250 265438.31 71.29 100.00 224386- 168849 250 196073.70 51.00 100.00 168831- 133333 250 151068.68 36.35 100.00 132963- 104313 250 118239.78 30.80 100.00 104311- 6446 250 59351.50 21.32 100.00 6414- 3701 250 4749.31 5.10 86.00 3700- 527 258 2734.15 3.18 43.02 ------------------------------------------------------------------------------------ 7155551- 527 2508 519646.55 55.98 92.74 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 250 791110.70 85.50 99.60 1.41- 1.05 250 775937.22 66.92 98.00 1.05- 0.92 250 619766.35 66.44 96.80 0.92- 0.82 250 486093.22 55.10 93.20 0.82- 0.74 250 535886.64 63.40 94.80 0.74- 0.67 250 531434.84 58.50 92.00 0.67- 0.61 250 316276.37 40.68 91.60 0.61- 0.56 250 439520.78 46.65 90.80 0.56- 0.50 250 370654.74 40.76 84.40 0.50- 0.40 258 335671.87 36.44 86.43 ------------------------------------------------------------------------------------ 5.26- 0.40 2508 519646.55 55.98 92.74 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:50:46 2018 Sorting 2508 observations 278 unique observations with > 7.00 F2/sig(F2) 2508 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 23 437 Total number of frames 437 Maximum number of 278 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2508 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 11 221 Total number of frames 221 2020 observations > 7.00 F2/sig(F2) 2020 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 11 221 Total number of frames 221 Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 2020 removed 28 = 1992, unique = 277) 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 1992 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 11 221 Total number of frames 221 277 unique data precomputed (should be 277) 277 unique data with 1992 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 1992 removed 0 = 1992, unique = 277) 277 unique data precomputed (should be 277) 277 unique data with 1992 observations RMS deviation of equivalent data = 0.74307 Rint = 0.68949 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66940, wR= 3.19337 Trying model 1 (ne=2, no=0)... Results: Rint= 0.74382, wR= 2.60507, Acormin=-0.303, Acormax=2.622, Acor_av=0.589 F test: Probability=0.000, F= 0.808 Trying model 2 (ne=2, no=1)... Results: Rint= 0.80887, wR= 2.18423, Acormin=-0.312, Acormax=2.498, Acor_av=0.424 F test: Probability=0.000, F= 0.682 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75157, wR= 2.07123, Acormin=-0.154, Acormax=2.869, Acor_av=0.523 F test: Probability=0.000, F= 0.787 Trying model 4 (ne=4, no=1)... Results: Rint= 0.83469, wR= 2.23052, Acormin=-0.335, Acormax=2.265, Acor_av=0.393 F test: Probability=0.000, F= 0.637 Trying model 5 (ne=4, no=3)... Results: Rint= 0.94910, wR= 2.32225, Acormin=-0.429, Acormax=3.295, Acor_av=0.144 F test: Probability=0.000, F= 0.490 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75996, wR= 2.65787, Acormin=-0.395, Acormax=3.537, Acor_av=0.477 F test: Probability=0.000, F= 0.764 Trying model 7 (ne=6, no=1)... Results: Rint= 0.85970, wR= 2.54039, Acormin=-0.478, Acormax=2.910, Acor_av=0.344 F test: Probability=0.000, F= 0.596 Trying model 8 (ne=6, no=3)... Results: Rint= 0.94002, wR= 1.76812, Acormin=-0.784, Acormax=3.382, Acor_av=0.122 F test: Probability=0.000, F= 0.496 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96931, wR= 1.44093, Acormin=-0.521, Acormax=3.129, Acor_av=0.076 F test: Probability=0.000, F= 0.463 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86414, wR= 2.16135, Acormin=-0.811, Acormax=2.005, Acor_av=0.255 F test: Probability=0.000, F= 0.585 Trying model 11 (ne=8, no=1)... Results: Rint= 0.90477, wR= 2.68198, Acormin=-0.654, Acormax=1.737, Acor_av=0.177 F test: Probability=0.000, F= 0.532 Trying model 12 (ne=8, no=3)... Results: Rint= 0.99372, wR= 2.03850, Acormin=-0.055, Acormax=0.079, Acor_av=0.002 F test: Probability=0.000, F= 0.439 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99549, wR= 1.74445, Acormin=-0.050, Acormax=0.071, Acor_av=0.002 F test: Probability=0.000, F= 0.435 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00261, wR= 1.90273, Acormin=-0.079, Acormax=0.078, Acor_av=0.000 F test: Probability=0.000, F= 0.425 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: 0.87033 There are 221 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 225 pars with 25425 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74307 Using Levenberg-Marquardt: 0.00010 New wR= 0.72593 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68949 with corrections 0.68572 Rint for all data: 0.87033 with corrections 0.87345 10 observations identified as outliers and rejected Cycle 2 wR= 0.67587 Using Levenberg-Marquardt: 0.00001 New wR= 0.69031 Using Levenberg-Marquardt: 0.00010 New wR= 0.68865 Using Levenberg-Marquardt: 0.00100 New wR= 0.68051 Using Levenberg-Marquardt: 0.01000 New wR= 0.67451 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67162 with corrections 0.65957 Rint for all data: 0.87033 with corrections 0.87027 8 observations identified as outliers and rejected Cycle 3 wR= 0.65449 Using Levenberg-Marquardt: 0.00100 New wR= 0.65307 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66271 with corrections 0.65209 Rint for all data: 0.87033 with corrections 0.87298 13 observations identified as outliers and rejected Cycle 4 wR= 0.63118 Using Levenberg-Marquardt: 0.00010 New wR= 0.62998 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65475 with corrections 0.64865 Rint for all data: 0.87033 with corrections 0.87405 7 observations identified as outliers and rejected Cycle 5 wR= 0.61156 Using Levenberg-Marquardt: 0.00001 New wR= 0.62342 Using Levenberg-Marquardt: 0.00010 New wR= 0.61870 Using Levenberg-Marquardt: 0.00100 New wR= 0.60700 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65249 with corrections 0.65737 Rint for all data: 0.87033 with corrections 0.87998 3 observations identified as outliers and rejected Final wR= 0.60700 Final frame scales: Min= 0.3470 Max= 2.1836 Final absorption correction factors: Amin= 0.5053 Amax= 1.4361 PROFFIT INFO: Inet (after scale3 abspack): min=451.8549 max=8122940.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=172.5315 max=138256.5000 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2508 reflections read from tmp file 1951 reflections are rejected (1880 as outliers, 71 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 81 57 26 9 5 4 1 1 Initial Chi^2= 0.84077 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.72340 Current error model SIG(F2)^2 = 476.71*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 344.85*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 344.85*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8122941- 1572494 250 2511738.48 73.31 100.00 1562097- 913894 250 1206860.62 41.11 100.00 907040- 334233 250 582653.23 35.66 100.00 334008- 213346 250 266855.75 26.25 100.00 212997- 162794 250 186796.25 17.65 100.00 162617- 121812 250 141473.61 14.13 100.00 121691- 87087 250 103972.47 11.42 100.00 87052- 7078 250 51905.05 8.40 90.40 7070- 3293 250 4505.30 2.70 21.60 3290- 452 258 2432.97 2.03 6.20 ------------------------------------------------------------------------------------ 8122941- 452 2508 504313.36 23.20 81.58 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 250 885821.05 45.75 92.80 1.41- 1.05 250 786766.69 34.36 87.20 1.05- 0.92 250 633211.18 26.80 85.60 0.92- 0.82 250 508261.51 21.99 80.00 0.82- 0.74 250 510237.00 23.07 82.80 0.74- 0.67 250 520805.12 20.90 81.20 0.67- 0.61 250 276002.50 14.72 76.00 0.61- 0.56 250 400878.76 16.77 77.60 0.56- 0.50 250 306297.44 14.72 76.40 0.50- 0.40 258 223827.87 13.21 76.36 ------------------------------------------------------------------------------------ 5.26- 0.40 2508 504313.36 23.20 81.58 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 250 885821.05 45.75 92.80 5.26- 1.05 500 836293.87 40.05 90.00 5.26- 0.92 750 768599.64 35.64 88.53 5.26- 0.82 1000 703515.11 32.23 86.40 5.26- 0.74 1250 664859.48 30.40 85.68 5.26- 0.67 1500 640850.42 28.81 84.93 5.26- 0.61 1750 588729.29 26.80 83.66 5.26- 0.56 2000 565247.97 25.55 82.90 5.26- 0.50 2250 536475.69 24.34 82.18 5.26- 0.40 2508 504313.36 23.20 81.58 ------------------------------------------------------------------------------------ 5.26- 0.40 2508 504313.36 23.20 81.58 Scale applied to data: s=0.123108 (maximum obs:8122940.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.880; Rsigma 0.028: data 2508 -> merged 318 With outlier rejection... Rint 0.800; Rsigma 0.028: data 2349 -> merged 318 Rejected total: 159, method kkm 148, method Blessing 11 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404352, 5.272099 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 12.20 100.00 183 1.46 - 1.12 15 15 16.80 100.00 252 1.08 - 0.96 15 15 15.60 100.00 234 0.96 - 0.86 15 15 15.13 100.00 227 0.86 - 0.79 15 15 12.20 100.00 183 0.79 - 0.73 15 15 9.40 100.00 141 0.73 - 0.69 15 15 9.13 100.00 137 0.69 - 0.65 15 15 9.60 100.00 144 0.65 - 0.63 15 15 5.73 100.00 86 0.63 - 0.60 21 21 6.76 100.00 142 --------------------------------------------------------------- 5.92 - 0.60 156 156 11.08 100.00 1729 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:50:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.922866 5.915766 5.912777 60.0439 90.0642 60.0132 2349 Reflections read from file xs1715a.hkl; mean (I/sigma) = 22.76 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1159 1241 1158 1187 1779 1580 1556 2349 N (int>3sigma) = 0 905 1241 904 932 1525 1296 1266 1913 Mean intensity = 0.0 50.1 24.3 50.4 57.0 41.2 59.0 57.1 57.5 Mean int/sigma = 0.0 21.1 19.0 21.3 22.1 20.5 22.8 22.7 22.8 Lattice type: P chosen Volume: 146.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.913 5.916 5.916 90.03 119.93 119.96 Niggli form: a.a = 34.961 b.b = 34.996 c.c = 35.003 b.c = -0.018 a.c = -17.456 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.205 [ 2194] Vol = 586.2 Cell: 8.369 8.374 8.364 90.10 89.99 90.02 Volume: 586.15 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.096 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 1924] Vol = 439.6 Cell: 5.918 5.916 14.506 89.99 90.07 120.05 Volume: 439.61 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.096 RHOMBOHEDRAL R-lattice R(int) = 0.173 [ 629] Vol = 439.6 Trigonal Cell: 5.918 5.916 14.506 89.99 90.07 120.05 Volume: 439.61 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.178 [ 1952] Vol = 293.1 Cell: 5.921 5.918 8.364 89.93 89.93 89.97 Volume: 293.08 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.096 TETRAGONAL I-lattice R(int) = 0.178 [ 1952] Vol = 293.1 Cell: 5.918 5.921 8.364 90.07 90.07 89.97 Volume: 293.08 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.064 ORTHORHOMBIC I-lattice R(int) = 0.179 [ 1900] Vol = 293.1 Cell: 5.918 5.921 8.364 89.93 89.93 89.97 Volume: 293.08 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.186 [ 1901] Vol = 293.1 Cell: 5.913 8.369 5.923 89.98 89.94 89.99 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.164 [ 1595] Vol = 293.1 Cell: 5.921 5.918 8.364 90.07 90.07 89.97 Volume: 293.08 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.041 MONOCLINIC I-lattice R(int) = 0.169 [ 1580] Vol = 293.1 Cell: 5.913 5.923 8.369 90.02 90.01 89.94 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.014 MONOCLINIC I-lattice R(int) = 0.166 [ 1604] Vol = 293.1 Cell: 5.913 8.369 5.923 89.98 90.06 90.01 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.029 MONOCLINIC I-lattice R(int) = 0.162 [ 1588] Vol = 293.1 Cell: 5.923 5.913 8.369 89.99 90.02 90.06 Volume: 293.08 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.068 MONOCLINIC C-lattice R(int) = 0.163 [ 1594] Vol = 293.1 Cell: 10.246 5.916 5.916 90.03 125.19 89.94 Volume: 293.08 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.129 [ 1064] Vol = 146.5 Cell: 5.913 5.916 5.916 90.03 119.93 119.96 Volume: 146.54 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1241 0 1574 1551 2349 N (int>3sigma) = 0 0 0 0 1241 0 1294 1262 1913 Mean intensity = 0.0 0.0 0.0 0.0 24.3 0.0 57.3 57.4 57.5 Mean int/sigma = 0.0 0.0 0.0 0.0 19.0 0.0 22.9 22.7 22.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.155 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 188 542 N I>3s 15 15 57 542 0.6 0.6 0.5 28.8 5.1 5.1 3.0 23.4 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 0.205 2026 Fd-3m 1 1 227 C N N N N 37 2284 0.205 2064 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368690 8.373754 8.364376 90.0977 89.9948 90.0223 ZERR 1.00 0.002670 0.001656 0.000282 0.0009 0.0105 0.0010 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4182210- 880953 340 318 31 10.3 1271889.61 45.20 0.655 0.583 879810- 681343 323 309 31 10.0 687694.33 29.57 0.945 0.848 675600- 540356 303 292 31 9.4 576508.11 27.30 0.979 0.992 536413- 438624 248 234 31 7.5 430139.12 21.11 0.869 0.808 437071- 337420 272 249 31 8.0 337783.30 22.60 0.877 0.965 337321- 248597 283 248 31 8.0 217818.09 15.28 0.849 0.985 247549- 122756 248 232 31 7.5 149757.43 14.53 0.586 0.588 121691- 90410 216 208 31 6.7 107270.07 11.17 0.490 0.360 87537- 68795 150 142 31 4.6 79662.78 8.95 0.473 0.357 67240- 1001 125 117 39 3.0 36606.23 5.54 0.662 0.573 ------------------------------------------------------------------------------------------- 4182210- 1001 2508 2349 318 7.4 466891.97 22.76 0.800 0.759 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 487 462 31 14.9 780949.67 39.90 0.755 0.772 0.017 1.05-0.83 479 464 32 14.5 557497.65 24.35 0.965 1.084 0.026 0.82-0.72 347 332 32 10.4 472125.28 21.39 0.761 0.799 0.032 0.72-0.65 296 281 32 8.8 358993.61 17.86 0.892 0.975 0.035 0.64-0.60 230 206 31 6.6 362603.11 16.80 0.733 0.808 0.038 0.59-0.56 192 174 31 5.6 259207.78 13.76 0.714 0.630 0.046 0.56-0.52 158 139 31 4.5 300737.18 15.56 0.685 0.646 0.042 0.52-0.49 135 125 34 3.7 211875.30 12.30 0.651 0.469 0.046 0.49-0.46 106 94 31 3.0 194582.30 12.03 0.465 0.312 0.052 0.46-0.40 78 72 33 2.2 184066.28 12.75 0.246 0.190 0.050 ------------------------------------------------------------------------------------------------------ inf-0.40 2508 2349 318 7.4 466891.97 22.76 0.800 0.759 0.028 inf-0.60 1819 1729 156 11.1 549149.13 26.08 0.827 0.879 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 462 31 31 100.0 14.9 780949.67 172.08 0.755 0.006 1.05-0.83 464 32 32 100.0 14.5 557497.65 114.39 0.965 0.009 0.82-0.72 332 32 32 100.0 10.4 472125.28 79.00 0.761 0.013 0.72-0.65 281 32 32 100.0 8.8 358993.61 67.58 0.892 0.015 0.64-0.60 206 31 31 100.0 6.6 362603.11 54.41 0.733 0.020 0.59-0.56 174 36 31 86.1 5.6 259207.78 40.29 0.714 0.024 0.56-0.52 139 35 31 88.6 4.5 300737.18 39.93 0.685 0.024 0.52-0.49 125 48 34 70.8 3.7 211875.30 29.51 0.651 0.026 0.49-0.46 94 57 31 54.4 3.0 194582.30 24.17 0.465 0.031 0.46-0.40 72 128 33 25.8 2.2 184066.28 21.25 0.246 0.034 -------------------------------------------------------------------------------------------- inf-0.40 2349 462 318 68.8 7.4 466891.97 89.00 0.800 0.016 inf-0.60 1729 156 156 100.0 11.1 549149.13 108.98 0.827 0.011 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: -0.007538 -0.076800 0.034840 ( 0.000007 0.000008 0.000007 ) -0.083540 0.011804 0.008049 ( 0.000005 0.000005 0.000005 ) -0.012152 -0.033719 -0.076893 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007183 0.000003 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007175 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000012 0.007191 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007538 -0.076800 0.034840 ( 0.000007 0.000008 0.000007 ) -0.083540 0.011804 0.008049 ( 0.000005 0.000005 0.000005 ) -0.012152 -0.033719 -0.076893 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3688(5) 8.3740(7) 8.3643(6) 90.096(6) 89.995(5) 90.021(6) V = 586.18(7) unit cell: 8.36904(19) 8.36904(19) 8.36904(19) 90.0 90.0 90.0 V = 586.18(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.968) Run 5 Omega scan: (-2.000 - 23.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=162.0000 max=22697200.0000 PROFFIT INFO: signal sum lp corr: min=241.7356 max=3279627.5737 PROFFIT INFO: background sum: min=808.0000 max=16676.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=11486.0000 PROFFIT INFO: num of signal pixels: min=60 max=996 PROFFIT INFO: Inet: min=527.4231 max=7155551.0000 PROFFIT INFO: sig(Inet): min=191.4736 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=399.27 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 106 364 638 1034 1134 1992 3310 4520 5016 Percent 0.0 0.1 2.1 7.3 12.7 20.6 22.6 39.7 66.0 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2509 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 2509 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7155551- 1631595 250 2475522.22 134.57 100.00 1630880- 1054386 250 1319925.33 112.51 100.00 1054104- 332081 250 619903.73 95.33 100.00 331887- 224926 250 265438.31 71.29 100.00 224386- 168849 250 196073.70 51.00 100.00 168831- 133333 250 151068.68 36.35 100.00 132963- 104313 250 118239.78 30.80 100.00 104311- 6446 250 59351.50 21.32 100.00 6414- 3701 250 4749.31 5.10 86.00 3700- 527 258 2734.15 3.18 43.02 ------------------------------------------------------------------------------------ 7155551- 527 2508 519646.55 55.98 92.74 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 250 852606.89 90.86 100.00 1.39- 1.12 250 877023.30 73.88 98.40 1.12- 0.96 250 618463.81 71.41 98.80 0.96- 0.88 250 507631.14 61.38 95.60 0.88- 0.81 250 657103.09 70.07 97.60 0.81- 0.73 250 381271.02 43.65 93.60 0.73- 0.71 250 263610.70 35.87 91.20 0.71- 0.65 250 534024.67 52.74 95.60 0.65- 0.62 250 266969.53 30.62 75.20 0.62- 0.58 258 246502.01 30.09 81.78 ------------------------------------------------------------------------------------ 4.82- 0.58 2508 519646.55 55.98 92.74 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:50:48 2018 Sorting 2508 observations 86 unique observations with > 7.00 F2/sig(F2) 2508 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 23 437 Total number of frames 437 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2508 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 3 75 Total number of frames 75 2020 observations > 7.00 F2/sig(F2) 2020 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 3 75 Total number of frames 75 Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2020 removed 4 = 2016, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2016 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 3 75 Total number of frames 75 90 unique data precomputed (should be 90) 90 unique data with 2016 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2016 removed 0 = 2016, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 2016 observations RMS deviation of equivalent data = 0.21605 Rint = 0.16238 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.15902, wR= 0.21607 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08635, wR= 0.11332, Acormin=0.644, Acormax=1.421, Acor_av=0.918 F test: Probability=1.000, F= 3.383 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08250, wR= 0.10344, Acormin=0.604, Acormax=1.369, Acor_av=0.877 F test: Probability=0.975, F= 1.094 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07261, wR= 0.09942, Acormin=0.642, Acormax=1.510, Acor_av=0.874 F test: Probability=1.000, F= 1.287 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06548, wR= 0.08666, Acormin=0.601, Acormax=1.491, Acor_av=0.867 F test: Probability=1.000, F= 1.228 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06366, wR= 0.08399, Acormin=0.520, Acormax=1.351, Acor_av=0.793 F test: Probability=0.874, F= 1.054 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06717, wR= 0.09153, Acormin=0.627, Acormax=1.537, Acor_av=0.866 F test: Probability=0.000, F= 0.945 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06055, wR= 0.08104, Acormin=0.591, Acormax=1.558, Acor_av=0.855 F test: Probability=0.999, F= 1.161 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05827, wR= 0.07679, Acormin=0.501, Acormax=1.432, Acor_av=0.784 F test: Probability=0.944, F= 1.076 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04605, wR= 0.06486, Acormin=0.414, Acormax=1.312, Acor_av=0.683 F test: Probability=1.000, F= 1.712 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06239, wR= 0.08337, Acormin=0.622, Acormax=1.558, Acor_av=0.867 F test: Probability=0.000, F= 0.546 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05671, wR= 0.07507, Acormin=0.504, Acormax=1.383, Acor_av=0.737 F test: Probability=0.000, F= 0.660 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05006, wR= 0.06519, Acormin=0.287, Acormax=0.848, Acor_av=0.453 F test: Probability=0.000, F= 0.843 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04124, wR= 0.05469, Acormin=0.326, Acormax=0.994, Acor_av=0.530 F test: Probability=1.000, F= 1.236 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03891, wR= 0.05126, Acormin=0.345, Acormax=1.100, Acor_av=0.563 F test: Probability=1.000, F= 1.377 Final absorption model (ne=8, no=7): Rint= 0.03891, Acormin=0.345, Acormax=1.100, Acor_av=0.563 Combined refinement in use Rint: 0.16249 There are 75 active scales (one needs to be fixed) Refinement control: frame scale #63 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 154 pars with 11935 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21605 Using Levenberg-Marquardt: 0.00010 New wR= 0.04588 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16238 with corrections 0.03416 Rint for all data: 0.16249 with corrections 0.03436 0 observations identified as outliers and rejected Cycle 2 wR= 0.04588 Using Levenberg-Marquardt: 0.00001 New wR= 0.04076 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16238 with corrections 0.03112 Rint for all data: 0.16249 with corrections 0.03133 2 observations identified as outliers and rejected Cycle 3 wR= 0.03960 Using Levenberg-Marquardt: 0.00000 New wR= 0.03879 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16217 with corrections 0.03019 Rint for all data: 0.16249 with corrections 0.03063 0 observations identified as outliers and rejected Cycle 4 wR= 0.03879 Using Levenberg-Marquardt: 0.00000 New wR= 0.03849 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16217 with corrections 0.02996 Rint for all data: 0.16249 with corrections 0.03040 0 observations identified as outliers and rejected Cycle 5 wR= 0.03849 Using Levenberg-Marquardt: 0.00000 New wR= 0.03828 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16217 with corrections 0.02979 Rint for all data: 0.16249 with corrections 0.03023 0 observations identified as outliers and rejected Final wR= 0.03828 Final frame scales: Min= 0.8976 Max= 1.0931 Final absorption correction factors: Amin= 0.4322 Amax= 1.3626 PROFFIT INFO: Inet (after scale3 abspack): min=549.7382 max=6085123.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=167.9654 max=70389.1641 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2508 reflections read from tmp file 282 reflections are rejected (281 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 2 1 3 1 8 2 1 85 Initial Chi^2= 0.33554 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.38694 Current error model SIG(F2)^2 = 120.42*I_RAW + 0.00*I_BACK+(0.00852*)^2 Cycle 2, Chi^2= 1.13014 Current error model SIG(F2)^2 = 65.97*I_RAW + 0.00*I_BACK+(0.02287*)^2 Cycle 3, Chi^2= 1.00802 Current error model SIG(F2)^2 = 98.32*I_RAW + 0.00*I_BACK+(0.01810*)^2 Cycle 4, Chi^2= 1.00017 Current error model SIG(F2)^2 = 93.30*I_RAW + 0.00*I_BACK+(0.01935*)^2 Cycle 5, Chi^2= 1.00008 Current error model SIG(F2)^2 = 94.73*I_RAW + 0.00*I_BACK+(0.01905*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 94.40*I_RAW + 0.00*I_BACK+(0.01912*)^2 Cycle 7, Chi^2= 1.00000 Current error model SIG(F2)^2 = 94.48*I_RAW + 0.00*I_BACK+(0.01910*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 94.48*I_RAW + 0.00*I_BACK+(0.01910*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6085124- 1613918 250 2389055.69 48.59 100.00 1603856- 1024212 250 1259585.74 42.28 100.00 1023630- 343217 250 625563.57 40.61 100.00 343177- 207595 250 254213.46 34.48 100.00 207363- 175743 250 190511.88 27.85 100.00 175579- 130140 250 145548.97 22.11 100.00 130127- 104343 250 117226.12 19.48 100.00 104136- 5953 250 61561.83 14.65 100.00 5932- 3560 250 4478.47 4.87 99.20 3555- 550 258 2744.05 3.83 79.07 ------------------------------------------------------------------------------------ 6085124- 550 2508 503446.73 25.81 97.77 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 250 878276.44 39.03 100.00 1.39- 1.12 250 882854.08 31.91 100.00 1.12- 0.96 250 579990.89 29.49 100.00 0.96- 0.88 250 489208.49 26.27 98.80 0.88- 0.81 250 622259.59 30.13 99.60 0.81- 0.73 250 356804.79 21.38 99.20 0.73- 0.71 250 252990.17 19.82 97.20 0.71- 0.65 250 497767.45 25.75 99.60 0.65- 0.62 250 250822.80 17.13 90.00 0.62- 0.58 258 232173.36 17.43 93.41 ------------------------------------------------------------------------------------ 4.82- 0.58 2508 503446.73 25.81 97.77 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 250 878276.44 39.03 100.00 4.82- 1.12 500 880565.26 35.47 100.00 4.82- 0.96 750 780373.80 33.48 100.00 4.82- 0.88 1000 707582.47 31.68 99.70 4.82- 0.81 1250 690517.90 31.37 99.68 4.82- 0.73 1500 634899.05 29.70 99.60 4.82- 0.71 1750 580340.64 28.29 99.26 4.82- 0.65 2000 570018.99 27.97 99.30 4.82- 0.62 2250 534552.74 26.77 98.27 4.82- 0.58 2508 503446.73 25.81 97.77 ------------------------------------------------------------------------------------ 4.82- 0.58 2508 503446.73 25.81 97.77 Scale applied to data: s=0.164335 (maximum obs:6085123.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.025: data 2508 -> merged 109 With outlier rejection... Rint 0.027; Rsigma 0.025: data 2490 -> merged 109 Rejected total: 18, method kkm 18, method Blessing 0 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585950, 4.831869 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 13.90 100.00 139 1.61 - 1.21 10 10 22.50 100.00 225 1.17 - 1.01 10 10 29.90 100.00 299 0.99 - 0.89 10 10 29.80 100.00 298 0.88 - 0.81 10 10 28.10 100.00 281 0.81 - 0.74 10 10 24.40 100.00 244 0.73 - 0.71 10 10 26.80 100.00 268 0.70 - 0.66 10 10 22.50 100.00 225 0.66 - 0.64 10 10 21.20 100.00 212 0.63 - 0.60 10 10 21.20 100.00 212 --------------------------------------------------------------- 5.92 - 0.60 100 100 24.03 100.00 2403 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:50:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.922866 5.915766 5.912777 60.0439 90.0642 60.0132 2349 Reflections read from file xs1715a.hkl; mean (I/sigma) = 22.76 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1159 1241 1158 1187 1779 1580 1556 2349 N (int>3sigma) = 0 905 1241 904 932 1525 1296 1266 1913 Mean intensity = 0.0 50.1 24.3 50.4 57.0 41.2 59.0 57.1 57.5 Mean int/sigma = 0.0 21.1 19.0 21.3 22.1 20.5 22.8 22.7 22.8 Lattice type: P chosen Volume: 146.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.913 5.916 5.916 90.03 119.93 119.96 Niggli form: a.a = 34.961 b.b = 34.996 c.c = 35.003 b.c = -0.018 a.c = -17.456 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.205 [ 2194] Vol = 586.2 Cell: 8.369 8.374 8.364 90.10 89.99 90.02 Volume: 586.15 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.096 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 1924] Vol = 439.6 Cell: 5.918 5.916 14.506 89.99 90.07 120.05 Volume: 439.61 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.096 RHOMBOHEDRAL R-lattice R(int) = 0.173 [ 629] Vol = 439.6 Trigonal Cell: 5.918 5.916 14.506 89.99 90.07 120.05 Volume: 439.61 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.178 [ 1952] Vol = 293.1 Cell: 5.921 5.918 8.364 89.93 89.93 89.97 Volume: 293.08 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.096 TETRAGONAL I-lattice R(int) = 0.178 [ 1952] Vol = 293.1 Cell: 5.918 5.921 8.364 90.07 90.07 89.97 Volume: 293.08 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.064 ORTHORHOMBIC I-lattice R(int) = 0.179 [ 1900] Vol = 293.1 Cell: 5.918 5.921 8.364 89.93 89.93 89.97 Volume: 293.08 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.186 [ 1901] Vol = 293.1 Cell: 5.913 8.369 5.923 89.98 89.94 89.99 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.164 [ 1595] Vol = 293.1 Cell: 5.921 5.918 8.364 90.07 90.07 89.97 Volume: 293.08 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.041 MONOCLINIC I-lattice R(int) = 0.169 [ 1580] Vol = 293.1 Cell: 5.913 5.923 8.369 90.02 90.01 89.94 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.014 MONOCLINIC I-lattice R(int) = 0.166 [ 1604] Vol = 293.1 Cell: 5.913 8.369 5.923 89.98 90.06 90.01 Volume: 293.08 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.029 MONOCLINIC I-lattice R(int) = 0.162 [ 1588] Vol = 293.1 Cell: 5.923 5.913 8.369 89.99 90.02 90.06 Volume: 293.08 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.068 MONOCLINIC C-lattice R(int) = 0.163 [ 1594] Vol = 293.1 Cell: 10.246 5.916 5.916 90.03 125.19 89.94 Volume: 293.08 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.129 [ 1064] Vol = 146.5 Cell: 5.913 5.916 5.916 90.03 119.93 119.96 Volume: 146.54 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1241 0 1574 1551 2349 N (int>3sigma) = 0 0 0 0 1241 0 1294 1262 1913 Mean intensity = 0.0 0.0 0.0 0.0 24.3 0.0 57.3 57.4 57.5 Mean int/sigma = 0.0 0.0 0.0 0.0 19.0 0.0 22.9 22.7 22.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.155 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 188 542 N I>3s 15 15 57 542 0.6 0.6 0.5 28.8 5.1 5.1 3.0 23.4 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 0.205 2026 Fd-3m 1 1 227 C N N N N 37 2284 0.205 2064 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368690 8.373754 8.364376 90.0977 89.9948 90.0223 ZERR 1.00 0.002670 0.001656 0.000282 0.0009 0.0105 0.0010 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5966934- 941440 558 551 27 20.4 1724066.56 44.60 0.025 0.031 911854- 165139 738 733 27 27.1 294157.93 33.46 0.029 0.036 148055- 55824 623 620 27 23.0 116082.72 19.45 0.045 0.059 23068- 1968 589 586 28 20.9 4780.73 4.95 0.148 0.181 ------------------------------------------------------------------------------------------- 5966934- 1968 2508 2490 109 22.8 498133.03 25.73 0.027 0.033 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 617 608 27 22.5 794994.44 35.10 0.025 0.030 0.021 1.01-0.78 744 743 27 27.5 507148.04 26.07 0.024 0.031 0.025 0.78-0.65 713 709 29 24.4 369516.70 21.25 0.031 0.038 0.029 0.65-0.59 434 430 26 16.5 274875.07 19.27 0.038 0.044 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 2508 2490 109 22.8 498133.03 25.73 0.027 0.033 0.025 inf-0.60 2416 2401 99 24.3 509690.31 26.07 0.027 0.033 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 608 27 27 100.0 22.5 794994.44 190.01 0.025 0.008 1.01-0.78 743 27 27 100.0 27.5 507148.04 147.58 0.024 0.005 0.78-0.65 709 29 29 100.0 24.4 369516.70 112.22 0.031 0.007 0.65-0.59 430 27 26 96.3 16.5 274875.07 90.12 0.038 0.011 -------------------------------------------------------------------------------------------- inf-0.59 2490 110 109 99.1 22.8 498133.03 137.95 0.027 0.008 inf-0.60 2401 99 99 100.0 24.3 509690.31 140.88 0.027 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 13:55:54 2018) ID: 2932; threads 39; handles 876; mem 520768.00 (1237724.00)kB; time: 1w 5d 23h 1m 25s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.6,peak PF: 708.5, WS: 272.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:510.4,peak PF: 708.5, WS: 274.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 13:55:54 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000012 0.000011 ) 5.91535 ( 0.00073 ) 5.92288 ( 0.00050 ) 5.91286 ( 0.00064 ) 59.95509 ( 0.01009 ) 89.89521 ( 0.00943 ) 59.99590 ( 0.01082 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 13:55:54 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000010 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000012 0.000011 ) M - matrix: 0.021518 -0.014360 0.007198 ( 0.000004 0.000003 0.000002 ) -0.014360 0.028735 -0.014372 ( 0.000003 0.000003 0.000002 ) 0.007198 -0.014372 0.021579 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(6) 59.955(10) 89.895(9) 59.996(11) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb PROFFITPEAK info: 557 peaks in the peak location table UB fit with 251 obs out of 263 (total:263,skipped:0) (95.44%) UB - matrix: -0.103872 -0.015237 0.050060 ( 0.000114 0.000111 0.000118 ) 0.087224 -0.167087 0.063335 ( 0.000081 0.000079 0.000084 ) 0.055920 -0.024516 0.122545 ( 0.000072 0.000070 0.000075 ) M - matrix: 0.021524 -0.014362 0.007177 ( 0.000029 0.000020 0.000019 ) -0.014362 0.028751 -0.014350 ( 0.000020 0.000027 0.000018 ) 0.007177 -0.014350 0.021535 ( 0.000019 0.000018 0.000024 ) unit cell: 5.921(6) 5.912(4) 5.916(4) 60.06(7) 90.04(7) 60.00(8) V = 146.54(19) UB fit with 251 obs out of 263 (total:263,skipped:0) (95.44%) UB - matrix: -0.103872 -0.015237 0.050060 ( 0.000114 0.000111 0.000118 ) 0.087224 -0.167087 0.063335 ( 0.000081 0.000079 0.000084 ) 0.055920 -0.024516 0.122545 ( 0.000072 0.000070 0.000075 ) M - matrix: 0.021524 -0.014362 0.007177 ( 0.000029 0.000020 0.000019 ) -0.014362 0.028751 -0.014350 ( 0.000020 0.000027 0.000018 ) 0.007177 -0.014350 0.021535 ( 0.000019 0.000018 0.000024 ) unit cell: 5.921(6) 5.912(4) 5.916(4) 60.06(7) 90.04(7) 60.00(8) V = 146.54(19) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.103811 -0.015198 0.049993 ( 0.000114 0.000111 0.000118 ) 0.087155 -0.167044 0.063299 ( 0.000083 0.000081 0.000086 ) 0.055816 -0.024405 0.122476 ( 0.000076 0.000075 0.000079 ) M - matrix: 0.021488 -0.014343 0.007163 ( 0.000029 0.000020 0.000019 ) -0.014343 0.028730 -0.014323 ( 0.000020 0.000027 0.000019 ) 0.007163 -0.014323 0.021507 ( 0.000019 0.000019 0.000025 ) UB fit with 251 obs out of 263 (total:263,skipped:0) (95.44%) unit cell: 5.926(6) 5.912(4) 5.918(5) 60.10(8) 90.05(7) 60.00(8) V = 146.7(2) UB fit with 251 obs out of 263 (total:263,skipped:0) (95.44%) UB - matrix: -0.103811 -0.015198 0.049993 ( 0.000114 0.000111 0.000118 ) 0.087155 -0.167044 0.063299 ( 0.000083 0.000081 0.000086 ) 0.055816 -0.024405 0.122476 ( 0.000076 0.000075 0.000079 ) M - matrix: 0.021488 -0.014343 0.007163 ( 0.000029 0.000020 0.000019 ) -0.014343 0.028730 -0.014323 ( 0.000020 0.000027 0.000019 ) 0.007163 -0.014323 0.021507 ( 0.000019 0.000019 0.000025 ) unit cell: 5.926(6) 5.912(4) 5.918(5) 60.10(8) 90.05(7) 60.00(8) V = 146.7(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 263 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Run 5 Omega scan: (-2.000 - 48.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 421 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103811 -0.015198 0.049993 ( 0.000114 0.000111 0.000118 ) 0.087155 -0.167044 0.063299 ( 0.000083 0.000081 0.000086 ) 0.055816 -0.024405 0.122476 ( 0.000076 0.000075 0.000079 ) M - matrix: 0.021488 -0.014343 0.007163 ( 0.000029 0.000020 0.000019 ) -0.014343 0.028730 -0.014323 ( 0.000020 0.000027 0.000019 ) 0.007163 -0.014323 0.021507 ( 0.000019 0.000019 0.000025 ) UB fit with 251 obs out of 263 (total:263,skipped:0) (95.44%) unit cell: 5.926(6) 5.912(4) 5.918(5) 60.10(8) 90.05(7) 60.00(8) V = 146.7(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 263 (total:263,skipped:0) (95.82%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb 4 of 218 peaks identified as outliers and rejected 214 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 214 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 214 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 1.41 | 21 | 1.020 ( 0.094) | 1.225 ( 0.481) | 1.397 ( 0.959) | 1.41- 1.17 | 21 | 1.056 ( 0.058) | 1.103 ( 0.181) | 1.061 ( 0.382) | 1.17- 1.01 | 21 | 1.084 ( 0.062) | 1.169 ( 0.307) | 1.126 ( 0.485) | 1.01- 0.92 | 21 | 1.124 ( 0.046) | 1.244 ( 0.448) | 1.177 ( 0.421) | 0.92- 0.82 | 21 | 1.147 ( 0.024) | 1.099 ( 0.084) | 1.179 ( 0.446) | 0.82- 0.76 | 21 | 1.170 ( 0.045) | 1.110 ( 0.123) | 1.222 ( 0.481) | 0.75- 0.71 | 21 | 1.163 ( 0.033) | 1.074 ( 0.141) | 1.275 ( 0.457) | 0.71- 0.68 | 21 | 1.183 ( 0.046) | 1.063 ( 0.124) | 1.334 ( 0.425) | 0.67- 0.64 | 21 | 1.162 ( 0.060) | 1.205 ( 0.145) | 1.239 ( 0.544) | 0.64- 0.59 | 25 | 1.197 ( 0.075) | 1.174 ( 0.157) | 1.321 ( 0.561) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.02- 0.59 | 214 | 1.132 ( 0.081) | 1.147 ( 0.263) | 1.235 ( 0.548) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) UB - matrix: -0.104026 -0.015515 0.050292 ( 0.000042 0.000045 0.000047 ) 0.087535 -0.167150 0.063476 ( 0.000029 0.000031 0.000032 ) 0.055929 -0.024538 0.122562 ( 0.000029 0.000031 0.000032 ) M - matrix: 0.021612 -0.014390 0.007179 ( 0.000011 0.000008 0.000007 ) -0.014390 0.028782 -0.014398 ( 0.000008 0.000011 0.000007 ) 0.007179 -0.014398 0.021580 ( 0.000007 0.000007 0.000010 ) unit cell: 5.907(2) 5.9145(15) 5.9154(18) 59.94(3) 89.93(3) 60.00(3) V = 146.10(8) OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 UB - matrix: -0.103922 -0.015411 0.050161 ( 0.000041 0.000044 0.000045 ) 0.087353 -0.167087 0.063401 ( 0.000026 0.000028 0.000029 ) 0.055759 -0.024431 0.122489 ( 0.000027 0.000029 0.000030 ) M - matrix: 0.021539 -0.014356 0.007155 ( 0.000010 0.000007 0.000007 ) -0.014356 0.028752 -0.014359 ( 0.000007 0.000010 0.000007 ) 0.007155 -0.014359 0.021539 ( 0.000007 0.000007 0.000009 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.917(2) 5.9140(14) 5.9173(17) 59.99(3) 89.94(3) 60.00(3) V = 146.45(7) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 48.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 418 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103922 -0.015411 0.050161 ( 0.000041 0.000044 0.000045 ) 0.087353 -0.167087 0.063401 ( 0.000026 0.000028 0.000029 ) 0.055759 -0.024431 0.122489 ( 0.000027 0.000029 0.000030 ) M - matrix: 0.021539 -0.014356 0.007155 ( 0.000010 0.000007 0.000007 ) -0.014356 0.028752 -0.014359 ( 0.000007 0.000010 0.000007 ) 0.007155 -0.014359 0.021539 ( 0.000007 0.000007 0.000009 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.917(2) 5.9140(14) 5.9173(17) 59.99(3) 89.94(3) 60.00(3) V = 146.45(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb 5 of 216 peaks identified as outliers and rejected 211 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 211 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 211 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.48 | 21 | 1.019 ( 0.087) | 1.195 ( 0.438) | 1.391 ( 0.991) | 1.41- 1.17 | 21 | 1.067 ( 0.054) | 1.151 ( 0.281) | 1.168 ( 0.457) | 1.17- 1.01 | 21 | 1.093 ( 0.086) | 1.298 ( 0.500) | 1.118 ( 0.554) | 0.99- 0.92 | 21 | 1.126 ( 0.037) | 1.122 ( 0.104) | 1.157 ( 0.383) | 0.92- 0.82 | 21 | 1.157 ( 0.041) | 1.109 ( 0.119) | 1.256 ( 0.514) | 0.82- 0.75 | 21 | 1.169 ( 0.039) | 1.063 ( 0.120) | 1.236 ( 0.464) | 0.75- 0.71 | 21 | 1.156 ( 0.030) | 1.107 ( 0.123) | 1.259 ( 0.433) | 0.71- 0.67 | 21 | 1.189 ( 0.043) | 1.104 ( 0.164) | 1.257 ( 0.420) | 0.67- 0.64 | 21 | 1.165 ( 0.074) | 1.171 ( 0.153) | 1.295 ( 0.452) | 0.63- 0.59 | 22 | 1.208 ( 0.070) | 1.161 ( 0.148) | 1.359 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 211 | 1.135 ( 0.082) | 1.148 ( 0.261) | 1.250 ( 0.556) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 199 | 1.150 ( 0.128) | 1.273 ( 0.433) | 1.364 ( 0.698) | 13.1-18.9 | 199 | 1.141 ( 0.111) | 1.200 ( 0.291) | 1.302 ( 0.669) | 19.0-23.0 | 199 | 1.149 ( 0.094) | 1.212 ( 0.311) | 1.247 ( 0.630) | 23.1-27.3 | 199 | 1.133 ( 0.095) | 1.177 ( 0.310) | 1.230 ( 0.572) | 27.3-30.4 | 199 | 1.141 ( 0.100) | 1.168 ( 0.213) | 1.218 ( 0.452) | 30.4-33.8 | 199 | 1.153 ( 0.090) | 1.143 ( 0.206) | 1.217 ( 0.437) | 33.8-37.1 | 199 | 1.139 ( 0.105) | 1.117 ( 0.168) | 1.162 ( 0.425) | 37.1-39.9 | 199 | 1.159 ( 0.115) | 1.121 ( 0.235) | 1.250 ( 0.527) | 39.9-42.9 | 199 | 1.168 ( 0.111) | 1.108 ( 0.192) | 1.226 ( 0.562) | 42.9-50.0 | 198 | 1.205 ( 0.161) | 1.127 ( 0.281) | 1.201 ( 0.484) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 1989 | 1.154 ( 0.114) | 1.165 ( 0.279) | 1.242 ( 0.556) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.96 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0025 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 462718 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 23405112 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 13:56:15 2018 PROFFITMAIN - Started at Wed Mar 28 13:56:15 2018 OTKP changes: 1989 2 4 5 OTKP changes: 1989 2 4 5 UB - matrix: -0.104098 -0.015136 0.049638 ( 0.000013 0.000014 0.000013 ) 0.087381 -0.167259 0.063726 ( 0.000009 0.000010 0.000009 ) 0.055428 -0.024388 0.122933 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.021544 -0.014391 0.007215 ( 0.000003 0.000002 0.000002 ) -0.014391 0.028799 -0.014408 ( 0.000002 0.000003 0.000002 ) 0.007215 -0.014408 0.021637 ( 0.000002 0.000002 0.000003 ) UB fit with 1989 obs out of 1989 (total:1989,skipped:0) (100.00%) unit cell: 5.9206(7) 5.9103(5) 5.9049(6) 60.046(10) 90.061(9) 59.996(11) V = 146.12(2) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104098 -0.015238 0.049855 ( 0.000025 0.000032 0.000028 ) 0.087341 -0.167045 0.063623 ( 0.000017 0.000021 0.000019 ) 0.055426 -0.024084 0.122532 ( 0.000020 0.000026 0.000023 ) M - matrix: 0.021537 -0.014338 0.007158 ( 0.000006 0.000005 0.000005 ) -0.014338 0.028716 -0.014339 ( 0.000005 0.000007 0.000005 ) 0.007158 -0.014339 0.021547 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9154(14) 5.9130(10) 5.9133(13) 60.04(2) 89.996(19) 60.03(2) V = 146.41(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104028 -0.015239 0.049824 ( 0.000024 0.000031 0.000027 ) 0.087392 -0.167130 0.063705 ( 0.000017 0.000021 0.000019 ) 0.055443 -0.024179 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028749 -0.014369 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014369 0.021558 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9147(10) 5.9157(13) 60.01(2) 90.002(18) 60.01(2) V = 146.48(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.961) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104028 -0.015239 0.049824 ( 0.000024 0.000031 0.000027 ) 0.087392 -0.167130 0.063705 ( 0.000017 0.000021 0.000019 ) 0.055443 -0.024179 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028749 -0.014369 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014369 0.021558 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9147(10) 5.9157(13) 60.01(2) 90.002(18) 60.01(2) V = 146.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104028 -0.015239 0.049824 ( 0.000024 0.000031 0.000027 ) 0.087392 -0.167130 0.063705 ( 0.000017 0.000021 0.000019 ) 0.055443 -0.024179 0.122545 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021533 -0.014361 0.007178 ( 0.000006 0.000005 0.000005 ) -0.014361 0.028749 -0.014369 ( 0.000005 0.000007 0.000005 ) 0.007178 -0.014369 0.021558 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9147(10) 5.9157(13) 60.01(2) 90.002(18) 60.01(2) V = 146.48(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104501 -0.014326 0.049159 ( 0.000036 0.000045 0.000039 ) 0.087143 -0.167063 0.063769 ( 0.000025 0.000031 0.000027 ) 0.055301 -0.024938 0.122900 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021573 -0.014440 0.007216 ( 0.000009 0.000007 0.000006 ) -0.014440 0.028737 -0.014423 ( 0.000007 0.000011 0.000007 ) 0.007216 -0.014423 0.021588 ( 0.000006 0.000007 0.000008 ) unit cell: 5.9281(19) 5.9372(14) 5.9213(16) 59.89(3) 89.88(2) 59.81(3) V = 146.87(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104428 -0.014604 0.048920 ( 0.000028 0.000035 0.000031 ) 0.087181 -0.167110 0.063645 ( 0.000023 0.000028 0.000025 ) 0.055326 -0.024809 0.123221 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021567 -0.014416 0.007257 ( 0.000008 0.000006 0.000006 ) -0.014416 0.028754 -0.014407 ( 0.000006 0.000010 0.000006 ) 0.007257 -0.014407 0.021627 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9234(15) 5.9194(13) 5.9090(16) 60.07(2) 90.14(2) 59.97(2) V = 146.41(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.961) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104428 -0.014604 0.048920 ( 0.000028 0.000035 0.000031 ) 0.087181 -0.167110 0.063645 ( 0.000023 0.000028 0.000025 ) 0.055326 -0.024809 0.123221 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021567 -0.014416 0.007257 ( 0.000008 0.000006 0.000006 ) -0.014416 0.028754 -0.014407 ( 0.000006 0.000010 0.000006 ) 0.007257 -0.014407 0.021627 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9234(15) 5.9194(13) 5.9090(16) 60.07(2) 90.14(2) 59.97(2) V = 146.41(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146777 -0.097919 0.049167 ( 0.000021 0.000027 0.000023 ) -0.000025 0.138439 -0.069270 ( 0.000023 0.000029 0.000025 ) -0.000023 0.000030 0.119948 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021544 -0.014376 0.007216 ( 0.000006 0.000005 0.000005 ) -0.014376 0.028754 -0.014401 ( 0.000005 0.000010 0.000006 ) 0.007216 -0.014401 0.021603 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9198(11) 5.9166(14) 5.9126(14) 60.00(2) 90.063(17) 60.02(2) V = 146.41(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104314 -0.014926 0.049255 ( 0.000024 0.000020 0.000017 ) 0.087228 -0.167260 0.063687 ( 0.000028 0.000023 0.000020 ) 0.055363 -0.024555 0.123016 ( 0.000023 0.000018 0.000016 ) M - matrix: 0.021555 -0.014392 0.007228 ( 0.000007 0.000006 0.000004 ) -0.014392 0.028802 -0.014408 ( 0.000006 0.000008 0.000004 ) 0.007228 -0.014408 0.021615 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9184(12) 5.9093(10) 5.9093(10) 60.047(18) 90.112(15) 60.033(19) V = 146.17(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104239 -0.015165 0.049343 ( 0.000023 0.000019 0.000017 ) 0.087176 -0.167196 0.063715 ( 0.000027 0.000022 0.000019 ) 0.055249 -0.024214 0.122736 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021518 -0.014332 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014332 0.028771 -0.014373 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014373 0.021558 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9154(11) 5.9046(9) 5.9154(9) 60.041(17) 90.127(14) 60.135(18) V = 146.33(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.961) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104239 -0.015165 0.049343 ( 0.000023 0.000019 0.000017 ) 0.087176 -0.167196 0.063715 ( 0.000027 0.000022 0.000019 ) 0.055249 -0.024214 0.122736 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021518 -0.014332 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014332 0.028771 -0.014373 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014373 0.021558 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9154(11) 5.9046(9) 5.9154(9) 60.041(17) 90.127(14) 60.135(18) V = 146.33(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104239 -0.015165 0.049343 ( 0.000023 0.000019 0.000017 ) 0.087176 -0.167196 0.063715 ( 0.000027 0.000022 0.000019 ) 0.055249 -0.024214 0.122736 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021518 -0.014332 0.007192 ( 0.000007 0.000005 0.000004 ) -0.014332 0.028771 -0.014373 ( 0.000005 0.000007 0.000004 ) 0.007192 -0.014373 0.021558 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9154(11) 5.9046(9) 5.9154(9) 60.041(17) 90.127(14) 60.135(18) V = 146.33(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) UB - matrix: -0.104075 -0.015411 0.050315 ( 0.000042 0.000046 0.000047 ) 0.087379 -0.167074 0.063408 ( 0.000027 0.000029 0.000030 ) 0.056043 -0.024586 0.122605 ( 0.000032 0.000035 0.000036 ) M - matrix: 0.021608 -0.014373 0.007175 ( 0.000011 0.000007 0.000008 ) -0.014373 0.028756 -0.014384 ( 0.000007 0.000010 0.000007 ) 0.007175 -0.014384 0.021584 ( 0.000008 0.000007 0.000011 ) unit cell: 5.906(2) 5.9140(15) 5.913(2) 59.96(3) 89.94(3) 60.02(3) V = 146.07(8) OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 UB - matrix: -0.103980 -0.015372 0.050251 ( 0.000041 0.000044 0.000045 ) 0.087464 -0.167213 0.063482 ( 0.000027 0.000029 0.000030 ) 0.055786 -0.024405 0.122489 ( 0.000028 0.000030 0.000031 ) M - matrix: 0.021574 -0.014388 0.007161 ( 0.000010 0.000007 0.000007 ) -0.014388 0.028792 -0.014377 ( 0.000007 0.000010 0.000007 ) 0.007161 -0.014377 0.021559 ( 0.000007 0.000007 0.000010 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 5.914(2) 5.9128(15) 5.9150(18) 59.98(3) 89.90(3) 59.95(3) V = 146.23(7) Run 5 Omega scan: (-2.000 - 48.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.961) HKL list info: 416 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015372 0.050251 ( 0.000041 0.000044 0.000045 ) 0.087464 -0.167213 0.063482 ( 0.000027 0.000029 0.000030 ) 0.055786 -0.024405 0.122489 ( 0.000028 0.000030 0.000031 ) M - matrix: 0.021574 -0.014388 0.007161 ( 0.000010 0.000007 0.000007 ) -0.014388 0.028792 -0.014377 ( 0.000007 0.000010 0.000007 ) 0.007161 -0.014377 0.021559 ( 0.000007 0.000007 0.000010 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 5.914(2) 5.9128(15) 5.9150(18) 59.98(3) 89.90(3) 59.95(3) V = 146.23(7) 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! 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: -0.103980 -0.015372 0.050251 ( 0.000041 0.000044 0.000045 ) 0.087464 -0.167213 0.063482 ( 0.000027 0.000029 0.000030 ) 0.055786 -0.024405 0.122489 ( 0.000028 0.000030 0.000031 ) M - matrix: 0.021574 -0.014388 0.007161 ( 0.000010 0.000007 0.000007 ) -0.014388 0.028792 -0.014377 ( 0.000007 0.000010 0.000007 ) 0.007161 -0.014377 0.021559 ( 0.000007 0.000007 0.000010 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 5.914(2) 5.9128(15) 5.9150(18) 59.98(3) 89.90(3) 59.95(3) V = 146.23(7) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104045 -0.015126 0.049555 ( 0.000014 0.000015 0.000013 ) 0.087302 -0.167096 0.063685 ( 0.000009 0.000010 0.000009 ) 0.055358 -0.024329 0.122788 ( 0.000011 0.000012 0.000011 ) M - matrix: 0.021511 -0.014361 0.007201 ( 0.000003 0.000002 0.000002 ) -0.014361 0.028742 -0.014378 ( 0.000002 0.000003 0.000002 ) 0.007201 -0.014378 0.021588 ( 0.000002 0.000002 0.000003 ) UB fit with 1989 obs out of 1989 (total:1989,skipped:0) (100.00%) unit cell: 5.9240(7) 5.9153(5) 5.9118(6) 60.042(10) 90.068(9) 60.014(10) V = 146.52(2) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 44 reflections under beam stop or inside a detector rejection region 20 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof 2653 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 13:56:21 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.961) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.961) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.961) Run 5 Omega scan: (-2.000 - 48.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.961) PROFFIT INFO: signal sum: min=162.0000 max=22536032.0000 PROFFIT INFO: signal sum lp corr: min=241.7621 max=3279574.6854 PROFFIT INFO: background sum: min=806.0000 max=17080.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=11616.0000 PROFFIT INFO: num of signal pixels: min=59 max=1005 PROFFIT INFO: Inet: min=527.4810 max=7155436.0000 PROFFIT INFO: sig(Inet): min=191.1008 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=399.15 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 55 194 339 546 600 1058 1753 2396 2652 Percent 0.0 0.1 2.1 7.3 12.8 20.6 22.6 39.9 66.1 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2653 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 2653 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7155436- 1624978 265 2464890.46 133.80 100.00 1624494- 1054947 265 1318520.57 112.78 100.00 1052628- 326643 265 617220.27 95.23 100.00 325668- 222487 265 261636.90 70.43 100.00 222429- 167941 265 193659.63 50.26 100.00 167890- 132249 265 150121.18 36.48 100.00 132196- 102748 265 117658.10 30.61 100.00 102464- 6302 265 57912.16 20.89 100.00 6231- 3644 265 4674.85 5.02 84.15 3643- 527 267 2696.86 3.19 43.07 ------------------------------------------------------------------------------------ 7155436- 527 2652 518509.80 55.83 92.68 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 265 801944.18 84.47 99.62 1.41- 1.05 265 781580.92 68.34 98.11 1.05- 0.93 265 628617.93 66.43 96.60 0.92- 0.82 265 481995.89 54.15 91.70 0.82- 0.74 265 505683.22 61.26 94.72 0.74- 0.67 265 499950.30 56.34 92.08 0.67- 0.61 265 342250.31 43.15 92.45 0.61- 0.56 265 454476.16 48.04 90.57 0.56- 0.50 265 363651.35 40.22 84.15 0.50- 0.40 267 326397.69 36.05 86.89 ------------------------------------------------------------------------------------ 5.26- 0.40 2652 518509.80 55.83 92.68 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:56:21 2018 Sorting 2652 observations 279 unique observations with > 7.00 F2/sig(F2) 2652 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 48 462 Total number of frames 462 Maximum number of 279 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2652 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 24 234 Total number of frames 234 2136 observations > 7.00 F2/sig(F2) 2136 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 24 234 Total number of frames 234 Removing 'redundancy=1' reflections Average redundancy: 7.6 (Out of 2136 removed 27 = 2109, unique = 277) 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 2109 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 24 234 Total number of frames 234 277 unique data precomputed (should be 277) 277 unique data with 2109 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.6 (Out of 2109 removed 0 = 2109, unique = 277) 277 unique data precomputed (should be 277) 277 unique data with 2109 observations RMS deviation of equivalent data = 0.74420 Rint = 0.68841 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66963, wR= 3.55008 Trying model 1 (ne=2, no=0)... Results: Rint= 0.74974, wR= 3.06698, Acormin=-0.311, Acormax=2.658, Acor_av=0.588 F test: Probability=0.000, F= 0.796 Trying model 2 (ne=2, no=1)... Results: Rint= 0.82140, wR= 2.53098, Acormin=-0.333, Acormax=2.507, Acor_av=0.409 F test: Probability=0.000, F= 0.662 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75501, wR= 2.17986, Acormin=-0.172, Acormax=2.988, Acor_av=0.518 F test: Probability=0.000, F= 0.781 Trying model 4 (ne=4, no=1)... Results: Rint= 0.84893, wR= 2.69477, Acormin=-0.352, Acormax=2.260, Acor_av=0.378 F test: Probability=0.000, F= 0.616 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96101, wR= 2.30945, Acormin=-0.364, Acormax=3.445, Acor_av=0.146 F test: Probability=0.000, F= 0.479 Trying model 6 (ne=6, no=0)... Results: Rint= 0.76214, wR= 2.89103, Acormin=-0.418, Acormax=3.682, Acor_av=0.469 F test: Probability=0.000, F= 0.761 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87005, wR= 3.09953, Acormin=-0.492, Acormax=2.919, Acor_av=0.333 F test: Probability=0.000, F= 0.583 Trying model 8 (ne=6, no=3)... Results: Rint= 0.94619, wR= 1.65024, Acormin=-0.824, Acormax=3.525, Acor_av=0.129 F test: Probability=0.000, F= 0.491 Trying model 9 (ne=6, no=5)... Results: Rint= 0.95642, wR= 1.41517, Acormin=-0.510, Acormax=3.307, Acor_av=0.078 F test: Probability=0.000, F= 0.477 Trying model 10 (ne=8, no=0)... Results: Rint= 0.87604, wR= 2.01623, Acormin=-0.775, Acormax=2.096, Acor_av=0.251 F test: Probability=0.000, F= 0.570 Trying model 11 (ne=8, no=1)... Results: Rint= 0.91422, wR= 2.69507, Acormin=-0.617, Acormax=1.853, Acor_av=0.176 F test: Probability=0.000, F= 0.523 Trying model 12 (ne=8, no=3)... Results: Rint= 0.99901, wR= 1.91865, Acormin=-0.052, Acormax=0.081, Acor_av=0.001 F test: Probability=0.000, F= 0.436 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99996, wR= 1.74752, Acormin=-0.049, Acormax=0.078, Acor_av=0.001 F test: Probability=0.000, F= 0.432 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00406, wR= 1.67241, Acormin=-0.073, Acormax=0.080, Acor_av=-0.000 F test: Probability=0.000, F= 0.425 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: 0.86986 There are 234 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 238 pars with 28441 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74420 Using Levenberg-Marquardt: 0.00010 New wR= 0.72728 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68841 with corrections 0.68209 Rint for all data: 0.86986 with corrections 0.87167 10 observations identified as outliers and rejected Cycle 2 wR= 0.67850 Using Levenberg-Marquardt: 0.00001 New wR= 0.68255 Using Levenberg-Marquardt: 0.00010 New wR= 0.68217 Using Levenberg-Marquardt: 0.00100 New wR= 0.67993 Using Levenberg-Marquardt: 0.01000 New wR= 0.67716 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67163 with corrections 0.65904 Rint for all data: 0.86986 with corrections 0.87011 10 observations identified as outliers and rejected Cycle 3 wR= 0.65632 Using Levenberg-Marquardt: 0.00100 New wR= 0.65462 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66153 with corrections 0.65152 Rint for all data: 0.86986 with corrections 0.87265 12 observations identified as outliers and rejected Cycle 4 wR= 0.63624 Using Levenberg-Marquardt: 0.00010 New wR= 0.63285 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65483 with corrections 0.64813 Rint for all data: 0.86986 with corrections 0.87403 9 observations identified as outliers and rejected Cycle 5 wR= 0.62208 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= 0.62509 Using Levenberg-Marquardt: 0.10000 New wR= 0.61689 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65081 with corrections 0.64669 Rint for all data: 0.86986 with corrections 0.87588 4 observations identified as outliers and rejected Final wR= 0.61689 Final frame scales: Min= 0.5208 Max= 2.3678 Final absorption correction factors: Amin= 0.4938 Amax= 1.4298 PROFFIT INFO: Inet (after scale3 abspack): min=402.1925 max=8433473.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=182.3198 max=93860.9531 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2652 reflections read from tmp file 2007 reflections are rejected (1938 as outliers, 69 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 80 51 32 12 10 5 1 1 3 Initial Chi^2= 0.56789 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.92318 Current error model SIG(F2)^2 = 226.52*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 209.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 209.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8433473- 1575374 265 2552036.46 95.66 100.00 1566132- 921769 265 1239077.07 51.78 100.00 910802- 330817 265 581754.96 45.88 100.00 329658- 219389 265 267098.31 33.78 100.00 219090- 162584 265 187132.22 22.29 100.00 162479- 124587 265 143479.67 17.96 100.00 124490- 89603 265 106067.50 14.33 100.00 89480- 6522 265 51730.03 10.76 96.98 6509- 3325 265 4512.09 3.27 47.17 3324- 402 267 2468.03 2.61 23.22 ------------------------------------------------------------------------------------ 8433473- 402 2652 513150.21 29.81 86.69 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 265 962108.15 58.70 98.87 1.41- 1.05 265 818367.19 44.62 94.72 1.05- 0.93 265 660220.28 34.82 91.70 0.92- 0.82 265 500836.19 27.95 84.53 0.82- 0.74 265 471658.45 28.63 88.30 0.74- 0.67 265 490752.94 25.89 85.28 0.67- 0.61 265 307680.52 19.99 83.77 0.61- 0.56 265 409342.70 22.15 84.15 0.56- 0.50 265 294628.72 18.67 76.60 0.50- 0.40 267 218133.52 16.79 79.03 ------------------------------------------------------------------------------------ 5.26- 0.40 2652 513150.21 29.81 86.69 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 265 962108.15 58.70 98.87 5.26- 1.05 530 890237.67 51.66 96.79 5.26- 0.93 795 813565.20 46.04 95.09 5.26- 0.82 1060 735382.95 41.52 92.45 5.26- 0.74 1325 682638.05 38.94 91.62 5.26- 0.67 1590 650657.20 36.77 90.57 5.26- 0.61 1855 601660.53 34.37 89.60 5.26- 0.56 2120 577620.80 32.85 88.92 5.26- 0.50 2385 546177.24 31.27 87.55 5.26- 0.40 2652 513150.21 29.81 86.69 ------------------------------------------------------------------------------------ 5.26- 0.40 2652 513150.21 29.81 86.69 Scale applied to data: s=0.118575 (maximum obs:8433473.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.876; Rsigma 0.021: data 2652 -> merged 317 With outlier rejection... Rint 0.803; Rsigma 0.022: data 2506 -> merged 317 Rejected total: 146, method kkm 135, method Blessing 11 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404338, 5.271922 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 12.80 100.00 192 1.46 - 1.12 15 15 18.33 100.00 275 1.08 - 0.96 15 15 17.33 100.00 260 0.96 - 0.86 15 15 16.27 100.00 244 0.86 - 0.79 15 15 13.00 100.00 195 0.79 - 0.73 15 15 10.07 100.00 151 0.73 - 0.69 15 15 9.93 100.00 149 0.69 - 0.65 15 15 10.20 100.00 153 0.65 - 0.63 15 15 6.20 100.00 93 0.63 - 0.60 21 21 7.14 100.00 150 --------------------------------------------------------------- 5.91 - 0.60 156 156 11.94 100.00 1862 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:56:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.924007 5.915335 5.911795 60.0417 90.0678 60.0139 2506 Reflections read from file xs1715a.hkl; mean (I/sigma) = 29.39 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1239 1318 1243 1280 1900 1686 1650 2506 N (int>3sigma) = 0 1049 1318 1053 1080 1710 1470 1432 2173 Mean intensity = 0.0 51.3 23.5 51.5 58.5 41.7 59.2 56.8 58.2 Mean int/sigma = 0.0 27.4 24.3 27.7 28.9 26.4 29.4 29.0 29.4 Lattice type: P chosen Volume: 146.52 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.912 5.915 5.916 90.02 119.92 119.96 Niggli form: a.a = 34.949 b.b = 34.991 c.c = 34.998 b.c = -0.014 a.c = -17.445 a.b = -17.463 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.208 [ 2351] Vol = 586.1 Cell: 8.368 8.374 8.364 90.12 89.99 90.04 Volume: 586.09 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.104 RHOMBOHEDRAL R-lattice R(int) = 0.192 [ 2078] Vol = 439.6 Cell: 5.917 5.915 14.508 89.99 90.08 120.05 Volume: 439.57 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.104 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 680] Vol = 439.6 Trigonal Cell: 5.917 5.915 14.508 89.99 90.08 120.05 Volume: 439.57 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.068 TETRAGONAL I-lattice R(int) = 0.188 [ 2110] Vol = 293.0 Cell: 5.921 5.917 8.364 89.92 89.91 89.96 Volume: 293.05 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.117 TETRAGONAL I-lattice R(int) = 0.188 [ 2110] Vol = 293.0 Cell: 5.917 5.921 8.364 90.09 90.08 89.96 Volume: 293.05 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.076 ORTHORHOMBIC I-lattice R(int) = 0.187 [ 2058] Vol = 293.0 Cell: 5.917 5.921 8.364 89.91 89.92 89.96 Volume: 293.05 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.183 [ 2061] Vol = 293.0 Cell: 5.912 8.368 5.924 89.97 89.93 89.98 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.050 MONOCLINIC I-lattice R(int) = 0.167 [ 1740] Vol = 293.0 Cell: 5.921 5.917 8.364 90.08 90.09 89.96 Volume: 293.05 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.041 MONOCLINIC I-lattice R(int) = 0.167 [ 1737] Vol = 293.0 Cell: 5.912 5.924 8.368 90.03 90.02 89.93 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC I-lattice R(int) = 0.171 [ 1761] Vol = 293.0 Cell: 5.912 8.368 5.924 89.97 90.07 90.02 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.032 MONOCLINIC I-lattice R(int) = 0.155 [ 1744] Vol = 293.0 Cell: 5.924 5.912 8.368 89.98 90.03 90.07 Volume: 293.05 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.069 MONOCLINIC C-lattice R(int) = 0.163 [ 1750] Vol = 293.0 Cell: 10.244 5.915 5.916 90.02 125.17 89.94 Volume: 293.05 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.131 [ 1193] Vol = 146.5 Cell: 5.912 5.915 5.916 90.02 119.92 119.96 Volume: 146.52 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1318 0 1684 1657 2506 N (int>3sigma) = 0 0 0 0 1318 0 1465 1445 2173 Mean intensity = 0.0 0.0 0.0 0.0 23.5 0.0 58.1 59.0 58.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.3 0.0 29.5 29.6 29.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 26 26 200 583 N I>3s 17 17 114 583 0.6 0.6 0.5 28.0 6.3 6.3 3.8 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.208 2171 Fd-3m 1 1 227 C N N N N 37 2284 0.209 2209 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367629 8.374131 8.364227 90.1182 89.9948 90.0351 ZERR 1.00 0.002587 0.001612 0.000267 0.0008 0.0101 0.0010 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3465710- 862688 352 332 31 10.7 1396413.31 59.63 0.668 0.643 860774- 658868 384 371 31 12.0 732599.10 38.48 0.977 0.871 653591- 528296 293 284 31 9.2 543034.32 31.80 0.914 0.845 522950- 423833 286 276 31 8.9 449421.60 30.90 0.894 0.911 416953- 331478 286 262 31 8.5 323248.71 26.63 0.863 0.970 330942- 250473 301 268 31 8.6 221251.03 20.92 0.786 0.919 250448- 126518 246 230 31 7.4 140625.21 16.40 0.610 0.641 126198- 87550 219 213 31 6.9 108735.91 14.26 0.504 0.351 86848- 68061 157 149 31 4.8 79376.05 11.38 0.468 0.363 67159- 1111 128 121 38 3.2 42069.68 7.64 0.711 0.601 ------------------------------------------------------------------------------------------- 3465710- 1111 2652 2506 317 7.9 490851.57 29.39 0.803 0.771 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 529 496 31 16.0 840525.61 50.93 0.758 0.794 0.013 1.05-0.83 506 499 31 16.1 572158.93 31.68 0.953 1.070 0.020 0.83-0.72 357 345 31 11.1 478914.19 27.46 0.760 0.800 0.024 0.72-0.65 319 307 33 9.3 376003.71 22.77 0.917 0.997 0.027 0.65-0.60 243 223 31 7.2 388963.62 22.31 0.764 0.839 0.028 0.60-0.56 215 199 33 6.0 276958.70 17.99 0.701 0.689 0.036 0.56-0.52 166 155 31 5.0 330503.17 20.42 0.746 0.701 0.032 0.52-0.49 132 118 33 3.6 201539.55 15.59 0.586 0.423 0.037 0.49-0.46 110 98 31 3.2 192577.20 15.56 0.419 0.283 0.040 0.45-0.40 75 66 32 2.1 170781.95 15.66 0.239 0.161 0.040 ------------------------------------------------------------------------------------------------------ inf-0.40 2652 2506 317 7.9 490851.57 29.39 0.803 0.771 0.022 inf-0.60 1944 1862 156 11.9 573948.13 33.50 0.828 0.886 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 496 31 31 100.0 16.0 840525.61 225.19 0.758 0.004 1.05-0.83 499 31 31 100.0 16.1 572158.93 156.52 0.953 0.007 0.83-0.72 345 31 31 100.0 11.1 478914.19 107.61 0.760 0.010 0.72-0.65 307 33 33 100.0 9.3 376003.71 90.39 0.917 0.012 0.65-0.60 223 31 31 100.0 7.2 388963.62 77.67 0.764 0.015 0.60-0.56 199 38 33 86.8 6.0 276958.70 54.00 0.701 0.017 0.56-0.52 155 36 31 86.1 5.0 330503.17 56.80 0.746 0.018 0.52-0.49 118 46 33 71.7 3.6 201539.55 36.07 0.586 0.021 0.49-0.46 98 58 31 53.4 3.2 192577.20 31.80 0.419 0.024 0.45-0.40 66 127 32 25.2 2.1 170781.95 24.77 0.239 0.027 -------------------------------------------------------------------------------------------- inf-0.40 2506 463 317 68.5 7.9 490851.57 119.93 0.803 0.012 inf-0.60 1862 156 156 100.0 11.9 573948.13 145.87 0.828 0.008 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: -0.007563 -0.076798 0.034808 ( 0.000007 0.000008 0.000007 ) -0.083547 0.011808 0.008054 ( 0.000005 0.000005 0.000005 ) -0.012164 -0.033714 -0.076908 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007185 0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007174 0.000015 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000015 0.007191 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007563 -0.076798 0.034808 ( 0.000007 0.000008 0.000007 ) -0.083547 0.011808 0.008054 ( 0.000005 0.000005 0.000005 ) -0.012164 -0.033714 -0.076908 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3678(5) 8.3743(7) 8.3643(6) 90.119(6) 89.994(5) 90.035(6) V = 586.12(7) unit cell: 8.36878(19) 8.36878(19) 8.36878(19) 90.0 90.0 90.0 V = 586.12(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.961) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.961) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.961) Run 5 Omega scan: (-2.000 - 48.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.961) PROFFIT INFO: signal sum: min=162.0000 max=22536032.0000 PROFFIT INFO: signal sum lp corr: min=241.7621 max=3279574.6854 PROFFIT INFO: background sum: min=806.0000 max=17080.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=11616.0000 PROFFIT INFO: num of signal pixels: min=59 max=1005 PROFFIT INFO: Inet: min=527.4810 max=7155436.0000 PROFFIT INFO: sig(Inet): min=191.1008 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=399.15 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 110 388 678 1092 1200 2116 3506 4792 5304 Percent 0.0 0.1 2.1 7.3 12.8 20.6 22.6 39.9 66.1 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2653 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 2653 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7155436- 1624978 265 2464890.46 133.80 100.00 1624494- 1054947 265 1318520.57 112.78 100.00 1052628- 326643 265 617220.27 95.23 100.00 325668- 222487 265 261636.90 70.43 100.00 222429- 167941 265 193659.63 50.26 100.00 167890- 132249 265 150121.18 36.48 100.00 132196- 102748 265 117658.10 30.61 100.00 102464- 6302 265 57912.16 20.89 100.00 6231- 3644 265 4674.85 5.02 84.15 3643- 527 267 2696.86 3.19 43.07 ------------------------------------------------------------------------------------ 7155436- 527 2652 518509.80 55.83 92.68 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 265 852172.49 90.08 100.00 1.41- 1.12 265 884523.09 73.94 98.49 1.12- 0.96 265 621315.82 71.77 98.87 0.96- 0.88 265 492213.32 60.34 95.09 0.88- 0.81 265 663224.63 70.53 97.36 0.81- 0.73 265 377714.16 43.47 93.21 0.73- 0.71 265 253429.29 35.06 91.32 0.71- 0.65 265 534527.86 52.99 95.47 0.65- 0.62 265 263671.77 30.45 75.85 0.62- 0.58 267 244374.55 29.85 81.27 ------------------------------------------------------------------------------------ 4.82- 0.58 2652 518509.80 55.83 92.68 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 13:56:22 2018 Sorting 2652 observations 85 unique observations with > 7.00 F2/sig(F2) 2652 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 48 462 Total number of frames 462 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2652 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 8 80 Total number of frames 80 2136 observations > 7.00 F2/sig(F2) 2136 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 8 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 23.9 (Out of 2136 removed 6 = 2130, unique = 89) 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 2130 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 8 80 Total number of frames 80 89 unique data precomputed (should be 89) 89 unique data with 2130 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.9 (Out of 2130 removed 0 = 2130, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 2130 observations RMS deviation of equivalent data = 0.21490 Rint = 0.16288 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16056, wR= 0.21717 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08536, wR= 0.11192, Acormin=0.639, Acormax=1.423, Acor_av=0.921 F test: Probability=1.000, F= 3.529 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08317, wR= 0.10426, Acormin=0.609, Acormax=1.381, Acor_av=0.880 F test: Probability=0.872, F= 1.052 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07141, wR= 0.09810, Acormin=0.638, Acormax=1.506, Acor_av=0.879 F test: Probability=1.000, F= 1.423 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06653, wR= 0.08821, Acormin=0.601, Acormax=1.484, Acor_av=0.869 F test: Probability=0.999, F= 1.150 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06417, wR= 0.08506, Acormin=0.509, Acormax=1.315, Acor_av=0.785 F test: Probability=0.939, F= 1.071 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06626, wR= 0.09046, Acormin=0.626, Acormax=1.533, Acor_av=0.870 F test: Probability=0.530, F= 1.003 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06181, wR= 0.08228, Acormin=0.593, Acormax=1.546, Acor_av=0.858 F test: Probability=0.999, F= 1.151 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05892, wR= 0.07725, Acormin=0.499, Acormax=1.412, Acor_av=0.782 F test: Probability=0.981, F= 1.097 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04964, wR= 0.06909, Acormin=0.398, Acormax=1.247, Acor_av=0.651 F test: Probability=1.000, F= 1.401 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06159, wR= 0.08242, Acormin=0.621, Acormax=1.546, Acor_av=0.866 F test: Probability=0.000, F= 0.651 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05921, wR= 0.07701, Acormin=0.496, Acormax=1.349, Acor_av=0.729 F test: Probability=0.000, F= 0.703 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05199, wR= 0.06693, Acormin=0.279, Acormax=0.805, Acor_av=0.435 F test: Probability=0.000, F= 0.909 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04550, wR= 0.05869, Acormin=0.310, Acormax=0.915, Acor_av=0.495 F test: Probability=1.000, F= 1.180 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04039, wR= 0.05241, Acormin=0.336, Acormax=1.118, Acor_av=0.549 F test: Probability=1.000, F= 1.486 Final absorption model (ne=8, no=7): Rint= 0.04039, Acormin=0.336, Acormax=1.118, Acor_av=0.549 Combined refinement in use Rint: 0.16299 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #63 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21490 Using Levenberg-Marquardt: 0.00010 New wR= 0.04532 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16288 with corrections 0.03454 Rint for all data: 0.16299 with corrections 0.03474 0 observations identified as outliers and rejected Cycle 2 wR= 0.04532 Using Levenberg-Marquardt: 0.00001 New wR= 0.04141 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16288 with corrections 0.03156 Rint for all data: 0.16299 with corrections 0.03178 2 observations identified as outliers and rejected Cycle 3 wR= 0.04036 Using Levenberg-Marquardt: 0.00000 New wR= 0.03965 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16290 with corrections 0.03061 Rint for all data: 0.16299 with corrections 0.03109 1 observations identified as outliers and rejected Cycle 4 wR= 0.03966 Using Levenberg-Marquardt: 0.00000 New wR= 0.03947 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16275 with corrections 0.03041 Rint for all data: 0.16299 with corrections 0.03088 1 observations identified as outliers and rejected Cycle 5 wR= 0.03908 Using Levenberg-Marquardt: 0.00000 New wR= 0.03891 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16282 with corrections 0.02996 Rint for all data: 0.16299 with corrections 0.03086 0 observations identified as outliers and rejected Final wR= 0.03891 Final frame scales: Min= 0.9050 Max= 1.1188 Final absorption correction factors: Amin= 0.4333 Amax= 1.3877 PROFFIT INFO: Inet (after scale3 abspack): min=548.3729 max=6009107.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=166.8541 max=69522.5859 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2652 reflections read from tmp file 305 reflections are rejected (304 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 1 0 5 1 5 4 3 84 Initial Chi^2= 0.33553 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.99492 Current error model SIG(F2)^2 = 125.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 249.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 249.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6009108- 1609371 265 2391571.38 90.85 100.00 1607773- 1022316 265 1258476.49 45.10 100.00 1018970- 340508 265 620535.08 44.23 100.00 338558- 206464 265 251802.11 29.56 100.00 206374- 174365 265 188973.08 20.69 100.00 174138- 129359 265 144446.37 15.01 100.00 129324- 103388 265 116464.51 12.98 100.00 103344- 5825 265 59860.11 9.39 96.23 5818- 3508 265 4402.15 3.02 37.36 3504- 548 267 2714.70 2.34 14.23 ------------------------------------------------------------------------------------ 6009108- 548 2652 503546.61 27.30 84.73 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 265 879542.37 59.67 99.25 1.41- 1.12 265 896388.60 44.79 93.96 1.12- 0.96 265 587611.86 32.15 91.70 0.96- 0.88 265 473190.09 25.37 82.64 0.88- 0.81 265 628917.18 29.46 94.34 0.81- 0.73 265 354072.39 18.48 77.74 0.73- 0.71 265 241779.83 14.99 76.23 0.71- 0.65 265 500301.32 22.23 91.32 0.65- 0.62 265 246878.60 13.12 67.17 0.62- 0.58 267 228857.00 12.84 73.03 ------------------------------------------------------------------------------------ 4.82- 0.58 2652 503546.61 27.30 84.73 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 265 879542.37 59.67 99.25 4.82- 1.12 530 887965.49 52.23 96.60 4.82- 0.96 795 787847.61 45.53 94.97 4.82- 0.88 1060 709183.23 40.49 91.89 4.82- 0.81 1325 693130.02 38.29 92.38 4.82- 0.73 1590 636620.42 34.99 89.94 4.82- 0.71 1855 580214.62 32.13 87.98 4.82- 0.65 2120 570225.46 30.89 88.40 4.82- 0.62 2385 534298.03 28.92 86.04 4.82- 0.58 2652 503546.61 27.30 84.73 ------------------------------------------------------------------------------------ 4.82- 0.58 2652 503546.61 27.30 84.73 Scale applied to data: s=0.166414 (maximum obs:6009107.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.031; Rsigma 0.024: data 2652 -> merged 109 With outlier rejection... Rint 0.027; Rsigma 0.024: data 2635 -> merged 109 Rejected total: 17, method kkm 11, method Blessing 6 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585932, 4.831717 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 15.00 100.00 150 1.61 - 1.21 10 10 23.80 100.00 238 1.17 - 1.01 10 10 31.60 100.00 316 0.99 - 0.89 10 10 31.20 100.00 312 0.88 - 0.81 10 10 29.80 100.00 298 0.81 - 0.74 10 10 26.00 100.00 260 0.73 - 0.71 10 10 28.30 100.00 283 0.70 - 0.66 10 10 23.80 100.00 238 0.66 - 0.64 10 10 22.50 100.00 225 0.63 - 0.60 10 10 22.40 100.00 224 --------------------------------------------------------------- 5.91 - 0.60 100 100 25.44 100.00 2544 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 13:56:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.924007 5.915335 5.911795 60.0417 90.0678 60.0139 2506 Reflections read from file xs1715a.hkl; mean (I/sigma) = 29.39 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1239 1318 1243 1280 1900 1686 1650 2506 N (int>3sigma) = 0 1049 1318 1053 1080 1710 1470 1432 2173 Mean intensity = 0.0 51.3 23.5 51.5 58.5 41.7 59.2 56.8 58.2 Mean int/sigma = 0.0 27.4 24.3 27.7 28.9 26.4 29.4 29.0 29.4 Lattice type: P chosen Volume: 146.52 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.912 5.915 5.916 90.02 119.92 119.96 Niggli form: a.a = 34.949 b.b = 34.991 c.c = 34.998 b.c = -0.014 a.c = -17.445 a.b = -17.463 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.208 [ 2351] Vol = 586.1 Cell: 8.368 8.374 8.364 90.12 89.99 90.04 Volume: 586.09 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.104 RHOMBOHEDRAL R-lattice R(int) = 0.192 [ 2078] Vol = 439.6 Cell: 5.917 5.915 14.508 89.99 90.08 120.05 Volume: 439.57 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.104 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 680] Vol = 439.6 Trigonal Cell: 5.917 5.915 14.508 89.99 90.08 120.05 Volume: 439.57 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.068 TETRAGONAL I-lattice R(int) = 0.188 [ 2110] Vol = 293.0 Cell: 5.921 5.917 8.364 89.92 89.91 89.96 Volume: 293.05 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.117 TETRAGONAL I-lattice R(int) = 0.188 [ 2110] Vol = 293.0 Cell: 5.917 5.921 8.364 90.09 90.08 89.96 Volume: 293.05 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.076 ORTHORHOMBIC I-lattice R(int) = 0.187 [ 2058] Vol = 293.0 Cell: 5.917 5.921 8.364 89.91 89.92 89.96 Volume: 293.05 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.183 [ 2061] Vol = 293.0 Cell: 5.912 8.368 5.924 89.97 89.93 89.98 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.050 MONOCLINIC I-lattice R(int) = 0.167 [ 1740] Vol = 293.0 Cell: 5.921 5.917 8.364 90.08 90.09 89.96 Volume: 293.05 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.041 MONOCLINIC I-lattice R(int) = 0.167 [ 1737] Vol = 293.0 Cell: 5.912 5.924 8.368 90.03 90.02 89.93 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC I-lattice R(int) = 0.171 [ 1761] Vol = 293.0 Cell: 5.912 8.368 5.924 89.97 90.07 90.02 Volume: 293.05 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.032 MONOCLINIC I-lattice R(int) = 0.155 [ 1744] Vol = 293.0 Cell: 5.924 5.912 8.368 89.98 90.03 90.07 Volume: 293.05 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.069 MONOCLINIC C-lattice R(int) = 0.163 [ 1750] Vol = 293.0 Cell: 10.244 5.915 5.916 90.02 125.17 89.94 Volume: 293.05 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.131 [ 1193] Vol = 146.5 Cell: 5.912 5.915 5.916 90.02 119.92 119.96 Volume: 146.52 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1318 0 1684 1657 2506 N (int>3sigma) = 0 0 0 0 1318 0 1465 1445 2173 Mean intensity = 0.0 0.0 0.0 0.0 23.5 0.0 58.1 59.0 58.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.3 0.0 29.5 29.6 29.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 26 26 200 583 N I>3s 17 17 114 583 0.6 0.6 0.5 28.0 6.3 6.3 3.8 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.208 2171 Fd-3m 1 1 227 C N N N N 37 2284 0.209 2209 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367629 8.374131 8.364227 90.1182 89.9948 90.0351 ZERR 1.00 0.002587 0.001612 0.000267 0.0008 0.0101 0.0010 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5926487- 933022 592 580 27 21.5 1709926.06 62.83 0.025 0.029 902887- 163869 781 777 27 28.8 291190.58 30.41 0.030 0.037 146942- 55334 657 657 27 24.3 115651.15 12.95 0.047 0.063 22786- 1961 622 621 28 22.2 4741.26 3.06 0.152 0.189 ------------------------------------------------------------------------------------------- 5926487- 1961 2652 2635 109 24.2 492197.09 26.75 0.027 0.032 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 656 645 27 23.9 782452.53 47.02 0.024 0.026 0.014 1.01-0.78 829 829 28 29.6 476334.12 24.35 0.024 0.032 0.024 0.76-0.65 711 708 28 25.3 388184.40 18.88 0.032 0.040 0.033 0.65-0.59 456 453 26 17.4 270511.93 14.56 0.039 0.044 0.045 ------------------------------------------------------------------------------------------------------ inf-0.59 2652 2635 109 24.2 492197.09 26.75 0.027 0.032 0.024 inf-0.60 2557 2543 99 25.7 503688.79 27.30 0.027 0.032 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 645 27 27 100.0 23.9 782452.53 237.96 0.024 0.004 1.01-0.78 829 28 28 100.0 29.6 476334.12 135.24 0.024 0.004 0.76-0.65 708 28 28 100.0 25.3 388184.40 100.72 0.032 0.007 0.65-0.59 453 27 26 96.3 17.4 270511.93 70.16 0.039 0.013 -------------------------------------------------------------------------------------------- inf-0.59 2635 110 109 99.1 24.2 492197.09 139.92 0.027 0.005 inf-0.60 2543 99 99 100.0 25.7 503688.79 143.48 0.027 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:01:18 2018) ID: 2932; threads 39; handles 878; mem 520228.00 (1237724.00)kB; time: 1w 5d 23h 6m 48s MEMORY INFO: Memory PF:0.0, Ph:173.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 708.5, WS: 271.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:173.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.8,peak PF: 708.5, WS: 273.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:01:18 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000009 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000011 0.000012 0.000011 ) 5.91535 ( 0.00071 ) 5.92288 ( 0.00049 ) 5.91286 ( 0.00062 ) 59.95509 ( 0.00980 ) 89.89521 ( 0.00917 ) 59.99590 ( 0.01050 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 14:01:18 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000014 0.000015 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000009 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000011 0.000012 0.000011 ) M - matrix: 0.021511 -0.014361 0.007201 ( 0.000003 0.000002 0.000002 ) -0.014361 0.028742 -0.014378 ( 0.000002 0.000003 0.000002 ) 0.007201 -0.014378 0.021588 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(6) 59.955(10) 89.895(9) 59.996(10) V = 146.51(2) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.145 ( 0.064) | 1.106 ( 0.082) | 1.109 ( 0.374) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.119 ( 0.156) | 1.433 ( 0.539) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.116 ( 0.180) | 1.328 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.133) | 1.124 ( 0.290) | 1.283 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb PROFFITPEAK info: 821 peaks in the peak location table UB fit with 379 obs out of 392 (total:392,skipped:0) (96.68%) UB - matrix: -0.103794 -0.015244 0.050012 ( 0.000054 0.000084 0.000080 ) 0.087281 -0.166938 0.063239 ( 0.000042 0.000065 0.000062 ) 0.055991 -0.024442 0.122451 ( 0.000039 0.000061 0.000058 ) M - matrix: 0.021526 -0.014357 0.007185 ( 0.000014 0.000013 0.000012 ) -0.014357 0.028698 -0.014312 ( 0.000013 0.000022 0.000014 ) 0.007185 -0.014312 0.021494 ( 0.000012 0.000014 0.000018 ) unit cell: 5.922(3) 5.916(3) 5.920(3) 60.12(5) 90.10(5) 60.00(5) V = 146.79(13) UB fit with 379 obs out of 392 (total:392,skipped:0) (96.68%) UB - matrix: -0.103794 -0.015244 0.050012 ( 0.000054 0.000084 0.000080 ) 0.087281 -0.166938 0.063239 ( 0.000042 0.000065 0.000062 ) 0.055991 -0.024442 0.122451 ( 0.000039 0.000061 0.000058 ) M - matrix: 0.021526 -0.014357 0.007185 ( 0.000014 0.000013 0.000012 ) -0.014357 0.028698 -0.014312 ( 0.000013 0.000022 0.000014 ) 0.007185 -0.014312 0.021494 ( 0.000012 0.000014 0.000018 ) unit cell: 5.922(3) 5.916(3) 5.920(3) 60.12(5) 90.10(5) 60.00(5) V = 146.79(13) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB fit with 379 obs out of 392 (total:392,skipped:0) (96.68%) UB - matrix: -0.103791 -0.015240 0.050013 ( 0.000054 0.000083 0.000080 ) 0.087282 -0.166936 0.063241 ( 0.000042 0.000065 0.000062 ) 0.055995 -0.024430 0.122452 ( 0.000041 0.000063 0.000060 ) M - matrix: 0.021526 -0.014357 0.007186 ( 0.000014 0.000013 0.000012 ) -0.014357 0.028697 -0.014311 ( 0.000013 0.000022 0.000014 ) 0.007186 -0.014311 0.021495 ( 0.000012 0.000014 0.000018 ) unit cell: 5.922(3) 5.916(3) 5.919(3) 60.12(5) 90.10(5) 60.00(5) V = 146.79(13) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 392 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Run 5 Omega scan: (-2.000 - 73.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 575 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103791 -0.015240 0.050013 ( 0.000054 0.000083 0.000080 ) 0.087282 -0.166936 0.063241 ( 0.000042 0.000065 0.000062 ) 0.055995 -0.024430 0.122452 ( 0.000041 0.000063 0.000060 ) M - matrix: 0.021526 -0.014357 0.007186 ( 0.000014 0.000013 0.000012 ) -0.014357 0.028697 -0.014311 ( 0.000013 0.000022 0.000014 ) 0.007186 -0.014311 0.021495 ( 0.000012 0.000014 0.000018 ) UB fit with 379 obs out of 392 (total:392,skipped:0) (96.68%) unit cell: 5.922(3) 5.916(3) 5.919(3) 60.12(5) 90.10(5) 60.00(5) V = 146.79(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 380 obs out of 392 (total:392,skipped:0) (96.94%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb 5 of 331 peaks identified as outliers and rejected 326 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 326 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 326 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 33 | 1.013 ( 0.096) | 1.142 ( 0.410) | 1.299 ( 0.903) | 1.41- 1.17 | 33 | 1.076 ( 0.081) | 1.186 ( 0.473) | 1.047 ( 0.434) | 1.15- 0.98 | 33 | 1.084 ( 0.067) | 1.209 ( 0.530) | 1.219 ( 0.499) | 0.98- 0.92 | 33 | 1.133 ( 0.038) | 1.136 ( 0.103) | 1.096 ( 0.393) | 0.91- 0.82 | 33 | 1.156 ( 0.042) | 1.100 ( 0.135) | 1.224 ( 0.492) | 0.82- 0.75 | 33 | 1.162 ( 0.033) | 1.072 ( 0.106) | 1.307 ( 0.489) | 0.75- 0.71 | 33 | 1.166 ( 0.032) | 1.083 ( 0.122) | 1.241 ( 0.452) | 0.71- 0.67 | 33 | 1.186 ( 0.043) | 1.139 ( 0.150) | 1.210 ( 0.433) | 0.67- 0.62 | 33 | 1.171 ( 0.069) | 1.173 ( 0.151) | 1.170 ( 0.467) | 0.62- 0.59 | 29 | 1.200 ( 0.066) | 1.146 ( 0.170) | 1.252 ( 0.551) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 326 | 1.134 ( 0.082) | 1.139 ( 0.287) | 1.206 ( 0.535) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 326 obs out of 326 (total:326,skipped:0) (100.00%) UB - matrix: -0.103998 -0.015518 0.050298 ( 0.000024 0.000040 0.000037 ) 0.087621 -0.167153 0.063475 ( 0.000016 0.000027 0.000024 ) 0.056078 -0.024621 0.122567 ( 0.000016 0.000027 0.000025 ) M - matrix: 0.021638 -0.014413 0.007204 ( 0.000006 0.000006 0.000005 ) -0.014413 0.028787 -0.014408 ( 0.000006 0.000009 0.000006 ) 0.007204 -0.014408 0.021582 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9064(15) 5.9164(12) 5.9170(14) 59.94(2) 89.96(2) 59.99(2) V = 146.10(5) OTKP changes: 326 1 1 1 OTKP changes: 326 1 1 1 OTKP changes: 326 1 1 1 UB - matrix: -0.103846 -0.015376 0.050100 ( 0.000022 0.000036 0.000033 ) 0.087394 -0.167042 0.063338 ( 0.000013 0.000022 0.000020 ) 0.055879 -0.024440 0.122425 ( 0.000015 0.000024 0.000022 ) M - matrix: 0.021544 -0.014367 0.007174 ( 0.000005 0.000005 0.000005 ) -0.014367 0.028737 -0.014343 ( 0.000005 0.000008 0.000005 ) 0.007174 -0.014343 0.021509 ( 0.000005 0.000005 0.000007 ) UB fit with 326 obs out of 326 (total:326,skipped:0) (100.00%) unit cell: 5.9188(13) 5.9155(10) 5.9209(13) 60.04(2) 90.012(19) 59.99(2) V = 146.63(5) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 73.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 570 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103846 -0.015376 0.050100 ( 0.000022 0.000036 0.000033 ) 0.087394 -0.167042 0.063338 ( 0.000013 0.000022 0.000020 ) 0.055879 -0.024440 0.122425 ( 0.000015 0.000024 0.000022 ) M - matrix: 0.021544 -0.014367 0.007174 ( 0.000005 0.000005 0.000005 ) -0.014367 0.028737 -0.014343 ( 0.000005 0.000008 0.000005 ) 0.007174 -0.014343 0.021509 ( 0.000005 0.000005 0.000007 ) UB fit with 326 obs out of 326 (total:326,skipped:0) (100.00%) unit cell: 5.9188(13) 5.9155(10) 5.9209(13) 60.04(2) 90.012(19) 59.99(2) V = 146.63(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 326 obs out of 326 (total:326,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb 4 of 327 peaks identified as outliers and rejected 323 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 323 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 323 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 32 | 1.008 ( 0.097) | 1.148 ( 0.437) | 1.304 ( 0.854) | 1.41- 1.17 | 32 | 1.060 ( 0.076) | 1.133 ( 0.429) | 1.153 ( 0.669) | 1.17- 1.01 | 32 | 1.099 ( 0.071) | 1.189 ( 0.390) | 1.159 ( 0.514) | 1.01- 0.92 | 32 | 1.154 ( 0.149) | 1.192 ( 0.241) | 1.099 ( 0.425) | 0.92- 0.82 | 32 | 1.146 ( 0.034) | 1.097 ( 0.109) | 1.225 ( 0.463) | 0.82- 0.75 | 32 | 1.167 ( 0.041) | 1.103 ( 0.122) | 1.212 ( 0.441) | 0.75- 0.71 | 32 | 1.171 ( 0.030) | 1.059 ( 0.131) | 1.302 ( 0.477) | 0.71- 0.67 | 32 | 1.182 ( 0.045) | 1.122 ( 0.140) | 1.212 ( 0.388) | 0.67- 0.64 | 32 | 1.167 ( 0.066) | 1.178 ( 0.159) | 1.270 ( 0.461) | 0.63- 0.59 | 35 | 1.207 ( 0.064) | 1.151 ( 0.174) | 1.211 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 323 | 1.137 ( 0.095) | 1.137 ( 0.268) | 1.215 ( 0.541) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 210 | 1.147 ( 0.126) | 1.267 ( 0.423) | 1.339 ( 0.682) | 13.1-18.9 | 210 | 1.141 ( 0.107) | 1.204 ( 0.320) | 1.336 ( 0.687) | 18.9-23.0 | 210 | 1.151 ( 0.091) | 1.204 ( 0.294) | 1.231 ( 0.621) | 23.0-27.3 | 210 | 1.131 ( 0.095) | 1.173 ( 0.306) | 1.220 ( 0.569) | 27.3-30.4 | 210 | 1.138 ( 0.100) | 1.164 ( 0.224) | 1.226 ( 0.455) | 30.4-33.8 | 210 | 1.153 ( 0.089) | 1.140 ( 0.202) | 1.223 ( 0.440) | 33.8-37.0 | 210 | 1.141 ( 0.099) | 1.118 ( 0.163) | 1.160 ( 0.428) | 37.1-39.7 | 210 | 1.156 ( 0.132) | 1.112 ( 0.246) | 1.229 ( 0.520) | 39.7-42.8 | 210 | 1.172 ( 0.104) | 1.115 ( 0.191) | 1.221 ( 0.556) | 42.8-50.0 | 211 | 1.200 ( 0.163) | 1.123 ( 0.281) | 1.185 ( 0.477) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 2101 | 1.153 ( 0.114) | 1.162 ( 0.279) | 1.237 ( 0.554) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.96 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0021 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 462718 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 23405112 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 14:01:40 2018 PROFFITMAIN - Started at Wed Mar 28 14:01:40 2018 OTKP changes: 2101 2 4 5 OTKP changes: 2101 2 4 5 UB - matrix: -0.104087 -0.015142 0.049652 ( 0.000013 0.000014 0.000013 ) 0.087413 -0.167269 0.063726 ( 0.000009 0.000010 0.000009 ) 0.055527 -0.024430 0.122957 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.021558 -0.014402 0.007230 ( 0.000003 0.000002 0.000002 ) -0.014402 0.028805 -0.014415 ( 0.000002 0.000003 0.000002 ) 0.007230 -0.014415 0.021645 ( 0.000002 0.000002 0.000003 ) UB fit with 2101 obs out of 2101 (total:2101,skipped:0) (100.00%) unit cell: 5.9195(7) 5.9101(5) 5.9045(7) 60.055(10) 90.090(9) 60.000(10) V = 146.07(2) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104096 -0.015256 0.049875 ( 0.000026 0.000032 0.000029 ) 0.087349 -0.167028 0.063615 ( 0.000017 0.000021 0.000019 ) 0.055446 -0.024081 0.122542 ( 0.000020 0.000026 0.000023 ) M - matrix: 0.021540 -0.014337 0.007159 ( 0.000007 0.000005 0.000005 ) -0.014337 0.028711 -0.014337 ( 0.000005 0.000007 0.000005 ) 0.007159 -0.014337 0.021551 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(14) 5.9130(10) 5.9126(13) 60.04(2) 90.000(19) 60.03(2) V = 146.39(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104040 -0.015237 0.049838 ( 0.000024 0.000031 0.000027 ) 0.087398 -0.167154 0.063716 ( 0.000017 0.000021 0.000019 ) 0.055457 -0.024184 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021538 -0.014365 0.007180 ( 0.000006 0.000005 0.000005 ) -0.014365 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007180 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.43(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104040 -0.015237 0.049838 ( 0.000024 0.000031 0.000027 ) 0.087398 -0.167154 0.063716 ( 0.000017 0.000021 0.000019 ) 0.055457 -0.024184 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021538 -0.014365 0.007180 ( 0.000006 0.000005 0.000005 ) -0.014365 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007180 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.43(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104040 -0.015237 0.049838 ( 0.000024 0.000031 0.000027 ) 0.087398 -0.167154 0.063716 ( 0.000017 0.000021 0.000019 ) 0.055457 -0.024184 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021538 -0.014365 0.007180 ( 0.000006 0.000005 0.000005 ) -0.014365 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007180 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.43(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104507 -0.014313 0.049165 ( 0.000037 0.000046 0.000040 ) 0.087141 -0.167048 0.063774 ( 0.000025 0.000031 0.000027 ) 0.055324 -0.024939 0.122883 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021576 -0.014441 0.007218 ( 0.000009 0.000007 0.000006 ) -0.014441 0.028732 -0.014422 ( 0.000007 0.000011 0.000007 ) 0.007218 -0.014422 0.021585 ( 0.000006 0.000007 0.000008 ) unit cell: 5.928(2) 5.9380(14) 5.9220(16) 59.89(3) 89.88(2) 59.81(3) V = 146.89(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104434 -0.014617 0.048931 ( 0.000028 0.000035 0.000031 ) 0.087197 -0.167130 0.063644 ( 0.000023 0.000028 0.000025 ) 0.055340 -0.024820 0.123242 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021572 -0.014420 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014420 0.028762 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014411 0.021633 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9227(15) 5.9186(13) 5.9082(16) 60.07(2) 90.14(2) 59.97(2) V = 146.35(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104434 -0.014617 0.048931 ( 0.000028 0.000035 0.000031 ) 0.087197 -0.167130 0.063644 ( 0.000023 0.000028 0.000025 ) 0.055340 -0.024820 0.123242 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021572 -0.014420 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014420 0.028762 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014411 0.021633 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9227(15) 5.9186(13) 5.9082(16) 60.07(2) 90.14(2) 59.97(2) V = 146.35(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146796 -0.097934 0.049179 ( 0.000021 0.000027 0.000023 ) -0.000024 0.138458 -0.069281 ( 0.000023 0.000029 0.000025 ) -0.000024 0.000032 0.119965 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021549 -0.014380 0.007218 ( 0.000006 0.000005 0.000005 ) -0.014380 0.028762 -0.014405 ( 0.000005 0.000010 0.000006 ) 0.007218 -0.014405 0.021610 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9191(11) 5.9158(14) 5.9118(14) 60.00(2) 90.064(17) 60.02(2) V = 146.35(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104318 -0.014895 0.049232 ( 0.000024 0.000020 0.000018 ) 0.087204 -0.167241 0.063673 ( 0.000028 0.000023 0.000020 ) 0.055381 -0.024575 0.123033 ( 0.000023 0.000019 0.000017 ) M - matrix: 0.021554 -0.014391 0.007230 ( 0.000007 0.000006 0.000004 ) -0.014391 0.028795 -0.014406 ( 0.000006 0.000008 0.000004 ) 0.007230 -0.014406 0.021615 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9188(12) 5.9096(10) 5.9091(10) 60.056(18) 90.123(15) 60.03(2) V = 146.19(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104245 -0.015179 0.049357 ( 0.000024 0.000019 0.000017 ) 0.087189 -0.167216 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055263 -0.024223 0.122753 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021523 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028778 -0.014376 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014376 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9146(11) 5.9037(9) 5.9146(9) 60.042(17) 90.128(14) 60.136(18) V = 146.27(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104245 -0.015179 0.049357 ( 0.000024 0.000019 0.000017 ) 0.087189 -0.167216 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055263 -0.024223 0.122753 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021523 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028778 -0.014376 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014376 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9146(11) 5.9037(9) 5.9146(9) 60.042(17) 90.128(14) 60.136(18) V = 146.27(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104245 -0.015179 0.049357 ( 0.000024 0.000019 0.000017 ) 0.087189 -0.167216 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055263 -0.024223 0.122753 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021523 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028778 -0.014376 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014376 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9146(11) 5.9037(9) 5.9146(9) 60.042(17) 90.128(14) 60.136(18) V = 146.27(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 323 obs out of 323 (total:323,skipped:0) (100.00%) UB - matrix: -0.103973 -0.015355 0.050215 ( 0.000022 0.000036 0.000033 ) 0.087386 -0.167049 0.063359 ( 0.000015 0.000025 0.000023 ) 0.056087 -0.024572 0.122558 ( 0.000018 0.000029 0.000027 ) M - matrix: 0.021592 -0.014379 0.007190 ( 0.000006 0.000005 0.000005 ) -0.014379 0.028745 -0.014367 ( 0.000005 0.000009 0.000006 ) 0.007190 -0.014367 0.021556 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9110(14) 5.9147(12) 5.9158(15) 60.01(2) 90.01(2) 60.01(2) V = 146.29(5) OTKP changes: 323 1 1 1 OTKP changes: 323 1 1 1 OTKP changes: 323 1 1 1 UB - matrix: -0.103890 -0.015337 0.050176 ( 0.000021 0.000035 0.000032 ) 0.087531 -0.167206 0.063423 ( 0.000015 0.000025 0.000023 ) 0.055886 -0.024391 0.122442 ( 0.000016 0.000026 0.000024 ) M - matrix: 0.021578 -0.014405 0.007181 ( 0.000005 0.000005 0.000005 ) -0.014405 0.028788 -0.014361 ( 0.000005 0.000009 0.000006 ) 0.007181 -0.014361 0.021532 ( 0.000005 0.000006 0.000007 ) UB fit with 323 obs out of 323 (total:323,skipped:0) (100.00%) unit cell: 5.9171(13) 5.9129(11) 5.9173(13) 60.04(2) 89.981(19) 59.94(2) V = 146.37(5) Run 5 Omega scan: (-2.000 - 73.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.949) HKL list info: 566 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103890 -0.015337 0.050176 ( 0.000021 0.000035 0.000032 ) 0.087531 -0.167206 0.063423 ( 0.000015 0.000025 0.000023 ) 0.055886 -0.024391 0.122442 ( 0.000016 0.000026 0.000024 ) M - matrix: 0.021578 -0.014405 0.007181 ( 0.000005 0.000005 0.000005 ) -0.014405 0.028788 -0.014361 ( 0.000005 0.000009 0.000006 ) 0.007181 -0.014361 0.021532 ( 0.000005 0.000006 0.000007 ) UB fit with 323 obs out of 323 (total:323,skipped:0) (100.00%) unit cell: 5.9171(13) 5.9129(11) 5.9173(13) 60.04(2) 89.981(19) 59.94(2) V = 146.37(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 323 obs out of 323 (total:323,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! 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: -0.103890 -0.015337 0.050176 ( 0.000021 0.000035 0.000032 ) 0.087531 -0.167206 0.063423 ( 0.000015 0.000025 0.000023 ) 0.055886 -0.024391 0.122442 ( 0.000016 0.000026 0.000024 ) M - matrix: 0.021578 -0.014405 0.007181 ( 0.000005 0.000005 0.000005 ) -0.014405 0.028788 -0.014361 ( 0.000005 0.000009 0.000006 ) 0.007181 -0.014361 0.021532 ( 0.000005 0.000006 0.000007 ) UB fit with 323 obs out of 323 (total:323,skipped:0) (100.00%) unit cell: 5.9171(13) 5.9129(11) 5.9173(13) 60.04(2) 89.981(19) 59.94(2) V = 146.37(5) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104024 -0.015141 0.049576 ( 0.000013 0.000014 0.000013 ) 0.087338 -0.167128 0.063690 ( 0.000009 0.000010 0.000009 ) 0.055441 -0.024374 0.122818 ( 0.000011 0.000012 0.000011 ) M - matrix: 0.021523 -0.014373 0.007215 ( 0.000003 0.000002 0.000002 ) -0.014373 0.028755 -0.014389 ( 0.000002 0.000003 0.000002 ) 0.007215 -0.014389 0.021598 ( 0.000002 0.000002 0.000003 ) UB fit with 2101 obs out of 2101 (total:2101,skipped:0) (100.00%) unit cell: 5.9235(7) 5.9147(5) 5.9111(6) 60.047(10) 90.090(9) 60.014(10) V = 146.46(2) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 44 reflections under beam stop or inside a detector rejection region 21 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof 2798 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:01:46 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) Run 5 Omega scan: (-2.000 - 73.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.949) PROFFIT INFO: signal sum: min=162.0000 max=22501328.0000 PROFFIT INFO: signal sum lp corr: min=241.8051 max=3285995.3825 PROFFIT INFO: background sum: min=776.0000 max=16465.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=11710.0000 PROFFIT INFO: num of signal pixels: min=59 max=1013 PROFFIT INFO: Inet: min=527.5747 max=7169445.0000 PROFFIT INFO: sig(Inet): min=191.1273 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=397.48 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 57 208 358 575 631 1120 1851 2529 2797 Percent 0.0 0.1 2.0 7.4 12.8 20.6 22.6 40.0 66.2 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2798 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 2798 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7169445- 1616119 279 2438475.51 133.29 100.00 1614965- 1051490 279 1305733.48 112.07 100.00 1050764- 323746 279 617972.53 95.11 100.00 323226- 221620 279 259096.76 70.12 100.00 221554- 166025 279 191725.64 49.69 100.00 165998- 131720 279 148780.24 37.00 100.00 131710- 102464 279 116846.40 30.66 100.00 102316- 6419 279 59532.96 21.45 100.00 6408- 3633 279 4689.16 5.01 83.87 3632- 528 286 2699.70 3.18 43.01 ------------------------------------------------------------------------------------ 7169445- 528 2797 513274.23 55.63 92.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 279 803458.44 84.09 99.64 1.41- 1.05 279 769052.83 68.14 98.21 1.05- 0.93 279 623682.93 67.03 96.77 0.92- 0.82 279 477242.15 53.77 91.76 0.82- 0.74 279 499593.31 60.92 94.62 0.74- 0.67 279 498730.53 55.90 91.40 0.67- 0.61 279 340667.75 43.40 92.83 0.61- 0.56 279 450066.86 48.04 91.04 0.56- 0.51 279 347613.56 39.12 82.44 0.51- 0.40 286 327299.95 36.35 87.06 ------------------------------------------------------------------------------------ 5.26- 0.40 2797 513274.23 55.63 92.56 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:01:46 2018 Sorting 2797 observations 286 unique observations with > 7.00 F2/sig(F2) 2797 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 73 487 Total number of frames 487 Maximum number of 286 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2797 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 36 246 Total number of frames 246 2255 observations > 7.00 F2/sig(F2) 2255 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 36 246 Total number of frames 246 Removing 'redundancy=1' reflections Average redundancy: 7.9 (Out of 2255 removed 22 = 2233, unique = 284) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2233 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 36 246 Total number of frames 246 284 unique data precomputed (should be 284) 284 unique data with 2233 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.9 (Out of 2233 removed 0 = 2233, unique = 284) 284 unique data precomputed (should be 284) 284 unique data with 2233 observations RMS deviation of equivalent data = 0.74238 Rint = 0.68622 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66722, wR= 3.56588 Trying model 1 (ne=2, no=0)... Results: Rint= 0.73829, wR= 2.69980, Acormin=-0.333, Acormax=2.600, Acor_av=0.615 F test: Probability=0.000, F= 0.815 Trying model 2 (ne=2, no=1)... Results: Rint= 0.83420, wR= 2.40812, Acormin=-0.394, Acormax=2.506, Acor_av=0.389 F test: Probability=0.000, F= 0.637 Trying model 3 (ne=4, no=0)... Results: Rint= 0.73554, wR= 1.93940, Acormin=-0.115, Acormax=2.971, Acor_av=0.564 F test: Probability=0.000, F= 0.817 Trying model 4 (ne=4, no=1)... Results: Rint= 0.85802, wR= 2.57541, Acormin=-0.381, Acormax=2.364, Acor_av=0.363 F test: Probability=0.000, F= 0.599 Trying model 5 (ne=4, no=3)... Results: Rint= 0.95478, wR= 2.13441, Acormin=-0.400, Acormax=3.607, Acor_av=0.145 F test: Probability=0.000, F= 0.482 Trying model 6 (ne=6, no=0)... Results: Rint= 0.74833, wR= 3.00352, Acormin=-0.384, Acormax=3.488, Acor_av=0.502 F test: Probability=0.000, F= 0.784 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87375, wR= 3.19898, Acormin=-0.468, Acormax=2.886, Acor_av=0.323 F test: Probability=0.000, F= 0.574 Trying model 8 (ne=6, no=3)... Results: Rint= 0.93933, wR= 1.94118, Acormin=-0.904, Acormax=3.709, Acor_av=0.130 F test: Probability=0.000, F= 0.495 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96024, wR= 1.81908, Acormin=-0.583, Acormax=3.812, Acor_av=0.082 F test: Probability=0.000, F= 0.471 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86649, wR= 2.10025, Acormin=-0.832, Acormax=2.093, Acor_av=0.256 F test: Probability=0.000, F= 0.579 Trying model 11 (ne=8, no=1)... Results: Rint= 0.91134, wR= 2.94306, Acormin=-0.617, Acormax=1.745, Acor_av=0.174 F test: Probability=0.000, F= 0.523 Trying model 12 (ne=8, no=3)... Results: Rint= 1.00462, wR= 1.73458, Acormin=-0.053, Acormax=0.074, Acor_av=0.001 F test: Probability=0.000, F= 0.429 Trying model 13 (ne=8, no=5)... Results: Rint= 1.00921, wR= 1.69112, Acormin=-0.052, Acormax=0.074, Acor_av=0.001 F test: Probability=0.000, F= 0.422 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00883, wR= 1.66372, Acormin=-0.091, Acormax=0.083, Acor_av=0.000 F test: Probability=0.000, F= 0.419 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: 0.86841 There are 246 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 250 pars with 31375 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74238 Using Levenberg-Marquardt: 0.00010 New wR= 0.72661 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68622 with corrections 0.67844 Rint for all data: 0.86841 with corrections 0.86861 12 observations identified as outliers and rejected Cycle 2 wR= 0.67635 Using Levenberg-Marquardt: 0.00001 New wR= 0.67477 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66684 with corrections 0.65307 Rint for all data: 0.86841 with corrections 0.86719 11 observations identified as outliers and rejected Cycle 3 wR= 0.65054 Using Levenberg-Marquardt: 0.00000 New wR= 0.64892 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65678 with corrections 0.64354 Rint for all data: 0.86841 with corrections 0.86823 17 observations identified as outliers and rejected Cycle 4 wR= 0.62171 Using Levenberg-Marquardt: 0.00000 New wR= 0.61748 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64996 with corrections 0.63753 Rint for all data: 0.86841 with corrections 0.86843 6 observations identified as outliers and rejected Cycle 5 wR= 0.61500 Using Levenberg-Marquardt: 0.00000 New wR= 0.61304 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64339 with corrections 0.63367 Rint for all data: 0.86841 with corrections 0.86882 5 observations identified as outliers and rejected Final wR= 0.61304 Final frame scales: Min= 1.0000 Max= 4.2154 Final absorption correction factors: Amin= 0.4951 Amax= 1.4466 PROFFIT INFO: Inet (after scale3 abspack): min=465.5399 max=7103216.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=187.0785 max=90413.4766 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2797 reflections read from tmp file 2147 reflections are rejected (2077 as outliers, 70 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 74 62 30 15 8 4 2 1 2 Initial Chi^2= 0.55831 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.20701 Current error model SIG(F2)^2 = 228.81*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 276.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 276.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7103217- 1537110 279 2472713.48 82.84 100.00 1529771- 962233 279 1222114.23 45.30 100.00 961663- 321382 279 607261.56 39.43 100.00 321170- 212866 279 262063.46 29.19 100.00 212212- 158194 279 181863.54 19.75 100.00 158058- 124216 279 141070.59 15.50 100.00 123984- 95889 279 110160.06 12.37 100.00 95474- 6486 279 56921.10 9.35 96.06 6467- 3389 279 4531.24 2.89 30.11 3379- 466 286 2525.93 2.26 11.89 ------------------------------------------------------------------------------------ 7103217- 466 2797 504862.18 25.83 83.63 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 279 942425.15 51.46 95.70 1.41- 1.05 279 797296.24 38.34 91.04 1.05- 0.93 279 644593.16 30.33 88.89 0.92- 0.82 279 473176.43 24.04 81.36 0.82- 0.74 279 454215.56 24.76 84.23 0.74- 0.67 279 474734.88 22.36 81.36 0.67- 0.61 279 310466.96 17.49 80.65 0.61- 0.56 279 404686.78 19.27 79.93 0.56- 0.51 279 299236.47 15.81 75.27 0.51- 0.40 286 254082.14 14.72 77.97 ------------------------------------------------------------------------------------ 5.26- 0.40 2797 504862.18 25.83 83.63 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 279 942425.15 51.46 95.70 5.26- 1.05 558 869860.69 44.90 93.37 5.26- 0.93 837 794771.52 40.04 91.88 5.26- 0.82 1116 714372.74 36.04 89.25 5.26- 0.74 1395 662341.31 33.78 88.24 5.26- 0.67 1674 631073.57 31.88 87.10 5.26- 0.61 1953 585272.62 29.82 86.18 5.26- 0.56 2232 562699.39 28.50 85.39 5.26- 0.51 2511 533425.73 27.09 84.27 5.26- 0.40 2797 504862.18 25.83 83.63 ------------------------------------------------------------------------------------ 5.26- 0.40 2797 504862.18 25.83 83.63 Scale applied to data: s=0.140781 (maximum obs:7103216.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.869; Rsigma 0.025: data 2797 -> merged 318 With outlier rejection... Rint 0.805; Rsigma 0.025: data 2679 -> merged 318 Rejected total: 118, method kkm 104, method Blessing 14 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404280, 5.271168 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 13.80 100.00 207 1.46 - 1.12 15 15 19.67 100.00 295 1.08 - 0.96 15 15 18.13 100.00 272 0.96 - 0.86 15 15 17.20 100.00 258 0.86 - 0.79 15 15 14.07 100.00 211 0.79 - 0.73 15 15 11.00 100.00 165 0.73 - 0.69 15 15 10.67 100.00 160 0.69 - 0.65 15 15 10.27 100.00 154 0.65 - 0.63 15 15 6.93 100.00 104 0.63 - 0.60 21 21 7.90 100.00 166 --------------------------------------------------------------- 5.92 - 0.60 156 156 12.77 100.00 1992 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:01:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.923515 5.914703 5.911104 60.0471 90.0904 60.0135 2679 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1329 1405 1328 1363 2031 1799 1772 2679 N (int>3sigma) = 0 1067 1405 1066 1105 1769 1515 1482 2241 Mean intensity = 0.0 61.2 27.5 61.5 68.4 49.6 68.8 67.0 68.0 Mean int/sigma = 0.0 23.9 20.9 24.2 25.1 23.0 25.5 25.4 25.6 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.915 90.03 119.95 119.91 Niggli form: a.a = 34.941 b.b = 34.968 c.c = 34.984 b.c = -0.017 a.c = -17.456 a.b = -17.430 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.155 CUBIC F-lattice R(int) = 0.190 [ 2524] Vol = 585.8 Cell: 8.366 8.375 8.362 90.12 89.99 89.97 Volume: 585.84 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.140 RHOMBOHEDRAL R-lattice R(int) = 0.176 [ 2250] Vol = 439.4 Cell: 5.920 5.913 14.501 89.96 90.10 120.06 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.140 RHOMBOHEDRAL R-lattice R(int) = 0.175 [ 712] Vol = 439.4 Trigonal Cell: 5.920 5.913 14.501 89.96 90.10 120.06 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.176 [ 2282] Vol = 292.9 Cell: 5.917 5.920 8.362 89.92 89.91 89.94 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.134 TETRAGONAL I-lattice R(int) = 0.176 [ 2282] Vol = 292.9 Cell: 5.920 5.917 8.362 90.09 90.08 89.94 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.177 [ 2229] Vol = 292.9 Cell: 5.920 5.917 8.362 89.91 89.92 89.94 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.161 [ 2230] Vol = 292.9 Cell: 5.911 8.366 5.924 90.01 89.91 90.03 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.047 MONOCLINIC I-lattice R(int) = 0.149 [ 1891] Vol = 292.9 Cell: 5.917 5.920 8.362 90.08 90.09 89.94 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.064 MONOCLINIC I-lattice R(int) = 0.148 [ 1901] Vol = 292.9 Cell: 5.911 5.924 8.366 89.99 90.03 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.028 MONOCLINIC I-lattice R(int) = 0.151 [ 1924] Vol = 292.9 Cell: 5.911 8.366 5.924 90.01 90.09 89.97 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.116 MONOCLINIC C-lattice R(int) = 0.159 [ 1903] Vol = 292.9 Cell: 10.248 5.913 5.915 90.03 125.19 89.90 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.128 [ 1319] Vol = 146.5 Cell: 5.911 5.913 5.915 90.03 119.95 119.91 Volume: 146.46 Matrix: 0.0000 0.0000 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 1405 0 1785 1799 2679 N (int>3sigma) = 0 0 0 0 1405 0 1503 1515 2241 Mean intensity = 0.0 0.0 0.0 0.0 27.5 0.0 68.2 68.8 68.0 Mean int/sigma = 0.0 0.0 0.0 0.0 20.9 0.0 25.7 25.5 25.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 22 22 209 620 N I>3s 13 13 82 620 0.7 0.7 0.6 32.5 5.8 5.8 3.3 25.6 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 0.190 2335 Fd-3m 1 1 227 C N N N N 37 2284 0.192 2373 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365716 8.374943 8.361740 90.1202 89.9873 89.9689 ZERR 1.00 0.002601 0.001602 0.000272 0.0003 0.0101 0.0004 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3578581- 891915 338 312 31 10.1 1406840.46 54.50 0.636 0.520 875766- 671779 365 360 31 11.6 761241.40 33.52 0.939 0.853 664684- 533464 338 327 31 10.5 560221.94 29.45 0.948 0.907 526161- 431901 348 343 31 11.1 452637.73 28.98 0.904 1.034 431194- 332460 297 286 31 9.2 338109.26 20.18 0.940 1.097 332167- 253092 312 282 31 9.1 228672.28 18.51 0.797 0.894 250925- 127928 262 249 31 8.0 147435.29 14.33 0.660 0.666 124110- 101171 196 189 31 6.1 112022.17 12.91 0.435 0.281 100026- 72793 203 197 31 6.4 86579.53 9.88 0.578 0.484 72113- 1194 138 134 39 3.4 46043.07 6.43 0.739 0.721 ------------------------------------------------------------------------------------------- 3578581- 1194 2797 2679 318 8.4 482912.58 25.55 0.805 0.759 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 556 533 31 17.2 822624.01 44.64 0.787 0.812 0.015 1.05-0.83 538 528 31 17.0 554182.93 27.39 0.930 1.047 0.023 0.83-0.72 400 391 33 11.8 453730.68 23.67 0.777 0.825 0.028 0.72-0.65 331 318 32 9.9 355940.89 19.66 0.876 0.897 0.031 0.64-0.60 253 239 31 7.7 380918.53 18.86 0.784 0.811 0.033 0.59-0.56 210 196 32 6.1 259717.72 15.08 0.747 0.648 0.041 0.56-0.52 175 164 31 5.3 346343.81 17.76 0.689 0.657 0.037 0.52-0.49 137 128 31 4.1 230854.33 13.46 0.688 0.567 0.041 0.49-0.46 111 105 31 3.4 252774.51 14.43 0.484 0.398 0.043 0.46-0.40 86 77 35 2.2 223668.01 13.99 0.217 0.163 0.046 ------------------------------------------------------------------------------------------------------ inf-0.40 2797 2679 318 8.4 482912.58 25.55 0.805 0.759 0.025 inf-0.60 2057 1992 156 12.8 557323.77 29.12 0.833 0.876 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 533 31 31 100.0 17.2 822624.01 203.48 0.787 0.005 1.05-0.83 528 31 31 100.0 17.0 554182.93 137.75 0.930 0.008 0.83-0.72 391 33 33 100.0 11.8 453730.68 95.98 0.777 0.011 0.72-0.65 318 32 32 100.0 9.9 355940.89 81.10 0.876 0.015 0.64-0.60 239 31 31 100.0 7.7 380918.53 66.21 0.784 0.016 0.59-0.56 196 36 32 88.9 6.1 259717.72 47.96 0.747 0.022 0.56-0.52 164 35 31 88.6 5.3 346343.81 49.94 0.689 0.020 0.52-0.49 128 45 31 68.9 4.1 230854.33 34.11 0.688 0.022 0.49-0.46 105 54 31 57.4 3.4 252774.51 31.05 0.484 0.026 0.46-0.40 77 130 35 26.9 2.2 223668.01 23.20 0.217 0.031 -------------------------------------------------------------------------------------------- inf-0.40 2679 459 318 69.3 8.4 482912.58 107.25 0.805 0.014 inf-0.60 1992 156 156 100.0 12.8 557323.77 130.31 0.833 0.009 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007570 0.076798 -0.034794 ( 0.000007 0.000008 0.000007 ) -0.083562 -0.011824 -0.008050 ( 0.000005 0.000005 0.000005 ) -0.012186 0.033690 0.076942 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007188 -0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007173 0.000015 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000015 0.007195 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007570 0.076798 -0.034794 ( 0.000007 0.000008 0.000007 ) -0.083562 -0.011824 -0.008050 ( 0.000005 0.000005 0.000005 ) -0.012186 0.033690 0.076942 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3659(5) 8.3751(7) 8.3618(6) 90.121(6) 89.988(5) 89.969(6) V = 585.87(7) unit cell: 8.36760(19) 8.36760(19) 8.36760(19) 90.0 90.0 90.0 V = 585.87(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.949) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.949) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.949) Run 5 Omega scan: (-2.000 - 73.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.949) PROFFIT INFO: signal sum: min=162.0000 max=22501328.0000 PROFFIT INFO: signal sum lp corr: min=241.8051 max=3285995.3825 PROFFIT INFO: background sum: min=776.0000 max=16465.0000 PROFFIT INFO: background sum sig2: min=601.0000 max=11710.0000 PROFFIT INFO: num of signal pixels: min=59 max=1013 PROFFIT INFO: Inet: min=527.5747 max=7169445.0000 PROFFIT INFO: sig(Inet): min=191.1273 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=397.48 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 114 416 716 1150 1262 2240 3702 5058 5594 Percent 0.0 0.1 2.0 7.4 12.8 20.6 22.6 40.0 66.2 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2798 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 2798 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7169445- 1616119 279 2438475.51 133.29 100.00 1614965- 1051490 279 1305733.48 112.07 100.00 1050764- 323746 279 617972.53 95.11 100.00 323226- 221620 279 259096.76 70.12 100.00 221554- 166025 279 191725.64 49.69 100.00 165998- 131720 279 148780.24 37.00 100.00 131710- 102464 279 116846.40 30.66 100.00 102316- 6419 279 59532.96 21.45 100.00 6408- 3633 279 4689.16 5.01 83.87 3632- 528 286 2699.70 3.18 43.01 ------------------------------------------------------------------------------------ 7169445- 528 2797 513274.23 55.63 92.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 279 857820.77 89.42 100.00 1.41- 1.12 279 831795.27 71.78 98.57 1.12- 0.96 279 641997.60 73.57 98.92 0.96- 0.88 279 493119.68 60.72 95.34 0.88- 0.81 279 656010.72 70.30 97.49 0.81- 0.74 279 364528.55 42.56 92.83 0.74- 0.71 279 266075.51 36.34 91.40 0.71- 0.65 279 525839.63 52.18 95.34 0.65- 0.62 279 258200.21 29.99 74.55 0.62- 0.58 286 244107.61 30.05 81.47 ------------------------------------------------------------------------------------ 4.82- 0.58 2797 513274.23 55.63 92.56 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:01:47 2018 Sorting 2797 observations 85 unique observations with > 7.00 F2/sig(F2) 2797 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 73 487 Total number of frames 487 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2797 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 12 84 Total number of frames 84 2255 observations > 7.00 F2/sig(F2) 2255 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 12 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 25.3 (Out of 2255 removed 6 = 2249, unique = 89) 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 2249 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 12 84 Total number of frames 84 89 unique data precomputed (should be 89) 89 unique data with 2249 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 25.3 (Out of 2249 removed 0 = 2249, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 2249 observations RMS deviation of equivalent data = 0.21819 Rint = 0.17021 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16831, wR= 0.22297 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08294, wR= 0.10864, Acormin=0.639, Acormax=1.424, Acor_av=0.934 F test: Probability=1.000, F= 4.109 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08382, wR= 0.10313, Acormin=0.608, Acormax=1.396, Acor_av=0.891 F test: Probability=0.000, F= 0.978 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06982, wR= 0.09612, Acormin=0.668, Acormax=1.530, Acor_av=0.918 F test: Probability=1.000, F= 1.405 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06473, wR= 0.08670, Acormin=0.607, Acormax=1.473, Acor_av=0.887 F test: Probability=1.000, F= 1.162 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06207, wR= 0.08294, Acormin=0.512, Acormax=1.308, Acor_av=0.802 F test: Probability=0.969, F= 1.084 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06447, wR= 0.08867, Acormin=0.632, Acormax=1.521, Acor_av=0.891 F test: Probability=0.000, F= 0.926 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06079, wR= 0.08162, Acormin=0.595, Acormax=1.513, Acor_av=0.869 F test: Probability=0.816, F= 1.040 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05804, wR= 0.07652, Acormin=0.502, Acormax=1.381, Acor_av=0.795 F test: Probability=0.998, F= 1.137 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04948, wR= 0.06989, Acormin=0.411, Acormax=1.252, Acor_av=0.687 F test: Probability=1.000, F= 1.369 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06207, wR= 0.08018, Acormin=0.465, Acormax=1.339, Acor_av=0.783 F test: Probability=0.000, F= 0.637 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05892, wR= 0.07650, Acormin=0.522, Acormax=1.403, Acor_av=0.802 F test: Probability=0.000, F= 0.706 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05272, wR= 0.06787, Acormin=0.265, Acormax=0.736, Acor_av=0.419 F test: Probability=0.000, F= 0.878 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04553, wR= 0.06025, Acormin=0.292, Acormax=0.835, Acor_av=0.473 F test: Probability=1.000, F= 1.172 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04139, wR= 0.05555, Acormin=0.310, Acormax=1.056, Acor_av=0.512 F test: Probability=1.000, F= 1.408 Final absorption model (ne=8, no=7): Rint= 0.04139, Acormin=0.310, Acormax=1.056, Acor_av=0.512 Combined refinement in use Rint: 0.17032 There are 84 active scales (one needs to be fixed) Refinement control: frame scale #63 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21819 Using Levenberg-Marquardt: 0.00010 New wR= 0.04655 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17021 with corrections 0.03392 Rint for all data: 0.17032 with corrections 0.03412 3 observations identified as outliers and rejected Cycle 2 wR= 0.04401 Using Levenberg-Marquardt: 0.00001 New wR= 0.04108 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.03079 Rint for all data: 0.17032 with corrections 0.03144 3 observations identified as outliers and rejected Cycle 3 wR= 0.03995 Using Levenberg-Marquardt: 0.00000 New wR= 0.03915 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17014 with corrections 0.02931 Rint for all data: 0.17032 with corrections 0.03085 0 observations identified as outliers and rejected Cycle 4 wR= 0.03915 Using Levenberg-Marquardt: 0.00000 New wR= 0.03893 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17014 with corrections 0.02909 Rint for all data: 0.17032 with corrections 0.03063 0 observations identified as outliers and rejected Cycle 5 wR= 0.03893 Using Levenberg-Marquardt: 0.00000 New wR= 0.03878 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17014 with corrections 0.02893 Rint for all data: 0.17032 with corrections 0.03048 0 observations identified as outliers and rejected Final wR= 0.03878 Final frame scales: Min= 0.8448 Max= 1.0809 Final absorption correction factors: Amin= 0.4314 Amax= 1.3754 PROFFIT INFO: Inet (after scale3 abspack): min=539.7397 max=5883121.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=166.9111 max=68957.5781 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2797 reflections read from tmp file 306 reflections are rejected (304 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 2 1 3 2 5 4 2 85 Initial Chi^2= 0.33019 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.87650 Current error model SIG(F2)^2 = 124.57*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 233.76*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 233.76*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5883121- 1601279 279 2372260.96 93.27 100.00 1597542- 1014486 279 1243535.60 46.44 100.00 1014315- 338673 279 619038.75 45.41 100.00 337799- 204612 279 251425.43 30.59 100.00 204590- 172189 279 187157.16 21.38 100.00 172050- 127362 279 142784.10 15.53 100.00 127327- 102491 279 115219.51 13.31 100.00 102346- 5892 279 61391.56 9.95 97.49 5865- 3474 279 4394.80 3.11 39.78 3472- 540 286 2703.77 2.40 16.08 ------------------------------------------------------------------------------------ 5883121- 540 2797 498746.61 28.07 85.16 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 279 900272.83 61.94 99.64 1.41- 1.12 279 844049.20 44.62 93.91 1.12- 0.96 279 606374.29 33.85 92.47 0.96- 0.88 279 475203.61 26.36 84.59 0.88- 0.81 279 620643.93 30.33 94.27 0.81- 0.74 279 339271.53 18.70 77.78 0.74- 0.71 279 253738.87 16.00 78.14 0.71- 0.65 279 487714.47 22.62 90.32 0.65- 0.62 279 239770.42 13.35 66.67 0.62- 0.58 286 227238.99 13.34 74.13 ------------------------------------------------------------------------------------ 4.82- 0.58 2797 498746.61 28.07 85.16 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 279 900272.83 61.94 99.64 4.82- 1.12 558 872161.02 53.28 96.77 4.82- 0.96 837 783565.44 46.80 95.34 4.82- 0.88 1116 706474.99 41.69 92.65 4.82- 0.81 1395 689308.77 39.42 92.97 4.82- 0.74 1674 630969.23 35.97 90.44 4.82- 0.71 1953 577079.18 33.11 88.68 4.82- 0.65 2232 565908.59 31.80 88.89 4.82- 0.62 2511 529671.02 29.75 86.42 4.82- 0.58 2797 498746.61 28.07 85.16 ------------------------------------------------------------------------------------ 4.82- 0.58 2797 498746.61 28.07 85.16 Scale applied to data: s=0.169978 (maximum obs:5883121.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.023: data 2797 -> merged 109 With outlier rejection... Rint 0.027; Rsigma 0.023: data 2779 -> merged 109 Rejected total: 18, method kkm 11, method Blessing 7 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585849, 4.831034 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 15.90 100.00 159 1.61 - 1.21 10 10 25.10 100.00 251 1.17 - 1.01 10 10 33.40 100.00 334 0.99 - 0.89 10 10 32.90 100.00 329 0.88 - 0.81 10 10 31.50 100.00 315 0.81 - 0.74 10 10 27.50 100.00 275 0.73 - 0.71 10 10 29.70 100.00 297 0.70 - 0.66 10 10 25.20 100.00 252 0.66 - 0.64 10 10 23.50 100.00 235 0.63 - 0.60 10 10 23.70 100.00 237 --------------------------------------------------------------- 5.92 - 0.60 100 100 26.84 100.00 2684 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:01:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.923515 5.914703 5.911104 60.0471 90.0904 60.0135 2679 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1329 1405 1328 1363 2031 1799 1772 2679 N (int>3sigma) = 0 1067 1405 1066 1105 1769 1515 1482 2241 Mean intensity = 0.0 61.2 27.5 61.5 68.4 49.6 68.8 67.0 68.0 Mean int/sigma = 0.0 23.9 20.9 24.2 25.1 23.0 25.5 25.4 25.6 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.911 5.913 5.915 90.03 119.95 119.91 Niggli form: a.a = 34.941 b.b = 34.968 c.c = 34.984 b.c = -0.017 a.c = -17.456 a.b = -17.430 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.155 CUBIC F-lattice R(int) = 0.190 [ 2524] Vol = 585.8 Cell: 8.366 8.375 8.362 90.12 89.99 89.97 Volume: 585.84 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.140 RHOMBOHEDRAL R-lattice R(int) = 0.176 [ 2250] Vol = 439.4 Cell: 5.920 5.913 14.501 89.96 90.10 120.06 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.140 RHOMBOHEDRAL R-lattice R(int) = 0.175 [ 712] Vol = 439.4 Trigonal Cell: 5.920 5.913 14.501 89.96 90.10 120.06 Volume: 439.38 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.176 [ 2282] Vol = 292.9 Cell: 5.917 5.920 8.362 89.92 89.91 89.94 Volume: 292.92 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.134 TETRAGONAL I-lattice R(int) = 0.176 [ 2282] Vol = 292.9 Cell: 5.920 5.917 8.362 90.09 90.08 89.94 Volume: 292.92 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.177 [ 2229] Vol = 292.9 Cell: 5.920 5.917 8.362 89.91 89.92 89.94 Volume: 292.92 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.161 [ 2230] Vol = 292.9 Cell: 5.911 8.366 5.924 90.01 89.91 90.03 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.047 MONOCLINIC I-lattice R(int) = 0.149 [ 1891] Vol = 292.9 Cell: 5.917 5.920 8.362 90.08 90.09 89.94 Volume: 292.92 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.064 MONOCLINIC I-lattice R(int) = 0.148 [ 1901] Vol = 292.9 Cell: 5.911 5.924 8.366 89.99 90.03 90.09 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.028 MONOCLINIC I-lattice R(int) = 0.151 [ 1924] Vol = 292.9 Cell: 5.911 8.366 5.924 90.01 90.09 89.97 Volume: 292.92 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.116 MONOCLINIC C-lattice R(int) = 0.159 [ 1903] Vol = 292.9 Cell: 10.248 5.913 5.915 90.03 125.19 89.90 Volume: 292.92 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.128 [ 1319] Vol = 146.5 Cell: 5.911 5.913 5.915 90.03 119.95 119.91 Volume: 146.46 Matrix: 0.0000 0.0000 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 1405 0 1785 1799 2679 N (int>3sigma) = 0 0 0 0 1405 0 1503 1515 2241 Mean intensity = 0.0 0.0 0.0 0.0 27.5 0.0 68.2 68.8 68.0 Mean int/sigma = 0.0 0.0 0.0 0.0 20.9 0.0 25.7 25.5 25.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.157 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 22 22 209 620 N I>3s 13 13 82 620 0.7 0.7 0.6 32.5 5.8 5.8 3.3 25.6 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 0.190 2335 Fd-3m 1 1 227 C N N N N 37 2284 0.192 2373 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365716 8.374943 8.361740 90.1202 89.9873 89.9689 ZERR 1.00 0.002601 0.001602 0.000272 0.0003 0.0101 0.0004 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5834751- 924776 626 614 27 22.7 1689973.75 64.46 0.024 0.029 884012- 161218 825 820 27 30.4 288270.58 31.16 0.031 0.040 144751- 54732 693 693 27 25.7 113774.96 13.33 0.045 0.061 22452- 1936 653 652 28 23.3 4702.48 3.14 0.149 0.186 ------------------------------------------------------------------------------------------- 5834751- 1936 2797 2779 109 25.5 487922.93 27.50 0.027 0.032 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 696 683 27 25.3 773778.79 48.06 0.025 0.027 0.014 1.01-0.78 827 827 27 30.6 500105.29 26.39 0.024 0.031 0.023 0.78-0.65 760 757 27 28.0 377325.01 19.18 0.030 0.038 0.032 0.65-0.59 514 512 28 18.3 250439.06 14.16 0.038 0.047 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 2797 2779 109 25.5 487922.93 27.50 0.027 0.032 0.023 inf-0.60 2698 2682 99 27.1 498720.40 28.04 0.027 0.032 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 683 27 27 100.0 25.3 773778.79 249.98 0.025 0.003 1.01-0.78 827 27 27 100.0 30.6 500105.29 150.43 0.024 0.004 0.78-0.65 757 27 27 100.0 28.0 377325.01 105.32 0.030 0.007 0.65-0.59 512 29 28 96.6 18.3 250439.06 69.27 0.038 0.012 -------------------------------------------------------------------------------------------- inf-0.59 2779 110 109 99.1 25.5 487922.93 147.65 0.027 0.005 inf-0.60 2682 99 99 100.0 27.1 498720.40 151.33 0.027 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:06:46 2018) ID: 2932; threads 39; handles 876; mem 520304.00 (1237724.00)kB; time: 1w 5d 23h 12m 16s MEMORY INFO: Memory PF:14.0, Ph:180.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.1,peak PF: 708.5, WS: 271.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:16.0, Ph:180.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:509.9,peak PF: 708.5, WS: 273.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:06:46 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000009 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000011 0.000012 0.000011 ) 5.91535 ( 0.00068 ) 5.92288 ( 0.00049 ) 5.91286 ( 0.00065 ) 59.95509 ( 0.01005 ) 89.89521 ( 0.00915 ) 59.99590 ( 0.01032 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 14:06:46 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000013 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000009 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000011 0.000012 0.000011 ) M - matrix: 0.021523 -0.014373 0.007215 ( 0.000003 0.000002 0.000002 ) -0.014373 0.028755 -0.014389 ( 0.000002 0.000003 0.000002 ) 0.007215 -0.014389 0.021598 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(6) 59.955(10) 89.895(9) 59.996(10) V = 146.51(2) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 453 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 44 | 1.225 ( 0.087) | 1.202 ( 0.224) | 1.348 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 442 peaks identified as outliers and rejected 438 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 438 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 438 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.89 | 44 | 1.139 ( 0.066) | 1.101 ( 0.081) | 1.136 ( 0.385) | 0.89- 0.82 | 44 | 1.182 ( 0.069) | 1.109 ( 0.091) | 1.190 ( 0.418) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.096 ( 0.090) | 1.278 ( 0.365) | 0.75- 0.71 | 44 | 1.217 ( 0.055) | 1.095 ( 0.118) | 1.289 ( 0.501) | 0.71- 0.67 | 44 | 1.249 ( 0.054) | 1.132 ( 0.150) | 1.273 ( 0.494) | 0.67- 0.63 | 44 | 1.244 ( 0.069) | 1.112 ( 0.152) | 1.498 ( 0.539) | 0.63- 0.59 | 42 | 1.289 ( 0.070) | 1.115 ( 0.182) | 1.322 ( 0.541) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 438 | 1.176 ( 0.134) | 1.110 ( 0.253) | 1.265 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086839 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021445 -0.014343 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014343 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 UB - matrix: -0.104420 -0.014288 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086790 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) unit cell: 5.9348(14) 5.9354(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104420 -0.014288 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086790 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) unit cell: 5.9348(14) 5.9354(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 438 obs out of 438 (total:438,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 442 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.044 ( 0.244) | 1.215 ( 0.698) | 1.367 ( 1.055) | 1.61- 1.17 | 44 | 1.095 ( 0.151) | 1.144 ( 0.391) | 1.316 ( 0.864) | 1.17- 0.99 | 44 | 1.109 ( 0.073) | 1.088 ( 0.082) | 1.163 ( 0.450) | 0.99- 0.92 | 44 | 1.142 ( 0.067) | 1.104 ( 0.084) | 1.101 ( 0.369) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.163 ( 0.385) | 0.82- 0.76 | 44 | 1.203 ( 0.051) | 1.096 ( 0.090) | 1.320 ( 0.430) | 0.76- 0.71 | 44 | 1.218 ( 0.054) | 1.094 ( 0.127) | 1.261 ( 0.525) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.136 ( 0.144) | 1.310 ( 0.491) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.118 ( 0.156) | 1.445 ( 0.543) | 0.63- 0.59 | 43 | 1.294 ( 0.075) | 1.115 ( 0.180) | 1.329 ( 0.577) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 439 | 1.176 ( 0.131) | 1.122 ( 0.278) | 1.278 ( 0.615) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb PROFFITPEAK info: 1101 peaks in the peak location table UB fit with 504 obs out of 521 (total:521,skipped:0) (96.74%) UB - matrix: -0.103822 -0.015274 0.050063 ( 0.000037 0.000066 0.000058 ) 0.087243 -0.166932 0.063294 ( 0.000033 0.000059 0.000052 ) 0.055983 -0.024399 0.122438 ( 0.000033 0.000059 0.000052 ) M - matrix: 0.021524 -0.014344 0.007179 ( 0.000010 0.000011 0.000009 ) -0.014344 0.028695 -0.014318 ( 0.000011 0.000020 0.000012 ) 0.007179 -0.014318 0.021504 ( 0.000009 0.000012 0.000015 ) unit cell: 5.920(2) 5.915(2) 5.919(3) 60.09(5) 90.09(4) 60.03(4) V = 146.73(11) UB fit with 504 obs out of 521 (total:521,skipped:0) (96.74%) UB - matrix: -0.103822 -0.015274 0.050063 ( 0.000037 0.000066 0.000058 ) 0.087243 -0.166932 0.063294 ( 0.000033 0.000059 0.000052 ) 0.055983 -0.024399 0.122438 ( 0.000033 0.000059 0.000052 ) M - matrix: 0.021524 -0.014344 0.007179 ( 0.000010 0.000011 0.000009 ) -0.014344 0.028695 -0.014318 ( 0.000011 0.000020 0.000012 ) 0.007179 -0.014318 0.021504 ( 0.000009 0.000012 0.000015 ) unit cell: 5.920(2) 5.915(2) 5.919(3) 60.09(5) 90.09(4) 60.03(4) V = 146.73(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.103719 -0.015342 0.049984 ( 0.000037 0.000066 0.000058 ) 0.087375 -0.167048 0.063317 ( 0.000031 0.000057 0.000050 ) 0.055814 -0.024330 0.122314 ( 0.000032 0.000057 0.000050 ) M - matrix: 0.021507 -0.014363 0.007175 ( 0.000010 0.000010 0.000009 ) -0.014363 0.028732 -0.014320 ( 0.000010 0.000019 0.000012 ) 0.007175 -0.014320 0.021468 ( 0.000009 0.000012 0.000015 ) UB fit with 506 obs out of 521 (total:521,skipped:0) (97.12%) unit cell: 5.926(2) 5.915(2) 5.925(3) 60.09(4) 90.07(4) 59.99(4) V = 146.92(10) UB fit with 506 obs out of 521 (total:521,skipped:0) (97.12%) UB - matrix: -0.103719 -0.015342 0.049984 ( 0.000037 0.000066 0.000058 ) 0.087375 -0.167048 0.063317 ( 0.000031 0.000057 0.000050 ) 0.055814 -0.024330 0.122314 ( 0.000032 0.000057 0.000050 ) M - matrix: 0.021507 -0.014363 0.007175 ( 0.000010 0.000010 0.000009 ) -0.014363 0.028732 -0.014320 ( 0.000010 0.000019 0.000012 ) 0.007175 -0.014320 0.021468 ( 0.000009 0.000012 0.000015 ) unit cell: 5.926(2) 5.915(2) 5.925(3) 60.09(4) 90.07(4) 59.99(4) V = 146.92(10) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.103719 -0.015342 0.049984 ( 0.000037 0.000066 0.000058 ) 0.087375 -0.167048 0.063317 ( 0.000031 0.000057 0.000050 ) 0.055814 -0.024330 0.122314 ( 0.000032 0.000057 0.000050 ) M - matrix: 0.021507 -0.014363 0.007175 ( 0.000010 0.000010 0.000009 ) -0.014363 0.028732 -0.014320 ( 0.000010 0.000019 0.000012 ) 0.007175 -0.014320 0.021468 ( 0.000009 0.000012 0.000015 ) UB fit with 506 obs out of 521 (total:521,skipped:0) (97.12%) unit cell: 5.926(2) 5.915(2) 5.925(3) 60.09(4) 90.07(4) 59.99(4) V = 146.92(10) 521 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Run 5 Omega scan: (-2.000 - 98.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103719 -0.015342 0.049984 ( 0.000037 0.000066 0.000058 ) 0.087375 -0.167048 0.063317 ( 0.000031 0.000057 0.000050 ) 0.055814 -0.024330 0.122314 ( 0.000032 0.000057 0.000050 ) M - matrix: 0.021507 -0.014363 0.007175 ( 0.000010 0.000010 0.000009 ) -0.014363 0.028732 -0.014320 ( 0.000010 0.000019 0.000012 ) 0.007175 -0.014320 0.021468 ( 0.000009 0.000012 0.000015 ) UB fit with 506 obs out of 521 (total:521,skipped:0) (97.12%) unit cell: 5.926(2) 5.915(2) 5.925(3) 60.09(4) 90.07(4) 59.99(4) V = 146.92(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 521 (total:521,skipped:0) (97.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb 4 of 441 peaks identified as outliers and rejected 437 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 437 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 437 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 44 | 1.021 ( 0.146) | 1.196 ( 0.566) | 1.414 ( 1.148) | 1.41- 1.17 | 44 | 1.073 ( 0.112) | 1.191 ( 0.472) | 1.082 ( 0.519) | 1.17- 1.02 | 44 | 1.092 ( 0.063) | 1.127 ( 0.237) | 1.191 ( 0.526) | 1.01- 0.92 | 44 | 1.114 ( 0.060) | 1.145 ( 0.342) | 1.101 ( 0.412) | 0.92- 0.82 | 44 | 1.153 ( 0.036) | 1.109 ( 0.098) | 1.111 ( 0.436) | 0.82- 0.75 | 44 | 1.172 ( 0.043) | 1.096 ( 0.115) | 1.326 ( 0.501) | 0.75- 0.71 | 44 | 1.171 ( 0.027) | 1.087 ( 0.123) | 1.250 ( 0.503) | 0.71- 0.67 | 44 | 1.193 ( 0.050) | 1.132 ( 0.141) | 1.235 ( 0.398) | 0.67- 0.62 | 44 | 1.185 ( 0.072) | 1.165 ( 0.160) | 1.184 ( 0.470) | 0.62- 0.59 | 41 | 1.224 ( 0.072) | 1.156 ( 0.180) | 1.312 ( 0.590) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 437 | 1.139 ( 0.097) | 1.140 ( 0.291) | 1.220 ( 0.597) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 437 obs out of 437 (total:437,skipped:0) (100.00%) UB - matrix: -0.103890 -0.015546 0.050200 ( 0.000017 0.000031 0.000026 ) 0.087735 -0.167270 0.063518 ( 0.000015 0.000027 0.000023 ) 0.055919 -0.024517 0.122420 ( 0.000014 0.000027 0.000023 ) M - matrix: 0.021618 -0.014431 0.007203 ( 0.000005 0.000005 0.000004 ) -0.014431 0.028822 -0.014406 ( 0.000005 0.000009 0.000006 ) 0.007203 -0.014406 0.021541 ( 0.000004 0.000006 0.000007 ) unit cell: 5.9125(11) 5.9159(11) 5.9231(13) 59.95(2) 89.959(17) 59.95(2) V = 146.32(5) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 UB - matrix: -0.103827 -0.015335 0.050064 ( 0.000015 0.000029 0.000024 ) 0.087381 -0.167068 0.063350 ( 0.000011 0.000021 0.000018 ) 0.055898 -0.024379 0.122349 ( 0.000014 0.000026 0.000022 ) M - matrix: 0.021540 -0.014369 0.007177 ( 0.000004 0.000004 0.000004 ) -0.014369 0.028741 -0.014334 ( 0.000004 0.000007 0.000005 ) 0.007177 -0.014334 0.021489 ( 0.000004 0.000005 0.000006 ) UB fit with 437 obs out of 437 (total:437,skipped:0) (100.00%) unit cell: 5.9198(10) 5.9142(10) 5.9232(12) 60.058(19) 90.041(16) 59.996(18) V = 146.70(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 98.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 723 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103827 -0.015335 0.050064 ( 0.000015 0.000029 0.000024 ) 0.087381 -0.167068 0.063350 ( 0.000011 0.000021 0.000018 ) 0.055898 -0.024379 0.122349 ( 0.000014 0.000026 0.000022 ) M - matrix: 0.021540 -0.014369 0.007177 ( 0.000004 0.000004 0.000004 ) -0.014369 0.028741 -0.014334 ( 0.000004 0.000007 0.000005 ) 0.007177 -0.014334 0.021489 ( 0.000004 0.000005 0.000006 ) UB fit with 437 obs out of 437 (total:437,skipped:0) (100.00%) unit cell: 5.9198(10) 5.9142(10) 5.9232(12) 60.058(19) 90.041(16) 59.996(18) V = 146.70(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 437 (total:437,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb 4 of 436 peaks identified as outliers and rejected 432 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 432 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 432 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 43 | 1.021 ( 0.147) | 1.172 ( 0.541) | 1.357 ( 1.116) | 1.41- 1.17 | 43 | 1.064 ( 0.077) | 1.124 ( 0.335) | 1.182 ( 0.850) | 1.17- 1.02 | 43 | 1.095 ( 0.072) | 1.163 ( 0.367) | 1.176 ( 0.535) | 1.02- 0.92 | 43 | 1.125 ( 0.075) | 1.203 ( 0.428) | 1.052 ( 0.407) | 0.92- 0.82 | 43 | 1.147 ( 0.041) | 1.111 ( 0.100) | 1.104 ( 0.412) | 0.82- 0.76 | 43 | 1.172 ( 0.043) | 1.106 ( 0.108) | 1.272 ( 0.486) | 0.76- 0.71 | 43 | 1.173 ( 0.028) | 1.073 ( 0.130) | 1.247 ( 0.454) | 0.71- 0.67 | 43 | 1.194 ( 0.049) | 1.139 ( 0.147) | 1.200 ( 0.393) | 0.67- 0.63 | 43 | 1.177 ( 0.063) | 1.182 ( 0.153) | 1.235 ( 0.459) | 0.63- 0.59 | 45 | 1.227 ( 0.072) | 1.151 ( 0.177) | 1.275 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 432 | 1.140 ( 0.095) | 1.142 ( 0.291) | 1.210 ( 0.616) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 221 | 1.149 ( 0.124) | 1.270 ( 0.434) | 1.342 ( 0.700) | 13.1-19.0 | 221 | 1.141 ( 0.106) | 1.202 ( 0.315) | 1.311 ( 0.716) | 19.0-23.0 | 221 | 1.148 ( 0.092) | 1.201 ( 0.290) | 1.249 ( 0.677) | 23.0-27.3 | 221 | 1.130 ( 0.095) | 1.172 ( 0.302) | 1.217 ( 0.567) | 27.3-30.4 | 221 | 1.141 ( 0.098) | 1.160 ( 0.208) | 1.217 ( 0.450) | 30.4-33.8 | 221 | 1.151 ( 0.090) | 1.137 ( 0.198) | 1.215 ( 0.443) | 33.8-37.0 | 221 | 1.139 ( 0.098) | 1.121 ( 0.165) | 1.151 ( 0.423) | 37.1-39.7 | 221 | 1.153 ( 0.123) | 1.120 ( 0.280) | 1.230 ( 0.521) | 39.7-42.9 | 221 | 1.170 ( 0.109) | 1.105 ( 0.192) | 1.229 ( 0.561) | 42.9-50.0 | 221 | 1.204 ( 0.159) | 1.128 ( 0.277) | 1.177 ( 0.475) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 2210 | 1.153 ( 0.113) | 1.162 ( 0.281) | 1.234 ( 0.566) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0023 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 462718 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 23405112 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 14:07:08 2018 PROFFITMAIN - Started at Wed Mar 28 14:07:08 2018 OTKP changes: 2210 2 4 5 OTKP changes: 2210 2 4 5 UB - matrix: -0.104103 -0.015132 0.049654 ( 0.000012 0.000014 0.000013 ) 0.087424 -0.167256 0.063708 ( 0.000008 0.000010 0.000009 ) 0.055612 -0.024437 0.122939 ( 0.000012 0.000014 0.000013 ) M - matrix: 0.021573 -0.014406 0.007237 ( 0.000003 0.000002 0.000002 ) -0.014406 0.028801 -0.014411 ( 0.000002 0.000003 0.000003 ) 0.007237 -0.014411 0.021638 ( 0.000002 0.000003 0.000004 ) UB fit with 2210 obs out of 2210 (total:2210,skipped:0) (100.00%) unit cell: 5.9175(7) 5.9098(5) 5.9053(7) 60.067(11) 90.116(9) 60.011(10) V = 146.05(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.104104 -0.015266 0.049896 ( 0.000026 0.000033 0.000029 ) 0.087350 -0.167019 0.063606 ( 0.000017 0.000021 0.000019 ) 0.055461 -0.024073 0.122552 ( 0.000021 0.000026 0.000023 ) M - matrix: 0.021544 -0.014335 0.007159 ( 0.000007 0.000005 0.000005 ) -0.014335 0.028708 -0.014335 ( 0.000005 0.000007 0.000005 ) 0.007159 -0.014335 0.021554 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9138(14) 5.9126(10) 5.9117(13) 60.05(2) 90.001(19) 60.04(2) V = 146.35(5) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 UB - matrix: -0.104045 -0.015235 0.049841 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167162 0.063721 ( 0.000017 0.000021 0.000019 ) 0.055462 -0.024184 0.122563 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021540 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028760 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9137(10) 5.9147(13) 60.01(2) 90.002(18) 60.01(2) V = 146.41(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.945) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104045 -0.015235 0.049841 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167162 0.063721 ( 0.000017 0.000021 0.000019 ) 0.055462 -0.024184 0.122563 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021540 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028760 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9137(10) 5.9147(13) 60.01(2) 90.002(18) 60.01(2) V = 146.41(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104045 -0.015235 0.049841 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167162 0.063721 ( 0.000017 0.000021 0.000019 ) 0.055462 -0.024184 0.122563 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021540 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028760 -0.014375 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014375 0.021566 ( 0.000005 0.000005 0.000006 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 5.9182(13) 5.9137(10) 5.9147(13) 60.01(2) 90.002(18) 60.01(2) V = 146.41(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104513 -0.014299 0.049157 ( 0.000037 0.000046 0.000040 ) 0.087129 -0.167022 0.063774 ( 0.000025 0.000031 0.000027 ) 0.055338 -0.024931 0.122862 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021577 -0.014438 0.007218 ( 0.000009 0.000007 0.000006 ) -0.014438 0.028723 -0.014418 ( 0.000007 0.000010 0.000007 ) 0.007218 -0.014418 0.021579 ( 0.000006 0.000007 0.000008 ) unit cell: 5.927(2) 5.9388(14) 5.9229(16) 59.89(3) 89.88(2) 59.82(3) V = 146.93(7) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104439 -0.014620 0.048934 ( 0.000028 0.000035 0.000031 ) 0.087202 -0.167136 0.063644 ( 0.000023 0.000028 0.000025 ) 0.055344 -0.024823 0.123248 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021575 -0.014421 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014421 0.028764 -0.014412 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014412 0.021635 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9223(15) 5.9184(13) 5.9079(16) 60.07(2) 90.14(2) 59.97(2) V = 146.33(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.945) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104439 -0.014620 0.048934 ( 0.000028 0.000035 0.000031 ) 0.087202 -0.167136 0.063644 ( 0.000023 0.000028 0.000025 ) 0.055344 -0.024823 0.123248 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021575 -0.014421 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014421 0.028764 -0.014412 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014412 0.021635 ( 0.000006 0.000006 0.000008 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9223(15) 5.9184(13) 5.9079(16) 60.07(2) 90.14(2) 59.97(2) V = 146.33(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146803 -0.097939 0.049183 ( 0.000021 0.000027 0.000023 ) -0.000023 0.138461 -0.069285 ( 0.000023 0.000029 0.000025 ) -0.000026 0.000038 0.119968 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021551 -0.014381 0.007219 ( 0.000006 0.000005 0.000005 ) -0.014381 0.028763 -0.014406 ( 0.000005 0.000010 0.000006 ) 0.007219 -0.014406 0.021612 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9188(11) 5.9156(14) 5.9115(14) 60.01(2) 90.065(17) 60.02(2) V = 146.33(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104320 -0.014872 0.049207 ( 0.000025 0.000020 0.000018 ) 0.087175 -0.167213 0.063660 ( 0.000027 0.000022 0.000020 ) 0.055391 -0.024579 0.123034 ( 0.000023 0.000019 0.000017 ) M - matrix: 0.021550 -0.014387 0.007231 ( 0.000007 0.000006 0.000004 ) -0.014387 0.028786 -0.014401 ( 0.000006 0.000008 0.000004 ) 0.007231 -0.014401 0.021611 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9191(12) 5.9100(10) 5.9094(10) 60.063(18) 90.135(15) 60.04(2) V = 146.23(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104248 -0.015182 0.049360 ( 0.000024 0.000019 0.000017 ) 0.087194 -0.167222 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055268 -0.024228 0.122760 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021525 -0.014337 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014337 0.028781 -0.014378 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014378 0.021566 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9035(9) 5.9143(9) 60.042(17) 90.128(14) 60.136(18) V = 146.25(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.945) HKL list info: 732 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104248 -0.015182 0.049360 ( 0.000024 0.000019 0.000017 ) 0.087194 -0.167222 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055268 -0.024228 0.122760 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021525 -0.014337 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014337 0.028781 -0.014378 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014378 0.021566 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9035(9) 5.9143(9) 60.042(17) 90.128(14) 60.136(18) V = 146.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104248 -0.015182 0.049360 ( 0.000024 0.000019 0.000017 ) 0.087194 -0.167222 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055268 -0.024228 0.122760 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021525 -0.014337 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014337 0.028781 -0.014378 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014378 0.021566 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9143(11) 5.9035(9) 5.9143(9) 60.042(17) 90.128(14) 60.136(18) V = 146.25(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) UB - matrix: -0.103958 -0.015317 0.050192 ( 0.000016 0.000030 0.000026 ) 0.087340 -0.167055 0.063381 ( 0.000013 0.000024 0.000020 ) 0.056112 -0.024509 0.122497 ( 0.000016 0.000029 0.000024 ) M - matrix: 0.021584 -0.014374 0.007191 ( 0.000004 0.000005 0.000004 ) -0.014374 0.028743 -0.014359 ( 0.000005 0.000008 0.000005 ) 0.007191 -0.014359 0.021542 ( 0.000004 0.000005 0.000007 ) unit cell: 5.9116(11) 5.9135(11) 5.9173(13) 60.03(2) 90.043(17) 60.030(19) V = 146.35(5) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 UB - matrix: -0.103880 -0.015307 0.050159 ( 0.000016 0.000029 0.000024 ) 0.087521 -0.167205 0.063421 ( 0.000013 0.000024 0.000020 ) 0.055918 -0.024336 0.122390 ( 0.000014 0.000027 0.000023 ) M - matrix: 0.021578 -0.014405 0.007184 ( 0.000004 0.000004 0.000004 ) -0.014405 0.028784 -0.014351 ( 0.000004 0.000008 0.000005 ) 0.007184 -0.014351 0.021518 ( 0.000004 0.000005 0.000007 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9171(10) 5.9119(10) 5.9185(12) 60.06(2) 90.010(16) 59.947(18) V = 146.41(5) Run 5 Omega scan: (-2.000 - 98.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.945) HKL list info: 717 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103880 -0.015307 0.050159 ( 0.000016 0.000029 0.000024 ) 0.087521 -0.167205 0.063421 ( 0.000013 0.000024 0.000020 ) 0.055918 -0.024336 0.122390 ( 0.000014 0.000027 0.000023 ) M - matrix: 0.021578 -0.014405 0.007184 ( 0.000004 0.000004 0.000004 ) -0.014405 0.028784 -0.014351 ( 0.000004 0.000008 0.000005 ) 0.007184 -0.014351 0.021518 ( 0.000004 0.000005 0.000007 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9171(10) 5.9119(10) 5.9185(12) 60.06(2) 90.010(16) 59.947(18) V = 146.41(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.103880 -0.015307 0.050159 ( 0.000016 0.000029 0.000024 ) 0.087521 -0.167205 0.063421 ( 0.000013 0.000024 0.000020 ) 0.055918 -0.024336 0.122390 ( 0.000014 0.000027 0.000023 ) M - matrix: 0.021578 -0.014405 0.007184 ( 0.000004 0.000004 0.000004 ) -0.014405 0.028784 -0.014351 ( 0.000004 0.000008 0.000005 ) 0.007184 -0.014351 0.021518 ( 0.000004 0.000005 0.000007 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9171(10) 5.9119(10) 5.9185(12) 60.06(2) 90.010(16) 59.947(18) V = 146.41(5) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104030 -0.015137 0.049584 ( 0.000012 0.000014 0.000013 ) 0.087364 -0.167138 0.063680 ( 0.000008 0.000010 0.000009 ) 0.055512 -0.024389 0.122804 ( 0.000012 0.000014 0.000013 ) M - matrix: 0.021536 -0.014381 0.007222 ( 0.000003 0.000002 0.000002 ) -0.014381 0.028759 -0.014389 ( 0.000002 0.000003 0.000002 ) 0.007222 -0.014389 0.021595 ( 0.000002 0.000002 0.000004 ) UB fit with 2210 obs out of 2210 (total:2210,skipped:0) (100.00%) unit cell: 5.9221(7) 5.9143(5) 5.9118(7) 60.055(11) 90.108(9) 60.015(10) V = 146.43(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 46 reflections under beam stop or inside a detector rejection region 22 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof 2952 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:07:15 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.945) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.945) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.945) Run 5 Omega scan: (-2.000 - 98.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.945) PROFFIT INFO: signal sum: min=162.0000 max=22415308.0000 PROFFIT INFO: signal sum lp corr: min=241.8188 max=3285678.8173 PROFFIT INFO: background sum: min=775.0000 max=16011.0000 PROFFIT INFO: background sum sig2: min=592.0000 max=11643.0000 PROFFIT INFO: num of signal pixels: min=59 max=1007 PROFFIT INFO: Inet: min=527.6048 max=7168754.0000 PROFFIT INFO: sig(Inet): min=191.1298 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=397.73 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 61 221 380 612 673 1191 1957 2672 2951 Percent 0.0 0.1 2.1 7.5 12.9 20.7 22.8 40.4 66.3 90.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2952 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 2952 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7168754- 1601112 295 2411182.07 133.97 100.00 1587549- 1038383 295 1290350.36 111.57 100.00 1037859- 315197 295 603551.25 94.49 100.00 315062- 219034 295 255006.23 69.03 100.00 218239- 164524 295 188367.90 48.90 100.00 164485- 130646 295 147036.68 37.25 100.00 130576- 101216 295 115480.65 30.38 100.00 101206- 6044 295 55891.35 20.54 100.00 6043- 3574 295 4574.18 4.94 83.73 3566- 528 296 2662.45 3.21 41.55 ------------------------------------------------------------------------------------ 7168754- 528 2951 507239.27 55.41 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 295 793063.69 83.62 99.66 1.41- 1.05 295 744715.40 66.94 97.97 1.05- 0.92 295 610549.89 67.18 96.95 0.92- 0.82 295 477011.05 53.78 91.86 0.82- 0.74 295 499244.84 61.28 94.58 0.74- 0.67 295 514000.48 56.93 92.20 0.67- 0.61 295 314053.34 41.21 91.53 0.61- 0.56 295 450271.41 48.00 90.51 0.56- 0.51 295 341506.57 38.62 83.05 0.51- 0.40 296 328581.66 36.60 86.82 ------------------------------------------------------------------------------------ 5.26- 0.40 2951 507239.27 55.41 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:07:15 2018 Sorting 2951 observations 291 unique observations with > 7.00 F2/sig(F2) 2951 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 99 513 Total number of frames 513 Maximum number of 291 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2951 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 49 259 Total number of frames 259 2373 observations > 7.00 F2/sig(F2) 2373 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 49 259 Total number of frames 259 Removing 'redundancy=1' reflections Average redundancy: 8.2 (Out of 2373 removed 17 = 2356, unique = 289) 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 2356 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 49 259 Total number of frames 259 289 unique data precomputed (should be 289) 289 unique data with 2356 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.2 (Out of 2356 removed 0 = 2356, unique = 289) 289 unique data precomputed (should be 289) 289 unique data with 2356 observations RMS deviation of equivalent data = 0.74185 Rint = 0.68606 14 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66402, wR= 3.60944 Trying model 1 (ne=2, no=0)... Results: Rint= 0.71525, wR= 2.61115, Acormin=-0.262, Acormax=2.296, Acor_av=0.688 F test: Probability=0.000, F= 0.860 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84142, wR= 2.46801, Acormin=-0.504, Acormax=2.282, Acor_av=0.403 F test: Probability=0.000, F= 0.620 Trying model 3 (ne=4, no=0)... Results: Rint= 0.70685, wR= 2.47924, Acormin=-0.104, Acormax=2.497, Acor_av=0.678 F test: Probability=0.000, F= 0.876 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86972, wR= 3.29617, Acormin=-0.474, Acormax=2.308, Acor_av=0.377 F test: Probability=0.000, F= 0.578 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96877, wR= 2.36905, Acormin=-0.451, Acormax=3.925, Acor_av=0.151 F test: Probability=0.000, F= 0.464 Trying model 6 (ne=6, no=0)... Results: Rint= 0.73032, wR= 3.54806, Acormin=-0.439, Acormax=2.587, Acor_av=0.586 F test: Probability=0.000, F= 0.816 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87484, wR= 3.75419, Acormin=-0.506, Acormax=2.217, Acor_av=0.352 F test: Probability=0.000, F= 0.568 Trying model 8 (ne=6, no=3)... Results: Rint= 0.94755, wR= 2.02927, Acormin=-0.825, Acormax=3.975, Acor_av=0.136 F test: Probability=0.000, F= 0.482 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96743, wR= 1.88610, Acormin=-0.669, Acormax=3.872, Acor_av=0.077 F test: Probability=0.000, F= 0.460 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86257, wR= 1.84018, Acormin=-0.895, Acormax=1.744, Acor_av=0.284 F test: Probability=0.000, F= 0.580 Trying model 11 (ne=8, no=1)... Results: Rint= 0.91567, wR= 2.67167, Acormin=-0.629, Acormax=1.404, Acor_av=0.179 F test: Probability=0.000, F= 0.514 Trying model 12 (ne=8, no=3)... Results: Rint= 1.01010, wR= 1.83773, Acormin=-0.051, Acormax=0.058, Acor_av=0.001 F test: Probability=0.000, F= 0.421 Trying model 13 (ne=8, no=5)... Results: Rint= 1.01674, wR= 1.76144, Acormin=-0.049, Acormax=0.053, Acor_av=0.001 F test: Probability=0.000, F= 0.413 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00276, wR= 1.67766, Acormin=-0.103, Acormax=0.067, Acor_av=0.001 F test: Probability=0.000, F= 0.421 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: 0.86794 There are 259 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 263 pars with 34716 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74185 Using Levenberg-Marquardt: 0.00010 New wR= 0.72600 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68606 with corrections 0.67840 Rint for all data: 0.86794 with corrections 0.86798 12 observations identified as outliers and rejected Cycle 2 wR= 0.69859 Using Levenberg-Marquardt: 0.00001 New wR= 0.69902 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66606 with corrections 0.65548 Rint for all data: 0.86794 with corrections 0.86551 Final wR= 0.69902 Final frame scales: Min= 1.0000 Max= 2.6593 Final absorption correction factors: Amin= 0.5690 Amax= 1.4184 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=465.5315 max=8161700.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=185.0840 max=72295.1016 PROFFIT INFO: 7 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2944 reflections read from tmp file 2224 reflections are rejected (2164 as outliers, 60 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 75 52 32 21 15 7 0 2 2 Initial Chi^2= 0.49738 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.00026 Current error model SIG(F2)^2 = 234.61*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 234.67*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 234.67*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8161701- 1543628 294 2402141.29 90.46 100.00 1538346- 988929 294 1236450.79 48.20 100.00 984977- 318495 294 603912.77 42.56 100.00 317137- 211825 294 256965.58 31.42 100.00 211282- 160868 294 184076.40 21.59 100.00 160578- 125813 294 142013.98 16.24 100.00 125628- 99225 294 113438.31 13.40 100.00 99078- 6185 294 56185.96 9.73 96.94 6115- 3402 294 4439.88 3.10 36.39 3397- 466 298 2605.47 2.41 16.11 ------------------------------------------------------------------------------------ 8161701- 466 2944 499546.93 27.88 84.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 294 886981.20 55.72 97.96 1.41- 1.05 294 753431.12 40.44 92.52 1.05- 0.92 294 624441.57 33.07 90.14 0.92- 0.82 294 476683.33 25.99 83.67 0.82- 0.74 294 459213.13 26.94 86.05 0.74- 0.67 294 502079.72 24.72 83.67 0.67- 0.61 294 294152.54 18.12 80.27 0.61- 0.56 294 420726.04 20.90 80.95 0.56- 0.51 294 308929.99 17.06 75.85 0.51- 0.40 298 271927.55 15.98 77.52 ------------------------------------------------------------------------------------ 5.26- 0.40 2944 499546.93 27.88 84.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 294 886981.20 55.72 97.96 5.26- 1.05 588 820206.16 48.08 95.24 5.26- 0.92 882 754951.30 43.08 93.54 5.26- 0.82 1176 685384.31 38.80 91.07 5.26- 0.74 1470 640150.07 36.43 90.07 5.26- 0.67 1764 617138.35 34.48 89.00 5.26- 0.61 2058 570997.52 32.14 87.76 5.26- 0.56 2352 552213.58 30.74 86.90 5.26- 0.51 2646 525182.07 29.22 85.68 5.26- 0.40 2944 499546.93 27.88 84.85 ------------------------------------------------------------------------------------ 5.26- 0.40 2944 499546.93 27.88 84.85 Scale applied to data: s=0.122523 (maximum obs:8161700.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.863; Rsigma 0.023: data 2944 -> merged 318 With outlier rejection... Rint 0.810; Rsigma 0.023: data 2845 -> merged 318 Rejected total: 99, method kkm 84, method Blessing 15 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404255, 5.270835 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 14.33 100.00 215 1.46 - 1.12 15 15 20.67 100.00 310 1.08 - 0.96 15 15 18.80 100.00 282 0.96 - 0.86 15 15 18.00 100.00 270 0.86 - 0.79 15 15 14.87 100.00 223 0.79 - 0.73 15 15 11.47 100.00 172 0.73 - 0.69 15 15 11.33 100.00 170 0.69 - 0.65 15 15 11.40 100.00 171 0.65 - 0.63 15 15 7.87 100.00 118 0.63 - 0.60 21 21 8.52 100.00 179 --------------------------------------------------------------- 5.92 - 0.60 156 156 13.53 100.00 2110 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:07:16 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.922136 5.914319 5.911787 60.0550 90.1078 60.0152 2845 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1408 1479 1417 1443 2152 1907 1881 2845 N (int>3sigma) = 0 1158 1479 1167 1191 1902 1632 1598 2415 Mean intensity = 0.0 53.4 23.7 53.3 58.9 43.2 59.9 58.7 59.6 Mean int/sigma = 0.0 25.9 22.6 26.1 27.2 24.8 27.6 27.5 27.7 Lattice type: P chosen Volume: 146.43 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.912 5.914 90.04 119.94 119.91 Niggli form: a.a = 34.949 b.b = 34.953 c.c = 34.979 b.c = -0.021 a.c = -17.453 a.b = -17.430 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.138 CUBIC F-lattice R(int) = 0.152 [ 2690] Vol = 585.7 Cell: 8.365 8.376 8.360 90.10 89.98 89.98 Volume: 585.73 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.124 RHOMBOHEDRAL R-lattice R(int) = 0.143 [ 2414] Vol = 439.3 Cell: 5.920 5.912 14.501 89.98 90.09 120.05 Volume: 439.30 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.124 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 770] Vol = 439.3 Trigonal Cell: 5.920 5.912 14.501 89.98 90.09 120.05 Volume: 439.30 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.046 TETRAGONAL I-lattice R(int) = 0.142 [ 2448] Vol = 292.9 Cell: 5.918 5.920 8.360 89.94 89.91 89.93 Volume: 292.87 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.132 TETRAGONAL I-lattice R(int) = 0.142 [ 2448] Vol = 292.9 Cell: 5.920 5.918 8.360 90.09 90.06 89.93 Volume: 292.87 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 2395] Vol = 292.9 Cell: 5.920 5.918 8.360 89.91 89.94 89.93 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.131 [ 2393] Vol = 292.9 Cell: 5.912 8.365 5.922 90.00 89.89 90.03 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.125 [ 2060] Vol = 292.9 Cell: 5.918 5.920 8.360 90.06 90.09 89.93 Volume: 292.87 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.088 MONOCLINIC I-lattice R(int) = 0.122 [ 2063] Vol = 292.9 Cell: 5.912 5.922 8.365 90.00 90.03 90.11 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.031 MONOCLINIC I-lattice R(int) = 0.126 [ 2084] Vol = 292.9 Cell: 5.912 8.365 5.922 90.00 90.11 89.97 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.049 MONOCLINIC I-lattice R(int) = 0.120 [ 2055] Vol = 292.9 Cell: 5.922 5.912 8.365 89.97 90.00 89.89 Volume: 292.87 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.098 MONOCLINIC C-lattice R(int) = 0.128 [ 2062] Vol = 292.9 Cell: 10.248 5.912 5.914 90.04 125.19 89.91 Volume: 292.87 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 1468] Vol = 146.4 Cell: 5.912 5.912 5.914 90.04 119.94 119.91 Volume: 146.43 Matrix: 0.0000 0.0000 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 1479 0 1907 1907 2845 N (int>3sigma) = 0 0 0 0 1479 0 1624 1632 2415 Mean intensity = 0.0 0.0 0.0 0.0 23.7 0.0 59.7 59.9 59.6 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 27.8 27.6 27.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.163 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 24 24 220 650 N I>3s 15 15 102 650 0.6 0.6 0.5 27.9 6.2 6.2 3.5 27.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.152 2490 Fd-3m 1 1 227 C N N N N 37 2284 0.153 2528 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365115 8.375719 8.359975 90.1002 89.9786 89.9843 ZERR 1.00 0.002702 0.001640 0.000279 0.0003 0.0105 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3288600- 914467 337 314 31 10.1 1414019.57 60.97 0.601 0.515 897673- 683603 367 363 31 11.7 781795.96 36.10 0.939 0.813 672461- 529136 373 369 31 11.9 584624.85 32.46 0.950 0.935 527444- 447575 360 356 31 11.5 464134.34 28.92 0.987 1.122 443003- 343944 297 285 31 9.2 374561.90 25.78 0.975 1.114 340997- 242292 352 328 31 10.6 246741.21 20.64 0.804 0.974 241439- 131938 298 284 31 9.2 142963.40 15.45 0.644 0.653 131911- 104495 186 181 31 5.8 115501.00 14.14 0.368 0.225 103164- 73905 221 215 31 6.9 89064.20 10.76 0.612 0.501 73500- 1248 153 150 39 3.8 49772.50 6.95 0.736 0.745 ------------------------------------------------------------------------------------------- 3288600- 1248 2944 2845 318 8.9 486662.81 27.75 0.810 0.774 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 578 557 31 18.0 803660.48 48.56 0.788 0.832 0.014 1.05-0.83 569 560 32 17.5 559296.35 30.06 0.930 1.037 0.021 0.82-0.72 413 402 32 12.6 443623.28 25.30 0.770 0.817 0.026 0.72-0.65 353 346 32 10.8 378485.12 21.57 0.879 0.917 0.028 0.64-0.60 274 265 31 8.5 410195.60 21.17 0.827 0.864 0.030 0.59-0.56 234 226 33 6.8 280394.99 16.54 0.746 0.732 0.037 0.56-0.52 190 183 32 5.7 364279.65 18.99 0.766 0.748 0.033 0.51-0.49 139 128 32 4.0 243556.91 14.88 0.581 0.474 0.039 0.49-0.46 118 108 31 3.5 241772.99 14.87 0.468 0.342 0.042 0.45-0.40 76 70 32 2.2 262820.00 15.59 0.278 0.198 0.041 ------------------------------------------------------------------------------------------------------ inf-0.40 2944 2845 318 8.9 486662.81 27.75 0.810 0.774 0.023 inf-0.60 2165 2110 156 13.5 555958.18 31.63 0.837 0.889 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 557 31 31 100.0 18.0 803660.48 232.12 0.788 0.004 1.05-0.83 560 32 32 100.0 17.5 559296.35 156.67 0.930 0.007 0.82-0.72 402 32 32 100.0 12.6 443623.28 107.62 0.770 0.010 0.72-0.65 346 32 32 100.0 10.8 378485.12 91.38 0.879 0.012 0.64-0.60 265 31 31 100.0 8.5 410195.60 80.11 0.827 0.014 0.59-0.56 226 37 33 89.2 6.8 280394.99 54.78 0.746 0.017 0.56-0.52 183 38 32 84.2 5.7 364279.65 55.38 0.766 0.017 0.51-0.49 128 42 32 76.2 4.0 243556.91 35.91 0.581 0.022 0.49-0.46 108 58 31 53.4 3.5 241772.99 32.78 0.468 0.025 0.45-0.40 70 129 32 24.8 2.2 262820.00 26.44 0.278 0.027 -------------------------------------------------------------------------------------------- inf-0.40 2845 464 318 68.5 8.9 486662.81 121.49 0.810 0.012 inf-0.60 2110 156 156 100.0 13.5 555958.18 147.79 0.837 0.008 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 -1.0 0.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.007569 0.076804 -0.034791 ( 0.000007 0.000007 0.000007 ) -0.083567 -0.011841 -0.008047 ( 0.000005 0.000005 0.000005 ) -0.012193 0.033648 0.076963 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007189 -0.000002 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007171 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007569 0.076804 -0.034791 ( 0.000007 0.000007 0.000007 ) -0.083567 -0.011841 -0.008047 ( 0.000005 0.000005 0.000005 ) -0.012193 0.033648 0.076963 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3653(5) 8.3759(7) 8.3601(7) 90.102(6) 89.979(6) 89.983(6) V = 585.76(7) unit cell: 8.36709(18) 8.36709(18) 8.36709(18) 90.0 90.0 90.0 V = 585.76(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.945) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.945) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.945) Run 5 Omega scan: (-2.000 - 98.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.945) PROFFIT INFO: signal sum: min=162.0000 max=22415308.0000 PROFFIT INFO: signal sum lp corr: min=241.8188 max=3285678.8173 PROFFIT INFO: background sum: min=775.0000 max=16011.0000 PROFFIT INFO: background sum sig2: min=592.0000 max=11643.0000 PROFFIT INFO: num of signal pixels: min=59 max=1007 PROFFIT INFO: Inet: min=527.6048 max=7168754.0000 PROFFIT INFO: sig(Inet): min=191.1298 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=397.73 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 122 442 760 1224 1346 2382 3914 5344 5902 Percent 0.0 0.1 2.1 7.5 12.9 20.7 22.8 40.4 66.3 90.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2952 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 2952 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7168754- 1601112 295 2411182.07 133.97 100.00 1587549- 1038383 295 1290350.36 111.57 100.00 1037859- 315197 295 603551.25 94.49 100.00 315062- 219034 295 255006.23 69.03 100.00 218239- 164524 295 188367.90 48.90 100.00 164485- 130646 295 147036.68 37.25 100.00 130576- 101216 295 115480.65 30.38 100.00 101206- 6044 295 55891.35 20.54 100.00 6043- 3574 295 4574.18 4.94 83.73 3566- 528 296 2662.45 3.21 41.55 ------------------------------------------------------------------------------------ 7168754- 528 2951 507239.27 55.41 92.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 295 843663.37 88.31 100.00 1.41- 1.12 295 796853.90 71.47 98.31 1.12- 0.96 295 650789.07 73.86 98.98 0.96- 0.88 295 491560.49 60.72 94.92 0.88- 0.81 295 646175.67 69.79 97.63 0.81- 0.73 295 366020.76 42.72 92.88 0.73- 0.71 295 257680.27 35.56 91.19 0.71- 0.65 295 515289.77 51.71 95.59 0.65- 0.62 295 258744.50 30.00 75.25 0.62- 0.58 296 246498.77 30.05 80.41 ------------------------------------------------------------------------------------ 4.82- 0.58 2951 507239.27 55.41 92.51 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:07:16 2018 Sorting 2951 observations 85 unique observations with > 7.00 F2/sig(F2) 2951 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 99 513 Total number of frames 513 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 2951 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 14 77 Total number of frames 77 2373 observations > 7.00 F2/sig(F2) 2373 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 14 77 Total number of frames 77 Removing 'redundancy=1' reflections Average redundancy: 26.6 (Out of 2373 removed 6 = 2367, unique = 89) 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 2367 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 14 77 Total number of frames 77 89 unique data precomputed (should be 89) 89 unique data with 2367 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.6 (Out of 2367 removed 0 = 2367, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 2367 observations RMS deviation of equivalent data = 0.21672 Rint = 0.17354 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17191, wR= 0.22322 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08201, wR= 0.10737, Acormin=0.654, Acormax=1.420, Acor_av=0.956 F test: Probability=1.000, F= 4.384 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08274, wR= 0.10203, Acormin=0.610, Acormax=1.390, Acor_av=0.903 F test: Probability=0.000, F= 0.981 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06875, wR= 0.09492, Acormin=0.674, Acormax=1.470, Acor_av=0.961 F test: Probability=1.000, F= 1.417 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06518, wR= 0.08585, Acormin=0.598, Acormax=1.478, Acor_av=0.905 F test: Probability=0.994, F= 1.111 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06187, wR= 0.08269, Acormin=0.507, Acormax=1.291, Acor_av=0.810 F test: Probability=0.992, F= 1.107 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06453, wR= 0.08735, Acormin=0.662, Acormax=1.544, Acor_av=0.926 F test: Probability=0.000, F= 0.918 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06143, wR= 0.08104, Acormin=0.600, Acormax=1.505, Acor_av=0.886 F test: Probability=0.608, F= 1.012 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05853, wR= 0.07720, Acormin=0.514, Acormax=1.348, Acor_av=0.806 F test: Probability=0.994, F= 1.111 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05158, wR= 0.07270, Acormin=0.417, Acormax=1.229, Acor_av=0.687 F test: Probability=1.000, F= 1.281 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06146, wR= 0.07911, Acormin=0.487, Acormax=1.356, Acor_av=0.799 F test: Probability=0.000, F= 0.706 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05937, wR= 0.07696, Acormin=0.520, Acormax=1.372, Acor_av=0.808 F test: Probability=0.000, F= 0.755 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05364, wR= 0.06951, Acormin=0.261, Acormax=0.688, Acor_av=0.411 F test: Probability=0.000, F= 0.922 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04751, wR= 0.06333, Acormin=0.283, Acormax=0.766, Acor_av=0.453 F test: Probability=1.000, F= 1.170 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04332, wR= 0.05830, Acormin=0.299, Acormax=1.014, Acor_av=0.491 F test: Probability=1.000, F= 1.398 Final absorption model (ne=8, no=7): Rint= 0.04332, Acormin=0.299, Acormax=1.014, Acor_av=0.491 Combined refinement in use Rint: 0.17364 There are 77 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: 8, max odd order: 7 (80 parameters) Refinement control: 156 pars with 12246 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21672 Using Levenberg-Marquardt: 0.00010 New wR= 0.05069 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17354 with corrections 0.03723 Rint for all data: 0.17364 with corrections 0.03744 0 observations identified as outliers and rejected Cycle 2 wR= 0.05069 Using Levenberg-Marquardt: 0.00001 New wR= 0.04690 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17354 with corrections 0.03465 Rint for all data: 0.17364 with corrections 0.03486 4 observations identified as outliers and rejected Cycle 3 wR= 0.04505 Using Levenberg-Marquardt: 0.00000 New wR= 0.04400 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17339 with corrections 0.03281 Rint for all data: 0.17364 with corrections 0.03368 2 observations identified as outliers and rejected Cycle 4 wR= 0.04270 Using Levenberg-Marquardt: 0.00000 New wR= 0.04221 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17330 with corrections 0.03192 Rint for all data: 0.17364 with corrections 0.03322 0 observations identified as outliers and rejected Cycle 5 wR= 0.04221 Using Levenberg-Marquardt: 0.00000 New wR= 0.04216 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17330 with corrections 0.03186 Rint for all data: 0.17364 with corrections 0.03319 0 observations identified as outliers and rejected Final wR= 0.04216 Final frame scales: Min= 0.8402 Max= 1.1103 Final absorption correction factors: Amin= 0.4459 Amax= 1.4092 PROFFIT INFO: Inet (after scale3 abspack): min=524.8054 max=5553506.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=164.4559 max=67470.7344 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2951 reflections read from tmp file 361 reflections are rejected (360 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 2 1 1 4 3 2 6 85 Initial Chi^2= 0.32821 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.31558 Current error model SIG(F2)^2 = 116.15*I_RAW + 0.00*I_BACK+(0.00805*)^2 Cycle 2, Chi^2= 1.05716 Current error model SIG(F2)^2 = 76.95*I_RAW + 0.00*I_BACK+(0.01961*)^2 Cycle 3, Chi^2= 1.00356 Current error model SIG(F2)^2 = 96.08*I_RAW + 0.00*I_BACK+(0.01655*)^2 Cycle 4, Chi^2= 1.00007 Current error model SIG(F2)^2 = 92.73*I_RAW + 0.00*I_BACK+(0.01735*)^2 Cycle 5, Chi^2= 1.00004 Current error model SIG(F2)^2 = 93.63*I_RAW + 0.00*I_BACK+(0.01716*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 93.42*I_RAW + 0.00*I_BACK+(0.01721*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 93.42*I_RAW + 0.00*I_BACK+(0.01721*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5553507- 1572164 295 2340830.31 53.05 100.00 1570136- 1004232 295 1230574.23 45.10 100.00 1002136- 330810 295 603173.99 43.24 100.00 330582- 201655 295 246852.55 35.59 100.00 201406- 169776 295 184770.32 28.63 100.00 169668- 126655 295 141492.48 22.49 100.00 126622- 100969 295 113898.35 19.62 100.00 100967- 5668 295 57296.44 14.38 100.00 5660- 3429 295 4313.75 4.85 100.00 3423- 525 296 2674.37 3.77 78.04 ------------------------------------------------------------------------------------ 5553507- 525 2951 492421.66 27.06 97.80 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 295 877948.43 41.91 100.00 1.41- 1.12 295 814466.18 33.50 100.00 1.12- 0.96 295 608462.25 31.55 100.00 0.96- 0.88 295 476930.85 27.46 98.64 0.88- 0.81 295 612375.53 31.80 99.32 0.81- 0.73 295 341263.50 22.04 98.98 0.73- 0.71 295 245043.62 20.40 97.97 0.71- 0.65 295 478463.10 26.59 98.98 0.65- 0.62 295 241001.42 17.45 90.17 0.62- 0.58 296 229154.19 17.95 93.92 ------------------------------------------------------------------------------------ 4.82- 0.58 2951 492421.66 27.06 97.80 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 295 877948.43 41.91 100.00 4.82- 1.12 590 846207.31 37.71 100.00 4.82- 0.96 885 766958.95 35.65 100.00 4.82- 0.88 1180 694451.93 33.61 99.66 4.82- 0.81 1475 678036.65 33.25 99.59 4.82- 0.73 1770 621907.79 31.38 99.49 4.82- 0.71 2065 568070.05 29.81 99.27 4.82- 0.65 2360 556869.18 29.41 99.24 4.82- 0.62 2655 521772.76 28.08 98.23 4.82- 0.58 2951 492421.66 27.06 97.80 ------------------------------------------------------------------------------------ 4.82- 0.58 2951 492421.66 27.06 97.80 Scale applied to data: s=0.180066 (maximum obs:5553506.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.033; Rsigma 0.024: data 2951 -> merged 109 With outlier rejection... Rint 0.031; Rsigma 0.024: data 2934 -> merged 109 Rejected total: 17, method kkm 15, method Blessing 2 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585813, 4.830740 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 16.90 100.00 169 1.61 - 1.21 10 10 27.20 100.00 272 1.17 - 1.01 10 10 34.90 100.00 349 0.99 - 0.89 10 10 34.70 100.00 347 0.88 - 0.81 10 10 33.10 100.00 331 0.81 - 0.74 10 10 28.90 100.00 289 0.73 - 0.71 10 10 31.60 100.00 316 0.70 - 0.66 10 10 26.20 100.00 262 0.66 - 0.64 10 10 25.00 100.00 250 0.63 - 0.60 10 10 24.80 100.00 248 --------------------------------------------------------------- 5.92 - 0.60 100 100 28.33 100.00 2833 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:07:16 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.922136 5.914319 5.911787 60.0550 90.1078 60.0152 2845 Reflections read from file xs1715a.hkl; mean (I/sigma) = 27.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1408 1479 1417 1443 2152 1907 1881 2845 N (int>3sigma) = 0 1158 1479 1167 1191 1902 1632 1598 2415 Mean intensity = 0.0 53.4 23.7 53.3 58.9 43.2 59.9 58.7 59.6 Mean int/sigma = 0.0 25.9 22.6 26.1 27.2 24.8 27.6 27.5 27.7 Lattice type: P chosen Volume: 146.43 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.912 5.912 5.914 90.04 119.94 119.91 Niggli form: a.a = 34.949 b.b = 34.953 c.c = 34.979 b.c = -0.021 a.c = -17.453 a.b = -17.430 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.138 CUBIC F-lattice R(int) = 0.152 [ 2690] Vol = 585.7 Cell: 8.365 8.376 8.360 90.10 89.98 89.98 Volume: 585.73 Matrix:-1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.124 RHOMBOHEDRAL R-lattice R(int) = 0.143 [ 2414] Vol = 439.3 Cell: 5.920 5.912 14.501 89.98 90.09 120.05 Volume: 439.30 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.124 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 770] Vol = 439.3 Trigonal Cell: 5.920 5.912 14.501 89.98 90.09 120.05 Volume: 439.30 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.046 TETRAGONAL I-lattice R(int) = 0.142 [ 2448] Vol = 292.9 Cell: 5.918 5.920 8.360 89.94 89.91 89.93 Volume: 292.87 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.132 TETRAGONAL I-lattice R(int) = 0.142 [ 2448] Vol = 292.9 Cell: 5.920 5.918 8.360 90.09 90.06 89.93 Volume: 292.87 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.142 [ 2395] Vol = 292.9 Cell: 5.920 5.918 8.360 89.91 89.94 89.93 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.131 [ 2393] Vol = 292.9 Cell: 5.912 8.365 5.922 90.00 89.89 90.03 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.125 [ 2060] Vol = 292.9 Cell: 5.918 5.920 8.360 90.06 90.09 89.93 Volume: 292.87 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.088 MONOCLINIC I-lattice R(int) = 0.122 [ 2063] Vol = 292.9 Cell: 5.912 5.922 8.365 90.00 90.03 90.11 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.031 MONOCLINIC I-lattice R(int) = 0.126 [ 2084] Vol = 292.9 Cell: 5.912 8.365 5.922 90.00 90.11 89.97 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.049 MONOCLINIC I-lattice R(int) = 0.120 [ 2055] Vol = 292.9 Cell: 5.922 5.912 8.365 89.97 90.00 89.89 Volume: 292.87 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.098 MONOCLINIC C-lattice R(int) = 0.128 [ 2062] Vol = 292.9 Cell: 10.248 5.912 5.914 90.04 125.19 89.91 Volume: 292.87 Matrix:-1.0000 1.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 1468] Vol = 146.4 Cell: 5.912 5.912 5.914 90.04 119.94 119.91 Volume: 146.43 Matrix: 0.0000 0.0000 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 1479 0 1907 1907 2845 N (int>3sigma) = 0 0 0 0 1479 0 1624 1632 2415 Mean intensity = 0.0 0.0 0.0 0.0 23.7 0.0 59.7 59.9 59.6 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 27.8 27.6 27.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.163 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 24 24 220 650 N I>3s 15 15 102 650 0.6 0.6 0.5 27.9 6.2 6.2 3.5 27.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.152 2490 Fd-3m 1 1 227 C N N N N 37 2284 0.153 2528 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365115 8.375719 8.359975 90.1002 89.9786 89.9843 ZERR 1.00 0.002702 0.001640 0.000279 0.0003 0.0105 0.0003 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5279237- 911495 657 649 27 24.0 1683520.19 48.02 0.028 0.035 896510- 158388 874 869 27 32.2 285735.06 34.82 0.034 0.043 144774- 53571 725 724 27 26.8 113156.91 19.67 0.048 0.063 22083- 1875 695 692 28 24.7 4657.62 4.91 0.149 0.181 ------------------------------------------------------------------------------------------- 5279237- 1875 2951 2934 109 26.9 486045.35 26.95 0.031 0.038 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 737 726 27 26.9 775730.44 37.25 0.030 0.036 0.020 1.01-0.78 897 895 27 33.1 479500.06 26.64 0.025 0.033 0.024 0.78-0.65 793 791 28 28.3 376814.07 22.93 0.034 0.043 0.027 0.65-0.59 524 522 27 19.3 259893.23 19.22 0.043 0.049 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 2951 2934 109 26.9 486045.35 26.95 0.031 0.038 0.024 inf-0.60 2846 2831 99 28.6 496946.41 27.31 0.031 0.038 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 726 27 27 100.0 26.9 775730.44 218.00 0.030 0.006 1.01-0.78 895 27 27 100.0 33.1 479500.06 163.35 0.025 0.004 0.78-0.65 791 28 28 100.0 28.3 376814.07 130.46 0.034 0.006 0.65-0.59 522 28 27 96.4 19.3 259893.23 97.64 0.043 0.009 -------------------------------------------------------------------------------------------- inf-0.59 2934 110 109 99.1 26.9 486045.35 156.32 0.031 0.006 inf-0.60 2831 99 99 100.0 28.6 496946.41 159.58 0.031 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:09:09 2018) ID: 2932; threads 38; handles 878; mem 520152.00 (1230560.00)kB; time: 1w 5d 23h 14m 39s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:508.0,peak PF: 708.5, WS: 271.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:509.7,peak PF: 708.5, WS: 273.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:09:09 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000012 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000008 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000014 0.000013 ) 5.91535 ( 0.00066 ) 5.92288 ( 0.00051 ) 5.91286 ( 0.00070 ) 59.95509 ( 0.01064 ) 89.89521 ( 0.00933 ) 59.99590 ( 0.01036 ) V = 146.51 Selected cell (from UM rr/UM ttt/UM f): 6 5.9154 5.9229 5.9129 59.9551 89.8952 59.9959 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.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 Mar 28 14:09:09 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.104160 -0.015332 0.049802 ( 0.000012 0.000014 0.000013 ) 0.087412 -0.166882 0.063604 ( 0.000008 0.000010 0.000009 ) 0.055227 -0.024260 0.122680 ( 0.000012 0.000014 0.000013 ) M - matrix: 0.021536 -0.014381 0.007222 ( 0.000003 0.000002 0.000002 ) -0.014381 0.028759 -0.014389 ( 0.000002 0.000003 0.000002 ) 0.007222 -0.014389 0.021595 ( 0.000002 0.000002 0.000004 ) unit cell: 5.9154(7) 5.9229(5) 5.9129(7) 59.955(11) 89.895(9) 59.996(10) V = 146.51(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.38 | 45 | 1.018 ( 0.208) | 1.280 ( 0.697) | 1.454 ( 1.104) | 1.32- 1.09 | 45 | 1.086 ( 0.069) | 1.165 ( 0.180) | 1.275 ( 0.647) | 1.09- 0.96 | 45 | 1.116 ( 0.079) | 1.179 ( 0.239) | 1.223 ( 0.536) | 0.96- 0.88 | 45 | 1.138 ( 0.052) | 1.142 ( 0.121) | 1.252 ( 0.490) | 0.85- 0.81 | 45 | 1.165 ( 0.059) | 1.192 ( 0.129) | 1.168 ( 0.408) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.154 ( 0.151) | 1.270 ( 0.437) | 0.74- 0.71 | 45 | 1.184 ( 0.045) | 1.191 ( 0.141) | 1.249 ( 0.451) | 0.71- 0.67 | 45 | 1.191 ( 0.057) | 1.201 ( 0.168) | 1.210 ( 0.378) | 0.67- 0.62 | 45 | 1.202 ( 0.082) | 1.216 ( 0.170) | 1.215 ( 0.496) | 0.62- 0.59 | 44 | 1.198 ( 0.065) | 1.208 ( 0.197) | 1.344 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 449 | 1.146 ( 0.105) | 1.193 ( 0.276) | 1.266 ( 0.585) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) UB - matrix: -0.104041 -0.015307 0.050077 ( 0.000057 0.000068 0.000061 ) 0.087217 -0.166672 0.063499 ( 0.000056 0.000067 0.000060 ) 0.055405 -0.023866 0.122328 ( 0.000056 0.000068 0.000061 ) M - matrix: 0.021501 -0.014266 0.007106 ( 0.000017 0.000014 0.000012 ) -0.014266 0.028584 -0.014270 ( 0.000014 0.000023 0.000014 ) 0.007106 -0.014270 0.021504 ( 0.000012 0.000014 0.000018 ) unit cell: 5.915(3) 5.921(3) 5.915(3) 60.05(6) 89.93(4) 60.05(5) V = 146.78(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) UB - matrix: -0.103878 -0.015264 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087220 -0.166770 0.063554 ( 0.000056 0.000067 0.000060 ) 0.055296 -0.024012 0.122169 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007111 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028622 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007111 -0.014295 0.021458 ( 0.000012 0.000014 0.000018 ) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) OTKP changes: 109 1 1 1 UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.30(13) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103873 -0.015266 0.049937 ( 0.000056 0.000068 0.000061 ) 0.087224 -0.166768 0.063556 ( 0.000056 0.000067 0.000060 ) 0.055299 -0.024016 0.122170 ( 0.000057 0.000069 0.000062 ) M - matrix: 0.021456 -0.014288 0.007112 ( 0.000016 0.000014 0.000012 ) -0.014288 0.028621 -0.014295 ( 0.000014 0.000023 0.000014 ) 0.007112 -0.014295 0.021459 ( 0.000012 0.000014 0.000018 ) UB fit with 572 obs out of 605 (total:605,skipped:0) (94.55%) unit cell: 5.927(3) 5.927(3) 5.928(3) 59.98(6) 89.90(4) 60.00(5) V = 147.29(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 569 obs out of 605 (total:605,skipped:0) (94.05%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.36 | 45 | 0.979 ( 0.150) | 1.234 ( 0.702) | 1.242 ( 0.768) | 1.36- 1.12 | 45 | 1.091 ( 0.084) | 1.216 ( 0.402) | 1.098 ( 0.495) | 1.12- 0.97 | 45 | 1.115 ( 0.084) | 1.145 ( 0.104) | 1.299 ( 0.508) | 0.97- 0.88 | 45 | 1.156 ( 0.073) | 1.181 ( 0.109) | 1.167 ( 0.446) | 0.88- 0.81 | 45 | 1.166 ( 0.079) | 1.145 ( 0.132) | 1.249 ( 0.414) | 0.81- 0.74 | 45 | 1.181 ( 0.066) | 1.154 ( 0.124) | 1.123 ( 0.374) | 0.73- 0.71 | 45 | 1.197 ( 0.066) | 1.211 ( 0.151) | 1.188 ( 0.381) | 0.70- 0.66 | 45 | 1.204 ( 0.061) | 1.196 ( 0.171) | 1.212 ( 0.428) | 0.66- 0.63 | 45 | 1.234 ( 0.080) | 1.193 ( 0.160) | 1.204 ( 0.453) | 0.62- 0.59 | 46 | 1.215 ( 0.092) | 1.213 ( 0.226) | 1.252 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.154 ( 0.113) | 1.189 ( 0.291) | 1.204 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.103881 -0.015136 0.049549 ( 0.000024 0.000030 0.000027 ) 0.087377 -0.167144 0.063771 ( 0.000019 0.000024 0.000021 ) 0.055236 -0.024245 0.122372 ( 0.000023 0.000028 0.000025 ) M - matrix: 0.021477 -0.014371 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014371 0.028754 -0.014376 ( 0.000005 0.000008 0.000005 ) 0.007184 -0.014376 0.021497 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9327(13) 5.9227(11) 5.9295(14) 59.96(2) 89.996(19) 59.96(2) V = 147.15(5) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 816 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103980 -0.015247 0.049772 ( 0.000022 0.000028 0.000025 ) 0.087386 -0.167043 0.063670 ( 0.000018 0.000023 0.000020 ) 0.055391 -0.024146 0.122476 ( 0.000019 0.000025 0.000022 ) M - matrix: 0.021516 -0.014349 0.007173 ( 0.000006 0.000005 0.000004 ) -0.014349 0.028719 -0.014352 ( 0.000005 0.000008 0.000005 ) 0.007173 -0.014352 0.021532 ( 0.000004 0.000005 0.000006 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 5.9218(12) 5.9178(10) 5.9192(12) 60.01(2) 90.007(17) 60.01(2) V = 146.71(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 452 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 45 | 0.991 ( 0.156) | 1.241 ( 0.656) | 1.302 ( 0.782) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.160 ( 0.165) | 1.179 ( 0.526) | 1.12- 0.97 | 45 | 1.121 ( 0.082) | 1.158 ( 0.137) | 1.177 ( 0.454) | 0.97- 0.88 | 45 | 1.140 ( 0.081) | 1.163 ( 0.121) | 1.184 ( 0.474) | 0.88- 0.81 | 45 | 1.156 ( 0.074) | 1.144 ( 0.131) | 1.235 ( 0.454) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.122) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.198 ( 0.068) | 1.202 ( 0.152) | 1.190 ( 0.379) | 0.70- 0.65 | 45 | 1.206 ( 0.061) | 1.212 ( 0.158) | 1.217 ( 0.424) | 0.65- 0.62 | 45 | 1.225 ( 0.082) | 1.202 ( 0.168) | 1.185 ( 0.456) | 0.62- 0.59 | 43 | 1.225 ( 0.088) | 1.201 ( 0.226) | 1.342 ( 0.577) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 448 | 1.154 ( 0.111) | 1.183 ( 0.257) | 1.221 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) UB fit with 515 obs out of 525 (total:525,skipped:0) (98.10%) UB - matrix: -0.104489 -0.014550 0.048996 ( 0.000040 0.000051 0.000045 ) 0.087157 -0.167014 0.063608 ( 0.000058 0.000074 0.000065 ) 0.055493 -0.024918 0.123107 ( 0.000048 0.000061 0.000054 ) M - matrix: 0.021594 -0.014419 0.007256 ( 0.000014 0.000013 0.000011 ) -0.014419 0.028726 -0.014404 ( 0.000013 0.000025 0.000014 ) 0.007256 -0.014404 0.021602 ( 0.000011 0.000014 0.000016 ) unit cell: 5.920(2) 5.925(3) 5.915(3) 60.02(5) 90.10(4) 59.96(5) V = 146.54(12) OTKP changes: 99 1 1 1 UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104367 -0.014334 0.048584 ( 0.000038 0.000048 0.000042 ) 0.086661 -0.166562 0.063495 ( 0.000057 0.000072 0.000063 ) 0.055097 -0.024633 0.122720 ( 0.000048 0.000060 0.000052 ) M - matrix: 0.021438 -0.014296 0.007194 ( 0.000014 0.000013 0.000010 ) -0.014296 0.028555 -0.014295 ( 0.000013 0.000024 0.000014 ) 0.007194 -0.014295 0.021452 ( 0.000010 0.000014 0.000016 ) UB fit with 517 obs out of 525 (total:525,skipped:0) (98.48%) unit cell: 5.935(2) 5.935(3) 5.932(3) 60.06(5) 90.15(3) 60.04(4) V = 147.80(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 525 (total:525,skipped:0) (98.29%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.039 ( 0.253) | 1.194 ( 0.705) | 1.296 ( 1.000) | 1.48- 1.17 | 44 | 1.094 ( 0.156) | 1.065 ( 0.084) | 1.219 ( 0.669) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.081 ( 0.083) | 1.154 ( 0.465) | 0.99- 0.92 | 44 | 1.141 ( 0.067) | 1.098 ( 0.082) | 1.156 ( 0.389) | 0.89- 0.82 | 44 | 1.179 ( 0.069) | 1.107 ( 0.089) | 1.185 ( 0.421) | 0.82- 0.76 | 44 | 1.204 ( 0.058) | 1.102 ( 0.090) | 1.278 ( 0.364) | 0.76- 0.71 | 44 | 1.218 ( 0.055) | 1.089 ( 0.118) | 1.269 ( 0.496) | 0.71- 0.67 | 44 | 1.245 ( 0.050) | 1.128 ( 0.145) | 1.286 ( 0.501) | 0.67- 0.63 | 44 | 1.245 ( 0.071) | 1.122 ( 0.157) | 1.488 ( 0.539) | 0.63- 0.59 | 43 | 1.291 ( 0.070) | 1.111 ( 0.181) | 1.332 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.176 ( 0.134) | 1.110 ( 0.252) | 1.266 ( 0.574) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) UB - matrix: -0.104368 -0.014415 0.048695 ( 0.000026 0.000033 0.000028 ) 0.086838 -0.166902 0.063584 ( 0.000024 0.000030 0.000026 ) 0.054871 -0.024666 0.122924 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021444 -0.014342 0.007184 ( 0.000007 0.000006 0.000005 ) -0.014342 0.028672 -0.014346 ( 0.000006 0.000010 0.000006 ) 0.007184 -0.014346 0.021524 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9377(14) 5.9277(13) 5.9219(15) 60.03(2) 90.03(2) 59.95(2) V = 147.29(6) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.196) HKL list info: 735 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104419 -0.014289 0.048707 ( 0.000026 0.000032 0.000028 ) 0.086789 -0.166730 0.063616 ( 0.000023 0.000029 0.000025 ) 0.055060 -0.024657 0.122750 ( 0.000021 0.000027 0.000023 ) M - matrix: 0.021467 -0.014336 0.007194 ( 0.000007 0.000006 0.000005 ) -0.014336 0.028611 -0.014329 ( 0.000006 0.000010 0.000006 ) 0.007194 -0.014329 0.021487 ( 0.000005 0.000006 0.000007 ) UB fit with 439 obs out of 439 (total:439,skipped:0) (100.00%) unit cell: 5.9347(14) 5.9353(12) 5.9293(13) 60.01(2) 90.056(19) 59.97(2) V = 147.56(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 439 (total:439,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= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 441 peaks identified as outliers and rejected 438 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 438 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 438 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 44 | 1.047 ( 0.255) | 1.228 ( 0.742) | 1.392 ( 1.098) | 1.61- 1.17 | 44 | 1.097 ( 0.151) | 1.150 ( 0.389) | 1.338 ( 0.868) | 1.17- 0.99 | 44 | 1.101 ( 0.078) | 1.080 ( 0.091) | 1.176 ( 0.497) | 0.99- 0.92 | 44 | 1.146 ( 0.064) | 1.107 ( 0.081) | 1.103 ( 0.367) | 0.92- 0.82 | 44 | 1.173 ( 0.072) | 1.113 ( 0.088) | 1.173 ( 0.398) | 0.82- 0.76 | 44 | 1.204 ( 0.051) | 1.094 ( 0.091) | 1.297 ( 0.426) | 0.76- 0.71 | 44 | 1.219 ( 0.055) | 1.100 ( 0.127) | 1.260 ( 0.526) | 0.71- 0.67 | 44 | 1.248 ( 0.054) | 1.133 ( 0.143) | 1.338 ( 0.498) | 0.67- 0.63 | 44 | 1.237 ( 0.064) | 1.118 ( 0.156) | 1.424 ( 0.532) | 0.63- 0.59 | 42 | 1.295 ( 0.076) | 1.117 ( 0.182) | 1.321 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 438 | 1.176 ( 0.133) | 1.124 ( 0.291) | 1.282 ( 0.626) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) UB fit with 544 obs out of 575 (total:575,skipped:0) (94.61%) UB - matrix: -0.104307 -0.014880 0.049105 ( 0.000055 0.000047 0.000037 ) 0.087183 -0.167004 0.063520 ( 0.000069 0.000059 0.000047 ) 0.055441 -0.024448 0.122987 ( 0.000060 0.000051 0.000041 ) M - matrix: 0.021555 -0.014363 0.007234 ( 0.000018 0.000014 0.000011 ) -0.014363 0.028709 -0.014346 ( 0.000014 0.000020 0.000011 ) 0.007234 -0.014346 0.021572 ( 0.000011 0.000011 0.000012 ) unit cell: 5.917(3) 5.911(2) 5.910(3) 60.16(4) 90.23(4) 60.08(5) V = 146.40(11) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) 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 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104346 -0.014833 0.048967 ( 0.000058 0.000049 0.000040 ) 0.087084 -0.166864 0.063517 ( 0.000065 0.000055 0.000045 ) 0.055464 -0.024380 0.122923 ( 0.000062 0.000053 0.000043 ) M - matrix: 0.021548 -0.014336 0.007240 ( 0.000018 0.000013 0.000011 ) -0.014336 0.028658 -0.014322 ( 0.000013 0.000019 0.000011 ) 0.007240 -0.014322 0.021542 ( 0.000011 0.000011 0.000013 ) UB fit with 551 obs out of 575 (total:575,skipped:0) (95.83%) unit cell: 5.916(3) 5.912(2) 5.914(3) 60.18(4) 90.30(4) 60.14(5) V = 146.58(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 552 obs out of 575 (total:575,skipped:0) (96.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 12 of 460 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 45 | 1.052 ( 0.231) | 1.190 ( 0.539) | 1.197 ( 0.748) | 1.41- 1.12 | 45 | 1.071 ( 0.071) | 1.209 ( 0.441) | 1.084 ( 0.522) | 1.11- 0.98 | 45 | 1.088 ( 0.089) | 1.176 ( 0.386) | 1.202 ( 0.570) | 0.98- 0.89 | 45 | 1.110 ( 0.078) | 1.126 ( 0.094) | 1.139 ( 0.413) | 0.89- 0.82 | 45 | 1.143 ( 0.079) | 1.146 ( 0.111) | 1.175 ( 0.398) | 0.81- 0.75 | 45 | 1.172 ( 0.077) | 1.133 ( 0.143) | 1.192 ( 0.469) | 0.75- 0.71 | 45 | 1.175 ( 0.071) | 1.166 ( 0.125) | 1.171 ( 0.403) | 0.71- 0.67 | 45 | 1.184 ( 0.060) | 1.112 ( 0.116) | 1.329 ( 0.476) | 0.67- 0.62 | 45 | 1.219 ( 0.069) | 1.164 ( 0.167) | 1.216 ( 0.421) | 0.62- 0.59 | 43 | 1.244 ( 0.088) | 1.114 ( 0.203) | 1.300 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 448 | 1.145 ( 0.119) | 1.154 ( 0.280) | 1.200 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104280 -0.015064 0.049312 ( 0.000022 0.000018 0.000016 ) 0.087253 -0.167246 0.063738 ( 0.000026 0.000021 0.000019 ) 0.055260 -0.024390 0.122868 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021541 -0.014370 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028793 -0.014399 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014399 0.021591 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9170(11) 5.9085(9) 5.9130(8) 60.020(16) 90.090(13) 60.066(18) V = 146.25(4) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=53.000) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104266 -0.015065 0.049226 ( 0.000022 0.000018 0.000016 ) 0.087137 -0.167090 0.063712 ( 0.000024 0.000019 0.000017 ) 0.055222 -0.024264 0.122740 ( 0.000019 0.000015 0.000014 ) M - matrix: 0.021514 -0.014329 0.007197 ( 0.000007 0.000005 0.000004 ) -0.014329 0.028735 -0.014365 ( 0.000005 0.000007 0.000004 ) 0.007197 -0.014365 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9173(11) 5.9100(8) 5.9179(8) 60.037(15) 90.134(13) 60.125(17) V = 146.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 1.057 ( 0.227) | 1.178 ( 0.496) | 1.196 ( 0.715) | 1.41- 1.15 | 44 | 1.076 ( 0.082) | 1.307 ( 0.548) | 1.016 ( 0.469) | 1.15- 0.99 | 44 | 1.083 ( 0.085) | 1.171 ( 0.390) | 1.171 ( 0.518) | 0.98- 0.89 | 44 | 1.127 ( 0.073) | 1.136 ( 0.092) | 1.137 ( 0.425) | 0.89- 0.82 | 44 | 1.150 ( 0.071) | 1.167 ( 0.098) | 1.184 ( 0.382) | 0.82- 0.75 | 44 | 1.168 ( 0.087) | 1.131 ( 0.145) | 1.151 ( 0.391) | 0.75- 0.71 | 44 | 1.173 ( 0.070) | 1.164 ( 0.122) | 1.207 ( 0.423) | 0.71- 0.67 | 44 | 1.190 ( 0.061) | 1.135 ( 0.158) | 1.357 ( 0.536) | 0.67- 0.63 | 44 | 1.212 ( 0.072) | 1.167 ( 0.150) | 1.260 ( 0.426) | 0.63- 0.59 | 45 | 1.233 ( 0.079) | 1.105 ( 0.195) | 1.257 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 441 | 1.147 ( 0.116) | 1.166 ( 0.294) | 1.194 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb PROFFITPEAK info: 1208 peaks in the peak location table UB fit with 548 obs out of 566 (total:566,skipped:0) (96.82%) UB - matrix: -0.103830 -0.015281 0.050081 ( 0.000034 0.000061 0.000051 ) 0.087246 -0.166952 0.063297 ( 0.000032 0.000057 0.000049 ) 0.055989 -0.024390 0.122422 ( 0.000031 0.000056 0.000048 ) M - matrix: 0.021527 -0.014345 0.007177 ( 0.000010 0.000010 0.000009 ) -0.014345 0.028701 -0.014319 ( 0.000010 0.000019 0.000012 ) 0.007177 -0.014319 0.021502 ( 0.000009 0.000012 0.000014 ) unit cell: 5.920(2) 5.914(2) 5.919(3) 60.09(4) 90.08(3) 60.03(4) V = 146.70(10) UB fit with 548 obs out of 566 (total:566,skipped:0) (96.82%) UB - matrix: -0.103830 -0.015281 0.050081 ( 0.000034 0.000061 0.000051 ) 0.087246 -0.166952 0.063297 ( 0.000032 0.000057 0.000049 ) 0.055989 -0.024390 0.122422 ( 0.000031 0.000056 0.000048 ) M - matrix: 0.021527 -0.014345 0.007177 ( 0.000010 0.000010 0.000009 ) -0.014345 0.028701 -0.014319 ( 0.000010 0.000019 0.000012 ) 0.007177 -0.014319 0.021502 ( 0.000009 0.000012 0.000014 ) unit cell: 5.920(2) 5.914(2) 5.919(3) 60.09(4) 90.08(3) 60.03(4) V = 146.70(10) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.103734 -0.015346 0.050009 ( 0.000034 0.000061 0.000051 ) 0.087382 -0.167064 0.063314 ( 0.000031 0.000056 0.000047 ) 0.055824 -0.024330 0.122309 ( 0.000030 0.000054 0.000046 ) M - matrix: 0.021513 -0.014365 0.007173 ( 0.000010 0.000010 0.000009 ) -0.014365 0.028738 -0.014321 ( 0.000010 0.000019 0.000011 ) 0.007173 -0.014321 0.021469 ( 0.000009 0.000011 0.000014 ) UB fit with 549 obs out of 566 (total:566,skipped:0) (97.00%) unit cell: 5.925(2) 5.914(2) 5.925(3) 60.09(4) 90.06(3) 59.98(4) V = 146.87(10) UB fit with 549 obs out of 566 (total:566,skipped:0) (97.00%) UB - matrix: -0.103734 -0.015346 0.050009 ( 0.000034 0.000061 0.000051 ) 0.087382 -0.167064 0.063314 ( 0.000031 0.000056 0.000047 ) 0.055824 -0.024330 0.122309 ( 0.000030 0.000054 0.000046 ) M - matrix: 0.021513 -0.014365 0.007173 ( 0.000010 0.000010 0.000009 ) -0.014365 0.028738 -0.014321 ( 0.000010 0.000019 0.000011 ) 0.007173 -0.014321 0.021469 ( 0.000009 0.000011 0.000014 ) unit cell: 5.925(2) 5.914(2) 5.925(3) 60.09(4) 90.06(3) 59.98(4) V = 146.87(10) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 566 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 791 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103734 -0.015346 0.050009 ( 0.000034 0.000061 0.000051 ) 0.087382 -0.167064 0.063314 ( 0.000031 0.000056 0.000047 ) 0.055824 -0.024330 0.122309 ( 0.000030 0.000054 0.000046 ) M - matrix: 0.021513 -0.014365 0.007173 ( 0.000010 0.000010 0.000009 ) -0.014365 0.028738 -0.014321 ( 0.000010 0.000019 0.000011 ) 0.007173 -0.014321 0.021469 ( 0.000009 0.000011 0.000014 ) UB fit with 549 obs out of 566 (total:566,skipped:0) (97.00%) unit cell: 5.925(2) 5.914(2) 5.925(3) 60.09(4) 90.06(3) 59.98(4) V = 146.87(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 549 obs out of 566 (total:566,skipped:0) (97.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 479 peaks identified as outliers and rejected 475 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 475 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 475 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 48 | 1.011 ( 0.147) | 1.172 ( 0.550) | 1.381 ( 1.124) | 1.41- 1.17 | 48 | 1.082 ( 0.109) | 1.184 ( 0.454) | 1.031 ( 0.468) | 1.17- 1.00 | 48 | 1.082 ( 0.070) | 1.159 ( 0.383) | 1.196 ( 0.528) | 0.98- 0.92 | 48 | 1.125 ( 0.051) | 1.112 ( 0.111) | 1.097 ( 0.420) | 0.92- 0.82 | 48 | 1.153 ( 0.036) | 1.100 ( 0.104) | 1.169 ( 0.491) | 0.82- 0.75 | 48 | 1.177 ( 0.047) | 1.089 ( 0.117) | 1.319 ( 0.481) | 0.75- 0.71 | 48 | 1.172 ( 0.036) | 1.090 ( 0.116) | 1.216 ( 0.488) | 0.71- 0.67 | 48 | 1.198 ( 0.049) | 1.134 ( 0.142) | 1.186 ( 0.385) | 0.67- 0.62 | 48 | 1.195 ( 0.075) | 1.149 ( 0.168) | 1.215 ( 0.498) | 0.62- 0.59 | 43 | 1.222 ( 0.070) | 1.151 ( 0.178) | 1.270 ( 0.575) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 475 | 1.141 ( 0.099) | 1.134 ( 0.283) | 1.207 ( 0.589) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 475 obs out of 475 (total:475,skipped:0) (100.00%) UB - matrix: -0.103899 -0.015527 0.050206 ( 0.000016 0.000029 0.000024 ) 0.087730 -0.167286 0.063537 ( 0.000014 0.000026 0.000021 ) 0.055921 -0.024540 0.122443 ( 0.000014 0.000026 0.000021 ) M - matrix: 0.021619 -0.014435 0.007205 ( 0.000004 0.000005 0.000004 ) -0.014435 0.028828 -0.014413 ( 0.000005 0.000009 0.000005 ) 0.007205 -0.014413 0.021550 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9128(10) 5.9161(11) 5.9224(12) 59.94(2) 89.951(15) 59.942(19) V = 146.29(4) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 UB - matrix: -0.103836 -0.015331 0.050076 ( 0.000014 0.000026 0.000022 ) 0.087377 -0.167083 0.063376 ( 0.000011 0.000020 0.000016 ) 0.055902 -0.024393 0.122366 ( 0.000014 0.000025 0.000021 ) M - matrix: 0.021542 -0.014371 0.007178 ( 0.000004 0.000004 0.000003 ) -0.014371 0.028747 -0.014342 ( 0.000004 0.000007 0.000005 ) 0.007178 -0.014342 0.021498 ( 0.000003 0.000005 0.000006 ) UB fit with 475 obs out of 475 (total:475,skipped:0) (100.00%) unit cell: 5.9196(9) 5.9143(9) 5.9227(11) 60.046(18) 90.035(14) 59.996(17) V = 146.67(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103836 -0.015331 0.050076 ( 0.000014 0.000026 0.000022 ) 0.087377 -0.167083 0.063376 ( 0.000011 0.000020 0.000016 ) 0.055902 -0.024393 0.122366 ( 0.000014 0.000025 0.000021 ) M - matrix: 0.021542 -0.014371 0.007178 ( 0.000004 0.000004 0.000003 ) -0.014371 0.028747 -0.014342 ( 0.000004 0.000007 0.000005 ) 0.007178 -0.014342 0.021498 ( 0.000003 0.000005 0.000006 ) UB fit with 475 obs out of 475 (total:475,skipped:0) (100.00%) unit cell: 5.9196(9) 5.9143(9) 5.9227(11) 60.046(18) 90.035(14) 59.996(17) V = 146.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 475 (total:475,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 473 peaks identified as outliers and rejected 469 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 469 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 469 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 47 | 1.015 ( 0.148) | 1.157 ( 0.522) | 1.320 ( 1.076) | 1.41- 1.17 | 47 | 1.071 ( 0.073) | 1.118 ( 0.320) | 1.154 ( 0.825) | 1.17- 1.00 | 47 | 1.098 ( 0.092) | 1.239 ( 0.523) | 1.142 ( 0.526) | 0.99- 0.92 | 47 | 1.130 ( 0.048) | 1.117 ( 0.105) | 1.074 ( 0.421) | 0.92- 0.82 | 47 | 1.151 ( 0.047) | 1.100 ( 0.102) | 1.188 ( 0.480) | 0.82- 0.75 | 47 | 1.174 ( 0.041) | 1.103 ( 0.112) | 1.245 ( 0.458) | 0.75- 0.71 | 47 | 1.175 ( 0.036) | 1.084 ( 0.129) | 1.193 ( 0.425) | 0.71- 0.67 | 47 | 1.195 ( 0.051) | 1.137 ( 0.148) | 1.177 ( 0.384) | 0.67- 0.62 | 47 | 1.191 ( 0.071) | 1.160 ( 0.159) | 1.228 ( 0.488) | 0.62- 0.59 | 46 | 1.224 ( 0.071) | 1.157 ( 0.178) | 1.248 ( 0.554) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 469 | 1.142 ( 0.096) | 1.137 ( 0.282) | 1.197 ( 0.604) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 225 | 1.149 ( 0.128) | 1.270 ( 0.445) | 1.349 ( 0.714) | 13.1-19.0 | 225 | 1.141 ( 0.106) | 1.199 ( 0.312) | 1.307 ( 0.713) | 19.0-23.1 | 225 | 1.148 ( 0.093) | 1.199 ( 0.288) | 1.255 ( 0.676) | 23.1-27.3 | 225 | 1.132 ( 0.094) | 1.171 ( 0.299) | 1.215 ( 0.566) | 27.3-30.5 | 225 | 1.141 ( 0.099) | 1.159 ( 0.208) | 1.212 ( 0.449) | 30.5-33.8 | 225 | 1.152 ( 0.090) | 1.138 ( 0.199) | 1.212 ( 0.440) | 33.8-37.1 | 225 | 1.137 ( 0.102) | 1.113 ( 0.167) | 1.151 ( 0.429) | 37.1-39.9 | 225 | 1.159 ( 0.118) | 1.126 ( 0.277) | 1.237 ( 0.523) | 39.9-42.9 | 225 | 1.166 ( 0.116) | 1.097 ( 0.192) | 1.204 ( 0.553) | 43.0-50.0 | 220 | 1.207 ( 0.156) | 1.131 ( 0.276) | 1.170 ( 0.473) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 2245 | 1.153 ( 0.113) | 1.160 ( 0.281) | 1.231 ( 0.567) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0024 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6340 lp-corr: 4527 Maximum peak integral for reflections I/sig<= 100 - raw: 462718 lp-corr: 681855 Maximum peak integral for reflections I/sig<= 10000 - raw: 23405112 lp-corr: 4158161 PROFFITPEAK - Finished at Wed Mar 28 14:09:32 2018 PROFFITMAIN - Started at Wed Mar 28 14:09:32 2018 OTKP changes: 2245 2 4 5 OTKP changes: 2245 2 4 5 UB - matrix: -0.104110 -0.015129 0.049655 ( 0.000012 0.000014 0.000013 ) 0.087422 -0.167246 0.063700 ( 0.000008 0.000010 0.000009 ) 0.055629 -0.024431 0.122921 ( 0.000012 0.000014 0.000013 ) M - matrix: 0.021576 -0.014405 0.007237 ( 0.000003 0.000002 0.000002 ) -0.014405 0.028797 -0.014408 ( 0.000002 0.000003 0.000003 ) 0.007237 -0.014408 0.021633 ( 0.000002 0.000003 0.000004 ) UB fit with 2245 obs out of 2245 (total:2245,skipped:0) (100.00%) unit cell: 5.9170(7) 5.9098(5) 5.9059(7) 60.069(11) 90.119(9) 60.014(10) V = 146.06(3) Run 1 has been already processed *** 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= -30.94 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.104109 -0.015266 0.049900 ( 0.000026 0.000033 0.000029 ) 0.087349 -0.167018 0.063604 ( 0.000017 0.000021 0.000019 ) 0.055463 -0.024069 0.122554 ( 0.000021 0.000026 0.000023 ) M - matrix: 0.021545 -0.014334 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014334 0.028707 -0.014335 ( 0.000005 0.000007 0.000005 ) 0.007158 -0.014335 0.021555 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9135(14) 5.9124(11) 5.9114(13) 60.05(2) 90.001(19) 60.04(2) V = 146.34(5) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.104041 -0.015235 0.049836 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167156 0.063719 ( 0.000017 0.000021 0.000019 ) 0.055458 -0.024183 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021539 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.42(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.947) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104041 -0.015235 0.049836 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167156 0.063719 ( 0.000017 0.000021 0.000019 ) 0.055458 -0.024183 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021539 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.42(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.104041 -0.015235 0.049836 ( 0.000024 0.000031 0.000027 ) 0.087401 -0.167156 0.063719 ( 0.000017 0.000021 0.000019 ) 0.055458 -0.024183 0.122559 ( 0.000020 0.000025 0.000022 ) M - matrix: 0.021539 -0.014366 0.007181 ( 0.000006 0.000005 0.000005 ) -0.014366 0.028758 -0.014374 ( 0.000005 0.000007 0.000005 ) 0.007181 -0.014374 0.021564 ( 0.000005 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9185(13) 5.9140(10) 5.9150(13) 60.01(2) 90.002(18) 60.01(2) V = 146.42(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.94 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) UB - matrix: -0.104511 -0.014296 0.049153 ( 0.000036 0.000045 0.000040 ) 0.087125 -0.167016 0.063773 ( 0.000025 0.000031 0.000027 ) 0.055340 -0.024930 0.122857 ( 0.000025 0.000031 0.000027 ) M - matrix: 0.021576 -0.014437 0.007218 ( 0.000009 0.000007 0.000006 ) -0.014437 0.028720 -0.014417 ( 0.000007 0.000010 0.000007 ) 0.007218 -0.014417 0.021577 ( 0.000006 0.000007 0.000008 ) unit cell: 5.928(2) 5.9389(14) 5.9232(16) 59.89(3) 89.89(2) 59.82(3) V = 146.95(7) OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 UB - matrix: -0.104437 -0.014618 0.048932 ( 0.000028 0.000035 0.000031 ) 0.087198 -0.167131 0.063643 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024822 0.123243 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021573 -0.014420 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014420 0.028763 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014411 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) unit cell: 5.9225(15) 5.9186(13) 5.9082(16) 60.07(2) 90.14(2) 59.97(2) V = 146.34(6) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.947) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104437 -0.014618 0.048932 ( 0.000028 0.000035 0.000031 ) 0.087198 -0.167131 0.063643 ( 0.000023 0.000028 0.000025 ) 0.055341 -0.024822 0.123243 ( 0.000025 0.000032 0.000028 ) M - matrix: 0.021573 -0.014420 0.007260 ( 0.000008 0.000006 0.000006 ) -0.014420 0.028763 -0.014411 ( 0.000006 0.000010 0.000006 ) 0.007260 -0.014411 0.021634 ( 0.000006 0.000006 0.000008 ) UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) unit cell: 5.9225(15) 5.9186(13) 5.9082(16) 60.07(2) 90.14(2) 59.97(2) V = 146.34(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.146799 -0.097934 0.049178 ( 0.000021 0.000027 0.000023 ) -0.000023 0.138459 -0.069283 ( 0.000023 0.000029 0.000025 ) -0.000024 0.000033 0.119965 ( 0.000022 0.000028 0.000024 ) M - matrix: 0.021550 -0.014380 0.007218 ( 0.000006 0.000005 0.000005 ) -0.014380 0.028762 -0.014405 ( 0.000005 0.000010 0.000006 ) 0.007218 -0.014405 0.021610 ( 0.000005 0.000006 0.000007 ) UB fit with 438 obs out of 438 (total:438,skipped:0) (100.00%) unit cell: 5.9189(11) 5.9157(14) 5.9117(14) 60.00(2) 90.064(17) 60.02(2) V = 146.35(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.104320 -0.014869 0.049201 ( 0.000025 0.000020 0.000018 ) 0.087168 -0.167205 0.063657 ( 0.000027 0.000022 0.000020 ) 0.055392 -0.024577 0.123031 ( 0.000023 0.000019 0.000017 ) M - matrix: 0.021549 -0.014385 0.007231 ( 0.000007 0.000006 0.000004 ) -0.014385 0.028783 -0.014399 ( 0.000006 0.000008 0.000004 ) 0.007231 -0.014399 0.021610 ( 0.000004 0.000004 0.000005 ) unit cell: 5.9191(12) 5.9101(10) 5.9096(10) 60.065(18) 90.138(15) 60.04(2) V = 146.24(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.104247 -0.015179 0.049356 ( 0.000024 0.000019 0.000017 ) 0.087191 -0.167217 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055265 -0.024226 0.122756 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021524 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028779 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014377 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9145(11) 5.9037(9) 5.9145(9) 60.042(17) 90.128(14) 60.136(18) V = 146.26(4) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.947) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.104247 -0.015179 0.049356 ( 0.000024 0.000019 0.000017 ) 0.087191 -0.167217 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055265 -0.024226 0.122756 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021524 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028779 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014377 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9145(11) 5.9037(9) 5.9145(9) 60.042(17) 90.128(14) 60.136(18) V = 146.26(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.104247 -0.015179 0.049356 ( 0.000024 0.000019 0.000017 ) 0.087191 -0.167217 0.063713 ( 0.000027 0.000022 0.000019 ) 0.055265 -0.024226 0.122756 ( 0.000020 0.000017 0.000015 ) M - matrix: 0.021524 -0.014336 0.007194 ( 0.000007 0.000005 0.000004 ) -0.014336 0.028779 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007194 -0.014377 0.021564 ( 0.000004 0.000004 0.000005 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9145(11) 5.9037(9) 5.9145(9) 60.042(17) 90.128(14) 60.136(18) V = 146.26(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 469 (total:469,skipped:0) (100.00%) UB - matrix: -0.103957 -0.015306 0.050186 ( 0.000015 0.000028 0.000023 ) 0.087322 -0.167062 0.063406 ( 0.000012 0.000022 0.000018 ) 0.056103 -0.024508 0.122503 ( 0.000015 0.000027 0.000022 ) M - matrix: 0.021580 -0.014372 0.007192 ( 0.000004 0.000004 0.000004 ) -0.014372 0.028745 -0.014363 ( 0.000004 0.000008 0.000005 ) 0.007192 -0.014363 0.021546 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9121(10) 5.9135(10) 5.9172(12) 60.03(2) 90.043(15) 60.033(18) V = 146.36(4) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 UB - matrix: -0.103886 -0.015304 0.050162 ( 0.000014 0.000026 0.000022 ) 0.087514 -0.167207 0.063441 ( 0.000012 0.000022 0.000018 ) 0.055916 -0.024347 0.122406 ( 0.000014 0.000025 0.000021 ) M - matrix: 0.021577 -0.014404 0.007185 ( 0.000004 0.000004 0.000004 ) -0.014404 0.028785 -0.014356 ( 0.000004 0.000008 0.000005 ) 0.007185 -0.014356 0.021524 ( 0.000004 0.000005 0.000006 ) UB fit with 469 obs out of 469 (total:469,skipped:0) (100.00%) unit cell: 5.9171(9) 5.9122(10) 5.9181(12) 60.056(19) 90.006(14) 59.949(17) V = 146.40(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.947) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.103886 -0.015304 0.050162 ( 0.000014 0.000026 0.000022 ) 0.087514 -0.167207 0.063441 ( 0.000012 0.000022 0.000018 ) 0.055916 -0.024347 0.122406 ( 0.000014 0.000025 0.000021 ) M - matrix: 0.021577 -0.014404 0.007185 ( 0.000004 0.000004 0.000004 ) -0.014404 0.028785 -0.014356 ( 0.000004 0.000008 0.000005 ) 0.007185 -0.014356 0.021524 ( 0.000004 0.000005 0.000006 ) UB fit with 469 obs out of 469 (total:469,skipped:0) (100.00%) unit cell: 5.9171(9) 5.9122(10) 5.9181(12) 60.056(19) 90.006(14) 59.949(17) V = 146.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 469 (total:469,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! 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: -0.103886 -0.015304 0.050162 ( 0.000014 0.000026 0.000022 ) 0.087514 -0.167207 0.063441 ( 0.000012 0.000022 0.000018 ) 0.055916 -0.024347 0.122406 ( 0.000014 0.000025 0.000021 ) M - matrix: 0.021577 -0.014404 0.007185 ( 0.000004 0.000004 0.000004 ) -0.014404 0.028785 -0.014356 ( 0.000004 0.000008 0.000005 ) 0.007185 -0.014356 0.021524 ( 0.000004 0.000005 0.000006 ) UB fit with 469 obs out of 469 (total:469,skipped:0) (100.00%) unit cell: 5.9171(9) 5.9122(10) 5.9181(12) 60.056(19) 90.006(14) 59.949(17) V = 146.40(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.104037 -0.015133 0.049586 ( 0.000012 0.000014 0.000013 ) 0.087369 -0.167136 0.063676 ( 0.000008 0.000010 0.000009 ) 0.055529 -0.024387 0.122788 ( 0.000012 0.000014 0.000013 ) M - matrix: 0.021541 -0.014382 0.007223 ( 0.000003 0.000002 0.000002 ) -0.014382 0.028758 -0.014387 ( 0.000002 0.000003 0.000003 ) 0.007223 -0.014387 0.021590 ( 0.000002 0.000003 0.000004 ) UB fit with 2245 obs out of 2245 (total:2245,skipped:0) (100.00%) unit cell: 5.9216(7) 5.9144(5) 5.9124(7) 60.056(11) 90.110(9) 60.016(10) V = 146.44(3) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 46 reflections under beam stop or inside a detector rejection region 22 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof 2997 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:09:39 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.947) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.947) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.947) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.947) PROFFIT INFO: signal sum: min=162.0000 max=22506412.0000 PROFFIT INFO: signal sum lp corr: min=241.8055 max=3282288.7828 PROFFIT INFO: background sum: min=775.0000 max=16037.0000 PROFFIT INFO: background sum sig2: min=592.0000 max=11657.0000 PROFFIT INFO: num of signal pixels: min=59 max=1009 PROFFIT INFO: Inet: min=527.5756 max=7161357.5000 PROFFIT INFO: sig(Inet): min=191.1236 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=398.18 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 64 226 384 619 680 1211 1986 2713 2996 Percent 0.0 0.1 2.1 7.5 12.8 20.7 22.7 40.4 66.3 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2997 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 2997 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7161358- 1589783 299 2406570.16 134.15 100.00 1587648- 1040811 299 1290234.87 111.49 100.00 1040513- 316710 299 611502.12 94.33 100.00 316104- 219218 299 255637.39 69.60 100.00 219115- 164781 299 188694.00 48.99 100.00 164524- 130816 299 147168.44 37.23 100.00 130699- 101451 299 115910.10 30.49 100.00 101429- 6230 299 57854.61 21.00 100.00 6210- 3595 299 4619.04 4.96 83.61 3589- 528 305 2668.42 3.21 41.97 ------------------------------------------------------------------------------------ 7161358- 528 2996 507073.73 55.44 92.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 299 808390.48 83.89 99.67 1.41- 1.05 299 724714.91 66.60 97.99 1.05- 0.92 299 614332.42 67.70 96.99 0.92- 0.82 299 477013.59 53.80 91.97 0.82- 0.74 299 494912.49 61.04 93.98 0.74- 0.67 299 516396.13 56.93 92.31 0.67- 0.61 299 317965.44 41.48 91.64 0.61- 0.56 299 451488.79 47.94 89.97 0.56- 0.51 299 345304.94 39.26 83.95 0.51- 0.40 305 323893.96 36.16 86.23 ------------------------------------------------------------------------------------ 5.26- 0.40 2996 507073.73 55.44 92.46 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:09:39 2018 Sorting 2996 observations 291 unique observations with > 7.00 F2/sig(F2) 2996 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 Total number of frames 522 Maximum number of 291 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2996 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 54 264 Total number of frames 264 2411 observations > 7.00 F2/sig(F2) 2411 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 53 263 Total number of frames 263 Removing 'redundancy=1' reflections Average redundancy: 8.3 (Out of 2411 removed 17 = 2394, unique = 289) 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 2394 observations in 5 runs Run # start # end # total # 1 0 53 54 2 0 54 109 3 0 49 159 4 0 49 209 5 0 53 263 Total number of frames 263 289 unique data precomputed (should be 289) 289 unique data with 2394 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.3 (Out of 2394 removed 0 = 2394, unique = 289) 289 unique data precomputed (should be 289) 289 unique data with 2394 observations RMS deviation of equivalent data = 0.74096 Rint = 0.68528 14 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66363, wR= 3.58553 Trying model 1 (ne=2, no=0)... Results: Rint= 0.71080, wR= 2.60819, Acormin=-0.226, Acormax=2.315, Acor_av=0.712 F test: Probability=0.000, F= 0.870 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84194, wR= 2.48966, Acormin=-0.506, Acormax=2.211, Acor_av=0.415 F test: Probability=0.000, F= 0.619 Trying model 3 (ne=4, no=0)... Results: Rint= 0.70327, wR= 2.53668, Acormin=-0.090, Acormax=2.263, Acor_av=0.706 F test: Probability=0.000, F= 0.884 Trying model 4 (ne=4, no=1)... Results: Rint= 0.87304, wR= 3.38405, Acormin=-0.491, Acormax=2.362, Acor_av=0.389 F test: Probability=0.000, F= 0.573 Trying model 5 (ne=4, no=3)... Results: Rint= 0.98314, wR= 2.41847, Acormin=-0.448, Acormax=4.018, Acor_av=0.162 F test: Probability=0.000, F= 0.450 Trying model 6 (ne=6, no=0)... Results: Rint= 0.73066, wR= 3.47414, Acormin=-0.465, Acormax=2.307, Acor_av=0.605 F test: Probability=0.000, F= 0.814 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87640, wR= 3.70732, Acormin=-0.521, Acormax=2.301, Acor_av=0.366 F test: Probability=0.000, F= 0.565 Trying model 8 (ne=6, no=3)... Results: Rint= 0.96348, wR= 2.09684, Acormin=-0.769, Acormax=4.077, Acor_av=0.148 F test: Probability=0.000, F= 0.466 Trying model 9 (ne=6, no=5)... Results: Rint= 0.99145, wR= 1.96856, Acormin=-0.607, Acormax=4.010, Acor_av=0.080 F test: Probability=0.000, F= 0.438 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86645, wR= 1.86299, Acormin=-0.888, Acormax=1.767, Acor_av=0.293 F test: Probability=0.000, F= 0.574 Trying model 11 (ne=8, no=1)... Results: Rint= 0.91285, wR= 2.65457, Acormin=-0.652, Acormax=1.409, Acor_av=0.180 F test: Probability=0.000, F= 0.517 Trying model 12 (ne=8, no=3)... Results: Rint= 1.00954, wR= 1.82523, Acormin=-0.051, Acormax=0.060, Acor_av=0.001 F test: Probability=0.000, F= 0.421 Trying model 13 (ne=8, no=5)... Results: Rint= 1.01969, wR= 1.75751, Acormin=-0.050, Acormax=0.053, Acor_av=0.001 F test: Probability=0.000, F= 0.410 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00614, wR= 1.71388, Acormin=-0.082, Acormax=0.067, Acor_av=0.001 F test: Probability=0.000, F= 0.418 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: 0.86749 There are 263 active scales (one needs to be fixed) Refinement control: frame scale #192 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 267 pars with 35778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74096 Using Levenberg-Marquardt: 0.00010 New wR= 0.72504 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.68528 with corrections 0.67533 Rint for all data: 0.86749 with corrections 0.86626 11 observations identified as outliers and rejected Cycle 2 wR= 0.71052 Using Levenberg-Marquardt: 0.00001 New wR= 0.70982 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.66696 with corrections 0.65232 Rint for all data: 0.86749 with corrections 0.86385 Final wR= 0.70982 Final frame scales: Min= 0.9321 Max= 2.2239 Final absorption correction factors: Amin= 0.6152 Amax= 1.3331 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=470.7301 max=8309506.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=203.4717 max=73323.4922 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2995 reflections read from tmp file 2224 reflections are rejected (2164 as outliers, 60 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 73 57 31 24 14 6 4 2 3 Initial Chi^2= 0.46748 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.00785 Current error model SIG(F2)^2 = 208.06*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 209.70*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 209.70*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8309506- 1534115 299 2380223.70 95.29 100.00 1533408- 997241 299 1237310.96 50.96 100.00 997082- 315023 299 605772.86 45.56 100.00 315006- 209148 299 256670.58 32.38 100.00 209069- 160497 299 182788.13 23.40 100.00 160478- 126092 299 142348.67 16.92 100.00 125845- 99802 299 113667.74 14.16 100.00 99433- 6293 299 57018.97 10.36 96.99 6277- 3423 299 4485.83 3.33 47.49 3422- 471 304 2610.05 2.54 20.39 ------------------------------------------------------------------------------------ 8309506- 471 2995 497462.24 29.45 86.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 299 882281.90 59.19 99.00 1.41- 1.05 299 732232.25 42.11 94.31 1.05- 0.92 299 624649.59 35.06 91.64 0.92- 0.82 299 475728.91 27.41 84.62 0.82- 0.74 299 460835.54 28.51 87.96 0.74- 0.67 299 505867.13 26.11 84.95 0.67- 0.61 299 300907.43 19.27 83.28 0.61- 0.56 299 418114.00 21.98 82.61 0.56- 0.51 299 314402.48 18.30 76.92 0.51- 0.40 304 263515.31 16.72 78.62 ------------------------------------------------------------------------------------ 5.26- 0.40 2995 497462.24 29.45 86.38 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 299 882281.90 59.19 99.00 5.26- 1.05 598 807257.07 50.65 96.66 5.26- 0.92 897 746387.91 45.46 94.98 5.26- 0.82 1196 678723.16 40.94 92.39 5.26- 0.74 1495 635145.64 38.46 91.51 5.26- 0.67 1794 613599.22 36.40 90.41 5.26- 0.61 2093 568928.96 33.95 89.39 5.26- 0.56 2392 550077.09 32.46 88.55 5.26- 0.51 2691 523891.02 30.88 87.25 5.26- 0.40 2995 497462.24 29.45 86.38 ------------------------------------------------------------------------------------ 5.26- 0.40 2995 497462.24 29.45 86.38 Scale applied to data: s=0.120344 (maximum obs:8309506.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.864; Rsigma 0.022: data 2995 -> merged 318 With outlier rejection... Rint 0.813; Rsigma 0.022: data 2897 -> merged 318 Rejected total: 98, method kkm 84, method Blessing 14 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404258, 5.270882 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 14.53 100.00 218 1.46 - 1.12 15 15 20.67 100.00 310 1.08 - 0.96 15 15 19.07 100.00 286 0.96 - 0.86 15 15 18.27 100.00 274 0.86 - 0.79 15 15 15.07 100.00 226 0.79 - 0.73 15 15 12.00 100.00 180 0.73 - 0.69 15 15 11.60 100.00 174 0.69 - 0.65 15 15 11.60 100.00 174 0.65 - 0.63 15 15 8.00 100.00 120 0.63 - 0.60 21 21 8.81 100.00 185 --------------------------------------------------------------- 5.92 - 0.60 156 156 13.76 100.00 2147 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:09:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921590 5.914411 5.912377 60.0559 90.1101 60.0159 2897 Reflections read from file xs1715a.hkl; mean (I/sigma) = 29.22 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1433 1509 1442 1465 2192 1939 1913 2897 N (int>3sigma) = 0 1207 1509 1216 1229 1966 1684 1655 2502 Mean intensity = 0.0 51.7 23.2 51.8 57.0 41.9 58.4 57.1 58.1 Mean int/sigma = 0.0 27.3 23.9 27.5 28.5 26.2 29.0 28.9 29.2 Lattice type: P chosen Volume: 146.44 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.912 5.912 5.914 119.94 90.04 119.92 Niggli form: a.a = 34.952 b.b = 34.956 c.c = 34.980 b.c = -17.455 a.c = -0.023 a.b = -17.434 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.100 CUBIC F-lattice R(int) = 0.156 [ 2742] Vol = 585.7 Cell: 8.360 8.376 8.365 89.99 89.98 90.09 Volume: 585.75 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.097 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 2467] Vol = 439.3 Cell: 5.912 5.912 14.501 90.01 90.08 119.92 Volume: 439.31 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.097 RHOMBOHEDRAL R-lattice R(int) = 0.147 [ 790] Vol = 439.3 Trigonal Cell: 5.912 5.912 14.501 90.01 90.08 119.92 Volume: 439.31 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.170 TETRAGONAL I-lattice R(int) = 0.147 [ 2501] Vol = 292.9 Cell: 5.919 5.918 8.360 89.92 90.05 90.07 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.125 TETRAGONAL I-lattice R(int) = 0.147 [ 2501] Vol = 292.9 Cell: 5.919 5.918 8.360 89.92 90.05 90.07 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.057 ORTHORHOMBIC I-lattice R(int) = 0.147 [ 2449] Vol = 292.9 Cell: 5.919 8.360 5.918 89.92 89.93 89.95 Volume: 292.87 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.042 MONOCLINIC I-lattice R(int) = 0.127 [ 2112] Vol = 292.9 Cell: 8.360 5.919 5.918 90.07 90.08 89.95 Volume: 292.87 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.048 MONOCLINIC I-lattice R(int) = 0.127 [ 2113] Vol = 292.9 Cell: 5.914 5.912 8.376 89.93 90.06 89.96 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.117 MONOCLINIC C-lattice R(int) = 0.119 [ 2138] Vol = 292.9 Cell: 8.360 8.376 5.912 89.93 134.97 90.09 Volume: 292.87 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.104 [ 1517] Vol = 146.4 Cell: 5.912 5.912 5.914 119.94 90.04 119.92 Volume: 146.44 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1509 0 1930 1939 2897 N (int>3sigma) = 0 0 0 0 1509 0 1678 1684 2502 Mean intensity = 0.0 0.0 0.0 0.0 23.2 0.0 59.8 58.4 58.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 29.7 29.0 29.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 24 24 224 666 N I>3s 15 15 123 666 0.6 0.6 0.5 27.2 6.5 6.5 3.7 29.2 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 0.156 2538 Fd-3m 1 1 227 C N N N N 37 2284 0.157 2576 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359837 8.375917 8.365280 89.9900 89.9770 90.0892 ZERR 1.00 0.000282 0.001642 0.002704 0.0006 0.0105 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 3338271- 887147 340 317 31 10.2 1398102.74 62.04 0.601 0.507 870072- 669566 402 394 31 12.7 762619.59 39.69 0.955 0.850 667909- 535642 375 371 31 12.0 585541.32 32.83 0.987 0.954 534738- 446531 345 340 31 11.0 454864.43 31.53 0.936 1.050 446093- 339680 305 297 31 9.6 377024.68 27.33 0.969 1.123 339140- 247523 343 319 31 10.3 239309.49 20.01 0.803 0.980 241914- 130830 324 311 31 10.0 155669.35 18.34 0.636 0.672 129834- 104122 183 179 31 5.8 114413.01 14.96 0.340 0.198 102588- 73571 226 220 31 7.1 87533.26 11.32 0.605 0.498 72616- 1272 152 149 39 3.8 49396.00 7.28 0.775 0.777 ------------------------------------------------------------------------------------------- 3338271- 1272 2995 2897 318 9.1 483046.91 29.22 0.813 0.776 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 584 561 31 18.1 790398.10 51.05 0.795 0.835 0.013 1.05-0.83 567 556 31 17.9 554303.81 31.80 0.924 1.023 0.020 0.83-0.72 432 425 33 12.9 454821.87 26.86 0.780 0.838 0.024 0.72-0.65 348 342 31 11.0 385264.87 23.01 0.881 0.920 0.026 0.65-0.60 290 283 32 8.8 405668.81 22.27 0.824 0.876 0.028 0.59-0.56 249 238 34 7.0 272350.00 17.28 0.748 0.716 0.036 0.55-0.52 187 181 31 5.8 376203.26 20.48 0.757 0.744 0.031 0.51-0.49 140 131 31 4.2 249350.42 16.00 0.615 0.515 0.037 0.49-0.46 118 108 31 3.5 230762.54 15.60 0.489 0.345 0.040 0.46-0.40 80 72 33 2.2 241904.79 15.98 0.288 0.192 0.040 ------------------------------------------------------------------------------------------------------ inf-0.40 2995 2897 318 9.1 483046.91 29.22 0.813 0.776 0.022 inf-0.60 2199 2147 156 13.8 552269.80 33.30 0.839 0.892 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 561 31 31 100.0 18.1 790398.10 247.84 0.795 0.004 1.05-0.83 556 31 31 100.0 17.9 554303.81 167.21 0.924 0.006 0.83-0.72 425 33 33 100.0 12.9 454821.87 114.85 0.780 0.009 0.72-0.65 342 31 31 100.0 11.0 385264.87 99.06 0.881 0.012 0.65-0.60 283 32 32 100.0 8.8 405668.81 84.45 0.824 0.013 0.59-0.56 238 38 34 89.5 7.0 272350.00 57.64 0.748 0.016 0.55-0.52 181 35 31 88.6 5.8 376203.26 60.49 0.757 0.016 0.51-0.49 131 42 31 73.8 4.2 249350.42 39.50 0.615 0.020 0.49-0.46 108 55 31 56.4 3.5 230762.54 35.00 0.489 0.024 0.46-0.40 72 134 33 24.6 2.2 241904.79 26.76 0.288 0.027 -------------------------------------------------------------------------------------------- inf-0.40 2897 464 318 68.5 9.1 483046.91 129.15 0.813 0.012 inf-0.60 2147 156 156 100.0 13.8 552269.80 157.07 0.839 0.008 Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.034792 -0.076809 0.007566 ( 0.000007 0.000007 0.000007 ) 0.008045 0.011846 0.083567 ( 0.000005 0.000005 0.000005 ) -0.076965 -0.033630 0.012193 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007199 0.000011 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000011 0.007171 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000003 -0.000001 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.034792 -0.076809 0.007566 ( 0.000007 0.000007 0.000007 ) 0.008045 0.011846 0.083567 ( 0.000005 0.000005 0.000005 ) -0.076965 -0.033630 0.012193 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3599(7) 8.3761(7) 8.3654(5) 89.990(6) 89.977(6) 90.090(6) V = 585.77(7) unit cell: 8.36713(18) 8.36713(18) 8.36713(18) 90.0 90.0 90.0 V = 585.77(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=53.000) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.947) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.947) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.947) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.947) PROFFIT INFO: signal sum: min=162.0000 max=22506412.0000 PROFFIT INFO: signal sum lp corr: min=241.8055 max=3282288.7828 PROFFIT INFO: background sum: min=775.0000 max=16037.0000 PROFFIT INFO: background sum sig2: min=592.0000 max=11657.0000 PROFFIT INFO: num of signal pixels: min=59 max=1009 PROFFIT INFO: Inet: min=527.5756 max=7161357.5000 PROFFIT INFO: sig(Inet): min=191.1236 max=63702.2305 PROFFIT INFO: Inet/sig(Inet): min=0.42 max=398.18 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 128 452 768 1238 1360 2422 3972 5426 5992 Percent 0.0 0.1 2.1 7.5 12.8 20.7 22.7 40.4 66.3 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2997 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 2997 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7161358- 1589783 299 2406570.16 134.15 100.00 1587648- 1040811 299 1290234.87 111.49 100.00 1040513- 316710 299 611502.12 94.33 100.00 316104- 219218 299 255637.39 69.60 100.00 219115- 164781 299 188694.00 48.99 100.00 164524- 130816 299 147168.44 37.23 100.00 130699- 101451 299 115910.10 30.49 100.00 101429- 6230 299 57854.61 21.00 100.00 6210- 3595 299 4619.04 4.96 83.61 3589- 528 305 2668.42 3.21 41.97 ------------------------------------------------------------------------------------ 7161358- 528 2996 507073.73 55.44 92.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 299 846154.89 88.61 100.00 1.41- 1.12 299 808740.07 72.42 98.33 1.12- 0.96 299 638409.23 73.13 99.00 0.96- 0.88 299 486476.52 60.32 94.98 0.88- 0.81 299 647735.10 69.85 97.32 0.81- 0.74 299 366099.61 42.73 92.98 0.73- 0.71 299 259302.34 35.86 91.30 0.71- 0.65 299 521774.86 52.04 95.32 0.65- 0.62 299 256658.01 29.93 74.92 0.62- 0.58 305 244652.65 30.01 80.66 ------------------------------------------------------------------------------------ 4.82- 0.58 2996 507073.73 55.44 92.46 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:09:40 2018 Sorting 2996 observations 85 unique observations with > 7.00 F2/sig(F2) 2996 observations in 5 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 Total number of frames 522 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 2996 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 Total number of frames 78 2411 observations > 7.00 F2/sig(F2) 2411 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 27.0 (Out of 2411 removed 6 = 2405, unique = 89) 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 2405 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 Total number of frames 78 89 unique data precomputed (should be 89) 89 unique data with 2405 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.0 (Out of 2405 removed 0 = 2405, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 2405 observations RMS deviation of equivalent data = 0.21574 Rint = 0.17325 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17167, wR= 0.22224 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08157, wR= 0.10719, Acormin=0.656, Acormax=1.421, Acor_av=0.960 F test: Probability=1.000, F= 4.420 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08215, wR= 0.10194, Acormin=0.611, Acormax=1.392, Acor_av=0.907 F test: Probability=0.000, F= 0.985 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06818, wR= 0.09434, Acormin=0.671, Acormax=1.468, Acor_av=0.964 F test: Probability=1.000, F= 1.426 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06466, wR= 0.08576, Acormin=0.594, Acormax=1.474, Acor_av=0.906 F test: Probability=0.994, F= 1.111 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06162, wR= 0.08299, Acormin=0.517, Acormax=1.326, Acor_av=0.829 F test: Probability=0.987, F= 1.098 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06395, wR= 0.08679, Acormin=0.663, Acormax=1.544, Acor_av=0.930 F test: Probability=0.000, F= 0.927 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06111, wR= 0.08090, Acormin=0.601, Acormax=1.506, Acor_av=0.892 F test: Probability=0.632, F= 1.014 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05755, wR= 0.07708, Acormin=0.532, Acormax=1.378, Acor_av=0.823 F test: Probability=0.999, F= 1.140 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05206, wR= 0.07198, Acormin=0.480, Acormax=1.343, Acor_av=0.757 F test: Probability=1.000, F= 1.216 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06135, wR= 0.08114, Acormin=0.658, Acormax=1.527, Acor_av=0.917 F test: Probability=0.000, F= 0.722 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05672, wR= 0.07418, Acormin=0.587, Acormax=1.488, Acor_av=0.876 F test: Probability=0.000, F= 0.843 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05354, wR= 0.06968, Acormin=0.262, Acormax=0.696, Acor_av=0.416 F test: Probability=0.000, F= 0.943 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04808, wR= 0.06385, Acormin=0.285, Acormax=0.772, Acor_av=0.457 F test: Probability=1.000, F= 1.164 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04343, wR= 0.05911, Acormin=0.300, Acormax=0.999, Acor_av=0.493 F test: Probability=1.000, F= 1.417 Final absorption model (ne=6, no=5): Rint= 0.05206, Acormin=0.480, Acormax=1.343, Acor_av=0.757 Combined refinement in use Rint: 0.17335 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: 6, max odd order: 5 (48 parameters) Refinement control: 125 pars with 7875 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21574 Using Levenberg-Marquardt: 0.00010 New wR= 0.05393 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17325 with corrections 0.04073 Rint for all data: 0.17335 with corrections 0.04093 0 observations identified as outliers and rejected Cycle 2 wR= 0.05393 Using Levenberg-Marquardt: 0.00001 New wR= 0.05007 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17325 with corrections 0.03709 Rint for all data: 0.17335 with corrections 0.03730 0 observations identified as outliers and rejected Cycle 3 wR= 0.05007 Using Levenberg-Marquardt: 0.00000 New wR= 0.04979 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17325 with corrections 0.03684 Rint for all data: 0.17335 with corrections 0.03705 0 observations identified as outliers and rejected Cycle 4 wR= 0.04979 Using Levenberg-Marquardt: 0.00000 New wR= 0.04978 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17325 with corrections 0.03683 Rint for all data: 0.17335 with corrections 0.03704 Final wR= 0.04978 Final frame scales: Min= 0.9039 Max= 1.1192 Final absorption correction factors: Amin= 0.5764 Amax= 1.5715 PROFFIT INFO: Inet (after scale3 abspack): min=532.7231 max=5625295.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=165.3843 max=67728.8359 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2996 reflections read from tmp file 444 reflections are rejected (443 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 2 3 2 1 6 2 87 Initial Chi^2= 0.32593 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.37095 Current error model SIG(F2)^2 = 111.79*I_RAW + 0.00*I_BACK+(0.00984*)^2 Cycle 2, Chi^2= 1.15224 Current error model SIG(F2)^2 = 59.44*I_RAW + 0.00*I_BACK+(0.02373*)^2 Cycle 3, Chi^2= 1.01296 Current error model SIG(F2)^2 = 94.95*I_RAW + 0.00*I_BACK+(0.01815*)^2 Cycle 4, Chi^2= 1.00100 Current error model SIG(F2)^2 = 87.48*I_RAW + 0.00*I_BACK+(0.02002*)^2 Cycle 5, Chi^2= 1.00024 Current error model SIG(F2)^2 = 90.35*I_RAW + 0.00*I_BACK+(0.01942*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 89.47*I_RAW + 0.00*I_BACK+(0.01961*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 89.76*I_RAW + 0.00*I_BACK+(0.01955*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 89.76*I_RAW + 0.00*I_BACK+(0.01955*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5625296- 1578091 299 2340747.98 47.80 100.00 1569013- 1001415 299 1235434.20 41.96 100.00 998449- 327498 299 609286.08 40.17 100.00 327336- 204793 299 248209.75 34.17 100.00 204533- 169158 299 185092.13 27.98 100.00 169135- 126931 299 142508.33 22.38 100.00 126655- 101086 299 113926.86 19.63 100.00 100892- 5859 299 59357.39 14.70 100.00 5807- 3473 299 4362.92 4.97 100.00 3461- 533 305 2677.84 3.84 79.67 ------------------------------------------------------------------------------------ 5625296- 533 2996 493176.07 25.71 97.93 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 299 880391.05 38.58 100.00 1.41- 1.12 299 822909.92 31.21 100.00 1.12- 0.96 299 602775.88 29.64 100.00 0.96- 0.88 299 472029.97 26.06 98.66 0.88- 0.81 299 615795.85 30.17 99.33 0.81- 0.74 299 341593.46 21.25 99.00 0.73- 0.71 299 247193.13 20.08 98.33 0.71- 0.65 299 486469.86 25.64 99.00 0.65- 0.62 299 239250.91 17.05 90.64 0.62- 0.58 305 228658.72 17.64 94.43 ------------------------------------------------------------------------------------ 4.82- 0.58 2996 493176.07 25.71 97.93 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 299 880391.05 38.58 100.00 4.82- 1.12 598 851650.49 34.89 100.00 4.82- 0.96 897 768692.29 33.14 100.00 4.82- 0.88 1196 694526.71 31.37 99.67 4.82- 0.81 1495 678780.54 31.13 99.60 4.82- 0.74 1794 622582.69 29.48 99.50 4.82- 0.71 2093 568955.61 28.14 99.33 4.82- 0.65 2392 558644.89 27.83 99.29 4.82- 0.62 2691 523156.67 26.63 98.33 4.82- 0.58 2996 493176.07 25.71 97.93 ------------------------------------------------------------------------------------ 4.82- 0.58 2996 493176.07 25.71 97.93 Scale applied to data: s=0.177768 (maximum obs:5625295.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.025: data 2996 -> merged 109 With outlier rejection... Rint 0.035; Rsigma 0.025: data 2982 -> merged 109 Rejected total: 14, method kkm 11, method Blessing 3 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585816, 4.830763 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 17.30 100.00 173 1.61 - 1.21 10 10 27.40 100.00 274 1.17 - 1.01 10 10 35.70 100.00 357 0.99 - 0.89 10 10 35.20 100.00 352 0.88 - 0.81 10 10 33.80 100.00 338 0.81 - 0.74 10 10 29.20 100.00 292 0.73 - 0.71 10 10 31.90 100.00 319 0.70 - 0.66 10 10 27.00 100.00 270 0.66 - 0.64 10 10 25.10 100.00 251 0.63 - 0.60 10 10 25.50 100.00 255 --------------------------------------------------------------- 5.92 - 0.60 100 100 28.81 100.00 2881 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:09:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921590 5.914411 5.912377 60.0559 90.1101 60.0159 2897 Reflections read from file xs1715a.hkl; mean (I/sigma) = 29.22 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1433 1509 1442 1465 2192 1939 1913 2897 N (int>3sigma) = 0 1207 1509 1216 1229 1966 1684 1655 2502 Mean intensity = 0.0 51.7 23.2 51.8 57.0 41.9 58.4 57.1 58.1 Mean int/sigma = 0.0 27.3 23.9 27.5 28.5 26.2 29.0 28.9 29.2 Lattice type: P chosen Volume: 146.44 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.912 5.912 5.914 119.94 90.04 119.92 Niggli form: a.a = 34.952 b.b = 34.956 c.c = 34.980 b.c = -17.455 a.c = -0.023 a.b = -17.434 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.100 CUBIC F-lattice R(int) = 0.156 [ 2742] Vol = 585.7 Cell: 8.360 8.376 8.365 89.99 89.98 90.09 Volume: 585.75 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.097 RHOMBOHEDRAL R-lattice R(int) = 0.145 [ 2467] Vol = 439.3 Cell: 5.912 5.912 14.501 90.01 90.08 119.92 Volume: 439.31 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.097 RHOMBOHEDRAL R-lattice R(int) = 0.147 [ 790] Vol = 439.3 Trigonal Cell: 5.912 5.912 14.501 90.01 90.08 119.92 Volume: 439.31 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.170 TETRAGONAL I-lattice R(int) = 0.147 [ 2501] Vol = 292.9 Cell: 5.919 5.918 8.360 89.92 90.05 90.07 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.125 TETRAGONAL I-lattice R(int) = 0.147 [ 2501] Vol = 292.9 Cell: 5.919 5.918 8.360 89.92 90.05 90.07 Volume: 292.87 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.057 ORTHORHOMBIC I-lattice R(int) = 0.147 [ 2449] Vol = 292.9 Cell: 5.919 8.360 5.918 89.92 89.93 89.95 Volume: 292.87 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.042 MONOCLINIC I-lattice R(int) = 0.127 [ 2112] Vol = 292.9 Cell: 8.360 5.919 5.918 90.07 90.08 89.95 Volume: 292.87 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.048 MONOCLINIC I-lattice R(int) = 0.127 [ 2113] Vol = 292.9 Cell: 5.914 5.912 8.376 89.93 90.06 89.96 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.117 MONOCLINIC C-lattice R(int) = 0.119 [ 2138] Vol = 292.9 Cell: 8.360 8.376 5.912 89.93 134.97 90.09 Volume: 292.87 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.104 [ 1517] Vol = 146.4 Cell: 5.912 5.912 5.914 119.94 90.04 119.92 Volume: 146.44 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1509 0 1930 1939 2897 N (int>3sigma) = 0 0 0 0 1509 0 1678 1684 2502 Mean intensity = 0.0 0.0 0.0 0.0 23.2 0.0 59.8 58.4 58.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 29.7 29.0 29.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 24 24 224 666 N I>3s 15 15 123 666 0.6 0.6 0.5 27.2 6.5 6.5 3.7 29.2 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 0.156 2538 Fd-3m 1 1 227 C N N N N 37 2284 0.157 2576 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 xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359837 8.375917 8.365280 89.9900 89.9770 90.0892 ZERR 1.00 0.000282 0.001642 0.002704 0.0006 0.0105 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\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5442481- 910439 669 663 27 24.6 1693160.05 44.08 0.033 0.041 900914- 157184 886 882 27 32.7 286777.61 33.23 0.038 0.050 145836- 53172 738 737 27 27.3 113315.60 19.66 0.052 0.068 22369- 1906 703 700 28 25.0 4682.41 5.00 0.152 0.182 ------------------------------------------------------------------------------------------- 5442481- 1906 2996 2982 109 27.4 490373.66 25.66 0.035 0.044 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 746 739 27 27.4 788848.69 34.74 0.033 0.040 0.022 1.01-0.78 888 886 27 32.8 492602.01 25.90 0.031 0.042 0.025 0.78-0.65 813 810 27 30.0 376001.37 22.04 0.039 0.047 0.029 0.65-0.59 549 547 28 19.5 252885.87 18.37 0.050 0.059 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 2996 2982 109 27.4 490373.66 25.66 0.035 0.044 0.025 inf-0.60 2891 2879 99 29.1 500902.66 25.98 0.035 0.044 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 739 27 27 100.0 27.4 788848.69 205.66 0.033 0.007 1.01-0.78 886 27 27 100.0 32.8 492602.01 160.05 0.031 0.005 0.78-0.65 810 27 27 100.0 30.0 376001.37 127.73 0.039 0.006 0.65-0.59 547 29 28 96.6 19.5 252885.87 94.13 0.050 0.010 -------------------------------------------------------------------------------------------- inf-0.59 2982 110 109 99.1 27.4 490373.66 150.48 0.035 0.006 inf-0.60 2879 99 99 100.0 29.1 500902.66 153.44 0.035 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC FULLAUTOANALYSECONCURRENT Process information (Wed Mar 28 14:13:45 2018) ID: 2932; threads 39; handles 877; mem 523852.00 (1237724.00)kB; time: 1w 5d 23h 19m 15s MEMORY INFO: Memory PF:8.0, Ph:179.0, V:1208.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:515.0,peak PF: 708.5, WS: 280.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) CRYSALIS auto analyse procedure 2005-2017 (version 1.0.2) AUTO INFO: Started at Wed Mar 28 14:13:45 2018 AUTO INFO: Experiment: D:\Data\xs1715a\xs1715a.run AUTO INFO: Clearing peak tables (hunting=200000 peaks,xyz=100000 peaks) MACHINE INFORMATION - GONIOMETER (RIGAKU) OXFORD DIFFRACTION/AGILENT TECHNOLOGIES KM4 XCALIBUR - ALPHA (DEG) 50.02178 BETA (DEG) -0.00611 - WAVELENGTH MO (ANG): A1 0.70930 A2 0.71359 B1 0.63229 - POLARISATION FACTOR 0.50000 - X-RAY BEAM ORIENTATION (DEG): X2 -0.00984 X3 0.00000 - BEAM PATH ABSORPTIONCOEFFICIENTS (MM-1): AIR 0.00013 BE 0.04736 - BE THICKNESS (MM): 0.50000 - SOFTWARE ZEROCORRECTION (DEG): OMEGA 0.00285 THETA -0.14800 KAPPA -0.13240 PHI 0.00000 DETECTOR 0.00000 - MACHINE OFFSETS (STEPS): OMEGA 0 THETA 0 KAPPA 0 PHI 0 DETECTOR 134439 - CCD DETECTOR ATLAS - CHIP: Kodak_KAF4320 B2 (2048x2048) 5629 - TAPER: Incom (B1,3620-2), ZOOM 2.005621 PIXELSIZE IN 1X1 BINNING (MM) 0.04813 - GAIN 90.00 (DOUBLE-CORRELATED-DIVIDE-BY-2 GAIN), IMAGE GAIN 90.00, ELECTRONS/ADU 2.10 - DETECTOR ROTATION (DEG): X1 0.74600 X2 -0.07600 X3 0.00000 - DETECTOR DISTANCE (MM): 53.00000 - DETECTOR ZERO (PIX, 1X1 BINNING): X 1028.28400 Y 1027.50900 - DETECTOR BINNING (PIX): X: 4 Y: 4 (XW: 2048, YW: 2048) - FLAT FIELD CORRECTION FILES: floodmo_a_101_calib_110512.ffiinffit floodcu_a_101_calib_110512.ffiinffit - GEOMETRIC CORRECTION FILE : a_101_020512.geo - GEOMETRIC CORRECTION STATUS: ALLOCATED:1, USED:1, GRIDX:255, GRIDY:255 - GEOMETRIC CORRECTION GRID LOADED: C:\Xcalibur\corrections\a_101\a_101_020512.geo - NO PIXEL DETECTOR CORRECTIONS! PROGRAM VERSION - PROGRAM RED 39.29c (release 19-06-2017) - (X)PAR FILE NAME xs1715a\xs1715a.par ******************************************************************************************************* Auto analyse stage: PEAK HUNTING (Wed Mar 28 14:13:45 2018) ******************************************************************************************************* CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -120.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.94 ka= -77.13 ph= -150.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= -57.13 ph= -60.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 90.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 76.87 ph= 150.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.65 ka= 56.87 ph= 0.00 AUTO INFO: 6268 peaks in the peak location table 6268 peak locations are merged to 2990 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 2990 unindexed peaks to the CrysAlis peak table (2990 with profile info) ******************************************************************************************************* Auto analyse stage: CELL FINDING (Wed Mar 28 14:13:50 2018) ******************************************************************************************************* Instrument model: dd: 53.00, x0: 1028.28, y0: 1027.51, beam: -0.01, o0: 0.00, t0: -0.15, k0: -0.13 AUTO INFO: Dirax started... UM TTT - Duisenberg-like algorithm lattice finding - Rigaku Oxford Diffraction 2004-2017 (version: 1.5) UM TTT INFO: random number seed 1522260830! 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: 1 466(sub) 2750(all), cF( 1,12) 8.38 8.38 8.35 89.95 90.01 89.99 pr: 146.49, r: 585.97 UM TTTSOLUTION 2: 2 383(sub) 2661(all), hP(12, 9) 5.92 5.92 14.49 90.16 89.83 119.83 pr: 440.03, r: 440.03 UM TTTSOLUTION 3: 3 403(sub) 2381(all), oC(23, 4) 11.83 16.76 5.91 90.02 90.22 89.97 pr: 586.55, r: 1173.11 UM TTTSOLUTION 4: 4 414(sub) 2107(all), hR( 9, 8) 5.91 5.93 28.99 90.01 90.18 120.05 pr: 293.30, r: 879.89 UM TTTSOLUTION 5: 5 391(sub) 2054(all), oI(42, 4) 5.92 10.26 28.97 90.03 90.13 90.11 pr: 879.74, r: 1759.48 Peak table: 500(sub) 2990(all) Best cell: 466 indexed, Niggli cF( 1,12): 8.38 8.38 8.35 89.95 90.01 89.99 prim: 146.49, red: 585.97 UM TTTSOLUTION 1: 6 466(sub) 2750(all), cF( 1,12) 8.38 8.38 8.35 89.95 90.01 89.99 pr: 146.49, r: 585.97 UM TTTSOLUTION 2: 7 383(sub) 2661(all), hP(12, 9) 5.92 5.92 14.49 90.16 89.83 119.83 pr: 440.03, r: 440.03 UM TTTSOLUTION 3: 8 403(sub) 2381(all), oC(23, 4) 11.83 16.76 5.91 90.02 90.22 89.97 pr: 586.55, r: 1173.11 UM TTTSOLUTION 4: 9 414(sub) 2107(all), hR( 9, 8) 5.91 5.93 28.99 90.01 90.18 120.05 pr: 293.30, r: 879.89 UM TTTSOLUTION 5: 10 391(sub) 2054(all), oI(42, 4) 5.92 10.26 28.97 90.03 90.13 90.11 pr: 879.74, r: 1759.48 Peak table: 500(sub) 2990(all) Best cell: 466 indexed, Niggli cF( 1,12): 8.38 8.38 8.35 89.95 90.01 89.99 prim: 146.49, red: 585.97 UM TTTSOLUTION 1: 11 466(sub) 2750(all), cF( 1,12) 8.38 8.38 8.35 89.95 90.01 89.99 pr: 146.49, r: 585.97 UM TTTSOLUTION 2: 12 383(sub) 2661(all), hP(12, 9) 5.92 5.92 14.49 90.16 89.83 119.83 pr: 440.03, r: 440.03 UM TTTSOLUTION 3: 13 403(sub) 2381(all), oC(23, 4) 11.83 16.76 5.91 90.02 90.22 89.97 pr: 586.55, r: 1173.11 UM TTTSOLUTION 4: 14 414(sub) 2107(all), hR( 9, 8) 5.91 5.93 28.99 90.01 90.18 120.05 pr: 293.30, r: 879.89 UM TTTSOLUTION 5: 15 391(sub) 2054(all), oI(42, 4) 5.92 10.26 28.97 90.03 90.13 90.11 pr: 879.74, r: 1759.48 Peak table: 500(sub) 2990(all) Best cell: 466 indexed, Niggli cF( 1,12): 8.38 8.38 8.35 89.95 90.01 89.99 prim: 146.49, red: 585.97 UM TTTSOLUTION 1: 16 466(sub) 2750(all), cF( 1,12) 8.38 8.38 8.35 89.95 90.01 89.99 pr: 146.49, r: 585.97 UM TTTSOLUTION 2: 17 383(sub) 2661(all), hP(12, 9) 5.92 5.92 14.49 90.16 89.83 119.83 pr: 440.03, r: 440.03 UM TTTSOLUTION 3: 18 403(sub) 2381(all), oC(23, 4) 11.83 16.76 5.91 90.02 90.22 89.97 pr: 586.55, r: 1173.11 UM TTTSOLUTION 4: 19 414(sub) 2107(all), hR( 9, 8) 5.91 5.93 28.99 90.01 90.18 120.05 pr: 293.30, r: 879.89 UM TTTSOLUTION 5: 20 391(sub) 2054(all), oI(42, 4) 5.92 10.26 28.97 90.03 90.13 90.11 pr: 879.74, r: 1759.48 Peak table: 500(sub) 2990(all) Best cell: 466 indexed, Niggli cF( 1,12): 8.38 8.38 8.35 89.95 90.01 89.99 prim: 146.49, red: 585.97 Make subset: 0.00019 Make T-vectors: 0.42812 Make unit cell: 0.65418 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 2854 obs out of 2990 (total:2990,skipped:0) (95.45%) UB - matrix: 0.104096 0.119158 0.153653 ( 0.000026 0.000024 0.000031 ) -0.087241 0.079636 -0.023710 ( 0.000017 0.000016 0.000021 ) -0.055677 -0.031298 0.067120 ( 0.000020 0.000019 0.000024 ) M - matrix: 0.021547 0.007199 0.014326 ( 0.000006 0.000005 0.000006 ) 0.007199 0.021520 0.014320 ( 0.000005 0.000006 0.000006 ) 0.014326 0.014320 0.028676 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9129(12) 5.9172(10) 5.9116(14) 119.89(2) 119.88(2) 90.179(15) V = 146.55(4) UB fit with 2856 obs out of 2990 (total:2990,skipped:0) (95.52%) UB - matrix: 0.104093 0.119157 0.153657 ( 0.000026 0.000024 0.000031 ) -0.087237 0.079634 -0.023709 ( 0.000017 0.000016 0.000021 ) -0.055674 -0.031294 0.067125 ( 0.000020 0.000019 0.000024 ) M - matrix: 0.021545 0.007199 0.014326 ( 0.000007 0.000005 0.000006 ) 0.007199 0.021519 0.014321 ( 0.000005 0.000006 0.000006 ) 0.014326 0.014321 0.028678 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9131(12) 5.9174(10) 5.9114(14) 119.89(2) 119.88(2) 90.179(15) V = 146.56(4) UB fit with 2855 obs out of 2990 (total:2990,skipped:0) (95.48%) UB - matrix: 0.104091 0.119157 0.153657 ( 0.000026 0.000024 0.000031 ) -0.087236 0.079633 -0.023710 ( 0.000017 0.000016 0.000021 ) -0.055673 -0.031294 0.067125 ( 0.000020 0.000019 0.000024 ) M - matrix: 0.021545 0.007199 0.014326 ( 0.000007 0.000005 0.000006 ) 0.007199 0.021519 0.014321 ( 0.000005 0.000006 0.000006 ) 0.014326 0.014321 0.028678 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9132(12) 5.9174(10) 5.9114(14) 119.89(2) 119.88(2) 90.179(15) V = 146.56(4) UM TTT INFO: No smaller volume found Primitive unit cell refinement UB fit with 2854 obs out of 2990 (total:2990,skipped:0) (95.45%) UB - matrix: 0.104096 0.119158 0.153653 ( 0.000026 0.000024 0.000031 ) -0.087241 0.079636 -0.023710 ( 0.000017 0.000016 0.000021 ) -0.055677 -0.031298 0.067120 ( 0.000020 0.000019 0.000024 ) M - matrix: 0.021547 0.007199 0.014326 ( 0.000006 0.000005 0.000006 ) 0.007199 0.021520 0.014320 ( 0.000005 0.000006 0.000006 ) 0.014326 0.014320 0.028676 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9129(12) 5.9172(10) 5.9116(14) 119.89(2) 119.88(2) 90.179(15) V = 146.55(4) No constraint UB - matrix: -0.007525 0.076798 -0.034813 ( 0.000011 0.000012 0.000011 ) -0.083431 -0.011845 -0.008052 ( 0.000009 0.000009 0.000008 ) -0.012193 0.033595 0.077030 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.007166 0.000001 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007167 0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 0.000010 0.007210 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007525 0.076798 -0.034813 ( 0.000011 0.000012 0.000011 ) -0.083431 -0.011845 -0.008052 ( 0.000009 0.000009 0.000008 ) -0.012193 0.033595 0.077030 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000000 ) UB fit with 2751 obs out of 2990 (total:2990,skipped:0) (92.01%) unit cell: 8.3789(8) 8.3785(12) 8.3531(10) 90.077(10) 89.957(9) 90.006(10) V = 586.41(12) unit cell: 8.3702(3) 8.3702(3) 8.3702(3) 90.0 90.0 90.0 V = 586.41(3) AUTO INFO: Dirax ended... LAMBDA HALF REJECTION: Number of processed reflections: 1110 Number of skipped reflections, because of (potential) lambda half effect: 32 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 1522260832! 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: 1 457(sub) 2745(all), cF( 1,12) 8.38 8.37 8.34 90.05 90.00 89.93 pr: 146.29, r: 585.16 UM TTTSOLUTION 2: 2 415(sub) 2658(all), hP(12, 9) 5.91 5.91 14.49 90.11 89.85 119.85 pr: 439.48, r: 439.48 UM TTTSOLUTION 3: 3 397(sub) 2622(all), tI(18, 7) 13.24 13.20 8.38 89.99 90.01 90.08 pr: 732.28, r: 1464.56 UM TTTSOLUTION 4: 4 412(sub) 2589(all), tI(15, 7) 8.38 8.38 16.70 90.00 89.99 90.04 pr: 585.89, r: 1171.78 UM TTTSOLUTION 5: 5 398(sub) 2375(all), mI(39, 2) 13.24 8.37 24.37 89.92 102.68 89.99 pr: 1318.19, r: 2636.38 UM TTTSOLUTION 6: 6 395(sub) 2277(all), oC(36, 4) 8.38 25.05 8.38 89.95 90.04 90.06 pr: 878.81, r: 1757.62 UM TTTSOLUTION 7: 7 388(sub) 2245(all), mI(39, 2) 14.48 5.93 24.40 90.02 101.61 89.93 pr: 1025.24, r: 2050.48 Peak table: 500(sub) 2985(all) Best cell: 457 indexed, Niggli cF( 1,12): 8.38 8.37 8.34 90.05 90.00 89.93 prim: 146.29, red: 585.16 UM TTTSOLUTION 1: 8 457(sub) 2745(all), cF( 1,12) 8.38 8.37 8.34 90.05 90.00 89.93 pr: 146.29, r: 585.16 UM TTTSOLUTION 2: 9 406(sub) 2745(all), cP( 3,10) 8.35 8.38 8.38 90.02 90.01 90.02 pr: 585.90, r: 585.90 UM TTTSOLUTION 3: 10 415(sub) 2658(all), hP(12, 9) 5.91 5.91 14.49 90.11 89.85 119.85 pr: 439.48, r: 439.48 UM TTTSOLUTION 4: 11 397(sub) 2622(all), tI(18, 7) 13.24 13.20 8.38 89.99 90.01 90.08 pr: 732.28, r: 1464.56 UM TTTSOLUTION 5: 12 398(sub) 2375(all), mI(39, 2) 13.24 8.37 24.37 89.92 102.68 89.99 pr: 1318.19, r: 2636.38 UM TTTSOLUTION 6: 13 395(sub) 2277(all), oC(36, 4) 8.38 25.05 8.38 89.95 90.04 90.06 pr: 878.81, r: 1757.62 UM TTTSOLUTION 7: 14 388(sub) 2245(all), mI(39, 2) 14.48 5.93 24.40 90.02 101.61 89.93 pr: 1025.24, r: 2050.48 Peak table: 500(sub) 2985(all) Best cell: 457 indexed, Niggli cF( 1,12): 8.38 8.37 8.34 90.05 90.00 89.93 prim: 146.29, red: 585.16 UM TTTSOLUTION 1: 15 457(sub) 2745(all), cF( 1,12) 8.38 8.37 8.34 90.05 90.00 89.93 pr: 146.29, r: 585.16 UM TTTSOLUTION 2: 16 406(sub) 2745(all), cP( 3,10) 8.35 8.38 8.38 90.02 90.01 90.02 pr: 585.90, r: 585.90 UM TTTSOLUTION 3: 17 415(sub) 2658(all), hP(12, 9) 5.91 5.91 14.49 90.11 89.85 119.85 pr: 439.48, r: 439.48 UM TTTSOLUTION 4: 18 397(sub) 2622(all), tI(18, 7) 13.24 13.20 8.38 89.99 90.01 90.08 pr: 732.28, r: 1464.56 UM TTTSOLUTION 5: 19 398(sub) 2375(all), mI(39, 2) 13.24 8.37 24.37 89.92 102.68 89.99 pr: 1318.19, r: 2636.38 UM TTTSOLUTION 6: 20 395(sub) 2277(all), oC(36, 4) 8.38 25.05 8.38 89.95 90.04 90.06 pr: 878.81, r: 1757.62 UM TTTSOLUTION 7: 21 388(sub) 2245(all), mI(39, 2) 14.48 5.93 24.40 90.02 101.61 89.93 pr: 1025.24, r: 2050.48 Peak table: 500(sub) 2985(all) Best cell: 457 indexed, Niggli cF( 1,12): 8.38 8.37 8.34 90.05 90.00 89.93 prim: 146.29, red: 585.16 UM TTTSOLUTION 1: 22 457(sub) 2745(all), cF( 1,12) 8.38 8.37 8.34 90.05 90.00 89.93 pr: 146.29, r: 585.16 UM TTTSOLUTION 2: 23 406(sub) 2745(all), cP( 3,10) 8.35 8.38 8.38 90.02 90.01 90.02 pr: 585.90, r: 585.90 UM TTTSOLUTION 3: 24 415(sub) 2658(all), hP(12, 9) 5.91 5.91 14.49 90.11 89.85 119.85 pr: 439.48, r: 439.48 UM TTTSOLUTION 4: 25 397(sub) 2622(all), tI(18, 7) 13.24 13.20 8.38 89.99 90.01 90.08 pr: 732.28, r: 1464.56 UM TTTSOLUTION 5: 26 398(sub) 2375(all), mI(39, 2) 13.24 8.37 24.37 89.92 102.68 89.99 pr: 1318.19, r: 2636.38 UM TTTSOLUTION 6: 27 395(sub) 2277(all), oC(36, 4) 8.38 25.05 8.38 89.95 90.04 90.06 pr: 878.81, r: 1757.62 UM TTTSOLUTION 7: 28 388(sub) 2245(all), mI(39, 2) 14.48 5.93 24.40 90.02 101.61 89.93 pr: 1025.24, r: 2050.48 Peak table: 500(sub) 2985(all) Best cell: 457 indexed, Niggli cF( 1,12): 8.38 8.37 8.34 90.05 90.00 89.93 prim: 146.29, red: 585.16 Make subset: 0.00016 Make T-vectors: 0.38267 Make unit cell: 0.68475 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 2859 obs out of 2985 (total:2990,skipped:5) (95.78%) UB - matrix: 0.015050 0.119139 -0.034463 ( 0.000025 0.000020 0.000022 ) 0.166875 0.079621 0.103361 ( 0.000025 0.000021 0.000022 ) 0.024382 -0.031294 -0.098425 ( 0.000024 0.000019 0.000021 ) M - matrix: 0.028668 0.014317 0.014330 ( 0.000009 0.000005 0.000005 ) 0.014317 0.021513 0.007204 ( 0.000005 0.000006 0.000004 ) 0.014330 0.007204 0.021559 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9126(12) 5.9184(11) 5.9117(13) 90.190(16) 119.88(2) 119.88(2) V = 146.57(5) UB fit with 2857 obs out of 2985 (total:2990,skipped:5) (95.71%) UB - matrix: 0.015055 0.119134 -0.034469 ( 0.000025 0.000020 0.000021 ) 0.166861 0.079613 0.103362 ( 0.000026 0.000021 0.000022 ) 0.024384 -0.031287 -0.098425 ( 0.000024 0.000019 0.000021 ) M - matrix: 0.028664 0.014315 0.014328 ( 0.000009 0.000005 0.000005 ) 0.014315 0.021510 0.007202 ( 0.000005 0.000006 0.000004 ) 0.014328 0.007202 0.021559 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9131(12) 5.9189(11) 5.9114(13) 90.184(16) 119.88(2) 119.89(2) V = 146.59(5) UB fit with 2855 obs out of 2985 (total:2990,skipped:5) (95.64%) UB - matrix: 0.015056 0.119133 -0.034469 ( 0.000025 0.000020 0.000021 ) 0.166859 0.079612 0.103362 ( 0.000026 0.000021 0.000023 ) 0.024383 -0.031285 -0.098426 ( 0.000024 0.000019 0.000021 ) M - matrix: 0.028663 0.014315 0.014328 ( 0.000009 0.000005 0.000005 ) 0.014315 0.021509 0.007202 ( 0.000005 0.000006 0.000004 ) 0.014328 0.007202 0.021559 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9132(12) 5.9190(11) 5.9114(13) 90.184(16) 119.88(2) 119.89(2) V = 146.59(5) UM TTT INFO: Primitive unit cell refinement unsuccessful Primitive unit cell refinement UB fit with 2859 obs out of 2985 (total:2990,skipped:5) (95.78%) UB - matrix: 0.015050 0.119139 -0.034463 ( 0.000025 0.000020 0.000022 ) 0.166875 0.079621 0.103361 ( 0.000025 0.000021 0.000022 ) 0.024382 -0.031294 -0.098425 ( 0.000024 0.000019 0.000021 ) M - matrix: 0.028668 0.014317 0.014330 ( 0.000009 0.000005 0.000005 ) 0.014317 0.021513 0.007204 ( 0.000005 0.000006 0.000004 ) 0.014330 0.007204 0.021559 ( 0.000005 0.000004 0.000006 ) unit cell: 5.9126(12) 5.9184(11) 5.9117(13) 90.190(16) 119.88(2) 119.88(2) V = 146.57(5) No constraint UB - matrix: -0.007524 0.076797 -0.034813 ( 0.000011 0.000012 0.000011 ) -0.083431 -0.011846 -0.008053 ( 0.000009 0.000009 0.000008 ) -0.012193 0.033598 0.077029 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007166 0.000001 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007167 0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 0.000010 0.007210 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007524 0.076797 -0.034813 ( 0.000011 0.000012 0.000011 ) -0.083431 -0.011846 -0.008053 ( 0.000009 0.000009 0.000008 ) -0.012193 0.033598 0.077029 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000000 ) UB fit with 2746 obs out of 2985 (total:2990,skipped:5) (91.99%) unit cell: 8.3790(8) 8.3784(12) 8.3532(10) 90.079(10) 89.957(9) 90.007(10) V = 586.41(12) unit cell: 8.3702(3) 8.3702(3) 8.3702(3) 90.0 90.0 90.0 V = 586.41(3) AUTO INFO: Dirax ended... Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" ******************************************************************************************************* Auto analyse stage: MODEL REFINEMENT (Wed Mar 28 14:13:53 2018) ******************************************************************************************************* UB fit with 2751 obs out of 2990 (total:2990,skipped:0) (92.01%) UB - matrix: -0.007525 0.076797 -0.034813 ( 0.000011 0.000012 0.000011 ) -0.083431 -0.011845 -0.008052 ( 0.000009 0.000009 0.000008 ) -0.012194 0.033597 0.077029 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007166 0.000001 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007167 0.000010 ( 0.000001 0.000002 0.000001 ) -0.000006 0.000010 0.007210 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3790(8) 8.3785(12) 8.3533(10) 90.078(10) 89.956(9) 90.006(10) V = 586.42(12) OTKP changes: 213 2 4 6 Cycle 1 - Res: 0.023363, da=0.020530, sx=0.002719, sy=0.003171, h=0.005088, k=0.007247, l=0.005338, LM=0.000000 Cycle 2 - Res: 0.022646, da=0.019899, sx=0.002631, sy=0.003001, h=0.005064, k=0.007070, l=0.005033, LM=0.000000 Cycle 3 - Res: 0.022646, da=0.019898, sx=0.002631, sy=0.003001, h=0.005064, k=0.007070, l=0.005033, LM=0.000000 Cycle 4 - Res: 0.022646, da=0.019898, sx=0.002631, sy=0.003001, h=0.005064, k=0.007070, l=0.005033, LM=0.000000 Model change (all parameters): Omega Offset 0.002850 0.055010 0.0521603 8.47144e-007 1 Kappa Offset -0.132400 -0.132400 0 0 0 Phi Offset 0.000000 0.000000 0 0 0 Alpha Value 50.021780 50.021780 0 0 0 Beta Value -0.006110 -0.006110 0 0 0 Theta Offset -0.148000 -0.139904 0.00809564 1.85266e-006 1 Det. D. Scale 53.000000 52.971313 -0.0286867 1.26236e-006 1 Det. Offset X 1028.284000 1027.945128 -0.338872 4.1339e-005 1 Det. Offset Y 1027.509000 1024.612809 -2.89619 4.28028e-005 1 Det. Rot. X 0.746000 0.751047 0.0050472 9.08593e-007 1 Det. Rot. Y -0.076000 0.039248 0.115248 1.80567e-006 1 Det. Rot. Z 0.000000 0.000000 0 0 0 Det. Pixel D 1.000000 1.000000 0 0 0 Det. Pixel X 1.000000 1.000000 0 0 0 Det. Pixel Y 1.000000 1.000000 0 0 0 Det. Alpha 90.000000 90.000000 0 0 0 Det. Beta 90.000000 90.000000 0 0 0 Det. Gamma 90.000000 90.000000 0 0 0 Beam. Rot. Y -0.009840 0.040312 0.0501521 9.50791e-007 1 Beam. Rot. Z 0.000000 0.000000 0 0 0 Cryst. Rot. X -23.644322 -23.654905 -0.0105823 7.92965e-007 1 Cryst. Rot. Y -8.281889 -8.246619 0.0352702 9.04271e-007 1 Cryst. Rot. Z 95.153486 95.127811 -0.0256744 1.08174e-006 1 Rec. latt. a* 0.119347 0.119452 0.000105141 1.92922e-009 1 Rec. latt. b* 0.119354 0.119355 1.32957e-006 1.75979e-009 1 Rec. latt. c* 0.119714 0.119644 -7.00428e-005 1.97972e-009 1 Rec. latt. al* 89.922008 89.900219 -0.0217892 1.05866e-006 1 Rec. latt. be* 90.043936 90.018663 -0.0252733 1.12558e-006 1 Rec. latt. ga* 89.994373 89.981997 -0.0123758 1.049e-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: -0.007493 0.076803 -0.034769 ( 0.000011 0.000012 0.000010 ) -0.083526 -0.011797 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033643 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007180 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007170 0.000015 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000015 0.007204 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007493 0.076803 -0.034769 ( 0.000011 0.000012 0.000010 ) -0.083526 -0.011797 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033643 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 2748 obs out of 2990 (total:2990,skipped:0) (91.91%) unit cell: 8.3706(8) 8.3769(11) 8.3571(10) 90.123(10) 89.987(9) 90.009(9) V = 585.99(12) unit cell: 8.3682(3) 8.3682(3) 8.3682(3) 90.0 90.0 90.0 V = 585.99(3) No constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011795 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007180 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007170 0.000016 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000016 0.007204 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011795 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 2748 obs out of 2990 (total:2990,skipped:0) (91.91%) unit cell: 8.3705(8) 8.3768(11) 8.3571(10) 90.125(10) 89.987(9) 90.007(9) V = 585.98(12) unit cell: 8.3681(3) 8.3681(3) 8.3681(3) 90.0 90.0 90.0 V = 585.98(3) No constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011794 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007181 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007170 0.000016 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000016 0.007204 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011794 -0.008061 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 2747 obs out of 2990 (total:2990,skipped:0) (91.87%) unit cell: 8.3705(8) 8.3768(11) 8.3571(10) 90.125(10) 89.987(9) 90.006(9) V = 585.98(12) unit cell: 8.3681(3) 8.3681(3) 8.3681(3) 90.0 90.0 90.0 V = 585.98(3) ******************************************************************************************************* Auto analyse stage: BRAVAIS LATTICE FINDING (Wed Mar 28 14:13:53 2018) ******************************************************************************************************* Bravais lattice type: F Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" 6268 peak locations are merged to 2991 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 2991 unindexed peaks to the CrysAlis peak table (2991 with profile info) No constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011793 -0.008060 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007181 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007170 0.000016 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000016 0.007204 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011793 -0.008060 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 2747 obs out of 2991 (total:2991,skipped:0) (91.84%) unit cell: 8.3705(8) 8.3768(11) 8.3571(10) 90.125(10) 89.986(9) 90.006(9) V = 585.98(12) unit cell: 8.3681(3) 8.3681(3) 8.3681(3) 90.0 90.0 90.0 V = 585.98(3) -------------------EXPERIMENT TAB SUMMARY------------------- CELL Niggli 1 cubic F 91.993 %(2746/2990) 8.3790(8) 8.3784(12) 8.3532(10) 90.079(10) 89.957(9) 90.007(10) V = 586.41(12) ------------------------------------------------------------ AUTO INFO: Finished at Wed Mar 28 14:13:53 2018 DC PROFFIT INFO: Meta algorithm started DELETE INFO: Deleting rpi files... (D:\Data\xs1715a\tmp\xs1715a_proffitpea*.rpi) DELETE INFO: Deleting tab files... (D:\Data\xs1715a\tmp\xs1715a_proffitpea*.tab) DELETE INFO: Deleting tabbin files... (D:\Data\xs1715a\tmp\xs1715a_proffitpea*.tabbin) DELETE INFO: Deleting rrpprof files... (D:\Data\xs1715a\tmp\xs1715a*.rrpprof) DELETE INFO: Deleting rrpprofinfo files... (D:\Data\xs1715a\tmp\xs1715a*.rrpprofinfo) DELETE INFO: Deleting bbm files... (D:\Data\xs1715a\tmp\xs1715a*.bbm) DELETE INFO: Deleting pcorr files... (D:\Data\xs1715a\tmp\xs1715a*.pcorr) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\tmp\xs1715a*.dat) DELETE INFO: Deleting ppc2 files... (D:\Data\xs1715a\tmp\xs1715a*.ppc2) DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:13:55 2018) ID: 2932; threads 39; handles 878; mem 518472.00 (1237728.00)kB; time: 1w 5d 23h 19m 25s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.3,peak PF: 708.5, WS: 270.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.1,peak PF: 708.5, WS: 272.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:13:55 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011793 -0.008060 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) 8.37051 ( 0.00084 ) 8.37682 ( 0.00111 ) 8.35710 ( 0.00096 ) 90.12473 ( 0.01000 ) 89.98579 ( 0.00876 ) 90.00567 ( 0.00942 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:13:55 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000011 0.000012 0.000010 ) -0.083527 -0.011793 -0.008060 ( 0.000008 0.000009 0.000008 ) -0.012149 0.033645 0.077005 ( 0.000010 0.000010 0.000009 ) M - matrix: 0.007181 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007170 0.000016 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000016 0.007204 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3705(8) 8.3768(11) 8.3571(10) 90.125(10) 89.986(9) 90.006(9) V = 585.98(12) unit cell: 8.3681(3) 8.3681(3) 8.3681(3) 90.0 90.0 90.0 V = 585.98(3) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=21, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=21, start=1, end=21, Data range for background initialization of run 6 more narrow than requested (is:21,should:25) BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb PROFFITPEAK info: 219 peaks in the peak location table UB fit with 106 obs out of 115 (total:115,skipped:0) (92.17%) UB - matrix: -0.007416 0.077085 -0.035165 ( 0.000132 0.000224 0.000137 ) -0.083598 -0.011595 -0.008105 ( 0.000068 0.000115 0.000070 ) -0.012124 0.033792 0.076772 ( 0.000066 0.000111 0.000068 ) M - matrix: 0.007191 -0.000012 0.000008 ( 0.000012 0.000014 0.000009 ) -0.000012 0.007218 -0.000022 ( 0.000014 0.000036 0.000016 ) 0.000008 -0.000022 0.007196 ( 0.000009 0.000016 0.000014 ) unit cell: 8.365(7) 8.349(18) 8.361(10) 89.82(13) 90.06(8) 89.90(11) V = 584(2) UB fit with 106 obs out of 115 (total:115,skipped:0) (92.17%) UB - matrix: -0.007416 0.077085 -0.035165 ( 0.000132 0.000224 0.000137 ) -0.083598 -0.011595 -0.008105 ( 0.000068 0.000115 0.000070 ) -0.012124 0.033792 0.076772 ( 0.000066 0.000111 0.000068 ) M - matrix: 0.007191 -0.000012 0.000008 ( 0.000012 0.000014 0.000009 ) -0.000012 0.007218 -0.000022 ( 0.000014 0.000036 0.000016 ) 0.000008 -0.000022 0.007196 ( 0.000009 0.000016 0.000014 ) unit cell: 8.365(7) 8.349(18) 8.361(10) 89.82(13) 90.06(8) 89.90(11) V = 584(2) OTKP changes: 21 1 1 1 No constraint UB - matrix: -0.007240 0.076835 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007147 -0.000018 0.000014 ( 0.000013 0.000015 0.000009 ) -0.000018 0.007156 -0.000028 ( 0.000015 0.000034 0.000015 ) 0.000014 -0.000028 0.007153 ( 0.000009 0.000015 0.000013 ) Constraint UB - matrix: -0.007240 0.076835 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007134 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007134 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007134 ( 0.000000 0.000000 0.000002 ) UB fit with 105 obs out of 115 (total:115,skipped:0) (91.30%) unit cell: 8.390(8) 8.385(18) 8.387(9) 89.78(13) 90.11(8) 89.86(11) V = 590(2) unit cell: 8.3871(13) 8.3871(13) 8.3871(13) 90.0 90.0 90.0 V = 589.98(16) UB fit with 105 obs out of 115 (total:115,skipped:0) (91.30%) UB - matrix: -0.007240 0.076836 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007147 -0.000018 0.000014 ( 0.000013 0.000015 0.000009 ) -0.000018 0.007156 -0.000028 ( 0.000015 0.000034 0.000015 ) 0.000014 -0.000028 0.007153 ( 0.000009 0.000015 0.000013 ) unit cell: 8.390(8) 8.385(18) 8.387(9) 89.78(13) 90.11(8) 89.86(11) V = 590(2) OTKP changes: 21 1 1 1 No constraint UB - matrix: -0.007240 0.076835 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007147 -0.000018 0.000014 ( 0.000013 0.000015 0.000009 ) -0.000018 0.007156 -0.000028 ( 0.000015 0.000034 0.000015 ) 0.000014 -0.000028 0.007153 ( 0.000009 0.000015 0.000013 ) Constraint UB - matrix: -0.007240 0.076835 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007134 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007134 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007134 ( 0.000000 0.000000 0.000002 ) UB fit with 105 obs out of 115 (total:115,skipped:0) (91.30%) unit cell: 8.390(8) 8.385(18) 8.387(9) 89.78(13) 90.11(8) 89.86(11) V = 590(2) unit cell: 8.3871(13) 8.3871(13) 8.3871(13) 90.0 90.0 90.0 V = 589.98(16) 115 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Run 6 Omega scan: (3.000 - 24.000,21 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=53.244) HKL list info: 238 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007240 0.076836 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007147 -0.000018 0.000014 ( 0.000013 0.000015 0.000009 ) -0.000018 0.007156 -0.000028 ( 0.000015 0.000034 0.000015 ) 0.000014 -0.000028 0.007153 ( 0.000009 0.000015 0.000013 ) Constraint UB - matrix: -0.007240 0.076836 -0.034989 ( 0.000125 0.000213 0.000129 ) -0.083373 -0.011280 -0.008139 ( 0.000077 0.000131 0.000079 ) -0.011989 0.033548 0.076567 ( 0.000060 0.000102 0.000062 ) M - matrix: 0.007134 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007134 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007134 ( 0.000000 0.000000 0.000002 ) UB fit with 105 obs out of 115 (total:115,skipped:0) (91.30%) unit cell: 8.390(8) 8.385(18) 8.387(9) 89.78(13) 90.11(8) 89.86(11) V = 590(2) unit cell: 8.3871(13) 8.3871(13) 8.3871(13) 90.0 90.0 90.0 V = 589.98(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 106 obs out of 115 (total:115,skipped:0) (92.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=21, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=21, start=1, end=21, Data range for background initialization of run 6 more narrow than requested (is:21,should:25) BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb 0 of 77 peaks identified as outliers and rejected 77 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 77 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 77 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 1.41 | 8 | 0.983 ( 0.135) | 0.995 ( 0.157) | 0.926 ( 0.272) | 1.41- 1.15 | 8 | 1.052 ( 0.061) | 1.096 ( 0.094) | 0.987 ( 0.192) | 1.12- 0.99 | 8 | 1.098 ( 0.052) | 1.073 ( 0.162) | 1.165 ( 0.485) | 0.98- 0.92 | 8 | 1.110 ( 0.035) | 1.067 ( 0.097) | 1.478 ( 0.549) | 0.92- 0.82 | 8 | 1.147 ( 0.041) | 1.148 ( 0.112) | 1.031 ( 0.248) | 0.82- 0.78 | 8 | 1.188 ( 0.083) | 1.178 ( 0.190) | 1.099 ( 0.446) | 0.75- 0.70 | 8 | 1.147 ( 0.025) | 1.251 ( 0.142) | 1.065 ( 0.279) | 0.70- 0.67 | 8 | 1.159 ( 0.046) | 1.120 ( 0.101) | 1.270 ( 0.526) | 0.67- 0.63 | 8 | 1.157 ( 0.065) | 1.208 ( 0.161) | 1.238 ( 0.515) | 0.62- 0.60 | 5 | 1.124 ( 0.050) | 1.265 ( 0.239) | 1.121 ( 0.330) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 0.60 | 77 | 1.116 ( 0.089) | 1.135 ( 0.168) | 1.139 ( 0.435) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 77 obs out of 77 (total:77,skipped:0) (100.00%) UB - matrix: -0.007319 0.076823 -0.034778 ( 0.000062 0.000101 0.000060 ) -0.083338 -0.011834 -0.007992 ( 0.000048 0.000079 0.000047 ) -0.011926 0.033493 0.076646 ( 0.000030 0.000049 0.000029 ) M - matrix: 0.007141 0.000025 0.000007 ( 0.000008 0.000008 0.000005 ) 0.000025 0.007164 -0.000010 ( 0.000008 0.000016 0.000007 ) 0.000007 -0.000010 0.007148 ( 0.000005 0.000007 0.000006 ) unit cell: 8.394(5) 8.381(8) 8.390(4) 89.92(6) 90.05(5) 90.20(6) V = 590.1(8) OTKP changes: 77 1 1 1 No constraint UB - matrix: -0.007317 0.077000 -0.035161 ( 0.000059 0.000097 0.000058 ) -0.083657 -0.011620 -0.008076 ( 0.000036 0.000059 0.000035 ) -0.012095 0.033875 0.076781 ( 0.000017 0.000029 0.000017 ) M - matrix: 0.007198 -0.000001 0.000004 ( 0.000006 0.000007 0.000004 ) -0.000001 0.007211 -0.000013 ( 0.000007 0.000015 0.000006 ) 0.000004 -0.000013 0.007197 ( 0.000004 0.000006 0.000005 ) Constraint UB - matrix: -0.007317 0.077000 -0.035161 ( 0.000059 0.000097 0.000058 ) -0.083657 -0.011620 -0.008076 ( 0.000036 0.000059 0.000035 ) -0.012095 0.033875 0.076781 ( 0.000017 0.000029 0.000017 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 77 obs out of 77 (total:77,skipped:0) (100.00%) unit cell: 8.360(4) 8.353(8) 8.361(3) 89.90(5) 90.03(3) 89.99(5) V = 583.8(7) unit cell: 8.3579(6) 8.3579(6) 8.3579(6) 90.0 90.0 90.0 V = 583.84(7) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (3.000 - 24.000,21 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) HKL list info: 237 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 77 obs out of 77 (total:77,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= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=21, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=21, start=1, end=21, Data range for background initialization of run 6 more narrow than requested (is:21,should:25) BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb 0 of 74 peaks identified as outliers and rejected 74 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 74 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 74 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.40- 1.41 | 7 | 0.987 ( 0.145) | 0.999 ( 0.170) | 0.943 ( 0.290) | 1.41- 1.17 | 7 | 1.069 ( 0.060) | 1.094 ( 0.099) | 0.985 ( 0.203) | 1.15- 1.09 | 7 | 1.096 ( 0.078) | 1.205 ( 0.223) | 1.421 ( 0.965) | 0.98- 0.93 | 7 | 1.105 ( 0.040) | 1.051 ( 0.136) | 1.420 ( 0.369) | 0.93- 0.87 | 7 | 1.151 ( 0.046) | 1.124 ( 0.088) | 1.219 ( 0.535) | 0.87- 0.81 | 7 | 1.157 ( 0.021) | 1.150 ( 0.132) | 1.158 ( 0.479) | 0.81- 0.72 | 7 | 1.189 ( 0.091) | 1.227 ( 0.201) | 1.272 ( 0.317) | 0.72- 0.69 | 7 | 1.172 ( 0.042) | 1.188 ( 0.175) | 1.093 ( 0.461) | 0.69- 0.67 | 7 | 1.143 ( 0.068) | 1.169 ( 0.110) | 1.136 ( 0.395) | 0.64- 0.60 | 11 | 1.147 ( 0.064) | 1.243 ( 0.206) | 1.177 ( 0.440) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.40- 0.60 | 74 | 1.123 ( 0.092) | 1.150 ( 0.180) | 1.182 ( 0.507) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 231 | 1.149 ( 0.124) | 1.246 ( 0.390) | 1.330 ( 0.664) | 13.1-18.9 | 231 | 1.134 ( 0.071) | 1.191 ( 0.272) | 1.271 ( 0.564) | 18.9-23.0 | 231 | 1.148 ( 0.091) | 1.201 ( 0.287) | 1.257 ( 0.685) | 23.0-27.2 | 231 | 1.131 ( 0.094) | 1.169 ( 0.295) | 1.224 ( 0.568) | 27.2-30.4 | 231 | 1.140 ( 0.099) | 1.166 ( 0.258) | 1.200 ( 0.457) | 30.4-33.6 | 231 | 1.150 ( 0.104) | 1.144 ( 0.229) | 1.206 ( 0.444) | 33.6-37.0 | 231 | 1.144 ( 0.093) | 1.124 ( 0.164) | 1.158 ( 0.430) | 37.0-39.7 | 231 | 1.149 ( 0.119) | 1.105 ( 0.214) | 1.232 ( 0.503) | 39.7-42.7 | 231 | 1.166 ( 0.111) | 1.097 ( 0.186) | 1.228 ( 0.545) | 42.8-49.8 | 235 | 1.206 ( 0.159) | 1.136 ( 0.278) | 1.180 ( 0.474) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2314 | 1.152 ( 0.111) | 1.158 ( 0.268) | 1.229 ( 0.542) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0024 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:14:21 2018 PROFFITMAIN - Started at Wed Mar 28 14:14:21 2018 OTKP changes: 2304 2 4 6 OTKP changes: 2304 2 4 6 No constraint UB - matrix: -0.007497 0.076886 -0.034778 ( 0.000007 0.000007 0.000006 ) -0.083623 -0.011798 -0.008052 ( 0.000005 0.000005 0.000004 ) -0.012181 0.033653 0.077067 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007197 0.000000 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007183 0.000015 ( 0.000001 0.000001 0.000001 ) -0.000005 0.000015 0.007214 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007497 0.076886 -0.034778 ( 0.000007 0.000007 0.000006 ) -0.083623 -0.011798 -0.008052 ( 0.000005 0.000005 0.000004 ) -0.012181 0.033653 0.077067 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000000 ) UB fit with 2307 obs out of 2314 (total:2314,skipped:0) (99.70%) unit cell: 8.3607(5) 8.3690(6) 8.3513(6) 90.116(6) 89.963(5) 90.002(5) V = 584.34(7) unit cell: 8.36032(15) 8.36032(15) 8.36032(15) 90.0 90.0 90.0 V = 584.343(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007600 0.076999 -0.034679 ( 0.000017 0.000015 0.000011 ) -0.083472 -0.011808 -0.008117 ( 0.000011 0.000010 0.000008 ) -0.012072 0.033515 0.076937 ( 0.000013 0.000012 0.000009 ) M - matrix: 0.007171 -0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007192 0.000004 ( 0.000002 0.000002 0.000001 ) 0.000012 0.000004 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3761(11) 8.3641(13) 8.3663(10) 90.033(11) 90.099(11) 89.967(13) V = 586.13(14) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 No constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3684(11) 8.3671(13) 8.3649(10) 90.042(11) 90.009(10) 89.970(12) V = 585.71(13) unit cell: 8.3668(4) 8.3668(4) 8.3668(4) 90.0 90.0 90.0 V = 585.71(4) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.954) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3684(11) 8.3671(13) 8.3649(10) 90.042(11) 90.009(10) 89.970(12) V = 585.71(13) unit cell: 8.3668(4) 8.3668(4) 8.3668(4) 90.0 90.0 90.0 V = 585.71(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007593 0.076975 -0.034655 ( 0.000016 0.000014 0.000011 ) -0.083544 -0.011809 -0.008032 ( 0.000011 0.000010 0.000007 ) -0.012121 0.033493 0.076972 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3684(11) 8.3671(13) 8.3649(10) 90.042(11) 90.009(10) 89.970(12) V = 585.71(13) unit cell: 8.3668(4) 8.3668(4) 8.3668(4) 90.0 90.0 90.0 V = 585.71(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007132 0.076861 -0.034847 ( 0.000018 0.000012 0.000019 ) -0.083555 -0.011649 -0.008026 ( 0.000014 0.000010 0.000015 ) -0.012433 0.033789 0.076710 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000005 -0.000035 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007185 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000035 0.000007 0.007163 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3669(13) 8.3679(14) 8.3808(15) 90.057(14) 89.724(14) 90.041(14) V = 586.76(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007251 0.076723 -0.035023 ( 0.000015 0.000010 0.000016 ) -0.083592 -0.011724 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012376 0.033949 0.076895 ( 0.000015 0.000011 0.000017 ) M - matrix: 0.007193 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007176 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007205 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007251 0.076723 -0.035023 ( 0.000015 0.000010 0.000016 ) -0.083592 -0.011724 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012376 0.033949 0.076895 ( 0.000015 0.000011 0.000017 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3631(13) 8.3730(12) 8.3566(15) 90.145(13) 89.820(13) 90.029(12) V = 585.16(16) unit cell: 8.3642(3) 8.3642(3) 8.3642(3) 90.0 90.0 90.0 V = 585.16(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.954) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007251 0.076723 -0.035023 ( 0.000015 0.000010 0.000016 ) -0.083592 -0.011724 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012376 0.033949 0.076895 ( 0.000015 0.000011 0.000017 ) M - matrix: 0.007193 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007176 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007205 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007251 0.076723 -0.035023 ( 0.000015 0.000010 0.000016 ) -0.083592 -0.011724 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012376 0.033949 0.076895 ( 0.000015 0.000011 0.000017 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3631(13) 8.3730(12) 8.3566(15) 90.145(13) 89.820(13) 90.029(12) V = 585.16(16) unit cell: 8.3642(3) 8.3642(3) 8.3642(3) 90.0 90.0 90.0 V = 585.16(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084688 0.000100 -0.000194 ( 0.000016 0.000011 0.000018 ) 0.000019 0.084770 0.000100 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084840 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007172 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007186 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007198 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084688 0.000100 -0.000194 ( 0.000016 0.000011 0.000018 ) 0.000019 0.084770 0.000100 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084840 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3755(16) 8.3673(8) 8.3604(10) 90.066(10) 89.870(13) 90.080(11) V = 585.90(14) unit cell: 8.3677(3) 8.3677(3) 8.3677(3) 90.0 90.0 90.0 V = 585.90(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007566 0.077024 -0.034598 ( 0.000015 0.000014 0.000012 ) -0.083436 -0.011869 -0.008156 ( 0.000012 0.000011 0.000010 ) -0.012263 0.033264 0.076991 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007169 -0.000000 -0.000002 ( 0.000002 0.000002 0.000001 ) -0.000000 0.007180 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000007 0.007191 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3708(13) 8.3643(11) 89.944(12) 89.985(11) 89.996(12) V = 586.53(15) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000006 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000006 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3649(11) 8.3683(12) 8.3660(10) 90.006(10) 90.052(10) 90.097(11) V = 585.62(13) unit cell: 8.3664(4) 8.3664(4) 8.3664(4) 90.0 90.0 90.0 V = 585.62(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.954) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000006 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000006 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3649(11) 8.3683(12) 8.3660(10) 90.006(10) 90.052(10) 90.097(11) V = 585.62(13) unit cell: 8.3664(4) 8.3664(4) 8.3664(4) 90.0 90.0 90.0 V = 585.62(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000006 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000006 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077014 -0.034557 ( 0.000013 0.000012 0.000011 ) -0.083576 -0.011980 -0.008139 ( 0.000011 0.000010 0.000009 ) -0.012155 0.033310 0.076993 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3649(11) 8.3683(12) 8.3660(10) 90.006(10) 90.052(10) 90.097(11) V = 585.62(13) unit cell: 8.3664(4) 8.3664(4) 8.3664(4) 90.0 90.0 90.0 V = 585.62(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 74 obs out of 74 (total:74,skipped:0) (100.00%) UB - matrix: -0.007376 0.077057 -0.035147 ( 0.000061 0.000099 0.000058 ) -0.083668 -0.011725 -0.008072 ( 0.000042 0.000069 0.000041 ) -0.012084 0.033814 0.076793 ( 0.000020 0.000032 0.000019 ) M - matrix: 0.007201 0.000004 0.000007 ( 0.000007 0.000008 0.000004 ) 0.000004 0.007219 -0.000017 ( 0.000008 0.000016 0.000006 ) 0.000007 -0.000017 0.007198 ( 0.000004 0.000006 0.000005 ) unit cell: 8.359(4) 8.348(8) 8.361(4) 89.86(5) 90.05(4) 90.03(6) V = 583.4(7) OTKP changes: 74 1 1 1 No constraint UB - matrix: -0.007337 0.077019 -0.035171 ( 0.000061 0.000099 0.000058 ) -0.083670 -0.011624 -0.008082 ( 0.000041 0.000066 0.000039 ) -0.012085 0.033892 0.076788 ( 0.000019 0.000032 0.000019 ) M - matrix: 0.007201 -0.000002 0.000006 ( 0.000007 0.000007 0.000004 ) -0.000002 0.007216 -0.000012 ( 0.000007 0.000015 0.000006 ) 0.000006 -0.000012 0.007199 ( 0.000004 0.000006 0.000005 ) Constraint UB - matrix: -0.007337 0.077019 -0.035171 ( 0.000061 0.000099 0.000058 ) -0.083670 -0.011624 -0.008082 ( 0.000041 0.000066 0.000039 ) -0.012085 0.033892 0.076788 ( 0.000019 0.000032 0.000019 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 74 obs out of 74 (total:74,skipped:0) (100.00%) unit cell: 8.359(4) 8.350(8) 8.360(4) 89.90(5) 90.05(4) 89.98(6) V = 583.5(7) unit cell: 8.3563(7) 8.3563(7) 8.3563(7) 90.0 90.0 90.0 V = 583.50(8) Run 6 Omega scan: (3.000 - 24.000,21 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) HKL list info: 232 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.007337 0.077019 -0.035171 ( 0.000061 0.000099 0.000058 ) -0.083670 -0.011624 -0.008082 ( 0.000041 0.000066 0.000039 ) -0.012085 0.033892 0.076788 ( 0.000019 0.000032 0.000019 ) M - matrix: 0.007201 -0.000002 0.000006 ( 0.000007 0.000007 0.000004 ) -0.000002 0.007216 -0.000012 ( 0.000007 0.000015 0.000006 ) 0.000006 -0.000012 0.007199 ( 0.000004 0.000006 0.000005 ) Constraint UB - matrix: -0.007337 0.077019 -0.035171 ( 0.000061 0.000099 0.000058 ) -0.083670 -0.011624 -0.008082 ( 0.000041 0.000066 0.000039 ) -0.012085 0.033892 0.076788 ( 0.000019 0.000032 0.000019 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 74 obs out of 74 (total:74,skipped:0) (100.00%) unit cell: 8.359(4) 8.350(8) 8.360(4) 89.90(5) 90.05(4) 89.98(6) V = 583.5(7) unit cell: 8.3563(7) 8.3563(7) 8.3563(7) 90.0 90.0 90.0 V = 583.50(8) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=21, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=21, start=1, end=21, Data range for background initialization of run 6 more narrow than requested (is:21,should:25) BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007477 0.076830 -0.034767 ( 0.000007 0.000007 0.000006 ) -0.083578 -0.011784 -0.008055 ( 0.000005 0.000005 0.000004 ) -0.012173 0.033635 0.077004 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007477 0.076830 -0.034767 ( 0.000007 0.000007 0.000006 ) -0.083578 -0.011784 -0.008055 ( 0.000005 0.000005 0.000004 ) -0.012173 0.033635 0.077004 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 2309 obs out of 2314 (total:2314,skipped:0) (99.78%) unit cell: 8.3654(4) 8.3750(6) 8.3573(6) 90.110(6) 89.967(5) 90.008(5) V = 585.51(7) unit cell: 8.36587(15) 8.36587(15) 8.36587(15) 90.0 90.0 90.0 V = 585.508(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 75 reflections under beam stop or inside a detector rejection region 30 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3099 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:14:29 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.954) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.954) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.954) Run 6 Omega scan: (3.000 - 24.000,21 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) PROFFIT INFO: signal sum: min=149.0000 max=22696260.0000 PROFFIT INFO: signal sum lp corr: min=222.3418 max=3261504.4647 PROFFIT INFO: background sum: min=741.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10979.0000 PROFFIT INFO: num of signal pixels: min=59 max=878 PROFFIT INFO: Inet: min=485.1093 max=7116010.0000 PROFFIT INFO: sig(Inet): min=187.9730 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=309.47 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 3 72 238 405 644 707 1262 2062 2816 3099 Percent 0.0 0.1 2.3 7.7 13.1 20.8 22.8 40.7 66.5 90.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3099 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 3099 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7116010- 1583016 309 2403736.51 134.26 100.00 1578462- 1037619 309 1286470.17 110.10 100.00 1036030- 311369 309 600711.70 94.27 100.00 310793- 216655 309 253444.69 68.78 100.00 216269- 163907 309 187506.31 48.63 100.00 163755- 130691 309 146765.57 37.53 100.00 130364- 101063 309 115049.36 30.18 100.00 100909- 6122 309 57159.40 20.98 100.00 6113- 3546 309 4595.11 4.93 83.82 3546- 485 318 2645.94 3.16 40.88 ------------------------------------------------------------------------------------ 7116010- 485 3099 504347.21 55.13 92.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 862131.87 88.16 100.00 1.41- 1.12 309 781562.23 70.55 98.38 1.12- 0.96 309 649115.37 74.48 99.03 0.96- 0.88 309 488901.32 60.67 95.47 0.88- 0.81 309 640002.85 69.40 97.41 0.81- 0.74 309 338988.59 40.65 93.53 0.74- 0.71 309 281114.35 37.46 90.61 0.71- 0.65 309 517002.75 51.61 95.15 0.65- 0.62 309 249793.43 29.28 73.46 0.62- 0.58 318 242486.38 29.79 80.50 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 504347.21 55.13 92.32 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:14:29 2018 Sorting 3099 observations 118 unique observations with > 7.00 F2/sig(F2) 3099 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 20 543 Total number of frames 543 Maximum number of 118 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3099 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 4 111 Total number of frames 111 2489 observations > 7.00 F2/sig(F2) 2489 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 4 111 Total number of frames 111 Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 2489 removed 8 = 2481, unique = 124) 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 2481 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 4 111 Total number of frames 111 124 unique data precomputed (should be 124) 124 unique data with 2481 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 2481 removed 0 = 2481, unique = 124) 124 unique data precomputed (should be 124) 124 unique data with 2481 observations RMS deviation of equivalent data = 0.20613 Rint = 0.17043 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16958, wR= 0.21814 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08184, wR= 0.10677, Acormin=0.655, Acormax=1.408, Acor_av=0.957 F test: Probability=1.000, F= 4.284 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08093, wR= 0.10126, Acormin=0.617, Acormax=1.392, Acor_av=0.912 F test: Probability=0.697, F= 1.021 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06841, wR= 0.09335, Acormin=0.673, Acormax=1.456, Acor_av=0.960 F test: Probability=1.000, F= 1.426 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06336, wR= 0.08373, Acormin=0.593, Acormax=1.479, Acor_av=0.910 F test: Probability=1.000, F= 1.164 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06085, wR= 0.08073, Acormin=0.553, Acormax=1.399, Acor_av=0.873 F test: Probability=0.970, F= 1.081 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06383, wR= 0.08569, Acormin=0.680, Acormax=1.547, Acor_av=0.928 F test: Probability=0.000, F= 0.907 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05942, wR= 0.07830, Acormin=0.605, Acormax=1.519, Acor_av=0.893 F test: Probability=0.860, F= 1.046 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05632, wR= 0.07483, Acormin=0.564, Acormax=1.444, Acor_av=0.856 F test: Probability=1.000, F= 1.161 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05102, wR= 0.06919, Acormin=0.533, Acormax=1.389, Acor_av=0.819 F test: Probability=1.000, F= 1.213 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06009, wR= 0.07771, Acormin=0.510, Acormax=1.405, Acor_av=0.825 F test: Probability=0.000, F= 0.722 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05700, wR= 0.07432, Acormin=0.553, Acormax=1.436, Acor_av=0.839 F test: Probability=0.000, F= 0.802 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05368, wR= 0.06988, Acormin=0.273, Acormax=0.713, Acor_av=0.424 F test: Probability=0.000, F= 0.901 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04842, wR= 0.06409, Acormin=0.289, Acormax=0.779, Acor_av=0.461 F test: Probability=0.990, F= 1.102 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04560, wR= 0.06134, Acormin=0.289, Acormax=0.821, Acor_av=0.482 F test: Probability=1.000, F= 1.234 Final absorption model (ne=6, no=5): Rint= 0.05102, Acormin=0.533, Acormax=1.389, Acor_av=0.819 Combined refinement in use Rint: 0.17055 There are 111 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20613 Using Levenberg-Marquardt: 0.00010 New wR= 0.05173 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17043 with corrections 0.04039 Rint for all data: 0.17055 with corrections 0.04060 0 observations identified as outliers and rejected Cycle 2 wR= 0.05173 Using Levenberg-Marquardt: 0.00001 New wR= 0.04760 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17043 with corrections 0.03549 Rint for all data: 0.17055 with corrections 0.03570 0 observations identified as outliers and rejected Cycle 3 wR= 0.04760 Using Levenberg-Marquardt: 0.00000 New wR= 0.04703 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17043 with corrections 0.03518 Rint for all data: 0.17055 with corrections 0.03539 0 observations identified as outliers and rejected Cycle 4 wR= 0.04703 Using Levenberg-Marquardt: 0.00000 New wR= 0.04670 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17043 with corrections 0.03503 Rint for all data: 0.17055 with corrections 0.03524 0 observations identified as outliers and rejected Cycle 5 wR= 0.04670 Using Levenberg-Marquardt: 0.00000 New wR= 0.04649 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17043 with corrections 0.03491 Rint for all data: 0.17055 with corrections 0.03512 0 observations identified as outliers and rejected Final wR= 0.04649 Final frame scales: Min= 0.7712 Max= 1.1472 Final absorption correction factors: Amin= 0.5885 Amax= 1.5331 PROFFIT INFO: Inet (after scale3 abspack): min=478.1044 max=5590631.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=165.0574 max=66821.3281 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3099 reflections read from tmp file 420 reflections are rejected (418 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 7 1 2 1 3 5 8 10 116 Initial Chi^2= 0.32937 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.43351 Current error model SIG(F2)^2 = 107.80*I_RAW + 0.00*I_BACK+(0.00794*)^2 Cycle 2, Chi^2= 1.06345 Current error model SIG(F2)^2 = 72.18*I_RAW + 0.00*I_BACK+(0.02142*)^2 Cycle 3, Chi^2= 1.00174 Current error model SIG(F2)^2 = 89.50*I_RAW + 0.00*I_BACK+(0.01868*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 88.05*I_RAW + 0.00*I_BACK+(0.01907*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 88.25*I_RAW + 0.00*I_BACK+(0.01902*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 88.25*I_RAW + 0.00*I_BACK+(0.01902*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5590631- 1585569 309 2345103.03 48.98 100.00 1578092- 993629 309 1230744.66 42.74 100.00 992317- 325078 309 599638.21 41.05 100.00 322861- 203000 309 246893.31 34.60 100.00 202880- 168798 309 184499.29 28.28 100.00 168644- 125783 309 141874.11 22.68 100.00 125746- 100111 309 113310.51 19.71 100.00 100111- 5760 309 58578.41 14.83 100.00 5746- 3451 309 4340.01 4.98 100.00 3450- 478 318 2655.25 3.89 79.87 ------------------------------------------------------------------------------------ 5590631- 478 3099 491340.32 26.11 97.93 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 903096.24 39.51 100.00 1.41- 1.12 309 795269.97 31.60 100.00 1.12- 0.96 309 611033.37 30.45 99.68 0.96- 0.88 309 475566.23 26.65 98.71 0.88- 0.81 309 609241.25 30.65 98.71 0.81- 0.74 309 316015.40 20.91 98.71 0.74- 0.71 309 269416.73 20.89 98.06 0.71- 0.65 309 482903.53 25.91 99.35 0.65- 0.62 309 232481.72 17.00 90.94 0.62- 0.58 318 226104.13 17.77 95.28 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 491340.32 26.11 97.93 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 903096.24 39.51 100.00 4.82- 1.12 618 849183.10 35.56 100.00 4.82- 0.96 927 769799.86 33.85 99.89 4.82- 0.88 1236 696241.45 32.05 99.60 4.82- 0.81 1545 678841.41 31.77 99.42 4.82- 0.74 1854 618370.41 29.96 99.30 4.82- 0.71 2163 568519.88 28.67 99.12 4.82- 0.65 2472 557817.84 28.32 99.15 4.82- 0.62 2781 521669.38 27.06 98.24 4.82- 0.58 3099 491340.32 26.11 97.93 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 491340.32 26.11 97.93 Scale applied to data: s=0.178871 (maximum obs:5590631.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.035; Rsigma 0.025: data 3099 -> merged 156 With outlier rejection... Rint 0.033; Rsigma 0.025: data 3080 -> merged 156 Rejected total: 19, method kkm 18, method Blessing 1 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585728, 4.830035 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 17.71 100.00 248 1.41 - 1.12 14 14 25.36 100.00 355 1.12 - 0.97 14 14 25.36 100.00 355 0.96 - 0.84 14 14 27.71 100.00 388 0.84 - 0.78 14 14 20.14 100.00 282 0.78 - 0.73 14 14 21.93 100.00 307 0.73 - 0.69 14 14 20.79 100.00 291 0.69 - 0.66 14 14 17.79 100.00 249 0.65 - 0.63 14 14 18.43 100.00 258 0.63 - 0.60 14 14 17.36 100.00 243 --------------------------------------------------------------- 8.36 - 0.60 140 140 21.26 100.00 2976 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:14:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.365379 8.374951 8.357296 90.1096 89.9672 90.0080 3080 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1570 0 2065 2063 3080 N (int>3sigma) = 0 0 0 0 1570 0 2021 2020 3016 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 87.2 87.5 87.3 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.1 26.2 26.0 Lattice type: F chosen Volume: 585.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.929 b.b = 34.936 c.c = 34.976 b.c = -0.034 a.c = -17.435 a.b = -17.420 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.139 CUBIC F-lattice R(int) = 0.033 [ 2924] Vol = 585.5 Cell: 8.365 8.375 8.357 90.11 89.97 90.01 Volume: 585.51 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.131 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 2647] Vol = 439.1 Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.13 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.131 RHOMBOHEDRAL R-lattice R(int) = 0.034 [ 848] Vol = 439.1 Trigonal Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.13 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.032 [ 2679] Vol = 292.8 Cell: 5.919 5.918 8.357 89.95 89.90 89.93 Volume: 292.75 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.148 TETRAGONAL I-lattice R(int) = 0.032 [ 2679] Vol = 292.8 Cell: 5.918 5.919 8.357 90.10 90.05 89.93 Volume: 292.75 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.032 [ 2626] Vol = 292.8 Cell: 5.918 5.919 8.357 89.90 89.95 89.93 Volume: 292.75 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 2625] Vol = 292.8 Cell: 5.910 8.365 5.921 89.97 89.88 90.02 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.031 [ 2283] Vol = 292.8 Cell: 5.919 5.918 8.357 90.05 90.10 89.93 Volume: 292.75 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.116 MONOCLINIC I-lattice R(int) = 0.030 [ 2283] Vol = 292.8 Cell: 5.910 5.921 8.365 90.03 90.02 90.12 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.028 [ 2301] Vol = 292.8 Cell: 5.910 8.365 5.921 89.97 90.12 89.98 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.053 MONOCLINIC I-lattice R(int) = 0.030 [ 2283] Vol = 292.8 Cell: 8.365 5.910 5.921 90.12 90.03 90.02 Volume: 292.75 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.102 MONOCLINIC C-lattice R(int) = 0.029 [ 2282] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.91 Volume: 292.75 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.026 [ 1641] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.38 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1570 0 2065 2063 3080 N (int>3sigma) = 0 0 0 0 1570 0 2021 2020 3016 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 87.2 87.5 87.3 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.1 26.2 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 29 29 242 686 N I>3s 25 25 231 686 0.7 0.7 0.7 39.3 8.6 8.6 5.6 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.033 2702 Fd-3m 1 1 227 C N N N N 37 2284 0.034 2741 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365379 8.374951 8.357296 90.1096 89.9672 90.0080 ZERR 3.00 0.000451 0.000647 0.000616 0.0061 0.0053 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5338665- 1163259 495 489 26 18.8 1958547.32 47.00 0.030 0.040 1153387- 289150 486 479 26 18.4 687658.63 40.91 0.038 0.052 285035- 136833 706 705 26 27.1 196556.77 29.30 0.035 0.047 133560- 100576 503 503 26 19.3 119306.01 20.26 0.048 0.063 99740- 3994 461 458 26 17.6 35172.84 10.64 0.057 0.070 3965- 1888 448 446 26 17.2 3182.70 4.28 0.190 0.225 ------------------------------------------------------------------------------------------- 5338665- 1888 3099 3080 156 19.7 488061.76 26.04 0.033 0.045 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 575 569 26 21.9 749742.70 34.52 0.038 0.047 0.021 1.12-0.88 692 691 26 26.6 626723.35 29.91 0.027 0.037 0.023 0.85-0.75 579 575 26 22.1 459230.79 25.18 0.027 0.035 0.026 0.74-0.68 508 506 26 19.5 405880.48 23.60 0.035 0.043 0.028 0.67-0.63 492 491 26 18.9 228742.31 18.60 0.046 0.063 0.035 0.62-0.59 253 248 26 9.5 249254.34 17.49 0.041 0.054 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 3099 3080 156 19.7 488061.76 26.04 0.033 0.045 0.025 inf-0.60 2990 2974 139 21.4 498622.76 26.37 0.033 0.044 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 569 26 26 100.0 21.9 749742.70 177.83 0.038 0.007 1.12-0.88 691 26 26 100.0 26.6 626723.35 157.54 0.027 0.005 0.85-0.75 575 26 26 100.0 22.1 459230.79 125.09 0.027 0.006 0.74-0.68 506 26 26 100.0 19.5 405880.48 108.05 0.035 0.007 0.67-0.63 491 26 26 100.0 18.9 228742.31 80.82 0.046 0.008 0.62-0.59 248 26 26 100.0 9.5 249254.34 62.98 0.041 0.013 -------------------------------------------------------------------------------------------- inf-0.59 3080 156 156 100.0 19.7 488061.76 127.26 0.033 0.007 inf-0.60 2974 139 139 100.0 21.4 498622.76 130.06 0.033 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007477 0.076830 -0.034767 ( 0.000007 0.000007 0.000006 ) -0.083578 -0.011784 -0.008055 ( 0.000005 0.000005 0.000004 ) -0.012173 0.033635 0.077004 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007477 0.076830 -0.034767 ( 0.000007 0.000007 0.000006 ) -0.083578 -0.011784 -0.008055 ( 0.000005 0.000005 0.000004 ) -0.012173 0.033635 0.077004 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3654(4) 8.3750(6) 8.3573(6) 90.110(6) 89.967(5) 90.008(5) V = 585.51(7) unit cell: 8.36587(15) 8.36587(15) 8.36587(15) 90.0 90.0 90.0 V = 585.509(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.954) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.954) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.954) Run 6 Omega scan: (3.000 - 24.000,21 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) PROFFIT INFO: signal sum: min=149.0000 max=22696260.0000 PROFFIT INFO: signal sum lp corr: min=222.3418 max=3261504.4647 PROFFIT INFO: background sum: min=741.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10979.0000 PROFFIT INFO: num of signal pixels: min=59 max=878 PROFFIT INFO: Inet: min=485.1093 max=7116010.0000 PROFFIT INFO: sig(Inet): min=187.9730 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=309.47 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 6 144 476 810 1288 1414 2524 4124 5632 6198 Percent 0.0 0.1 2.3 7.7 13.1 20.8 22.8 40.7 66.5 90.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3099 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 3099 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7116010- 1583016 309 2403736.51 134.26 100.00 1578462- 1037619 309 1286470.17 110.10 100.00 1036030- 311369 309 600711.70 94.27 100.00 310793- 216655 309 253444.69 68.78 100.00 216269- 163907 309 187506.31 48.63 100.00 163755- 130691 309 146765.57 37.53 100.00 130364- 101063 309 115049.36 30.18 100.00 100909- 6122 309 57159.40 20.98 100.00 6113- 3546 309 4595.11 4.93 83.82 3546- 485 318 2645.94 3.16 40.88 ------------------------------------------------------------------------------------ 7116010- 485 3099 504347.21 55.13 92.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 862131.87 88.16 100.00 1.41- 1.12 309 781562.23 70.55 98.38 1.12- 0.96 309 649115.37 74.48 99.03 0.96- 0.88 309 488901.32 60.67 95.47 0.88- 0.81 309 640002.85 69.40 97.41 0.81- 0.74 309 338988.59 40.65 93.53 0.74- 0.71 309 281114.35 37.46 90.61 0.71- 0.65 309 517002.75 51.61 95.15 0.65- 0.62 309 249793.43 29.28 73.46 0.62- 0.58 318 242486.38 29.79 80.50 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 504347.21 55.13 92.32 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:14:31 2018 Sorting 3099 observations 85 unique observations with > 7.00 F2/sig(F2) 3099 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 20 543 Total number of frames 543 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3099 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 2 81 Total number of frames 81 2489 observations > 7.00 F2/sig(F2) 2489 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 2 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 27.9 (Out of 2489 removed 6 = 2483, unique = 89) 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 2483 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 2 81 Total number of frames 81 89 unique data precomputed (should be 89) 89 unique data with 2483 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.9 (Out of 2483 removed 0 = 2483, unique = 89) 89 unique data precomputed (should be 89) 89 unique data with 2483 observations RMS deviation of equivalent data = 0.20657 Rint = 0.17055 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16952, wR= 0.21791 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08208, wR= 0.10748, Acormin=0.656, Acormax=1.406, Acor_av=0.957 F test: Probability=1.000, F= 4.256 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08087, wR= 0.10131, Acormin=0.619, Acormax=1.388, Acor_av=0.911 F test: Probability=0.758, F= 1.029 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06889, wR= 0.09480, Acormin=0.678, Acormax=1.443, Acor_av=0.959 F test: Probability=1.000, F= 1.414 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06384, wR= 0.08520, Acormin=0.596, Acormax=1.466, Acor_av=0.910 F test: Probability=1.000, F= 1.163 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06159, wR= 0.08178, Acormin=0.549, Acormax=1.378, Acor_av=0.869 F test: Probability=0.953, F= 1.071 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06474, wR= 0.08812, Acormin=0.682, Acormax=1.533, Acor_av=0.926 F test: Probability=0.000, F= 0.904 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06075, wR= 0.08067, Acormin=0.607, Acormax=1.500, Acor_av=0.892 F test: Probability=0.729, F= 1.025 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05739, wR= 0.07662, Acormin=0.564, Acormax=1.423, Acor_av=0.851 F test: Probability=1.000, F= 1.146 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05165, wR= 0.07032, Acormin=0.535, Acormax=1.369, Acor_av=0.815 F test: Probability=1.000, F= 1.229 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06101, wR= 0.07940, Acormin=0.515, Acormax=1.382, Acor_av=0.822 F test: Probability=0.000, F= 0.718 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05809, wR= 0.07610, Acormin=0.553, Acormax=1.416, Acor_av=0.836 F test: Probability=0.000, F= 0.791 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05420, wR= 0.07072, Acormin=0.268, Acormax=0.691, Acor_av=0.414 F test: Probability=0.000, F= 0.906 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04862, wR= 0.06460, Acormin=0.287, Acormax=0.763, Acor_av=0.455 F test: Probability=0.997, F= 1.120 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04567, wR= 0.06168, Acormin=0.286, Acormax=0.810, Acor_av=0.478 F test: Probability=1.000, F= 1.262 Final absorption model (ne=6, no=5): Rint= 0.05165, Acormin=0.535, Acormax=1.369, Acor_av=0.815 Combined refinement in use Rint: 0.17066 There are 81 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: 6, max odd order: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20657 Using Levenberg-Marquardt: 0.00010 New wR= 0.05474 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17055 with corrections 0.04227 Rint for all data: 0.17066 with corrections 0.04248 1 observations identified as outliers and rejected Cycle 2 wR= 0.05458 Using Levenberg-Marquardt: 0.00001 New wR= 0.05014 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17003 with corrections 0.03708 Rint for all data: 0.17066 with corrections 0.03745 0 observations identified as outliers and rejected Cycle 3 wR= 0.05014 Using Levenberg-Marquardt: 0.00000 New wR= 0.04975 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17003 with corrections 0.03678 Rint for all data: 0.17066 with corrections 0.03715 0 observations identified as outliers and rejected Cycle 4 wR= 0.04975 Using Levenberg-Marquardt: 0.00000 New wR= 0.04957 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17003 with corrections 0.03662 Rint for all data: 0.17066 with corrections 0.03698 0 observations identified as outliers and rejected Cycle 5 wR= 0.04957 Using Levenberg-Marquardt: 0.00000 New wR= 0.04944 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17003 with corrections 0.03651 Rint for all data: 0.17066 with corrections 0.03686 0 observations identified as outliers and rejected Final wR= 0.04944 Final frame scales: Min= 0.8764 Max= 1.1294 Final absorption correction factors: Amin= 0.5790 Amax= 1.5585 PROFFIT INFO: Inet (after scale3 abspack): min=483.1750 max=5594922.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=166.3456 max=67641.1094 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3099 reflections read from tmp file 449 reflections are rejected (448 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 3 2 2 2 4 3 87 Initial Chi^2= 0.32203 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.71436 Current error model SIG(F2)^2 = 113.77*I_RAW + 0.00*I_BACK+(0.00682*)^2 Cycle 2, Chi^2= 1.58973 Current error model SIG(F2)^2 = 32.58*I_RAW + 0.00*I_BACK+(0.02597*)^2 Cycle 3, Chi^2= 1.03785 Current error model SIG(F2)^2 = 96.11*I_RAW + 0.00*I_BACK+(0.01716*)^2 Cycle 4, Chi^2= 1.00347 Current error model SIG(F2)^2 = 84.58*I_RAW + 0.00*I_BACK+(0.02042*)^2 Cycle 5, Chi^2= 1.00056 Current error model SIG(F2)^2 = 89.61*I_RAW + 0.00*I_BACK+(0.01939*)^2 Cycle 6, Chi^2= 0.99998 Current error model SIG(F2)^2 = 88.17*I_RAW + 0.00*I_BACK+(0.01972*)^2 Cycle 7, Chi^2= 1.00002 Current error model SIG(F2)^2 = 88.64*I_RAW + 0.00*I_BACK+(0.01961*)^2 Cycle 8, Chi^2= 0.99999 Current error model SIG(F2)^2 = 88.49*I_RAW + 0.00*I_BACK+(0.01965*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 88.49*I_RAW + 0.00*I_BACK+(0.01965*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5594923- 1562619 309 2344782.85 47.65 100.00 1561155- 997550 309 1230218.40 41.84 100.00 994202- 325115 309 599923.41 40.18 100.00 323596- 203647 309 247048.19 34.07 100.00 203576- 168615 309 184583.84 27.95 100.00 168555- 125960 309 141791.35 22.54 100.00 125932- 100694 309 113197.64 19.56 100.00 100685- 5756 309 58604.07 14.77 100.00 5744- 3452 309 4347.95 4.97 100.00 3451- 483 318 2652.80 3.88 79.25 ------------------------------------------------------------------------------------ 5594923- 483 3099 491291.83 25.68 97.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 903641.90 38.58 100.00 1.41- 1.12 309 795045.23 30.98 100.00 1.12- 0.96 309 611691.13 29.88 99.68 0.96- 0.88 309 474998.64 26.21 98.71 0.88- 0.81 309 609166.05 30.13 98.71 0.81- 0.74 309 316411.85 20.63 98.71 0.74- 0.71 309 268092.91 20.65 98.06 0.71- 0.65 309 482188.65 25.53 99.35 0.65- 0.62 309 233035.23 16.81 90.29 0.62- 0.58 318 226363.07 17.60 95.28 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 491291.83 25.68 97.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 309 903641.90 38.58 100.00 4.82- 1.12 618 849343.57 34.78 100.00 4.82- 0.96 927 770126.09 33.15 99.89 4.82- 0.88 1236 696344.23 31.41 99.60 4.82- 0.81 1545 678908.59 31.16 99.42 4.82- 0.74 1854 618492.47 29.40 99.30 4.82- 0.71 2163 568435.39 28.15 99.12 4.82- 0.65 2472 557654.55 27.82 99.15 4.82- 0.62 2781 521585.73 26.60 98.17 4.82- 0.58 3099 491291.83 25.68 97.87 ------------------------------------------------------------------------------------ 4.82- 0.58 3099 491291.83 25.68 97.87 Scale applied to data: s=0.178733 (maximum obs:5594922.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.025: data 3099 -> merged 109 With outlier rejection... Rint 0.036; Rsigma 0.025: data 3088 -> merged 109 Rejected total: 11, method kkm 10, method Blessing 1 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585728, 4.830037 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 18.00 100.00 180 1.61 - 1.21 10 10 28.50 100.00 285 1.17 - 1.01 10 10 36.80 100.00 368 0.99 - 0.89 10 10 36.60 100.00 366 0.88 - 0.81 10 10 34.60 100.00 346 0.81 - 0.74 10 10 30.50 100.00 305 0.73 - 0.71 10 10 32.80 100.00 328 0.70 - 0.66 10 10 28.10 100.00 281 0.66 - 0.64 10 10 25.90 100.00 259 0.63 - 0.60 10 10 26.40 100.00 264 --------------------------------------------------------------- 8.36 - 0.60 100 100 29.82 100.00 2982 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:14:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.365379 8.374951 8.357296 90.1096 89.9672 90.0080 3080 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1570 0 2065 2063 3080 N (int>3sigma) = 0 0 0 0 1570 0 2021 2020 3016 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 87.2 87.5 87.3 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.1 26.2 26.0 Lattice type: F chosen Volume: 585.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.929 b.b = 34.936 c.c = 34.976 b.c = -0.034 a.c = -17.435 a.b = -17.420 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.139 CUBIC F-lattice R(int) = 0.033 [ 2924] Vol = 585.5 Cell: 8.365 8.375 8.357 90.11 89.97 90.01 Volume: 585.51 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.131 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 2647] Vol = 439.1 Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.13 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.131 RHOMBOHEDRAL R-lattice R(int) = 0.034 [ 848] Vol = 439.1 Trigonal Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.13 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.032 [ 2679] Vol = 292.8 Cell: 5.919 5.918 8.357 89.95 89.90 89.93 Volume: 292.75 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.148 TETRAGONAL I-lattice R(int) = 0.032 [ 2679] Vol = 292.8 Cell: 5.918 5.919 8.357 90.10 90.05 89.93 Volume: 292.75 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.032 [ 2626] Vol = 292.8 Cell: 5.918 5.919 8.357 89.90 89.95 89.93 Volume: 292.75 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 2625] Vol = 292.8 Cell: 5.910 8.365 5.921 89.97 89.88 90.02 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.031 [ 2283] Vol = 292.8 Cell: 5.919 5.918 8.357 90.05 90.10 89.93 Volume: 292.75 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.116 MONOCLINIC I-lattice R(int) = 0.030 [ 2283] Vol = 292.8 Cell: 5.910 5.921 8.365 90.03 90.02 90.12 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.028 [ 2301] Vol = 292.8 Cell: 5.910 8.365 5.921 89.97 90.12 89.98 Volume: 292.75 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.053 MONOCLINIC I-lattice R(int) = 0.030 [ 2283] Vol = 292.8 Cell: 8.365 5.910 5.921 90.12 90.03 90.02 Volume: 292.75 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.102 MONOCLINIC C-lattice R(int) = 0.029 [ 2282] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.91 Volume: 292.75 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.026 [ 1641] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.38 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1570 0 2065 2063 3080 N (int>3sigma) = 0 0 0 0 1570 0 2021 2020 3016 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 87.2 87.5 87.3 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.1 26.2 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 29 29 242 686 N I>3s 25 25 231 686 0.7 0.7 0.7 39.3 8.6 8.6 5.6 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.033 2702 Fd-3m 1 1 227 C N N N N 37 2284 0.034 2741 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365379 8.374951 8.357296 90.1096 89.9672 90.0080 ZERR 3.00 0.000451 0.000647 0.000616 0.0061 0.0053 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5416779- 911652 688 685 27 25.4 1700939.61 43.99 0.034 0.046 894279- 156666 918 914 27 33.9 285566.71 33.24 0.039 0.049 144621- 53326 762 761 27 28.2 112727.37 19.72 0.051 0.067 22206- 1892 731 728 28 26.0 4673.64 5.04 0.153 0.183 ------------------------------------------------------------------------------------------- 5416779- 1892 3099 3088 109 28.3 490718.77 25.64 0.036 0.048 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 773 768 27 28.4 796352.77 34.72 0.036 0.049 0.022 1.01-0.78 944 941 27 34.9 476552.30 25.34 0.030 0.040 0.025 0.78-0.65 814 813 27 30.1 386875.91 22.59 0.039 0.048 0.029 0.65-0.59 568 566 28 20.2 248718.71 18.21 0.049 0.057 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 3099 3088 109 28.3 490718.77 25.64 0.036 0.048 0.025 inf-0.60 2990 2981 99 30.1 501530.64 25.97 0.036 0.048 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 768 27 27 100.0 28.4 796352.77 208.80 0.036 0.006 1.01-0.78 941 27 27 100.0 34.9 476552.30 160.21 0.030 0.005 0.78-0.65 813 27 27 100.0 30.1 386875.91 132.08 0.039 0.006 0.65-0.59 566 28 28 100.0 20.2 248718.71 94.24 0.049 0.009 -------------------------------------------------------------------------------------------- inf-0.59 3088 109 109 100.0 28.3 490718.77 152.80 0.036 0.006 inf-0.60 2981 99 99 100.0 30.1 501530.64 155.83 0.036 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:15:33 2018) ID: 2932; threads 38; handles 877; mem 519496.00 (1229536.00)kB; time: 1w 5d 23h 21m 4s MEMORY INFO: Memory PF:0.0, Ph:174.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:507.3,peak PF: 708.5, WS: 271.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:174.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:509.1,peak PF: 708.5, WS: 273.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:15:33 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000007 0.000007 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000005 0.000005 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000007 0.000006 ) 8.37051 ( 0.00045 ) 8.37682 ( 0.00065 ) 8.35710 ( 0.00062 ) 90.12473 ( 0.00612 ) 89.98579 ( 0.00528 ) 90.00567 ( 0.00538 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:15:34 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000007 0.000007 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000005 0.000005 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000007 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(6) 90.125(6) 89.986(5) 90.006(5) V = 585.98(7) unit cell: 8.36587(15) 8.36587(15) 8.36587(15) 90.0 90.0 90.0 V = 585.509(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 448 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.129 ( 0.095) | 1.187 ( 0.460) | 0.89- 0.82 | 44 | 1.149 ( 0.080) | 1.146 ( 0.112) | 1.137 ( 0.379) | 0.82- 0.75 | 44 | 1.165 ( 0.079) | 1.132 ( 0.151) | 1.170 ( 0.385) | 0.75- 0.71 | 44 | 1.179 ( 0.070) | 1.163 ( 0.122) | 1.208 ( 0.418) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.129 ( 0.136) | 1.367 ( 0.527) | 0.67- 0.63 | 44 | 1.213 ( 0.070) | 1.171 ( 0.161) | 1.249 ( 0.427) | 0.62- 0.59 | 43 | 1.235 ( 0.080) | 1.116 ( 0.203) | 1.267 ( 0.451) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 439 | 1.147 ( 0.116) | 1.159 ( 0.275) | 1.203 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=5, end=29, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_6_5.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_5.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_6_5.rpb PROFFITPEAK info: 316 peaks in the peak location table UB fit with 143 obs out of 153 (total:153,skipped:0) (93.46%) UB - matrix: -0.007451 0.076983 -0.035096 ( 0.000117 0.000174 0.000116 ) -0.083640 -0.011610 -0.008091 ( 0.000062 0.000092 0.000062 ) -0.012145 0.033870 0.076721 ( 0.000055 0.000082 0.000055 ) M - matrix: 0.007199 -0.000014 0.000007 ( 0.000011 0.000012 0.000008 ) -0.000014 0.007208 -0.000009 ( 0.000012 0.000027 0.000013 ) 0.000007 -0.000009 0.007183 ( 0.000008 0.000013 0.000012 ) unit cell: 8.360(6) 8.354(14) 8.369(8) 89.93(11) 90.05(7) 89.89(9) V = 584(1) UB fit with 143 obs out of 153 (total:153,skipped:0) (93.46%) UB - matrix: -0.007451 0.076983 -0.035096 ( 0.000117 0.000174 0.000116 ) -0.083640 -0.011610 -0.008091 ( 0.000062 0.000092 0.000062 ) -0.012145 0.033870 0.076721 ( 0.000055 0.000082 0.000055 ) M - matrix: 0.007199 -0.000014 0.000007 ( 0.000011 0.000012 0.000008 ) -0.000014 0.007208 -0.000009 ( 0.000012 0.000027 0.000013 ) 0.000007 -0.000009 0.007183 ( 0.000008 0.000013 0.000012 ) unit cell: 8.360(6) 8.354(14) 8.369(8) 89.93(11) 90.05(7) 89.89(9) V = 584(1) OTKP changes: 29 1 1 1 No constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007178 -0.000020 0.000010 ( 0.000012 0.000012 0.000008 ) -0.000020 0.007185 -0.000020 ( 0.000012 0.000026 0.000012 ) 0.000010 -0.000020 0.007167 ( 0.000008 0.000012 0.000011 ) Constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007158 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007158 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007158 ( 0.000000 0.000000 0.000002 ) UB fit with 142 obs out of 153 (total:153,skipped:0) (92.81%) unit cell: 8.372(7) 8.368(14) 8.379(7) 89.84(10) 90.08(7) 89.84(10) V = 587(1) unit cell: 8.3728(13) 8.3728(13) 8.3728(13) 90.0 90.0 90.0 V = 586.97(16) UB fit with 142 obs out of 153 (total:153,skipped:0) (92.81%) UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007178 -0.000020 0.000010 ( 0.000012 0.000012 0.000008 ) -0.000020 0.007185 -0.000020 ( 0.000012 0.000026 0.000012 ) 0.000010 -0.000020 0.007167 ( 0.000008 0.000012 0.000011 ) unit cell: 8.372(7) 8.368(14) 8.379(7) 89.84(10) 90.08(7) 89.84(10) V = 587(1) OTKP changes: 29 1 1 1 No constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007178 -0.000020 0.000010 ( 0.000012 0.000012 0.000008 ) -0.000020 0.007185 -0.000020 ( 0.000012 0.000026 0.000012 ) 0.000010 -0.000020 0.007167 ( 0.000008 0.000012 0.000011 ) Constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007158 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007158 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007158 ( 0.000000 0.000000 0.000002 ) UB fit with 142 obs out of 153 (total:153,skipped:0) (92.81%) unit cell: 8.372(7) 8.368(14) 8.379(7) 89.84(10) 90.08(7) 89.84(10) V = 587(1) unit cell: 8.3728(13) 8.3728(13) 8.3728(13) 90.0 90.0 90.0 V = 586.97(16) 153 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Run 6 Omega scan: (3.000 - 32.000,29 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=53.095) HKL list info: 291 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007178 -0.000020 0.000010 ( 0.000012 0.000012 0.000008 ) -0.000020 0.007185 -0.000020 ( 0.000012 0.000026 0.000012 ) 0.000010 -0.000020 0.007167 ( 0.000008 0.000012 0.000011 ) Constraint UB - matrix: -0.007389 0.076921 -0.035064 ( 0.000113 0.000168 0.000113 ) -0.083533 -0.011436 -0.008094 ( 0.000068 0.000102 0.000068 ) -0.012071 0.033726 0.076627 ( 0.000050 0.000074 0.000050 ) M - matrix: 0.007158 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007158 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007158 ( 0.000000 0.000000 0.000002 ) UB fit with 142 obs out of 153 (total:153,skipped:0) (92.81%) unit cell: 8.372(7) 8.368(14) 8.379(7) 89.84(10) 90.08(7) 89.84(10) V = 587(1) unit cell: 8.3728(13) 8.3728(13) 8.3728(13) 90.0 90.0 90.0 V = 586.97(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 142 obs out of 153 (total:153,skipped:0) (92.81%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=5, end=29, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_5.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_5.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_5.rpb 1 of 120 peaks identified as outliers and rejected 119 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 119 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 119 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.88- 1.47 | 12 | 0.950 ( 0.140) | 1.080 ( 0.434) | 1.097 ( 0.498) | 1.41- 1.17 | 12 | 1.065 ( 0.052) | 1.087 ( 0.078) | 1.182 ( 0.388) | 1.16- 1.02 | 12 | 1.087 ( 0.072) | 1.050 ( 0.171) | 1.164 ( 0.526) | 0.99- 0.96 | 12 | 1.105 ( 0.046) | 1.098 ( 0.122) | 1.291 ( 0.458) | 0.93- 0.84 | 12 | 1.142 ( 0.040) | 1.135 ( 0.110) | 1.095 ( 0.327) | 0.84- 0.78 | 12 | 1.165 ( 0.054) | 1.114 ( 0.101) | 1.065 ( 0.414) | 0.78- 0.72 | 12 | 1.164 ( 0.055) | 1.186 ( 0.142) | 1.146 ( 0.268) | 0.71- 0.67 | 12 | 1.171 ( 0.037) | 1.155 ( 0.118) | 1.135 ( 0.480) | 0.67- 0.64 | 12 | 1.175 ( 0.044) | 1.239 ( 0.099) | 1.171 ( 0.367) | 0.62- 0.60 | 11 | 1.131 ( 0.064) | 1.197 ( 0.152) | 1.146 ( 0.401) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.88- 0.60 | 119 | 1.116 ( 0.094) | 1.134 ( 0.190) | 1.149 ( 0.424) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 119 obs out of 119 (total:119,skipped:0) (100.00%) UB - matrix: -0.007500 0.077050 -0.034927 ( 0.000046 0.000065 0.000046 ) -0.083535 -0.011805 -0.008034 ( 0.000036 0.000051 0.000037 ) -0.011977 0.033613 0.076738 ( 0.000026 0.000037 0.000026 ) M - matrix: 0.007178 0.000006 0.000014 ( 0.000006 0.000006 0.000004 ) 0.000006 0.007206 -0.000017 ( 0.000006 0.000010 0.000005 ) 0.000014 -0.000017 0.007173 ( 0.000004 0.000005 0.000005 ) unit cell: 8.372(4) 8.356(6) 8.375(3) 89.87(4) 90.11(3) 90.05(4) V = 585.9(5) OTKP changes: 119 1 1 1 No constraint UB - matrix: -0.007402 0.077047 -0.035152 ( 0.000043 0.000061 0.000043 ) -0.083684 -0.011611 -0.008085 ( 0.000027 0.000038 0.000027 ) -0.012080 0.033835 0.076815 ( 0.000022 0.000031 0.000022 ) M - matrix: 0.007204 -0.000007 0.000009 ( 0.000005 0.000005 0.000003 ) -0.000007 0.007216 -0.000015 ( 0.000005 0.000010 0.000005 ) 0.000009 -0.000015 0.007202 ( 0.000003 0.000005 0.000005 ) Constraint UB - matrix: -0.007402 0.077047 -0.035152 ( 0.000043 0.000061 0.000043 ) -0.083684 -0.011611 -0.008085 ( 0.000027 0.000038 0.000027 ) -0.012080 0.033835 0.076815 ( 0.000022 0.000031 0.000022 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 119 obs out of 119 (total:119,skipped:0) (100.00%) unit cell: 8.357(3) 8.350(5) 8.358(3) 89.88(4) 90.07(3) 89.94(4) V = 583.2(5) unit cell: 8.3551(5) 8.3551(5) 8.3551(5) 90.0 90.0 90.0 V = 583.25(6) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (3.000 - 32.000,29 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.918) HKL list info: 289 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007402 0.077047 -0.035152 ( 0.000043 0.000061 0.000043 ) -0.083684 -0.011611 -0.008085 ( 0.000027 0.000038 0.000027 ) -0.012080 0.033835 0.076815 ( 0.000022 0.000031 0.000022 ) M - matrix: 0.007204 -0.000007 0.000009 ( 0.000005 0.000005 0.000003 ) -0.000007 0.007216 -0.000015 ( 0.000005 0.000010 0.000005 ) 0.000009 -0.000015 0.007202 ( 0.000003 0.000005 0.000005 ) Constraint UB - matrix: -0.007402 0.077047 -0.035152 ( 0.000043 0.000061 0.000043 ) -0.083684 -0.011611 -0.008085 ( 0.000027 0.000038 0.000027 ) -0.012080 0.033835 0.076815 ( 0.000022 0.000031 0.000022 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 119 obs out of 119 (total:119,skipped:0) (100.00%) unit cell: 8.357(3) 8.350(5) 8.358(3) 89.88(4) 90.07(3) 89.94(4) V = 583.2(5) unit cell: 8.3551(5) 8.3551(5) 8.3551(5) 90.0 90.0 90.0 V = 583.25(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 119 obs out of 119 (total:119,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=5, end=29, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_5.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_5.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_5.rpb 1 of 118 peaks identified as outliers and rejected 117 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 117 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 117 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 12 | 0.951 ( 0.141) | 1.105 ( 0.505) | 1.051 ( 0.403) | 1.41- 1.15 | 12 | 1.064 ( 0.059) | 1.158 ( 0.217) | 1.095 ( 0.358) | 1.15- 0.98 | 12 | 1.084 ( 0.065) | 1.117 ( 0.144) | 1.244 ( 0.544) | 0.98- 0.93 | 12 | 1.110 ( 0.047) | 1.075 ( 0.118) | 1.249 ( 0.419) | 0.92- 0.82 | 12 | 1.157 ( 0.037) | 1.151 ( 0.102) | 1.091 ( 0.421) | 0.82- 0.78 | 12 | 1.183 ( 0.072) | 1.169 ( 0.165) | 1.163 ( 0.486) | 0.78- 0.71 | 12 | 1.155 ( 0.022) | 1.168 ( 0.100) | 1.112 ( 0.318) | 0.71- 0.67 | 12 | 1.171 ( 0.038) | 1.126 ( 0.095) | 1.191 ( 0.479) | 0.67- 0.62 | 12 | 1.191 ( 0.048) | 1.282 ( 0.121) | 1.165 ( 0.424) | 0.62- 0.60 | 9 | 1.117 ( 0.045) | 1.221 ( 0.194) | 1.225 ( 0.406) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.60 | 117 | 1.118 ( 0.096) | 1.156 ( 0.219) | 1.157 ( 0.436) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 236 | 1.149 ( 0.123) | 1.250 ( 0.398) | 1.330 ( 0.660) | 13.1-18.9 | 236 | 1.133 ( 0.072) | 1.192 ( 0.273) | 1.269 ( 0.560) | 18.9-23.0 | 236 | 1.145 ( 0.092) | 1.197 ( 0.283) | 1.257 ( 0.670) | 23.1-27.3 | 236 | 1.133 ( 0.093) | 1.169 ( 0.292) | 1.226 ( 0.565) | 27.3-30.4 | 236 | 1.138 ( 0.100) | 1.165 ( 0.255) | 1.196 ( 0.451) | 30.4-33.7 | 236 | 1.151 ( 0.103) | 1.143 ( 0.226) | 1.203 ( 0.445) | 33.7-37.0 | 236 | 1.140 ( 0.098) | 1.121 ( 0.167) | 1.145 ( 0.427) | 37.0-39.8 | 236 | 1.152 ( 0.118) | 1.108 ( 0.214) | 1.235 ( 0.511) | 39.8-42.8 | 236 | 1.165 ( 0.110) | 1.096 ( 0.184) | 1.220 ( 0.535) | 42.8-49.8 | 231 | 1.207 ( 0.159) | 1.136 ( 0.280) | 1.182 ( 0.476) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2355 | 1.151 ( 0.111) | 1.158 ( 0.268) | 1.227 ( 0.538) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0026 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:16:03 2018 PROFFITMAIN - Started at Wed Mar 28 14:16:03 2018 OTKP changes: 2345 2 4 6 OTKP changes: 2345 2 4 6 No constraint UB - matrix: -0.007496 0.076884 -0.034781 ( 0.000006 0.000007 0.000006 ) -0.083621 -0.011795 -0.008051 ( 0.000005 0.000005 0.000004 ) -0.012177 0.033655 0.077063 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007197 0.000000 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007183 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007213 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007496 0.076884 -0.034781 ( 0.000006 0.000007 0.000006 ) -0.083621 -0.011795 -0.008051 ( 0.000005 0.000005 0.000004 ) -0.012177 0.033655 0.077063 ( 0.000007 0.000007 0.000006 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000000 ) UB fit with 2348 obs out of 2355 (total:2355,skipped:0) (99.70%) unit cell: 8.3609(5) 8.3691(6) 8.3515(6) 90.115(6) 89.965(5) 90.001(5) V = 584.38(7) unit cell: 8.36051(15) 8.36051(15) 8.36051(15) 90.0 90.0 90.0 V = 584.385(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007598 0.077000 -0.034680 ( 0.000017 0.000015 0.000011 ) -0.083474 -0.011806 -0.008121 ( 0.000011 0.000010 0.000008 ) -0.012071 0.033517 0.076934 ( 0.000013 0.000012 0.000009 ) M - matrix: 0.007171 -0.000004 0.000013 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007192 0.000004 ( 0.000002 0.000002 0.000001 ) 0.000013 0.000004 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3759(11) 8.3640(13) 8.3664(10) 90.033(11) 90.102(11) 89.967(13) V = 586.11(14) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 No constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3686(11) 8.3673(13) 8.3651(10) 90.041(11) 90.009(10) 89.971(12) V = 585.74(13) unit cell: 8.3670(4) 8.3670(4) 8.3670(4) 90.0 90.0 90.0 V = 585.74(4) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.956) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3686(11) 8.3673(13) 8.3651(10) 90.041(11) 90.009(10) 89.971(12) V = 585.74(13) unit cell: 8.3670(4) 8.3670(4) 8.3670(4) 90.0 90.0 90.0 V = 585.74(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007184 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007592 0.076973 -0.034656 ( 0.000016 0.000014 0.000011 ) -0.083542 -0.011810 -0.008030 ( 0.000011 0.000010 0.000007 ) -0.012120 0.033492 0.076970 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3686(11) 8.3673(13) 8.3651(10) 90.041(11) 90.009(10) 89.971(12) V = 585.74(13) unit cell: 8.3670(4) 8.3670(4) 8.3670(4) 90.0 90.0 90.0 V = 585.74(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007133 0.076857 -0.034850 ( 0.000018 0.000012 0.000019 ) -0.083554 -0.011649 -0.008029 ( 0.000014 0.000010 0.000015 ) -0.012432 0.033793 0.076709 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007187 0.000005 -0.000034 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007185 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000034 0.000007 0.007163 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3670(13) 8.3682(14) 8.3807(15) 90.058(14) 89.727(14) 90.040(14) V = 586.78(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007250 0.076722 -0.035022 ( 0.000015 0.000010 0.000016 ) -0.083590 -0.011723 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012375 0.033948 0.076892 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007193 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007176 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007204 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007250 0.076722 -0.035022 ( 0.000015 0.000010 0.000016 ) -0.083590 -0.011723 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012375 0.033948 0.076892 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3633(13) 8.3731(12) 8.3568(15) 90.144(13) 89.820(13) 90.029(12) V = 585.19(16) unit cell: 8.3644(3) 8.3644(3) 8.3644(3) 90.0 90.0 90.0 V = 585.19(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.956) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007250 0.076722 -0.035022 ( 0.000015 0.000010 0.000016 ) -0.083590 -0.011723 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012375 0.033948 0.076892 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007193 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007176 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007204 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007250 0.076722 -0.035022 ( 0.000015 0.000010 0.000016 ) -0.083590 -0.011723 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012375 0.033948 0.076892 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3633(13) 8.3731(12) 8.3568(15) 90.144(13) 89.820(13) 90.029(12) V = 585.19(16) unit cell: 8.3644(3) 8.3644(3) 8.3644(3) 90.0 90.0 90.0 V = 585.19(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084686 0.000100 -0.000194 ( 0.000016 0.000011 0.000018 ) 0.000018 0.084769 0.000099 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084838 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007172 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007186 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007198 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084686 0.000100 -0.000194 ( 0.000016 0.000011 0.000018 ) 0.000018 0.084769 0.000099 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084838 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3757(16) 8.3675(8) 8.3606(10) 90.065(10) 89.870(13) 90.080(11) V = 585.94(14) unit cell: 8.3679(3) 8.3679(3) 8.3679(3) 90.0 90.0 90.0 V = 585.94(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083602 -0.011659 -0.008126 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007191 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3642(9) 8.3764(13) 8.3562(12) 90.036(12) 90.109(11) 89.923(11) V = 585.44(14) OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000010 0.000013 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000013 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 438 obs out of 439 (total:439,skipped:0) (99.77%) unit cell: 8.3639(10) 8.3764(13) 8.3559(12) 90.039(12) 90.107(11) 89.924(11) V = 585.41(14) unit cell: 8.3654(4) 8.3654(4) 8.3654(4) 90.0 90.0 90.0 V = 585.41(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000010 0.000013 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000013 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 438 obs out of 439 (total:439,skipped:0) (99.77%) unit cell: 8.3639(10) 8.3764(13) 8.3559(12) 90.039(12) 90.107(11) 89.924(11) V = 585.41(14) unit cell: 8.3654(4) 8.3654(4) 8.3654(4) 90.0 90.0 90.0 V = 585.41(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084795 -0.000099 0.000200 ( 0.000009 0.000014 0.000014 ) -0.000001 0.084708 0.000094 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000002 0.084892 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007190 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007207 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084795 -0.000099 0.000200 ( 0.000009 0.000014 0.000014 ) -0.000001 0.084708 0.000094 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000002 0.084892 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3649(9) 8.3734(14) 8.3554(9) 90.065(12) 90.132(11) 89.932(11) V = 585.23(13) unit cell: 8.3646(4) 8.3646(4) 8.3646(4) 90.0 90.0 90.0 V = 585.23(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007568 0.077021 -0.034599 ( 0.000015 0.000014 0.000012 ) -0.083439 -0.011872 -0.008154 ( 0.000012 0.000011 0.000010 ) -0.012263 0.033265 0.076987 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007170 -0.000000 -0.000002 ( 0.000002 0.000002 0.000001 ) -0.000000 0.007180 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000007 0.007191 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3768(11) 8.3709(13) 8.3647(11) 89.944(12) 89.985(11) 89.998(12) V = 586.55(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3650(11) 8.3686(12) 8.3661(10) 90.006(10) 90.052(10) 90.096(11) V = 585.65(13) unit cell: 8.3666(4) 8.3666(4) 8.3666(4) 90.0 90.0 90.0 V = 585.65(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.956) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3650(11) 8.3686(12) 8.3661(10) 90.006(10) 90.052(10) 90.096(11) V = 585.65(13) unit cell: 8.3666(4) 8.3666(4) 8.3666(4) 90.0 90.0 90.0 V = 585.65(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007190 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007184 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007585 0.077012 -0.034558 ( 0.000013 0.000012 0.000011 ) -0.083574 -0.011979 -0.008141 ( 0.000011 0.000010 0.000009 ) -0.012156 0.033310 0.076991 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3650(11) 8.3686(12) 8.3661(10) 90.006(10) 90.052(10) 90.096(11) V = 585.65(13) unit cell: 8.3666(4) 8.3666(4) 8.3666(4) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 117 obs out of 117 (total:117,skipped:0) (100.00%) UB - matrix: -0.007438 0.077082 -0.035148 ( 0.000045 0.000063 0.000045 ) -0.083690 -0.011670 -0.008077 ( 0.000029 0.000040 0.000029 ) -0.012094 0.033847 0.076808 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007206 -0.000006 0.000009 ( 0.000005 0.000005 0.000003 ) -0.000006 0.007223 -0.000015 ( 0.000005 0.000010 0.000005 ) 0.000009 -0.000015 0.007200 ( 0.000003 0.000005 0.000005 ) unit cell: 8.356(3) 8.346(5) 8.359(3) 89.88(4) 90.07(3) 89.95(4) V = 582.9(5) OTKP changes: 117 1 1 1 No constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007203 -0.000008 0.000008 ( 0.000005 0.000005 0.000003 ) -0.000008 0.007217 -0.000014 ( 0.000005 0.000010 0.000005 ) 0.000008 -0.000014 0.007199 ( 0.000003 0.000005 0.000005 ) Constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 117 obs out of 117 (total:117,skipped:0) (100.00%) unit cell: 8.357(3) 8.349(5) 8.360(3) 89.89(4) 90.06(3) 89.94(4) V = 583.3(5) unit cell: 8.3554(6) 8.3554(6) 8.3554(6) 90.0 90.0 90.0 V = 583.32(7) Run 6 Omega scan: (3.000 - 32.000,29 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) HKL list info: 283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007203 -0.000008 0.000008 ( 0.000005 0.000005 0.000003 ) -0.000008 0.007217 -0.000014 ( 0.000005 0.000010 0.000005 ) 0.000008 -0.000014 0.007199 ( 0.000003 0.000005 0.000005 ) Constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 117 obs out of 117 (total:117,skipped:0) (100.00%) unit cell: 8.357(3) 8.349(5) 8.360(3) 89.89(4) 90.06(3) 89.94(4) V = 583.3(5) unit cell: 8.3554(6) 8.3554(6) 8.3554(6) 90.0 90.0 90.0 V = 583.32(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 117 obs out of 117 (total:117,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007203 -0.000008 0.000008 ( 0.000005 0.000005 0.000003 ) -0.000008 0.007217 -0.000014 ( 0.000005 0.000010 0.000005 ) 0.000008 -0.000014 0.007199 ( 0.000003 0.000005 0.000005 ) Constraint UB - matrix: -0.007405 0.077046 -0.035147 ( 0.000045 0.000062 0.000044 ) -0.083678 -0.011612 -0.008081 ( 0.000028 0.000039 0.000028 ) -0.012090 0.033858 0.076802 ( 0.000024 0.000033 0.000024 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 117 obs out of 117 (total:117,skipped:0) (100.00%) unit cell: 8.357(3) 8.349(5) 8.360(3) 89.89(4) 90.06(3) 89.94(4) V = 583.3(5) unit cell: 8.3554(6) 8.3554(6) 8.3554(6) 90.0 90.0 90.0 V = 583.32(7) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=29, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=5, end=29, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_5.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_5.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_5.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007476 0.076829 -0.034769 ( 0.000006 0.000007 0.000006 ) -0.083576 -0.011781 -0.008053 ( 0.000004 0.000005 0.000004 ) -0.012170 0.033637 0.077004 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007476 0.076829 -0.034769 ( 0.000006 0.000007 0.000006 ) -0.083576 -0.011781 -0.008053 ( 0.000004 0.000005 0.000004 ) -0.012170 0.033637 0.077004 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 2350 obs out of 2355 (total:2355,skipped:0) (99.79%) unit cell: 8.3656(4) 8.3749(6) 8.3573(6) 90.110(6) 89.967(5) 90.007(5) V = 585.52(7) unit cell: 8.36594(15) 8.36594(15) 8.36594(15) 90.0 90.0 90.0 V = 585.524(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 74 reflections under beam stop or inside a detector rejection region 30 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3155 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:16:11 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.956) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.956) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.956) Run 6 Omega scan: (3.000 - 32.000,29 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) PROFFIT INFO: signal sum: min=68.0000 max=22692716.0000 PROFFIT INFO: signal sum lp corr: min=222.3350 max=3262864.4285 PROFFIT INFO: background sum: min=736.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10944.0000 PROFFIT INFO: num of signal pixels: min=59 max=879 PROFFIT INFO: Inet: min=485.0947 max=7118977.5000 PROFFIT INFO: sig(Inet): min=187.9576 max=63744.1094 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=309.53 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 73 244 413 658 721 1288 2099 2865 3155 Percent 0.0 0.1 2.3 7.7 13.1 20.9 22.9 40.8 66.5 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3155 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 3155 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7118978- 1583700 315 2394747.04 134.50 100.00 1579488- 1030570 315 1285583.53 110.02 100.00 1026917- 309368 315 596511.81 94.29 100.00 309081- 215760 315 252334.31 68.68 100.00 215623- 163404 315 186573.57 48.55 100.00 163304- 130169 315 146253.86 37.56 100.00 130037- 100514 315 114921.14 30.15 100.00 100420- 6074 315 55950.18 20.63 100.00 6046- 3525 315 4545.67 4.92 83.17 3525- 485 320 2627.75 3.14 40.31 ------------------------------------------------------------------------------------ 7118978- 485 3155 503210.31 55.16 92.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 861475.89 87.88 100.00 1.41- 1.12 315 758845.02 70.56 98.41 1.12- 0.96 315 672228.59 75.72 99.05 0.96- 0.88 315 480394.47 59.86 94.92 0.88- 0.81 315 642843.83 69.59 97.46 0.81- 0.74 315 339450.95 40.84 93.65 0.74- 0.71 315 276509.32 37.11 90.16 0.71- 0.65 315 509751.49 51.21 95.24 0.65- 0.62 315 251847.25 29.47 73.65 0.62- 0.58 320 242888.39 29.77 80.31 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 503210.31 55.16 92.27 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:16:11 2018 Sorting 3155 observations 119 unique observations with > 7.00 F2/sig(F2) 3155 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 27 550 Total number of frames 550 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3155 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 5 112 Total number of frames 112 2532 observations > 7.00 F2/sig(F2) 2532 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 5 112 Total number of frames 112 Removing 'redundancy=1' reflections Average redundancy: 20.2 (Out of 2532 removed 7 = 2525, 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 2525 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 5 112 Total number of frames 112 125 unique data precomputed (should be 125) 125 unique data with 2525 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.2 (Out of 2525 removed 0 = 2525, unique = 125) 125 unique data precomputed (should be 125) 125 unique data with 2525 observations RMS deviation of equivalent data = 0.20510 Rint = 0.17010 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16918, wR= 0.21722 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08216, wR= 0.10766, Acormin=0.651, Acormax=1.401, Acor_av=0.955 F test: Probability=1.000, F= 4.231 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08082, wR= 0.10164, Acormin=0.618, Acormax=1.389, Acor_av=0.913 F test: Probability=0.780, F= 1.032 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06894, wR= 0.09468, Acormin=0.673, Acormax=1.453, Acor_av=0.958 F test: Probability=1.000, F= 1.415 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06359, wR= 0.08467, Acormin=0.587, Acormax=1.480, Acor_av=0.912 F test: Probability=1.000, F= 1.174 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06093, wR= 0.08141, Acormin=0.556, Acormax=1.402, Acor_av=0.880 F test: Probability=0.978, F= 1.086 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06455, wR= 0.08724, Acormin=0.677, Acormax=1.547, Acor_av=0.925 F test: Probability=0.000, F= 0.890 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05990, wR= 0.07929, Acormin=0.602, Acormax=1.520, Acor_av=0.892 F test: Probability=0.778, F= 1.032 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05684, wR= 0.07599, Acormin=0.574, Acormax=1.449, Acor_av=0.860 F test: Probability=0.999, F= 1.143 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05158, wR= 0.06994, Acormin=0.540, Acormax=1.393, Acor_av=0.823 F test: Probability=1.000, F= 1.209 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06028, wR= 0.07780, Acormin=0.513, Acormax=1.405, Acor_av=0.823 F test: Probability=0.000, F= 0.733 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05762, wR= 0.07497, Acormin=0.544, Acormax=1.426, Acor_av=0.833 F test: Probability=0.000, F= 0.802 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05453, wR= 0.07106, Acormin=0.273, Acormax=0.701, Acor_av=0.418 F test: Probability=0.000, F= 0.892 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04937, wR= 0.06512, Acormin=0.291, Acormax=0.770, Acor_av=0.458 F test: Probability=0.974, F= 1.083 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04594, wR= 0.06172, Acormin=0.290, Acormax=0.819, Acor_av=0.482 F test: Probability=1.000, F= 1.243 Final absorption model (ne=6, no=5): Rint= 0.05158, Acormin=0.540, Acormax=1.393, Acor_av=0.823 Combined refinement in use Rint: 0.17021 There are 112 active scales (one needs to be fixed) Refinement control: frame scale #111 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20510 Using Levenberg-Marquardt: 0.00010 New wR= 0.05263 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.04086 Rint for all data: 0.17021 with corrections 0.04107 0 observations identified as outliers and rejected Cycle 2 wR= 0.05263 Using Levenberg-Marquardt: 0.00001 New wR= 0.04849 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.03613 Rint for all data: 0.17021 with corrections 0.03634 0 observations identified as outliers and rejected Cycle 3 wR= 0.04849 Using Levenberg-Marquardt: 0.00000 New wR= 0.04820 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.03602 Rint for all data: 0.17021 with corrections 0.03624 0 observations identified as outliers and rejected Cycle 4 wR= 0.04820 Using Levenberg-Marquardt: 0.00000 New wR= 0.04807 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.03601 Rint for all data: 0.17021 with corrections 0.03622 0 observations identified as outliers and rejected Cycle 5 wR= 0.04807 Using Levenberg-Marquardt: 0.00000 New wR= 0.04801 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17010 with corrections 0.03600 Rint for all data: 0.17021 with corrections 0.03622 0 observations identified as outliers and rejected Final wR= 0.04801 Final frame scales: Min= 0.8265 Max= 1.1935 Final absorption correction factors: Amin= 0.6562 Amax= 1.5482 PROFFIT INFO: Inet (after scale3 abspack): min=491.3714 max=5591335.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=165.9026 max=66591.2422 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3155 reflections read from tmp file 447 reflections are rejected (446 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 7 1 3 3 1 6 8 10 115 Initial Chi^2= 0.34213 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.02743 Current error model SIG(F2)^2 = 121.78*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 246.90*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 246.90*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5591336- 1575445 315 2338113.96 89.86 100.00 1575160- 985700 315 1230193.99 44.79 100.00 984198- 326040 315 595809.14 43.77 100.00 325070- 202085 315 245718.48 29.25 100.00 202042- 168119 315 183694.95 20.50 100.00 167943- 125642 315 141894.35 15.14 100.00 125624- 99848 315 112823.66 12.79 100.00 99535- 5712 315 57107.83 9.33 95.56 5708- 3431 315 4308.79 2.98 36.51 3422- 491 320 2640.02 2.33 14.06 ------------------------------------------------------------------------------------ 5591336- 491 3155 490456.21 27.03 84.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 906091.65 60.18 98.73 1.41- 1.12 315 775426.13 41.07 93.65 1.12- 0.96 315 629562.49 34.13 91.11 0.96- 0.88 315 466565.07 25.29 83.49 0.88- 0.81 315 612317.38 29.21 93.97 0.81- 0.74 315 315972.77 17.49 77.14 0.74- 0.71 315 264706.22 15.89 78.10 0.71- 0.65 315 475826.40 21.61 90.16 0.65- 0.62 315 235264.83 12.80 66.35 0.62- 0.58 320 227010.79 12.87 72.50 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 490456.21 27.03 84.50 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 906091.65 60.18 98.73 4.82- 1.12 630 840758.89 50.63 96.19 4.82- 0.96 945 770360.09 45.13 94.50 4.82- 0.88 1260 694411.34 40.17 91.75 4.82- 0.81 1575 677992.54 37.98 92.19 4.82- 0.74 1890 617655.91 34.56 89.68 4.82- 0.71 2205 567234.53 31.90 88.03 4.82- 0.65 2520 555808.51 30.61 88.29 4.82- 0.62 2835 520192.55 28.63 85.86 4.82- 0.58 3155 490456.21 27.03 84.50 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 490456.21 27.03 84.50 Scale applied to data: s=0.178848 (maximum obs:5591335.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.036; Rsigma 0.024: data 3155 -> merged 156 With outlier rejection... Rint 0.033; Rsigma 0.024: data 3135 -> merged 156 Rejected total: 20, method kkm 12, method Blessing 8 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585733, 4.830080 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 17.93 100.00 251 1.41 - 1.12 14 14 25.79 100.00 361 1.12 - 0.97 14 14 25.93 100.00 363 0.96 - 0.84 14 14 28.07 100.00 393 0.84 - 0.78 14 14 20.71 100.00 290 0.78 - 0.73 14 14 22.14 100.00 310 0.73 - 0.69 14 14 21.07 100.00 295 0.69 - 0.66 14 14 18.00 100.00 252 0.65 - 0.63 14 14 19.00 100.00 266 0.63 - 0.60 14 14 17.64 100.00 247 --------------------------------------------------------------- 8.36 - 0.60 140 140 21.63 100.00 3028 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:16:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.365624 8.374927 8.357305 90.1101 89.9671 90.0070 3135 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1601 0 2103 2102 3135 N (int>3sigma) = 0 0 0 0 1601 0 1779 1789 2646 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 85.9 85.3 85.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.9 0.0 26.7 26.3 26.5 Lattice type: F chosen Volume: 585.52 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.929 b.b = 34.937 c.c = 34.977 b.c = -0.035 a.c = -17.435 a.b = -17.420 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.141 CUBIC F-lattice R(int) = 0.033 [ 2979] Vol = 585.5 Cell: 8.366 8.375 8.357 90.11 89.97 90.01 Volume: 585.52 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 2701] Vol = 439.1 Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.14 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.033 [ 863] Vol = 439.1 Trigonal Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.14 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.032 [ 2734] Vol = 292.8 Cell: 5.919 5.918 8.357 89.95 89.90 89.94 Volume: 292.76 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.147 TETRAGONAL I-lattice R(int) = 0.032 [ 2734] Vol = 292.8 Cell: 5.918 5.919 8.357 90.10 90.05 89.94 Volume: 292.76 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.072 ORTHORHOMBIC I-lattice R(int) = 0.032 [ 2681] Vol = 292.8 Cell: 5.918 5.919 8.357 89.90 89.95 89.94 Volume: 292.76 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 2678] Vol = 292.8 Cell: 5.910 8.366 5.921 89.97 89.88 90.02 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.031 [ 2337] Vol = 292.8 Cell: 5.919 5.918 8.357 90.05 90.10 89.94 Volume: 292.76 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.115 MONOCLINIC I-lattice R(int) = 0.030 [ 2336] Vol = 292.8 Cell: 5.910 5.921 8.366 90.03 90.02 90.12 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.027 [ 2355] Vol = 292.8 Cell: 5.910 8.366 5.921 89.97 90.12 89.98 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.053 MONOCLINIC I-lattice R(int) = 0.030 [ 2335] Vol = 292.8 Cell: 5.921 5.910 8.366 89.98 90.03 89.88 Volume: 292.76 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.104 MONOCLINIC C-lattice R(int) = 0.029 [ 2337] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.91 Volume: 292.76 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.025 [ 1694] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.38 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1601 0 2103 2102 3135 N (int>3sigma) = 0 0 0 0 1601 0 1779 1789 2646 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 85.9 85.3 85.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.9 0.0 26.7 26.3 26.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.171 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 31 31 249 700 N I>3s 17 17 116 700 0.7 0.7 0.7 39.4 5.3 5.3 3.4 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.033 2750 Fd-3m 1 1 227 C N N N N 37 2284 0.033 2789 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365624 8.374927 8.357305 90.1101 89.9671 90.0070 ZERR 3.00 0.000447 0.000638 0.000609 0.0060 0.0052 0.0053 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5363680- 1152049 509 495 26 19.0 1919154.45 72.14 0.027 0.035 1151237- 287370 491 487 26 18.7 681038.20 42.39 0.043 0.058 282692- 137725 716 715 26 27.5 195908.33 21.95 0.036 0.048 133709- 100502 513 513 26 19.7 119444.38 13.18 0.054 0.071 98924- 4037 468 467 26 18.0 35429.27 6.72 0.065 0.083 3962- 1897 458 458 26 17.6 3185.31 2.58 0.193 0.234 ------------------------------------------------------------------------------------------- 5363680- 1897 3155 3135 156 20.1 478788.14 26.51 0.033 0.043 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 588 577 26 22.2 702852.75 46.52 0.031 0.036 0.013 1.12-0.88 705 703 26 27.0 623708.39 32.20 0.027 0.036 0.019 0.85-0.75 588 586 26 22.5 462220.80 22.94 0.031 0.042 0.027 0.74-0.68 515 513 26 19.7 402776.22 19.52 0.038 0.046 0.033 0.67-0.63 501 501 26 19.3 232068.40 13.70 0.055 0.078 0.046 0.62-0.59 258 255 26 9.8 247983.99 13.03 0.046 0.054 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 3155 3135 156 20.1 478788.14 26.51 0.033 0.043 0.024 inf-0.60 3045 3026 139 21.8 488887.05 27.03 0.033 0.042 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 577 26 26 100.0 22.2 702852.75 217.11 0.031 0.003 1.12-0.88 703 26 26 100.0 27.0 623708.39 163.94 0.027 0.004 0.85-0.75 586 26 26 100.0 22.5 462220.80 113.00 0.031 0.006 0.74-0.68 513 26 26 100.0 19.7 402776.22 88.26 0.038 0.008 0.67-0.63 501 26 26 100.0 19.3 232068.40 59.53 0.055 0.010 0.62-0.59 255 27 26 96.3 9.8 247983.99 46.90 0.046 0.018 -------------------------------------------------------------------------------------------- inf-0.59 3135 157 156 99.4 20.1 478788.14 125.61 0.033 0.006 inf-0.60 3026 139 139 100.0 21.8 488887.05 128.90 0.033 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007476 0.076829 -0.034769 ( 0.000006 0.000007 0.000006 ) -0.083576 -0.011781 -0.008053 ( 0.000004 0.000005 0.000004 ) -0.012170 0.033637 0.077003 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007476 0.076829 -0.034769 ( 0.000006 0.000007 0.000006 ) -0.083576 -0.011781 -0.008053 ( 0.000004 0.000005 0.000004 ) -0.012170 0.033637 0.077003 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3656(4) 8.3749(6) 8.3573(6) 90.110(6) 89.967(5) 90.007(5) V = 585.52(7) unit cell: 8.36595(15) 8.36595(15) 8.36595(15) 90.0 90.0 90.0 V = 585.525(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.956) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.956) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.956) Run 6 Omega scan: (3.000 - 32.000,29 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.928) PROFFIT INFO: signal sum: min=68.0000 max=22692716.0000 PROFFIT INFO: signal sum lp corr: min=222.3350 max=3262864.4285 PROFFIT INFO: background sum: min=736.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10944.0000 PROFFIT INFO: num of signal pixels: min=59 max=879 PROFFIT INFO: Inet: min=485.0947 max=7118977.5000 PROFFIT INFO: sig(Inet): min=187.9576 max=63744.1094 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=309.53 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 146 488 826 1316 1442 2576 4198 5730 6310 Percent 0.0 0.1 2.3 7.7 13.1 20.9 22.9 40.8 66.5 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3155 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 3155 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7118978- 1583700 315 2394747.04 134.50 100.00 1579488- 1030570 315 1285583.53 110.02 100.00 1026917- 309368 315 596511.81 94.29 100.00 309081- 215760 315 252334.31 68.68 100.00 215623- 163404 315 186573.57 48.55 100.00 163304- 130169 315 146253.86 37.56 100.00 130037- 100514 315 114921.14 30.15 100.00 100420- 6074 315 55950.18 20.63 100.00 6046- 3525 315 4545.67 4.92 83.17 3525- 485 320 2627.75 3.14 40.31 ------------------------------------------------------------------------------------ 7118978- 485 3155 503210.31 55.16 92.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 861475.89 87.88 100.00 1.41- 1.12 315 758845.02 70.56 98.41 1.12- 0.96 315 672228.59 75.72 99.05 0.96- 0.88 315 480394.47 59.86 94.92 0.88- 0.81 315 642843.83 69.59 97.46 0.81- 0.74 315 339450.95 40.84 93.65 0.74- 0.71 315 276509.32 37.11 90.16 0.71- 0.65 315 509751.49 51.21 95.24 0.65- 0.62 315 251847.25 29.47 73.65 0.62- 0.58 320 242888.39 29.77 80.31 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 503210.31 55.16 92.27 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:16:12 2018 Sorting 3155 observations 86 unique observations with > 7.00 F2/sig(F2) 3155 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 27 550 Total number of frames 550 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3155 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 3 82 Total number of frames 82 2532 observations > 7.00 F2/sig(F2) 2532 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 3 82 Total number of frames 82 Removing 'redundancy=1' reflections Average redundancy: 28.1 (Out of 2532 removed 5 = 2527, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2527 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 3 82 Total number of frames 82 90 unique data precomputed (should be 90) 90 unique data with 2527 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 28.1 (Out of 2527 removed 0 = 2527, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 2527 observations RMS deviation of equivalent data = 0.20564 Rint = 0.17022 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16941, wR= 0.21832 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08244, wR= 0.10810, Acormin=0.652, Acormax=1.400, Acor_av=0.955 F test: Probability=1.000, F= 4.214 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08078, wR= 0.10168, Acormin=0.618, Acormax=1.387, Acor_av=0.913 F test: Probability=0.834, F= 1.040 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06934, wR= 0.09589, Acormin=0.678, Acormax=1.439, Acor_av=0.957 F test: Probability=1.000, F= 1.408 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06422, wR= 0.08622, Acormin=0.592, Acormax=1.467, Acor_av=0.912 F test: Probability=1.000, F= 1.164 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06156, wR= 0.08260, Acormin=0.555, Acormax=1.384, Acor_av=0.877 F test: Probability=0.978, F= 1.085 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06546, wR= 0.08932, Acormin=0.680, Acormax=1.530, Acor_av=0.924 F test: Probability=0.000, F= 0.883 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06118, wR= 0.08152, Acormin=0.604, Acormax=1.500, Acor_av=0.891 F test: Probability=0.594, F= 1.010 Trying model 8 (ne=6, no=3)... Results: Rint= 0.05769, wR= 0.07775, Acormin=0.575, Acormax=1.432, Acor_av=0.856 F test: Probability=0.999, F= 1.133 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05214, wR= 0.07090, Acormin=0.541, Acormax=1.378, Acor_av=0.819 F test: Probability=1.000, F= 1.218 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06129, wR= 0.07946, Acormin=0.520, Acormax=1.383, Acor_av=0.820 F test: Probability=0.000, F= 0.725 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05889, wR= 0.07696, Acormin=0.544, Acormax=1.405, Acor_av=0.828 F test: Probability=0.000, F= 0.784 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05504, wR= 0.07211, Acormin=0.264, Acormax=0.674, Acor_av=0.404 F test: Probability=0.000, F= 0.895 Trying model 13 (ne=8, no=5)... Results: Rint= 0.04954, wR= 0.06559, Acormin=0.286, Acormax=0.751, Acor_av=0.449 F test: Probability=0.990, F= 1.100 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04603, wR= 0.06205, Acormin=0.285, Acormax=0.804, Acor_av=0.474 F test: Probability=1.000, F= 1.266 Final absorption model (ne=6, no=5): Rint= 0.05214, Acormin=0.541, Acormax=1.378, Acor_av=0.819 Combined refinement in use Rint: 0.17034 There are 82 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: 6, max odd order: 5 (48 parameters) Refinement control: 129 pars with 8385 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20564 Using Levenberg-Marquardt: 0.00010 New wR= 0.05498 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17022 with corrections 0.04237 Rint for all data: 0.17034 with corrections 0.04258 1 observations identified as outliers and rejected Cycle 2 wR= 0.05482 Using Levenberg-Marquardt: 0.00001 New wR= 0.05020 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16971 with corrections 0.03716 Rint for all data: 0.17034 with corrections 0.03752 0 observations identified as outliers and rejected Cycle 3 wR= 0.05020 Using Levenberg-Marquardt: 0.00000 New wR= 0.04977 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16971 with corrections 0.03684 Rint for all data: 0.17034 with corrections 0.03720 0 observations identified as outliers and rejected Cycle 4 wR= 0.04977 Using Levenberg-Marquardt: 0.00000 New wR= 0.04955 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16971 with corrections 0.03666 Rint for all data: 0.17034 with corrections 0.03702 0 observations identified as outliers and rejected Cycle 5 wR= 0.04955 Using Levenberg-Marquardt: 0.00000 New wR= 0.04940 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16971 with corrections 0.03653 Rint for all data: 0.17034 with corrections 0.03688 0 observations identified as outliers and rejected Final wR= 0.04940 Final frame scales: Min= 0.8718 Max= 1.1267 Final absorption correction factors: Amin= 0.6098 Amax= 1.5739 PROFFIT INFO: Inet (after scale3 abspack): min=492.7034 max=5607288.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=165.5531 max=67416.4844 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3155 reflections read from tmp file 464 reflections are rejected (464 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 2 2 4 1 1 3 5 87 Initial Chi^2= 0.32511 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.50612 Current error model SIG(F2)^2 = 121.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 303.47*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 303.47*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5607289- 1578900 315 2340831.15 81.06 100.00 1577503- 994021 315 1228780.58 40.41 100.00 993309- 323877 315 596501.93 39.53 100.00 322488- 201845 315 245917.38 26.40 100.00 201775- 167996 315 183848.80 18.40 100.00 167912- 125735 315 141465.01 13.67 100.00 125720- 99841 315 112815.52 11.52 100.00 99834- 5719 315 57166.62 8.40 93.02 5694- 3434 315 4311.21 2.70 21.59 3417- 493 320 2636.92 2.10 8.13 ------------------------------------------------------------------------------------ 5607289- 493 3155 490652.88 24.38 82.16 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 908581.72 54.29 97.78 1.41- 1.12 315 775849.99 37.05 88.25 1.12- 0.96 315 630485.61 30.78 86.03 0.96- 0.88 315 466766.07 22.82 80.95 0.88- 0.81 315 612400.90 26.35 91.43 0.81- 0.74 315 316536.69 15.77 73.97 0.74- 0.71 315 263777.69 14.33 77.46 0.71- 0.65 315 474980.46 19.50 87.94 0.65- 0.62 315 234689.21 11.55 65.71 0.62- 0.58 320 226651.00 11.61 72.19 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 490652.88 24.38 82.16 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 315 908581.72 54.29 97.78 4.82- 1.12 630 842215.86 45.67 93.02 4.82- 0.96 945 771639.11 40.71 90.69 4.82- 0.88 1260 695420.85 36.23 88.25 4.82- 0.81 1575 678816.86 34.26 88.89 4.82- 0.74 1890 618436.83 31.18 86.40 4.82- 0.71 2205 567771.24 28.77 85.12 4.82- 0.65 2520 556172.39 27.61 85.48 4.82- 0.62 2835 520452.04 25.83 83.28 4.82- 0.58 3155 490652.88 24.38 82.16 ------------------------------------------------------------------------------------ 4.82- 0.58 3155 490652.88 24.38 82.16 Scale applied to data: s=0.178339 (maximum obs:5607288.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.026: data 3155 -> merged 109 With outlier rejection... Rint 0.034; Rsigma 0.027: data 3138 -> merged 109 Rejected total: 17, method kkm 9, method Blessing 8 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585733, 4.830081 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 18.70 100.00 187 1.61 - 1.21 10 10 28.20 100.00 282 1.17 - 1.01 10 10 37.40 100.00 374 0.99 - 0.89 10 10 37.50 100.00 375 0.88 - 0.81 10 10 35.40 100.00 354 0.81 - 0.74 10 10 30.70 100.00 307 0.73 - 0.71 10 10 33.50 100.00 335 0.70 - 0.66 10 10 28.30 100.00 283 0.66 - 0.64 10 10 26.60 100.00 266 0.63 - 0.60 10 10 26.80 100.00 268 --------------------------------------------------------------- 8.36 - 0.60 100 100 30.31 100.00 3031 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:16:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.365624 8.374927 8.357305 90.1101 89.9671 90.0070 3135 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1601 0 2103 2102 3135 N (int>3sigma) = 0 0 0 0 1601 0 1779 1789 2646 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 85.9 85.3 85.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.9 0.0 26.7 26.3 26.5 Lattice type: F chosen Volume: 585.52 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.929 b.b = 34.937 c.c = 34.977 b.c = -0.035 a.c = -17.435 a.b = -17.420 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.141 CUBIC F-lattice R(int) = 0.033 [ 2979] Vol = 585.5 Cell: 8.366 8.375 8.357 90.11 89.97 90.01 Volume: 585.52 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 2701] Vol = 439.1 Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.14 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.033 [ 863] Vol = 439.1 Trigonal Cell: 5.918 5.911 14.503 90.00 90.08 120.05 Volume: 439.14 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.032 [ 2734] Vol = 292.8 Cell: 5.919 5.918 8.357 89.95 89.90 89.94 Volume: 292.76 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.147 TETRAGONAL I-lattice R(int) = 0.032 [ 2734] Vol = 292.8 Cell: 5.918 5.919 8.357 90.10 90.05 89.94 Volume: 292.76 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.072 ORTHORHOMBIC I-lattice R(int) = 0.032 [ 2681] Vol = 292.8 Cell: 5.918 5.919 8.357 89.90 89.95 89.94 Volume: 292.76 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 2678] Vol = 292.8 Cell: 5.910 8.366 5.921 89.97 89.88 90.02 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.031 [ 2337] Vol = 292.8 Cell: 5.919 5.918 8.357 90.05 90.10 89.94 Volume: 292.76 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.115 MONOCLINIC I-lattice R(int) = 0.030 [ 2336] Vol = 292.8 Cell: 5.910 5.921 8.366 90.03 90.02 90.12 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.027 [ 2355] Vol = 292.8 Cell: 5.910 8.366 5.921 89.97 90.12 89.98 Volume: 292.76 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.053 MONOCLINIC I-lattice R(int) = 0.030 [ 2335] Vol = 292.8 Cell: 5.921 5.910 8.366 89.98 90.03 89.88 Volume: 292.76 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.104 MONOCLINIC C-lattice R(int) = 0.029 [ 2337] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.91 Volume: 292.76 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.025 [ 1694] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.38 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1601 0 2103 2102 3135 N (int>3sigma) = 0 0 0 0 1601 0 1779 1789 2646 Mean intensity = 0.0 0.0 0.0 0.0 33.5 0.0 85.9 85.3 85.6 Mean int/sigma = 0.0 0.0 0.0 0.0 21.9 0.0 26.7 26.3 26.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.171 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 31 31 249 700 N I>3s 17 17 116 700 0.7 0.7 0.7 39.4 5.3 5.3 3.4 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.033 2750 Fd-3m 1 1 227 C N N N N 37 2284 0.033 2789 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.365624 8.374927 8.357305 90.1101 89.9671 90.0070 ZERR 3.00 0.000447 0.000638 0.000609 0.0060 0.0052 0.0053 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5385443- 909910 700 686 27 25.4 1673610.48 56.44 0.031 0.039 897750- 156182 934 932 27 34.5 285639.51 27.18 0.039 0.047 144529- 53041 776 776 27 28.7 112661.42 11.63 0.052 0.069 22145- 1892 745 744 28 26.6 4646.74 2.75 0.155 0.187 ------------------------------------------------------------------------------------------- 5385443- 1892 3155 3138 109 28.8 479667.07 23.94 0.034 0.042 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 790 777 27 28.8 756950.39 41.79 0.032 0.038 0.016 1.01-0.78 962 960 27 35.6 476169.40 22.33 0.030 0.039 0.027 0.78-0.65 800 799 27 29.6 395444.32 17.57 0.039 0.050 0.036 0.65-0.59 603 602 28 21.5 239139.82 11.90 0.049 0.053 0.050 ------------------------------------------------------------------------------------------------------ inf-0.59 3155 3138 109 28.8 479667.07 23.94 0.034 0.042 0.027 inf-0.60 3045 3029 99 30.6 489928.98 24.41 0.034 0.042 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 777 27 27 100.0 28.8 756950.39 230.65 0.032 0.004 1.01-0.78 960 27 27 100.0 35.6 476169.40 136.15 0.030 0.005 0.78-0.65 799 27 27 100.0 29.6 395444.32 101.33 0.039 0.008 0.65-0.59 602 29 28 96.6 21.5 239139.82 62.16 0.049 0.015 -------------------------------------------------------------------------------------------- inf-0.59 3138 110 109 99.1 28.8 479667.07 136.49 0.034 0.006 inf-0.60 3029 99 99 100.0 30.6 489928.98 139.88 0.034 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:19:58 2018) ID: 2932; threads 39; handles 876; mem 519588.00 (1237728.00)kB; time: 1w 5d 23h 25m 29s MEMORY INFO: Memory PF:0.0, Ph:173.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.4,peak PF: 708.5, WS: 271.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:173.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:509.2,peak PF: 708.5, WS: 273.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:19:58 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000007 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000005 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) 8.37051 ( 0.00045 ) 8.37682 ( 0.00064 ) 8.35710 ( 0.00061 ) 90.12473 ( 0.00604 ) 89.98579 ( 0.00523 ) 90.00567 ( 0.00533 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:19:58 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000007 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000005 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007189 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(6) 90.125(6) 89.986(5) 90.006(5) V = 585.98(7) unit cell: 8.36595(15) 8.36595(15) 8.36595(15) 90.0 90.0 90.0 V = 585.525(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 449 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 440 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 440 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.214 ( 0.070) | 1.161 ( 0.152) | 1.248 ( 0.429) | 0.63- 0.59 | 44 | 1.235 ( 0.080) | 1.126 ( 0.210) | 1.257 ( 0.451) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 440 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb PROFFITPEAK info: 546 peaks in the peak location table UB fit with 250 obs out of 262 (total:262,skipped:0) (95.42%) UB - matrix: -0.007340 0.076735 -0.034991 ( 0.000070 0.000072 0.000070 ) -0.083550 -0.011809 -0.007995 ( 0.000043 0.000044 0.000043 ) -0.012149 0.033873 0.076721 ( 0.000034 0.000036 0.000035 ) M - matrix: 0.007182 0.000012 -0.000007 ( 0.000007 0.000007 0.000005 ) 0.000012 0.007175 0.000008 ( 0.000007 0.000011 0.000007 ) -0.000007 0.000008 0.007174 ( 0.000005 0.000007 0.000007 ) unit cell: 8.370(4) 8.374(7) 8.374(4) 90.07(5) 89.94(4) 90.10(5) V = 586.9(6) UB fit with 250 obs out of 262 (total:262,skipped:0) (95.42%) UB - matrix: -0.007340 0.076735 -0.034991 ( 0.000070 0.000072 0.000070 ) -0.083550 -0.011809 -0.007995 ( 0.000043 0.000044 0.000043 ) -0.012149 0.033873 0.076721 ( 0.000034 0.000036 0.000035 ) M - matrix: 0.007182 0.000012 -0.000007 ( 0.000007 0.000007 0.000005 ) 0.000012 0.007175 0.000008 ( 0.000007 0.000011 0.000007 ) -0.000007 0.000008 0.007174 ( 0.000005 0.000007 0.000007 ) unit cell: 8.370(4) 8.374(7) 8.374(4) 90.07(5) 89.94(4) 90.10(5) V = 586.9(6) OTKP changes: 50 1 1 1 No constraint UB - matrix: -0.007262 0.076560 -0.034853 ( 0.000067 0.000069 0.000067 ) -0.083394 -0.011666 -0.007939 ( 0.000045 0.000046 0.000045 ) -0.012096 0.033774 0.076596 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007154 0.000008 -0.000011 ( 0.000008 0.000007 0.000005 ) 0.000008 0.007138 0.000011 ( 0.000007 0.000011 0.000006 ) -0.000011 0.000011 0.007145 ( 0.000005 0.000006 0.000007 ) Constraint UB - matrix: -0.007262 0.076560 -0.034853 ( 0.000067 0.000069 0.000067 ) -0.083394 -0.011666 -0.007939 ( 0.000045 0.000046 0.000045 ) -0.012096 0.033774 0.076596 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007153 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007153 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007153 ( 0.000000 0.000000 0.000002 ) UB fit with 247 obs out of 262 (total:262,skipped:0) (94.27%) unit cell: 8.386(4) 8.395(6) 8.392(4) 90.09(5) 89.91(4) 90.07(5) V = 590.8(6) unit cell: 8.3910(9) 8.3910(9) 8.3910(9) 90.0 90.0 90.0 V = 590.80(11) UB fit with 247 obs out of 262 (total:262,skipped:0) (94.27%) UB - matrix: -0.007262 0.076560 -0.034853 ( 0.000067 0.000069 0.000067 ) -0.083394 -0.011666 -0.007939 ( 0.000045 0.000046 0.000045 ) -0.012096 0.033774 0.076596 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007154 0.000008 -0.000011 ( 0.000008 0.000007 0.000005 ) 0.000008 0.007138 0.000011 ( 0.000007 0.000011 0.000006 ) -0.000011 0.000011 0.007145 ( 0.000005 0.000006 0.000007 ) unit cell: 8.386(4) 8.395(6) 8.392(4) 90.09(5) 89.91(4) 90.07(5) V = 590.8(6) OTKP changes: 50 1 1 1 No constraint UB - matrix: -0.007263 0.076566 -0.034864 ( 0.000067 0.000069 0.000067 ) -0.083401 -0.011669 -0.007941 ( 0.000045 0.000046 0.000045 ) -0.012099 0.033784 0.076602 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007155 0.000008 -0.000011 ( 0.000008 0.000007 0.000005 ) 0.000008 0.007140 0.000011 ( 0.000007 0.000011 0.000006 ) -0.000011 0.000011 0.007146 ( 0.000005 0.000006 0.000007 ) Constraint UB - matrix: -0.007263 0.076566 -0.034864 ( 0.000067 0.000069 0.000067 ) -0.083401 -0.011669 -0.007941 ( 0.000045 0.000046 0.000045 ) -0.012099 0.033784 0.076602 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007154 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007154 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007154 ( 0.000000 0.000000 0.000002 ) UB fit with 247 obs out of 262 (total:262,skipped:0) (94.27%) unit cell: 8.386(4) 8.394(6) 8.390(4) 90.09(5) 89.91(4) 90.07(5) V = 590.6(6) unit cell: 8.3901(9) 8.3901(9) 8.3901(9) 90.0 90.0 90.0 V = 590.61(11) 262 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Run 6 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=53.099) HKL list info: 419 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007263 0.076566 -0.034864 ( 0.000067 0.000069 0.000067 ) -0.083401 -0.011669 -0.007941 ( 0.000045 0.000046 0.000045 ) -0.012099 0.033784 0.076602 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007155 0.000008 -0.000011 ( 0.000008 0.000007 0.000005 ) 0.000008 0.007140 0.000011 ( 0.000007 0.000011 0.000006 ) -0.000011 0.000011 0.007146 ( 0.000005 0.000006 0.000007 ) Constraint UB - matrix: -0.007263 0.076566 -0.034864 ( 0.000067 0.000069 0.000067 ) -0.083401 -0.011669 -0.007941 ( 0.000045 0.000046 0.000045 ) -0.012099 0.033784 0.076602 ( 0.000032 0.000033 0.000032 ) M - matrix: 0.007154 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007154 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007154 ( 0.000000 0.000000 0.000002 ) UB fit with 247 obs out of 262 (total:262,skipped:0) (94.27%) unit cell: 8.386(4) 8.394(6) 8.390(4) 90.09(5) 89.91(4) 90.07(5) V = 590.6(6) unit cell: 8.3901(9) 8.3901(9) 8.3901(9) 90.0 90.0 90.0 V = 590.61(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 248 obs out of 262 (total:262,skipped:0) (94.66%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb 2 of 213 peaks identified as outliers and rejected 211 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 211 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 211 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.87- 1.70 | 21 | 0.962 ( 0.125) | 1.056 ( 0.334) | 1.291 ( 0.837) | 1.60- 1.26 | 21 | 1.051 ( 0.066) | 1.191 ( 0.688) | 1.149 ( 0.518) | 1.17- 1.09 | 21 | 1.083 ( 0.056) | 1.137 ( 0.179) | 0.967 ( 0.255) | 1.02- 0.93 | 21 | 1.093 ( 0.059) | 1.090 ( 0.111) | 1.189 ( 0.450) | 0.93- 0.84 | 21 | 1.139 ( 0.053) | 1.122 ( 0.104) | 1.042 ( 0.272) | 0.84- 0.81 | 21 | 1.140 ( 0.075) | 1.075 ( 0.100) | 0.994 ( 0.374) | 0.78- 0.73 | 21 | 1.164 ( 0.047) | 1.153 ( 0.141) | 1.281 ( 0.366) | 0.72- 0.68 | 21 | 1.170 ( 0.037) | 1.159 ( 0.118) | 1.183 ( 0.396) | 0.68- 0.64 | 21 | 1.182 ( 0.040) | 1.243 ( 0.108) | 1.179 ( 0.395) | 0.64- 0.59 | 22 | 1.159 ( 0.059) | 1.213 ( 0.165) | 1.240 ( 0.400) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.87- 0.59 | 211 | 1.115 ( 0.093) | 1.144 ( 0.275) | 1.152 ( 0.466) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) UB - matrix: -0.007380 0.076847 -0.034846 ( 0.000033 0.000032 0.000032 ) -0.083503 -0.011797 -0.007985 ( 0.000025 0.000024 0.000024 ) -0.012011 0.033702 0.076686 ( 0.000017 0.000016 0.000016 ) M - matrix: 0.007171 0.000013 0.000003 ( 0.000004 0.000003 0.000003 ) 0.000013 0.007180 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000003 0.000001 0.007159 ( 0.000003 0.000003 0.000003 ) unit cell: 8.376(2) 8.371(3) 8.383(2) 90.01(2) 90.02(2) 90.10(3) V = 587.7(3) OTKP changes: 211 1 1 1 No constraint UB - matrix: -0.007282 0.076835 -0.035051 ( 0.000029 0.000028 0.000028 ) -0.083591 -0.011725 -0.008002 ( 0.000022 0.000021 0.000021 ) -0.012112 0.033859 0.076806 ( 0.000014 0.000013 0.000013 ) M - matrix: 0.007187 0.000010 -0.000006 ( 0.000004 0.000003 0.000002 ) 0.000010 0.007187 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000006 0.000001 0.007192 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: -0.007282 0.076835 -0.035051 ( 0.000029 0.000028 0.000028 ) -0.083591 -0.011725 -0.008002 ( 0.000022 0.000021 0.000021 ) -0.012112 0.033859 0.076806 ( 0.000014 0.000013 0.000013 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 8.367(2) 8.366(3) 8.3640(17) 90.01(2) 89.951(19) 90.08(2) V = 585.5(3) unit cell: 8.3657(5) 8.3657(5) 8.3657(5) 90.0 90.0 90.0 V = 585.48(6) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.920) HKL list info: 416 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007282 0.076835 -0.035051 ( 0.000029 0.000028 0.000028 ) -0.083591 -0.011725 -0.008002 ( 0.000022 0.000021 0.000021 ) -0.012112 0.033859 0.076806 ( 0.000014 0.000013 0.000013 ) M - matrix: 0.007187 0.000010 -0.000006 ( 0.000004 0.000003 0.000002 ) 0.000010 0.007187 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000006 0.000001 0.007192 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: -0.007282 0.076835 -0.035051 ( 0.000029 0.000028 0.000028 ) -0.083591 -0.011725 -0.008002 ( 0.000022 0.000021 0.000021 ) -0.012112 0.033859 0.076806 ( 0.000014 0.000013 0.000013 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 8.367(2) 8.366(3) 8.3640(17) 90.01(2) 89.951(19) 90.08(2) V = 585.5(3) unit cell: 8.3657(5) 8.3657(5) 8.3657(5) 90.0 90.0 90.0 V = 585.48(6) 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! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb 2 of 215 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 213 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 213 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.70 | 21 | 0.955 ( 0.136) | 1.062 ( 0.403) | 1.257 ( 0.843) | 1.61- 1.26 | 21 | 1.052 ( 0.058) | 1.105 ( 0.281) | 1.135 ( 0.459) | 1.26- 1.09 | 21 | 1.090 ( 0.060) | 1.134 ( 0.081) | 1.083 ( 0.381) | 1.09- 0.96 | 21 | 1.084 ( 0.062) | 1.067 ( 0.132) | 1.107 ( 0.397) | 0.96- 0.84 | 21 | 1.143 ( 0.053) | 1.113 ( 0.088) | 1.149 ( 0.434) | 0.84- 0.81 | 21 | 1.153 ( 0.069) | 1.105 ( 0.122) | 1.064 ( 0.377) | 0.81- 0.73 | 21 | 1.158 ( 0.061) | 1.147 ( 0.143) | 1.288 ( 0.395) | 0.73- 0.69 | 21 | 1.167 ( 0.040) | 1.124 ( 0.088) | 1.121 ( 0.414) | 0.69- 0.64 | 21 | 1.181 ( 0.035) | 1.253 ( 0.127) | 1.018 ( 0.341) | 0.64- 0.59 | 24 | 1.165 ( 0.060) | 1.221 ( 0.156) | 1.279 ( 0.407) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 213 | 1.116 ( 0.096) | 1.134 ( 0.197) | 1.152 ( 0.473) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 245 | 1.148 ( 0.121) | 1.245 ( 0.391) | 1.325 ( 0.655) | 13.1-18.9 | 245 | 1.132 ( 0.071) | 1.186 ( 0.265) | 1.253 ( 0.556) | 18.9-22.9 | 245 | 1.146 ( 0.090) | 1.197 ( 0.279) | 1.267 ( 0.690) | 23.0-27.2 | 245 | 1.128 ( 0.099) | 1.168 ( 0.297) | 1.211 ( 0.561) | 27.2-30.4 | 245 | 1.137 ( 0.099) | 1.158 ( 0.252) | 1.206 ( 0.456) | 30.4-33.6 | 245 | 1.149 ( 0.103) | 1.144 ( 0.223) | 1.192 ( 0.436) | 33.6-37.0 | 245 | 1.143 ( 0.096) | 1.123 ( 0.164) | 1.167 ( 0.433) | 37.0-39.7 | 245 | 1.143 ( 0.119) | 1.100 ( 0.211) | 1.220 ( 0.498) | 39.7-42.6 | 245 | 1.167 ( 0.105) | 1.106 ( 0.184) | 1.219 ( 0.536) | 42.7-49.8 | 247 | 1.202 ( 0.160) | 1.134 ( 0.277) | 1.175 ( 0.471) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2452 | 1.150 ( 0.111) | 1.156 ( 0.265) | 1.223 ( 0.538) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.96 e2 dimension: a=-0.0010 b=1.02 e3 dimension: a=-0.0025 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:20:28 2018 PROFFITMAIN - Started at Wed Mar 28 14:20:28 2018 OTKP changes: 2442 2 4 6 OTKP changes: 2442 2 4 6 No constraint UB - matrix: -0.007492 0.076875 -0.034787 ( 0.000006 0.000006 0.000006 ) -0.083618 -0.011789 -0.008054 ( 0.000005 0.000004 0.000004 ) -0.012165 0.033664 0.077052 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007196 0.000000 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007182 0.000015 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000015 0.007212 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007492 0.076875 -0.034787 ( 0.000006 0.000006 0.000006 ) -0.083618 -0.011789 -0.008054 ( 0.000005 0.000004 0.000004 ) -0.012165 0.033664 0.077052 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000000 ) UB fit with 2444 obs out of 2452 (total:2452,skipped:0) (99.67%) unit cell: 8.3615(4) 8.3697(6) 8.3523(6) 90.116(6) 89.974(5) 90.002(5) V = 584.51(7) unit cell: 8.36112(15) 8.36112(15) 8.36112(15) 90.0 90.0 90.0 V = 584.512(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007591 0.077004 -0.034683 ( 0.000017 0.000015 0.000011 ) -0.083480 -0.011800 -0.008133 ( 0.000012 0.000010 0.000008 ) -0.012068 0.033521 0.076930 ( 0.000013 0.000012 0.000009 ) M - matrix: 0.007172 -0.000004 0.000014 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007193 0.000004 ( 0.000002 0.000002 0.000001 ) 0.000014 0.000004 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3754(11) 8.3635(13) 8.3666(10) 90.032(11) 90.110(11) 89.968(13) V = 586.06(14) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 No constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007185 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3694(11) 8.3680(13) 8.3657(10) 90.041(11) 90.008(10) 89.973(12) V = 585.89(13) unit cell: 8.3677(4) 8.3677(4) 8.3677(4) 90.0 90.0 90.0 V = 585.89(4) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.965) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007185 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3694(11) 8.3680(13) 8.3657(10) 90.041(11) 90.008(10) 89.973(12) V = 585.89(13) unit cell: 8.3677(4) 8.3677(4) 8.3677(4) 90.0 90.0 90.0 V = 585.89(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007185 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007591 0.076965 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083534 -0.011812 -0.008027 ( 0.000011 0.000010 0.000007 ) -0.012118 0.033492 0.076963 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3694(11) 8.3680(13) 8.3657(10) 90.041(11) 90.008(10) 89.973(12) V = 585.89(13) unit cell: 8.3677(4) 8.3677(4) 8.3677(4) 90.0 90.0 90.0 V = 585.89(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007135 0.076846 -0.034858 ( 0.000017 0.000012 0.000019 ) -0.083551 -0.011646 -0.008034 ( 0.000014 0.000010 0.000015 ) -0.012427 0.033800 0.076707 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007186 0.000005 -0.000033 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007183 0.000008 ( 0.000002 0.000002 0.000002 ) -0.000033 0.000008 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3673(13) 8.3689(14) 8.3805(15) 90.061(14) 89.734(14) 90.038(14) V = 586.84(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007245 0.076717 -0.035020 ( 0.000015 0.000010 0.000016 ) -0.083584 -0.011717 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033945 0.076884 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007192 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007203 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007245 0.076717 -0.035020 ( 0.000015 0.000010 0.000016 ) -0.083584 -0.011717 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033945 0.076884 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3640(13) 8.3737(12) 8.3577(15) 90.142(13) 89.820(13) 90.029(12) V = 585.35(16) unit cell: 8.3651(3) 8.3651(3) 8.3651(3) 90.0 90.0 90.0 V = 585.35(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.965) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007245 0.076717 -0.035020 ( 0.000015 0.000010 0.000016 ) -0.083584 -0.011717 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033945 0.076884 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007192 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007203 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007245 0.076717 -0.035020 ( 0.000015 0.000010 0.000016 ) -0.083584 -0.011717 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033945 0.076884 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3640(13) 8.3737(12) 8.3577(15) 90.142(13) 89.820(13) 90.029(12) V = 585.35(16) unit cell: 8.3651(3) 8.3651(3) 8.3651(3) 90.0 90.0 90.0 V = 585.35(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084679 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084762 0.000096 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084829 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007171 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007185 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007196 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084679 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084762 0.000096 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084829 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3764(16) 8.3681(8) 8.3615(10) 90.064(10) 89.870(13) 90.080(11) V = 586.09(14) unit cell: 8.3687(3) 8.3687(3) 8.3687(3) 90.0 90.0 90.0 V = 586.09(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 438 obs out of 440 (total:440,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083602 -0.011658 -0.008127 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007191 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007170 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3642(9) 8.3764(13) 8.3562(12) 90.036(12) 90.110(11) 89.923(11) V = 585.44(14) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 No constraint UB - matrix: -0.007504 0.076769 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000010 0.000013 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007170 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000013 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076769 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 440 (total:440,skipped:0) (99.77%) unit cell: 8.3639(10) 8.3764(13) 8.3559(12) 90.039(12) 90.107(11) 89.924(11) V = 585.41(14) unit cell: 8.3654(4) 8.3654(4) 8.3654(4) 90.0 90.0 90.0 V = 585.41(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076769 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000010 0.000013 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007170 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000013 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076769 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083604 -0.011658 -0.008131 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 440 (total:440,skipped:0) (99.77%) unit cell: 8.3639(10) 8.3764(13) 8.3559(12) 90.039(12) 90.107(11) 89.924(11) V = 585.41(14) unit cell: 8.3654(4) 8.3654(4) 8.3654(4) 90.0 90.0 90.0 V = 585.41(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 438 obs out of 440 (total:440,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084795 -0.000099 0.000201 ( 0.000009 0.000014 0.000014 ) -0.000001 0.084708 0.000095 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000002 0.084891 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007190 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007207 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084795 -0.000099 0.000201 ( 0.000009 0.000014 0.000014 ) -0.000001 0.084708 0.000095 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000002 0.084891 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 438 obs out of 440 (total:440,skipped:0) (99.55%) unit cell: 8.3649(9) 8.3734(14) 8.3554(9) 90.065(12) 90.132(11) 89.933(11) V = 585.23(13) unit cell: 8.3645(4) 8.3645(4) 8.3645(4) 90.0 90.0 90.0 V = 585.23(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007572 0.077014 -0.034602 ( 0.000015 0.000014 0.000012 ) -0.083444 -0.011879 -0.008149 ( 0.000012 0.000011 0.000009 ) -0.012260 0.033269 0.076976 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007171 0.000000 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000000 0.007179 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3763(11) 8.3714(13) 8.3656(11) 89.943(12) 89.986(11) 90.001(12) V = 586.61(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007189 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3658(11) 8.3694(12) 8.3667(10) 90.004(10) 90.053(10) 90.094(11) V = 585.81(13) unit cell: 8.3673(4) 8.3673(4) 8.3673(4) 90.0 90.0 90.0 V = 585.81(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.965) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007189 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3658(11) 8.3694(12) 8.3667(10) 90.004(10) 90.053(10) 90.094(11) V = 585.81(13) unit cell: 8.3673(4) 8.3673(4) 8.3673(4) 90.0 90.0 90.0 V = 585.81(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007189 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007583 0.077004 -0.034559 ( 0.000013 0.000012 0.000011 ) -0.083566 -0.011975 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076983 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3658(11) 8.3694(12) 8.3667(10) 90.004(10) 90.053(10) 90.094(11) V = 585.81(13) unit cell: 8.3673(4) 8.3673(4) 8.3673(4) 90.0 90.0 90.0 V = 585.81(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 213 obs out of 213 (total:213,skipped:0) (100.00%) UB - matrix: -0.007343 0.076891 -0.035045 ( 0.000027 0.000026 0.000027 ) -0.083622 -0.011769 -0.008026 ( 0.000019 0.000018 0.000019 ) -0.012113 0.033862 0.076809 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007193 0.000009 -0.000002 ( 0.000003 0.000003 0.000002 ) 0.000009 0.007197 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000002 0.000001 0.007192 ( 0.000002 0.000003 0.000003 ) unit cell: 8.3631(19) 8.361(2) 8.3637(19) 90.01(2) 89.984(18) 90.07(2) V = 584.8(2) OTKP changes: 213 1 1 1 No constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007190 0.000008 -0.000004 ( 0.000003 0.000003 0.000002 ) 0.000008 0.007191 0.000002 ( 0.000003 0.000004 0.000003 ) -0.000004 0.000002 0.007192 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 213 obs out of 213 (total:213,skipped:0) (100.00%) unit cell: 8.3648(19) 8.365(2) 8.3639(19) 90.02(2) 89.967(18) 90.07(2) V = 585.2(2) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.20(5) Run 6 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.922) HKL list info: 409 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007190 0.000008 -0.000004 ( 0.000003 0.000003 0.000002 ) 0.000008 0.007191 0.000002 ( 0.000003 0.000004 0.000003 ) -0.000004 0.000002 0.007192 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 213 obs out of 213 (total:213,skipped:0) (100.00%) unit cell: 8.3648(19) 8.365(2) 8.3639(19) 90.02(2) 89.967(18) 90.07(2) V = 585.2(2) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.20(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 213 obs out of 213 (total:213,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007190 0.000008 -0.000004 ( 0.000003 0.000003 0.000002 ) 0.000008 0.007191 0.000002 ( 0.000003 0.000004 0.000003 ) -0.000004 0.000002 0.007192 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: -0.007315 0.076854 -0.035039 ( 0.000026 0.000025 0.000026 ) -0.083607 -0.011730 -0.008016 ( 0.000019 0.000018 0.000019 ) -0.012116 0.033860 0.076811 ( 0.000017 0.000017 0.000017 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 213 obs out of 213 (total:213,skipped:0) (100.00%) unit cell: 8.3648(19) 8.365(2) 8.3639(19) 90.02(2) 89.967(18) 90.07(2) V = 585.2(2) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.20(5) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007471 0.076822 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083572 -0.011775 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033649 0.077000 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007188 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076822 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083572 -0.011775 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033649 0.077000 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 2447 obs out of 2452 (total:2452,skipped:0) (99.80%) unit cell: 8.3662(4) 8.3752(6) 8.3574(6) 90.115(6) 89.968(5) 90.006(5) V = 585.58(7) unit cell: 8.36623(15) 8.36623(15) 8.36623(15) 90.0 90.0 90.0 V = 585.584(18) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 74 reflections under beam stop or inside a detector rejection region 30 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3278 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:20:36 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.965) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.965) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.965) Run 6 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.922) PROFFIT INFO: signal sum: min=36.0000 max=22698252.0000 PROFFIT INFO: signal sum lp corr: min=222.3081 max=3262067.6626 PROFFIT INFO: background sum: min=748.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10956.0000 PROFFIT INFO: num of signal pixels: min=55 max=875 PROFFIT INFO: Inet: min=485.0358 max=7117239.0000 PROFFIT INFO: sig(Inet): min=187.0055 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=308.40 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 72 253 432 683 749 1330 2179 2975 3278 Percent 0.0 0.1 2.2 7.7 13.2 20.8 22.8 40.6 66.5 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3278 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 3278 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117239- 1560377 327 2373028.94 134.51 100.00 1559299- 1023000 327 1278440.76 109.45 100.00 1022488- 308029 327 593914.32 94.28 100.00 306392- 213935 327 250137.23 68.43 100.00 213530- 163061 327 185295.16 49.26 100.00 163014- 130571 327 146083.80 37.70 100.00 130432- 100275 327 115054.39 30.38 100.00 100196- 6083 327 57124.98 20.77 100.00 6070- 3546 327 4563.03 4.87 82.87 3543- 485 335 2629.51 3.17 41.19 ------------------------------------------------------------------------------------ 7117239- 485 3278 499411.84 55.16 92.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 855805.10 88.10 100.00 1.41- 1.12 327 737454.61 70.42 98.47 1.12- 0.96 327 674920.04 76.19 99.08 0.96- 0.88 327 474555.32 59.28 94.50 0.88- 0.81 327 639044.97 69.57 97.55 0.81- 0.74 327 330069.50 40.49 93.27 0.74- 0.71 327 296795.99 38.85 89.91 0.71- 0.65 327 497253.60 49.98 95.72 0.65- 0.62 327 253304.44 29.55 74.01 0.62- 0.58 335 241231.19 29.75 80.60 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 499411.84 55.16 92.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:20:36 2018 Sorting 3278 observations 119 unique observations with > 7.00 F2/sig(F2) 3278 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 48 571 Total number of frames 571 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3278 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 9 116 Total number of frames 116 2630 observations > 7.00 F2/sig(F2) 2630 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 9 116 Total number of frames 116 Removing 'redundancy=1' reflections Average redundancy: 21.0 (Out of 2630 removed 7 = 2623, 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 2623 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 21 44 3 0 19 64 4 0 19 84 5 0 21 106 6 0 9 116 Total number of frames 116 125 unique data precomputed (should be 125) 125 unique data with 2623 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.0 (Out of 2623 removed 0 = 2623, unique = 125) 125 unique data precomputed (should be 125) 125 unique data with 2623 observations RMS deviation of equivalent data = 0.20848 Rint = 0.17337 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17204, wR= 0.22285 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08681, wR= 0.11535, Acormin=0.637, Acormax=1.390, Acor_av=0.954 F test: Probability=1.000, F= 3.920 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08527, wR= 0.10856, Acormin=0.606, Acormax=1.381, Acor_av=0.915 F test: Probability=0.805, F= 1.035 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07360, wR= 0.10270, Acormin=0.681, Acormax=1.443, Acor_av=0.961 F test: Probability=1.000, F= 1.386 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06955, wR= 0.09229, Acormin=0.583, Acormax=1.472, Acor_av=0.918 F test: Probability=0.997, F= 1.118 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06474, wR= 0.08627, Acormin=0.565, Acormax=1.386, Acor_av=0.885 F test: Probability=1.000, F= 1.151 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06891, wR= 0.09298, Acormin=0.668, Acormax=1.552, Acor_av=0.926 F test: Probability=0.000, F= 0.881 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06522, wR= 0.08587, Acormin=0.600, Acormax=1.523, Acor_av=0.897 F test: Probability=0.000, F= 0.983 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06056, wR= 0.08033, Acormin=0.569, Acormax=1.449, Acor_av=0.867 F test: Probability=0.999, F= 1.137 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05372, wR= 0.07231, Acormin=0.537, Acormax=1.386, Acor_av=0.827 F test: Probability=1.000, F= 1.265 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06546, wR= 0.08337, Acormin=0.482, Acormax=1.382, Acor_av=0.820 F test: Probability=0.000, F= 0.675 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06389, wR= 0.08172, Acormin=0.494, Acormax=1.406, Acor_av=0.825 F test: Probability=0.000, F= 0.707 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05895, wR= 0.07518, Acormin=0.241, Acormax=0.635, Acor_av=0.383 F test: Probability=0.000, F= 0.828 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05120, wR= 0.06707, Acormin=0.270, Acormax=0.720, Acor_av=0.434 F test: Probability=0.986, F= 1.093 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04755, wR= 0.06341, Acormin=0.273, Acormax=0.771, Acor_av=0.459 F test: Probability=1.000, F= 1.259 Final absorption model (ne=6, no=5): Rint= 0.05372, Acormin=0.537, Acormax=1.386, Acor_av=0.827 Combined refinement in use Rint: 0.17347 There are 116 active scales (one needs to be fixed) Refinement control: frame scale #111 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20848 Using Levenberg-Marquardt: 0.00010 New wR= 0.05290 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17337 with corrections 0.04071 Rint for all data: 0.17347 with corrections 0.04092 1 observations identified as outliers and rejected Cycle 2 wR= 0.05277 Using Levenberg-Marquardt: 0.00001 New wR= 0.04900 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17304 with corrections 0.03631 Rint for all data: 0.17347 with corrections 0.03670 0 observations identified as outliers and rejected Cycle 3 wR= 0.04900 Using Levenberg-Marquardt: 0.00000 New wR= 0.04825 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17304 with corrections 0.03580 Rint for all data: 0.17347 with corrections 0.03619 0 observations identified as outliers and rejected Cycle 4 wR= 0.04825 Using Levenberg-Marquardt: 0.00000 New wR= 0.04796 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17304 with corrections 0.03569 Rint for all data: 0.17347 with corrections 0.03607 0 observations identified as outliers and rejected Cycle 5 wR= 0.04796 Using Levenberg-Marquardt: 0.00000 New wR= 0.04789 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17304 with corrections 0.03573 Rint for all data: 0.17347 with corrections 0.03611 0 observations identified as outliers and rejected Final wR= 0.04789 Final frame scales: Min= 0.6489 Max= 1.1183 Final absorption correction factors: Amin= 0.4813 Amax= 1.5891 PROFFIT INFO: Inet (after scale3 abspack): min=488.3448 max=5617415.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=161.7700 max=74244.7031 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3278 reflections read from tmp file 483 reflections are rejected (482 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 3 2 1 2 6 9 7 119 Initial Chi^2= 0.35132 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.08968 Current error model SIG(F2)^2 = 115.81*I_RAW + 0.00*I_BACK+(0.01239*)^2 Cycle 2, Chi^2= 1.02126 Current error model SIG(F2)^2 = 87.53*I_RAW + 0.00*I_BACK+(0.01982*)^2 Cycle 3, Chi^2= 1.00174 Current error model SIG(F2)^2 = 99.47*I_RAW + 0.00*I_BACK+(0.01752*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 97.05*I_RAW + 0.00*I_BACK+(0.01812*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 97.05*I_RAW + 0.00*I_BACK+(0.01812*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5617415- 1565379 327 2327203.92 50.62 100.00 1563947- 985873 327 1219027.66 43.33 100.00 982255- 323246 327 591505.07 41.72 100.00 322850- 201345 327 246093.27 34.30 100.00 201248- 167017 327 182815.63 27.77 100.00 166797- 125789 327 141001.36 22.08 100.00 125702- 99701 327 112529.95 19.01 100.00 99540- 5710 327 57651.22 14.25 100.00 5677- 3407 327 4300.83 4.72 99.39 3395- 488 335 2635.71 3.72 74.33 ------------------------------------------------------------------------------------ 5617415- 488 3278 487290.76 26.10 97.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 915448.23 40.45 100.00 1.41- 1.12 327 751287.94 31.82 100.00 1.12- 0.96 327 635620.97 31.04 99.69 0.96- 0.88 327 462436.01 26.13 98.47 0.88- 0.81 327 606152.03 30.71 98.78 0.81- 0.74 327 307391.52 20.75 98.47 0.74- 0.71 327 282812.16 21.07 96.94 0.71- 0.65 327 460837.54 25.03 98.47 0.65- 0.62 327 234464.82 16.80 88.38 0.62- 0.58 335 222924.10 17.37 94.03 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 487290.76 26.10 97.32 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 915448.23 40.45 100.00 4.82- 1.12 654 833368.08 36.13 100.00 4.82- 0.96 981 767452.38 34.43 99.90 4.82- 0.88 1308 691198.29 32.36 99.54 4.82- 0.81 1635 674189.04 32.03 99.39 4.82- 0.74 1962 613056.12 30.15 99.24 4.82- 0.71 2289 565878.41 28.85 98.91 4.82- 0.65 2616 552748.30 28.38 98.85 4.82- 0.62 2943 517383.47 27.09 97.69 4.82- 0.58 3278 487290.76 26.10 97.32 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 487290.76 26.10 97.32 Scale applied to data: s=0.178018 (maximum obs:5617415.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.036; Rsigma 0.025: data 3278 -> merged 156 With outlier rejection... Rint 0.035; Rsigma 0.025: data 3264 -> merged 156 Rejected total: 14, method kkm 12, method Blessing 2 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585753, 4.830244 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 19.21 100.00 269 1.41 - 1.12 14 14 26.86 100.00 376 1.12 - 0.97 14 14 26.93 100.00 377 0.96 - 0.84 14 14 29.14 100.00 408 0.84 - 0.78 14 14 21.79 100.00 305 0.78 - 0.73 14 14 23.00 100.00 322 0.73 - 0.69 14 14 22.00 100.00 308 0.69 - 0.66 14 14 18.57 100.00 260 0.65 - 0.63 14 14 19.93 100.00 279 0.63 - 0.60 14 14 18.14 100.00 254 --------------------------------------------------------------- 8.36 - 0.60 140 140 22.56 100.00 3158 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:20:37 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366158 8.375162 8.357393 90.1145 89.9680 90.0062 3264 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1662 0 2187 2182 3264 N (int>3sigma) = 0 0 0 0 1662 0 2126 2119 3176 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 86.1 86.0 86.3 Mean int/sigma = 0.0 0.0 0.0 0.0 26.7 0.0 26.1 26.1 26.0 Lattice type: F chosen Volume: 585.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.927 b.b = 34.940 c.c = 34.979 b.c = -0.037 a.c = -17.434 a.b = -17.419 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.147 CUBIC F-lattice R(int) = 0.035 [ 3108] Vol = 585.6 Cell: 8.366 8.375 8.357 90.11 89.97 90.01 Volume: 585.58 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.138 RHOMBOHEDRAL R-lattice R(int) = 0.040 [ 2828] Vol = 439.2 Cell: 5.919 5.911 14.504 90.00 90.08 120.05 Volume: 439.19 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.138 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 912] Vol = 439.2 Trigonal Cell: 5.919 5.911 14.504 90.00 90.08 120.05 Volume: 439.19 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.061 TETRAGONAL I-lattice R(int) = 0.034 [ 2862] Vol = 292.8 Cell: 5.919 5.919 8.357 89.94 89.90 89.94 Volume: 292.79 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.148 TETRAGONAL I-lattice R(int) = 0.034 [ 2862] Vol = 292.8 Cell: 5.919 5.919 8.357 90.10 90.06 89.94 Volume: 292.79 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.075 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 2808] Vol = 292.8 Cell: 5.919 5.919 8.357 89.90 89.94 89.94 Volume: 292.79 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.066 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 2805] Vol = 292.8 Cell: 5.910 8.366 5.922 89.97 89.88 90.02 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.032 [ 2465] Vol = 292.8 Cell: 5.919 5.919 8.357 90.06 90.10 89.94 Volume: 292.79 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.115 MONOCLINIC I-lattice R(int) = 0.032 [ 2463] Vol = 292.8 Cell: 5.910 5.922 8.366 90.03 90.02 90.12 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC I-lattice R(int) = 0.029 [ 2481] Vol = 292.8 Cell: 5.910 8.366 5.922 89.97 90.12 89.98 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.054 MONOCLINIC I-lattice R(int) = 0.032 [ 2463] Vol = 292.8 Cell: 8.366 5.910 5.922 90.12 90.03 90.02 Volume: 292.79 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.110 MONOCLINIC C-lattice R(int) = 0.030 [ 2464] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.90 Volume: 292.79 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.027 [ 1817] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.40 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1662 0 2187 2182 3264 N (int>3sigma) = 0 0 0 0 1662 0 2126 2119 3176 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 86.1 86.0 86.3 Mean int/sigma = 0.0 0.0 0.0 0.0 26.7 0.0 26.1 26.1 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 261 724 N I>3s 28 28 244 724 0.7 0.7 0.7 39.0 8.0 8.0 5.3 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 2867 Fd-3m 1 1 227 C N N N N 37 2284 0.036 2906 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366158 8.375162 8.357393 90.1145 89.9680 90.0062 ZERR 3.00 0.000441 0.000616 0.000595 0.0059 0.0051 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5365037- 1151499 525 521 26 20.0 1938943.69 48.29 0.031 0.042 1136188- 284915 517 513 26 19.7 676646.83 41.45 0.042 0.053 283265- 135702 751 749 26 28.8 194128.91 28.65 0.035 0.047 132177- 99854 524 524 26 20.2 118262.28 19.58 0.051 0.066 98629- 3971 489 486 26 18.7 34690.66 10.17 0.062 0.076 3923- 1931 472 471 26 18.1 3159.38 4.09 0.194 0.236 ------------------------------------------------------------------------------------------- 5365037- 1931 3278 3264 156 20.9 484996.69 26.04 0.035 0.046 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 614 609 26 23.4 746402.43 35.12 0.039 0.050 0.020 1.12-0.88 733 732 26 28.2 613683.12 29.84 0.028 0.036 0.023 0.85-0.75 609 607 26 23.3 463797.14 25.25 0.029 0.040 0.026 0.74-0.68 537 535 26 20.6 398496.40 23.28 0.038 0.045 0.028 0.67-0.63 522 522 26 20.1 228376.65 18.24 0.052 0.068 0.035 0.62-0.59 263 259 26 10.0 252204.77 17.28 0.046 0.048 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 3278 3264 156 20.9 484996.69 26.04 0.035 0.046 0.025 inf-0.60 3166 3156 139 22.7 495222.35 26.38 0.035 0.046 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 609 26 26 100.0 23.4 746402.43 185.78 0.039 0.006 1.12-0.88 732 26 26 100.0 28.2 613683.12 161.33 0.028 0.005 0.85-0.75 607 26 26 100.0 23.3 463797.14 129.40 0.029 0.005 0.74-0.68 535 26 26 100.0 20.6 398496.40 108.77 0.038 0.007 0.67-0.63 522 26 26 100.0 20.1 228376.65 81.80 0.052 0.008 0.62-0.59 259 26 26 100.0 10.0 252204.77 64.11 0.046 0.014 -------------------------------------------------------------------------------------------- inf-0.59 3264 156 156 100.0 20.9 484996.69 130.91 0.035 0.007 inf-0.60 3156 139 139 100.0 22.7 495222.35 133.80 0.035 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007471 0.076822 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083571 -0.011775 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033649 0.077000 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007188 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076822 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083571 -0.011775 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033649 0.077000 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3662(4) 8.3752(6) 8.3574(6) 90.115(6) 89.968(5) 90.006(5) V = 585.58(7) unit cell: 8.36623(15) 8.36623(15) 8.36623(15) 90.0 90.0 90.0 V = 585.585(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: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.965) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.965) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.965) Run 6 Omega scan: (3.000 - 53.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.922) PROFFIT INFO: signal sum: min=36.0000 max=22698252.0000 PROFFIT INFO: signal sum lp corr: min=222.3081 max=3262067.6626 PROFFIT INFO: background sum: min=748.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=600.0000 max=10956.0000 PROFFIT INFO: num of signal pixels: min=55 max=875 PROFFIT INFO: Inet: min=485.0358 max=7117239.0000 PROFFIT INFO: sig(Inet): min=187.0055 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=308.40 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 144 506 864 1366 1498 2660 4358 5950 6556 Percent 0.0 0.1 2.2 7.7 13.2 20.8 22.8 40.6 66.5 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3278 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 3278 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117239- 1560377 327 2373028.94 134.51 100.00 1559299- 1023000 327 1278440.76 109.45 100.00 1022488- 308029 327 593914.32 94.28 100.00 306392- 213935 327 250137.23 68.43 100.00 213530- 163061 327 185295.16 49.26 100.00 163014- 130571 327 146083.80 37.70 100.00 130432- 100275 327 115054.39 30.38 100.00 100196- 6083 327 57124.98 20.77 100.00 6070- 3546 327 4563.03 4.87 82.87 3543- 485 335 2629.51 3.17 41.19 ------------------------------------------------------------------------------------ 7117239- 485 3278 499411.84 55.16 92.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 855805.10 88.10 100.00 1.41- 1.12 327 737454.61 70.42 98.47 1.12- 0.96 327 674920.04 76.19 99.08 0.96- 0.88 327 474555.32 59.28 94.50 0.88- 0.81 327 639044.97 69.57 97.55 0.81- 0.74 327 330069.50 40.49 93.27 0.74- 0.71 327 296795.99 38.85 89.91 0.71- 0.65 327 497253.60 49.98 95.72 0.65- 0.62 327 253304.44 29.55 74.01 0.62- 0.58 335 241231.19 29.75 80.60 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 499411.84 55.16 92.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:20:38 2018 Sorting 3278 observations 86 unique observations with > 7.00 F2/sig(F2) 3278 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 48 571 Total number of frames 571 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3278 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 6 85 Total number of frames 85 2630 observations > 7.00 F2/sig(F2) 2630 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 6 85 Total number of frames 85 Removing 'redundancy=1' reflections Average redundancy: 29.2 (Out of 2630 removed 5 = 2625, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2625 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 6 85 Total number of frames 85 90 unique data precomputed (should be 90) 90 unique data with 2625 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 29.2 (Out of 2625 removed 0 = 2625, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 2625 observations RMS deviation of equivalent data = 0.20894 Rint = 0.17349 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17214, wR= 0.22333 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08731, wR= 0.11628, Acormin=0.637, Acormax=1.386, Acor_av=0.954 F test: Probability=1.000, F= 3.880 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08546, wR= 0.10916, Acormin=0.605, Acormax=1.378, Acor_av=0.914 F test: Probability=0.852, F= 1.043 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07434, wR= 0.10481, Acormin=0.686, Acormax=1.427, Acor_av=0.959 F test: Probability=1.000, F= 1.374 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07062, wR= 0.09423, Acormin=0.582, Acormax=1.460, Acor_av=0.916 F test: Probability=0.995, F= 1.107 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06546, wR= 0.08765, Acormin=0.563, Acormax=1.372, Acor_av=0.881 F test: Probability=1.000, F= 1.161 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07000, wR= 0.09610, Acormin=0.669, Acormax=1.535, Acor_av=0.925 F test: Probability=0.000, F= 0.873 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06702, wR= 0.08874, Acormin=0.589, Acormax=1.502, Acor_av=0.895 F test: Probability=0.000, F= 0.952 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06145, wR= 0.08259, Acormin=0.570, Acormax=1.431, Acor_av=0.863 F test: Probability=0.999, F= 1.129 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05422, wR= 0.07335, Acormin=0.537, Acormax=1.370, Acor_av=0.823 F test: Probability=1.000, F= 1.279 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06666, wR= 0.08545, Acormin=0.478, Acormax=1.370, Acor_av=0.814 F test: Probability=0.000, F= 0.663 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06512, wR= 0.08393, Acormin=0.486, Acormax=1.386, Acor_av=0.818 F test: Probability=0.000, F= 0.693 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05961, wR= 0.07656, Acormin=0.233, Acormax=0.610, Acor_av=0.370 F test: Probability=0.000, F= 0.825 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05136, wR= 0.06761, Acormin=0.265, Acormax=0.705, Acor_av=0.427 F test: Probability=0.994, F= 1.107 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04781, wR= 0.06399, Acormin=0.268, Acormax=0.756, Acor_av=0.452 F test: Probability=1.000, F= 1.270 Final absorption model (ne=6, no=5): Rint= 0.05422, Acormin=0.537, Acormax=1.370, Acor_av=0.823 Combined refinement in use Rint: 0.17360 There are 85 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: 6, max odd order: 5 (48 parameters) Refinement control: 132 pars with 8778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.20894 Using Levenberg-Marquardt: 0.00010 New wR= 0.05544 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17349 with corrections 0.04262 Rint for all data: 0.17360 with corrections 0.04283 1 observations identified as outliers and rejected Cycle 2 wR= 0.05529 Using Levenberg-Marquardt: 0.00001 New wR= 0.05136 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17308 with corrections 0.03848 Rint for all data: 0.17360 with corrections 0.03883 0 observations identified as outliers and rejected Cycle 3 wR= 0.05136 Using Levenberg-Marquardt: 0.00000 New wR= 0.05078 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17308 with corrections 0.03805 Rint for all data: 0.17360 with corrections 0.03840 0 observations identified as outliers and rejected Cycle 4 wR= 0.05078 Using Levenberg-Marquardt: 0.00000 New wR= 0.05048 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17308 with corrections 0.03783 Rint for all data: 0.17360 with corrections 0.03817 0 observations identified as outliers and rejected Cycle 5 wR= 0.05048 Using Levenberg-Marquardt: 0.00000 New wR= 0.05029 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17308 with corrections 0.03769 Rint for all data: 0.17360 with corrections 0.03803 0 observations identified as outliers and rejected Final wR= 0.05029 Final frame scales: Min= 0.7938 Max= 1.1359 Final absorption correction factors: Amin= 0.5552 Amax= 1.5145 PROFFIT INFO: Inet (after scale3 abspack): min=486.5052 max=5694324.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=163.3539 max=76456.7422 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3278 reflections read from tmp file 513 reflections are rejected (513 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 1 3 3 2 3 2 89 Initial Chi^2= 0.33192 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.08312 Current error model SIG(F2)^2 = 112.12*I_RAW + 0.00*I_BACK+(0.01335*)^2 Cycle 2, Chi^2= 1.02090 Current error model SIG(F2)^2 = 85.58*I_RAW + 0.00*I_BACK+(0.01994*)^2 Cycle 3, Chi^2= 1.00254 Current error model SIG(F2)^2 = 98.71*I_RAW + 0.00*I_BACK+(0.01752*)^2 Cycle 4, Chi^2= 1.00013 Current error model SIG(F2)^2 = 95.12*I_RAW + 0.00*I_BACK+(0.01833*)^2 Cycle 5, Chi^2= 1.00007 Current error model SIG(F2)^2 = 96.42*I_RAW + 0.00*I_BACK+(0.01806*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 95.99*I_RAW + 0.00*I_BACK+(0.01815*)^2 Cycle 7, Chi^2= 1.00001 Current error model SIG(F2)^2 = 96.14*I_RAW + 0.00*I_BACK+(0.01812*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 96.14*I_RAW + 0.00*I_BACK+(0.01812*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5694324- 1556449 327 2324589.19 50.66 100.00 1554203- 986857 327 1218625.93 43.43 100.00 986810- 321169 327 592375.54 41.77 100.00 320861- 201067 327 245985.00 34.39 100.00 200974- 167029 327 182747.54 27.88 100.00 166744- 125061 327 141018.31 22.18 100.00 125056- 99650 327 112378.85 19.09 100.00 99642- 5685 327 57964.68 14.29 100.00 5685- 3420 327 4310.78 4.75 99.69 3409- 487 335 2636.00 3.73 74.63 ------------------------------------------------------------------------------------ 5694324- 487 3278 487078.00 26.16 97.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 914208.64 40.51 100.00 1.41- 1.12 327 751421.86 31.88 100.00 1.12- 0.96 327 635216.96 31.11 99.69 0.96- 0.88 327 461392.49 26.20 98.47 0.88- 0.81 327 605528.45 30.79 98.78 0.81- 0.74 327 307525.00 20.82 98.47 0.74- 0.71 327 282589.50 21.15 96.94 0.71- 0.65 327 460585.05 25.11 98.78 0.65- 0.62 327 235374.88 16.85 88.38 0.62- 0.58 335 223388.31 17.43 94.33 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 487078.00 26.16 97.38 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 327 914208.64 40.51 100.00 4.82- 1.12 654 832815.25 36.20 100.00 4.82- 0.96 981 766949.15 34.50 99.90 4.82- 0.88 1308 690559.99 32.43 99.54 4.82- 0.81 1635 673553.68 32.10 99.39 4.82- 0.74 1962 612548.90 30.22 99.24 4.82- 0.71 2289 565411.84 28.92 98.91 4.82- 0.65 2616 552308.49 28.44 98.89 4.82- 0.62 2943 517093.65 27.16 97.72 4.82- 0.58 3278 487078.00 26.16 97.38 ------------------------------------------------------------------------------------ 4.82- 0.58 3278 487078.00 26.16 97.38 Scale applied to data: s=0.175613 (maximum obs:5694324.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.038; Rsigma 0.025: data 3278 -> merged 109 With outlier rejection... Rint 0.037; Rsigma 0.025: data 3268 -> merged 109 Rejected total: 10, method kkm 9, method Blessing 1 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585753, 4.830246 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 19.80 100.00 198 1.61 - 1.21 10 10 30.30 100.00 303 1.17 - 1.01 10 10 38.80 100.00 388 0.99 - 0.89 10 10 38.80 100.00 388 0.88 - 0.81 10 10 37.00 100.00 370 0.81 - 0.74 10 10 31.70 100.00 317 0.73 - 0.71 10 10 35.10 100.00 351 0.70 - 0.66 10 10 28.90 100.00 289 0.66 - 0.64 10 10 28.20 100.00 282 0.63 - 0.60 10 10 27.40 100.00 274 --------------------------------------------------------------- 8.36 - 0.60 100 100 31.60 100.00 3160 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:20:37 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366158 8.375162 8.357393 90.1145 89.9680 90.0062 3264 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1662 0 2187 2182 3264 N (int>3sigma) = 0 0 0 0 1662 0 2126 2119 3176 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 86.1 86.0 86.3 Mean int/sigma = 0.0 0.0 0.0 0.0 26.7 0.0 26.1 26.1 26.0 Lattice type: F chosen Volume: 585.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.914 90.06 119.92 119.91 Niggli form: a.a = 34.927 b.b = 34.940 c.c = 34.979 b.c = -0.037 a.c = -17.434 a.b = -17.419 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.147 CUBIC F-lattice R(int) = 0.035 [ 3108] Vol = 585.6 Cell: 8.366 8.375 8.357 90.11 89.97 90.01 Volume: 585.58 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.138 RHOMBOHEDRAL R-lattice R(int) = 0.040 [ 2828] Vol = 439.2 Cell: 5.919 5.911 14.504 90.00 90.08 120.05 Volume: 439.19 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.138 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 912] Vol = 439.2 Trigonal Cell: 5.919 5.911 14.504 90.00 90.08 120.05 Volume: 439.19 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.061 TETRAGONAL I-lattice R(int) = 0.034 [ 2862] Vol = 292.8 Cell: 5.919 5.919 8.357 89.94 89.90 89.94 Volume: 292.79 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.148 TETRAGONAL I-lattice R(int) = 0.034 [ 2862] Vol = 292.8 Cell: 5.919 5.919 8.357 90.10 90.06 89.94 Volume: 292.79 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.075 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 2808] Vol = 292.8 Cell: 5.919 5.919 8.357 89.90 89.94 89.94 Volume: 292.79 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.066 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 2805] Vol = 292.8 Cell: 5.910 8.366 5.922 89.97 89.88 90.02 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.040 MONOCLINIC I-lattice R(int) = 0.032 [ 2465] Vol = 292.8 Cell: 5.919 5.919 8.357 90.06 90.10 89.94 Volume: 292.79 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.115 MONOCLINIC I-lattice R(int) = 0.032 [ 2463] Vol = 292.8 Cell: 5.910 5.922 8.366 90.03 90.02 90.12 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC I-lattice R(int) = 0.029 [ 2481] Vol = 292.8 Cell: 5.910 8.366 5.922 89.97 90.12 89.98 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.054 MONOCLINIC I-lattice R(int) = 0.032 [ 2463] Vol = 292.8 Cell: 8.366 5.910 5.922 90.12 90.03 90.02 Volume: 292.79 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.110 MONOCLINIC C-lattice R(int) = 0.030 [ 2464] Vol = 292.8 Cell: 10.246 5.911 5.914 90.06 125.17 89.90 Volume: 292.79 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.027 [ 1817] Vol = 146.4 Cell: 5.910 5.911 5.914 90.06 119.92 119.91 Volume: 146.40 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1662 0 2187 2182 3264 N (int>3sigma) = 0 0 0 0 1662 0 2126 2119 3176 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 86.1 86.0 86.3 Mean int/sigma = 0.0 0.0 0.0 0.0 26.7 0.0 26.1 26.1 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.178 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 261 724 N I>3s 28 28 244 724 0.7 0.7 0.7 39.0 8.0 8.0 5.3 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 2867 Fd-3m 1 1 227 C N N N N 37 2284 0.036 2906 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366158 8.375162 8.357393 90.1145 89.9680 90.0062 ZERR 3.00 0.000441 0.000616 0.000595 0.0059 0.0051 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5440621- 899853 726 722 27 26.7 1681519.82 46.16 0.035 0.046 886055- 154743 975 972 27 36.0 284074.29 33.79 0.040 0.048 143332- 52464 804 803 27 29.7 112020.41 19.26 0.053 0.069 21810- 1931 773 771 28 27.5 4629.52 4.83 0.155 0.187 ------------------------------------------------------------------------------------------- 5440621- 1931 3278 3268 109 30.0 484608.10 26.12 0.037 0.048 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 826 821 27 30.4 779295.03 36.01 0.037 0.048 0.021 1.01-0.78 973 971 27 36.0 483007.10 26.24 0.031 0.042 0.024 0.78-0.65 878 877 28 31.3 372554.40 22.26 0.040 0.050 0.028 0.65-0.59 601 599 27 22.2 247358.82 18.03 0.051 0.053 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 3278 3268 109 30.0 484608.10 26.12 0.037 0.048 0.025 inf-0.60 3166 3158 99 31.9 494863.86 26.46 0.037 0.048 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 821 27 27 100.0 30.4 779295.03 223.30 0.037 0.006 1.01-0.78 971 27 27 100.0 36.0 483007.10 170.22 0.031 0.004 0.78-0.65 877 28 28 100.0 31.3 372554.40 133.33 0.040 0.006 0.65-0.59 599 27 27 100.0 22.2 247358.82 96.49 0.051 0.010 -------------------------------------------------------------------------------------------- inf-0.59 3268 109 109 100.0 30.0 484608.10 160.14 0.037 0.006 inf-0.60 3158 99 99 100.0 31.9 494863.86 163.41 0.037 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:25:25 2018) ID: 2932; threads 39; handles 876; mem 516720.00 (1237728.00)kB; time: 1w 5d 23h 30m 56s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:504.7,peak PF: 708.5, WS: 269.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.5,peak PF: 708.5, WS: 270.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:25:25 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) 8.37051 ( 0.00044 ) 8.37682 ( 0.00062 ) 8.35710 ( 0.00059 ) 90.12473 ( 0.00586 ) 89.98579 ( 0.00514 ) 90.00567 ( 0.00521 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:25:25 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007188 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007203 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(6) 90.125(6) 89.986(5) 90.006(5) V = 585.98(7) unit cell: 8.36623(15) 8.36623(15) 8.36623(15) 90.0 90.0 90.0 V = 585.585(18) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb PROFFITPEAK info: 799 peaks in the peak location table UB fit with 363 obs out of 380 (total:380,skipped:0) (95.53%) UB - matrix: -0.007439 0.076815 -0.035015 ( 0.000046 0.000033 0.000045 ) -0.083550 -0.011795 -0.008020 ( 0.000035 0.000025 0.000035 ) -0.012076 0.033742 0.076833 ( 0.000029 0.000021 0.000029 ) M - matrix: 0.007182 0.000007 0.000003 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007178 -0.000003 ( 0.000004 0.000005 0.000004 ) 0.000003 -0.000003 0.007194 ( 0.000004 0.000004 0.000005 ) unit cell: 8.370(3) 8.372(3) 8.363(3) 89.98(3) 90.02(3) 90.05(3) V = 586.0(4) UB fit with 363 obs out of 380 (total:380,skipped:0) (95.53%) UB - matrix: -0.007439 0.076815 -0.035015 ( 0.000046 0.000033 0.000045 ) -0.083550 -0.011795 -0.008020 ( 0.000035 0.000025 0.000035 ) -0.012076 0.033742 0.076833 ( 0.000029 0.000021 0.000029 ) M - matrix: 0.007182 0.000007 0.000003 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007178 -0.000003 ( 0.000004 0.000005 0.000004 ) 0.000003 -0.000003 0.007194 ( 0.000004 0.000004 0.000005 ) unit cell: 8.370(3) 8.372(3) 8.363(3) 89.98(3) 90.02(3) 90.05(3) V = 586.0(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 No constraint UB - matrix: -0.007399 0.076760 -0.035017 ( 0.000044 0.000032 0.000044 ) -0.083529 -0.011765 -0.007983 ( 0.000035 0.000025 0.000035 ) -0.012086 0.033709 0.076793 ( 0.000028 0.000020 0.000028 ) M - matrix: 0.007178 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007167 -0.000005 ( 0.000004 0.000005 0.000004 ) -0.000002 -0.000005 0.007187 ( 0.000004 0.000004 0.000005 ) Constraint UB - matrix: -0.007399 0.076760 -0.035017 ( 0.000044 0.000032 0.000044 ) -0.083529 -0.011765 -0.007983 ( 0.000035 0.000025 0.000035 ) -0.012086 0.033709 0.076793 ( 0.000028 0.000020 0.000028 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 360 obs out of 380 (total:380,skipped:0) (94.74%) unit cell: 8.372(3) 8.378(3) 8.367(3) 89.96(3) 89.98(3) 90.06(3) V = 586.9(4) unit cell: 8.3724(7) 8.3724(7) 8.3724(7) 90.0 90.0 90.0 V = 586.88(9) UB fit with 360 obs out of 380 (total:380,skipped:0) (94.74%) UB - matrix: -0.007399 0.076760 -0.035017 ( 0.000044 0.000032 0.000044 ) -0.083529 -0.011765 -0.007983 ( 0.000035 0.000025 0.000035 ) -0.012086 0.033709 0.076793 ( 0.000028 0.000020 0.000028 ) M - matrix: 0.007178 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007167 -0.000005 ( 0.000004 0.000005 0.000004 ) -0.000002 -0.000005 0.007187 ( 0.000004 0.000004 0.000005 ) unit cell: 8.372(3) 8.378(3) 8.367(3) 89.96(3) 89.98(3) 90.06(3) V = 586.9(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 380 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Run 6 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.971) HKL list info: 581 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007399 0.076760 -0.035017 ( 0.000044 0.000032 0.000044 ) -0.083529 -0.011765 -0.007983 ( 0.000035 0.000025 0.000035 ) -0.012086 0.033709 0.076793 ( 0.000028 0.000020 0.000028 ) M - matrix: 0.007178 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007167 -0.000005 ( 0.000004 0.000005 0.000004 ) -0.000002 -0.000005 0.007187 ( 0.000004 0.000004 0.000005 ) Constraint UB - matrix: -0.007399 0.076760 -0.035017 ( 0.000044 0.000032 0.000044 ) -0.083529 -0.011765 -0.007983 ( 0.000035 0.000025 0.000035 ) -0.012086 0.033709 0.076793 ( 0.000028 0.000020 0.000028 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 360 obs out of 380 (total:380,skipped:0) (94.74%) unit cell: 8.372(3) 8.378(3) 8.367(3) 89.96(3) 89.98(3) 90.06(3) V = 586.9(4) unit cell: 8.3724(7) 8.3724(7) 8.3724(7) 90.0 90.0 90.0 V = 586.88(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 360 obs out of 380 (total:380,skipped:0) (94.74%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb 5 of 338 peaks identified as outliers and rejected 333 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 333 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 333 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.87- 1.42 | 33 | 0.963 ( 0.126) | 1.022 ( 0.293) | 1.202 ( 0.695) | 1.42- 1.17 | 33 | 1.065 ( 0.063) | 1.157 ( 0.553) | 1.177 ( 0.521) | 1.17- 1.02 | 33 | 1.093 ( 0.058) | 1.077 ( 0.115) | 1.007 ( 0.394) | 1.01- 0.92 | 33 | 1.094 ( 0.078) | 1.070 ( 0.118) | 1.135 ( 0.419) | 0.92- 0.84 | 33 | 1.141 ( 0.062) | 1.102 ( 0.099) | 1.081 ( 0.365) | 0.84- 0.76 | 33 | 1.155 ( 0.077) | 1.103 ( 0.122) | 1.146 ( 0.392) | 0.76- 0.72 | 33 | 1.164 ( 0.038) | 1.100 ( 0.121) | 1.172 ( 0.365) | 0.72- 0.67 | 33 | 1.172 ( 0.035) | 1.117 ( 0.142) | 1.153 ( 0.410) | 0.67- 0.64 | 33 | 1.184 ( 0.047) | 1.142 ( 0.168) | 1.265 ( 0.465) | 0.64- 0.59 | 36 | 1.184 ( 0.061) | 1.108 ( 0.163) | 1.218 ( 0.396) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.87- 0.59 | 333 | 1.122 ( 0.095) | 1.100 ( 0.233) | 1.156 ( 0.457) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 333 obs out of 333 (total:333,skipped:0) (100.00%) UB - matrix: -0.007469 0.076990 -0.034983 ( 0.000020 0.000013 0.000020 ) -0.083624 -0.011890 -0.008022 ( 0.000017 0.000011 0.000016 ) -0.011989 0.033658 0.076854 ( 0.000013 0.000008 0.000013 ) M - matrix: 0.007193 0.000016 0.000011 ( 0.000003 0.000002 0.000002 ) 0.000016 0.007202 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000011 -0.000011 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3636(16) 8.3582(14) 8.3623(13) 89.911(14) 90.085(14) 90.126(15) V = 584.56(17) OTKP changes: 333 1 1 1 OTKP changes: 333 1 1 1 OTKP changes: 333 1 1 1 No constraint UB - matrix: -0.007363 0.076873 -0.035001 ( 0.000018 0.000011 0.000018 ) -0.083532 -0.011752 -0.007994 ( 0.000015 0.000009 0.000014 ) -0.012016 0.033713 0.076874 ( 0.000012 0.000008 0.000012 ) M - matrix: 0.007176 0.000011 0.000002 ( 0.000002 0.000002 0.000002 ) 0.000011 0.007184 -0.000005 ( 0.000002 0.000002 0.000002 ) 0.000002 -0.000005 0.007199 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007363 0.076873 -0.035001 ( 0.000018 0.000011 0.000018 ) -0.083532 -0.011752 -0.007994 ( 0.000015 0.000009 0.000014 ) -0.012016 0.033713 0.076874 ( 0.000012 0.000008 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 333 obs out of 333 (total:333,skipped:0) (100.00%) unit cell: 8.3730(14) 8.3684(13) 8.3600(12) 89.959(12) 90.014(13) 90.084(14) V = 585.77(15) unit cell: 8.3671(3) 8.3671(3) 8.3671(3) 90.0 90.0 90.0 V = 585.77(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.971) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007363 0.076873 -0.035001 ( 0.000018 0.000011 0.000018 ) -0.083532 -0.011752 -0.007994 ( 0.000015 0.000009 0.000014 ) -0.012016 0.033713 0.076874 ( 0.000012 0.000008 0.000012 ) M - matrix: 0.007176 0.000011 0.000002 ( 0.000002 0.000002 0.000002 ) 0.000011 0.007184 -0.000005 ( 0.000002 0.000002 0.000002 ) 0.000002 -0.000005 0.007199 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007363 0.076873 -0.035001 ( 0.000018 0.000011 0.000018 ) -0.083532 -0.011752 -0.007994 ( 0.000015 0.000009 0.000014 ) -0.012016 0.033713 0.076874 ( 0.000012 0.000008 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 333 obs out of 333 (total:333,skipped:0) (100.00%) unit cell: 8.3730(14) 8.3684(13) 8.3600(12) 89.959(12) 90.014(13) 90.084(14) V = 585.77(15) unit cell: 8.3671(3) 8.3671(3) 8.3671(3) 90.0 90.0 90.0 V = 585.77(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 333 obs out of 333 (total:333,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb 2 of 341 peaks identified as outliers and rejected 339 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 339 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 339 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.47 | 34 | 0.976 ( 0.164) | 1.116 ( 0.587) | 1.233 ( 0.753) | 1.41- 1.17 | 34 | 1.058 ( 0.069) | 1.239 ( 0.553) | 1.203 ( 0.528) | 1.17- 1.02 | 34 | 1.097 ( 0.057) | 1.103 ( 0.094) | 1.082 ( 0.422) | 1.02- 0.92 | 34 | 1.094 ( 0.078) | 1.070 ( 0.119) | 1.138 ( 0.430) | 0.92- 0.84 | 34 | 1.142 ( 0.064) | 1.104 ( 0.100) | 1.135 ( 0.423) | 0.84- 0.76 | 34 | 1.149 ( 0.080) | 1.092 ( 0.126) | 1.151 ( 0.385) | 0.76- 0.72 | 34 | 1.163 ( 0.038) | 1.103 ( 0.118) | 1.197 ( 0.399) | 0.72- 0.67 | 34 | 1.174 ( 0.035) | 1.116 ( 0.132) | 1.203 ( 0.455) | 0.67- 0.63 | 34 | 1.186 ( 0.054) | 1.128 ( 0.159) | 1.259 ( 0.458) | 0.63- 0.59 | 33 | 1.185 ( 0.060) | 1.136 ( 0.199) | 1.184 ( 0.397) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 339 | 1.122 ( 0.100) | 1.121 ( 0.286) | 1.178 ( 0.479) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 258 | 1.149 ( 0.121) | 1.249 ( 0.417) | 1.328 ( 0.657) | 13.1-18.9 | 258 | 1.132 ( 0.071) | 1.182 ( 0.259) | 1.250 ( 0.552) | 18.9-23.0 | 258 | 1.145 ( 0.089) | 1.191 ( 0.273) | 1.261 ( 0.680) | 23.0-27.2 | 258 | 1.128 ( 0.099) | 1.182 ( 0.344) | 1.223 ( 0.567) | 27.3-30.4 | 258 | 1.138 ( 0.098) | 1.156 ( 0.248) | 1.197 ( 0.448) | 30.4-33.6 | 258 | 1.147 ( 0.102) | 1.139 ( 0.219) | 1.202 ( 0.438) | 33.7-37.1 | 258 | 1.141 ( 0.097) | 1.115 ( 0.166) | 1.163 ( 0.430) | 37.1-39.8 | 258 | 1.146 ( 0.119) | 1.095 ( 0.211) | 1.224 ( 0.502) | 39.9-42.8 | 258 | 1.160 ( 0.115) | 1.095 ( 0.184) | 1.212 ( 0.526) | 42.8-49.8 | 257 | 1.202 ( 0.155) | 1.128 ( 0.272) | 1.174 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2579 | 1.149 ( 0.110) | 1.153 ( 0.273) | 1.223 ( 0.535) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0026 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:25:56 2018 PROFFITMAIN - Started at Wed Mar 28 14:25:56 2018 OTKP changes: 2566 2 4 6 OTKP changes: 2566 2 4 6 No constraint UB - matrix: -0.007488 0.076879 -0.034792 ( 0.000006 0.000006 0.000006 ) -0.083615 -0.011788 -0.008055 ( 0.000004 0.000004 0.000004 ) -0.012157 0.033667 0.077046 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007195 0.000001 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007183 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000014 0.007211 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007488 0.076879 -0.034792 ( 0.000006 0.000006 0.000006 ) -0.083615 -0.011788 -0.008055 ( 0.000004 0.000004 0.000004 ) -0.012157 0.033667 0.077046 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000000 ) UB fit with 2571 obs out of 2579 (total:2579,skipped:0) (99.69%) unit cell: 8.3619(4) 8.3692(6) 8.3526(6) 90.112(6) 89.979(5) 90.005(5) V = 584.53(7) unit cell: 8.36121(15) 8.36121(15) 8.36121(15) 90.0 90.0 90.0 V = 584.532(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007590 0.077008 -0.034684 ( 0.000017 0.000015 0.000011 ) -0.083482 -0.011799 -0.008137 ( 0.000012 0.000010 0.000008 ) -0.012066 0.033522 0.076931 ( 0.000013 0.000012 0.000009 ) M - matrix: 0.007172 -0.000004 0.000014 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007193 0.000004 ( 0.000002 0.000002 0.000001 ) 0.000014 0.000004 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3752(12) 8.3631(13) 8.3664(10) 90.031(11) 90.114(11) 89.968(13) V = 586.01(14) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 No constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007184 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3697(11) 8.3683(13) 8.3659(10) 90.040(11) 90.008(10) 89.974(12) V = 585.95(13) unit cell: 8.3680(4) 8.3680(4) 8.3680(4) 90.0 90.0 90.0 V = 585.95(4) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007184 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3697(11) 8.3683(13) 8.3659(10) 90.040(11) 90.008(10) 89.974(12) V = 585.95(13) unit cell: 8.3680(4) 8.3680(4) 8.3680(4) 90.0 90.0 90.0 V = 585.95(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007182 -0.000003 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007184 0.000005 ( 0.000002 0.000002 0.000001 ) 0.000001 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007591 0.076961 -0.034658 ( 0.000016 0.000014 0.000011 ) -0.083531 -0.011813 -0.008025 ( 0.000011 0.000010 0.000007 ) -0.012117 0.033492 0.076960 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3697(11) 8.3683(13) 8.3659(10) 90.040(11) 90.008(10) 89.974(12) V = 585.95(13) unit cell: 8.3680(4) 8.3680(4) 8.3680(4) 90.0 90.0 90.0 V = 585.95(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007134 0.076841 -0.034861 ( 0.000017 0.000012 0.000018 ) -0.083548 -0.011644 -0.008035 ( 0.000014 0.000010 0.000015 ) -0.012424 0.033800 0.076706 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007186 0.000005 -0.000033 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007183 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000033 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3677(13) 8.3693(14) 8.3805(15) 90.060(14) 89.737(14) 90.038(14) V = 586.89(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011715 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033944 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011715 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033944 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3739(12) 8.3580(15) 90.141(13) 89.821(13) 90.029(12) V = 585.41(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.41(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011715 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033944 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011715 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033944 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3739(12) 8.3580(15) 90.141(13) 89.821(13) 90.029(12) V = 585.41(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.41(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084676 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084760 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007170 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007184 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007195 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084676 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084760 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3766(16) 8.3684(8) 8.3618(10) 90.063(10) 89.870(13) 90.081(11) V = 586.15(14) unit cell: 8.3689(3) 8.3689(3) 8.3689(3) 90.0 90.0 90.0 V = 586.15(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007572 0.077009 -0.034602 ( 0.000015 0.000014 0.000012 ) -0.083444 -0.011880 -0.008149 ( 0.000012 0.000011 0.000009 ) -0.012258 0.033270 0.076972 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007171 0.000000 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000000 0.007178 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3763(11) 8.3717(13) 8.3660(11) 89.944(12) 89.988(11) 90.003(12) V = 586.66(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 338 obs out of 339 (total:339,skipped:0) (99.71%) UB - matrix: -0.007404 0.076927 -0.035029 ( 0.000021 0.000013 0.000021 ) -0.083565 -0.011781 -0.008009 ( 0.000015 0.000010 0.000015 ) -0.012011 0.033731 0.076884 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007182 0.000010 0.000005 ( 0.000003 0.000002 0.000002 ) 0.000010 0.007194 -0.000007 ( 0.000002 0.000002 0.000002 ) 0.000005 -0.000007 0.007202 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3696(15) 8.3625(15) 8.3579(14) 89.944(15) 90.041(14) 90.078(15) V = 584.97(17) OTKP changes: 338 1 1 1 OTKP changes: 338 1 1 1 OTKP changes: 338 1 1 1 No constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007177 0.000009 0.000000 ( 0.000003 0.000002 0.000002 ) 0.000009 0.007186 -0.000007 ( 0.000002 0.000002 0.000002 ) 0.000000 -0.000007 0.007201 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 339 obs out of 339 (total:339,skipped:0) (100.00%) unit cell: 8.3724(15) 8.3676(15) 8.3586(14) 89.945(15) 90.000(14) 90.075(16) V = 585.58(18) unit cell: 8.3662(4) 8.3662(4) 8.3662(4) 90.0 90.0 90.0 V = 585.58(5) Run 6 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) HKL list info: 570 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007177 0.000009 0.000000 ( 0.000003 0.000002 0.000002 ) 0.000009 0.007186 -0.000007 ( 0.000002 0.000002 0.000002 ) 0.000000 -0.000007 0.007201 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 339 obs out of 339 (total:339,skipped:0) (100.00%) unit cell: 8.3724(15) 8.3676(15) 8.3586(14) 89.945(15) 90.000(14) 90.075(16) V = 585.58(18) unit cell: 8.3662(4) 8.3662(4) 8.3662(4) 90.0 90.0 90.0 V = 585.58(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 339 obs out of 339 (total:339,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007177 0.000009 0.000000 ( 0.000003 0.000002 0.000002 ) 0.000009 0.007186 -0.000007 ( 0.000002 0.000002 0.000002 ) 0.000000 -0.000007 0.007201 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007368 0.076883 -0.035022 ( 0.000021 0.000014 0.000021 ) -0.083535 -0.011752 -0.007989 ( 0.000015 0.000010 0.000015 ) -0.012036 0.033712 0.076880 ( 0.000014 0.000009 0.000014 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 339 obs out of 339 (total:339,skipped:0) (100.00%) unit cell: 8.3724(15) 8.3676(15) 8.3586(14) 89.945(15) 90.000(14) 90.075(16) V = 585.58(18) unit cell: 8.3662(4) 8.3662(4) 8.3662(4) 90.0 90.0 90.0 V = 585.58(5) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007467 0.076828 -0.034777 ( 0.000006 0.000006 0.000006 ) -0.083567 -0.011768 -0.008049 ( 0.000004 0.000004 0.000004 ) -0.012162 0.033648 0.076993 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007202 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007467 0.076828 -0.034777 ( 0.000006 0.000006 0.000006 ) -0.083567 -0.011768 -0.008049 ( 0.000004 0.000004 0.000004 ) -0.012162 0.033648 0.076993 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 2574 obs out of 2579 (total:2579,skipped:0) (99.81%) unit cell: 8.3667(4) 8.3748(6) 8.3580(6) 90.108(6) 89.967(5) 90.004(5) V = 585.64(6) unit cell: 8.36648(15) 8.36648(15) 8.36648(15) 90.0 90.0 90.0 V = 585.637(18) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 74 reflections under beam stop or inside a detector rejection region 32 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3429 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:26:05 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=94.0000 max=22696308.0000 PROFFIT INFO: signal sum lp corr: min=222.2978 max=3262989.7721 PROFFIT INFO: background sum: min=741.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=539.0000 max=10933.0000 PROFFIT INFO: num of signal pixels: min=58 max=876 PROFFIT INFO: Inet: min=485.0135 max=7119250.5000 PROFFIT INFO: sig(Inet): min=186.6733 max=63744.1094 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 79 268 448 713 779 1400 2278 3115 3429 Percent 0.0 0.1 2.3 7.8 13.1 20.8 22.7 40.8 66.4 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3429 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 3429 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7119251- 1546087 342 2345729.64 134.71 100.00 1544077- 1018361 342 1264988.10 108.69 100.00 1017833- 305277 342 593897.60 94.47 100.00 304344- 211142 342 248112.92 67.98 100.00 211061- 160862 342 182668.62 48.91 100.00 160791- 129848 342 144615.89 37.36 100.00 129528- 100161 342 114800.51 30.23 100.00 100066- 6128 342 58369.24 20.98 100.00 6117- 3532 342 4573.04 4.94 83.63 3528- 485 351 2602.28 3.16 39.60 ------------------------------------------------------------------------------------ 7119251- 485 3429 494740.68 55.01 92.18 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 829951.78 88.10 100.00 1.41- 1.12 342 753482.81 71.17 98.25 1.12- 0.96 342 655493.27 74.62 98.83 0.96- 0.88 342 466226.77 58.85 93.86 0.88- 0.81 342 636901.82 69.67 97.37 0.81- 0.74 342 332050.09 40.57 93.57 0.74- 0.71 342 284339.26 37.85 90.06 0.71- 0.65 342 500096.66 50.22 94.74 0.65- 0.62 342 255587.69 29.81 73.98 0.62- 0.58 351 239980.90 29.86 81.48 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 494740.68 55.01 92.18 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:26:06 2018 Sorting 3429 observations 119 unique observations with > 7.00 F2/sig(F2) 3429 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 74 597 Total number of frames 597 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3429 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 12 103 Total number of frames 103 2755 observations > 7.00 F2/sig(F2) 2755 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 12 102 Total number of frames 102 Removing 'redundancy=1' reflections Average redundancy: 21.8 (Out of 2755 removed 6 = 2749, unique = 126) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2749 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 12 102 Total number of frames 102 126 unique data precomputed (should be 126) 126 unique data with 2749 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.8 (Out of 2749 removed 0 = 2749, unique = 126) 126 unique data precomputed (should be 126) 126 unique data with 2749 observations RMS deviation of equivalent data = 0.21028 Rint = 0.17621 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17549, wR= 0.22542 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09112, wR= 0.12074, Acormin=0.625, Acormax=1.380, Acor_av=0.955 F test: Probability=1.000, F= 3.702 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08785, wR= 0.11101, Acormin=0.596, Acormax=1.378, Acor_av=0.919 F test: Probability=0.967, F= 1.075 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07850, wR= 0.10819, Acormin=0.675, Acormax=1.436, Acor_av=0.965 F test: Probability=1.000, F= 1.249 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07293, wR= 0.09449, Acormin=0.573, Acormax=1.472, Acor_av=0.924 F test: Probability=1.000, F= 1.157 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06589, wR= 0.08673, Acormin=0.572, Acormax=1.380, Acor_av=0.896 F test: Probability=1.000, F= 1.222 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07255, wR= 0.09715, Acormin=0.666, Acormax=1.563, Acor_av=0.929 F test: Probability=0.000, F= 0.824 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06833, wR= 0.08803, Acormin=0.591, Acormax=1.536, Acor_av=0.906 F test: Probability=0.000, F= 0.928 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06143, wR= 0.08045, Acormin=0.573, Acormax=1.453, Acor_av=0.881 F test: Probability=1.000, F= 1.144 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05496, wR= 0.07325, Acormin=0.552, Acormax=1.399, Acor_av=0.847 F test: Probability=1.000, F= 1.244 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06781, wR= 0.08513, Acormin=0.440, Acormax=1.392, Acor_av=0.823 F test: Probability=0.000, F= 0.658 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06617, wR= 0.08318, Acormin=0.458, Acormax=1.421, Acor_av=0.831 F test: Probability=0.000, F= 0.690 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05971, wR= 0.07529, Acormin=0.234, Acormax=0.627, Acor_av=0.381 F test: Probability=0.000, F= 0.845 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05221, wR= 0.06768, Acormin=0.271, Acormax=0.701, Acor_av=0.429 F test: Probability=0.992, F= 1.101 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04830, wR= 0.06376, Acormin=0.271, Acormax=0.751, Acor_av=0.454 F test: Probability=1.000, F= 1.279 Final absorption model (ne=6, no=5): Rint= 0.05496, Acormin=0.552, Acormax=1.399, Acor_av=0.847 Combined refinement in use Rint: 0.17631 There are 102 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 149 pars with 11175 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21028 Using Levenberg-Marquardt: 0.00010 New wR= 0.05334 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17621 with corrections 0.04115 Rint for all data: 0.17631 with corrections 0.04136 0 observations identified as outliers and rejected Cycle 2 wR= 0.05334 Using Levenberg-Marquardt: 0.00001 New wR= 0.05005 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17621 with corrections 0.03785 Rint for all data: 0.17631 with corrections 0.03806 0 observations identified as outliers and rejected Cycle 3 wR= 0.05005 Using Levenberg-Marquardt: 0.00000 New wR= 0.04933 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17621 with corrections 0.03725 Rint for all data: 0.17631 with corrections 0.03747 0 observations identified as outliers and rejected Cycle 4 wR= 0.04933 Using Levenberg-Marquardt: 0.00000 New wR= 0.04891 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17621 with corrections 0.03689 Rint for all data: 0.17631 with corrections 0.03711 0 observations identified as outliers and rejected Cycle 5 wR= 0.04891 Using Levenberg-Marquardt: 0.00000 New wR= 0.04865 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17621 with corrections 0.03670 Rint for all data: 0.17631 with corrections 0.03692 0 observations identified as outliers and rejected Final wR= 0.04865 Final frame scales: Min= 0.7539 Max= 1.1409 Final absorption correction factors: Amin= 0.5773 Amax= 1.5041 PROFFIT INFO: Inet (after scale3 abspack): min=486.3511 max=5560249.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=160.7452 max=73365.1797 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3429 reflections read from tmp file 525 reflections are rejected (524 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 3 3 3 2 5 1 8 124 Initial Chi^2= 0.34813 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.96422 Current error model SIG(F2)^2 = 106.97*I_RAW + 0.00*I_BACK+(0.01606*)^2 Cycle 2, Chi^2= 1.00008 Current error model SIG(F2)^2 = 99.28*I_RAW + 0.00*I_BACK+(0.01664*)^2 Cycle 3, Chi^2= 1.00003 Current error model SIG(F2)^2 = 100.04*I_RAW + 0.00*I_BACK+(0.01646*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 99.90*I_RAW + 0.00*I_BACK+(0.01650*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 99.90*I_RAW + 0.00*I_BACK+(0.01650*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5560249- 1559867 342 2288277.40 54.41 100.00 1558329- 976237 342 1211364.83 45.44 100.00 976079- 314660 342 587942.95 43.60 100.00 314522- 199108 342 242875.65 35.03 100.00 198957- 166231 342 181049.81 28.06 100.00 166202- 125080 342 140762.86 22.05 100.00 124981- 99689 342 112186.26 19.03 100.00 99686- 5721 342 58975.13 14.29 100.00 5717- 3374 342 4301.70 4.67 99.71 3371- 486 351 2608.79 3.63 72.36 ------------------------------------------------------------------------------------ 5560249- 486 3429 481773.58 26.96 97.14 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 873198.35 42.68 100.00 1.41- 1.12 342 772033.99 33.59 100.00 1.12- 0.96 342 615086.71 31.91 99.42 0.96- 0.88 342 454375.19 26.90 98.54 0.88- 0.81 342 606343.28 31.91 98.54 0.81- 0.74 342 311918.47 21.24 98.25 0.74- 0.71 342 268805.13 21.01 97.08 0.71- 0.65 342 464198.67 25.80 97.66 0.65- 0.62 342 237705.74 17.13 87.72 0.62- 0.58 351 220934.47 17.64 94.30 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 481773.58 26.96 97.14 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 873198.35 42.68 100.00 4.82- 1.12 684 822616.17 38.14 100.00 4.82- 0.96 1026 753439.68 36.06 99.81 4.82- 0.88 1368 678673.56 33.77 99.49 4.82- 0.81 1710 664207.50 33.40 99.30 4.82- 0.74 2052 605492.66 31.37 99.12 4.82- 0.71 2394 557394.44 29.89 98.83 4.82- 0.65 2736 545744.97 29.38 98.68 4.82- 0.62 3078 511518.39 28.02 97.47 4.82- 0.58 3429 481773.58 26.96 97.14 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 481773.58 26.96 97.14 Scale applied to data: s=0.179848 (maximum obs:5560249.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.024: data 3429 -> merged 156 With outlier rejection... Rint 0.036; Rsigma 0.024: data 3419 -> merged 156 Rejected total: 10, method kkm 8, method Blessing 2 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585771, 4.830389 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 19.86 100.00 278 1.41 - 1.12 14 14 28.14 100.00 394 1.12 - 0.97 14 14 28.36 100.00 397 0.96 - 0.84 14 14 30.64 100.00 429 0.84 - 0.78 14 14 22.57 100.00 316 0.78 - 0.73 14 14 24.29 100.00 340 0.73 - 0.69 14 14 22.71 100.00 318 0.69 - 0.66 14 14 19.57 100.00 274 0.65 - 0.63 14 14 21.00 100.00 294 0.63 - 0.60 14 14 19.07 100.00 267 --------------------------------------------------------------- 8.37 - 0.60 140 140 23.62 100.00 3307 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:26:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366661 8.374830 8.357972 90.1078 89.9673 90.0037 3418 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.91 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1745 0 2288 2284 3418 N (int>3sigma) = 0 0 0 0 1745 0 2220 2211 3320 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 85.8 85.9 86.0 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.9 27.0 26.9 Lattice type: F chosen Volume: 585.64 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.915 90.06 119.93 119.91 Niggli form: a.a = 34.933 b.b = 34.944 c.c = 34.984 b.c = -0.036 a.c = -17.440 a.b = -17.422 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.141 CUBIC F-lattice R(int) = 0.036 [ 3262] Vol = 585.6 Cell: 8.367 8.375 8.358 90.11 89.97 90.00 Volume: 585.64 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 2982] Vol = 439.2 Cell: 5.919 5.911 14.503 90.01 90.08 120.05 Volume: 439.23 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 964] Vol = 439.2 Trigonal Cell: 5.919 5.911 14.503 90.01 90.08 120.05 Volume: 439.23 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.035 [ 3016] Vol = 292.8 Cell: 5.919 5.919 8.358 89.95 89.90 89.94 Volume: 292.82 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.141 TETRAGONAL I-lattice R(int) = 0.035 [ 3016] Vol = 292.8 Cell: 5.919 5.919 8.358 90.10 90.05 89.94 Volume: 292.82 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.072 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 2962] Vol = 292.8 Cell: 5.919 5.919 8.358 89.90 89.95 89.94 Volume: 292.82 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.065 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 2960] Vol = 292.8 Cell: 5.910 8.367 5.922 89.97 89.88 90.02 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.036 MONOCLINIC I-lattice R(int) = 0.034 [ 2618] Vol = 292.8 Cell: 5.919 5.919 8.358 90.05 90.10 89.94 Volume: 292.82 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.109 MONOCLINIC I-lattice R(int) = 0.032 [ 2618] Vol = 292.8 Cell: 5.910 5.922 8.367 90.03 90.02 90.12 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.030 [ 2633] Vol = 292.8 Cell: 5.910 8.367 5.922 89.97 90.12 89.98 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.051 MONOCLINIC I-lattice R(int) = 0.033 [ 2617] Vol = 292.8 Cell: 8.367 5.910 5.922 90.12 90.03 90.02 Volume: 292.82 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.107 MONOCLINIC C-lattice R(int) = 0.032 [ 2617] Vol = 292.8 Cell: 10.246 5.911 5.915 90.06 125.18 89.91 Volume: 292.82 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 1968] Vol = 146.4 Cell: 5.910 5.911 5.915 90.06 119.93 119.91 Volume: 146.41 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1745 0 2288 2284 3418 N (int>3sigma) = 0 0 0 0 1745 0 2220 2211 3320 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 85.8 85.9 86.0 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.9 27.0 26.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.175 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 272 766 N I>3s 29 29 249 766 0.7 0.7 0.7 38.9 7.7 7.7 5.2 30.3 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 0.036 3010 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3049 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366661 8.374830 8.357972 90.1078 89.9673 90.0037 ZERR 3.00 0.000440 0.000589 0.000573 0.0056 0.0050 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5353473- 1147262 549 546 26 21.0 1912864.31 51.56 0.032 0.043 1130371- 279739 538 534 26 20.5 674228.30 43.33 0.041 0.053 279502- 135464 791 790 26 30.4 192690.63 29.01 0.037 0.050 131937- 99598 553 553 26 21.3 117529.56 19.45 0.053 0.069 98797- 3931 525 523 26 20.1 33574.35 9.89 0.062 0.080 3927- 1872 473 473 26 18.2 3101.55 4.00 0.197 0.246 ------------------------------------------------------------------------------------------- 5353473- 1872 3429 3419 156 21.9 479879.40 26.92 0.036 0.047 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 639 635 26 24.4 730073.37 36.96 0.038 0.047 0.019 1.12-0.88 769 769 26 29.6 608223.64 30.95 0.030 0.041 0.022 0.85-0.75 637 636 26 24.5 464641.36 26.04 0.033 0.043 0.024 0.74-0.68 563 562 26 21.6 392773.08 23.69 0.038 0.048 0.027 0.67-0.63 548 547 26 21.0 229329.83 18.48 0.052 0.070 0.035 0.62-0.59 273 270 26 10.4 250715.99 17.65 0.047 0.051 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 3429 3419 156 21.9 479879.40 26.92 0.036 0.047 0.024 inf-0.60 3313 3306 139 23.8 490016.27 27.27 0.036 0.047 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 635 26 26 100.0 24.4 730073.37 198.84 0.038 0.006 1.12-0.88 769 26 26 100.0 29.6 608223.64 170.60 0.030 0.004 0.85-0.75 636 26 26 100.0 24.5 464641.36 136.11 0.033 0.005 0.74-0.68 562 26 26 100.0 21.6 392773.08 112.80 0.038 0.006 0.67-0.63 547 26 26 100.0 21.0 229329.83 84.78 0.052 0.008 0.62-0.59 270 27 26 96.3 10.4 250715.99 67.32 0.047 0.014 -------------------------------------------------------------------------------------------- inf-0.59 3419 157 156 99.4 21.9 479879.40 138.04 0.036 0.006 inf-0.60 3306 139 139 100.0 23.8 490016.27 141.10 0.036 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007467 0.076828 -0.034777 ( 0.000006 0.000006 0.000006 ) -0.083567 -0.011768 -0.008049 ( 0.000004 0.000004 0.000004 ) -0.012162 0.033648 0.076993 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007202 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007467 0.076828 -0.034777 ( 0.000006 0.000006 0.000006 ) -0.083567 -0.011768 -0.008049 ( 0.000004 0.000004 0.000004 ) -0.012162 0.033648 0.076993 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3667(4) 8.3748(6) 8.3580(6) 90.108(6) 89.967(5) 90.004(5) V = 585.64(6) unit cell: 8.36648(15) 8.36648(15) 8.36648(15) 90.0 90.0 90.0 V = 585.637(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: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=52.968) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 78.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=94.0000 max=22696308.0000 PROFFIT INFO: signal sum lp corr: min=222.2978 max=3262989.7721 PROFFIT INFO: background sum: min=741.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=539.0000 max=10933.0000 PROFFIT INFO: num of signal pixels: min=58 max=876 PROFFIT INFO: Inet: min=485.0135 max=7119250.5000 PROFFIT INFO: sig(Inet): min=186.6733 max=63744.1094 PROFFIT INFO: Inet/sig(Inet): min=0.39 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 8 158 536 896 1426 1558 2800 4556 6230 6858 Percent 0.0 0.1 2.3 7.8 13.1 20.8 22.7 40.8 66.4 90.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3429 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 3429 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7119251- 1546087 342 2345729.64 134.71 100.00 1544077- 1018361 342 1264988.10 108.69 100.00 1017833- 305277 342 593897.60 94.47 100.00 304344- 211142 342 248112.92 67.98 100.00 211061- 160862 342 182668.62 48.91 100.00 160791- 129848 342 144615.89 37.36 100.00 129528- 100161 342 114800.51 30.23 100.00 100066- 6128 342 58369.24 20.98 100.00 6117- 3532 342 4573.04 4.94 83.63 3528- 485 351 2602.28 3.16 39.60 ------------------------------------------------------------------------------------ 7119251- 485 3429 494740.68 55.01 92.18 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 829951.78 88.10 100.00 1.41- 1.12 342 753482.81 71.17 98.25 1.12- 0.96 342 655493.27 74.62 98.83 0.96- 0.88 342 466226.77 58.85 93.86 0.88- 0.81 342 636901.82 69.67 97.37 0.81- 0.74 342 332050.09 40.57 93.57 0.74- 0.71 342 284339.26 37.85 90.06 0.71- 0.65 342 500096.66 50.22 94.74 0.65- 0.62 342 255587.69 29.81 73.98 0.62- 0.58 351 239980.90 29.86 81.48 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 494740.68 55.01 92.18 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:26:07 2018 Sorting 3429 observations 86 unique observations with > 7.00 F2/sig(F2) 3429 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 74 597 Total number of frames 597 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3429 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 10 89 Total number of frames 89 2755 observations > 7.00 F2/sig(F2) 2755 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 10 89 Total number of frames 89 Removing 'redundancy=1' reflections Average redundancy: 30.2 (Out of 2755 removed 4 = 2751, 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): 4/m3bar2/m 2751 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 10 89 Total number of frames 89 91 unique data precomputed (should be 91) 91 unique data with 2751 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 30.2 (Out of 2751 removed 0 = 2751, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 2751 observations RMS deviation of equivalent data = 0.21067 Rint = 0.17639 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17522, wR= 0.22536 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09164, wR= 0.12180, Acormin=0.625, Acormax=1.377, Acor_av=0.954 F test: Probability=1.000, F= 3.649 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08795, wR= 0.11169, Acormin=0.597, Acormax=1.375, Acor_av=0.918 F test: Probability=0.982, F= 1.084 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07914, wR= 0.11032, Acormin=0.680, Acormax=1.419, Acor_av=0.964 F test: Probability=1.000, F= 1.232 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07378, wR= 0.09641, Acormin=0.573, Acormax=1.458, Acor_av=0.922 F test: Probability=1.000, F= 1.149 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06652, wR= 0.08824, Acormin=0.571, Acormax=1.363, Acor_av=0.893 F test: Probability=1.000, F= 1.227 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07374, wR= 0.10006, Acormin=0.665, Acormax=1.547, Acor_av=0.927 F test: Probability=0.000, F= 0.813 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06992, wR= 0.09074, Acormin=0.579, Acormax=1.514, Acor_av=0.903 F test: Probability=0.000, F= 0.903 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06232, wR= 0.08264, Acormin=0.575, Acormax=1.433, Acor_av=0.877 F test: Probability=0.999, F= 1.134 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05550, wR= 0.07426, Acormin=0.551, Acormax=1.380, Acor_av=0.843 F test: Probability=1.000, F= 1.256 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06870, wR= 0.08719, Acormin=0.441, Acormax=1.376, Acor_av=0.818 F test: Probability=0.000, F= 0.654 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06707, wR= 0.08532, Acormin=0.458, Acormax=1.403, Acor_av=0.825 F test: Probability=0.000, F= 0.685 Trying model 12 (ne=8, no=3)... Results: Rint= 0.06016, wR= 0.07660, Acormin=0.227, Acormax=0.604, Acor_av=0.369 F test: Probability=0.000, F= 0.849 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05222, wR= 0.06819, Acormin=0.267, Acormax=0.687, Acor_av=0.422 F test: Probability=0.998, F= 1.122 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04844, wR= 0.06437, Acormin=0.266, Acormax=0.735, Acor_av=0.447 F test: Probability=1.000, F= 1.296 Final absorption model (ne=6, no=5): Rint= 0.05550, Acormin=0.551, Acormax=1.380, Acor_av=0.843 Combined refinement in use Rint: 0.17650 There are 89 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: 6, max odd order: 5 (48 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21067 Using Levenberg-Marquardt: 0.00010 New wR= 0.05613 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17639 with corrections 0.04299 Rint for all data: 0.17650 with corrections 0.04320 3 observations identified as outliers and rejected Cycle 2 wR= 0.05585 Using Levenberg-Marquardt: 0.00001 New wR= 0.05209 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17524 with corrections 0.03906 Rint for all data: 0.17650 with corrections 0.03959 0 observations identified as outliers and rejected Cycle 3 wR= 0.05209 Using Levenberg-Marquardt: 0.00000 New wR= 0.05137 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17524 with corrections 0.03833 Rint for all data: 0.17650 with corrections 0.03885 0 observations identified as outliers and rejected Cycle 4 wR= 0.05137 Using Levenberg-Marquardt: 0.00000 New wR= 0.05101 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17524 with corrections 0.03795 Rint for all data: 0.17650 with corrections 0.03845 1 observations identified as outliers and rejected Cycle 5 wR= 0.05106 Using Levenberg-Marquardt: 0.00000 New wR= 0.05080 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17507 with corrections 0.03765 Rint for all data: 0.17650 with corrections 0.03818 0 observations identified as outliers and rejected Final wR= 0.05080 Final frame scales: Min= 0.8119 Max= 1.1406 Final absorption correction factors: Amin= 0.5763 Amax= 1.5590 PROFFIT INFO: Inet (after scale3 abspack): min=473.9118 max=5564307.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=163.7146 max=73691.2813 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3429 reflections read from tmp file 536 reflections are rejected (536 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 2 2 3 2 0 4 90 Initial Chi^2= 0.33613 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.98933 Current error model SIG(F2)^2 = 110.06*I_RAW + 0.00*I_BACK+(0.01699*)^2 Cycle 2, Chi^2= 1.00162 Current error model SIG(F2)^2 = 96.27*I_RAW + 0.00*I_BACK+(0.01932*)^2 Cycle 3, Chi^2= 1.00022 Current error model SIG(F2)^2 = 99.62*I_RAW + 0.00*I_BACK+(0.01865*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 98.85*I_RAW + 0.00*I_BACK+(0.01882*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 99.05*I_RAW + 0.00*I_BACK+(0.01878*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 99.05*I_RAW + 0.00*I_BACK+(0.01878*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5564307- 1546220 342 2296094.55 49.00 100.00 1540615- 976802 342 1209735.45 42.16 100.00 976758- 316453 342 588276.07 40.51 100.00 315747- 198957 342 243127.23 33.43 100.00 198688- 166217 342 181288.17 27.18 100.00 166078- 124414 342 140416.89 21.69 100.00 124368- 99130 342 111803.14 18.80 100.00 99100- 5751 342 59055.73 14.15 100.00 5713- 3393 342 4306.88 4.70 99.42 3389- 474 351 2610.16 3.63 72.65 ------------------------------------------------------------------------------------ 5564307- 474 3429 482408.80 25.47 97.14 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 878117.90 39.12 100.00 1.41- 1.12 342 774683.49 31.17 100.00 1.12- 0.96 342 617213.90 29.89 99.42 0.96- 0.88 342 454160.23 25.50 98.54 0.88- 0.81 342 606008.41 30.12 98.54 0.81- 0.74 342 311791.02 20.37 98.25 0.74- 0.71 342 267999.06 20.32 97.08 0.71- 0.65 342 463444.75 24.63 97.66 0.65- 0.62 342 237234.90 16.60 87.72 0.62- 0.58 351 220331.11 17.18 94.30 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 482408.80 25.47 97.14 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 342 878117.90 39.12 100.00 4.82- 1.12 684 826400.70 35.15 100.00 4.82- 0.96 1026 756671.76 33.39 99.81 4.82- 0.88 1368 681043.88 31.42 99.49 4.82- 0.81 1710 666036.79 31.16 99.30 4.82- 0.74 2052 606995.83 29.36 99.12 4.82- 0.71 2394 558567.72 28.07 98.83 4.82- 0.65 2736 546677.34 27.64 98.68 4.82- 0.62 3078 512294.85 26.41 97.47 4.82- 0.58 3429 482408.80 25.47 97.14 ------------------------------------------------------------------------------------ 4.82- 0.58 3429 482408.80 25.47 97.14 Scale applied to data: s=0.179717 (maximum obs:5564307.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.038; Rsigma 0.025: data 3429 -> merged 109 With outlier rejection... Rint 0.038; Rsigma 0.025: data 3422 -> merged 109 Rejected total: 7, method kkm 6, method Blessing 1 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585771, 4.830391 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 20.50 100.00 205 1.61 - 1.21 10 10 31.80 100.00 318 1.17 - 1.01 10 10 40.80 100.00 408 0.99 - 0.89 10 10 40.40 100.00 404 0.88 - 0.81 10 10 38.70 100.00 387 0.81 - 0.74 10 10 33.40 100.00 334 0.73 - 0.71 10 10 36.50 100.00 365 0.70 - 0.66 10 10 30.50 100.00 305 0.66 - 0.64 10 10 29.50 100.00 295 0.63 - 0.60 10 10 28.90 100.00 289 --------------------------------------------------------------- 8.37 - 0.60 100 100 33.10 100.00 3310 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:26:06 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366661 8.374830 8.357972 90.1078 89.9673 90.0037 3418 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.91 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1745 0 2288 2284 3418 N (int>3sigma) = 0 0 0 0 1745 0 2220 2211 3320 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 85.8 85.9 86.0 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.9 27.0 26.9 Lattice type: F chosen Volume: 585.64 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.910 5.911 5.915 90.06 119.93 119.91 Niggli form: a.a = 34.933 b.b = 34.944 c.c = 34.984 b.c = -0.036 a.c = -17.440 a.b = -17.422 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.141 CUBIC F-lattice R(int) = 0.036 [ 3262] Vol = 585.6 Cell: 8.367 8.375 8.358 90.11 89.97 90.00 Volume: 585.64 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 2982] Vol = 439.2 Cell: 5.919 5.911 14.503 90.01 90.08 120.05 Volume: 439.23 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.132 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 964] Vol = 439.2 Trigonal Cell: 5.919 5.911 14.503 90.01 90.08 120.05 Volume: 439.23 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.035 [ 3016] Vol = 292.8 Cell: 5.919 5.919 8.358 89.95 89.90 89.94 Volume: 292.82 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.141 TETRAGONAL I-lattice R(int) = 0.035 [ 3016] Vol = 292.8 Cell: 5.919 5.919 8.358 90.10 90.05 89.94 Volume: 292.82 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.072 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 2962] Vol = 292.8 Cell: 5.919 5.919 8.358 89.90 89.95 89.94 Volume: 292.82 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.065 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 2960] Vol = 292.8 Cell: 5.910 8.367 5.922 89.97 89.88 90.02 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.036 MONOCLINIC I-lattice R(int) = 0.034 [ 2618] Vol = 292.8 Cell: 5.919 5.919 8.358 90.05 90.10 89.94 Volume: 292.82 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.109 MONOCLINIC I-lattice R(int) = 0.032 [ 2618] Vol = 292.8 Cell: 5.910 5.922 8.367 90.03 90.02 90.12 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.042 MONOCLINIC I-lattice R(int) = 0.030 [ 2633] Vol = 292.8 Cell: 5.910 8.367 5.922 89.97 90.12 89.98 Volume: 292.82 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.051 MONOCLINIC I-lattice R(int) = 0.033 [ 2617] Vol = 292.8 Cell: 8.367 5.910 5.922 90.12 90.03 90.02 Volume: 292.82 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.107 MONOCLINIC C-lattice R(int) = 0.032 [ 2617] Vol = 292.8 Cell: 10.246 5.911 5.915 90.06 125.18 89.91 Volume: 292.82 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 1968] Vol = 146.4 Cell: 5.910 5.911 5.915 90.06 119.93 119.91 Volume: 146.41 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1745 0 2288 2284 3418 N (int>3sigma) = 0 0 0 0 1745 0 2220 2211 3320 Mean intensity = 0.0 0.0 0.0 0.0 33.2 0.0 85.8 85.9 86.0 Mean int/sigma = 0.0 0.0 0.0 0.0 27.1 0.0 26.9 27.0 26.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.175 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 272 766 N I>3s 29 29 249 766 0.7 0.7 0.7 38.9 7.7 7.7 5.2 30.3 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 0.036 3010 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3049 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366661 8.374830 8.357972 90.1078 89.9673 90.0037 ZERR 3.00 0.000440 0.000589 0.000573 0.0056 0.0050 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5360861- 892303 761 759 27 28.1 1664278.39 44.74 0.035 0.047 886641- 153812 1021 1018 27 37.7 280338.17 32.82 0.041 0.049 142688- 52080 844 843 27 31.2 111146.98 18.85 0.053 0.069 21594- 1887 803 802 28 28.6 4567.60 4.72 0.156 0.192 ------------------------------------------------------------------------------------------- 5360861- 1887 3429 3422 109 31.4 480985.29 25.44 0.038 0.049 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 861 857 27 31.7 771826.92 34.94 0.037 0.048 0.021 1.01-0.78 1017 1017 27 37.7 481603.98 25.57 0.032 0.045 0.025 0.78-0.65 925 924 27 34.2 367617.11 21.57 0.040 0.050 0.029 0.65-0.59 626 624 28 22.3 248407.92 17.91 0.052 0.054 0.035 ------------------------------------------------------------------------------------------------------ inf-0.59 3429 3422 109 31.4 480985.29 25.44 0.038 0.049 0.025 inf-0.60 3313 3308 99 33.4 491134.30 25.76 0.037 0.049 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 857 27 27 100.0 31.7 771826.92 221.08 0.037 0.006 1.01-0.78 1017 27 27 100.0 37.7 481603.98 168.80 0.032 0.004 0.78-0.65 924 27 27 100.0 34.2 367617.11 132.38 0.040 0.006 0.65-0.59 624 29 28 96.6 22.3 248407.92 98.03 0.052 0.010 -------------------------------------------------------------------------------------------- inf-0.59 3422 110 109 99.1 31.4 480985.29 159.16 0.038 0.006 inf-0.60 3308 99 99 100.0 33.4 491134.30 162.33 0.037 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:30:55 2018) ID: 2932; threads 39; handles 879; mem 516760.00 (1237728.00)kB; time: 1w 5d 23h 36m 25s MEMORY INFO: Memory PF:0.0, Ph:168.0, V:1208.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:504.6,peak PF: 708.5, WS: 269.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:168.0, V:1210.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:506.4,peak PF: 708.5, WS: 270.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:30:55 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) 8.37051 ( 0.00044 ) 8.37682 ( 0.00059 ) 8.35710 ( 0.00057 ) 90.12473 ( 0.00563 ) 89.98579 ( 0.00503 ) 90.00567 ( 0.00511 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:30:55 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007187 0.000000 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007173 0.000014 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000014 0.007202 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(6) 90.125(6) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36648(15) 8.36648(15) 8.36648(15) 90.0 90.0 90.0 V = 585.637(18) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 454 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.74 | 45 | 1.188 ( 0.065) | 1.146 ( 0.124) | 1.151 ( 0.393) | 0.74- 0.71 | 45 | 1.194 ( 0.067) | 1.214 ( 0.145) | 1.165 ( 0.375) | 0.71- 0.66 | 45 | 1.200 ( 0.059) | 1.204 ( 0.168) | 1.160 ( 0.402) | 0.66- 0.63 | 45 | 1.224 ( 0.083) | 1.187 ( 0.154) | 1.131 ( 0.431) | 0.63- 0.59 | 45 | 1.221 ( 0.086) | 1.222 ( 0.228) | 1.310 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 450 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.195 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076673 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3921(11) 90.059(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011819 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011819 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3741(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011819 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011819 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3741(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.138 ( 0.133) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.188 ( 0.062) | 1.141 ( 0.119) | 1.200 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_6_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_6_76.rpb PROFFITPEAK info: 1110 peaks in the peak location table UB fit with 489 obs out of 520 (total:520,skipped:0) (94.04%) UB - matrix: -0.007468 0.076817 -0.034992 ( 0.000032 0.000020 0.000032 ) -0.083536 -0.011815 -0.008018 ( 0.000029 0.000018 0.000029 ) -0.012057 0.033709 0.076892 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007179 0.000007 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000007 0.007177 -0.000001 ( 0.000003 0.000003 0.000003 ) 0.000004 -0.000001 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.371(3) 8.373(2) 8.359(2) 89.99(2) 90.03(2) 90.05(2) V = 585.8(3) UB fit with 489 obs out of 520 (total:520,skipped:0) (94.04%) UB - matrix: -0.007468 0.076817 -0.034992 ( 0.000032 0.000020 0.000032 ) -0.083536 -0.011815 -0.008018 ( 0.000029 0.000018 0.000029 ) -0.012057 0.033709 0.076892 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007179 0.000007 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000007 0.007177 -0.000001 ( 0.000003 0.000003 0.000003 ) 0.000004 -0.000001 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.371(3) 8.373(2) 8.359(2) 89.99(2) 90.03(2) 90.05(2) V = 585.8(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: -0.007463 0.076821 -0.035025 ( 0.000032 0.000020 0.000032 ) -0.083538 -0.011815 -0.008012 ( 0.000029 0.000018 0.000029 ) -0.012053 0.033712 0.076876 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007180 0.000007 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000007 0.007178 -0.000004 ( 0.000003 0.000003 0.000003 ) 0.000004 -0.000004 0.007201 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007463 0.076821 -0.035025 ( 0.000032 0.000020 0.000032 ) -0.083538 -0.011815 -0.008012 ( 0.000029 0.000018 0.000029 ) -0.012053 0.033712 0.076876 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 488 obs out of 520 (total:520,skipped:0) (93.85%) unit cell: 8.371(3) 8.372(2) 8.359(2) 89.97(2) 90.03(2) 90.06(2) V = 585.8(3) unit cell: 8.3674(6) 8.3674(6) 8.3674(6) 90.0 90.0 90.0 V = 585.82(8) UB fit with 488 obs out of 520 (total:520,skipped:0) (93.85%) UB - matrix: -0.007463 0.076821 -0.035025 ( 0.000032 0.000020 0.000032 ) -0.083538 -0.011815 -0.008012 ( 0.000029 0.000018 0.000029 ) -0.012053 0.033712 0.076876 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007180 0.000007 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000007 0.007178 -0.000004 ( 0.000003 0.000003 0.000003 ) 0.000004 -0.000004 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.371(3) 8.372(2) 8.359(2) 89.97(2) 90.03(2) 90.06(2) V = 585.8(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 520 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007463 0.076821 -0.035025 ( 0.000032 0.000020 0.000032 ) -0.083538 -0.011815 -0.008012 ( 0.000029 0.000018 0.000029 ) -0.012053 0.033712 0.076876 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007180 0.000007 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000007 0.007178 -0.000004 ( 0.000003 0.000003 0.000003 ) 0.000004 -0.000004 0.007201 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007463 0.076821 -0.035025 ( 0.000032 0.000020 0.000032 ) -0.083538 -0.011815 -0.008012 ( 0.000029 0.000018 0.000029 ) -0.012053 0.033712 0.076876 ( 0.000025 0.000015 0.000025 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 488 obs out of 520 (total:520,skipped:0) (93.85%) unit cell: 8.371(3) 8.372(2) 8.359(2) 89.97(2) 90.03(2) 90.06(2) V = 585.8(3) unit cell: 8.3674(6) 8.3674(6) 8.3674(6) 90.0 90.0 90.0 V = 585.82(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 487 obs out of 520 (total:520,skipped:0) (93.65%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_76.rpb 5 of 453 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.88- 1.41 | 45 | 0.987 ( 0.108) | 1.123 ( 0.550) | 1.203 ( 0.679) | 1.41- 1.16 | 45 | 1.066 ( 0.066) | 1.177 ( 0.460) | 1.155 ( 0.656) | 1.16- 1.01 | 45 | 1.075 ( 0.075) | 1.045 ( 0.132) | 1.009 ( 0.359) | 0.98- 0.91 | 45 | 1.116 ( 0.063) | 1.098 ( 0.097) | 1.181 ( 0.543) | 0.91- 0.82 | 45 | 1.136 ( 0.060) | 1.087 ( 0.094) | 1.152 ( 0.425) | 0.82- 0.76 | 45 | 1.170 ( 0.073) | 1.121 ( 0.121) | 1.176 ( 0.435) | 0.76- 0.71 | 45 | 1.165 ( 0.037) | 1.106 ( 0.120) | 1.213 ( 0.388) | 0.71- 0.67 | 45 | 1.177 ( 0.038) | 1.101 ( 0.136) | 1.223 ( 0.471) | 0.67- 0.62 | 45 | 1.195 ( 0.050) | 1.108 ( 0.152) | 1.281 ( 0.450) | 0.62- 0.59 | 43 | 1.206 ( 0.065) | 1.102 ( 0.178) | 1.341 ( 0.528) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.88- 0.59 | 448 | 1.129 ( 0.093) | 1.107 ( 0.258) | 1.193 ( 0.511) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.007540 0.077052 -0.035005 ( 0.000016 0.000009 0.000016 ) -0.083651 -0.011916 -0.008057 ( 0.000013 0.000007 0.000013 ) -0.011938 0.033666 0.076928 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007197 0.000014 0.000020 ( 0.000002 0.000001 0.000002 ) 0.000014 0.007212 -0.000011 ( 0.000001 0.000001 0.000001 ) 0.000020 -0.000011 0.007208 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3611(13) 8.3520(11) 8.3545(11) 89.909(11) 90.156(12) 90.111(12) V = 583.40(14) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007417 0.076887 -0.034966 ( 0.000013 0.000007 0.000013 ) -0.083541 -0.011772 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012009 0.033665 0.076922 ( 0.000011 0.000006 0.000011 ) M - matrix: 0.007178 0.000009 0.000003 ( 0.000002 0.000001 0.000001 ) 0.000009 0.007184 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 -0.000005 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007417 0.076887 -0.034966 ( 0.000013 0.000007 0.000013 ) -0.083541 -0.011772 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012009 0.033665 0.076922 ( 0.000011 0.000006 0.000011 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 8.3718(11) 8.3688(9) 8.3572(10) 89.962(9) 90.025(10) 90.071(10) V = 585.51(12) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007417 0.076887 -0.034966 ( 0.000013 0.000007 0.000013 ) -0.083541 -0.011772 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012009 0.033665 0.076922 ( 0.000011 0.000006 0.000011 ) M - matrix: 0.007178 0.000009 0.000003 ( 0.000002 0.000001 0.000001 ) 0.000009 0.007184 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 -0.000005 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007417 0.076887 -0.034966 ( 0.000013 0.000007 0.000013 ) -0.083541 -0.011772 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012009 0.033665 0.076922 ( 0.000011 0.000006 0.000011 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 8.3718(11) 8.3688(9) 8.3572(10) 89.962(9) 90.025(10) 90.071(10) V = 585.51(12) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_76.rpb 3 of 457 peaks identified as outliers and rejected 454 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" 454 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6.tabbin file 454 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 269 | 1.147 ( 0.119) | 1.244 ( 0.409) | 1.318 ( 0.650) | 13.2-18.8 | 269 | 1.132 ( 0.071) | 1.179 ( 0.254) | 1.249 ( 0.559) | 18.9-23.0 | 269 | 1.142 ( 0.091) | 1.186 ( 0.269) | 1.256 ( 0.677) | 23.0-27.3 | 269 | 1.132 ( 0.098) | 1.173 ( 0.308) | 1.232 ( 0.567) | 27.3-30.4 | 269 | 1.135 ( 0.098) | 1.153 ( 0.245) | 1.192 ( 0.444) | 30.4-33.6 | 269 | 1.147 ( 0.101) | 1.136 ( 0.215) | 1.204 ( 0.443) | 33.6-37.0 | 269 | 1.141 ( 0.096) | 1.121 ( 0.195) | 1.163 ( 0.427) | 37.0-39.8 | 269 | 1.144 ( 0.119) | 1.091 ( 0.207) | 1.219 ( 0.505) | 39.8-42.8 | 269 | 1.163 ( 0.109) | 1.108 ( 0.257) | 1.216 ( 0.529) | 42.8-49.8 | 273 | 1.204 ( 0.152) | 1.123 ( 0.266) | 1.201 ( 0.478) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2694 | 1.149 ( 0.109) | 1.151 ( 0.272) | 1.225 ( 0.536) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0024 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:31:27 2018 PROFFITMAIN - Started at Wed Mar 28 14:31:27 2018 OTKP changes: 2682 2 4 6 OTKP changes: 2682 2 4 6 No constraint UB - matrix: -0.007489 0.076885 -0.034796 ( 0.000006 0.000006 0.000006 ) -0.083610 -0.011788 -0.008056 ( 0.000004 0.000004 0.000004 ) -0.012153 0.033663 0.077047 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007194 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007183 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000013 0.007212 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007489 0.076885 -0.034796 ( 0.000006 0.000006 0.000006 ) -0.083610 -0.011788 -0.008056 ( 0.000004 0.000004 0.000004 ) -0.012153 0.033663 0.077047 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 2686 obs out of 2694 (total:2694,skipped:0) (99.70%) unit cell: 8.3624(4) 8.3688(6) 8.3523(6) 90.106(5) 89.983(5) 90.006(5) V = 584.52(6) unit cell: 8.36117(14) 8.36117(14) 8.36117(14) 90.0 90.0 90.0 V = 584.523(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007132 0.076840 -0.034861 ( 0.000017 0.000012 0.000018 ) -0.083544 -0.011642 -0.008034 ( 0.000013 0.000010 0.000015 ) -0.012423 0.033796 0.076706 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007185 0.000005 -0.000033 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007182 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000033 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3681(13) 8.3696(14) 8.3805(15) 90.057(14) 89.736(14) 90.038(14) V = 586.94(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011714 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011714 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3739(12) 8.3581(15) 90.141(13) 89.821(13) 90.029(12) V = 585.41(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.41(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011714 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007243 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011714 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3739(12) 8.3581(15) 90.141(13) 89.821(13) 90.029(12) V = 585.41(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.41(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084676 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084760 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007170 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007184 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007195 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084676 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084760 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3766(16) 8.3684(8) 8.3619(10) 90.063(10) 89.870(13) 90.081(11) V = 586.15(14) unit cell: 8.3689(3) 8.3689(3) 8.3689(3) 90.0 90.0 90.0 V = 586.15(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007570 0.077005 -0.034601 ( 0.000015 0.000014 0.000012 ) -0.083443 -0.011879 -0.008153 ( 0.000011 0.000011 0.000009 ) -0.012255 0.033270 0.076970 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007170 0.000001 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007178 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3766(11) 8.3721(13) 8.3661(11) 89.946(12) 89.991(11) 90.004(12) V = 586.71(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.87(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.87(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" UB fit with 453 obs out of 454 (total:454,skipped:0) (99.78%) UB - matrix: -0.007433 0.076922 -0.034997 ( 0.000014 0.000008 0.000014 ) -0.083558 -0.011778 -0.008014 ( 0.000012 0.000006 0.000011 ) -0.011999 0.033699 0.076939 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007181 0.000008 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000008 0.007191 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000007 -0.000005 0.007209 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3701(11) 8.3642(10) 8.3542(11) 89.961(10) 90.052(11) 90.064(11) V = 584.88(13) OTKP changes: 453 1 1 1 OTKP changes: 453 1 1 1 OTKP changes: 453 1 1 1 No constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007178 0.000009 0.000002 ( 0.000002 0.000001 0.000001 ) 0.000009 0.007184 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 -0.000006 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 454 obs out of 454 (total:454,skipped:0) (100.00%) unit cell: 8.3717(11) 8.3683(10) 8.3558(11) 89.955(10) 90.016(11) 90.072(11) V = 585.38(13) unit cell: 8.3653(3) 8.3653(3) 8.3653(3) 90.0 90.0 90.0 V = 585.38(4) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) HKL list info: 726 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007178 0.000009 0.000002 ( 0.000002 0.000001 0.000001 ) 0.000009 0.007184 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 -0.000006 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 454 obs out of 454 (total:454,skipped:0) (100.00%) unit cell: 8.3717(11) 8.3683(10) 8.3558(11) 89.955(10) 90.016(11) 90.072(11) V = 585.38(13) unit cell: 8.3653(3) 8.3653(3) 8.3653(3) 90.0 90.0 90.0 V = 585.38(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 454 obs out of 454 (total:454,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007178 0.000009 0.000002 ( 0.000002 0.000001 0.000001 ) 0.000009 0.007184 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 -0.000006 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007411 0.076892 -0.034980 ( 0.000014 0.000008 0.000014 ) -0.083541 -0.011773 -0.007991 ( 0.000012 0.000006 0.000012 ) -0.012021 0.033665 0.076931 ( 0.000012 0.000007 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 454 obs out of 454 (total:454,skipped:0) (100.00%) unit cell: 8.3717(11) 8.3683(10) 8.3558(11) 89.955(10) 90.016(11) 90.072(11) V = 585.38(13) unit cell: 8.3653(3) 8.3653(3) 8.3653(3) 90.0 90.0 90.0 V = 585.38(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_6_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007470 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007470 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) UB fit with 2688 obs out of 2694 (total:2694,skipped:0) (99.78%) unit cell: 8.3674(4) 8.3747(6) 8.3606(6) 90.103(5) 89.966(5) 90.006(5) V = 585.86(6) unit cell: 8.36752(16) 8.36752(16) 8.36752(16) 90.0 90.0 90.0 V = 585.856(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 75 reflections under beam stop or inside a detector rejection region 34 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3574 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:31:36 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3262192.3525 PROFFIT INFO: background sum: min=702.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11006.0000 PROFFIT INFO: num of signal pixels: min=56 max=881 PROFFIT INFO: Inet: min=530.6313 max=7117510.5000 PROFFIT INFO: sig(Inet): min=186.6679 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 3 82 279 464 740 813 1464 2370 3251 3574 Percent 0.0 0.1 2.3 7.8 13.0 20.7 22.7 41.0 66.3 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3574 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 3574 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117511- 1539705 357 2343116.29 134.25 100.00 1538340- 1001044 357 1254463.60 108.20 100.00 999967- 305134 357 586090.42 94.14 100.00 304280- 210545 357 248736.49 68.26 100.00 210481- 159018 357 181225.20 48.50 100.00 158934- 127691 357 142915.44 37.12 100.00 127551- 98475 357 113226.34 29.90 100.00 98346- 6068 357 56170.96 20.58 100.00 6059- 3507 357 4518.82 4.93 82.91 3505- 531 361 2587.53 3.14 39.61 ------------------------------------------------------------------------------------ 7117511- 531 3574 492755.90 54.84 92.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 850316.08 87.88 100.00 1.41- 1.12 357 738619.57 70.57 98.32 1.12- 0.96 357 652963.45 75.16 98.88 0.96- 0.88 357 466319.62 58.96 94.12 0.88- 0.81 357 627563.06 68.84 97.48 0.81- 0.74 357 346837.94 41.58 93.28 0.73- 0.71 357 255537.94 35.67 89.64 0.71- 0.65 357 498058.72 50.37 95.24 0.65- 0.62 357 252463.28 29.65 73.95 0.62- 0.58 361 241692.39 30.04 81.16 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 492755.90 54.84 92.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:31:36 2018 Sorting 3574 observations 119 unique observations with > 7.00 F2/sig(F2) 3574 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 Total number of frames 622 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3574 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 Total number of frames 107 2875 observations > 7.00 F2/sig(F2) 2875 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 Total number of frames 106 Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 2875 removed 6 = 2869, unique = 126) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2869 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 Total number of frames 106 126 unique data precomputed (should be 126) 126 unique data with 2869 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 2869 removed 0 = 2869, unique = 126) 126 unique data precomputed (should be 126) 126 unique data with 2869 observations RMS deviation of equivalent data = 0.21068 Rint = 0.17668 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17599, wR= 0.22512 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09780, wR= 0.12703, Acormin=0.625, Acormax=1.371, Acor_av=0.953 F test: Probability=1.000, F= 3.233 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09023, wR= 0.11236, Acormin=0.591, Acormax=1.375, Acor_av=0.918 F test: Probability=1.000, F= 1.174 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08366, wR= 0.11334, Acormin=0.662, Acormax=1.431, Acor_av=0.965 F test: Probability=1.000, F= 1.161 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07374, wR= 0.09487, Acormin=0.563, Acormax=1.473, Acor_av=0.925 F test: Probability=1.000, F= 1.286 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06486, wR= 0.08553, Acormin=0.573, Acormax=1.378, Acor_av=0.902 F test: Probability=1.000, F= 1.289 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07575, wR= 0.10118, Acormin=0.660, Acormax=1.556, Acor_av=0.931 F test: Probability=0.000, F= 0.732 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06865, wR= 0.08813, Acormin=0.587, Acormax=1.535, Acor_av=0.910 F test: Probability=0.000, F= 0.891 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06038, wR= 0.07927, Acormin=0.574, Acormax=1.450, Acor_av=0.889 F test: Probability=1.000, F= 1.148 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05415, wR= 0.07244, Acormin=0.558, Acormax=1.402, Acor_av=0.858 F test: Probability=1.000, F= 1.238 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06734, wR= 0.08459, Acormin=0.429, Acormax=1.389, Acor_av=0.826 F test: Probability=0.000, F= 0.648 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06558, wR= 0.08238, Acormin=0.454, Acormax=1.422, Acor_av=0.836 F test: Probability=0.000, F= 0.682 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05865, wR= 0.07423, Acormin=0.239, Acormax=0.637, Acor_av=0.390 F test: Probability=0.000, F= 0.851 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05144, wR= 0.06687, Acormin=0.276, Acormax=0.709, Acor_av=0.438 F test: Probability=0.994, F= 1.101 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04740, wR= 0.06278, Acormin=0.275, Acormax=0.760, Acor_av=0.464 F test: Probability=1.000, F= 1.289 Final absorption model (ne=6, no=5): Rint= 0.05415, Acormin=0.558, Acormax=1.402, Acor_av=0.858 Combined refinement in use Rint: 0.17679 There are 106 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21068 Using Levenberg-Marquardt: 0.00010 New wR= 0.05293 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17668 with corrections 0.04092 Rint for all data: 0.17679 with corrections 0.04113 0 observations identified as outliers and rejected Cycle 2 wR= 0.05293 Using Levenberg-Marquardt: 0.00001 New wR= 0.04992 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17668 with corrections 0.03815 Rint for all data: 0.17679 with corrections 0.03836 0 observations identified as outliers and rejected Cycle 3 wR= 0.04992 Using Levenberg-Marquardt: 0.00000 New wR= 0.04928 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17668 with corrections 0.03751 Rint for all data: 0.17679 with corrections 0.03772 0 observations identified as outliers and rejected Cycle 4 wR= 0.04928 Using Levenberg-Marquardt: 0.00000 New wR= 0.04892 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17668 with corrections 0.03714 Rint for all data: 0.17679 with corrections 0.03735 0 observations identified as outliers and rejected Cycle 5 wR= 0.04892 Using Levenberg-Marquardt: 0.00000 New wR= 0.04867 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17668 with corrections 0.03689 Rint for all data: 0.17679 with corrections 0.03710 0 observations identified as outliers and rejected Final wR= 0.04867 Final frame scales: Min= 0.8001 Max= 1.1240 Final absorption correction factors: Amin= 0.5725 Amax= 1.5241 PROFFIT INFO: Inet (after scale3 abspack): min=575.7786 max=5500365.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=160.1047 max=72458.8984 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3574 reflections read from tmp file 554 reflections are rejected (553 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 5 3 3 0 4 3 8 125 Initial Chi^2= 0.35435 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.97664 Current error model SIG(F2)^2 = 114.41*I_RAW + 0.00*I_BACK+(0.01551*)^2 Cycle 2, Chi^2= 1.00279 Current error model SIG(F2)^2 = 96.12*I_RAW + 0.00*I_BACK+(0.01855*)^2 Cycle 3, Chi^2= 1.00033 Current error model SIG(F2)^2 = 100.26*I_RAW + 0.00*I_BACK+(0.01766*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 99.39*I_RAW + 0.00*I_BACK+(0.01787*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 99.60*I_RAW + 0.00*I_BACK+(0.01782*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 99.60*I_RAW + 0.00*I_BACK+(0.01782*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5500366- 1544968 357 2272276.60 51.12 100.00 1544445- 973862 357 1201731.17 43.35 100.00 971834- 311065 357 584464.77 41.57 100.00 310795- 197103 357 241564.63 34.36 100.00 196778- 164485 357 179440.39 27.23 100.00 164470- 123597 357 139115.19 21.72 100.00 123438- 98430 357 111044.50 18.73 100.00 98371- 5611 357 57247.72 13.97 100.00 5598- 3339 357 4256.60 4.74 99.44 3336- 576 361 2598.62 3.63 70.91 ------------------------------------------------------------------------------------ 5500366- 576 3574 478840.41 26.02 97.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 882129.76 40.64 100.00 1.41- 1.12 357 745823.94 31.91 100.00 1.12- 0.96 357 616989.05 30.82 99.44 0.96- 0.88 357 453926.87 26.05 98.60 0.88- 0.81 357 598858.72 30.57 98.60 0.81- 0.74 357 323955.88 21.05 97.76 0.73- 0.71 357 243808.32 19.80 96.36 0.71- 0.65 357 464960.03 25.24 97.76 0.65- 0.62 357 236549.04 16.75 87.68 0.62- 0.58 361 224255.04 17.44 93.91 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 478840.41 26.02 97.01 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 882129.76 40.64 100.00 4.82- 1.12 714 813976.85 36.27 100.00 4.82- 0.96 1071 748314.25 34.45 99.81 4.82- 0.88 1428 674717.41 32.35 99.51 4.82- 0.81 1785 659545.67 32.00 99.33 4.82- 0.74 2142 603614.04 30.17 99.07 4.82- 0.71 2499 552213.22 28.69 98.68 4.82- 0.65 2856 541306.57 28.26 98.56 4.82- 0.62 3213 507444.62 26.98 97.35 4.82- 0.58 3574 478840.41 26.02 97.01 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 478840.41 26.02 97.01 Scale applied to data: s=0.181806 (maximum obs:5500365.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.025: data 3574 -> merged 156 With outlier rejection... Rint 0.036; Rsigma 0.025: data 3565 -> merged 156 Rejected total: 9, method kkm 8, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585844, 4.830992 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 20.79 100.00 291 1.41 - 1.12 14 14 29.50 100.00 413 1.12 - 0.97 14 14 29.50 100.00 413 0.96 - 0.84 14 14 31.64 100.00 443 0.84 - 0.78 14 14 23.79 100.00 333 0.78 - 0.73 14 14 25.07 100.00 351 0.73 - 0.69 14 14 23.86 100.00 334 0.69 - 0.66 14 14 20.57 100.00 288 0.65 - 0.63 14 14 21.86 100.00 306 0.63 - 0.60 14 14 19.86 100.00 278 --------------------------------------------------------------- 8.37 - 0.60 140 140 24.64 100.00 3450 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:31:37 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367359 8.374665 8.360570 90.1026 89.9657 90.0060 3565 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2384 2386 3565 N (int>3sigma) = 0 0 0 0 1816 0 2310 2309 3458 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.1 26.1 26.0 Lattice type: F chosen Volume: 585.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.912 5.916 90.05 119.94 119.92 Niggli form: a.a = 34.946 b.b = 34.957 c.c = 34.999 b.c = -0.028 a.c = -17.452 a.b = -17.435 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.120 CUBIC F-lattice R(int) = 0.036 [ 3409] Vol = 585.9 Cell: 8.367 8.375 8.361 90.10 89.97 90.01 Volume: 585.86 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3128] Vol = 439.4 Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1008] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.036 [ 3163] Vol = 292.9 Cell: 5.920 5.919 8.361 89.95 89.90 89.95 Volume: 292.93 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.036 [ 3163] Vol = 292.9 Cell: 5.919 5.920 8.361 90.10 90.05 89.95 Volume: 292.93 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 3108] Vol = 292.9 Cell: 5.919 5.920 8.361 89.90 89.95 89.95 Volume: 292.93 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 3105] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 89.90 90.02 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 2764] Vol = 292.9 Cell: 5.920 5.919 8.361 90.05 90.10 89.95 Volume: 292.93 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.096 MONOCLINIC I-lattice R(int) = 0.032 [ 2763] Vol = 292.9 Cell: 5.912 5.922 8.367 90.03 90.02 90.10 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.044 MONOCLINIC I-lattice R(int) = 0.031 [ 2778] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 90.10 89.98 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.043 MONOCLINIC I-lattice R(int) = 0.033 [ 2762] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.03 89.90 Volume: 292.93 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.032 [ 2762] Vol = 292.9 Cell: 10.247 5.912 5.916 90.05 125.19 89.92 Volume: 292.93 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 2112] Vol = 146.5 Cell: 5.912 5.912 5.916 90.05 119.94 119.92 Volume: 146.46 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2384 2386 3565 N (int>3sigma) = 0 0 0 0 1816 0 2310 2309 3458 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.1 26.1 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 284 793 N I>3s 29 29 258 793 0.7 0.7 0.7 39.1 7.7 7.7 5.2 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.036 3145 Fd-3m 1 1 227 C N N N N 37 2284 0.037 3184 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367359 8.374665 8.360570 90.1026 89.9657 90.0060 ZERR 3.00 0.000435 0.000557 0.000556 0.0054 0.0049 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5306703- 1140066 571 568 26 21.8 1901809.05 48.67 0.032 0.042 1115222- 276865 566 563 26 21.7 670978.86 41.45 0.044 0.057 276117- 134537 817 816 26 31.4 191346.68 28.39 0.037 0.050 131300- 99070 579 579 26 22.3 116730.72 19.23 0.054 0.071 98318- 3936 551 549 26 21.1 33155.78 9.77 0.063 0.080 3904- 1860 490 490 26 18.8 3092.73 4.06 0.196 0.246 ------------------------------------------------------------------------------------------- 5306703- 1860 3574 3565 156 22.9 477260.19 25.98 0.036 0.048 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 668 664 26 25.5 724169.19 35.22 0.038 0.047 0.020 1.12-0.88 799 799 26 30.7 607303.68 29.83 0.028 0.040 0.023 0.85-0.75 662 661 26 25.4 459246.74 25.15 0.033 0.044 0.026 0.74-0.68 591 590 26 22.7 386987.75 22.90 0.040 0.050 0.028 0.67-0.63 570 570 26 21.9 231854.32 18.22 0.055 0.075 0.035 0.62-0.59 284 281 26 10.8 253760.76 17.43 0.050 0.055 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 3574 3565 156 22.9 477260.19 25.98 0.036 0.048 0.025 inf-0.60 3454 3448 139 24.8 487344.35 26.31 0.036 0.048 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 664 26 26 100.0 25.5 724169.19 194.21 0.038 0.006 1.12-0.88 799 26 26 100.0 30.7 607303.68 167.73 0.028 0.005 0.85-0.75 661 26 26 100.0 25.4 459246.74 134.23 0.033 0.005 0.74-0.68 590 26 26 100.0 22.7 386987.75 111.69 0.040 0.007 0.67-0.63 570 26 26 100.0 21.9 231854.32 85.22 0.055 0.008 0.62-0.59 281 27 26 96.3 10.8 253760.76 68.51 0.050 0.014 -------------------------------------------------------------------------------------------- inf-0.59 3565 157 156 99.4 22.9 477260.19 136.16 0.036 0.006 inf-0.60 3448 139 139 100.0 24.8 487344.35 139.13 0.036 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007471 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3674(4) 8.3747(6) 8.3606(5) 90.103(5) 89.966(5) 90.006(5) V = 585.86(6) unit cell: 8.36754(16) 8.36754(16) 8.36754(16) 90.0 90.0 90.0 V = 585.860(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3262192.3525 PROFFIT INFO: background sum: min=702.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11006.0000 PROFFIT INFO: num of signal pixels: min=56 max=881 PROFFIT INFO: Inet: min=530.6313 max=7117510.5000 PROFFIT INFO: sig(Inet): min=186.6679 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 6 164 558 928 1480 1626 2928 4740 6502 7148 Percent 0.0 0.1 2.3 7.8 13.0 20.7 22.7 41.0 66.3 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3574 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 3574 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117511- 1539705 357 2343116.29 134.25 100.00 1538340- 1001044 357 1254463.60 108.20 100.00 999967- 305134 357 586090.42 94.14 100.00 304280- 210545 357 248736.49 68.26 100.00 210481- 159018 357 181225.20 48.50 100.00 158934- 127691 357 142915.44 37.12 100.00 127551- 98475 357 113226.34 29.90 100.00 98346- 6068 357 56170.96 20.58 100.00 6059- 3507 357 4518.82 4.93 82.91 3505- 531 361 2587.53 3.14 39.61 ------------------------------------------------------------------------------------ 7117511- 531 3574 492755.90 54.84 92.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 850316.08 87.88 100.00 1.41- 1.12 357 738619.57 70.57 98.32 1.12- 0.96 357 652963.45 75.16 98.88 0.96- 0.88 357 466319.62 58.96 94.12 0.88- 0.81 357 627563.06 68.84 97.48 0.81- 0.74 357 346837.94 41.58 93.28 0.73- 0.71 357 255537.94 35.67 89.64 0.71- 0.65 357 498058.72 50.37 95.24 0.65- 0.62 357 252463.28 29.65 73.95 0.62- 0.58 361 241692.39 30.04 81.16 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 492755.90 54.84 92.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:31:38 2018 Sorting 3574 observations 86 unique observations with > 7.00 F2/sig(F2) 3574 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 Total number of frames 622 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3574 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 2875 observations > 7.00 F2/sig(F2) 2875 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 31.5 (Out of 2875 removed 4 = 2871, 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): 4/m3bar2/m 2871 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 91 unique data precomputed (should be 91) 91 unique data with 2871 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 31.5 (Out of 2871 removed 0 = 2871, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 2871 observations RMS deviation of equivalent data = 0.21107 Rint = 0.17674 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17564, wR= 0.22507 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09803, wR= 0.12797, Acormin=0.626, Acormax=1.368, Acor_av=0.952 F test: Probability=1.000, F= 3.204 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09031, wR= 0.11296, Acormin=0.591, Acormax=1.373, Acor_av=0.917 F test: Probability=1.000, F= 1.177 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08423, wR= 0.11516, Acormin=0.666, Acormax=1.416, Acor_av=0.964 F test: Probability=1.000, F= 1.147 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07440, wR= 0.09663, Acormin=0.565, Acormax=1.459, Acor_av=0.924 F test: Probability=1.000, F= 1.280 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06556, wR= 0.08705, Acormin=0.572, Acormax=1.361, Acor_av=0.899 F test: Probability=1.000, F= 1.285 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07699, wR= 0.10346, Acormin=0.658, Acormax=1.542, Acor_av=0.929 F test: Probability=0.000, F= 0.724 Trying model 7 (ne=6, no=1)... Results: Rint= 0.07020, wR= 0.09057, Acormin=0.578, Acormax=1.515, Acor_av=0.907 F test: Probability=0.000, F= 0.870 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06117, wR= 0.08135, Acormin=0.576, Acormax=1.431, Acor_av=0.885 F test: Probability=1.000, F= 1.143 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05468, wR= 0.07355, Acormin=0.553, Acormax=1.382, Acor_av=0.855 F test: Probability=1.000, F= 1.247 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06806, wR= 0.08645, Acormin=0.436, Acormax=1.376, Acor_av=0.822 F test: Probability=0.000, F= 0.646 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06628, wR= 0.08433, Acormin=0.460, Acormax=1.407, Acor_av=0.832 F test: Probability=0.000, F= 0.681 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05902, wR= 0.07545, Acormin=0.232, Acormax=0.615, Acor_av=0.379 F test: Probability=0.000, F= 0.856 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05151, wR= 0.06742, Acormin=0.272, Acormax=0.695, Acor_av=0.430 F test: Probability=0.998, F= 1.120 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04761, wR= 0.06344, Acormin=0.270, Acormax=0.744, Acor_av=0.456 F test: Probability=1.000, F= 1.303 Final absorption model (ne=6, no=5): Rint= 0.05468, Acormin=0.553, Acormax=1.382, Acor_av=0.855 Combined refinement in use Rint: 0.17685 There are 81 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: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21107 Using Levenberg-Marquardt: 0.00010 New wR= 0.05604 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17674 with corrections 0.04291 Rint for all data: 0.17685 with corrections 0.04312 3 observations identified as outliers and rejected Cycle 2 wR= 0.05578 Using Levenberg-Marquardt: 0.00001 New wR= 0.05246 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17565 with corrections 0.03975 Rint for all data: 0.17685 with corrections 0.04024 1 observations identified as outliers and rejected Cycle 3 wR= 0.05251 Using Levenberg-Marquardt: 0.00000 New wR= 0.05159 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17549 with corrections 0.03888 Rint for all data: 0.17685 with corrections 0.03939 1 observations identified as outliers and rejected Cycle 4 wR= 0.05160 Using Levenberg-Marquardt: 0.00000 New wR= 0.05108 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17521 with corrections 0.03839 Rint for all data: 0.17685 with corrections 0.03897 0 observations identified as outliers and rejected Cycle 5 wR= 0.05108 Using Levenberg-Marquardt: 0.00000 New wR= 0.05078 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17521 with corrections 0.03811 Rint for all data: 0.17685 with corrections 0.03869 0 observations identified as outliers and rejected Final wR= 0.05078 Final frame scales: Min= 0.8171 Max= 1.1231 Final absorption correction factors: Amin= 0.5520 Amax= 1.5118 PROFFIT INFO: Inet (after scale3 abspack): min=582.8835 max=5488821.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=160.7504 max=71500.2969 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3574 reflections read from tmp file 574 reflections are rejected (574 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 0 3 2 2 2 4 90 Initial Chi^2= 0.34778 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93225 Current error model SIG(F2)^2 = 112.42*I_RAW + 0.00*I_BACK+(0.01996*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 102.64*I_RAW + 0.00*I_BACK+(0.01971*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 102.64*I_RAW + 0.00*I_BACK+(0.01971*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5488822- 1537208 357 2275141.66 46.91 100.00 1537012- 976512 357 1203078.47 40.51 100.00 975959- 311384 357 584728.19 38.96 100.00 311098- 197748 357 241699.26 32.56 100.00 197555- 163935 357 179621.72 26.21 100.00 163859- 123197 357 139035.70 21.14 100.00 123177- 98348 357 110882.07 18.20 100.00 98265- 5648 357 57243.41 13.72 100.00 5641- 3364 357 4258.52 4.60 98.32 3364- 583 361 2593.44 3.59 69.53 ------------------------------------------------------------------------------------ 5488822- 583 3574 479294.13 24.62 96.75 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 883272.53 37.71 100.00 1.41- 1.12 357 746812.33 29.87 100.00 1.12- 0.96 357 617878.71 28.98 99.44 0.96- 0.88 357 454715.02 24.69 98.60 0.88- 0.81 357 599492.52 28.90 98.60 0.81- 0.74 357 324256.38 20.08 97.76 0.73- 0.71 357 243775.61 19.04 96.08 0.71- 0.65 357 464983.94 24.04 97.20 0.65- 0.62 357 236405.49 16.10 86.83 0.62- 0.58 361 224206.84 16.82 93.07 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 479294.13 24.62 96.75 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 883272.53 37.71 100.00 4.82- 1.12 714 815042.43 33.79 100.00 4.82- 0.96 1071 749321.19 32.19 99.81 4.82- 0.88 1428 675669.65 30.31 99.51 4.82- 0.81 1785 660434.22 30.03 99.33 4.82- 0.74 2142 604404.58 28.37 99.07 4.82- 0.71 2499 552886.16 27.04 98.64 4.82- 0.65 2856 541898.38 26.67 98.46 4.82- 0.62 3213 507954.73 25.49 97.17 4.82- 0.58 3574 479294.13 24.62 96.75 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 479294.13 24.62 96.75 Scale applied to data: s=0.182188 (maximum obs:5488821.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.026: data 3574 -> merged 109 With outlier rejection... Rint 0.038; Rsigma 0.026: data 3566 -> merged 109 Rejected total: 8, method kkm 6, method Blessing 2 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585845, 4.831004 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 21.50 100.00 215 1.61 - 1.21 10 10 33.10 100.00 331 1.17 - 1.01 10 10 42.60 100.00 426 0.99 - 0.89 10 10 42.20 100.00 422 0.88 - 0.81 10 10 40.30 100.00 403 0.81 - 0.74 10 10 34.30 100.00 343 0.73 - 0.71 10 10 38.40 100.00 384 0.70 - 0.66 10 10 31.90 100.00 319 0.66 - 0.64 10 10 30.60 100.00 306 0.63 - 0.60 10 10 30.10 100.00 301 --------------------------------------------------------------- 8.37 - 0.60 100 100 34.50 100.00 3450 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:31:37 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367359 8.374665 8.360570 90.1026 89.9657 90.0060 3565 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2384 2386 3565 N (int>3sigma) = 0 0 0 0 1816 0 2310 2309 3458 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.1 26.1 26.0 Lattice type: F chosen Volume: 585.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.912 5.916 90.05 119.94 119.92 Niggli form: a.a = 34.946 b.b = 34.957 c.c = 34.999 b.c = -0.028 a.c = -17.452 a.b = -17.435 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.120 CUBIC F-lattice R(int) = 0.036 [ 3409] Vol = 585.9 Cell: 8.367 8.375 8.361 90.10 89.97 90.01 Volume: 585.86 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3128] Vol = 439.4 Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1008] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.036 [ 3163] Vol = 292.9 Cell: 5.920 5.919 8.361 89.95 89.90 89.95 Volume: 292.93 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.036 [ 3163] Vol = 292.9 Cell: 5.919 5.920 8.361 90.10 90.05 89.95 Volume: 292.93 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 3108] Vol = 292.9 Cell: 5.919 5.920 8.361 89.90 89.95 89.95 Volume: 292.93 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 3105] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 89.90 90.02 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 2764] Vol = 292.9 Cell: 5.920 5.919 8.361 90.05 90.10 89.95 Volume: 292.93 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.096 MONOCLINIC I-lattice R(int) = 0.032 [ 2763] Vol = 292.9 Cell: 5.912 5.922 8.367 90.03 90.02 90.10 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.044 MONOCLINIC I-lattice R(int) = 0.031 [ 2778] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 90.10 89.98 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.043 MONOCLINIC I-lattice R(int) = 0.033 [ 2762] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.03 89.90 Volume: 292.93 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.032 [ 2762] Vol = 292.9 Cell: 10.247 5.912 5.916 90.05 125.19 89.92 Volume: 292.93 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 2112] Vol = 146.5 Cell: 5.912 5.912 5.916 90.05 119.94 119.92 Volume: 146.46 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2384 2386 3565 N (int>3sigma) = 0 0 0 0 1816 0 2310 2309 3458 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.1 26.1 26.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 284 793 N I>3s 29 29 258 793 0.7 0.7 0.7 39.1 7.7 7.7 5.2 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.036 3145 Fd-3m 1 1 227 C N N N N 37 2284 0.037 3184 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367359 8.374665 8.360570 90.1026 89.9657 90.0060 ZERR 3.00 0.000435 0.000557 0.000556 0.0054 0.0049 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5206429- 884648 794 791 27 29.3 1652510.72 42.93 0.035 0.047 882306- 152662 1060 1057 27 39.1 279287.70 31.80 0.042 0.050 142897- 51513 881 880 27 32.6 110681.89 18.37 0.056 0.072 21382- 1865 839 838 28 29.9 4594.68 4.68 0.156 0.197 ------------------------------------------------------------------------------------------- 5206429- 1865 3574 3566 109 32.7 477732.33 24.58 0.038 0.049 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 899 895 27 33.1 765396.09 33.69 0.036 0.048 0.022 1.01-0.78 1085 1085 27 40.2 467384.93 24.20 0.032 0.044 0.026 0.78-0.65 961 959 28 34.3 364290.00 20.82 0.042 0.051 0.030 0.65-0.59 629 627 27 23.2 258528.27 17.99 0.055 0.057 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3574 3566 109 32.7 477732.33 24.58 0.038 0.049 0.026 inf-0.60 3454 3448 99 34.8 487821.43 24.88 0.038 0.049 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 895 27 27 100.0 33.1 765396.09 217.74 0.036 0.006 1.01-0.78 1085 27 27 100.0 40.2 467384.93 163.38 0.032 0.004 0.78-0.65 959 28 28 100.0 34.3 364290.00 130.16 0.042 0.006 0.65-0.59 627 28 27 96.4 23.2 258528.27 101.22 0.055 0.011 -------------------------------------------------------------------------------------------- inf-0.59 3566 110 109 99.1 32.7 477732.33 157.16 0.038 0.006 inf-0.60 3448 99 99 100.0 34.8 487821.43 160.25 0.038 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:32:41 2018) ID: 2932; threads 38; handles 875; mem 517012.00 (1229536.00)kB; time: 1w 5d 23h 38m 11s MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1200.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:504.9,peak PF: 708.5, WS: 269.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:167.0, V:1202.0; MEMORY INFO: Process info - Handles: 876, Memory: PF:506.7,peak PF: 708.5, WS: 270.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:32:41 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) 8.37051 ( 0.00044 ) 8.37682 ( 0.00056 ) 8.35710 ( 0.00055 ) 90.12473 ( 0.00537 ) 89.98579 ( 0.00489 ) 90.00567 ( 0.00494 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:32:41 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(5) 90.125(5) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36754(16) 8.36754(16) 8.36754(16) 90.0 90.0 90.0 V = 585.860(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 269 | 1.147 ( 0.119) | 1.244 ( 0.409) | 1.318 ( 0.650) | 13.2-18.8 | 269 | 1.132 ( 0.071) | 1.179 ( 0.254) | 1.249 ( 0.559) | 18.9-23.0 | 269 | 1.142 ( 0.091) | 1.186 ( 0.269) | 1.256 ( 0.677) | 23.0-27.3 | 269 | 1.132 ( 0.098) | 1.173 ( 0.308) | 1.232 ( 0.567) | 27.3-30.4 | 269 | 1.135 ( 0.098) | 1.153 ( 0.245) | 1.192 ( 0.444) | 30.4-33.6 | 269 | 1.147 ( 0.101) | 1.136 ( 0.215) | 1.204 ( 0.443) | 33.6-37.0 | 269 | 1.141 ( 0.096) | 1.121 ( 0.195) | 1.163 ( 0.427) | 37.0-39.8 | 269 | 1.144 ( 0.119) | 1.091 ( 0.207) | 1.219 ( 0.505) | 39.8-42.8 | 269 | 1.163 ( 0.109) | 1.108 ( 0.257) | 1.216 ( 0.529) | 42.8-49.8 | 273 | 1.204 ( 0.152) | 1.123 ( 0.266) | 1.201 ( 0.478) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2694 | 1.149 ( 0.109) | 1.151 ( 0.272) | 1.225 ( 0.536) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.97 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0024 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:33:07 2018 PROFFITMAIN - Started at Wed Mar 28 14:33:07 2018 OTKP changes: 2682 2 4 6 OTKP changes: 2682 2 4 6 No constraint UB - matrix: -0.007489 0.076885 -0.034796 ( 0.000006 0.000006 0.000006 ) -0.083610 -0.011788 -0.008056 ( 0.000004 0.000004 0.000004 ) -0.012153 0.033663 0.077047 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007194 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007183 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000013 0.007212 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007489 0.076885 -0.034796 ( 0.000006 0.000006 0.000006 ) -0.083610 -0.011788 -0.008056 ( 0.000004 0.000004 0.000004 ) -0.012153 0.033663 0.077047 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 2686 obs out of 2694 (total:2694,skipped:0) (99.70%) unit cell: 8.3624(4) 8.3688(6) 8.3523(6) 90.106(5) 89.983(5) 90.006(5) V = 584.52(6) unit cell: 8.36117(14) 8.36117(14) 8.36117(14) 90.0 90.0 90.0 V = 584.523(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007132 0.076839 -0.034861 ( 0.000017 0.000012 0.000018 ) -0.083545 -0.011641 -0.008035 ( 0.000014 0.000010 0.000015 ) -0.012423 0.033796 0.076706 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007185 0.000005 -0.000033 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007182 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000033 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3680(13) 8.3697(14) 8.3805(15) 90.058(14) 89.736(14) 90.038(14) V = 586.95(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007242 0.076715 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011713 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007174 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007242 0.076715 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011713 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3741(12) 8.3580(15) 90.141(13) 89.821(13) 90.028(12) V = 585.42(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.42(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007242 0.076715 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011713 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007191 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007174 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007242 0.076715 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083581 -0.011713 -0.008076 ( 0.000013 0.000009 0.000014 ) -0.012371 0.033943 0.076880 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3643(13) 8.3741(12) 8.3580(15) 90.141(13) 89.821(13) 90.028(12) V = 585.42(16) unit cell: 8.3654(3) 8.3654(3) 8.3654(3) 90.0 90.0 90.0 V = 585.42(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084679 0.000099 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084758 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007170 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007184 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007195 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084679 0.000099 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084758 0.000095 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084826 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3764(16) 8.3686(8) 8.3618(10) 90.063(10) 89.870(13) 90.079(11) V = 586.15(14) unit cell: 8.3689(3) 8.3689(3) 8.3689(3) 90.0 90.0 90.0 V = 586.15(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007570 0.077005 -0.034601 ( 0.000015 0.000014 0.000012 ) -0.083443 -0.011879 -0.008153 ( 0.000011 0.000011 0.000009 ) -0.012255 0.033270 0.076970 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007170 0.000001 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007178 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3766(11) 8.3721(13) 8.3661(11) 89.946(12) 89.991(11) 90.004(12) V = 586.71(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.86(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.86(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.86(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.86(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077000 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083563 -0.011973 -0.008144 ( 0.000011 0.000010 0.000009 ) -0.012158 0.033309 0.076980 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3661(11) 8.3697(12) 8.3669(10) 90.004(10) 90.053(10) 90.093(11) V = 585.86(13) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.86(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007471 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076828 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2688 obs out of 2694 (total:2694,skipped:0) (99.78%) unit cell: 8.3674(4) 8.3747(6) 8.3606(6) 90.103(5) 89.966(5) 90.006(5) V = 585.86(6) unit cell: 8.36754(16) 8.36754(16) 8.36754(16) 90.0 90.0 90.0 V = 585.858(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region 29 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof 3574 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:33:14 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3262195.4919 PROFFIT INFO: background sum: min=702.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11006.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7117517.5000 PROFFIT INFO: sig(Inet): min=186.6696 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 3 82 279 464 740 813 1464 2370 3251 3574 Percent 0.0 0.1 2.3 7.8 13.0 20.7 22.7 41.0 66.3 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3574 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 3574 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117518- 1539708 357 2343142.28 134.25 100.00 1538345- 1001044 357 1254478.43 108.20 100.00 999967- 305135 357 586094.06 94.14 100.00 304281- 210562 357 248735.26 68.27 100.00 210545- 159022 357 181230.26 48.49 100.00 158935- 127691 357 142919.39 37.12 100.00 127551- 98475 357 113226.15 29.90 100.00 98364- 6068 357 56170.47 20.58 100.00 6059- 3505 357 4519.18 4.93 82.91 3502- 531 361 2587.52 3.14 39.61 ------------------------------------------------------------------------------------ 7117518- 531 3574 492761.09 54.85 92.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 850315.92 87.88 100.00 1.41- 1.12 357 738627.85 70.57 98.32 1.12- 0.96 357 652982.45 75.16 98.88 0.96- 0.88 357 466326.13 58.96 94.12 0.88- 0.81 357 627582.54 68.84 97.48 0.81- 0.74 357 346844.41 41.58 93.28 0.73- 0.71 357 255539.30 35.68 89.64 0.71- 0.65 357 498060.56 50.37 95.24 0.65- 0.62 357 252461.90 29.65 73.95 0.62- 0.58 361 241683.00 30.04 81.16 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 492761.09 54.85 92.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:33:15 2018 Sorting 3574 observations 119 unique observations with > 7.00 F2/sig(F2) 3574 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 Total number of frames 622 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3574 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 Total number of frames 107 2875 observations > 7.00 F2/sig(F2) 2875 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 Total number of frames 106 Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 2875 removed 6 = 2869, unique = 126) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2869 observations in 6 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 Total number of frames 106 126 unique data precomputed (should be 126) 126 unique data with 2869 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 2869 removed 0 = 2869, unique = 126) 126 unique data precomputed (should be 126) 126 unique data with 2869 observations RMS deviation of equivalent data = 0.21067 Rint = 0.17667 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17598, wR= 0.22512 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09780, wR= 0.12702, Acormin=0.625, Acormax=1.371, Acor_av=0.953 F test: Probability=1.000, F= 3.232 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09022, wR= 0.11235, Acormin=0.591, Acormax=1.375, Acor_av=0.918 F test: Probability=1.000, F= 1.174 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08365, wR= 0.11333, Acormin=0.661, Acormax=1.431, Acor_av=0.965 F test: Probability=1.000, F= 1.161 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07373, wR= 0.09485, Acormin=0.563, Acormax=1.473, Acor_av=0.925 F test: Probability=1.000, F= 1.286 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06486, wR= 0.08552, Acormin=0.573, Acormax=1.378, Acor_av=0.902 F test: Probability=1.000, F= 1.289 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07576, wR= 0.10118, Acormin=0.660, Acormax=1.556, Acor_av=0.931 F test: Probability=0.000, F= 0.732 Trying model 7 (ne=6, no=1)... Results: Rint= 0.06864, wR= 0.08813, Acormin=0.587, Acormax=1.535, Acor_av=0.910 F test: Probability=0.000, F= 0.891 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06039, wR= 0.07926, Acormin=0.574, Acormax=1.450, Acor_av=0.889 F test: Probability=1.000, F= 1.148 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05415, wR= 0.07243, Acormin=0.558, Acormax=1.401, Acor_av=0.858 F test: Probability=1.000, F= 1.238 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06734, wR= 0.08459, Acormin=0.429, Acormax=1.389, Acor_av=0.826 F test: Probability=0.000, F= 0.648 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06558, wR= 0.08237, Acormin=0.454, Acormax=1.422, Acor_av=0.836 F test: Probability=0.000, F= 0.682 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05865, wR= 0.07424, Acormin=0.239, Acormax=0.637, Acor_av=0.390 F test: Probability=0.000, F= 0.851 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05143, wR= 0.06687, Acormin=0.276, Acormax=0.709, Acor_av=0.438 F test: Probability=0.994, F= 1.101 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04741, wR= 0.06279, Acormin=0.275, Acormax=0.760, Acor_av=0.464 F test: Probability=1.000, F= 1.289 Final absorption model (ne=6, no=5): Rint= 0.05415, Acormin=0.558, Acormax=1.401, Acor_av=0.858 Combined refinement in use Rint: 0.17678 There are 106 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21067 Using Levenberg-Marquardt: 0.00010 New wR= 0.05291 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17667 with corrections 0.04085 Rint for all data: 0.17678 with corrections 0.04106 0 observations identified as outliers and rejected Cycle 2 wR= 0.05291 Using Levenberg-Marquardt: 0.00001 New wR= 0.04991 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17667 with corrections 0.03792 Rint for all data: 0.17678 with corrections 0.03813 0 observations identified as outliers and rejected Cycle 3 wR= 0.04991 Using Levenberg-Marquardt: 0.00000 New wR= 0.04925 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17667 with corrections 0.03723 Rint for all data: 0.17678 with corrections 0.03745 0 observations identified as outliers and rejected Cycle 4 wR= 0.04925 Using Levenberg-Marquardt: 0.00000 New wR= 0.04888 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17667 with corrections 0.03684 Rint for all data: 0.17678 with corrections 0.03705 0 observations identified as outliers and rejected Cycle 5 wR= 0.04888 Using Levenberg-Marquardt: 0.00000 New wR= 0.04864 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17667 with corrections 0.03660 Rint for all data: 0.17678 with corrections 0.03681 0 observations identified as outliers and rejected Final wR= 0.04864 Final frame scales: Min= 0.8037 Max= 1.1244 Final absorption correction factors: Amin= 0.5414 Amax= 1.5270 PROFFIT INFO: Inet (after scale3 abspack): min=580.1333 max=5498107.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=159.9406 max=71129.6172 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3574 reflections read from tmp file 548 reflections are rejected (547 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 4 3 2 1 3 3 7 127 Initial Chi^2= 0.35460 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.96928 Current error model SIG(F2)^2 = 114.72*I_RAW + 0.00*I_BACK+(0.01523*)^2 Cycle 2, Chi^2= 1.00121 Current error model SIG(F2)^2 = 98.97*I_RAW + 0.00*I_BACK+(0.01759*)^2 Cycle 3, Chi^2= 1.00015 Current error model SIG(F2)^2 = 101.48*I_RAW + 0.00*I_BACK+(0.01703*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 101.07*I_RAW + 0.00*I_BACK+(0.01713*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 101.14*I_RAW + 0.00*I_BACK+(0.01712*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 101.14*I_RAW + 0.00*I_BACK+(0.01712*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5498108- 1543406 357 2272945.94 52.77 100.00 1542686- 971734 357 1201428.52 44.23 100.00 969013- 311840 357 584613.48 42.41 100.00 310963- 197187 357 241561.23 34.73 100.00 197159- 164355 357 179436.28 27.37 100.00 164342- 123524 357 139020.43 21.68 100.00 123483- 98299 357 111058.87 18.72 100.00 98260- 5617 357 57224.17 13.91 100.00 5601- 3348 357 4255.23 4.70 99.16 3338- 580 361 2598.67 3.60 69.81 ------------------------------------------------------------------------------------ 5498108- 580 3574 478880.63 26.39 96.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 882307.53 41.67 100.00 1.41- 1.12 357 745987.41 32.58 100.00 1.12- 0.96 357 617629.90 31.36 99.44 0.96- 0.88 357 453786.99 26.39 98.60 0.88- 0.81 357 598902.30 31.01 98.60 0.81- 0.74 357 323734.20 21.24 97.76 0.73- 0.71 357 243663.43 19.90 96.08 0.71- 0.65 357 464934.76 25.50 97.48 0.65- 0.62 357 236442.33 16.83 87.39 0.62- 0.58 361 224270.24 17.50 93.35 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 478880.63 26.39 96.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 882307.53 41.67 100.00 4.82- 1.12 714 814147.47 37.13 100.00 4.82- 0.96 1071 748641.61 35.20 99.81 4.82- 0.88 1428 674927.96 33.00 99.51 4.82- 0.81 1785 659722.83 32.60 99.33 4.82- 0.74 2142 603724.72 30.71 99.07 4.82- 0.71 2499 552287.39 29.16 98.64 4.82- 0.65 2856 541368.32 28.71 98.49 4.82- 0.62 3213 507487.65 27.39 97.26 4.82- 0.58 3574 478880.63 26.39 96.87 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 478880.63 26.39 96.87 Scale applied to data: s=0.181881 (maximum obs:5498107.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.024: data 3574 -> merged 156 With outlier rejection... Rint 0.036; Rsigma 0.024: data 3564 -> merged 156 Rejected total: 10, method kkm 9, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585845, 4.830999 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 20.79 100.00 291 1.41 - 1.12 14 14 29.50 100.00 413 1.12 - 0.97 14 14 29.50 100.00 413 0.96 - 0.84 14 14 31.64 100.00 443 0.84 - 0.78 14 14 23.79 100.00 333 0.78 - 0.73 14 14 25.07 100.00 351 0.73 - 0.69 14 14 23.79 100.00 333 0.69 - 0.66 14 14 20.57 100.00 288 0.65 - 0.63 14 14 21.86 100.00 306 0.63 - 0.60 14 14 19.86 100.00 278 --------------------------------------------------------------- 8.37 - 0.60 140 140 24.64 100.00 3449 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:33:16 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367365 8.374698 8.360563 90.1026 89.9657 90.0058 3564 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2383 2385 3564 N (int>3sigma) = 0 0 0 0 1816 0 2305 2305 3452 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.6 0.0 26.4 26.4 26.3 Lattice type: F chosen Volume: 585.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.912 5.916 90.05 119.94 119.92 Niggli form: a.a = 34.946 b.b = 34.957 c.c = 34.999 b.c = -0.028 a.c = -17.452 a.b = -17.435 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.120 CUBIC F-lattice R(int) = 0.036 [ 3408] Vol = 585.9 Cell: 8.367 8.375 8.361 90.10 89.97 90.01 Volume: 585.86 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3127] Vol = 439.4 Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1008] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.035 [ 3162] Vol = 292.9 Cell: 5.920 5.919 8.361 89.95 89.90 89.95 Volume: 292.93 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.035 [ 3162] Vol = 292.9 Cell: 5.919 5.920 8.361 90.10 90.05 89.95 Volume: 292.93 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3107] Vol = 292.9 Cell: 5.919 5.920 8.361 89.90 89.95 89.95 Volume: 292.93 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 3104] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 89.90 90.02 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 2763] Vol = 292.9 Cell: 5.920 5.919 8.361 90.05 90.10 89.95 Volume: 292.93 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.097 MONOCLINIC I-lattice R(int) = 0.032 [ 2762] Vol = 292.9 Cell: 5.912 5.922 8.367 90.03 90.02 90.10 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.044 MONOCLINIC I-lattice R(int) = 0.031 [ 2777] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 90.10 89.98 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.044 MONOCLINIC I-lattice R(int) = 0.033 [ 2761] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.03 89.90 Volume: 292.93 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.032 [ 2761] Vol = 292.9 Cell: 10.247 5.912 5.916 90.05 125.19 89.92 Volume: 292.93 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 2111] Vol = 146.5 Cell: 5.912 5.912 5.916 90.05 119.94 119.92 Volume: 146.46 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2383 2385 3564 N (int>3sigma) = 0 0 0 0 1816 0 2305 2305 3452 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.6 0.0 26.4 26.4 26.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 284 793 N I>3s 29 29 256 793 0.7 0.7 0.7 39.1 7.7 7.7 5.2 29.9 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 0.036 3144 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3183 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367365 8.374698 8.360563 90.1026 89.9657 90.0058 ZERR 3.00 0.000435 0.000558 0.000556 0.0054 0.0049 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5267291- 1138320 571 567 26 21.8 1903234.67 50.09 0.031 0.042 1116416- 277001 566 563 26 21.7 670947.81 42.24 0.044 0.056 275878- 134025 817 816 26 31.4 191304.76 28.56 0.037 0.050 131581- 98951 579 579 26 22.3 116743.32 19.19 0.054 0.071 98182- 3935 551 549 26 21.1 33130.52 9.72 0.063 0.080 3911- 1860 490 490 26 18.8 3092.44 4.03 0.196 0.246 ------------------------------------------------------------------------------------------- 5267291- 1860 3574 3564 156 22.8 477070.90 26.35 0.036 0.048 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 668 664 26 25.5 724552.68 36.02 0.038 0.047 0.020 1.12-0.88 799 799 26 30.7 607404.98 30.32 0.028 0.039 0.022 0.85-0.75 662 661 26 25.4 459171.36 25.46 0.033 0.043 0.025 0.74-0.68 591 589 26 22.7 385240.66 23.08 0.039 0.047 0.028 0.67-0.63 570 570 26 21.9 231821.34 18.29 0.055 0.074 0.035 0.62-0.59 284 281 26 10.8 253750.74 17.51 0.050 0.053 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 3574 3564 156 22.8 477070.90 26.35 0.036 0.048 0.024 inf-0.60 3454 3447 139 24.8 487169.16 26.69 0.036 0.048 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 664 26 26 100.0 25.5 724552.68 198.28 0.038 0.006 1.12-0.88 799 26 26 100.0 30.7 607404.98 170.34 0.028 0.004 0.85-0.75 661 26 26 100.0 25.4 459171.36 135.80 0.033 0.005 0.74-0.68 589 26 26 100.0 22.7 385240.66 112.43 0.039 0.007 0.67-0.63 570 26 26 100.0 21.9 231821.34 85.47 0.055 0.008 0.62-0.59 281 27 26 96.3 10.8 253750.74 68.81 0.050 0.014 -------------------------------------------------------------------------------------------- inf-0.59 3564 157 156 99.4 22.8 477070.90 137.99 0.036 0.006 inf-0.60 3447 139 139 100.0 24.8 487169.16 141.02 0.036 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007471 0.076827 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076827 -0.034774 ( 0.000006 0.000006 0.000006 ) -0.083559 -0.011777 -0.008047 ( 0.000004 0.000004 0.000004 ) -0.012167 0.033648 0.076965 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3674(4) 8.3747(6) 8.3606(5) 90.103(5) 89.966(5) 90.006(5) V = 585.86(6) unit cell: 8.36756(16) 8.36756(16) 8.36756(16) 90.0 90.0 90.0 V = 585.863(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.968) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.968) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3262195.4919 PROFFIT INFO: background sum: min=702.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11006.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7117517.5000 PROFFIT INFO: sig(Inet): min=186.6696 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.44 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 6 164 558 928 1480 1626 2928 4740 6502 7148 Percent 0.0 0.1 2.3 7.8 13.0 20.7 22.7 41.0 66.3 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3574 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 3574 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7117518- 1539708 357 2343142.28 134.25 100.00 1538345- 1001044 357 1254478.43 108.20 100.00 999967- 305135 357 586094.06 94.14 100.00 304281- 210562 357 248735.26 68.27 100.00 210545- 159022 357 181230.26 48.49 100.00 158935- 127691 357 142919.39 37.12 100.00 127551- 98475 357 113226.15 29.90 100.00 98364- 6068 357 56170.47 20.58 100.00 6059- 3505 357 4519.18 4.93 82.91 3502- 531 361 2587.52 3.14 39.61 ------------------------------------------------------------------------------------ 7117518- 531 3574 492761.09 54.85 92.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 850315.92 87.88 100.00 1.41- 1.12 357 738627.85 70.57 98.32 1.12- 0.96 357 652982.45 75.16 98.88 0.96- 0.88 357 466326.13 58.96 94.12 0.88- 0.81 357 627582.54 68.84 97.48 0.81- 0.74 357 346844.41 41.58 93.28 0.73- 0.71 357 255539.30 35.68 89.64 0.71- 0.65 357 498060.56 50.37 95.24 0.65- 0.62 357 252461.90 29.65 73.95 0.62- 0.58 361 241683.00 30.04 81.16 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 492761.09 54.85 92.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:33:16 2018 Sorting 3574 observations 86 unique observations with > 7.00 F2/sig(F2) 3574 observations in 6 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 Total number of frames 622 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3574 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 2875 observations > 7.00 F2/sig(F2) 2875 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 31.5 (Out of 2875 removed 4 = 2871, 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): 4/m3bar2/m 2871 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 Total number of frames 81 91 unique data precomputed (should be 91) 91 unique data with 2871 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 31.5 (Out of 2871 removed 0 = 2871, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 2871 observations RMS deviation of equivalent data = 0.21106 Rint = 0.17674 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17564, wR= 0.22507 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09804, wR= 0.12796, Acormin=0.626, Acormax=1.368, Acor_av=0.952 F test: Probability=1.000, F= 3.204 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09031, wR= 0.11295, Acormin=0.591, Acormax=1.373, Acor_av=0.917 F test: Probability=1.000, F= 1.177 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08422, wR= 0.11515, Acormin=0.666, Acormax=1.416, Acor_av=0.964 F test: Probability=1.000, F= 1.147 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07439, wR= 0.09662, Acormin=0.565, Acormax=1.459, Acor_av=0.924 F test: Probability=1.000, F= 1.280 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06556, wR= 0.08703, Acormin=0.572, Acormax=1.360, Acor_av=0.899 F test: Probability=1.000, F= 1.284 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07699, wR= 0.10346, Acormin=0.658, Acormax=1.542, Acor_av=0.929 F test: Probability=0.000, F= 0.724 Trying model 7 (ne=6, no=1)... Results: Rint= 0.07019, wR= 0.09056, Acormin=0.578, Acormax=1.514, Acor_av=0.907 F test: Probability=0.000, F= 0.871 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06118, wR= 0.08134, Acormin=0.576, Acormax=1.430, Acor_av=0.885 F test: Probability=1.000, F= 1.143 Trying model 9 (ne=6, no=5)... Results: Rint= 0.05468, wR= 0.07354, Acormin=0.553, Acormax=1.382, Acor_av=0.855 F test: Probability=1.000, F= 1.247 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06806, wR= 0.08645, Acormin=0.436, Acormax=1.375, Acor_av=0.822 F test: Probability=0.000, F= 0.646 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06627, wR= 0.08433, Acormin=0.460, Acormax=1.407, Acor_av=0.832 F test: Probability=0.000, F= 0.681 Trying model 12 (ne=8, no=3)... Results: Rint= 0.05902, wR= 0.07545, Acormin=0.232, Acormax=0.615, Acor_av=0.379 F test: Probability=0.000, F= 0.856 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05149, wR= 0.06742, Acormin=0.272, Acormax=0.695, Acor_av=0.430 F test: Probability=0.999, F= 1.121 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04761, wR= 0.06344, Acormin=0.270, Acormax=0.743, Acor_av=0.456 F test: Probability=1.000, F= 1.304 Final absorption model (ne=6, no=5): Rint= 0.05468, Acormin=0.553, Acormax=1.382, Acor_av=0.855 Combined refinement in use Rint: 0.17685 There are 81 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: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21106 Using Levenberg-Marquardt: 0.00010 New wR= 0.05600 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17674 with corrections 0.04297 Rint for all data: 0.17685 with corrections 0.04318 3 observations identified as outliers and rejected Cycle 2 wR= 0.05572 Using Levenberg-Marquardt: 0.00001 New wR= 0.05234 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17565 with corrections 0.03971 Rint for all data: 0.17685 with corrections 0.04020 1 observations identified as outliers and rejected Cycle 3 wR= 0.05239 Using Levenberg-Marquardt: 0.00000 New wR= 0.05145 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17548 with corrections 0.03882 Rint for all data: 0.17685 with corrections 0.03933 1 observations identified as outliers and rejected Cycle 4 wR= 0.05146 Using Levenberg-Marquardt: 0.00000 New wR= 0.05094 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17520 with corrections 0.03834 Rint for all data: 0.17685 with corrections 0.03891 0 observations identified as outliers and rejected Cycle 5 wR= 0.05094 Using Levenberg-Marquardt: 0.00000 New wR= 0.05063 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17520 with corrections 0.03805 Rint for all data: 0.17685 with corrections 0.03863 0 observations identified as outliers and rejected Final wR= 0.05063 Final frame scales: Min= 0.8149 Max= 1.1223 Final absorption correction factors: Amin= 0.5554 Amax= 1.5177 PROFFIT INFO: Inet (after scale3 abspack): min=582.1468 max=5486688.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=160.4388 max=71518.3906 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3574 reflections read from tmp file 578 reflections are rejected (578 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 0 3 1 3 2 4 90 Initial Chi^2= 0.34661 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93887 Current error model SIG(F2)^2 = 111.91*I_RAW + 0.00*I_BACK+(0.01966*)^2 Cycle 2, Chi^2= 1.00003 Current error model SIG(F2)^2 = 101.66*I_RAW + 0.00*I_BACK+(0.01974*)^2 Cycle 3, Chi^2= 1.00004 Current error model SIG(F2)^2 = 102.48*I_RAW + 0.00*I_BACK+(0.01957*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 102.29*I_RAW + 0.00*I_BACK+(0.01961*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 102.29*I_RAW + 0.00*I_BACK+(0.01961*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5486689- 1539196 357 2275288.13 47.13 100.00 1537310- 978274 357 1203100.52 40.65 100.00 977831- 311572 357 584717.10 39.11 100.00 311465- 197600 357 241709.30 32.69 100.00 197420- 164010 357 179620.26 26.27 100.00 163875- 123197 357 139007.91 21.19 100.00 123136- 98350 357 110880.94 18.23 100.00 98334- 5645 357 57263.28 13.75 100.00 5632- 3368 357 4259.23 4.61 98.32 3362- 582 361 2593.45 3.60 69.25 ------------------------------------------------------------------------------------ 5486689- 582 3574 479309.87 24.70 96.73 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 883461.33 37.86 100.00 1.41- 1.12 357 746826.62 29.99 100.00 1.12- 0.96 357 617808.96 29.08 99.44 0.96- 0.88 357 454673.96 24.77 98.60 0.88- 0.81 357 599505.04 29.00 98.60 0.81- 0.74 357 324223.08 20.14 97.76 0.73- 0.71 357 243854.53 19.09 96.08 0.71- 0.65 357 465087.94 24.12 96.92 0.65- 0.62 357 236331.84 16.15 86.83 0.62- 0.58 361 224183.99 16.87 93.07 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 479309.87 24.70 96.73 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 357 883461.33 37.86 100.00 4.82- 1.12 714 815143.98 33.92 100.00 4.82- 0.96 1071 749365.64 32.31 99.81 4.82- 0.88 1428 675692.72 30.43 99.51 4.82- 0.81 1785 660455.18 30.14 99.33 4.82- 0.74 2142 604416.50 28.47 99.07 4.82- 0.71 2499 552907.65 27.13 98.64 4.82- 0.65 2856 541930.18 26.76 98.42 4.82- 0.62 3213 507974.81 25.58 97.14 4.82- 0.58 3574 479309.87 24.70 96.73 ------------------------------------------------------------------------------------ 4.82- 0.58 3574 479309.87 24.70 96.73 Scale applied to data: s=0.182259 (maximum obs:5486688.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.026: data 3574 -> merged 109 With outlier rejection... Rint 0.038; Rsigma 0.026: data 3566 -> merged 109 Rejected total: 8, method kkm 6, method Blessing 2 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585846, 4.831010 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 21.50 100.00 215 1.61 - 1.21 10 10 33.10 100.00 331 1.17 - 1.01 10 10 42.60 100.00 426 0.99 - 0.89 10 10 42.20 100.00 422 0.88 - 0.81 10 10 40.30 100.00 403 0.81 - 0.74 10 10 34.30 100.00 343 0.73 - 0.71 10 10 38.40 100.00 384 0.70 - 0.66 10 10 31.90 100.00 319 0.66 - 0.64 10 10 30.60 100.00 306 0.63 - 0.60 10 10 30.10 100.00 301 --------------------------------------------------------------- 8.37 - 0.60 100 100 34.50 100.00 3450 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:33:16 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367365 8.374698 8.360563 90.1026 89.9657 90.0058 3564 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2383 2385 3564 N (int>3sigma) = 0 0 0 0 1816 0 2305 2305 3452 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.6 0.0 26.4 26.4 26.3 Lattice type: F chosen Volume: 585.86 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.912 5.916 90.05 119.94 119.92 Niggli form: a.a = 34.946 b.b = 34.957 c.c = 34.999 b.c = -0.028 a.c = -17.452 a.b = -17.435 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.120 CUBIC F-lattice R(int) = 0.036 [ 3408] Vol = 585.9 Cell: 8.367 8.375 8.361 90.10 89.97 90.01 Volume: 585.86 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3127] Vol = 439.4 Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1008] Vol = 439.4 Trigonal Cell: 5.919 5.912 14.505 90.00 90.07 120.05 Volume: 439.39 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.035 [ 3162] Vol = 292.9 Cell: 5.920 5.919 8.361 89.95 89.90 89.95 Volume: 292.93 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.035 [ 3162] Vol = 292.9 Cell: 5.919 5.920 8.361 90.10 90.05 89.95 Volume: 292.93 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.071 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3107] Vol = 292.9 Cell: 5.919 5.920 8.361 89.90 89.95 89.95 Volume: 292.93 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 3104] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 89.90 90.02 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 2763] Vol = 292.9 Cell: 5.920 5.919 8.361 90.05 90.10 89.95 Volume: 292.93 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.097 MONOCLINIC I-lattice R(int) = 0.032 [ 2762] Vol = 292.9 Cell: 5.912 5.922 8.367 90.03 90.02 90.10 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.044 MONOCLINIC I-lattice R(int) = 0.031 [ 2777] Vol = 292.9 Cell: 5.912 8.367 5.922 89.97 90.10 89.98 Volume: 292.93 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.044 MONOCLINIC I-lattice R(int) = 0.033 [ 2761] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.03 89.90 Volume: 292.93 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.032 [ 2761] Vol = 292.9 Cell: 10.247 5.912 5.916 90.05 125.19 89.92 Volume: 292.93 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.029 [ 2111] Vol = 146.5 Cell: 5.912 5.912 5.916 90.05 119.94 119.92 Volume: 146.46 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1816 0 2383 2385 3564 N (int>3sigma) = 0 0 0 0 1816 0 2305 2305 3452 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.7 87.0 86.8 Mean int/sigma = 0.0 0.0 0.0 0.0 26.6 0.0 26.4 26.4 26.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 284 793 N I>3s 29 29 256 793 0.7 0.7 0.7 39.1 7.7 7.7 5.2 29.9 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 0.036 3144 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3183 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367365 8.374698 8.360563 90.1026 89.9657 90.0058 ZERR 3.00 0.000435 0.000558 0.000556 0.0054 0.0049 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5205542- 885746 794 791 27 29.3 1652615.91 43.11 0.035 0.047 881877- 152737 1060 1057 27 39.1 279284.36 31.91 0.042 0.050 142881- 51520 881 880 27 32.6 110672.69 18.41 0.055 0.072 21385- 1866 839 838 28 29.9 4594.88 4.69 0.156 0.197 ------------------------------------------------------------------------------------------- 5205542- 1866 3574 3566 109 32.7 477752.45 24.66 0.038 0.049 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 899 895 27 33.1 765485.77 33.82 0.036 0.048 0.022 1.01-0.78 1117 1117 28 39.9 454050.42 23.69 0.032 0.044 0.026 0.76-0.65 900 898 27 33.3 388966.39 22.10 0.041 0.051 0.030 0.65-0.59 658 656 27 24.3 247087.41 17.34 0.055 0.057 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3574 3566 109 32.7 477752.45 24.66 0.038 0.049 0.026 inf-0.60 3454 3448 99 34.8 487842.75 24.97 0.038 0.049 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 895 27 27 100.0 33.1 765485.77 218.56 0.036 0.006 1.01-0.78 1117 28 28 100.0 39.9 454050.42 159.78 0.032 0.004 0.76-0.65 898 27 27 100.0 33.3 388966.39 137.93 0.041 0.006 0.65-0.59 656 28 27 96.4 24.3 247087.41 98.03 0.055 0.011 -------------------------------------------------------------------------------------------- inf-0.59 3566 110 109 99.1 32.7 477752.45 157.67 0.038 0.006 inf-0.60 3448 99 99 100.0 34.8 487842.75 160.77 0.038 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:36:37 2018) ID: 2932; threads 39; handles 878; mem 517032.00 (1237728.00)kB; time: 1w 5d 23h 42m 8s MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:504.9,peak PF: 708.5, WS: 269.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:169.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.7,peak PF: 708.5, WS: 270.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:36:37 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) 8.37051 ( 0.00044 ) 8.37682 ( 0.00056 ) 8.35710 ( 0.00055 ) 90.12473 ( 0.00537 ) 89.98579 ( 0.00490 ) 90.00567 ( 0.00494 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:36:37 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000006 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007173 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000013 0.007198 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(6) 8.3571(5) 90.125(5) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36756(16) 8.36756(16) 8.36756(16) 90.0 90.0 90.0 V = 585.863(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 454 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 45 | 1.222 ( 0.087) | 1.214 ( 0.230) | 1.310 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 450 | 1.151 ( 0.112) | 1.180 ( 0.274) | 1.197 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007582 0.076666 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033515 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007176 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3734(11) 8.3945(13) 8.3922(11) 90.058(12) 89.976(11) 89.946(12) V = 589.89(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008034 ( 0.000010 0.000009 0.000007 ) -0.012119 0.033498 0.076868 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008034 ( 0.000010 0.000009 0.000007 ) -0.012119 0.033498 0.076868 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3741(9) 90.047(10) 90.025(10) 89.953(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008034 ( 0.000010 0.000009 0.000007 ) -0.012119 0.033498 0.076868 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034658 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008034 ( 0.000010 0.000009 0.000007 ) -0.012119 0.033498 0.076868 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3741(9) 90.047(10) 90.025(10) 89.953(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.138 ( 0.133) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.188 ( 0.062) | 1.141 ( 0.119) | 1.200 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb PROFFITPEAK info: 218 peaks in the peak location table UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) UB - matrix: -0.007486 0.076857 -0.034869 ( 0.000076 0.000078 0.000070 ) -0.083607 -0.011792 -0.008125 ( 0.000099 0.000102 0.000092 ) -0.012090 0.033482 0.076856 ( 0.000114 0.000118 0.000105 ) M - matrix: 0.007192 0.000006 0.000011 ( 0.000017 0.000011 0.000012 ) 0.000006 0.007167 -0.000011 ( 0.000011 0.000015 0.000012 ) 0.000011 -0.000011 0.007189 ( 0.000012 0.000012 0.000017 ) unit cell: 8.364(10) 8.378(8) 8.366(10) 89.91(9) 90.09(10) 90.05(9) V = 586(1) UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) UB - matrix: -0.007486 0.076857 -0.034869 ( 0.000076 0.000078 0.000070 ) -0.083607 -0.011792 -0.008125 ( 0.000099 0.000102 0.000092 ) -0.012090 0.033482 0.076856 ( 0.000114 0.000118 0.000105 ) M - matrix: 0.007192 0.000006 0.000011 ( 0.000017 0.000011 0.000012 ) 0.000006 0.007167 -0.000011 ( 0.000011 0.000015 0.000012 ) 0.000011 -0.000011 0.007189 ( 0.000012 0.000012 0.000017 ) unit cell: 8.364(10) 8.378(8) 8.366(10) 89.91(9) 90.09(10) 90.05(9) V = 586(1) OTKP changes: 25 1 1 1 UB - matrix: -0.007292 0.076613 -0.034530 ( 0.000078 0.000080 0.000072 ) -0.083191 -0.011530 -0.008114 ( 0.000098 0.000101 0.000091 ) -0.012105 0.033102 0.076499 ( 0.000112 0.000116 0.000103 ) M - matrix: 0.007120 -0.000000 0.000001 ( 0.000017 0.000011 0.000012 ) -0.000000 0.007098 -0.000020 ( 0.000011 0.000015 0.000011 ) 0.000001 -0.000020 0.007110 ( 0.000012 0.000011 0.000017 ) UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) unit cell: 8.406(10) 8.419(8) 8.412(10) 89.84(9) 90.01(10) 90.00(9) V = 595(1) UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) UB - matrix: -0.007292 0.076613 -0.034530 ( 0.000078 0.000080 0.000072 ) -0.083191 -0.011530 -0.008114 ( 0.000098 0.000101 0.000091 ) -0.012105 0.033102 0.076499 ( 0.000112 0.000116 0.000103 ) M - matrix: 0.007120 -0.000000 0.000001 ( 0.000017 0.000011 0.000012 ) -0.000000 0.007098 -0.000020 ( 0.000011 0.000015 0.000011 ) 0.000001 -0.000020 0.007110 ( 0.000012 0.000011 0.000017 ) unit cell: 8.406(10) 8.419(8) 8.412(10) 89.84(9) 90.01(10) 90.00(9) V = 595(1) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 122 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Run 7 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.369) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007292 0.076613 -0.034530 ( 0.000078 0.000080 0.000072 ) -0.083191 -0.011530 -0.008114 ( 0.000098 0.000101 0.000091 ) -0.012105 0.033102 0.076499 ( 0.000112 0.000116 0.000103 ) M - matrix: 0.007120 -0.000000 0.000001 ( 0.000017 0.000011 0.000012 ) -0.000000 0.007098 -0.000020 ( 0.000011 0.000015 0.000011 ) 0.000001 -0.000020 0.007110 ( 0.000012 0.000011 0.000017 ) UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) unit cell: 8.406(10) 8.419(8) 8.412(10) 89.84(9) 90.01(10) 90.00(9) V = 595(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 117 obs out of 122 (total:122,skipped:0) (95.90%) 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= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb 1 of 103 peaks identified as outliers and rejected 102 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 102 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 102 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 1.70 | 10 | 1.133 ( 0.455) | 1.127 ( 0.231) | 1.675 ( 0.937) | 1.61- 1.26 | 10 | 1.034 ( 0.056) | 1.076 ( 0.060) | 1.089 ( 0.533) | 1.21- 1.02 | 10 | 1.065 ( 0.061) | 1.076 ( 0.119) | 0.955 ( 0.285) | 0.99- 0.92 | 10 | 1.103 ( 0.042) | 1.098 ( 0.070) | 1.001 ( 0.475) | 0.92- 0.84 | 10 | 1.115 ( 0.048) | 1.092 ( 0.074) | 1.018 ( 0.412) | 0.84- 0.81 | 10 | 1.141 ( 0.051) | 1.117 ( 0.059) | 1.118 ( 0.481) | 0.78- 0.73 | 10 | 1.156 ( 0.039) | 1.122 ( 0.093) | 1.139 ( 0.447) | 0.73- 0.68 | 10 | 1.181 ( 0.029) | 1.122 ( 0.068) | 1.049 ( 0.343) | 0.67- 0.64 | 10 | 1.207 ( 0.050) | 1.230 ( 0.106) | 1.251 ( 0.282) | 0.64- 0.59 | 12 | 1.176 ( 0.085) | 1.198 ( 0.108) | 1.190 ( 0.325) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 0.59 | 102 | 1.132 ( 0.160) | 1.127 ( 0.120) | 1.149 ( 0.521) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) UB - matrix: -0.007429 0.076680 -0.034683 ( 0.000052 0.000055 0.000050 ) -0.083298 -0.011644 -0.008089 ( 0.000054 0.000058 0.000053 ) -0.011703 0.033411 0.076790 ( 0.000055 0.000058 0.000053 ) M - matrix: 0.007131 0.000009 0.000033 ( 0.000009 0.000007 0.000006 ) 0.000009 0.007132 0.000000 ( 0.000007 0.000009 0.000007 ) 0.000033 0.000000 0.007165 ( 0.000006 0.000007 0.000009 ) unit cell: 8.400(5) 8.399(5) 8.380(5) 90.00(5) 90.26(5) 90.07(5) V = 591.2(7) OTKP changes: 102 1 1 1 No constraint UB - matrix: -0.007401 0.076885 -0.034742 ( 0.000038 0.000041 0.000037 ) -0.083567 -0.011842 -0.008226 ( 0.000055 0.000059 0.000054 ) -0.012026 0.033560 0.076956 ( 0.000049 0.000052 0.000047 ) M - matrix: 0.007183 0.000017 0.000019 ( 0.000009 0.000006 0.000006 ) 0.000017 0.007178 0.000009 ( 0.000006 0.000007 0.000005 ) 0.000019 0.000009 0.007197 ( 0.000006 0.000005 0.000008 ) Constraint UB - matrix: -0.007401 0.076885 -0.034742 ( 0.000038 0.000041 0.000037 ) -0.083567 -0.011842 -0.008226 ( 0.000055 0.000059 0.000054 ) -0.012026 0.033560 0.076956 ( 0.000049 0.000052 0.000047 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) unit cell: 8.369(5) 8.372(4) 8.361(5) 90.07(4) 90.15(5) 90.14(5) V = 585.8(6) unit cell: 8.3674(7) 8.3674(7) 8.3674(7) 90.0 90.0 90.0 V = 585.83(9) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 272 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007401 0.076885 -0.034742 ( 0.000038 0.000041 0.000037 ) -0.083567 -0.011842 -0.008226 ( 0.000055 0.000059 0.000054 ) -0.012026 0.033560 0.076956 ( 0.000049 0.000052 0.000047 ) M - matrix: 0.007183 0.000017 0.000019 ( 0.000009 0.000006 0.000006 ) 0.000017 0.007178 0.000009 ( 0.000006 0.000007 0.000005 ) 0.000019 0.000009 0.007197 ( 0.000006 0.000005 0.000008 ) Constraint UB - matrix: -0.007401 0.076885 -0.034742 ( 0.000038 0.000041 0.000037 ) -0.083567 -0.011842 -0.008226 ( 0.000055 0.000059 0.000054 ) -0.012026 0.033560 0.076956 ( 0.000049 0.000052 0.000047 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) unit cell: 8.369(5) 8.372(4) 8.361(5) 90.07(4) 90.15(5) 90.14(5) V = 585.8(6) unit cell: 8.3674(7) 8.3674(7) 8.3674(7) 90.0 90.0 90.0 V = 585.83(9) 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! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb 1 of 105 peaks identified as outliers and rejected 104 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 104 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 104 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.70 | 10 | 1.082 ( 0.291) | 1.329 ( 0.791) | 1.630 ( 0.887) | 1.61- 1.26 | 10 | 1.040 ( 0.058) | 1.083 ( 0.060) | 1.077 ( 0.517) | 1.21- 1.09 | 10 | 1.087 ( 0.042) | 1.108 ( 0.085) | 0.966 ( 0.274) | 1.01- 0.93 | 10 | 1.089 ( 0.069) | 1.079 ( 0.109) | 0.862 ( 0.331) | 0.92- 0.84 | 10 | 1.115 ( 0.049) | 1.100 ( 0.083) | 1.046 ( 0.410) | 0.84- 0.81 | 10 | 1.145 ( 0.054) | 1.103 ( 0.066) | 1.057 ( 0.502) | 0.81- 0.73 | 10 | 1.157 ( 0.038) | 1.113 ( 0.075) | 1.097 ( 0.288) | 0.73- 0.70 | 10 | 1.177 ( 0.026) | 1.156 ( 0.072) | 1.063 ( 0.459) | 0.68- 0.64 | 10 | 1.205 ( 0.052) | 1.200 ( 0.089) | 1.177 ( 0.302) | 0.64- 0.59 | 14 | 1.180 ( 0.076) | 1.227 ( 0.119) | 1.224 ( 0.313) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 104 | 1.130 ( 0.116) | 1.153 ( 0.270) | 1.124 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 280 | 1.145 ( 0.117) | 1.241 ( 0.401) | 1.305 ( 0.642) | 13.2-18.8 | 280 | 1.134 ( 0.085) | 1.181 ( 0.282) | 1.247 ( 0.560) | 18.8-23.0 | 280 | 1.142 ( 0.090) | 1.193 ( 0.284) | 1.264 ( 0.676) | 23.0-27.3 | 280 | 1.129 ( 0.097) | 1.165 ( 0.293) | 1.212 ( 0.557) | 27.3-30.4 | 280 | 1.134 ( 0.098) | 1.149 ( 0.241) | 1.193 ( 0.446) | 30.4-33.6 | 280 | 1.146 ( 0.101) | 1.135 ( 0.213) | 1.197 ( 0.442) | 33.6-37.0 | 280 | 1.140 ( 0.096) | 1.120 ( 0.192) | 1.154 ( 0.424) | 37.0-39.9 | 280 | 1.146 ( 0.118) | 1.095 ( 0.205) | 1.225 ( 0.520) | 39.9-42.8 | 280 | 1.162 ( 0.108) | 1.109 ( 0.254) | 1.214 ( 0.524) | 42.8-49.8 | 278 | 1.204 ( 0.151) | 1.126 ( 0.264) | 1.200 ( 0.477) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2798 | 1.148 ( 0.110) | 1.151 ( 0.272) | 1.221 ( 0.535) | Fitted profile normalization line parameters e1 dimension: a=0.0019 b=0.96 e2 dimension: a=-0.0010 b=1.02 e3 dimension: a=-0.0024 b=1.12 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681623 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:37:06 2018 PROFFITMAIN - Started at Wed Mar 28 14:37:06 2018 OTKP changes: 2785 2 4 6 OTKP changes: 2785 2 4 6 No constraint UB - matrix: -0.007489 0.076887 -0.034799 ( 0.000006 0.000006 0.000006 ) -0.083609 -0.011786 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012147 0.033658 0.077049 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007194 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007183 0.000013 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000013 0.007212 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007489 0.076887 -0.034799 ( 0.000006 0.000006 0.000006 ) -0.083609 -0.011786 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012147 0.033658 0.077049 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 2790 obs out of 2798 (total:2798,skipped:0) (99.71%) unit cell: 8.3626(4) 8.3688(5) 8.3520(6) 90.101(5) 89.988(5) 90.006(5) V = 584.51(6) unit cell: 8.36112(14) 8.36112(14) 8.36112(14) 90.0 90.0 90.0 V = 584.513(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076875 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3772(11) 8.3756(13) 8.3740(10) 90.048(11) 90.021(10) 89.956(12) V = 587.55(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 811 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007130 0.076840 -0.034860 ( 0.000017 0.000012 0.000018 ) -0.083541 -0.011641 -0.008032 ( 0.000013 0.000009 0.000015 ) -0.012422 0.033791 0.076706 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007184 0.000005 -0.000033 ( 0.000002 0.000002 0.000002 ) 0.000005 0.007182 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000033 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3684(13) 8.3698(14) 8.3805(15) 90.054(14) 89.734(14) 90.039(14) V = 586.98(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007244 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083582 -0.011716 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033944 0.076882 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007192 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007244 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083582 -0.011716 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033944 0.076882 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3642(13) 8.3739(12) 8.3579(15) 90.142(13) 89.820(13) 90.029(12) V = 585.38(16) unit cell: 8.3653(3) 8.3653(3) 8.3653(3) 90.0 90.0 90.0 V = 585.38(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.966) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007244 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083582 -0.011716 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033944 0.076882 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007192 0.000004 -0.000023 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007175 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000023 0.000018 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007244 0.076716 -0.035019 ( 0.000015 0.000010 0.000016 ) -0.083582 -0.011716 -0.008075 ( 0.000013 0.000009 0.000014 ) -0.012372 0.033944 0.076882 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3642(13) 8.3739(12) 8.3579(15) 90.142(13) 89.820(13) 90.029(12) V = 585.38(16) unit cell: 8.3653(3) 8.3653(3) 8.3653(3) 90.0 90.0 90.0 V = 585.38(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084677 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084761 0.000096 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084827 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007170 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007184 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000008 0.007196 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084677 0.000102 -0.000193 ( 0.000016 0.000011 0.000018 ) 0.000017 0.084761 0.000096 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084827 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3765(16) 8.3683(8) 8.3617(10) 90.063(10) 89.870(13) 90.081(11) V = 586.13(14) unit cell: 8.3688(3) 8.3688(3) 8.3688(3) 90.0 90.0 90.0 V = 586.13(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007568 0.077002 -0.034599 ( 0.000015 0.000014 0.000012 ) -0.083440 -0.011876 -0.008157 ( 0.000011 0.000011 0.000009 ) -0.012253 0.033269 0.076971 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.007170 0.000001 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007177 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3769(11) 8.3724(13) 8.3661(11) 89.948(12) 89.994(11) 90.005(12) V = 586.75(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3660(11) 8.3696(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.84(13) unit cell: 8.3675(4) 8.3675(4) 8.3675(4) 90.0 90.0 90.0 V = 585.84(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.966) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3660(11) 8.3696(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.84(13) unit cell: 8.3675(4) 8.3675(4) 8.3675(4) 90.0 90.0 90.0 V = 585.84(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007188 0.000012 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000012 0.007182 0.000001 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000001 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007582 0.077002 -0.034560 ( 0.000013 0.000012 0.000011 ) -0.083565 -0.011974 -0.008143 ( 0.000011 0.000010 0.000009 ) -0.012157 0.033309 0.076981 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3660(11) 8.3696(12) 8.3669(10) 90.004(10) 90.053(10) 90.094(11) V = 585.84(13) unit cell: 8.3675(4) 8.3675(4) 8.3675(4) 90.0 90.0 90.0 V = 585.84(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) UB - matrix: -0.007471 0.076879 -0.034861 ( 0.000052 0.000055 0.000049 ) -0.083513 -0.011832 -0.008088 ( 0.000044 0.000047 0.000041 ) -0.011773 0.033656 0.077103 ( 0.000062 0.000065 0.000058 ) M - matrix: 0.007169 0.000018 0.000028 ( 0.000008 0.000006 0.000006 ) 0.000018 0.007183 0.000011 ( 0.000006 0.000010 0.000007 ) 0.000028 0.000011 0.007226 ( 0.000006 0.000007 0.000010 ) unit cell: 8.377(4) 8.369(5) 8.344(6) 90.08(5) 90.22(5) 90.14(5) V = 585.0(6) OTKP changes: 104 1 1 1 No constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007191 0.000018 0.000021 ( 0.000008 0.000006 0.000006 ) 0.000018 0.007191 0.000012 ( 0.000006 0.000009 0.000006 ) 0.000021 0.000012 0.007208 ( 0.000006 0.000006 0.000008 ) Constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) unit cell: 8.364(4) 8.365(5) 8.354(5) 90.10(5) 90.17(5) 90.14(4) V = 584.5(6) unit cell: 8.3611(7) 8.3611(7) 8.3611(7) 90.0 90.0 90.0 V = 584.50(8) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 261 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007191 0.000018 0.000021 ( 0.000008 0.000006 0.000006 ) 0.000018 0.007191 0.000012 ( 0.000006 0.000009 0.000006 ) 0.000021 0.000012 0.007208 ( 0.000006 0.000006 0.000008 ) Constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) unit cell: 8.364(4) 8.365(5) 8.354(5) 90.10(5) 90.17(5) 90.14(4) V = 584.5(6) unit cell: 8.3611(7) 8.3611(7) 8.3611(7) 90.0 90.0 90.0 V = 584.50(8) 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! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007191 0.000018 0.000021 ( 0.000008 0.000006 0.000006 ) 0.000018 0.007191 0.000012 ( 0.000006 0.000009 0.000006 ) 0.000021 0.000012 0.007208 ( 0.000006 0.000006 0.000008 ) Constraint UB - matrix: -0.007396 0.076933 -0.034779 ( 0.000047 0.000049 0.000044 ) -0.083613 -0.011876 -0.008291 ( 0.000045 0.000048 0.000042 ) -0.012070 0.033630 0.077006 ( 0.000055 0.000058 0.000051 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) unit cell: 8.364(4) 8.365(5) 8.354(5) 90.10(5) 90.17(5) 90.14(4) V = 584.5(6) unit cell: 8.3611(7) 8.3611(7) 8.3611(7) 90.0 90.0 90.0 V = 584.50(8) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007471 0.076831 -0.034777 ( 0.000006 0.000005 0.000006 ) -0.083560 -0.011774 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033644 0.076968 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007174 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000012 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076831 -0.034777 ( 0.000006 0.000005 0.000006 ) -0.083560 -0.011774 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033644 0.076968 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2792 obs out of 2798 (total:2798,skipped:0) (99.79%) unit cell: 8.3673(4) 8.3746(5) 8.3602(5) 90.099(5) 89.971(5) 90.005(5) V = 585.82(6) unit cell: 8.36735(15) 8.36735(15) 8.36735(15) 90.0 90.0 90.0 V = 585.819(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region 29 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof 3712 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:37:14 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.966) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.966) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3261638.0656 PROFFIT INFO: background sum: min=486.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11068.0000 PROFFIT INFO: num of signal pixels: min=56 max=883 PROFFIT INFO: Inet: min=530.6313 max=7116301.5000 PROFFIT INFO: sig(Inet): min=187.5980 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 90 296 486 767 850 1533 2474 3378 3712 Percent 0.0 0.1 2.4 8.0 13.1 20.7 22.9 41.3 66.6 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3712 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 3712 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7116302- 1533447 371 2327028.98 134.39 100.00 1532747- 976853 371 1240588.61 107.34 100.00 976310- 303997 371 569115.90 93.55 100.00 303673- 209635 371 247806.79 68.07 100.00 209312- 157808 371 179738.46 48.34 100.00 157734- 125338 371 141255.33 36.73 100.00 125254- 95496 371 111141.92 29.59 100.00 95226- 6053 371 53189.37 20.29 100.00 6031- 3439 371 4466.19 4.88 82.21 3438- 531 373 2512.11 3.10 38.34 ------------------------------------------------------------------------------------ 7116302- 531 3712 487422.96 54.60 92.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 846224.29 87.62 100.00 1.41- 1.12 371 733611.61 70.40 98.38 1.12- 0.96 371 644305.88 74.89 98.38 0.96- 0.88 371 461586.21 58.73 94.34 0.88- 0.81 371 624712.97 68.95 97.30 0.81- 0.74 371 329000.39 40.46 92.45 0.74- 0.71 371 262360.82 36.24 88.68 0.71- 0.65 371 486700.68 49.52 95.42 0.65- 0.62 371 248447.96 29.41 74.12 0.62- 0.58 373 238620.02 29.91 81.23 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 487422.96 54.60 92.03 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:37:14 2018 Sorting 3712 observations 120 unique observations with > 7.00 F2/sig(F2) 3712 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 24 647 Total number of frames 647 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3712 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 7 0 4 112 Total number of frames 112 2985 observations > 7.00 F2/sig(F2) 2985 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 4 111 Total number of frames 111 Removing 'redundancy=1' reflections Average redundancy: 23.5 (Out of 2985 removed 5 = 2980, 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 2980 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 4 111 Total number of frames 111 127 unique data precomputed (should be 127) 127 unique data with 2980 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.5 (Out of 2980 removed 0 = 2980, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 2980 observations RMS deviation of equivalent data = 0.22062 Rint = 0.18319 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18253, wR= 0.23494 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11502, wR= 0.16125, Acormin=0.635, Acormax=1.341, Acor_av=0.949 F test: Probability=1.000, F= 2.514 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10420, wR= 0.13636, Acormin=0.564, Acormax=1.352, Acor_av=0.905 F test: Probability=1.000, F= 1.217 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09876, wR= 0.14321, Acormin=0.633, Acormax=1.427, Acor_av=0.962 F test: Probability=0.997, F= 1.111 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08464, wR= 0.11536, Acormin=0.520, Acormax=1.488, Acor_av=0.917 F test: Probability=1.000, F= 1.360 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07708, wR= 0.10680, Acormin=0.519, Acormax=1.404, Acor_av=0.886 F test: Probability=1.000, F= 1.203 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09054, wR= 0.13203, Acormin=0.644, Acormax=1.515, Acor_av=0.926 F test: Probability=0.000, F= 0.724 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08068, wR= 0.11041, Acormin=0.528, Acormax=1.502, Acor_av=0.901 F test: Probability=0.000, F= 0.911 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07363, wR= 0.10197, Acormin=0.508, Acormax=1.411, Acor_av=0.873 F test: Probability=0.989, F= 1.091 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07182, wR= 0.09830, Acormin=0.452, Acormax=1.313, Acor_av=0.805 F test: Probability=0.889, F= 1.047 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08223, wR= 0.10971, Acormin=0.295, Acormax=1.328, Acor_av=0.793 F test: Probability=0.000, F= 0.800 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08032, wR= 0.10703, Acormin=0.331, Acormax=1.361, Acor_av=0.806 F test: Probability=0.000, F= 0.837 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07302, wR= 0.09808, Acormin=0.145, Acormax=0.425, Acor_av=0.261 F test: Probability=0.611, F= 1.011 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06689, wR= 0.09200, Acormin=0.163, Acormax=0.459, Acor_av=0.283 F test: Probability=1.000, F= 1.200 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06243, wR= 0.08741, Acormin=0.164, Acormax=0.487, Acor_av=0.298 F test: Probability=1.000, F= 1.370 Final absorption model (ne=6, no=3): Rint= 0.07363, Acormin=0.508, Acormax=1.411, Acor_av=0.873 Combined refinement in use Rint: 0.18331 There are 111 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 147 pars with 10878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22062 Using Levenberg-Marquardt: 0.00010 New wR= 0.05729 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18319 with corrections 0.04527 Rint for all data: 0.18331 with corrections 0.04548 1 observations identified as outliers and rejected Cycle 2 wR= 0.05723 Using Levenberg-Marquardt: 0.00001 New wR= 0.05240 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.04010 Rint for all data: 0.18331 with corrections 0.04035 0 observations identified as outliers and rejected Cycle 3 wR= 0.05240 Using Levenberg-Marquardt: 0.00000 New wR= 0.05159 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.03929 Rint for all data: 0.18331 with corrections 0.03953 0 observations identified as outliers and rejected Cycle 4 wR= 0.05159 Using Levenberg-Marquardt: 0.00000 New wR= 0.05118 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.03887 Rint for all data: 0.18331 with corrections 0.03910 0 observations identified as outliers and rejected Cycle 5 wR= 0.05118 Using Levenberg-Marquardt: 0.00000 New wR= 0.05093 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.03861 Rint for all data: 0.18331 with corrections 0.03884 0 observations identified as outliers and rejected Final wR= 0.05093 Final frame scales: Min= 0.7930 Max= 1.2353 Final absorption correction factors: Amin= 0.5615 Amax= 1.5768 PROFFIT INFO: Inet (after scale3 abspack): min=557.0052 max=5377269.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=157.3514 max=68013.2422 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 3712 reflections read from tmp file 583 reflections are rejected (583 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 5 2 2 2 3 2 5 130 Initial Chi^2= 0.37999 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.87163 Current error model SIG(F2)^2 = 123.25*I_RAW + 0.00*I_BACK+(0.02014*)^2 Cycle 2, Chi^2= 1.00013 Current error model SIG(F2)^2 = 109.34*I_RAW + 0.00*I_BACK+(0.01837*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 108.96*I_RAW + 0.00*I_BACK+(0.01846*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 109.04*I_RAW + 0.00*I_BACK+(0.01844*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 109.04*I_RAW + 0.00*I_BACK+(0.01844*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5377270- 1498838 371 2228783.87 49.28 100.00 1488659- 945980 371 1179059.08 41.58 100.00 945686- 310047 371 573752.47 39.76 100.00 309865- 192964 371 237618.03 32.86 100.00 192954- 160501 371 175706.75 26.14 100.00 160468- 120957 371 135952.91 20.66 100.00 120698- 96193 371 108682.06 17.72 100.00 96189- 5526 371 55700.53 13.18 100.00 5514- 3257 371 4156.55 4.49 96.77 3255- 557 373 2533.48 3.44 62.20 ------------------------------------------------------------------------------------ 5377270- 557 3712 469942.60 24.90 95.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 864749.30 39.04 100.00 1.41- 1.12 371 730279.83 30.65 99.19 1.12- 0.96 371 605541.28 29.43 98.92 0.96- 0.88 371 445672.62 25.01 98.11 0.88- 0.81 371 596877.41 29.37 98.38 0.81- 0.74 371 305999.02 19.88 96.50 0.74- 0.71 371 246961.92 19.14 94.61 0.71- 0.65 371 451796.93 23.89 96.77 0.65- 0.62 371 232986.56 15.95 84.91 0.62- 0.58 373 219909.02 16.68 91.42 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 469942.60 24.90 95.88 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 864749.30 39.04 100.00 4.82- 1.12 742 797514.57 34.84 99.60 4.82- 0.96 1113 733523.47 33.04 99.37 4.82- 0.88 1484 661560.76 31.03 99.06 4.82- 0.81 1855 648624.09 30.70 98.92 4.82- 0.74 2226 591519.91 28.90 98.52 4.82- 0.71 2597 542297.34 27.50 97.96 4.82- 0.65 2968 530984.79 27.05 97.81 4.82- 0.62 3339 497873.87 25.82 96.38 4.82- 0.58 3712 469942.60 24.90 95.88 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 469942.60 24.90 95.88 Scale applied to data: s=0.185968 (maximum obs:5377269.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.026: data 3712 -> merged 156 With outlier rejection... Rint 0.038; Rsigma 0.026: data 3701 -> merged 156 Rejected total: 11, method kkm 9, method Blessing 2 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585831, 4.830890 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 21.57 100.00 302 1.41 - 1.12 14 14 30.71 100.00 430 1.12 - 0.97 14 14 30.71 100.00 430 0.96 - 0.84 14 14 32.71 100.00 458 0.84 - 0.78 14 14 25.00 100.00 350 0.78 - 0.73 14 14 25.93 100.00 363 0.73 - 0.69 14 14 25.07 100.00 351 0.69 - 0.66 14 14 21.07 100.00 295 0.65 - 0.63 14 14 22.86 100.00 320 0.63 - 0.60 14 14 20.43 100.00 286 --------------------------------------------------------------- 8.36 - 0.60 140 140 25.61 100.00 3585 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:37:15 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367314 8.374551 8.360195 90.0986 89.9708 90.0047 3701 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1884 0 2472 2475 3701 N (int>3sigma) = 0 0 0 0 1884 0 2369 2370 3548 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 87.1 87.6 87.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 24.9 24.9 24.9 Lattice type: F chosen Volume: 585.82 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.913 5.916 90.05 119.93 119.92 Niggli form: a.a = 34.946 b.b = 34.958 c.c = 34.994 b.c = -0.030 a.c = -17.451 a.b = -17.436 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.122 CUBIC F-lattice R(int) = 0.038 [ 3545] Vol = 585.8 Cell: 8.367 8.375 8.360 90.10 89.97 90.00 Volume: 585.82 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 3263] Vol = 439.4 Cell: 5.919 5.913 14.504 90.00 90.07 120.05 Volume: 439.36 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1055] Vol = 439.4 Trigonal Cell: 5.919 5.913 14.504 90.00 90.07 120.05 Volume: 439.36 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.055 TETRAGONAL I-lattice R(int) = 0.037 [ 3299] Vol = 292.9 Cell: 5.919 5.919 8.360 89.95 89.91 89.95 Volume: 292.91 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.128 TETRAGONAL I-lattice R(int) = 0.037 [ 3299] Vol = 292.9 Cell: 5.919 5.919 8.360 90.09 90.05 89.95 Volume: 292.91 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.066 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3244] Vol = 292.9 Cell: 5.919 5.919 8.360 89.91 89.95 89.95 Volume: 292.91 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 3240] Vol = 292.9 Cell: 5.912 8.367 5.922 89.98 89.90 90.02 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.036 [ 2900] Vol = 292.9 Cell: 5.919 5.919 8.360 90.05 90.09 89.95 Volume: 292.91 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.094 MONOCLINIC I-lattice R(int) = 0.035 [ 2897] Vol = 292.9 Cell: 5.912 5.922 8.367 90.02 90.02 90.10 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.037 MONOCLINIC I-lattice R(int) = 0.033 [ 2912] Vol = 292.9 Cell: 5.912 8.367 5.922 89.98 90.10 89.98 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.044 MONOCLINIC I-lattice R(int) = 0.035 [ 2897] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.02 89.90 Volume: 292.91 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.035 [ 2896] Vol = 292.9 Cell: 10.247 5.913 5.916 90.05 125.19 89.92 Volume: 292.91 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2246] Vol = 146.5 Cell: 5.912 5.913 5.916 90.05 119.93 119.92 Volume: 146.45 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1884 0 2472 2475 3701 N (int>3sigma) = 0 0 0 0 1884 0 2369 2370 3548 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 87.1 87.6 87.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 24.9 24.9 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.184 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 35 35 294 825 N I>3s 28 28 258 825 0.7 0.7 0.7 39.1 7.5 7.5 5.0 28.2 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 0.038 3271 Fd-3m 1 1 227 C N N N N 37 2284 0.039 3310 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367314 8.374551 8.360195 90.0986 89.9708 90.0047 ZERR 3.00 0.000430 0.000541 0.000544 0.0053 0.0048 0.0048 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5137356- 1126527 597 594 26 22.8 1860954.95 46.75 0.033 0.046 1092626- 271209 586 581 26 22.3 654743.26 39.67 0.047 0.059 270976- 131207 850 849 26 32.7 187223.79 27.07 0.039 0.052 128016- 95706 621 621 26 23.9 113622.60 18.21 0.055 0.073 93471- 3829 536 534 26 20.5 30435.47 9.11 0.068 0.091 3753- 1819 522 522 26 20.1 3051.52 3.87 0.198 0.249 ------------------------------------------------------------------------------------------- 5137356- 1819 3712 3701 156 23.7 468298.07 24.85 0.038 0.051 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 695 690 26 26.5 710800.66 33.79 0.038 0.050 0.021 1.12-0.88 830 830 26 31.9 595211.34 28.58 0.031 0.042 0.024 0.85-0.75 689 688 26 26.5 450429.53 24.01 0.035 0.048 0.027 0.74-0.68 615 614 26 23.6 380464.62 21.86 0.043 0.054 0.030 0.67-0.63 592 592 26 22.8 226117.33 17.31 0.057 0.079 0.037 0.62-0.59 291 287 26 11.0 248540.13 16.61 0.054 0.056 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3712 3701 156 23.7 468298.07 24.85 0.038 0.051 0.026 inf-0.60 3590 3583 139 25.8 477974.02 25.16 0.038 0.051 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 690 26 26 100.0 26.5 710800.66 190.33 0.038 0.006 1.12-0.88 830 26 26 100.0 31.9 595211.34 163.71 0.031 0.005 0.85-0.75 688 26 26 100.0 26.5 450429.53 131.08 0.035 0.005 0.74-0.68 614 26 26 100.0 23.6 380464.62 108.84 0.043 0.007 0.67-0.63 592 26 26 100.0 22.8 226117.33 82.41 0.057 0.008 0.62-0.59 287 27 26 96.3 11.0 248540.13 66.10 0.054 0.015 -------------------------------------------------------------------------------------------- inf-0.59 3701 157 156 99.4 23.7 468298.07 132.93 0.038 0.007 inf-0.60 3583 139 139 100.0 25.8 477974.02 135.78 0.038 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007472 0.076831 -0.034777 ( 0.000006 0.000005 0.000006 ) -0.083560 -0.011774 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033644 0.076967 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007174 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000012 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007472 0.076831 -0.034777 ( 0.000006 0.000005 0.000006 ) -0.083560 -0.011774 -0.008051 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033644 0.076967 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3673(4) 8.3745(5) 8.3602(5) 90.099(5) 89.971(5) 90.005(5) V = 585.82(6) unit cell: 8.36736(15) 8.36736(15) 8.36736(15) 90.0 90.0 90.0 V = 585.822(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.966) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.966) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3261638.0656 PROFFIT INFO: background sum: min=486.0000 max=17427.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11068.0000 PROFFIT INFO: num of signal pixels: min=56 max=883 PROFFIT INFO: Inet: min=530.6313 max=7116301.5000 PROFFIT INFO: sig(Inet): min=187.5980 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=308.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 8 180 592 972 1534 1700 3066 4948 6756 7424 Percent 0.0 0.1 2.4 8.0 13.1 20.7 22.9 41.3 66.6 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3712 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 3712 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7116302- 1533447 371 2327028.98 134.39 100.00 1532747- 976853 371 1240588.61 107.34 100.00 976310- 303997 371 569115.90 93.55 100.00 303673- 209635 371 247806.79 68.07 100.00 209312- 157808 371 179738.46 48.34 100.00 157734- 125338 371 141255.33 36.73 100.00 125254- 95496 371 111141.92 29.59 100.00 95226- 6053 371 53189.37 20.29 100.00 6031- 3439 371 4466.19 4.88 82.21 3438- 531 373 2512.11 3.10 38.34 ------------------------------------------------------------------------------------ 7116302- 531 3712 487422.96 54.60 92.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 846224.29 87.62 100.00 1.41- 1.12 371 733611.61 70.40 98.38 1.12- 0.96 371 644305.88 74.89 98.38 0.96- 0.88 371 461586.21 58.73 94.34 0.88- 0.81 371 624712.97 68.95 97.30 0.81- 0.74 371 329000.39 40.46 92.45 0.74- 0.71 371 262360.82 36.24 88.68 0.71- 0.65 371 486700.68 49.52 95.42 0.65- 0.62 371 248447.96 29.41 74.12 0.62- 0.58 373 238620.02 29.91 81.23 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 487422.96 54.60 92.03 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:37:16 2018 Sorting 3712 observations 86 unique observations with > 7.00 F2/sig(F2) 3712 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 24 647 Total number of frames 647 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3712 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 3 85 Total number of frames 85 2985 observations > 7.00 F2/sig(F2) 2985 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 3 85 Total number of frames 85 Removing 'redundancy=1' reflections Average redundancy: 32.8 (Out of 2985 removed 4 = 2981, 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): 4/m3bar2/m 2981 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 3 85 Total number of frames 85 91 unique data precomputed (should be 91) 91 unique data with 2981 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 32.8 (Out of 2981 removed 0 = 2981, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 2981 observations RMS deviation of equivalent data = 0.22104 Rint = 0.18339 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18236, wR= 0.23507 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11501, wR= 0.16251, Acormin=0.636, Acormax=1.337, Acor_av=0.949 F test: Probability=1.000, F= 2.510 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10452, wR= 0.13703, Acormin=0.564, Acormax=1.350, Acor_av=0.904 F test: Probability=1.000, F= 1.209 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09943, wR= 0.14535, Acormin=0.640, Acormax=1.420, Acor_av=0.961 F test: Probability=0.996, F= 1.103 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08573, wR= 0.11704, Acormin=0.521, Acormax=1.480, Acor_av=0.915 F test: Probability=1.000, F= 1.344 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07773, wR= 0.10842, Acormin=0.517, Acormax=1.413, Acor_av=0.882 F test: Probability=1.000, F= 1.213 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09185, wR= 0.13392, Acormin=0.637, Acormax=1.502, Acor_av=0.924 F test: Probability=0.000, F= 0.715 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08242, wR= 0.11221, Acormin=0.521, Acormax=1.484, Acor_av=0.899 F test: Probability=0.000, F= 0.888 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07437, wR= 0.10365, Acormin=0.508, Acormax=1.420, Acor_av=0.869 F test: Probability=0.988, F= 1.088 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07250, wR= 0.09938, Acormin=0.447, Acormax=1.313, Acor_av=0.802 F test: Probability=0.895, F= 1.048 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08296, wR= 0.11108, Acormin=0.305, Acormax=1.324, Acor_av=0.790 F test: Probability=0.000, F= 0.802 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08110, wR= 0.10833, Acormin=0.340, Acormax=1.349, Acor_av=0.803 F test: Probability=0.000, F= 0.838 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07344, wR= 0.09879, Acormin=0.144, Acormax=0.422, Acor_av=0.257 F test: Probability=0.695, F= 1.019 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06720, wR= 0.09237, Acormin=0.162, Acormax=0.454, Acor_av=0.280 F test: Probability=1.000, F= 1.213 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06248, wR= 0.08796, Acormin=0.162, Acormax=0.480, Acor_av=0.294 F test: Probability=1.000, F= 1.395 Final absorption model (ne=6, no=3): Rint= 0.07437, Acormin=0.508, Acormax=1.420, Acor_av=0.869 Combined refinement in use Rint: 0.18351 There are 85 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: 3 (37 parameters) Refinement control: 121 pars with 7381 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22104 Using Levenberg-Marquardt: 0.00010 New wR= 0.06675 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18339 with corrections 0.05221 Rint for all data: 0.18351 with corrections 0.05242 3 observations identified as outliers and rejected Cycle 2 wR= 0.06643 Using Levenberg-Marquardt: 0.00001 New wR= 0.05865 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18285 with corrections 0.04486 Rint for all data: 0.18351 with corrections 0.04529 0 observations identified as outliers and rejected Cycle 3 wR= 0.05865 Using Levenberg-Marquardt: 0.00000 New wR= 0.05662 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18285 with corrections 0.04319 Rint for all data: 0.18351 with corrections 0.04357 0 observations identified as outliers and rejected Cycle 4 wR= 0.05662 Using Levenberg-Marquardt: 0.00000 New wR= 0.05564 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18285 with corrections 0.04236 Rint for all data: 0.18351 with corrections 0.04271 1 observations identified as outliers and rejected Cycle 5 wR= 0.05561 Using Levenberg-Marquardt: 0.00000 New wR= 0.05509 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18231 with corrections 0.04186 Rint for all data: 0.18351 with corrections 0.04227 1 observations identified as outliers and rejected Final wR= 0.05509 Final frame scales: Min= 0.7436 Max= 1.1698 Final absorption correction factors: Amin= 0.6190 Amax= 1.6103 PROFFIT INFO: Inet (after scale3 abspack): min=565.9799 max=5469736.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=160.7312 max=67309.7344 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 3712 reflections read from tmp file 658 reflections are rejected (658 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 2 2 0 4 2 1 3 92 Initial Chi^2= 0.35887 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.90460 Current error model SIG(F2)^2 = 115.45*I_RAW + 0.00*I_BACK+(0.02006*)^2 Cycle 2, Chi^2= 1.00047 Current error model SIG(F2)^2 = 109.86*I_RAW + 0.00*I_BACK+(0.01792*)^2 Cycle 3, Chi^2= 0.99998 Current error model SIG(F2)^2 = 108.70*I_RAW + 0.00*I_BACK+(0.01817*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 108.98*I_RAW + 0.00*I_BACK+(0.01811*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 108.98*I_RAW + 0.00*I_BACK+(0.01811*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5469736- 1487174 371 2232884.14 50.11 100.00 1486125- 955413 371 1180752.78 41.98 100.00 955210- 308798 371 573651.63 40.10 100.00 308698- 193330 371 238025.56 33.13 100.00 193235- 159690 371 176088.01 26.32 100.00 159679- 120322 371 136067.33 20.75 100.00 120303- 95978 371 108534.64 17.67 100.00 95970- 5587 371 55561.70 13.27 100.00 5526- 3268 371 4159.13 4.51 96.77 3266- 566 373 2529.76 3.42 62.20 ------------------------------------------------------------------------------------ 5469736- 566 3712 470573.15 25.11 95.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 866640.53 39.52 100.00 1.41- 1.12 371 732196.56 31.02 99.19 1.12- 0.96 371 605703.12 29.70 98.92 0.96- 0.88 371 446057.44 25.21 98.11 0.88- 0.81 371 597119.73 29.63 98.38 0.81- 0.74 371 306287.67 20.01 96.50 0.74- 0.71 371 246770.06 19.24 94.61 0.71- 0.65 371 453101.78 24.06 96.77 0.65- 0.62 371 233041.18 16.04 84.91 0.62- 0.58 373 220163.39 16.75 91.42 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 470573.15 25.11 95.88 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 371 866640.53 39.52 100.00 4.82- 1.12 742 799418.55 35.27 99.60 4.82- 0.96 1113 734846.74 33.41 99.37 4.82- 0.88 1484 662649.41 31.36 99.06 4.82- 0.81 1855 649543.48 31.02 98.92 4.82- 0.74 2226 592334.18 29.18 98.52 4.82- 0.71 2597 542967.87 27.76 97.96 4.82- 0.65 2968 531734.61 27.30 97.81 4.82- 0.62 3339 498546.45 26.05 96.38 4.82- 0.58 3712 470573.15 25.11 95.88 ------------------------------------------------------------------------------------ 4.82- 0.58 3712 470573.15 25.11 95.88 Scale applied to data: s=0.182824 (maximum obs:5469736.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.042; Rsigma 0.025: data 3712 -> merged 109 With outlier rejection... Rint 0.041; Rsigma 0.026: data 3703 -> merged 109 Rejected total: 9, method kkm 8, method Blessing 1 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585833, 4.830900 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 22.60 100.00 226 1.61 - 1.21 10 10 34.40 100.00 344 1.17 - 1.01 10 10 44.20 100.00 442 0.99 - 0.89 10 10 44.00 100.00 440 0.88 - 0.81 10 10 41.90 100.00 419 0.81 - 0.74 10 10 35.60 100.00 356 0.73 - 0.71 10 10 40.10 100.00 401 0.70 - 0.66 10 10 32.60 100.00 326 0.66 - 0.64 10 10 32.30 100.00 323 0.63 - 0.60 10 10 30.90 100.00 309 --------------------------------------------------------------- 8.36 - 0.60 100 100 35.86 100.00 3586 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:37:15 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367314 8.374551 8.360195 90.0986 89.9708 90.0047 3701 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1884 0 2472 2475 3701 N (int>3sigma) = 0 0 0 0 1884 0 2369 2370 3548 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 87.1 87.6 87.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 24.9 24.9 24.9 Lattice type: F chosen Volume: 585.82 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.913 5.916 90.05 119.93 119.92 Niggli form: a.a = 34.946 b.b = 34.958 c.c = 34.994 b.c = -0.030 a.c = -17.451 a.b = -17.436 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.122 CUBIC F-lattice R(int) = 0.038 [ 3545] Vol = 585.8 Cell: 8.367 8.375 8.360 90.10 89.97 90.00 Volume: 585.82 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 3263] Vol = 439.4 Cell: 5.919 5.913 14.504 90.00 90.07 120.05 Volume: 439.36 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.115 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1055] Vol = 439.4 Trigonal Cell: 5.919 5.913 14.504 90.00 90.07 120.05 Volume: 439.36 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.055 TETRAGONAL I-lattice R(int) = 0.037 [ 3299] Vol = 292.9 Cell: 5.919 5.919 8.360 89.95 89.91 89.95 Volume: 292.91 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.128 TETRAGONAL I-lattice R(int) = 0.037 [ 3299] Vol = 292.9 Cell: 5.919 5.919 8.360 90.09 90.05 89.95 Volume: 292.91 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.066 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3244] Vol = 292.9 Cell: 5.919 5.919 8.360 89.91 89.95 89.95 Volume: 292.91 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 3240] Vol = 292.9 Cell: 5.912 8.367 5.922 89.98 89.90 90.02 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.036 [ 2900] Vol = 292.9 Cell: 5.919 5.919 8.360 90.05 90.09 89.95 Volume: 292.91 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.094 MONOCLINIC I-lattice R(int) = 0.035 [ 2897] Vol = 292.9 Cell: 5.912 5.922 8.367 90.02 90.02 90.10 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.037 MONOCLINIC I-lattice R(int) = 0.033 [ 2912] Vol = 292.9 Cell: 5.912 8.367 5.922 89.98 90.10 89.98 Volume: 292.91 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.044 MONOCLINIC I-lattice R(int) = 0.035 [ 2897] Vol = 292.9 Cell: 5.922 5.912 8.367 89.98 90.02 89.90 Volume: 292.91 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.035 [ 2896] Vol = 292.9 Cell: 10.247 5.913 5.916 90.05 125.19 89.92 Volume: 292.91 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2246] Vol = 146.5 Cell: 5.912 5.913 5.916 90.05 119.93 119.92 Volume: 146.45 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1884 0 2472 2475 3701 N (int>3sigma) = 0 0 0 0 1884 0 2369 2370 3548 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 87.1 87.6 87.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 24.9 24.9 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.184 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 35 35 294 825 N I>3s 28 28 258 825 0.7 0.7 0.7 39.1 7.5 7.5 5.0 28.2 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 0.038 3271 Fd-3m 1 1 227 C N N N N 37 2284 0.039 3310 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367314 8.374551 8.360195 90.0986 89.9708 90.0047 ZERR 3.00 0.000430 0.000541 0.000544 0.0053 0.0048 0.0048 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5091459- 866554 827 823 27 30.5 1614456.80 45.04 0.039 0.052 860277- 148705 1097 1094 27 40.5 273973.21 32.37 0.045 0.054 140573- 50219 917 916 27 33.9 108524.63 17.94 0.061 0.080 21006- 1839 871 870 28 31.1 4512.03 4.52 0.161 0.204 ------------------------------------------------------------------------------------------- 5091459- 1839 3712 3703 109 34.0 467663.70 25.08 0.041 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-1.02 935 931 27 34.5 747129.65 35.05 0.038 0.051 0.021 1.01-0.78 1164 1164 28 41.6 445660.25 24.04 0.036 0.050 0.025 0.76-0.65 987 985 28 35.2 358482.29 21.06 0.047 0.060 0.030 0.65-0.59 626 623 26 24.0 263767.85 18.45 0.060 0.062 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3712 3703 109 34.0 467663.70 25.08 0.041 0.054 0.026 inf-0.60 3590 3584 99 36.2 477262.11 25.39 0.041 0.054 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 931 27 27 100.0 34.5 747129.65 231.23 0.038 0.006 1.01-0.78 1164 28 28 100.0 41.6 445660.25 165.14 0.036 0.004 0.76-0.65 985 28 28 100.0 35.2 358482.29 133.20 0.047 0.006 0.65-0.59 623 27 26 96.3 24.0 263767.85 106.00 0.060 0.010 -------------------------------------------------------------------------------------------- inf-0.59 3703 110 109 99.1 34.0 467663.70 163.31 0.041 0.006 inf-0.60 3584 99 99 100.0 36.2 477262.11 166.55 0.041 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:41:59 2018) ID: 2932; threads 39; handles 878; mem 515948.00 (1237728.00)kB; time: 1w 5d 23h 47m 29s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:503.9,peak PF: 708.5, WS: 268.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.6,peak PF: 708.5, WS: 270.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:41:59 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) 8.37051 ( 0.00043 ) 8.37682 ( 0.00054 ) 8.35710 ( 0.00054 ) 90.12473 ( 0.00524 ) 89.98579 ( 0.00481 ) 90.00567 ( 0.00484 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:41:59 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007186 0.000001 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007174 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000004 0.000012 0.007198 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36736(15) 8.36736(15) 8.36736(15) 90.0 90.0 90.0 V = 585.822(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb PROFFITPEAK info: 499 peaks in the peak location table UB fit with 243 obs out of 257 (total:257,skipped:0) (94.55%) UB - matrix: -0.007440 0.076866 -0.034921 ( 0.000039 0.000050 0.000036 ) -0.083541 -0.011753 -0.008052 ( 0.000046 0.000059 0.000042 ) -0.012176 0.033467 0.076763 ( 0.000051 0.000065 0.000046 ) M - matrix: 0.007183 0.000002 -0.000002 ( 0.000008 0.000006 0.000005 ) 0.000002 0.007166 -0.000021 ( 0.000006 0.000009 0.000006 ) -0.000002 -0.000021 0.007177 ( 0.000005 0.000006 0.000008 ) unit cell: 8.369(5) 8.379(5) 8.373(5) 89.84(5) 89.98(5) 90.02(5) V = 587.1(6) UB fit with 243 obs out of 257 (total:257,skipped:0) (94.55%) UB - matrix: -0.007440 0.076866 -0.034921 ( 0.000039 0.000050 0.000036 ) -0.083541 -0.011753 -0.008052 ( 0.000046 0.000059 0.000042 ) -0.012176 0.033467 0.076763 ( 0.000051 0.000065 0.000046 ) M - matrix: 0.007183 0.000002 -0.000002 ( 0.000008 0.000006 0.000005 ) 0.000002 0.007166 -0.000021 ( 0.000006 0.000009 0.000006 ) -0.000002 -0.000021 0.007177 ( 0.000005 0.000006 0.000008 ) unit cell: 8.369(5) 8.379(5) 8.373(5) 89.84(5) 89.98(5) 90.02(5) V = 587.1(6) OTKP changes: 50 1 1 1 UB - matrix: -0.007332 0.076625 -0.034662 ( 0.000039 0.000050 0.000035 ) -0.083207 -0.011556 -0.008124 ( 0.000047 0.000059 0.000042 ) -0.012252 0.033183 0.076497 ( 0.000048 0.000062 0.000043 ) M - matrix: 0.007127 -0.000007 -0.000007 ( 0.000008 0.000006 0.000005 ) -0.000007 0.007106 -0.000024 ( 0.000006 0.000009 0.000006 ) -0.000007 -0.000024 0.007119 ( 0.000005 0.000006 0.000007 ) UB fit with 244 obs out of 257 (total:257,skipped:0) (94.94%) unit cell: 8.402(5) 8.414(5) 8.406(5) 89.81(5) 89.94(4) 89.94(5) V = 594.3(6) UB fit with 244 obs out of 257 (total:257,skipped:0) (94.94%) UB - matrix: -0.007332 0.076625 -0.034662 ( 0.000039 0.000050 0.000035 ) -0.083207 -0.011556 -0.008124 ( 0.000047 0.000059 0.000042 ) -0.012252 0.033183 0.076497 ( 0.000048 0.000062 0.000043 ) M - matrix: 0.007127 -0.000007 -0.000007 ( 0.000008 0.000006 0.000005 ) -0.000007 0.007106 -0.000024 ( 0.000006 0.000009 0.000006 ) -0.000007 -0.000024 0.007119 ( 0.000005 0.000006 0.000007 ) unit cell: 8.402(5) 8.414(5) 8.406(5) 89.81(5) 89.94(4) 89.94(5) V = 594.3(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 257 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Run 7 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.282) HKL list info: 436 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007332 0.076625 -0.034662 ( 0.000039 0.000050 0.000035 ) -0.083207 -0.011556 -0.008124 ( 0.000047 0.000059 0.000042 ) -0.012252 0.033183 0.076497 ( 0.000048 0.000062 0.000043 ) M - matrix: 0.007127 -0.000007 -0.000007 ( 0.000008 0.000006 0.000005 ) -0.000007 0.007106 -0.000024 ( 0.000006 0.000009 0.000006 ) -0.000007 -0.000024 0.007119 ( 0.000005 0.000006 0.000007 ) UB fit with 244 obs out of 257 (total:257,skipped:0) (94.94%) unit cell: 8.402(5) 8.414(5) 8.406(5) 89.81(5) 89.94(4) 89.94(5) V = 594.3(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 244 obs out of 257 (total:257,skipped:0) (94.94%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 219 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 219 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.10- 1.60 | 22 | 1.152 ( 0.355) | 1.449 ( 0.763) | 1.932 ( 1.218) | 1.60- 1.17 | 22 | 1.041 ( 0.064) | 1.073 ( 0.090) | 0.988 ( 0.409) | 1.17- 1.02 | 22 | 1.067 ( 0.065) | 1.063 ( 0.100) | 1.051 ( 0.421) | 0.99- 0.92 | 22 | 1.110 ( 0.046) | 1.099 ( 0.082) | 1.046 ( 0.385) | 0.92- 0.82 | 22 | 1.145 ( 0.040) | 1.081 ( 0.089) | 1.256 ( 0.524) | 0.82- 0.76 | 22 | 1.161 ( 0.054) | 1.094 ( 0.092) | 1.303 ( 0.495) | 0.76- 0.71 | 22 | 1.177 ( 0.050) | 1.112 ( 0.121) | 1.256 ( 0.426) | 0.71- 0.67 | 22 | 1.178 ( 0.043) | 1.116 ( 0.104) | 1.257 ( 0.481) | 0.67- 0.63 | 22 | 1.199 ( 0.075) | 1.196 ( 0.121) | 1.228 ( 0.392) | 0.63- 0.59 | 21 | 1.194 ( 0.085) | 1.170 ( 0.117) | 1.371 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.10- 0.59 | 219 | 1.142 ( 0.136) | 1.145 ( 0.282) | 1.268 ( 0.627) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 217 obs out of 219 (total:219,skipped:0) (99.09%) UB - matrix: -0.007399 0.076720 -0.034766 ( 0.000024 0.000031 0.000022 ) -0.083327 -0.011664 -0.008134 ( 0.000026 0.000033 0.000023 ) -0.012051 0.033264 0.076636 ( 0.000026 0.000033 0.000023 ) M - matrix: 0.007143 0.000003 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000003 0.007128 -0.000023 ( 0.000003 0.000005 0.000003 ) 0.000012 -0.000023 0.007148 ( 0.000003 0.000003 0.000004 ) unit cell: 8.392(3) 8.401(3) 8.390(3) 89.81(3) 90.09(2) 90.03(3) V = 591.5(3) OTKP changes: 218 1 1 1 No constraint UB - matrix: -0.007426 0.076791 -0.034831 ( 0.000023 0.000030 0.000021 ) -0.083497 -0.011729 -0.008165 ( 0.000026 0.000034 0.000024 ) -0.012286 0.033409 0.076762 ( 0.000024 0.000030 0.000022 ) M - matrix: 0.007178 -0.000001 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007151 -0.000014 ( 0.000003 0.000005 0.000003 ) -0.000003 -0.000014 0.007172 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007426 0.076791 -0.034831 ( 0.000023 0.000030 0.000021 ) -0.083497 -0.011729 -0.008165 ( 0.000026 0.000034 0.000024 ) -0.012286 0.033409 0.076762 ( 0.000024 0.000030 0.000022 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) unit cell: 8.372(3) 8.388(3) 8.375(2) 89.89(2) 89.98(2) 89.99(3) V = 588.2(3) unit cell: 8.3785(5) 8.3785(5) 8.3785(5) 90.0 90.0 90.0 V = 588.16(7) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.044) HKL list info: 433 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007426 0.076791 -0.034831 ( 0.000023 0.000030 0.000021 ) -0.083497 -0.011729 -0.008165 ( 0.000026 0.000034 0.000024 ) -0.012286 0.033409 0.076762 ( 0.000024 0.000030 0.000022 ) M - matrix: 0.007178 -0.000001 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007151 -0.000014 ( 0.000003 0.000005 0.000003 ) -0.000003 -0.000014 0.007172 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007426 0.076791 -0.034831 ( 0.000023 0.000030 0.000021 ) -0.083497 -0.011729 -0.008165 ( 0.000026 0.000034 0.000024 ) -0.012286 0.033409 0.076762 ( 0.000024 0.000030 0.000022 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) unit cell: 8.372(3) 8.388(3) 8.375(2) 89.89(2) 89.98(2) 89.99(3) V = 588.2(3) unit cell: 8.3785(5) 8.3785(5) 8.3785(5) 90.0 90.0 90.0 V = 588.16(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb 2 of 220 peaks identified as outliers and rejected 218 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 218 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 218 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.48 | 22 | 1.086 ( 0.228) | 1.339 ( 0.665) | 1.608 ( 1.027) | 1.41- 1.17 | 22 | 1.056 ( 0.059) | 1.091 ( 0.074) | 1.031 ( 0.410) | 1.17- 0.99 | 22 | 1.077 ( 0.061) | 1.072 ( 0.092) | 1.162 ( 0.544) | 0.99- 0.92 | 22 | 1.126 ( 0.044) | 1.109 ( 0.085) | 1.044 ( 0.393) | 0.92- 0.82 | 22 | 1.150 ( 0.054) | 1.086 ( 0.087) | 1.285 ( 0.557) | 0.82- 0.76 | 22 | 1.160 ( 0.055) | 1.080 ( 0.101) | 1.285 ( 0.451) | 0.75- 0.71 | 22 | 1.175 ( 0.048) | 1.116 ( 0.105) | 1.252 ( 0.448) | 0.71- 0.67 | 22 | 1.177 ( 0.043) | 1.147 ( 0.120) | 1.173 ( 0.435) | 0.67- 0.62 | 22 | 1.207 ( 0.072) | 1.192 ( 0.120) | 1.245 ( 0.371) | 0.62- 0.59 | 20 | 1.194 ( 0.081) | 1.187 ( 0.123) | 1.408 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 218 | 1.140 ( 0.104) | 1.141 ( 0.245) | 1.248 ( 0.572) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 291 | 1.144 ( 0.115) | 1.242 ( 0.405) | 1.312 ( 0.644) | 13.1-18.8 | 291 | 1.133 ( 0.084) | 1.180 ( 0.278) | 1.250 ( 0.559) | 18.8-23.0 | 291 | 1.142 ( 0.089) | 1.191 ( 0.279) | 1.264 ( 0.672) | 23.0-27.2 | 291 | 1.130 ( 0.098) | 1.166 ( 0.292) | 1.227 ( 0.588) | 27.2-30.4 | 291 | 1.134 ( 0.097) | 1.147 ( 0.236) | 1.204 ( 0.451) | 30.4-33.6 | 291 | 1.145 ( 0.100) | 1.136 ( 0.212) | 1.194 ( 0.438) | 33.6-37.0 | 291 | 1.141 ( 0.096) | 1.117 ( 0.189) | 1.168 ( 0.427) | 37.0-39.8 | 291 | 1.147 ( 0.117) | 1.096 ( 0.205) | 1.230 ( 0.523) | 39.9-42.8 | 291 | 1.161 ( 0.109) | 1.107 ( 0.252) | 1.217 ( 0.531) | 42.8-49.8 | 293 | 1.204 ( 0.149) | 1.126 ( 0.260) | 1.201 ( 0.477) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 2912 | 1.148 ( 0.109) | 1.151 ( 0.270) | 1.227 ( 0.538) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0024 b=1.11 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:42:28 2018 PROFFITMAIN - Started at Wed Mar 28 14:42:28 2018 OTKP changes: 2898 2 4 6 OTKP changes: 2898 2 4 6 OTKP changes: 2898 2 4 6 No constraint UB - matrix: -0.007487 0.076883 -0.034809 ( 0.000006 0.000005 0.000006 ) -0.083601 -0.011780 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012145 0.033660 0.077027 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007193 0.000000 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007183 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000011 0.007210 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007487 0.076883 -0.034809 ( 0.000006 0.000005 0.000006 ) -0.083601 -0.011780 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012145 0.033660 0.077027 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) UB fit with 2904 obs out of 2912 (total:2912,skipped:0) (99.73%) unit cell: 8.3634(4) 8.3692(5) 8.3535(5) 90.092(5) 89.991(5) 90.004(5) V = 584.71(6) unit cell: 8.36205(14) 8.36205(14) 8.36205(14) 90.0 90.0 90.0 V = 584.708(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007135 0.076825 -0.034873 ( 0.000016 0.000012 0.000018 ) -0.083541 -0.011639 -0.008043 ( 0.000013 0.000009 0.000015 ) -0.012416 0.033809 0.076703 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007184 0.000004 -0.000032 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007181 0.000008 ( 0.000002 0.000002 0.000002 ) -0.000032 0.000008 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3684(13) 8.3705(13) 8.3802(15) 90.062(14) 89.747(14) 90.035(13) V = 587.00(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007233 0.076710 -0.035016 ( 0.000015 0.000010 0.000016 ) -0.083570 -0.011703 -0.008077 ( 0.000013 0.000009 0.000014 ) -0.012368 0.033936 0.076862 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007189 0.000003 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007173 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007199 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007233 0.076710 -0.035016 ( 0.000015 0.000010 0.000016 ) -0.083570 -0.011703 -0.008077 ( 0.000013 0.000009 0.000014 ) -0.012368 0.033936 0.076862 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3655(13) 8.3749(12) 8.3598(15) 90.134(13) 89.822(13) 90.028(12) V = 585.68(16) unit cell: 8.3667(3) 8.3667(3) 8.3667(3) 90.0 90.0 90.0 V = 585.68(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.982) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007233 0.076710 -0.035016 ( 0.000015 0.000010 0.000016 ) -0.083570 -0.011703 -0.008077 ( 0.000013 0.000009 0.000014 ) -0.012368 0.033936 0.076862 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007189 0.000003 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007173 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007199 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007233 0.076710 -0.035016 ( 0.000015 0.000010 0.000016 ) -0.083570 -0.011703 -0.008077 ( 0.000013 0.000009 0.000014 ) -0.012368 0.033936 0.076862 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007185 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007185 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3655(13) 8.3749(12) 8.3598(15) 90.134(13) 89.822(13) 90.028(12) V = 585.68(16) unit cell: 8.3667(3) 8.3667(3) 8.3667(3) 90.0 90.0 90.0 V = 585.68(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084664 0.000105 -0.000193 ( 0.000016 0.000011 0.000017 ) 0.000014 0.084749 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084809 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007168 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007182 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007193 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084664 0.000105 -0.000193 ( 0.000016 0.000011 0.000017 ) 0.000014 0.084749 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084809 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3779(16) 8.3694(8) 8.3635(10) 90.058(10) 89.870(13) 90.081(11) V = 586.43(14) unit cell: 8.3702(3) 8.3702(3) 8.3702(3) 90.0 90.0 90.0 V = 586.43(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007577 0.076996 -0.034605 ( 0.000014 0.000014 0.000012 ) -0.083451 -0.011890 -0.008144 ( 0.000012 0.000011 0.000009 ) -0.012252 0.033276 0.076955 ( 0.000013 0.000012 0.000010 ) M - matrix: 0.007172 0.000001 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007177 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007186 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3757(11) 8.3726(13) 8.3674(11) 89.945(11) 89.992(11) 90.009(12) V = 586.77(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007179 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3674(11) 8.3713(12) 8.3678(10) 90.000(10) 90.055(10) 90.087(11) V = 586.13(13) unit cell: 8.3688(4) 8.3688(4) 8.3688(4) 90.0 90.0 90.0 V = 586.13(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.982) HKL list info: 781 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007179 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3674(11) 8.3713(12) 8.3678(10) 90.000(10) 90.055(10) 90.087(11) V = 586.13(13) unit cell: 8.3688(4) 8.3688(4) 8.3688(4) 90.0 90.0 90.0 V = 586.13(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007179 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007581 0.076985 -0.034565 ( 0.000013 0.000012 0.000011 ) -0.083549 -0.011964 -0.008151 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076967 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3674(11) 8.3713(12) 8.3678(10) 90.000(10) 90.055(10) 90.087(11) V = 586.13(13) unit cell: 8.3688(4) 8.3688(4) 8.3688(4) 90.0 90.0 90.0 V = 586.13(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 216 obs out of 218 (total:218,skipped:0) (99.08%) UB - matrix: -0.007441 0.076854 -0.034933 ( 0.000020 0.000026 0.000018 ) -0.083488 -0.011786 -0.008029 ( 0.000021 0.000026 0.000018 ) -0.012048 0.033404 0.076835 ( 0.000028 0.000036 0.000025 ) M - matrix: 0.007171 0.000010 0.000005 ( 0.000004 0.000003 0.000003 ) 0.000010 0.007161 -0.000024 ( 0.000003 0.000005 0.000003 ) 0.000005 -0.000024 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.376(2) 8.382(2) 8.366(3) 89.81(3) 90.04(2) 90.08(2) V = 587.4(3) OTKP changes: 216 1 1 1 No constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 -0.000002 0.000002 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007159 -0.000015 ( 0.000003 0.000005 0.000003 ) 0.000002 -0.000015 0.007177 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 218 obs out of 218 (total:218,skipped:0) (100.00%) unit cell: 8.371(2) 8.383(3) 8.373(2) 89.88(2) 90.01(2) 89.99(2) V = 587.5(3) unit cell: 8.3755(4) 8.3755(4) 8.3755(4) 90.0 90.0 90.0 V = 587.54(5) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.042) HKL list info: 432 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 -0.000002 0.000002 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007159 -0.000015 ( 0.000003 0.000005 0.000003 ) 0.000002 -0.000015 0.007177 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 218 obs out of 218 (total:218,skipped:0) (100.00%) unit cell: 8.371(2) 8.383(3) 8.373(2) 89.88(2) 90.01(2) 89.99(2) V = 587.5(3) unit cell: 8.3755(4) 8.3755(4) 8.3755(4) 90.0 90.0 90.0 V = 587.54(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 218 obs out of 218 (total:218,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 -0.000002 0.000002 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007159 -0.000015 ( 0.000003 0.000005 0.000003 ) 0.000002 -0.000015 0.007177 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007441 0.076828 -0.034862 ( 0.000022 0.000028 0.000020 ) -0.083509 -0.011743 -0.008206 ( 0.000022 0.000028 0.000020 ) -0.012281 0.033442 0.076775 ( 0.000024 0.000030 0.000021 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 218 obs out of 218 (total:218,skipped:0) (100.00%) unit cell: 8.371(2) 8.383(3) 8.373(2) 89.88(2) 90.01(2) 89.99(2) V = 587.5(3) unit cell: 8.3755(4) 8.3755(4) 8.3755(4) 90.0 90.0 90.0 V = 587.54(5) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007470 0.076829 -0.034780 ( 0.000006 0.000005 0.000006 ) -0.083556 -0.011765 -0.008062 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033648 0.076954 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000000 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000012 0.007197 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007470 0.076829 -0.034780 ( 0.000006 0.000005 0.000006 ) -0.083556 -0.011765 -0.008062 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033648 0.076954 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2906 obs out of 2912 (total:2912,skipped:0) (99.79%) unit cell: 8.3676(4) 8.3748(5) 8.3612(5) 90.096(5) 89.975(5) 89.997(5) V = 585.93(6) unit cell: 8.36786(15) 8.36786(15) 8.36786(15) 90.0 90.0 90.0 V = 585.926(18) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 74 reflections under beam stop or inside a detector rejection region 31 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof 3864 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:42:37 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.982) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.982) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.042) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3260728.6724 PROFFIT INFO: background sum: min=515.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=10993.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7114317.5000 PROFFIT INFO: sig(Inet): min=186.7852 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=310.00 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 5 98 313 506 800 885 1608 2582 3519 3864 Percent 0.0 0.1 2.5 8.1 13.1 20.7 22.9 41.6 66.8 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3864 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 3864 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7114318- 1522688 386 2307227.51 134.45 100.00 1522681- 958897 386 1226423.32 106.51 100.00 956450- 300907 386 557435.22 93.56 100.00 300847- 206394 386 245815.23 67.58 100.00 206360- 156685 386 177676.71 47.95 100.00 156526- 124223 386 139909.92 36.70 100.00 124043- 92508 386 109570.38 29.24 100.00 92505- 6052 386 51309.77 20.10 100.00 6017- 3423 386 4435.66 4.85 80.83 3415- 531 390 2476.69 3.08 38.72 ------------------------------------------------------------------------------------ 7114318- 531 3864 481731.40 54.35 91.90 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 829122.49 87.14 100.00 1.41- 1.12 386 727586.22 70.10 98.45 1.12- 0.96 386 641160.45 75.08 98.45 0.96- 0.88 386 454337.34 58.15 94.30 0.88- 0.81 386 620369.77 68.84 97.41 0.81- 0.74 386 321281.41 40.08 91.71 0.74- 0.71 386 270491.59 36.84 88.34 0.71- 0.65 386 478528.52 48.91 95.60 0.65- 0.62 386 243825.01 29.07 73.58 0.62- 0.58 390 233186.82 29.53 81.28 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 481731.40 54.35 91.90 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:42:37 2018 Sorting 3864 observations 120 unique observations with > 7.00 F2/sig(F2) 3864 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 48 671 Total number of frames 671 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3864 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 7 0 8 116 Total number of frames 116 3107 observations > 7.00 F2/sig(F2) 3107 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 8 115 Total number of frames 115 Removing 'redundancy=1' reflections Average redundancy: 24.4 (Out of 3107 removed 5 = 3102, 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 3102 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 8 115 Total number of frames 115 127 unique data precomputed (should be 127) 127 unique data with 3102 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.4 (Out of 3102 removed 0 = 3102, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3102 observations RMS deviation of equivalent data = 0.21993 Rint = 0.18492 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18437, wR= 0.23371 Trying model 1 (ne=2, no=0)... Results: Rint= 0.12745, wR= 0.17448, Acormin=0.673, Acormax=1.311, Acor_av=0.943 F test: Probability=1.000, F= 2.089 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10902, wR= 0.13933, Acormin=0.542, Acormax=1.351, Acor_av=0.898 F test: Probability=1.000, F= 1.365 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10959, wR= 0.15272, Acormin=0.629, Acormax=1.427, Acor_av=0.959 F test: Probability=0.000, F= 0.988 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08665, wR= 0.11559, Acormin=0.494, Acormax=1.493, Acor_av=0.917 F test: Probability=1.000, F= 1.578 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08051, wR= 0.10847, Acormin=0.481, Acormax=1.403, Acor_av=0.882 F test: Probability=1.000, F= 1.156 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10282, wR= 0.14289, Acormin=0.611, Acormax=1.500, Acor_av=0.920 F test: Probability=0.000, F= 0.613 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08388, wR= 0.11181, Acormin=0.493, Acormax=1.492, Acor_av=0.901 F test: Probability=0.000, F= 0.919 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07817, wR= 0.10470, Acormin=0.475, Acormax=1.405, Acor_av=0.868 F test: Probability=0.931, F= 1.056 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07360, wR= 0.09849, Acormin=0.438, Acormax=1.308, Acor_av=0.805 F test: Probability=1.000, F= 1.187 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08963, wR= 0.11504, Acormin=0.253, Acormax=1.312, Acor_av=0.783 F test: Probability=0.000, F= 0.675 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08402, wR= 0.10823, Acormin=0.339, Acormax=1.377, Acor_av=0.818 F test: Probability=0.000, F= 0.768 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07734, wR= 0.09990, Acormin=0.136, Acormax=0.422, Acor_av=0.258 F test: Probability=0.000, F= 0.904 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06853, wR= 0.09172, Acormin=0.162, Acormax=0.464, Acor_av=0.288 F test: Probability=1.000, F= 1.147 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06405, wR= 0.08739, Acormin=0.162, Acormax=0.490, Acor_av=0.301 F test: Probability=1.000, F= 1.306 Final absorption model (ne=6, no=5): Rint= 0.07360, Acormin=0.438, Acormax=1.308, Acor_av=0.805 Combined refinement in use Rint: 0.18504 There are 115 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 162 pars with 13203 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21993 Using Levenberg-Marquardt: 0.00010 New wR= 0.05475 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18492 with corrections 0.04310 Rint for all data: 0.18504 with corrections 0.04331 0 observations identified as outliers and rejected Cycle 2 wR= 0.05475 Using Levenberg-Marquardt: 0.00001 New wR= 0.05074 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18492 with corrections 0.03918 Rint for all data: 0.18504 with corrections 0.03940 0 observations identified as outliers and rejected Cycle 3 wR= 0.05074 Using Levenberg-Marquardt: 0.00000 New wR= 0.05019 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18492 with corrections 0.03859 Rint for all data: 0.18504 with corrections 0.03881 0 observations identified as outliers and rejected Cycle 4 wR= 0.05019 Using Levenberg-Marquardt: 0.00000 New wR= 0.04999 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18492 with corrections 0.03833 Rint for all data: 0.18504 with corrections 0.03855 0 observations identified as outliers and rejected Cycle 5 wR= 0.04999 Using Levenberg-Marquardt: 0.00000 New wR= 0.04991 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18492 with corrections 0.03821 Rint for all data: 0.18504 with corrections 0.03843 0 observations identified as outliers and rejected Final wR= 0.04991 Final frame scales: Min= 0.7606 Max= 1.2838 Final absorption correction factors: Amin= 0.6252 Amax= 1.6170 PROFFIT INFO: Inet (after scale3 abspack): min=549.3686 max=5317443.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=155.1793 max=71123.3516 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 3864 reflections read from tmp file 614 reflections are rejected (614 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 4 1 2 3 2 5 4 129 Initial Chi^2= 0.38056 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88074 Current error model SIG(F2)^2 = 122.55*I_RAW + 0.00*I_BACK+(0.01945*)^2 Cycle 2, Chi^2= 1.00004 Current error model SIG(F2)^2 = 108.17*I_RAW + 0.00*I_BACK+(0.01820*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 108.14*I_RAW + 0.00*I_BACK+(0.01821*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 108.14*I_RAW + 0.00*I_BACK+(0.01821*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5317444- 1472790 386 2199991.38 49.74 100.00 1470598- 939632 386 1163211.91 41.81 100.00 939560- 304589 386 564458.28 40.00 100.00 304552- 190542 386 234120.58 32.96 100.00 190522- 158564 386 173503.77 26.19 100.00 158429- 119018 386 134195.64 20.68 100.00 118982- 94691 386 107131.07 17.68 100.00 94664- 5465 386 54594.22 13.15 100.00 5457- 3240 386 4111.92 4.51 95.85 3235- 549 390 2504.51 3.43 62.05 ------------------------------------------------------------------------------------ 5317444- 549 3864 463304.81 24.99 95.76 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 844044.92 39.06 100.00 1.41- 1.12 386 718614.74 30.81 99.22 1.12- 0.96 386 604589.05 29.75 98.96 0.96- 0.88 386 435899.02 25.03 97.93 0.88- 0.81 386 590243.61 29.66 98.45 0.81- 0.74 386 299490.22 19.89 96.37 0.74- 0.71 386 254784.00 19.48 94.82 0.71- 0.65 386 444203.05 23.82 97.15 0.65- 0.62 386 228443.07 15.91 83.94 0.62- 0.58 390 215306.38 16.61 90.77 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 463304.81 24.99 95.76 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 844044.92 39.06 100.00 4.82- 1.12 772 781329.83 34.94 99.61 4.82- 0.96 1158 722416.24 33.21 99.40 4.82- 0.88 1544 650786.93 31.16 99.03 4.82- 0.81 1930 638678.27 30.86 98.91 4.82- 0.74 2316 582146.93 29.03 98.49 4.82- 0.71 2702 535380.79 27.67 97.96 4.82- 0.65 3088 523983.58 27.19 97.86 4.82- 0.62 3474 491145.74 25.93 96.32 4.82- 0.58 3864 463304.81 24.99 95.76 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 463304.81 24.99 95.76 Scale applied to data: s=0.188060 (maximum obs:5317443.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.038; Rsigma 0.026: data 3864 -> merged 156 With outlier rejection... Rint 0.038; Rsigma 0.026: data 3853 -> merged 156 Rejected total: 11, method kkm 8, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585867, 4.831184 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.48 14 14 22.43 100.00 314 1.41 - 1.12 14 14 32.00 100.00 448 1.12 - 0.97 14 14 31.93 100.00 447 0.96 - 0.84 14 14 34.29 100.00 480 0.84 - 0.78 14 14 25.71 100.00 360 0.78 - 0.73 14 14 27.14 100.00 380 0.73 - 0.69 14 14 26.00 100.00 364 0.69 - 0.66 14 14 22.07 100.00 309 0.65 - 0.63 14 14 23.64 100.00 331 0.63 - 0.60 14 14 21.21 100.00 297 --------------------------------------------------------------- 8.38 - 0.60 140 140 26.64 100.00 3730 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:42:38 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367586 8.374796 8.361205 90.0960 89.9754 89.9968 3853 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1962 0 2579 2581 3853 N (int>3sigma) = 0 0 0 0 1962 0 2467 2468 3689 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 86.7 87.5 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 25.3 0.0 25.0 25.1 24.9 Lattice type: F chosen Volume: 585.93 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.913 5.916 90.04 119.94 119.92 Niggli form: a.a = 34.953 b.b = 34.967 c.c = 34.997 b.c = -0.027 a.c = -17.457 a.b = -17.440 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.122 CUBIC F-lattice R(int) = 0.038 [ 3697] Vol = 585.9 Cell: 8.368 8.375 8.361 90.10 89.98 90.00 Volume: 585.93 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.114 RHOMBOHEDRAL R-lattice R(int) = 0.042 [ 3415] Vol = 439.4 Cell: 5.919 5.913 14.503 90.00 90.07 120.05 Volume: 439.44 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.114 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1101] Vol = 439.4 Trigonal Cell: 5.919 5.913 14.503 90.00 90.07 120.05 Volume: 439.44 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.052 TETRAGONAL I-lattice R(int) = 0.037 [ 3449] Vol = 293.0 Cell: 5.919 5.919 8.361 89.95 89.91 89.95 Volume: 292.96 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.120 TETRAGONAL I-lattice R(int) = 0.037 [ 3449] Vol = 293.0 Cell: 5.919 5.919 8.361 90.09 90.05 89.95 Volume: 292.96 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3395] Vol = 293.0 Cell: 5.919 5.919 8.361 89.91 89.95 89.95 Volume: 292.96 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3391] Vol = 293.0 Cell: 5.912 8.368 5.922 89.98 89.91 90.02 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.035 [ 3050] Vol = 293.0 Cell: 5.919 5.919 8.361 90.05 90.09 89.95 Volume: 292.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.084 MONOCLINIC I-lattice R(int) = 0.034 [ 3048] Vol = 293.0 Cell: 5.912 5.922 8.368 90.02 90.02 90.09 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC I-lattice R(int) = 0.033 [ 3062] Vol = 293.0 Cell: 5.912 8.368 5.922 89.98 90.09 89.98 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.042 MONOCLINIC I-lattice R(int) = 0.034 [ 3046] Vol = 293.0 Cell: 8.368 5.912 5.922 90.09 90.02 90.02 Volume: 292.96 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.034 [ 3047] Vol = 293.0 Cell: 10.248 5.913 5.916 90.04 125.19 89.92 Volume: 292.96 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2395] Vol = 146.5 Cell: 5.912 5.913 5.916 90.04 119.94 119.92 Volume: 146.48 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1962 0 2579 2581 3853 N (int>3sigma) = 0 0 0 0 1962 0 2467 2468 3689 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 86.7 87.5 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 25.3 0.0 25.0 25.1 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.187 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 306 857 N I>3s 32 32 270 857 0.8 0.8 0.7 39.2 7.9 7.9 5.1 28.3 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 0.037 3411 Fd-3m 1 1 227 C N N N N 37 2284 0.038 3450 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367586 8.374796 8.361205 90.0960 89.9754 89.9968 ZERR 3.00 0.000428 0.000529 0.000528 0.0051 0.0047 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5163023- 1100900 619 615 26 23.7 1836665.58 47.18 0.033 0.042 1089341- 269731 608 604 26 23.2 650205.28 39.94 0.046 0.062 267961- 130187 885 884 26 34.0 185206.55 27.18 0.038 0.051 126809- 94218 645 645 26 24.8 112162.85 18.18 0.055 0.072 92553- 3758 562 560 26 21.5 30284.79 9.16 0.068 0.093 3744- 1837 545 545 26 21.0 3020.36 3.87 0.199 0.249 ------------------------------------------------------------------------------------------- 5163023- 1837 3864 3853 156 24.7 461185.19 24.95 0.038 0.049 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 724 718 26 27.6 693539.97 33.86 0.036 0.044 0.021 1.12-0.88 864 864 26 33.2 586910.96 28.74 0.030 0.040 0.023 0.85-0.75 719 718 26 27.6 448273.45 24.23 0.035 0.047 0.027 0.74-0.68 639 638 26 24.5 376696.64 21.95 0.043 0.052 0.030 0.67-0.63 614 614 26 23.6 221182.72 17.24 0.057 0.079 0.037 0.62-0.59 304 301 26 11.6 245497.59 16.59 0.057 0.064 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3864 3853 156 24.7 461185.19 24.95 0.038 0.049 0.026 inf-0.60 3736 3728 139 26.8 470810.59 25.27 0.037 0.049 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 718 26 26 100.0 27.6 693539.97 194.32 0.036 0.006 1.12-0.88 864 26 26 100.0 33.2 586910.96 168.18 0.030 0.005 0.85-0.75 718 26 26 100.0 27.6 448273.45 135.45 0.035 0.005 0.74-0.68 638 26 26 100.0 24.5 376696.64 111.65 0.043 0.007 0.67-0.63 614 26 26 100.0 23.6 221182.72 83.42 0.057 0.008 0.62-0.59 301 27 26 96.3 11.6 245497.59 67.10 0.057 0.015 -------------------------------------------------------------------------------------------- inf-0.59 3853 157 156 99.4 24.7 461185.19 136.19 0.038 0.007 inf-0.60 3728 139 139 100.0 26.8 470810.59 139.15 0.037 0.006 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007471 0.076829 -0.034780 ( 0.000006 0.000005 0.000006 ) -0.083556 -0.011765 -0.008062 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033648 0.076953 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000000 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000012 0.007196 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007471 0.076829 -0.034780 ( 0.000006 0.000005 0.000006 ) -0.083556 -0.011765 -0.008062 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033648 0.076953 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3676(4) 8.3748(5) 8.3612(5) 90.096(5) 89.976(5) 89.997(5) V = 585.93(6) unit cell: 8.36787(15) 8.36787(15) 8.36787(15) 90.0 90.0 90.0 V = 585.929(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: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.982) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.982) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.042) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3260728.6724 PROFFIT INFO: background sum: min=515.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=10993.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7114317.5000 PROFFIT INFO: sig(Inet): min=186.7852 max=63740.3359 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=310.00 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 10 196 626 1012 1600 1770 3216 5164 7038 7728 Percent 0.0 0.1 2.5 8.1 13.1 20.7 22.9 41.6 66.8 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3864 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 3864 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7114318- 1522688 386 2307227.51 134.45 100.00 1522681- 958897 386 1226423.32 106.51 100.00 956450- 300907 386 557435.22 93.56 100.00 300847- 206394 386 245815.23 67.58 100.00 206360- 156685 386 177676.71 47.95 100.00 156526- 124223 386 139909.92 36.70 100.00 124043- 92508 386 109570.38 29.24 100.00 92505- 6052 386 51309.77 20.10 100.00 6017- 3423 386 4435.66 4.85 80.83 3415- 531 390 2476.69 3.08 38.72 ------------------------------------------------------------------------------------ 7114318- 531 3864 481731.40 54.35 91.90 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 829122.49 87.14 100.00 1.41- 1.12 386 727586.22 70.10 98.45 1.12- 0.96 386 641160.45 75.08 98.45 0.96- 0.88 386 454337.34 58.15 94.30 0.88- 0.81 386 620369.77 68.84 97.41 0.81- 0.74 386 321281.41 40.08 91.71 0.74- 0.71 386 270491.59 36.84 88.34 0.71- 0.65 386 478528.52 48.91 95.60 0.65- 0.62 386 243825.01 29.07 73.58 0.62- 0.58 390 233186.82 29.53 81.28 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 481731.40 54.35 91.90 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:42:39 2018 Sorting 3864 observations 86 unique observations with > 7.00 F2/sig(F2) 3864 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 48 671 Total number of frames 671 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3864 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 6 88 Total number of frames 88 3107 observations > 7.00 F2/sig(F2) 3107 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 6 88 Total number of frames 88 Removing 'redundancy=1' reflections Average redundancy: 34.1 (Out of 3107 removed 4 = 3103, 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): 4/m3bar2/m 3103 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 13 28 3 0 12 41 4 0 12 54 5 0 13 68 6 0 12 81 7 0 6 88 Total number of frames 88 91 unique data precomputed (should be 91) 91 unique data with 3103 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 34.1 (Out of 3103 removed 0 = 3103, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3103 observations RMS deviation of equivalent data = 0.22040 Rint = 0.18501 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18448, wR= 0.23442 Trying model 1 (ne=2, no=0)... Results: Rint= 0.12772, wR= 0.17562, Acormin=0.673, Acormax=1.307, Acor_av=0.943 F test: Probability=1.000, F= 2.083 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10936, wR= 0.13987, Acormin=0.542, Acormax=1.349, Acor_av=0.898 F test: Probability=1.000, F= 1.363 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11087, wR= 0.15478, Acormin=0.635, Acormax=1.420, Acor_av=0.958 F test: Probability=0.000, F= 0.971 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08776, wR= 0.11713, Acormin=0.494, Acormax=1.486, Acor_av=0.916 F test: Probability=1.000, F= 1.548 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08112, wR= 0.10984, Acormin=0.480, Acormax=1.414, Acor_av=0.879 F test: Probability=1.000, F= 1.168 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10421, wR= 0.14479, Acormin=0.616, Acormax=1.488, Acor_av=0.918 F test: Probability=0.000, F= 0.605 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08531, wR= 0.11350, Acormin=0.485, Acormax=1.476, Acor_av=0.899 F test: Probability=0.000, F= 0.902 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07881, wR= 0.10616, Acormin=0.475, Acormax=1.414, Acor_av=0.864 F test: Probability=0.927, F= 1.055 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07408, wR= 0.09938, Acormin=0.436, Acormax=1.309, Acor_av=0.803 F test: Probability=1.000, F= 1.189 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09022, wR= 0.11643, Acormin=0.264, Acormax=1.309, Acor_av=0.780 F test: Probability=0.000, F= 0.675 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08463, wR= 0.10943, Acormin=0.348, Acormax=1.370, Acor_av=0.816 F test: Probability=0.000, F= 0.767 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07766, wR= 0.10048, Acormin=0.135, Acormax=0.420, Acor_av=0.254 F test: Probability=0.000, F= 0.908 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06871, wR= 0.09195, Acormin=0.161, Acormax=0.460, Acor_av=0.284 F test: Probability=1.000, F= 1.156 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06405, wR= 0.08780, Acormin=0.159, Acormax=0.483, Acor_av=0.297 F test: Probability=1.000, F= 1.323 Final absorption model (ne=6, no=5): Rint= 0.07408, Acormin=0.436, Acormax=1.309, Acor_av=0.803 Combined refinement in use Rint: 0.18513 There are 88 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: 5 (48 parameters) Refinement control: 135 pars with 9180 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22040 Using Levenberg-Marquardt: 0.00010 New wR= 0.05990 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18501 with corrections 0.04657 Rint for all data: 0.18513 with corrections 0.04679 3 observations identified as outliers and rejected Cycle 2 wR= 0.05974 Using Levenberg-Marquardt: 0.00001 New wR= 0.05401 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18415 with corrections 0.04176 Rint for all data: 0.18513 with corrections 0.04220 1 observations identified as outliers and rejected Cycle 3 wR= 0.05359 Using Levenberg-Marquardt: 0.00000 New wR= 0.05211 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18419 with corrections 0.04014 Rint for all data: 0.18513 with corrections 0.04072 3 observations identified as outliers and rejected Cycle 4 wR= 0.05217 Using Levenberg-Marquardt: 0.00000 New wR= 0.05153 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18401 with corrections 0.03949 Rint for all data: 0.18513 with corrections 0.04013 4 observations identified as outliers and rejected Cycle 5 wR= 0.05166 Using Levenberg-Marquardt: 0.00000 New wR= 0.05128 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18352 with corrections 0.03912 Rint for all data: 0.18513 with corrections 0.03980 1 observations identified as outliers and rejected Final wR= 0.05128 Final frame scales: Min= 0.7747 Max= 1.1997 Final absorption correction factors: Amin= 0.5540 Amax= 1.5814 PROFFIT INFO: Inet (after scale3 abspack): min=557.7663 max=5275483.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=154.4034 max=68747.4531 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 3864 reflections read from tmp file 643 reflections are rejected (643 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 1 1 2 1 4 1 93 Initial Chi^2= 0.34745 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.96953 Current error model SIG(F2)^2 = 113.12*I_RAW + 0.00*I_BACK+(0.01728*)^2 Cycle 2, Chi^2= 1.00080 Current error model SIG(F2)^2 = 99.84*I_RAW + 0.00*I_BACK+(0.01897*)^2 Cycle 3, Chi^2= 1.00016 Current error model SIG(F2)^2 = 102.35*I_RAW + 0.00*I_BACK+(0.01844*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 101.79*I_RAW + 0.00*I_BACK+(0.01857*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 101.93*I_RAW + 0.00*I_BACK+(0.01854*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 101.93*I_RAW + 0.00*I_BACK+(0.01854*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5275483- 1475256 386 2195186.91 49.30 100.00 1473303- 951643 386 1164429.08 41.84 100.00 951448- 302143 386 564811.16 40.22 100.00 301236- 190568 386 233293.50 33.21 100.00 190396- 158575 386 173401.11 26.55 100.00 158416- 119217 386 134280.08 21.17 100.00 119172- 94794 386 107254.33 18.10 100.00 94644- 5469 386 54672.72 13.56 100.00 5445- 3241 386 4114.53 4.64 97.15 3238- 558 390 2499.42 3.54 66.67 ------------------------------------------------------------------------------------ 5275483- 558 3864 462917.17 25.19 96.35 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 841013.57 38.93 100.00 1.41- 1.12 386 716467.56 30.90 100.00 1.12- 0.96 386 603387.72 29.88 99.22 0.96- 0.88 386 435820.63 25.25 98.19 0.88- 0.81 386 588979.03 29.88 98.45 0.81- 0.74 386 299820.73 20.15 96.63 0.74- 0.71 386 255054.01 19.81 94.82 0.71- 0.65 386 445794.54 24.11 97.41 0.65- 0.62 386 229393.05 16.18 86.53 0.62- 0.58 390 215999.57 16.92 92.31 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 462917.17 25.19 96.35 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 386 841013.57 38.93 100.00 4.82- 1.12 772 778740.56 34.91 100.00 4.82- 0.96 1158 720289.62 33.24 99.74 4.82- 0.88 1544 649172.37 31.24 99.35 4.82- 0.81 1930 637133.70 30.97 99.17 4.82- 0.74 2316 580914.87 29.16 98.75 4.82- 0.71 2702 534363.32 27.83 98.19 4.82- 0.65 3088 523292.22 27.36 98.09 4.82- 0.62 3474 490636.76 26.12 96.80 4.82- 0.58 3864 462917.17 25.19 96.35 ------------------------------------------------------------------------------------ 4.82- 0.58 3864 462917.17 25.19 96.35 Scale applied to data: s=0.189556 (maximum obs:5275483.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.040; Rsigma 0.026: data 3864 -> merged 109 With outlier rejection... Rint 0.039; Rsigma 0.026: data 3855 -> merged 109 Rejected total: 9, method kkm 6, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585868, 4.831194 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.71 10 10 23.50 100.00 235 1.61 - 1.21 10 10 36.00 100.00 360 1.17 - 1.01 10 10 46.00 100.00 460 0.99 - 0.89 10 10 45.60 100.00 456 0.88 - 0.81 10 10 43.60 100.00 436 0.81 - 0.74 10 10 37.30 100.00 373 0.73 - 0.71 10 10 41.70 100.00 417 0.70 - 0.66 10 10 34.10 100.00 341 0.66 - 0.64 10 10 33.30 100.00 333 0.63 - 0.60 10 10 32.00 100.00 320 --------------------------------------------------------------- 8.38 - 0.60 100 100 37.31 100.00 3731 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:42:38 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367586 8.374796 8.361205 90.0960 89.9754 89.9968 3853 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1962 0 2579 2581 3853 N (int>3sigma) = 0 0 0 0 1962 0 2467 2468 3689 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 86.7 87.5 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 25.3 0.0 25.0 25.1 24.9 Lattice type: F chosen Volume: 585.93 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.912 5.913 5.916 90.04 119.94 119.92 Niggli form: a.a = 34.953 b.b = 34.967 c.c = 34.997 b.c = -0.027 a.c = -17.457 a.b = -17.440 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.122 CUBIC F-lattice R(int) = 0.038 [ 3697] Vol = 585.9 Cell: 8.368 8.375 8.361 90.10 89.98 90.00 Volume: 585.93 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.114 RHOMBOHEDRAL R-lattice R(int) = 0.042 [ 3415] Vol = 439.4 Cell: 5.919 5.913 14.503 90.00 90.07 120.05 Volume: 439.44 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.114 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1101] Vol = 439.4 Trigonal Cell: 5.919 5.913 14.503 90.00 90.07 120.05 Volume: 439.44 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.052 TETRAGONAL I-lattice R(int) = 0.037 [ 3449] Vol = 293.0 Cell: 5.919 5.919 8.361 89.95 89.91 89.95 Volume: 292.96 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.120 TETRAGONAL I-lattice R(int) = 0.037 [ 3449] Vol = 293.0 Cell: 5.919 5.919 8.361 90.09 90.05 89.95 Volume: 292.96 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3395] Vol = 293.0 Cell: 5.919 5.919 8.361 89.91 89.95 89.95 Volume: 292.96 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3391] Vol = 293.0 Cell: 5.912 8.368 5.922 89.98 89.91 90.02 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.035 [ 3050] Vol = 293.0 Cell: 5.919 5.919 8.361 90.05 90.09 89.95 Volume: 292.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.084 MONOCLINIC I-lattice R(int) = 0.034 [ 3048] Vol = 293.0 Cell: 5.912 5.922 8.368 90.02 90.02 90.09 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC I-lattice R(int) = 0.033 [ 3062] Vol = 293.0 Cell: 5.912 8.368 5.922 89.98 90.09 89.98 Volume: 292.96 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.042 MONOCLINIC I-lattice R(int) = 0.034 [ 3046] Vol = 293.0 Cell: 8.368 5.912 5.922 90.09 90.02 90.02 Volume: 292.96 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.093 MONOCLINIC C-lattice R(int) = 0.034 [ 3047] Vol = 293.0 Cell: 10.248 5.913 5.916 90.04 125.19 89.92 Volume: 292.96 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2395] Vol = 146.5 Cell: 5.912 5.913 5.916 90.04 119.94 119.92 Volume: 146.48 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1962 0 2579 2581 3853 N (int>3sigma) = 0 0 0 0 1962 0 2467 2468 3689 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 86.7 87.5 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 25.3 0.0 25.0 25.1 24.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.187 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 306 857 N I>3s 32 32 270 857 0.8 0.8 0.7 39.2 7.9 7.9 5.1 28.3 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 0.037 3411 Fd-3m 1 1 227 C N N N N 37 2284 0.038 3450 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367586 8.374796 8.361205 90.0960 89.9754 89.9968 ZERR 3.00 0.000428 0.000529 0.000528 0.0051 0.0047 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5065140- 866550 859 855 27 31.7 1599256.11 44.66 0.036 0.049 857445- 147161 1144 1141 27 42.3 269640.72 32.54 0.042 0.052 138768- 49834 952 951 27 35.2 107071.22 18.30 0.057 0.075 20689- 1830 909 908 28 32.4 4451.01 4.67 0.159 0.200 ------------------------------------------------------------------------------------------- 5065140- 1830 3864 3855 109 35.4 461968.94 25.15 0.039 0.051 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 976 972 27 36.0 736336.58 34.79 0.036 0.050 0.021 1.01-0.78 1176 1176 27 43.6 451816.97 24.77 0.034 0.047 0.025 0.78-0.65 1062 1060 29 36.6 345377.60 20.74 0.043 0.054 0.030 0.65-0.59 650 647 26 24.9 259249.01 18.59 0.058 0.059 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 3864 3855 109 35.4 461968.94 25.15 0.039 0.051 0.026 inf-0.60 3736 3729 99 37.7 471627.28 25.47 0.039 0.052 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 972 27 27 100.0 36.0 736336.58 234.19 0.036 0.006 1.01-0.78 1176 27 27 100.0 43.6 451816.97 173.96 0.034 0.004 0.78-0.65 1060 29 29 100.0 36.6 345377.60 134.51 0.043 0.006 0.65-0.59 647 27 26 96.3 24.9 259249.01 107.93 0.058 0.010 -------------------------------------------------------------------------------------------- inf-0.59 3855 110 109 99.1 35.4 461968.94 167.22 0.039 0.006 inf-0.60 3729 99 99 100.0 37.7 471627.28 170.59 0.039 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:47:19 2018) ID: 2932; threads 39; handles 879; mem 515836.00 (1237728.00)kB; time: 1w 5d 23h 52m 50s MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:503.7,peak PF: 708.5, WS: 268.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:172.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.5,peak PF: 708.5, WS: 270.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:47:19 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000005 ) 8.37051 ( 0.00043 ) 8.37682 ( 0.00053 ) 8.35710 ( 0.00052 ) 90.12473 ( 0.00510 ) 89.98579 ( 0.00471 ) 90.00567 ( 0.00475 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:47:20 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000006 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000000 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000012 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000012 0.007196 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36787(15) 8.36787(15) 8.36787(15) 90.0 90.0 90.0 V = 585.929(18) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083723 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.118(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035006 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035006 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.038(13) 90.109(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035006 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035006 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.038(13) 90.109(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.174 ( 0.518) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.203 ( 0.492) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb PROFFITPEAK info: 791 peaks in the peak location table UB fit with 362 obs out of 389 (total:389,skipped:0) (93.06%) UB - matrix: -0.007419 0.076840 -0.034993 ( 0.000032 0.000042 0.000028 ) -0.083573 -0.011779 -0.008046 ( 0.000028 0.000037 0.000025 ) -0.012189 0.033500 0.076779 ( 0.000032 0.000042 0.000028 ) M - matrix: 0.007188 0.000006 -0.000004 ( 0.000005 0.000004 0.000003 ) 0.000006 0.007165 -0.000022 ( 0.000004 0.000007 0.000004 ) -0.000004 -0.000022 0.007184 ( 0.000003 0.000004 0.000005 ) unit cell: 8.366(3) 8.379(4) 8.368(3) 89.82(3) 89.97(3) 90.05(3) V = 586.6(4) UB fit with 362 obs out of 389 (total:389,skipped:0) (93.06%) UB - matrix: -0.007419 0.076840 -0.034993 ( 0.000032 0.000042 0.000028 ) -0.083573 -0.011779 -0.008046 ( 0.000028 0.000037 0.000025 ) -0.012189 0.033500 0.076779 ( 0.000032 0.000042 0.000028 ) M - matrix: 0.007188 0.000006 -0.000004 ( 0.000005 0.000004 0.000003 ) 0.000006 0.007165 -0.000022 ( 0.000004 0.000007 0.000004 ) -0.000004 -0.000022 0.007184 ( 0.000003 0.000004 0.000005 ) unit cell: 8.366(3) 8.379(4) 8.368(3) 89.82(3) 89.97(3) 90.05(3) V = 586.6(4) OTKP changes: 75 1 1 1 UB - matrix: -0.007276 0.076580 -0.034700 ( 0.000031 0.000041 0.000027 ) -0.083237 -0.011565 -0.008101 ( 0.000027 0.000036 0.000024 ) -0.012213 0.033214 0.076487 ( 0.000030 0.000040 0.000026 ) M - matrix: 0.007131 -0.000000 -0.000007 ( 0.000005 0.000004 0.000003 ) -0.000000 0.007101 -0.000023 ( 0.000004 0.000007 0.000004 ) -0.000007 -0.000023 0.007120 ( 0.000003 0.000004 0.000004 ) UB fit with 363 obs out of 389 (total:389,skipped:0) (93.32%) unit cell: 8.400(3) 8.417(4) 8.406(3) 89.81(3) 89.94(3) 90.00(3) V = 594.3(4) UB fit with 363 obs out of 389 (total:389,skipped:0) (93.32%) UB - matrix: -0.007276 0.076580 -0.034700 ( 0.000031 0.000041 0.000027 ) -0.083237 -0.011565 -0.008101 ( 0.000027 0.000036 0.000024 ) -0.012213 0.033214 0.076487 ( 0.000030 0.000040 0.000026 ) M - matrix: 0.007131 -0.000000 -0.000007 ( 0.000005 0.000004 0.000003 ) -0.000000 0.007101 -0.000023 ( 0.000004 0.000007 0.000004 ) -0.000007 -0.000023 0.007120 ( 0.000003 0.000004 0.000004 ) unit cell: 8.400(3) 8.417(4) 8.406(3) 89.81(3) 89.94(3) 90.00(3) V = 594.3(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 389 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Run 7 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.320) HKL list info: 584 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007276 0.076580 -0.034700 ( 0.000031 0.000041 0.000027 ) -0.083237 -0.011565 -0.008101 ( 0.000027 0.000036 0.000024 ) -0.012213 0.033214 0.076487 ( 0.000030 0.000040 0.000026 ) M - matrix: 0.007131 -0.000000 -0.000007 ( 0.000005 0.000004 0.000003 ) -0.000000 0.007101 -0.000023 ( 0.000004 0.000007 0.000004 ) -0.000007 -0.000023 0.007120 ( 0.000003 0.000004 0.000004 ) UB fit with 363 obs out of 389 (total:389,skipped:0) (93.32%) unit cell: 8.400(3) 8.417(4) 8.406(3) 89.81(3) 89.94(3) 90.00(3) V = 594.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 364 obs out of 389 (total:389,skipped:0) (93.57%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb 0 of 329 peaks identified as outliers and rejected 329 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 329 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 329 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.60 | 33 | 1.105 ( 0.303) | 1.365 ( 0.732) | 1.663 ( 1.073) | 1.60- 1.17 | 33 | 1.054 ( 0.063) | 1.072 ( 0.081) | 1.019 ( 0.408) | 1.17- 0.99 | 33 | 1.088 ( 0.057) | 1.083 ( 0.100) | 1.142 ( 0.532) | 0.99- 0.92 | 33 | 1.128 ( 0.045) | 1.105 ( 0.099) | 1.061 ( 0.435) | 0.92- 0.82 | 33 | 1.153 ( 0.040) | 1.079 ( 0.100) | 1.252 ( 0.467) | 0.82- 0.76 | 33 | 1.169 ( 0.053) | 1.083 ( 0.118) | 1.286 ( 0.514) | 0.76- 0.72 | 33 | 1.196 ( 0.054) | 1.081 ( 0.131) | 1.320 ( 0.447) | 0.72- 0.67 | 33 | 1.192 ( 0.047) | 1.100 ( 0.107) | 1.326 ( 0.482) | 0.67- 0.63 | 33 | 1.210 ( 0.071) | 1.200 ( 0.119) | 1.299 ( 0.442) | 0.63- 0.59 | 32 | 1.226 ( 0.103) | 1.134 ( 0.124) | 1.478 ( 0.556) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 329 | 1.152 ( 0.125) | 1.130 ( 0.268) | 1.284 ( 0.595) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 326 obs out of 329 (total:329,skipped:0) (99.09%) UB - matrix: -0.007344 0.076645 -0.034797 ( 0.000016 0.000020 0.000014 ) -0.083298 -0.011618 -0.008109 ( 0.000015 0.000019 0.000013 ) -0.012012 0.033293 0.076622 ( 0.000016 0.000021 0.000015 ) M - matrix: 0.007137 0.000005 0.000011 ( 0.000003 0.000002 0.000002 ) 0.000005 0.007118 -0.000022 ( 0.000002 0.000003 0.000002 ) 0.000011 -0.000022 0.007148 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3961(15) 8.4073(19) 8.3899(16) 89.824(17) 90.085(15) 90.040(16) V = 592.2(2) OTKP changes: 327 1 1 1 No constraint UB - matrix: -0.007454 0.076743 -0.034901 ( 0.000016 0.000020 0.000014 ) -0.083500 -0.011720 -0.008153 ( 0.000015 0.000019 0.000014 ) -0.012274 0.033460 0.076791 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007178 -0.000004 -0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007146 -0.000013 ( 0.000002 0.000003 0.000002 ) -0.000002 -0.000013 0.007181 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007454 0.076743 -0.034901 ( 0.000016 0.000020 0.000014 ) -0.083500 -0.011720 -0.008153 ( 0.000015 0.000019 0.000014 ) -0.012274 0.033460 0.076791 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) unit cell: 8.3718(15) 8.3905(18) 8.3700(15) 89.893(16) 89.987(15) 89.967(16) V = 587.9(2) unit cell: 8.3774(4) 8.3774(4) 8.3774(4) 90.0 90.0 90.0 V = 587.93(5) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.031) HKL list info: 580 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007454 0.076743 -0.034901 ( 0.000016 0.000020 0.000014 ) -0.083500 -0.011720 -0.008153 ( 0.000015 0.000019 0.000014 ) -0.012274 0.033460 0.076791 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007178 -0.000004 -0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007146 -0.000013 ( 0.000002 0.000003 0.000002 ) -0.000002 -0.000013 0.007181 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007454 0.076743 -0.034901 ( 0.000016 0.000020 0.000014 ) -0.083500 -0.011720 -0.008153 ( 0.000015 0.000019 0.000014 ) -0.012274 0.033460 0.076791 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) unit cell: 8.3718(15) 8.3905(18) 8.3700(15) 89.893(16) 89.987(15) 89.967(16) V = 587.9(2) unit cell: 8.3774(4) 8.3774(4) 8.3774(4) 90.0 90.0 90.0 V = 587.93(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb 1 of 330 peaks identified as outliers and rejected 329 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 329 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 329 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.61 | 33 | 1.067 ( 0.185) | 1.362 ( 0.755) | 1.572 ( 1.029) | 1.48- 1.17 | 33 | 1.064 ( 0.066) | 1.091 ( 0.085) | 1.017 ( 0.425) | 1.17- 0.99 | 33 | 1.089 ( 0.061) | 1.077 ( 0.100) | 1.131 ( 0.475) | 0.98- 0.92 | 33 | 1.140 ( 0.044) | 1.108 ( 0.095) | 1.090 ( 0.412) | 0.92- 0.82 | 33 | 1.153 ( 0.048) | 1.077 ( 0.103) | 1.272 ( 0.510) | 0.82- 0.76 | 33 | 1.167 ( 0.061) | 1.090 ( 0.116) | 1.257 ( 0.508) | 0.76- 0.72 | 33 | 1.198 ( 0.056) | 1.079 ( 0.126) | 1.308 ( 0.457) | 0.72- 0.67 | 33 | 1.193 ( 0.049) | 1.117 ( 0.120) | 1.329 ( 0.483) | 0.67- 0.63 | 33 | 1.212 ( 0.066) | 1.198 ( 0.124) | 1.286 ( 0.424) | 0.63- 0.59 | 32 | 1.233 ( 0.104) | 1.139 ( 0.135) | 1.566 ( 0.553) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 329 | 1.151 ( 0.102) | 1.134 ( 0.275) | 1.282 ( 0.581) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 302 | 1.144 ( 0.114) | 1.239 ( 0.398) | 1.296 ( 0.636) | 13.1-18.7 | 302 | 1.133 ( 0.079) | 1.184 ( 0.299) | 1.263 ( 0.582) | 18.8-22.9 | 302 | 1.143 ( 0.088) | 1.185 ( 0.265) | 1.276 ( 0.666) | 23.0-27.2 | 302 | 1.130 ( 0.098) | 1.168 ( 0.297) | 1.227 ( 0.588) | 27.2-30.4 | 302 | 1.135 ( 0.097) | 1.151 ( 0.265) | 1.206 ( 0.455) | 30.4-33.6 | 302 | 1.145 ( 0.100) | 1.133 ( 0.210) | 1.193 ( 0.436) | 33.6-37.0 | 302 | 1.143 ( 0.095) | 1.117 ( 0.188) | 1.175 ( 0.437) | 37.0-39.8 | 302 | 1.148 ( 0.116) | 1.098 ( 0.203) | 1.239 ( 0.523) | 39.8-42.8 | 302 | 1.161 ( 0.111) | 1.101 ( 0.251) | 1.217 ( 0.531) | 42.8-49.8 | 305 | 1.208 ( 0.150) | 1.120 ( 0.257) | 1.221 ( 0.490) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 3023 | 1.149 ( 0.108) | 1.149 ( 0.273) | 1.231 ( 0.541) | Fitted profile normalization line parameters e1 dimension: a=0.0020 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464175 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:47:50 2018 PROFFITMAIN - Started at Wed Mar 28 14:47:50 2018 OTKP changes: 3008 2 4 6 OTKP changes: 3008 2 4 6 OTKP changes: 3008 2 4 6 No constraint UB - matrix: -0.007485 0.076875 -0.034819 ( 0.000006 0.000005 0.000006 ) -0.083594 -0.011776 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012146 0.033658 0.077005 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007192 0.000000 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007181 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000010 0.007207 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007485 0.076875 -0.034819 ( 0.000006 0.000005 0.000006 ) -0.083594 -0.011776 -0.008059 ( 0.000004 0.000004 0.000004 ) -0.012146 0.033658 0.077005 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) UB fit with 3014 obs out of 3023 (total:3023,skipped:0) (99.70%) unit cell: 8.3641(4) 8.3700(5) 8.3550(5) 90.080(5) 89.992(5) 90.001(5) V = 584.92(6) unit cell: 8.36305(13) 8.36305(13) 8.36305(13) 90.0 90.0 90.0 V = 584.916(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007470 0.076920 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008083 ( 0.000009 0.000010 0.000008 ) -0.012185 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3654(9) 8.3679(12) 8.3670(11) 90.054(11) 89.986(10) 89.998(10) V = 585.69(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007478 0.076933 -0.034755 ( 0.000012 0.000013 0.000010 ) -0.083578 -0.011769 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012174 0.033614 0.076916 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007478 0.076933 -0.034755 ( 0.000012 0.000013 0.000010 ) -0.083578 -0.011769 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012174 0.033614 0.076916 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3654(11) 90.054(11) 89.991(10) 89.992(10) V = 585.50(13) unit cell: 8.3658(3) 8.3658(3) 8.3658(3) 90.0 90.0 90.0 V = 585.50(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.945) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007478 0.076933 -0.034755 ( 0.000012 0.000013 0.000010 ) -0.083578 -0.011769 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012174 0.033614 0.076916 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007478 0.076933 -0.034755 ( 0.000012 0.000013 0.000010 ) -0.083578 -0.011769 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012174 0.033614 0.076916 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3654(11) 90.054(11) 89.991(10) 89.992(10) V = 585.50(13) unit cell: 8.3658(3) 8.3658(3) 8.3658(3) 90.0 90.0 90.0 V = 585.50(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084801 -0.000002 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000065 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084783 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 -0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) -0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084801 -0.000002 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000065 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084783 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3661(9) 90.024(11) 90.000(9) 89.992(11) V = 585.64(13) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007135 0.076822 -0.034875 ( 0.000016 0.000012 0.000018 ) -0.083540 -0.011639 -0.008044 ( 0.000013 0.000009 0.000015 ) -0.012415 0.033810 0.076702 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007184 0.000004 -0.000031 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007180 0.000008 ( 0.000002 0.000002 0.000002 ) -0.000031 0.000008 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3686(13) 8.3707(13) 8.3801(15) 90.062(14) 89.749(14) 90.035(13) V = 587.03(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007226 0.076699 -0.035010 ( 0.000015 0.000010 0.000016 ) -0.083559 -0.011694 -0.008074 ( 0.000013 0.000009 0.000014 ) -0.012360 0.033933 0.076849 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000003 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007171 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007197 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007226 0.076699 -0.035010 ( 0.000015 0.000010 0.000016 ) -0.083559 -0.011694 -0.008074 ( 0.000013 0.000009 0.000014 ) -0.012360 0.033933 0.076849 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3668(13) 8.3761(12) 8.3611(15) 90.135(13) 89.822(13) 90.028(12) V = 585.95(16) unit cell: 8.3680(3) 8.3680(3) 8.3680(3) 90.0 90.0 90.0 V = 585.95(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.996) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007226 0.076699 -0.035010 ( 0.000015 0.000010 0.000016 ) -0.083559 -0.011694 -0.008074 ( 0.000013 0.000009 0.000014 ) -0.012360 0.033933 0.076849 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007187 0.000003 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007171 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007197 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007226 0.076699 -0.035010 ( 0.000015 0.000010 0.000016 ) -0.083559 -0.011694 -0.008074 ( 0.000013 0.000009 0.000014 ) -0.012360 0.033933 0.076849 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3668(13) 8.3761(12) 8.3611(15) 90.135(13) 89.822(13) 90.028(12) V = 585.95(16) unit cell: 8.3680(3) 8.3680(3) 8.3680(3) 90.0 90.0 90.0 V = 585.95(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084651 0.000108 -0.000192 ( 0.000016 0.000011 0.000017 ) 0.000012 0.084736 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084795 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007166 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007180 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084651 0.000108 -0.000192 ( 0.000016 0.000011 0.000017 ) 0.000012 0.084736 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084795 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3791(16) 8.3707(8) 8.3648(10) 90.058(10) 89.871(13) 90.081(11) V = 586.70(14) unit cell: 8.3715(3) 8.3715(3) 8.3715(3) 90.0 90.0 90.0 V = 586.70(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3763(13) 8.3562(12) 90.037(12) 90.111(11) 89.923(11) V = 585.43(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007577 0.076994 -0.034606 ( 0.000014 0.000014 0.000012 ) -0.083452 -0.011891 -0.008144 ( 0.000012 0.000011 0.000009 ) -0.012251 0.033277 0.076952 ( 0.000013 0.000012 0.000010 ) M - matrix: 0.007172 0.000001 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007177 -0.000007 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000007 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3757(11) 8.3727(13) 8.3676(11) 89.945(11) 89.992(11) 90.010(12) V = 586.80(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007184 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007177 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007183 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3687(11) 8.3726(12) 8.3691(10) 90.000(10) 90.054(10) 90.087(11) V = 586.40(13) unit cell: 8.3701(4) 8.3701(4) 8.3701(4) 90.0 90.0 90.0 V = 586.40(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.996) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007184 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007177 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007183 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3687(11) 8.3726(12) 8.3691(10) 90.000(10) 90.054(10) 90.087(11) V = 586.40(13) unit cell: 8.3701(4) 8.3701(4) 8.3701(4) 90.0 90.0 90.0 V = 586.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007184 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007177 0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 0.000000 0.007183 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007574 0.076972 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083537 -0.011958 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012162 0.033307 0.076953 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3687(11) 8.3726(12) 8.3691(10) 90.000(10) 90.054(10) 90.087(11) V = 586.40(13) unit cell: 8.3701(4) 8.3701(4) 8.3701(4) 90.0 90.0 90.0 V = 586.40(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) UB - matrix: -0.007451 0.076747 -0.034910 ( 0.000015 0.000019 0.000014 ) -0.083498 -0.011725 -0.008161 ( 0.000014 0.000018 0.000013 ) -0.012274 0.033468 0.076802 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007178 -0.000004 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000004 0.007148 -0.000013 ( 0.000002 0.000003 0.000002 ) -0.000001 -0.000013 0.007184 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3719(14) 8.3897(18) 8.3686(15) 89.895(16) 89.991(14) 89.971(15) V = 587.79(19) OTKP changes: 329 1 1 1 No constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007185 -0.000005 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000005 0.007152 -0.000012 ( 0.000002 0.000003 0.000002 ) -0.000001 -0.000012 0.007186 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) unit cell: 8.3682(14) 8.3871(17) 8.3674(15) 89.902(16) 89.994(14) 89.963(15) V = 587.26(19) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.26(4) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.005) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007185 -0.000005 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000005 0.007152 -0.000012 ( 0.000002 0.000003 0.000002 ) -0.000001 -0.000012 0.007186 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) unit cell: 8.3682(14) 8.3871(17) 8.3674(15) 89.902(16) 89.994(14) 89.963(15) V = 587.26(19) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.26(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007185 -0.000005 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000005 0.007152 -0.000012 ( 0.000002 0.000003 0.000002 ) -0.000001 -0.000012 0.007186 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007463 0.076763 -0.034924 ( 0.000015 0.000019 0.000013 ) -0.083532 -0.011735 -0.008180 ( 0.000014 0.000018 0.000013 ) -0.012300 0.033494 0.076807 ( 0.000015 0.000019 0.000013 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 329 obs out of 329 (total:329,skipped:0) (100.00%) unit cell: 8.3682(14) 8.3871(17) 8.3674(15) 89.902(16) 89.994(14) 89.963(15) V = 587.26(19) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.26(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007473 0.076825 -0.034789 ( 0.000006 0.000005 0.000005 ) -0.083555 -0.011761 -0.008067 ( 0.000004 0.000004 0.000004 ) -0.012180 0.033649 0.076939 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000001 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007173 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000011 0.007195 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007473 0.076825 -0.034789 ( 0.000006 0.000005 0.000005 ) -0.083555 -0.011761 -0.008067 ( 0.000004 0.000004 0.000004 ) -0.012180 0.033649 0.076939 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 3017 obs out of 3023 (total:3023,skipped:0) (99.80%) unit cell: 8.3675(4) 8.3751(5) 8.3622(5) 90.089(5) 89.975(5) 89.990(5) V = 586.01(6) unit cell: 8.36826(15) 8.36826(15) 8.36826(15) 90.0 90.0 90.0 V = 586.010(18) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 76 reflections under beam stop or inside a detector rejection region 32 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof 4006 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:47:59 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.945) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.996) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.996) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.005) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256697.8833 PROFFIT INFO: background sum: min=512.0000 max=17440.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11095.0000 PROFFIT INFO: num of signal pixels: min=56 max=883 PROFFIT INFO: Inet: min=530.6313 max=7105523.0000 PROFFIT INFO: sig(Inet): min=187.6440 max=63740.2305 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 6 104 328 529 833 919 1673 2677 3647 4006 Percent 0.0 0.1 2.6 8.2 13.2 20.8 22.9 41.8 66.8 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4006 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 4006 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7105523- 1525132 400 2314472.29 134.37 100.00 1523014- 950651 400 1226303.35 106.69 100.00 949808- 300963 400 557418.16 93.49 100.00 300763- 206055 400 245846.82 67.66 100.00 205680- 156614 400 177646.64 47.87 100.00 156609- 123378 400 139460.36 36.62 100.00 123290- 92345 400 108903.88 29.08 100.00 92305- 6039 400 51376.48 20.02 100.00 6007- 3408 400 4424.60 4.83 80.50 3405- 531 406 2460.11 3.06 38.42 ------------------------------------------------------------------------------------ 7105523- 531 4006 482111.79 54.29 91.81 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 845255.46 87.54 100.00 1.41- 1.12 400 719497.22 69.36 98.75 1.12- 0.96 400 657167.45 76.10 98.00 0.96- 0.88 400 451606.77 58.14 94.25 0.88- 0.81 400 616056.47 68.47 97.25 0.81- 0.74 400 312984.89 39.64 91.75 0.74- 0.71 400 278065.87 37.39 89.00 0.71- 0.65 400 469630.11 48.18 95.25 0.65- 0.62 400 244923.45 29.20 73.50 0.62- 0.58 406 229716.16 29.25 80.54 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 482111.79 54.29 91.81 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:47:59 2018 Sorting 4006 observations 120 unique observations with > 7.00 F2/sig(F2) 4006 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 73 696 Total number of frames 696 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4006 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 7 0 12 120 Total number of frames 120 3217 observations > 7.00 F2/sig(F2) 3217 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 12 119 Total number of frames 119 Removing 'redundancy=1' reflections Average redundancy: 25.3 (Out of 3217 removed 5 = 3212, 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 3212 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 12 119 Total number of frames 119 127 unique data precomputed (should be 127) 127 unique data with 3212 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 25.3 (Out of 3212 removed 0 = 3212, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3212 observations RMS deviation of equivalent data = 0.21644 Rint = 0.18248 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18198, wR= 0.22929 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13149, wR= 0.17500, Acormin=0.689, Acormax=1.296, Acor_av=0.938 F test: Probability=1.000, F= 1.912 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10654, wR= 0.13620, Acormin=0.541, Acormax=1.350, Acor_av=0.901 F test: Probability=1.000, F= 1.522 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11348, wR= 0.15377, Acormin=0.625, Acormax=1.423, Acor_av=0.954 F test: Probability=0.000, F= 0.880 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08443, wR= 0.11295, Acormin=0.489, Acormax=1.491, Acor_av=0.919 F test: Probability=1.000, F= 1.588 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07880, wR= 0.10589, Acormin=0.477, Acormax=1.401, Acor_av=0.888 F test: Probability=1.000, F= 1.146 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10577, wR= 0.14292, Acormin=0.602, Acormax=1.501, Acor_av=0.916 F test: Probability=0.000, F= 0.554 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08146, wR= 0.10890, Acormin=0.488, Acormax=1.500, Acor_av=0.907 F test: Probability=0.000, F= 0.934 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07630, wR= 0.10196, Acormin=0.469, Acormax=1.414, Acor_av=0.878 F test: Probability=0.952, F= 1.062 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07142, wR= 0.09597, Acormin=0.433, Acormax=1.303, Acor_av=0.810 F test: Probability=1.000, F= 1.137 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09042, wR= 0.11471, Acormin=0.249, Acormax=1.304, Acor_av=0.780 F test: Probability=0.000, F= 0.625 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08202, wR= 0.10577, Acormin=0.346, Acormax=1.386, Acor_av=0.825 F test: Probability=0.000, F= 0.759 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07565, wR= 0.09780, Acormin=0.142, Acormax=0.441, Acor_av=0.272 F test: Probability=0.000, F= 0.889 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06686, wR= 0.08988, Acormin=0.169, Acormax=0.481, Acor_av=0.303 F test: Probability=1.000, F= 1.135 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06266, wR= 0.08526, Acormin=0.171, Acormax=0.516, Acor_av=0.318 F test: Probability=1.000, F= 1.285 Final absorption model (ne=6, no=5): Rint= 0.07142, Acormin=0.433, Acormax=1.303, Acor_av=0.810 Combined refinement in use Rint: 0.18261 There are 119 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 166 pars with 13861 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21644 Using Levenberg-Marquardt: 0.00010 New wR= 0.05334 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18248 with corrections 0.04162 Rint for all data: 0.18261 with corrections 0.04184 1 observations identified as outliers and rejected Cycle 2 wR= 0.05291 Using Levenberg-Marquardt: 0.00001 New wR= 0.04905 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18252 with corrections 0.03781 Rint for all data: 0.18261 with corrections 0.03816 0 observations identified as outliers and rejected Cycle 3 wR= 0.04905 Using Levenberg-Marquardt: 0.00000 New wR= 0.04833 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18252 with corrections 0.03706 Rint for all data: 0.18261 with corrections 0.03739 0 observations identified as outliers and rejected Cycle 4 wR= 0.04833 Using Levenberg-Marquardt: 0.00000 New wR= 0.04801 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18252 with corrections 0.03674 Rint for all data: 0.18261 with corrections 0.03705 0 observations identified as outliers and rejected Cycle 5 wR= 0.04801 Using Levenberg-Marquardt: 0.00000 New wR= 0.04786 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18252 with corrections 0.03658 Rint for all data: 0.18261 with corrections 0.03689 0 observations identified as outliers and rejected Final wR= 0.04786 Final frame scales: Min= 0.7301 Max= 1.1573 Final absorption correction factors: Amin= 0.5708 Amax= 1.5426 PROFFIT INFO: Inet (after scale3 abspack): min=555.2953 max=5303334.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=153.4741 max=69659.9375 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 4006 reflections read from tmp file 591 reflections are rejected (591 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 4 2 0 3 3 2 3 134 Initial Chi^2= 0.36971 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88884 Current error model SIG(F2)^2 = 118.62*I_RAW + 0.00*I_BACK+(0.01732*)^2 Cycle 2, Chi^2= 1.00007 Current error model SIG(F2)^2 = 106.33*I_RAW + 0.00*I_BACK+(0.01611*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 106.17*I_RAW + 0.00*I_BACK+(0.01615*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 106.17*I_RAW + 0.00*I_BACK+(0.01615*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5303334- 1488752 400 2204142.35 54.93 100.00 1482326- 942871 400 1162397.51 44.83 100.00 941694- 305219 400 564760.26 42.97 100.00 305030- 190958 400 233723.21 34.65 100.00 190721- 158433 400 173337.59 27.07 100.00 158320- 119188 400 133766.64 21.08 100.00 119170- 94833 400 107063.80 17.99 100.00 94813- 5470 400 54595.39 13.45 100.00 5461- 3217 400 4112.55 4.51 96.25 3215- 555 406 2485.86 3.47 64.04 ------------------------------------------------------------------------------------ 5303334- 555 4006 463347.22 26.46 95.98 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 855006.68 42.66 100.00 1.41- 1.12 400 708240.68 33.05 99.50 1.12- 0.96 400 620464.06 31.86 98.75 0.96- 0.88 400 434009.46 26.50 98.00 0.88- 0.81 400 584327.69 31.26 98.25 0.81- 0.74 400 292017.36 20.69 96.75 0.74- 0.71 400 262527.88 20.44 94.75 0.71- 0.65 400 436814.27 24.67 97.00 0.65- 0.62 400 231153.55 16.58 85.50 0.62- 0.58 406 212670.75 17.03 91.38 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 463347.22 26.46 95.98 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 855006.68 42.66 100.00 4.82- 1.12 800 781623.68 37.86 99.75 4.82- 0.96 1200 727903.80 35.86 99.42 4.82- 0.88 1600 654430.22 33.52 99.06 4.82- 0.81 2000 640409.71 33.07 98.90 4.82- 0.74 2400 582344.32 31.00 98.54 4.82- 0.71 2800 536656.26 29.49 98.00 4.82- 0.65 3200 524176.01 28.89 97.88 4.82- 0.62 3600 491617.96 27.52 96.50 4.82- 0.58 4006 463347.22 26.46 95.98 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 463347.22 26.46 95.98 Scale applied to data: s=0.188560 (maximum obs:5303334.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.024: data 4006 -> merged 156 With outlier rejection... Rint 0.036; Rsigma 0.024: data 3995 -> merged 156 Rejected total: 11, method kkm 7, method Blessing 4 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585895, 4.831414 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.48 14 14 23.29 100.00 326 1.41 - 1.12 14 14 33.14 100.00 464 1.12 - 0.97 14 14 33.07 100.00 463 0.96 - 0.84 14 14 35.29 100.00 494 0.84 - 0.78 14 14 27.14 100.00 380 0.78 - 0.73 14 14 28.07 100.00 393 0.73 - 0.69 14 14 26.93 100.00 377 0.69 - 0.66 14 14 22.71 100.00 318 0.65 - 0.63 14 14 24.57 100.00 344 0.63 - 0.60 14 14 21.93 100.00 307 --------------------------------------------------------------- 8.39 - 0.60 140 140 27.61 100.00 3866 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:48:01 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367481 8.375137 8.362163 90.0887 89.9751 89.9897 3994 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2033 0 2671 2673 3994 N (int>3sigma) = 0 0 0 0 2033 0 2560 2562 3833 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 87.0 87.4 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.5 26.4 Lattice type: F chosen Volume: 586.01 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.913 5.914 5.916 90.04 119.95 119.93 Niggli form: a.a = 34.963 b.b = 34.970 c.c = 35.000 b.c = -0.022 a.c = -17.465 a.b = -17.444 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.116 CUBIC F-lattice R(int) = 0.036 [ 3838] Vol = 586.0 Cell: 8.367 8.375 8.362 90.09 89.98 89.99 Volume: 586.01 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.107 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3556] Vol = 439.5 Cell: 5.920 5.914 14.503 89.99 90.07 120.04 Volume: 439.51 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.107 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1150] Vol = 439.5 Trigonal Cell: 5.920 5.914 14.503 89.99 90.07 120.04 Volume: 439.51 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.047 TETRAGONAL I-lattice R(int) = 0.035 [ 3590] Vol = 293.0 Cell: 5.919 5.920 8.362 89.95 89.92 89.95 Volume: 293.00 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.117 TETRAGONAL I-lattice R(int) = 0.035 [ 3590] Vol = 293.0 Cell: 5.920 5.919 8.362 90.08 90.05 89.95 Volume: 293.00 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.057 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3536] Vol = 293.0 Cell: 5.920 5.919 8.362 89.92 89.95 89.95 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.051 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 3533] Vol = 293.0 Cell: 5.913 8.367 5.922 89.99 89.91 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 3192] Vol = 293.0 Cell: 5.919 5.920 8.362 90.05 90.08 89.95 Volume: 293.00 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.077 MONOCLINIC I-lattice R(int) = 0.033 [ 3190] Vol = 293.0 Cell: 5.913 5.922 8.367 90.01 90.02 90.09 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.034 MONOCLINIC I-lattice R(int) = 0.031 [ 3204] Vol = 293.0 Cell: 5.913 8.367 5.922 89.99 90.09 89.98 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.041 MONOCLINIC I-lattice R(int) = 0.034 [ 3188] Vol = 293.0 Cell: 5.922 5.913 8.367 89.98 90.01 89.91 Volume: 293.00 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.088 MONOCLINIC C-lattice R(int) = 0.032 [ 3188] Vol = 293.0 Cell: 10.249 5.914 5.916 90.04 125.20 89.92 Volume: 293.00 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.030 [ 2537] Vol = 146.5 Cell: 5.913 5.914 5.916 90.04 119.95 119.93 Volume: 146.50 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2033 0 2671 2673 3994 N (int>3sigma) = 0 0 0 0 2033 0 2560 2562 3833 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 87.0 87.4 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.5 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.186 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 41 41 322 889 N I>3s 34 34 283 889 0.7 0.7 0.7 39.3 7.7 7.7 5.0 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.036 3536 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3575 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367481 8.375137 8.362163 90.0887 89.9751 89.9897 ZERR 3.00 0.000419 0.000525 0.000518 0.0051 0.0046 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5124602- 1105094 643 639 26 24.6 1835784.11 51.68 0.031 0.040 1080232- 267880 630 627 26 24.1 646770.57 42.71 0.043 0.055 267186- 130304 917 915 26 35.2 184580.36 28.16 0.037 0.049 126244- 94263 667 667 26 25.7 111930.21 18.52 0.053 0.069 92681- 3729 597 595 26 22.9 29643.45 9.13 0.068 0.091 3709- 1824 552 552 26 21.2 2979.44 3.90 0.200 0.252 ------------------------------------------------------------------------------------------- 5124602- 1824 4006 3995 156 25.6 460931.71 26.41 0.036 0.046 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 753 746 26 28.7 696477.64 36.69 0.034 0.042 0.019 1.12-0.88 896 896 26 34.5 586844.04 30.61 0.029 0.040 0.022 0.85-0.75 744 744 26 28.6 446143.67 25.49 0.033 0.045 0.025 0.74-0.68 662 661 26 25.4 371961.75 22.79 0.041 0.051 0.028 0.67-0.63 636 636 26 24.5 224094.36 17.88 0.054 0.072 0.036 0.62-0.59 315 312 26 12.0 242679.41 17.06 0.048 0.052 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 4006 3995 156 25.6 460931.71 26.41 0.036 0.046 0.024 inf-0.60 3873 3865 139 27.8 470782.66 26.77 0.036 0.046 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 746 26 26 100.0 28.7 696477.64 214.55 0.034 0.005 1.12-0.88 896 26 26 100.0 34.5 586844.04 181.56 0.029 0.004 0.85-0.75 744 26 26 100.0 28.6 446143.67 144.15 0.033 0.005 0.74-0.68 661 26 26 100.0 25.4 371961.75 117.09 0.041 0.006 0.67-0.63 636 26 26 100.0 24.5 224094.36 87.96 0.054 0.007 0.62-0.59 312 27 26 96.3 12.0 242679.41 69.96 0.048 0.014 -------------------------------------------------------------------------------------------- inf-0.59 3995 157 156 99.4 25.6 460931.71 146.47 0.036 0.006 inf-0.60 3865 139 139 100.0 27.8 470782.66 149.75 0.036 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007473 0.076825 -0.034788 ( 0.000006 0.000005 0.000005 ) -0.083555 -0.011761 -0.008066 ( 0.000004 0.000004 0.000004 ) -0.012180 0.033649 0.076938 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000001 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007173 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000011 0.007195 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007473 0.076825 -0.034788 ( 0.000006 0.000005 0.000005 ) -0.083555 -0.011761 -0.008066 ( 0.000004 0.000004 0.000004 ) -0.012180 0.033649 0.076938 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3675(4) 8.3751(5) 8.3622(5) 90.089(5) 89.975(5) 89.990(5) V = 586.01(6) unit cell: 8.36827(15) 8.36827(15) 8.36827(15) 90.0 90.0 90.0 V = 586.013(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: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.945) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=52.996) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=52.996) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.005) PROFFIT INFO: signal sum: min=159.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256697.8833 PROFFIT INFO: background sum: min=512.0000 max=17440.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11095.0000 PROFFIT INFO: num of signal pixels: min=56 max=883 PROFFIT INFO: Inet: min=530.6313 max=7105523.0000 PROFFIT INFO: sig(Inet): min=187.6440 max=63740.2305 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 12 208 656 1058 1666 1838 3346 5354 7294 8012 Percent 0.0 0.1 2.6 8.2 13.2 20.8 22.9 41.8 66.8 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4006 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 4006 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7105523- 1525132 400 2314472.29 134.37 100.00 1523014- 950651 400 1226303.35 106.69 100.00 949808- 300963 400 557418.16 93.49 100.00 300763- 206055 400 245846.82 67.66 100.00 205680- 156614 400 177646.64 47.87 100.00 156609- 123378 400 139460.36 36.62 100.00 123290- 92345 400 108903.88 29.08 100.00 92305- 6039 400 51376.48 20.02 100.00 6007- 3408 400 4424.60 4.83 80.50 3405- 531 406 2460.11 3.06 38.42 ------------------------------------------------------------------------------------ 7105523- 531 4006 482111.79 54.29 91.81 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 845255.46 87.54 100.00 1.41- 1.12 400 719497.22 69.36 98.75 1.12- 0.96 400 657167.45 76.10 98.00 0.96- 0.88 400 451606.77 58.14 94.25 0.88- 0.81 400 616056.47 68.47 97.25 0.81- 0.74 400 312984.89 39.64 91.75 0.74- 0.71 400 278065.87 37.39 89.00 0.71- 0.65 400 469630.11 48.18 95.25 0.65- 0.62 400 244923.45 29.20 73.50 0.62- 0.58 406 229716.16 29.25 80.54 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 482111.79 54.29 91.81 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:48:01 2018 Sorting 4006 observations 86 unique observations with > 7.00 F2/sig(F2) 4006 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 73 696 Total number of frames 696 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4006 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 12 60 6 0 11 72 7 0 8 81 Total number of frames 81 3217 observations > 7.00 F2/sig(F2) 3217 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 8 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 35.3 (Out of 3217 removed 4 = 3213, 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): 4/m3bar2/m 3213 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 8 80 Total number of frames 80 91 unique data precomputed (should be 91) 91 unique data with 3213 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 35.3 (Out of 3213 removed 0 = 3213, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3213 observations RMS deviation of equivalent data = 0.21686 Rint = 0.18265 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18254, wR= 0.23046 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13196, wR= 0.17587, Acormin=0.689, Acormax=1.293, Acor_av=0.938 F test: Probability=1.000, F= 1.910 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10693, wR= 0.13675, Acormin=0.541, Acormax=1.349, Acor_av=0.901 F test: Probability=1.000, F= 1.521 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11477, wR= 0.15554, Acormin=0.631, Acormax=1.415, Acor_av=0.952 F test: Probability=0.000, F= 0.866 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08552, wR= 0.11441, Acormin=0.490, Acormax=1.485, Acor_av=0.918 F test: Probability=1.000, F= 1.559 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07943, wR= 0.10718, Acormin=0.477, Acormax=1.410, Acor_av=0.885 F test: Probability=1.000, F= 1.157 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10755, wR= 0.14496, Acormin=0.610, Acormax=1.492, Acor_av=0.914 F test: Probability=0.000, F= 0.545 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08296, wR= 0.11070, Acormin=0.481, Acormax=1.487, Acor_av=0.905 F test: Probability=0.000, F= 0.915 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07702, wR= 0.10351, Acormin=0.470, Acormax=1.423, Acor_av=0.875 F test: Probability=0.944, F= 1.059 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07200, wR= 0.09709, Acormin=0.430, Acormax=1.302, Acor_av=0.807 F test: Probability=1.000, F= 1.208 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09177, wR= 0.11634, Acormin=0.261, Acormax=1.302, Acor_av=0.777 F test: Probability=0.000, F= 0.616 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08290, wR= 0.10715, Acormin=0.357, Acormax=1.380, Acor_av=0.823 F test: Probability=0.000, F= 0.755 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07604, wR= 0.09849, Acormin=0.141, Acormax=0.438, Acor_av=0.267 F test: Probability=0.000, F= 0.895 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06726, wR= 0.09029, Acormin=0.168, Acormax=0.475, Acor_av=0.299 F test: Probability=1.000, F= 1.140 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06275, wR= 0.08569, Acormin=0.168, Acormax=0.508, Acor_av=0.314 F test: Probability=1.000, F= 1.303 Final absorption model (ne=6, no=5): Rint= 0.07200, Acormin=0.430, Acormax=1.302, Acor_av=0.807 Combined refinement in use Rint: 0.18278 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #35 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 127 pars with 8128 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21686 Using Levenberg-Marquardt: 0.00010 New wR= 0.06081 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.04706 Rint for all data: 0.18278 with corrections 0.04728 0 observations identified as outliers and rejected Cycle 2 wR= 0.06081 Using Levenberg-Marquardt: 0.00001 New wR= 0.05437 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18265 with corrections 0.04186 Rint for all data: 0.18278 with corrections 0.04209 3 observations identified as outliers and rejected Cycle 3 wR= 0.05439 Using Levenberg-Marquardt: 0.00000 New wR= 0.05300 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18307 with corrections 0.04051 Rint for all data: 0.18278 with corrections 0.04077 0 observations identified as outliers and rejected Cycle 4 wR= 0.05300 Using Levenberg-Marquardt: 0.00000 New wR= 0.05238 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18307 with corrections 0.03989 Rint for all data: 0.18278 with corrections 0.04016 0 observations identified as outliers and rejected Cycle 5 wR= 0.05238 Using Levenberg-Marquardt: 0.00000 New wR= 0.05200 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18307 with corrections 0.03953 Rint for all data: 0.18278 with corrections 0.03980 0 observations identified as outliers and rejected Final wR= 0.05200 Final frame scales: Min= 0.7971 Max= 1.2181 Final absorption correction factors: Amin= 0.5663 Amax= 1.6134 PROFFIT INFO: Inet (after scale3 abspack): min=555.9548 max=5314694.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=153.4271 max=67350.3125 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 4006 reflections read from tmp file 653 reflections are rejected (653 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 5 0 1 2 3 2 1 94 Initial Chi^2= 0.34543 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94444 Current error model SIG(F2)^2 = 110.54*I_RAW + 0.00*I_BACK+(0.01812*)^2 Cycle 2, Chi^2= 1.00001 Current error model SIG(F2)^2 = 103.94*I_RAW + 0.00*I_BACK+(0.01770*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 103.94*I_RAW + 0.00*I_BACK+(0.01770*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5314695- 1471875 400 2202702.00 51.16 100.00 1471721- 946579 400 1164696.03 42.89 100.00 946186- 304226 400 564941.71 41.09 100.00 303852- 191285 400 233095.99 33.74 100.00 190939- 158047 400 173470.68 26.67 100.00 158021- 118579 400 133795.28 21.04 100.00 118555- 94483 400 106886.67 18.03 100.00 94436- 5534 400 54719.75 13.46 100.00 5525- 3238 400 4114.72 4.57 97.00 3233- 556 406 2487.27 3.48 64.29 ------------------------------------------------------------------------------------ 5314695- 556 4006 463399.64 25.58 96.08 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 854760.66 40.32 100.00 1.41- 1.12 400 708025.87 31.53 100.00 1.12- 0.96 400 620172.24 30.56 98.75 0.96- 0.88 400 432790.80 25.68 98.00 0.88- 0.81 400 584125.61 30.21 98.25 0.81- 0.74 400 292217.12 20.25 96.75 0.74- 0.71 400 262864.34 20.12 95.00 0.71- 0.65 400 438278.35 24.07 97.00 0.65- 0.62 400 231181.06 16.34 85.75 0.62- 0.58 406 213331.38 16.85 91.38 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 463399.64 25.58 96.08 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 400 854760.66 40.32 100.00 4.82- 1.12 800 781393.27 35.92 100.00 4.82- 0.96 1200 727652.93 34.14 99.58 4.82- 0.88 1600 653937.39 32.02 99.19 4.82- 0.81 2000 639975.04 31.66 99.00 4.82- 0.74 2400 582015.38 29.76 98.63 4.82- 0.71 2800 536422.38 28.38 98.11 4.82- 0.65 3200 524154.38 27.84 97.97 4.82- 0.62 3600 491601.78 26.56 96.61 4.82- 0.58 4006 463399.64 25.58 96.08 ------------------------------------------------------------------------------------ 4.82- 0.58 4006 463399.64 25.58 96.08 Scale applied to data: s=0.188157 (maximum obs:5314694.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.040; Rsigma 0.025: data 4006 -> merged 109 With outlier rejection... Rint 0.039; Rsigma 0.025: data 3998 -> merged 109 Rejected total: 8, method kkm 5, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585896, 4.831424 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.71 10 10 24.50 100.00 245 1.61 - 1.21 10 10 37.20 100.00 372 1.17 - 1.01 10 10 47.90 100.00 479 0.99 - 0.89 10 10 47.20 100.00 472 0.88 - 0.81 10 10 45.30 100.00 453 0.81 - 0.74 10 10 38.60 100.00 386 0.73 - 0.71 10 10 43.30 100.00 433 0.70 - 0.66 10 10 35.00 100.00 350 0.66 - 0.64 10 10 34.70 100.00 347 0.63 - 0.60 10 10 33.20 100.00 332 --------------------------------------------------------------- 8.39 - 0.60 100 100 38.69 100.00 3869 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:48:01 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367481 8.375137 8.362163 90.0887 89.9751 89.9897 3994 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2033 0 2671 2673 3994 N (int>3sigma) = 0 0 0 0 2033 0 2560 2562 3833 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 87.0 87.4 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.5 26.4 Lattice type: F chosen Volume: 586.01 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.913 5.914 5.916 90.04 119.95 119.93 Niggli form: a.a = 34.963 b.b = 34.970 c.c = 35.000 b.c = -0.022 a.c = -17.465 a.b = -17.444 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.116 CUBIC F-lattice R(int) = 0.036 [ 3838] Vol = 586.0 Cell: 8.367 8.375 8.362 90.09 89.98 89.99 Volume: 586.01 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.107 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3556] Vol = 439.5 Cell: 5.920 5.914 14.503 89.99 90.07 120.04 Volume: 439.51 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.107 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1150] Vol = 439.5 Trigonal Cell: 5.920 5.914 14.503 89.99 90.07 120.04 Volume: 439.51 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.047 TETRAGONAL I-lattice R(int) = 0.035 [ 3590] Vol = 293.0 Cell: 5.919 5.920 8.362 89.95 89.92 89.95 Volume: 293.00 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.117 TETRAGONAL I-lattice R(int) = 0.035 [ 3590] Vol = 293.0 Cell: 5.920 5.919 8.362 90.08 90.05 89.95 Volume: 293.00 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.057 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3536] Vol = 293.0 Cell: 5.920 5.919 8.362 89.92 89.95 89.95 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.051 ORTHORHOMBIC I-lattice R(int) = 0.034 [ 3533] Vol = 293.0 Cell: 5.913 8.367 5.922 89.99 89.91 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.034 [ 3192] Vol = 293.0 Cell: 5.919 5.920 8.362 90.05 90.08 89.95 Volume: 293.00 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.077 MONOCLINIC I-lattice R(int) = 0.033 [ 3190] Vol = 293.0 Cell: 5.913 5.922 8.367 90.01 90.02 90.09 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.034 MONOCLINIC I-lattice R(int) = 0.031 [ 3204] Vol = 293.0 Cell: 5.913 8.367 5.922 89.99 90.09 89.98 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.041 MONOCLINIC I-lattice R(int) = 0.034 [ 3188] Vol = 293.0 Cell: 5.922 5.913 8.367 89.98 90.01 89.91 Volume: 293.00 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.088 MONOCLINIC C-lattice R(int) = 0.032 [ 3188] Vol = 293.0 Cell: 10.249 5.914 5.916 90.04 125.20 89.92 Volume: 293.00 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.030 [ 2537] Vol = 146.5 Cell: 5.913 5.914 5.916 90.04 119.95 119.93 Volume: 146.50 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2033 0 2671 2673 3994 N (int>3sigma) = 0 0 0 0 2033 0 2560 2562 3833 Mean intensity = 0.0 0.0 0.0 0.0 33.4 0.0 87.0 87.4 86.7 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.5 26.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.186 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 41 41 322 889 N I>3s 34 34 283 889 0.7 0.7 0.7 39.3 7.7 7.7 5.0 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.036 3536 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3575 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367481 8.375137 8.362163 90.0887 89.9751 89.9897 ZERR 3.00 0.000419 0.000525 0.000518 0.0051 0.0046 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5072851- 860012 891 888 27 32.9 1600360.47 46.02 0.036 0.049 849374- 146858 1184 1181 27 43.7 269621.04 33.00 0.042 0.052 138707- 49653 988 987 27 36.6 106715.82 18.20 0.058 0.076 20549- 1813 943 942 28 33.6 4431.97 4.60 0.159 0.201 ------------------------------------------------------------------------------------------- 5072851- 1813 4006 3998 109 36.7 462492.74 25.55 0.039 0.051 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1013 1009 27 37.4 743388.71 35.78 0.034 0.048 0.021 1.01-0.78 1254 1254 28 44.8 436963.89 24.50 0.035 0.048 0.025 0.76-0.65 1065 1063 28 38.0 353990.76 21.42 0.044 0.055 0.029 0.65-0.59 674 672 26 25.8 260002.80 18.68 0.057 0.061 0.035 ------------------------------------------------------------------------------------------------------ inf-0.59 4006 3998 109 36.7 462492.74 25.55 0.039 0.051 0.025 inf-0.60 3873 3867 99 39.1 472328.95 25.88 0.039 0.051 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1009 27 27 100.0 37.4 743388.71 245.17 0.034 0.005 1.01-0.78 1254 28 28 100.0 44.8 436963.89 174.54 0.035 0.004 0.76-0.65 1063 28 28 100.0 38.0 353990.76 140.91 0.044 0.006 0.65-0.59 672 27 26 96.3 25.8 260002.80 110.98 0.057 0.010 -------------------------------------------------------------------------------------------- inf-0.59 3998 110 109 99.1 36.7 462492.74 172.74 0.039 0.006 inf-0.60 3867 99 99 100.0 39.1 472328.95 176.28 0.039 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:51:57 2018) ID: 2932; threads 39; handles 878; mem 516128.00 (1237728.00)kB; time: 1w 5d 23h 57m 27s MEMORY INFO: Memory PF:0.0, Ph:170.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:504.0,peak PF: 708.5, WS: 268.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:170.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.8,peak PF: 708.5, WS: 270.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:51:57 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000005 ) 8.37051 ( 0.00042 ) 8.37682 ( 0.00052 ) 8.35710 ( 0.00052 ) 90.12473 ( 0.00503 ) 89.98579 ( 0.00461 ) 90.00567 ( 0.00467 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:51:57 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007186 -0.000001 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007173 0.000011 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000011 0.007195 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(5) 90.006(5) V = 585.98(6) unit cell: 8.36827(15) 8.36827(15) 8.36827(15) 90.0 90.0 90.0 V = 586.013(18) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb PROFFITPEAK info: 1006 peaks in the peak location table UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) OTKP changes: 94 1 1 1 UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) 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 1 487 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.307) HKL list info: 707 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 457 obs out of 487 (total:487,skipped:0) (93.84%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 1 of 419 peaks identified as outliers and rejected 418 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 418 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 418 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 42 | 1.093 ( 0.273) | 1.325 ( 0.679) | 1.498 ( 1.008) | 1.42- 1.17 | 42 | 1.077 ( 0.066) | 1.144 ( 0.405) | 1.094 ( 0.487) | 1.17- 0.99 | 42 | 1.098 ( 0.065) | 1.070 ( 0.105) | 1.114 ( 0.480) | 0.99- 0.92 | 42 | 1.140 ( 0.048) | 1.099 ( 0.110) | 1.080 ( 0.426) | 0.92- 0.82 | 42 | 1.171 ( 0.047) | 1.098 ( 0.111) | 1.244 ( 0.490) | 0.82- 0.76 | 42 | 1.178 ( 0.059) | 1.079 ( 0.121) | 1.263 ( 0.485) | 0.76- 0.71 | 42 | 1.207 ( 0.058) | 1.096 ( 0.157) | 1.313 ( 0.450) | 0.71- 0.67 | 42 | 1.212 ( 0.066) | 1.118 ( 0.133) | 1.335 ( 0.459) | 0.67- 0.63 | 42 | 1.213 ( 0.079) | 1.199 ( 0.128) | 1.310 ( 0.450) | 0.63- 0.59 | 40 | 1.251 ( 0.107) | 1.125 ( 0.120) | 1.547 ( 0.592) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 418 | 1.164 ( 0.122) | 1.135 ( 0.284) | 1.279 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 415 obs out of 418 (total:418,skipped:0) (99.28%) UB - matrix: -0.007354 0.076558 -0.034855 ( 0.000014 0.000017 0.000013 ) -0.083297 -0.011621 -0.008117 ( 0.000012 0.000014 0.000011 ) -0.011999 0.033378 0.076669 ( 0.000014 0.000017 0.000013 ) M - matrix: 0.007136 0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) 0.000004 0.007110 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000015 0.007159 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3964(12) 8.4117(16) 8.3831(14) 89.879(14) 90.100(12) 90.036(13) V = 592.08(17) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 703 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 3 of 420 peaks identified as outliers and rejected 417 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 417 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 417 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 42 | 1.065 ( 0.164) | 1.299 ( 0.681) | 1.465 ( 0.960) | 1.41- 1.17 | 42 | 1.085 ( 0.067) | 1.159 ( 0.376) | 1.063 ( 0.455) | 1.17- 0.98 | 42 | 1.104 ( 0.068) | 1.081 ( 0.108) | 1.141 ( 0.463) | 0.98- 0.92 | 42 | 1.145 ( 0.044) | 1.099 ( 0.103) | 1.097 ( 0.417) | 0.92- 0.82 | 42 | 1.172 ( 0.053) | 1.097 ( 0.119) | 1.207 ( 0.493) | 0.82- 0.76 | 42 | 1.182 ( 0.066) | 1.088 ( 0.124) | 1.323 ( 0.462) | 0.76- 0.71 | 42 | 1.209 ( 0.056) | 1.100 ( 0.155) | 1.304 ( 0.443) | 0.71- 0.67 | 42 | 1.214 ( 0.069) | 1.131 ( 0.134) | 1.371 ( 0.474) | 0.67- 0.62 | 42 | 1.225 ( 0.076) | 1.206 ( 0.140) | 1.310 ( 0.480) | 0.62- 0.59 | 39 | 1.253 ( 0.105) | 1.137 ( 0.127) | 1.584 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 417 | 1.165 ( 0.103) | 1.140 ( 0.279) | 1.284 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 311 | 1.145 ( 0.113) | 1.245 ( 0.413) | 1.294 ( 0.633) | 13.1-18.7 | 311 | 1.133 ( 0.078) | 1.183 ( 0.295) | 1.264 ( 0.581) | 18.7-23.0 | 311 | 1.144 ( 0.088) | 1.184 ( 0.261) | 1.270 ( 0.662) | 23.0-27.2 | 311 | 1.132 ( 0.097) | 1.167 ( 0.293) | 1.226 ( 0.583) | 27.2-30.4 | 311 | 1.137 ( 0.097) | 1.153 ( 0.263) | 1.201 ( 0.451) | 30.4-33.6 | 311 | 1.146 ( 0.100) | 1.132 ( 0.208) | 1.200 ( 0.441) | 33.6-37.0 | 311 | 1.145 ( 0.096) | 1.116 ( 0.188) | 1.176 ( 0.434) | 37.0-39.7 | 311 | 1.151 ( 0.116) | 1.094 ( 0.200) | 1.247 ( 0.523) | 39.8-42.8 | 311 | 1.165 ( 0.112) | 1.102 ( 0.251) | 1.224 ( 0.531) | 42.8-50.5 | 312 | 1.212 ( 0.149) | 1.120 ( 0.254) | 1.227 ( 0.497) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.5 | 3111 | 1.151 ( 0.109) | 1.150 ( 0.273) | 1.233 ( 0.540) | Fitted profile normalization line parameters e1 dimension: a=0.0021 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0020 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464571 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:52:29 2018 PROFFITMAIN - Started at Wed Mar 28 14:52:29 2018 OTKP changes: 3096 2 4 6 OTKP changes: 3096 2 4 6 OTKP changes: 3096 2 4 6 No constraint UB - matrix: -0.007487 0.076861 -0.034834 ( 0.000006 0.000006 0.000006 ) -0.083584 -0.011770 -0.008061 ( 0.000004 0.000004 0.000004 ) -0.012142 0.033654 0.076992 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007190 -0.000000 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007179 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000009 0.007206 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007487 0.076861 -0.034834 ( 0.000006 0.000006 0.000006 ) -0.083584 -0.011770 -0.008061 ( 0.000004 0.000004 0.000004 ) -0.012142 0.033654 0.076992 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007190 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007190 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007190 ( 0.000000 0.000000 0.000000 ) UB fit with 3101 obs out of 3111 (total:3111,skipped:0) (99.68%) unit cell: 8.3651(4) 8.3716(5) 8.3556(5) 90.068(5) 89.998(5) 89.998(5) V = 585.14(6) unit cell: 8.36410(13) 8.36410(13) 8.36410(13) 90.0 90.0 90.0 V = 585.136(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007134 0.076820 -0.034876 ( 0.000016 0.000011 0.000018 ) -0.083536 -0.011636 -0.008043 ( 0.000013 0.000009 0.000015 ) -0.012413 0.033806 0.076702 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007183 0.000004 -0.000031 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007180 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000031 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3690(13) 8.3711(13) 8.3801(15) 90.059(14) 89.749(14) 90.035(13) V = 587.09(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007220 0.076689 -0.035005 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011686 -0.008070 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076838 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007220 0.076689 -0.035005 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011686 -0.008070 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076838 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3679(13) 8.3772(12) 8.3623(15) 90.135(13) 89.822(13) 90.028(12) V = 586.19(16) unit cell: 8.3691(3) 8.3691(3) 8.3691(3) 90.0 90.0 90.0 V = 586.19(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.009) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007220 0.076689 -0.035005 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011686 -0.008070 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076838 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007220 0.076689 -0.035005 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011686 -0.008070 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076838 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3679(13) 8.3772(12) 8.3623(15) 90.135(13) 89.822(13) 90.028(12) V = 586.19(16) unit cell: 8.3691(3) 8.3691(3) 8.3691(3) 90.0 90.0 90.0 V = 586.19(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084640 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000010 0.084724 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084783 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007164 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007178 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007188 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084640 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000010 0.084724 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084783 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3802(16) 8.3718(8) 8.3661(10) 90.058(10) 89.872(13) 90.082(11) V = 586.94(14) unit cell: 8.3727(3) 8.3727(3) 8.3727(3) 90.0 90.0 90.0 V = 586.94(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007575 0.076989 -0.034604 ( 0.000014 0.000013 0.000012 ) -0.083450 -0.011890 -0.008147 ( 0.000011 0.000011 0.000009 ) -0.012249 0.033277 0.076950 ( 0.000012 0.000012 0.000010 ) M - matrix: 0.007171 0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) 0.000001 0.007176 -0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 -0.000007 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3759(11) 8.3731(13) 8.3678(11) 89.947(11) 89.996(11) 90.011(12) V = 586.86(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3699(11) 8.3737(12) 8.3702(10) 90.000(10) 90.053(10) 90.087(11) V = 586.64(13) unit cell: 8.3713(4) 8.3713(4) 8.3713(4) 90.0 90.0 90.0 V = 586.64(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.009) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3699(11) 8.3737(12) 8.3702(10) 90.000(10) 90.053(10) 90.087(11) V = 586.64(13) unit cell: 8.3713(4) 8.3713(4) 8.3713(4) 90.0 90.0 90.0 V = 586.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076959 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083525 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076940 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3699(11) 8.3737(12) 8.3702(10) 90.000(10) 90.053(10) 90.087(11) V = 586.64(13) unit cell: 8.3713(4) 8.3713(4) 8.3713(4) 90.0 90.0 90.0 V = 586.64(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) UB - matrix: -0.007468 0.076669 -0.034978 ( 0.000013 0.000016 0.000012 ) -0.083544 -0.011732 -0.008154 ( 0.000011 0.000013 0.000010 ) -0.012244 0.033568 0.076823 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000003 0.000002 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007143 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000002 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3678(11) 8.3927(14) 8.3640(13) 89.942(13) 90.014(11) 89.973(12) V = 587.39(16) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 701 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007479 0.076814 -0.034803 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008071 ( 0.000004 0.000004 0.000004 ) -0.012183 0.033647 0.076927 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007186 -0.000002 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007171 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007479 0.076814 -0.034803 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008071 ( 0.000004 0.000004 0.000004 ) -0.012183 0.033647 0.076927 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 3104 obs out of 3111 (total:3111,skipped:0) (99.77%) unit cell: 8.3673(4) 8.3762(5) 8.3626(5) 90.080(5) 89.980(5) 89.984(5) V = 586.10(6) unit cell: 8.36868(15) 8.36868(15) 8.36868(15) 90.0 90.0 90.0 V = 586.099(18) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 76 reflections under beam stop or inside a detector rejection region 33 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof 4122 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:52:38 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.009) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.009) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) PROFFIT INFO: signal sum: min=159.0000 max=22699116.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257847.0086 PROFFIT INFO: background sum: min=524.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11129.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7108030.0000 PROFFIT INFO: sig(Inet): min=187.7619 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 5 108 338 545 859 948 1727 2753 3754 4122 Percent 0.0 0.1 2.6 8.2 13.2 20.8 23.0 41.9 66.8 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4122 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 4122 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7108030- 1521585 412 2305613.52 134.68 100.00 1520973- 947870 412 1219417.46 106.12 100.00 947103- 299057 412 552858.92 93.63 100.00 298872- 204935 412 245003.32 67.32 100.00 204618- 156199 412 176934.37 47.47 100.00 156175- 123245 412 139073.16 36.64 100.00 123057- 91797 412 108441.15 28.97 100.00 91789- 5932 412 50437.45 19.79 100.00 5917- 3408 412 4384.34 4.79 79.85 3404- 531 414 2457.90 3.04 38.41 ------------------------------------------------------------------------------------ 7108030- 531 4122 480230.23 54.22 91.80 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 828754.07 87.41 100.00 1.41- 1.12 412 738853.01 69.97 98.79 1.12- 0.96 412 640434.37 75.31 98.30 0.96- 0.88 412 449954.94 58.16 94.17 0.88- 0.81 412 613738.75 68.30 97.09 0.81- 0.74 412 318437.25 39.80 91.75 0.74- 0.71 412 268094.70 36.60 89.32 0.71- 0.65 412 470694.40 48.48 95.39 0.65- 0.62 412 244831.91 29.10 73.30 0.62- 0.58 414 229724.95 29.19 79.95 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 480230.23 54.22 91.80 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:52:38 2018 Sorting 4122 observations 120 unique observations with > 7.00 F2/sig(F2) 4122 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 Total number of frames 715 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4122 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 18 90 6 0 16 107 7 0 15 123 Total number of frames 123 3311 observations > 7.00 F2/sig(F2) 3311 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 15 122 Total number of frames 122 Removing 'redundancy=1' reflections Average redundancy: 26.0 (Out of 3311 removed 5 = 3306, 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 3306 observations in 7 runs Run # start # end # total # 1 0 17 18 2 0 18 37 3 0 16 54 4 0 16 71 5 0 17 89 6 0 16 106 7 0 15 122 Total number of frames 122 127 unique data precomputed (should be 127) 127 unique data with 3306 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.0 (Out of 3306 removed 0 = 3306, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3306 observations RMS deviation of equivalent data = 0.21449 Rint = 0.17980 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17928, wR= 0.22696 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13062, wR= 0.17238, Acormin=0.688, Acormax=1.301, Acor_av=0.939 F test: Probability=1.000, F= 1.881 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10511, wR= 0.13425, Acormin=0.545, Acormax=1.355, Acor_av=0.905 F test: Probability=1.000, F= 1.543 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11221, wR= 0.15217, Acormin=0.625, Acormax=1.424, Acor_av=0.954 F test: Probability=0.000, F= 0.876 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08304, wR= 0.11125, Acormin=0.490, Acormax=1.491, Acor_av=0.921 F test: Probability=1.000, F= 1.598 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07825, wR= 0.10484, Acormin=0.476, Acormax=1.389, Acor_av=0.895 F test: Probability=0.999, F= 1.124 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10488, wR= 0.14199, Acormin=0.608, Acormax=1.501, Acor_av=0.916 F test: Probability=0.000, F= 0.556 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08002, wR= 0.10733, Acormin=0.489, Acormax=1.502, Acor_av=0.908 F test: Probability=0.000, F= 0.954 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07540, wR= 0.10065, Acormin=0.472, Acormax=1.411, Acor_av=0.884 F test: Probability=0.975, F= 1.072 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07051, wR= 0.09501, Acormin=0.431, Acormax=1.298, Acor_av=0.816 F test: Probability=1.000, F= 1.139 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08927, wR= 0.11293, Acormin=0.284, Acormax=1.317, Acor_av=0.788 F test: Probability=0.000, F= 0.625 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08060, wR= 0.10367, Acormin=0.372, Acormax=1.407, Acor_av=0.833 F test: Probability=0.000, F= 0.766 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07480, wR= 0.09701, Acormin=0.149, Acormax=0.449, Acor_av=0.278 F test: Probability=0.000, F= 0.887 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06654, wR= 0.08914, Acormin=0.173, Acormax=0.495, Acor_av=0.311 F test: Probability=0.999, F= 1.117 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06211, wR= 0.08419, Acormin=0.177, Acormax=0.533, Acor_av=0.328 F test: Probability=1.000, F= 1.276 Final absorption model (ne=6, no=5): Rint= 0.07051, Acormin=0.431, Acormax=1.298, Acor_av=0.816 Combined refinement in use Rint: 0.17993 There are 122 active scales (one needs to be fixed) Refinement control: frame scale #93 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 169 pars with 14365 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21449 Using Levenberg-Marquardt: 0.00010 New wR= 0.05284 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17980 with corrections 0.04107 Rint for all data: 0.17993 with corrections 0.04129 2 observations identified as outliers and rejected Cycle 2 wR= 0.05233 Using Levenberg-Marquardt: 0.00001 New wR= 0.04890 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17942 with corrections 0.03747 Rint for all data: 0.17993 with corrections 0.03785 1 observations identified as outliers and rejected Cycle 3 wR= 0.04893 Using Levenberg-Marquardt: 0.00000 New wR= 0.04828 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17962 with corrections 0.03672 Rint for all data: 0.17993 with corrections 0.03710 0 observations identified as outliers and rejected Cycle 4 wR= 0.04828 Using Levenberg-Marquardt: 0.00000 New wR= 0.04794 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17962 with corrections 0.03634 Rint for all data: 0.17993 with corrections 0.03672 0 observations identified as outliers and rejected Cycle 5 wR= 0.04794 Using Levenberg-Marquardt: 0.00000 New wR= 0.04774 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17962 with corrections 0.03612 Rint for all data: 0.17993 with corrections 0.03650 0 observations identified as outliers and rejected Final wR= 0.04774 Final frame scales: Min= 0.7745 Max= 1.1736 Final absorption correction factors: Amin= 0.5765 Amax= 1.5360 PROFFIT INFO: Inet (after scale3 abspack): min=549.7477 max=5318282.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=152.9574 max=69133.7031 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 4122 reflections read from tmp file 594 reflections are rejected (594 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 4 2 1 3 2 1 2 136 Initial Chi^2= 0.36475 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.90241 Current error model SIG(F2)^2 = 116.83*I_RAW + 0.00*I_BACK+(0.01700*)^2 Cycle 2, Chi^2= 0.99999 Current error model SIG(F2)^2 = 103.54*I_RAW + 0.00*I_BACK+(0.01659*)^2 Cycle 3, Chi^2= 1.00002 Current error model SIG(F2)^2 = 103.93*I_RAW + 0.00*I_BACK+(0.01649*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 103.85*I_RAW + 0.00*I_BACK+(0.01651*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 103.85*I_RAW + 0.00*I_BACK+(0.01651*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5318283- 1472041 412 2195970.57 54.06 100.00 1467376- 938935 412 1157628.97 44.45 100.00 937918- 302007 412 560384.70 42.64 100.00 301696- 190615 412 232756.13 34.61 100.00 190614- 158165 412 173155.71 27.08 100.00 158165- 118648 412 133519.01 21.14 100.00 118638- 94541 412 106573.58 18.13 100.00 94460- 5399 412 53623.98 13.38 100.00 5392- 3216 412 4094.98 4.56 96.84 3214- 550 414 2482.42 3.49 65.22 ------------------------------------------------------------------------------------ 5318283- 550 4122 461796.04 26.34 96.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 837704.06 42.06 100.00 1.41- 1.12 412 726047.36 32.96 100.00 1.12- 0.96 412 605324.53 31.42 99.03 0.96- 0.88 412 433470.09 26.51 98.30 0.88- 0.81 412 581046.45 31.14 98.30 0.81- 0.74 412 297870.03 20.70 96.84 0.74- 0.71 412 253698.49 20.20 95.15 0.71- 0.65 412 439435.38 24.86 97.33 0.65- 0.62 412 231526.81 16.56 85.92 0.62- 0.58 414 213044.71 17.07 91.06 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 461796.04 26.34 96.19 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 837704.06 42.06 100.00 4.82- 1.12 824 781875.71 37.51 100.00 4.82- 0.96 1236 723025.32 35.48 99.68 4.82- 0.88 1648 650636.51 33.24 99.33 4.82- 0.81 2060 636718.50 32.82 99.13 4.82- 0.74 2472 580243.75 30.80 98.75 4.82- 0.71 2884 533594.43 29.28 98.23 4.82- 0.65 3296 521824.55 28.73 98.12 4.82- 0.62 3708 489569.24 27.38 96.76 4.82- 0.58 4122 461796.04 26.34 96.19 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 461796.04 26.34 96.19 Scale applied to data: s=0.188030 (maximum obs:5318282.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.037; Rsigma 0.024: data 4122 -> merged 156 With outlier rejection... Rint 0.036; Rsigma 0.024: data 4111 -> merged 156 Rejected total: 11, method kkm 8, method Blessing 3 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585925, 4.831659 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.48 14 14 24.00 100.00 336 1.41 - 1.12 14 14 34.14 100.00 478 1.12 - 0.97 14 14 34.07 100.00 477 0.96 - 0.84 14 14 36.50 100.00 511 0.84 - 0.78 14 14 27.50 100.00 385 0.78 - 0.73 14 14 29.07 100.00 407 0.73 - 0.69 14 14 27.57 100.00 386 0.69 - 0.66 14 14 23.36 100.00 327 0.65 - 0.63 14 14 25.36 100.00 355 0.63 - 0.60 14 14 22.50 100.00 315 --------------------------------------------------------------- 8.39 - 0.60 140 140 28.41 100.00 3977 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:52:39 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367294 8.376175 8.362583 90.0795 89.9797 89.9843 4111 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2093 0 2749 2754 4111 N (int>3sigma) = 0 0 0 0 2093 0 2642 2646 3954 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.6 87.6 86.5 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.4 26.4 26.3 Lattice type: F chosen Volume: 586.10 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.914 5.914 5.916 119.96 90.03 119.93 Niggli form: a.a = 34.974 b.b = 34.975 c.c = 34.998 b.c = -17.470 a.c = -0.020 a.b = -17.448 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.092 CUBIC F-lattice R(int) = 0.036 [ 3955] Vol = 586.1 Cell: 8.363 8.376 8.367 89.98 89.98 90.08 Volume: 586.10 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.089 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3673] Vol = 439.6 Cell: 5.914 5.914 14.502 90.01 90.06 119.93 Volume: 439.57 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.089 RHOMBOHEDRAL R-lattice R(int) = 0.035 [ 1185] Vol = 439.6 Trigonal Cell: 5.914 5.914 14.502 90.01 90.06 119.93 Volume: 439.57 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.150 TETRAGONAL I-lattice R(int) = 0.035 [ 3706] Vol = 293.0 Cell: 5.921 5.919 8.363 89.93 90.04 90.06 Volume: 293.05 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.110 TETRAGONAL I-lattice R(int) = 0.035 [ 3706] Vol = 293.0 Cell: 5.921 5.919 8.363 89.93 90.04 90.06 Volume: 293.05 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.050 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3653] Vol = 293.0 Cell: 5.921 8.363 5.919 89.93 89.94 89.96 Volume: 293.05 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.036 MONOCLINIC I-lattice R(int) = 0.034 [ 3309] Vol = 293.0 Cell: 8.363 5.921 5.919 90.06 90.07 89.96 Volume: 293.05 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.044 MONOCLINIC I-lattice R(int) = 0.032 [ 3304] Vol = 293.0 Cell: 5.916 5.914 8.376 89.93 90.05 89.97 Volume: 293.05 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.106 MONOCLINIC C-lattice R(int) = 0.032 [ 3326] Vol = 293.0 Cell: 8.363 8.376 5.914 89.93 134.97 90.08 Volume: 293.05 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.030 [ 2653] Vol = 146.5 Cell: 5.914 5.914 5.916 119.96 90.03 119.93 Volume: 146.52 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2093 0 2732 2754 4111 N (int>3sigma) = 0 0 0 0 2093 0 2632 2646 3954 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 89.0 87.6 86.5 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.4 26.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.188 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 328 918 N I>3s 36 36 293 918 0.7 0.7 0.7 39.1 7.7 7.7 5.1 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 3647 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3686 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362583 8.376175 8.367294 89.9843 89.9797 90.0795 ZERR 3.00 0.000511 0.000529 0.000413 0.0047 0.0046 0.0050 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5130060- 1102708 658 654 26 25.2 1836581.25 51.04 0.031 0.042 1078889- 267712 649 646 26 24.8 648141.43 42.43 0.042 0.055 267656- 130227 945 944 26 36.3 184972.42 28.30 0.037 0.050 125439- 94975 687 687 26 26.4 111746.39 18.64 0.053 0.069 92601- 3753 611 609 26 23.4 29678.66 9.20 0.066 0.089 3726- 1825 572 571 26 22.0 2996.75 3.95 0.201 0.253 ------------------------------------------------------------------------------------------- 5130060- 1825 4122 4111 156 26.4 459983.62 26.31 0.036 0.047 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 773 768 26 29.5 695003.24 36.36 0.035 0.045 0.019 1.12-0.88 924 923 26 35.5 585075.03 30.46 0.030 0.042 0.022 0.85-0.75 765 764 26 29.4 443602.10 25.36 0.032 0.044 0.025 0.74-0.68 679 678 26 26.1 374830.12 22.90 0.040 0.050 0.028 0.67-0.63 654 654 26 25.2 223590.51 17.91 0.052 0.071 0.036 0.62-0.59 327 324 26 12.5 240527.51 17.03 0.048 0.052 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 4122 4111 156 26.4 459983.62 26.31 0.036 0.047 0.024 inf-0.60 3983 3975 139 28.6 470123.00 26.68 0.035 0.047 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 768 26 26 100.0 29.5 695003.24 215.64 0.035 0.005 1.12-0.88 923 26 26 100.0 35.5 585075.03 183.75 0.030 0.004 0.85-0.75 764 26 26 100.0 29.4 443602.10 144.92 0.032 0.005 0.74-0.68 678 26 26 100.0 26.1 374830.12 119.81 0.040 0.006 0.67-0.63 654 26 26 100.0 25.2 223590.51 89.52 0.052 0.007 0.62-0.59 324 27 26 96.3 12.5 240527.51 71.44 0.048 0.014 -------------------------------------------------------------------------------------------- inf-0.59 4111 157 156 99.4 26.4 459983.62 148.10 0.036 0.006 inf-0.60 3975 139 139 100.0 28.6 470123.00 151.47 0.035 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007479 0.076814 -0.034802 ( 0.000006 0.000005 0.000005 ) -0.083557 -0.011758 -0.008071 ( 0.000004 0.000004 0.000004 ) -0.012183 0.033647 0.076927 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007186 -0.000002 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007171 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007479 0.076814 -0.034802 ( 0.000006 0.000005 0.000005 ) -0.083557 -0.011758 -0.008071 ( 0.000004 0.000004 0.000004 ) -0.012183 0.033647 0.076927 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3673(4) 8.3762(5) 8.3626(5) 90.080(5) 89.980(4) 89.984(5) V = 586.10(6) unit cell: 8.36870(14) 8.36870(14) 8.36870(14) 90.0 90.0 90.0 V = 586.104(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: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.009) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.009) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) PROFFIT INFO: signal sum: min=159.0000 max=22699116.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257847.0086 PROFFIT INFO: background sum: min=524.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11129.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7108030.0000 PROFFIT INFO: sig(Inet): min=187.7619 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 10 216 676 1090 1718 1896 3454 5506 7508 8244 Percent 0.0 0.1 2.6 8.2 13.2 20.8 23.0 41.9 66.8 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4122 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 4122 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7108030- 1521585 412 2305613.52 134.68 100.00 1520973- 947870 412 1219417.46 106.12 100.00 947103- 299057 412 552858.92 93.63 100.00 298872- 204935 412 245003.32 67.32 100.00 204618- 156199 412 176934.37 47.47 100.00 156175- 123245 412 139073.16 36.64 100.00 123057- 91797 412 108441.15 28.97 100.00 91789- 5932 412 50437.45 19.79 100.00 5917- 3408 412 4384.34 4.79 79.85 3404- 531 414 2457.90 3.04 38.41 ------------------------------------------------------------------------------------ 7108030- 531 4122 480230.23 54.22 91.80 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 828754.07 87.41 100.00 1.41- 1.12 412 738853.01 69.97 98.79 1.12- 0.96 412 640434.37 75.31 98.30 0.96- 0.88 412 449954.94 58.16 94.17 0.88- 0.81 412 613738.75 68.30 97.09 0.81- 0.74 412 318437.25 39.80 91.75 0.74- 0.71 412 268094.70 36.60 89.32 0.71- 0.65 412 470694.40 48.48 95.39 0.65- 0.62 412 244831.91 29.10 73.30 0.62- 0.58 414 229724.95 29.19 79.95 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 480230.23 54.22 91.80 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:52:40 2018 Sorting 4122 observations 86 unique observations with > 7.00 F2/sig(F2) 4122 observations in 7 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 Total number of frames 715 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4122 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 12 60 6 0 11 72 7 0 10 83 Total number of frames 83 3311 observations > 7.00 F2/sig(F2) 3311 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 Total number of frames 82 Removing 'redundancy=1' reflections Average redundancy: 36.3 (Out of 3311 removed 4 = 3307, 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): 4/m3bar2/m 3307 observations in 7 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 Total number of frames 82 91 unique data precomputed (should be 91) 91 unique data with 3307 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 36.3 (Out of 3307 removed 0 = 3307, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3307 observations RMS deviation of equivalent data = 0.21496 Rint = 0.18003 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17955, wR= 0.22761 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13107, wR= 0.17343, Acormin=0.688, Acormax=1.298, Acor_av=0.939 F test: Probability=1.000, F= 1.874 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10548, wR= 0.13483, Acormin=0.545, Acormax=1.353, Acor_av=0.905 F test: Probability=1.000, F= 1.543 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11352, wR= 0.15403, Acormin=0.631, Acormax=1.418, Acor_av=0.952 F test: Probability=0.000, F= 0.862 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08405, wR= 0.11265, Acormin=0.489, Acormax=1.484, Acor_av=0.920 F test: Probability=1.000, F= 1.570 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07884, wR= 0.10619, Acormin=0.475, Acormax=1.400, Acor_av=0.893 F test: Probability=1.000, F= 1.134 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10661, wR= 0.14394, Acormin=0.609, Acormax=1.489, Acor_av=0.913 F test: Probability=0.000, F= 0.546 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08134, wR= 0.10887, Acormin=0.480, Acormax=1.487, Acor_av=0.906 F test: Probability=0.000, F= 0.938 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07610, wR= 0.10212, Acormin=0.472, Acormax=1.422, Acor_av=0.881 F test: Probability=0.970, F= 1.069 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07106, wR= 0.09595, Acormin=0.429, Acormax=1.297, Acor_av=0.814 F test: Probability=1.000, F= 1.143 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09050, wR= 0.11465, Acormin=0.298, Acormax=1.314, Acor_av=0.786 F test: Probability=0.000, F= 0.617 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08162, wR= 0.10506, Acormin=0.383, Acormax=1.398, Acor_av=0.831 F test: Probability=0.000, F= 0.758 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07521, wR= 0.09788, Acormin=0.148, Acormax=0.446, Acor_av=0.273 F test: Probability=0.000, F= 0.891 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06675, wR= 0.08954, Acormin=0.171, Acormax=0.487, Acor_av=0.307 F test: Probability=1.000, F= 1.127 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06232, wR= 0.08475, Acormin=0.173, Acormax=0.525, Acor_av=0.324 F test: Probability=1.000, F= 1.287 Final absorption model (ne=6, no=5): Rint= 0.07106, Acormin=0.429, Acormax=1.297, Acor_av=0.814 Combined refinement in use Rint: 0.18016 There are 82 active scales (one needs to be fixed) Refinement control: frame scale #35 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 129 pars with 8385 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21496 Using Levenberg-Marquardt: 0.00010 New wR= 0.06005 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18003 with corrections 0.04658 Rint for all data: 0.18016 with corrections 0.04680 3 observations identified as outliers and rejected Cycle 2 wR= 0.05983 Using Levenberg-Marquardt: 0.00001 New wR= 0.05371 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17925 with corrections 0.04126 Rint for all data: 0.18016 with corrections 0.04176 7 observations identified as outliers and rejected Cycle 3 wR= 0.05326 Using Levenberg-Marquardt: 0.00000 New wR= 0.05170 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17836 with corrections 0.03946 Rint for all data: 0.18016 with corrections 0.04026 5 observations identified as outliers and rejected Cycle 4 wR= 0.05181 Using Levenberg-Marquardt: 0.00000 New wR= 0.05116 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17794 with corrections 0.03879 Rint for all data: 0.18016 with corrections 0.03965 1 observations identified as outliers and rejected Cycle 5 wR= 0.05122 Using Levenberg-Marquardt: 0.00000 New wR= 0.05085 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.17803 with corrections 0.03843 Rint for all data: 0.18016 with corrections 0.03926 0 observations identified as outliers and rejected Final wR= 0.05085 Final frame scales: Min= 0.8067 Max= 1.2142 Final absorption correction factors: Amin= 0.5448 Amax= 1.5935 PROFFIT INFO: Inet (after scale3 abspack): min=551.9525 max=5322547.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=152.1259 max=67347.1641 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 4122 reflections read from tmp file 653 reflections are rejected (653 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 0 1 3 2 2 1 94 Initial Chi^2= 0.32334 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93543 Current error model SIG(F2)^2 = 110.79*I_RAW + 0.00*I_BACK+(0.01665*)^2 Cycle 2, Chi^2= 0.99993 Current error model SIG(F2)^2 = 100.15*I_RAW + 0.00*I_BACK+(0.01684*)^2 Cycle 3, Chi^2= 1.00001 Current error model SIG(F2)^2 = 100.40*I_RAW + 0.00*I_BACK+(0.01679*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 100.40*I_RAW + 0.00*I_BACK+(0.01679*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5322547- 1474730 412 2190620.89 53.58 100.00 1472422- 941208 412 1161144.41 44.44 100.00 941059- 299457 412 560357.16 42.61 100.00 299017- 190519 412 232017.02 34.72 100.00 190474- 157995 412 173092.89 27.29 100.00 157955- 118463 412 133594.74 21.45 100.00 118441- 94023 412 106684.64 18.40 100.00 93993- 5416 412 53703.58 13.60 100.00 5393- 3231 412 4097.06 4.60 97.57 3231- 552 414 2481.30 3.56 67.39 ------------------------------------------------------------------------------------ 5322547- 552 4122 461556.52 26.41 96.48 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 834656.90 41.86 100.00 1.41- 1.12 412 724258.69 32.94 100.00 1.12- 0.96 412 604010.10 31.43 99.03 0.96- 0.88 412 433057.93 26.59 98.54 0.88- 0.81 412 580873.27 31.21 98.54 0.81- 0.74 412 298024.23 20.83 96.84 0.74- 0.71 412 254404.45 20.37 95.39 0.71- 0.65 412 441614.69 25.00 98.06 0.65- 0.62 412 231682.43 16.71 86.65 0.62- 0.58 414 214183.33 17.24 91.79 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 461556.52 26.41 96.48 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 834656.90 41.86 100.00 4.82- 1.12 824 779457.79 37.40 100.00 4.82- 0.96 1236 720975.23 35.41 99.68 4.82- 0.88 1648 648995.90 33.20 99.39 4.82- 0.81 2060 635371.38 32.81 99.22 4.82- 0.74 2472 579146.85 30.81 98.83 4.82- 0.71 2884 532755.08 29.32 98.34 4.82- 0.65 3296 521362.53 28.78 98.30 4.82- 0.62 3708 489175.85 27.44 97.01 4.82- 0.58 4122 461556.52 26.41 96.48 ------------------------------------------------------------------------------------ 4.82- 0.58 4122 461556.52 26.41 96.48 Scale applied to data: s=0.187880 (maximum obs:5322547.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.024: data 4122 -> merged 109 With outlier rejection... Rint 0.038; Rsigma 0.024: data 4114 -> merged 109 Rejected total: 8, method kkm 5, method Blessing 3 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585927, 4.831674 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.71 10 10 25.10 100.00 251 1.61 - 1.21 10 10 38.40 100.00 384 1.17 - 1.01 10 10 49.40 100.00 494 0.99 - 0.89 10 10 48.40 100.00 484 0.88 - 0.81 10 10 46.50 100.00 465 0.81 - 0.74 10 10 39.80 100.00 398 0.73 - 0.71 10 10 44.50 100.00 445 0.70 - 0.66 10 10 36.00 100.00 360 0.66 - 0.64 10 10 35.60 100.00 356 0.63 - 0.60 10 10 34.20 100.00 342 --------------------------------------------------------------- 8.39 - 0.60 100 100 39.79 100.00 3979 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:52:39 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367294 8.376175 8.362583 90.0795 89.9797 89.9843 4111 Reflections read from file xs1715a.hkl; mean (I/sigma) = 26.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2093 0 2749 2754 4111 N (int>3sigma) = 0 0 0 0 2093 0 2642 2646 3954 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 86.6 87.6 86.5 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.4 26.4 26.3 Lattice type: F chosen Volume: 586.10 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.914 5.914 5.916 119.96 90.03 119.93 Niggli form: a.a = 34.974 b.b = 34.975 c.c = 34.998 b.c = -17.470 a.c = -0.020 a.b = -17.448 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.092 CUBIC F-lattice R(int) = 0.036 [ 3955] Vol = 586.1 Cell: 8.363 8.376 8.367 89.98 89.98 90.08 Volume: 586.10 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.089 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 3673] Vol = 439.6 Cell: 5.914 5.914 14.502 90.01 90.06 119.93 Volume: 439.57 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.089 RHOMBOHEDRAL R-lattice R(int) = 0.035 [ 1185] Vol = 439.6 Trigonal Cell: 5.914 5.914 14.502 90.01 90.06 119.93 Volume: 439.57 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.150 TETRAGONAL I-lattice R(int) = 0.035 [ 3706] Vol = 293.0 Cell: 5.921 5.919 8.363 89.93 90.04 90.06 Volume: 293.05 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.110 TETRAGONAL I-lattice R(int) = 0.035 [ 3706] Vol = 293.0 Cell: 5.921 5.919 8.363 89.93 90.04 90.06 Volume: 293.05 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.050 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3653] Vol = 293.0 Cell: 5.921 8.363 5.919 89.93 89.94 89.96 Volume: 293.05 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.036 MONOCLINIC I-lattice R(int) = 0.034 [ 3309] Vol = 293.0 Cell: 8.363 5.921 5.919 90.06 90.07 89.96 Volume: 293.05 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.044 MONOCLINIC I-lattice R(int) = 0.032 [ 3304] Vol = 293.0 Cell: 5.916 5.914 8.376 89.93 90.05 89.97 Volume: 293.05 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.106 MONOCLINIC C-lattice R(int) = 0.032 [ 3326] Vol = 293.0 Cell: 8.363 8.376 5.914 89.93 134.97 90.08 Volume: 293.05 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.030 [ 2653] Vol = 146.5 Cell: 5.914 5.914 5.916 119.96 90.03 119.93 Volume: 146.52 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2093 0 2732 2754 4111 N (int>3sigma) = 0 0 0 0 2093 0 2632 2646 3954 Mean intensity = 0.0 0.0 0.0 0.0 33.3 0.0 89.0 87.6 86.5 Mean int/sigma = 0.0 0.0 0.0 0.0 26.4 0.0 26.5 26.4 26.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.188 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 328 918 N I>3s 36 36 293 918 0.7 0.7 0.7 39.1 7.7 7.7 5.1 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 3647 Fd-3m 1 1 227 C N N N N 37 2284 0.036 3686 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362583 8.376175 8.367294 89.9843 89.9797 90.0795 ZERR 3.00 0.000511 0.000529 0.000413 0.0047 0.0046 0.0050 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5069350- 862975 915 912 27 33.8 1595641.02 47.96 0.036 0.048 851843- 146410 1222 1219 27 45.1 268875.04 34.02 0.041 0.050 138050- 49598 1013 1012 27 37.5 106641.15 18.57 0.056 0.073 20595- 1811 972 971 28 34.7 4424.53 4.68 0.161 0.202 ------------------------------------------------------------------------------------------- 5069350- 1811 4122 4114 109 37.7 460670.96 26.38 0.038 0.050 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1042 1038 27 38.4 736480.69 37.14 0.034 0.048 0.020 1.01-0.78 1290 1290 28 46.1 435812.30 25.27 0.035 0.047 0.024 0.76-0.65 1095 1093 28 39.0 355072.06 22.08 0.043 0.052 0.028 0.65-0.59 695 693 26 26.7 260377.71 19.14 0.056 0.059 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 4122 4114 109 37.7 460670.96 26.38 0.038 0.050 0.024 inf-0.60 3983 3977 99 40.2 470763.31 26.75 0.038 0.050 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1038 27 27 100.0 38.4 736480.69 258.09 0.034 0.005 1.01-0.78 1290 28 28 100.0 46.1 435812.30 181.89 0.035 0.004 0.76-0.65 1093 28 28 100.0 39.0 355072.06 147.44 0.043 0.005 0.65-0.59 693 27 26 96.3 26.7 260377.71 115.36 0.056 0.009 -------------------------------------------------------------------------------------------- inf-0.59 4114 110 109 99.1 37.7 460670.96 180.76 0.038 0.005 inf-0.60 3977 99 99 100.0 40.2 470763.31 184.55 0.038 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 14:57:04 2018) ID: 2932; threads 39; handles 876; mem 516676.00 (1237728.00)kB; time: 1w 6d 0h 2m 34s MEMORY INFO: Memory PF:0.0, Ph:173.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:504.6,peak PF: 708.5, WS: 269.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:173.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.4,peak PF: 708.5, WS: 271.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 14:57:04 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) 8.37051 ( 0.00041 ) 8.37682 ( 0.00053 ) 8.35710 ( 0.00051 ) 90.12473 ( 0.00500 ) 89.98579 ( 0.00454 ) 90.00567 ( 0.00465 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 14:57:04 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007186 -0.000002 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007171 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(4) 90.006(5) V = 585.98(6) unit cell: 8.36870(14) 8.36870(14) 8.36870(14) 90.0 90.0 90.0 V = 586.104(18) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) OTKP changes: 94 1 1 1 UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) 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 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.307) HKL list info: 707 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 457 obs out of 487 (total:487,skipped:0) (93.84%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 1 of 419 peaks identified as outliers and rejected 418 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 418 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 418 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 42 | 1.093 ( 0.273) | 1.325 ( 0.679) | 1.498 ( 1.008) | 1.42- 1.17 | 42 | 1.077 ( 0.066) | 1.144 ( 0.405) | 1.094 ( 0.487) | 1.17- 0.99 | 42 | 1.098 ( 0.065) | 1.070 ( 0.105) | 1.114 ( 0.480) | 0.99- 0.92 | 42 | 1.140 ( 0.048) | 1.099 ( 0.110) | 1.080 ( 0.426) | 0.92- 0.82 | 42 | 1.171 ( 0.047) | 1.098 ( 0.111) | 1.244 ( 0.490) | 0.82- 0.76 | 42 | 1.178 ( 0.059) | 1.079 ( 0.121) | 1.263 ( 0.485) | 0.76- 0.71 | 42 | 1.207 ( 0.058) | 1.096 ( 0.157) | 1.313 ( 0.450) | 0.71- 0.67 | 42 | 1.212 ( 0.066) | 1.118 ( 0.133) | 1.335 ( 0.459) | 0.67- 0.63 | 42 | 1.213 ( 0.079) | 1.199 ( 0.128) | 1.310 ( 0.450) | 0.63- 0.59 | 40 | 1.251 ( 0.107) | 1.125 ( 0.120) | 1.547 ( 0.592) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 418 | 1.164 ( 0.122) | 1.135 ( 0.284) | 1.279 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 415 obs out of 418 (total:418,skipped:0) (99.28%) UB - matrix: -0.007354 0.076558 -0.034855 ( 0.000014 0.000017 0.000013 ) -0.083297 -0.011621 -0.008117 ( 0.000012 0.000014 0.000011 ) -0.011999 0.033378 0.076669 ( 0.000014 0.000017 0.000013 ) M - matrix: 0.007136 0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) 0.000004 0.007110 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000015 0.007159 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3964(12) 8.4117(16) 8.3831(14) 89.879(14) 90.100(12) 90.036(13) V = 592.08(17) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 703 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 3 of 420 peaks identified as outliers and rejected 417 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 417 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 417 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 42 | 1.065 ( 0.164) | 1.299 ( 0.681) | 1.465 ( 0.960) | 1.41- 1.17 | 42 | 1.085 ( 0.067) | 1.159 ( 0.376) | 1.063 ( 0.455) | 1.17- 0.98 | 42 | 1.104 ( 0.068) | 1.081 ( 0.108) | 1.141 ( 0.463) | 0.98- 0.92 | 42 | 1.145 ( 0.044) | 1.099 ( 0.103) | 1.097 ( 0.417) | 0.92- 0.82 | 42 | 1.172 ( 0.053) | 1.097 ( 0.119) | 1.207 ( 0.493) | 0.82- 0.76 | 42 | 1.182 ( 0.066) | 1.088 ( 0.124) | 1.323 ( 0.462) | 0.76- 0.71 | 42 | 1.209 ( 0.056) | 1.100 ( 0.155) | 1.304 ( 0.443) | 0.71- 0.67 | 42 | 1.214 ( 0.069) | 1.131 ( 0.134) | 1.371 ( 0.474) | 0.67- 0.62 | 42 | 1.225 ( 0.076) | 1.206 ( 0.140) | 1.310 ( 0.480) | 0.62- 0.59 | 39 | 1.253 ( 0.105) | 1.137 ( 0.127) | 1.584 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 417 | 1.165 ( 0.103) | 1.140 ( 0.279) | 1.284 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb PROFFITPEAK info: 253 peaks in the peak location table UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) UB - matrix: -0.007501 0.076964 -0.034973 ( 0.000055 0.000076 0.000166 ) -0.083562 -0.011723 -0.008040 ( 0.000029 0.000039 0.000087 ) -0.012051 0.033479 0.077010 ( 0.000048 0.000065 0.000144 ) M - matrix: 0.007184 -0.000001 0.000006 ( 0.000005 0.000006 0.000009 ) -0.000001 0.007182 -0.000019 ( 0.000006 0.000012 0.000015 ) 0.000006 -0.000019 0.007218 ( 0.000009 0.000015 0.000025 ) unit cell: 8.368(3) 8.370(10) 8.349(13) 89.85(12) 90.05(6) 89.99(6) V = 585(1) UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) UB - matrix: -0.007501 0.076964 -0.034973 ( 0.000055 0.000076 0.000166 ) -0.083562 -0.011723 -0.008040 ( 0.000029 0.000039 0.000087 ) -0.012051 0.033479 0.077010 ( 0.000048 0.000065 0.000144 ) M - matrix: 0.007184 -0.000001 0.000006 ( 0.000005 0.000006 0.000009 ) -0.000001 0.007182 -0.000019 ( 0.000006 0.000012 0.000015 ) 0.000006 -0.000019 0.007218 ( 0.000009 0.000015 0.000025 ) unit cell: 8.368(3) 8.370(10) 8.349(13) 89.85(12) 90.05(6) 89.99(6) V = 585(1) OTKP changes: 25 1 1 1 No constraint UB - matrix: -0.007430 0.076874 -0.034841 ( 0.000054 0.000074 0.000162 ) -0.083431 -0.011643 -0.008149 ( 0.000028 0.000039 0.000086 ) -0.012060 0.033398 0.076828 ( 0.000052 0.000072 0.000157 ) M - matrix: 0.007161 -0.000003 0.000012 ( 0.000005 0.000006 0.000009 ) -0.000003 0.007161 -0.000018 ( 0.000006 0.000012 0.000015 ) 0.000012 -0.000018 0.007183 ( 0.000009 0.000015 0.000027 ) Constraint UB - matrix: -0.007430 0.076874 -0.034841 ( 0.000054 0.000074 0.000162 ) -0.083431 -0.011643 -0.008149 ( 0.000028 0.000039 0.000086 ) -0.012060 0.033398 0.076828 ( 0.000052 0.000072 0.000157 ) M - matrix: 0.007159 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007159 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007159 ( 0.000000 0.000000 0.000002 ) UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) unit cell: 8.382(3) 8.382(10) 8.369(14) 89.86(12) 90.10(7) 89.98(6) V = 588(1) unit cell: 8.3777(12) 8.3777(12) 8.3777(12) 90.0 90.0 90.0 V = 587.99(14) UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) UB - matrix: -0.007430 0.076874 -0.034841 ( 0.000054 0.000074 0.000162 ) -0.083431 -0.011643 -0.008149 ( 0.000028 0.000039 0.000086 ) -0.012060 0.033398 0.076828 ( 0.000052 0.000072 0.000157 ) M - matrix: 0.007161 -0.000003 0.000012 ( 0.000005 0.000006 0.000009 ) -0.000003 0.007161 -0.000018 ( 0.000006 0.000012 0.000015 ) 0.000012 -0.000018 0.007183 ( 0.000009 0.000015 0.000027 ) unit cell: 8.382(3) 8.382(10) 8.369(14) 89.86(12) 90.10(7) 89.98(6) V = 588(1) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 126 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Run 8 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=53.094) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007430 0.076874 -0.034841 ( 0.000054 0.000074 0.000162 ) -0.083431 -0.011643 -0.008149 ( 0.000028 0.000039 0.000086 ) -0.012060 0.033398 0.076828 ( 0.000052 0.000072 0.000157 ) M - matrix: 0.007161 -0.000003 0.000012 ( 0.000005 0.000006 0.000009 ) -0.000003 0.007161 -0.000018 ( 0.000006 0.000012 0.000015 ) 0.000012 -0.000018 0.007183 ( 0.000009 0.000015 0.000027 ) Constraint UB - matrix: -0.007430 0.076874 -0.034841 ( 0.000054 0.000074 0.000162 ) -0.083431 -0.011643 -0.008149 ( 0.000028 0.000039 0.000086 ) -0.012060 0.033398 0.076828 ( 0.000052 0.000072 0.000157 ) M - matrix: 0.007159 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007159 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007159 ( 0.000000 0.000000 0.000002 ) UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) unit cell: 8.382(3) 8.382(10) 8.369(14) 89.86(12) 90.10(7) 89.98(6) V = 588(1) unit cell: 8.3777(12) 8.3777(12) 8.3777(12) 90.0 90.0 90.0 V = 587.99(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 119 obs out of 126 (total:126,skipped:0) (94.44%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb 2 of 100 peaks identified as outliers and rejected 98 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 98 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 98 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 10 | 0.974 ( 0.091) | 1.088 ( 0.176) | 1.154 ( 0.449) | 1.41- 1.12 | 10 | 1.033 ( 0.091) | 1.172 ( 0.403) | 1.126 ( 0.496) | 1.12- 0.98 | 10 | 1.115 ( 0.065) | 1.083 ( 0.079) | 1.110 ( 0.522) | 0.97- 0.88 | 10 | 1.132 ( 0.077) | 1.107 ( 0.090) | 1.109 ( 0.480) | 0.85- 0.81 | 10 | 1.159 ( 0.055) | 1.113 ( 0.089) | 1.220 ( 0.393) | 0.81- 0.74 | 10 | 1.175 ( 0.073) | 1.094 ( 0.076) | 1.176 ( 0.384) | 0.73- 0.71 | 10 | 1.166 ( 0.057) | 1.138 ( 0.097) | 1.191 ( 0.487) | 0.71- 0.65 | 10 | 1.207 ( 0.074) | 1.079 ( 0.095) | 1.239 ( 0.466) | 0.64- 0.62 | 10 | 1.215 ( 0.092) | 1.124 ( 0.123) | 1.341 ( 0.554) | 0.62- 0.59 | 8 | 1.291 ( 0.106) | 1.086 ( 0.195) | 1.487 ( 0.675) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 98 | 1.144 ( 0.116) | 1.109 ( 0.173) | 1.210 ( 0.504) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) UB - matrix: -0.007463 0.076870 -0.034665 ( 0.000020 0.000027 0.000062 ) -0.083528 -0.011781 -0.007913 ( 0.000023 0.000031 0.000071 ) -0.012131 0.033338 0.076993 ( 0.000025 0.000034 0.000076 ) M - matrix: 0.007180 0.000006 -0.000014 ( 0.000004 0.000003 0.000006 ) 0.000006 0.007159 -0.000005 ( 0.000003 0.000005 0.000006 ) -0.000014 -0.000005 0.007192 ( 0.000006 0.000006 0.000013 ) unit cell: 8.371(3) 8.383(4) 8.364(6) 89.96(5) 89.89(5) 90.05(3) V = 586.9(6) OTKP changes: 98 1 1 1 No constraint UB - matrix: -0.007451 0.077009 -0.034984 ( 0.000019 0.000026 0.000059 ) -0.083614 -0.011754 -0.008056 ( 0.000016 0.000022 0.000049 ) -0.012070 0.033685 0.076897 ( 0.000019 0.000025 0.000057 ) M - matrix: 0.007193 0.000002 0.000006 ( 0.000003 0.000002 0.000004 ) 0.000002 0.007203 -0.000009 ( 0.000002 0.000004 0.000005 ) 0.000006 -0.000009 0.007202 ( 0.000004 0.000005 0.000010 ) Constraint UB - matrix: -0.007451 0.077009 -0.034984 ( 0.000019 0.000026 0.000059 ) -0.083614 -0.011754 -0.008056 ( 0.000016 0.000022 0.000049 ) -0.012070 0.033685 0.076897 ( 0.000019 0.000025 0.000057 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 8.3635(18) 8.357(4) 8.358(5) 89.93(4) 90.05(3) 90.02(3) V = 584.2(4) unit cell: 8.3596(6) 8.3596(6) 8.3596(6) 90.0 90.0 90.0 V = 584.20(7) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.904) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb 1 of 99 peaks identified as outliers and rejected 98 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 98 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 98 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.60 | 10 | 1.010 ( 0.160) | 1.331 ( 0.756) | 1.475 ( 0.963) | 1.41- 1.17 | 10 | 1.019 ( 0.106) | 1.120 ( 0.286) | 1.162 ( 0.418) | 1.12- 0.98 | 10 | 1.121 ( 0.068) | 1.087 ( 0.081) | 1.119 ( 0.515) | 0.98- 0.88 | 10 | 1.119 ( 0.071) | 1.112 ( 0.090) | 1.079 ( 0.445) | 0.88- 0.81 | 10 | 1.172 ( 0.064) | 1.112 ( 0.090) | 1.090 ( 0.351) | 0.81- 0.74 | 10 | 1.175 ( 0.076) | 1.104 ( 0.076) | 1.270 ( 0.388) | 0.73- 0.71 | 10 | 1.178 ( 0.058) | 1.104 ( 0.084) | 1.230 ( 0.462) | 0.71- 0.65 | 10 | 1.203 ( 0.081) | 1.112 ( 0.113) | 1.212 ( 0.493) | 0.64- 0.62 | 10 | 1.230 ( 0.112) | 1.115 ( 0.115) | 1.368 ( 0.578) | 0.62- 0.59 | 8 | 1.284 ( 0.095) | 1.098 ( 0.196) | 1.463 ( 0.654) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 98 | 1.148 ( 0.124) | 1.130 ( 0.284) | 1.242 ( 0.567) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 321 | 1.144 ( 0.112) | 1.241 ( 0.407) | 1.293 ( 0.630) | 13.0-18.8 | 321 | 1.133 ( 0.078) | 1.182 ( 0.290) | 1.261 ( 0.580) | 18.8-23.0 | 321 | 1.144 ( 0.090) | 1.190 ( 0.289) | 1.278 ( 0.671) | 23.0-27.2 | 321 | 1.133 ( 0.097) | 1.165 ( 0.289) | 1.229 ( 0.579) | 27.2-30.4 | 321 | 1.136 ( 0.098) | 1.150 ( 0.260) | 1.203 ( 0.452) | 30.4-33.6 | 321 | 1.145 ( 0.101) | 1.134 ( 0.210) | 1.193 ( 0.440) | 33.6-37.0 | 321 | 1.146 ( 0.098) | 1.117 ( 0.188) | 1.181 ( 0.441) | 37.0-39.8 | 321 | 1.152 ( 0.116) | 1.094 ( 0.200) | 1.250 ( 0.527) | 39.8-42.8 | 321 | 1.165 ( 0.113) | 1.101 ( 0.247) | 1.214 ( 0.527) | 42.8-50.5 | 320 | 1.213 ( 0.149) | 1.119 ( 0.253) | 1.232 ( 0.498) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.5 | 3209 | 1.151 ( 0.109) | 1.149 ( 0.274) | 1.233 ( 0.541) | Fitted profile normalization line parameters e1 dimension: a=0.0021 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0019 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464571 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 14:57:37 2018 PROFFITMAIN - Started at Wed Mar 28 14:57:37 2018 OTKP changes: 3194 2 4 7 OTKP changes: 3194 2 4 7 OTKP changes: 3194 2 4 7 No constraint UB - matrix: -0.007486 0.076863 -0.034836 ( 0.000006 0.000005 0.000006 ) -0.083584 -0.011770 -0.008061 ( 0.000004 0.000004 0.000004 ) -0.012142 0.033652 0.076994 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007190 -0.000000 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007179 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000008 0.007207 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007486 0.076863 -0.034836 ( 0.000006 0.000005 0.000006 ) -0.083584 -0.011770 -0.008061 ( 0.000004 0.000004 0.000004 ) -0.012142 0.033652 0.076994 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007190 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007190 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007190 ( 0.000000 0.000000 0.000000 ) UB fit with 3200 obs out of 3209 (total:3209,skipped:0) (99.72%) unit cell: 8.3652(4) 8.3715(5) 8.3554(5) 90.066(5) 89.997(4) 89.998(5) V = 585.12(6) unit cell: 8.36400(13) 8.36400(13) 8.36400(13) 90.0 90.0 90.0 V = 585.116(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011768 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012175 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011768 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012175 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.992(10) 89.991(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.947) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011768 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012175 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011768 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012175 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.992(10) 89.991(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084801 -0.000004 -0.000001 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000063 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084801 -0.000004 -0.000001 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000063 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.022(11) 90.000(9) 89.991(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007133 0.076820 -0.034876 ( 0.000016 0.000011 0.000018 ) -0.083536 -0.011636 -0.008042 ( 0.000013 0.000009 0.000014 ) -0.012413 0.033805 0.076702 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007183 0.000004 -0.000032 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007179 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000032 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3691(13) 8.3711(13) 8.3801(15) 90.059(14) 89.748(14) 90.035(13) V = 587.09(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007221 0.076691 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083551 -0.011688 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012355 0.033931 0.076841 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007186 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007221 0.076691 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083551 -0.011688 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012355 0.033931 0.076841 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3676(13) 8.3770(12) 8.3621(15) 90.135(13) 89.822(13) 90.028(12) V = 586.14(16) unit cell: 8.3689(3) 8.3689(3) 8.3689(3) 90.0 90.0 90.0 V = 586.14(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.006) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007221 0.076691 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083551 -0.011688 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012355 0.033931 0.076841 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007186 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007221 0.076691 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083551 -0.011688 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012355 0.033931 0.076841 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3676(13) 8.3770(12) 8.3621(15) 90.135(13) 89.822(13) 90.028(12) V = 586.14(16) unit cell: 8.3689(3) 8.3689(3) 8.3689(3) 90.0 90.0 90.0 V = 586.14(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084642 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000011 0.084727 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084785 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007164 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007179 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084642 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000011 0.084727 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084785 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3800(16) 8.3716(8) 8.3658(10) 90.058(10) 89.872(13) 90.082(11) V = 586.89(14) unit cell: 8.3725(3) 8.3725(3) 8.3725(3) 90.0 90.0 90.0 V = 586.89(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007575 0.076989 -0.034604 ( 0.000014 0.000013 0.000012 ) -0.083449 -0.011890 -0.008148 ( 0.000011 0.000011 0.000009 ) -0.012248 0.033277 0.076950 ( 0.000012 0.000012 0.000010 ) M - matrix: 0.007171 0.000001 -0.000000 ( 0.000002 0.000001 0.000001 ) 0.000001 0.007176 -0.000007 ( 0.000001 0.000002 0.000001 ) -0.000000 -0.000007 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3759(11) 8.3732(13) 8.3678(11) 89.947(11) 89.996(11) 90.011(12) V = 586.86(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3696(11) 8.3735(12) 8.3700(10) 90.000(10) 90.053(10) 90.087(11) V = 586.59(13) unit cell: 8.3710(4) 8.3710(4) 8.3710(4) 90.0 90.0 90.0 V = 586.59(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.006) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3696(11) 8.3735(12) 8.3700(10) 90.000(10) 90.053(10) 90.087(11) V = 586.59(13) unit cell: 8.3710(4) 8.3710(4) 8.3710(4) 90.0 90.0 90.0 V = 586.59(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007570 0.076962 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083528 -0.011954 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076943 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3696(11) 8.3735(12) 8.3700(10) 90.000(10) 90.053(10) 90.087(11) V = 586.59(13) unit cell: 8.3710(4) 8.3710(4) 8.3710(4) 90.0 90.0 90.0 V = 586.59(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) UB - matrix: -0.007468 0.076669 -0.034978 ( 0.000013 0.000016 0.000012 ) -0.083544 -0.011732 -0.008154 ( 0.000011 0.000013 0.000010 ) -0.012244 0.033568 0.076823 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000003 0.000002 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007143 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000002 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3678(11) 8.3927(14) 8.3640(13) 89.942(13) 90.014(11) 89.973(12) V = 587.39(16) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 701 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.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= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) UB - matrix: -0.007509 0.077014 -0.034793 ( 0.000029 0.000039 0.000089 ) -0.083615 -0.011765 -0.008015 ( 0.000021 0.000028 0.000063 ) -0.012102 0.033579 0.077005 ( 0.000020 0.000027 0.000062 ) M - matrix: 0.007194 -0.000001 -0.000001 ( 0.000004 0.000003 0.000006 ) -0.000001 0.007197 0.000001 ( 0.000003 0.000006 0.000008 ) -0.000001 0.000001 0.007205 ( 0.000006 0.000008 0.000011 ) unit cell: 8.362(2) 8.361(5) 8.357(6) 90.00(6) 90.00(4) 89.99(3) V = 584.3(5) OTKP changes: 98 1 1 1 No constraint UB - matrix: -0.007467 0.077024 -0.034920 ( 0.000029 0.000038 0.000088 ) -0.083609 -0.011756 -0.008052 ( 0.000020 0.000027 0.000062 ) -0.012083 0.033679 0.076907 ( 0.000020 0.000026 0.000060 ) M - matrix: 0.007192 0.000001 0.000005 ( 0.000003 0.000003 0.000006 ) 0.000001 0.007205 -0.000005 ( 0.000003 0.000006 0.000008 ) 0.000005 -0.000005 0.007199 ( 0.000006 0.000008 0.000011 ) Constraint UB - matrix: -0.007467 0.077024 -0.034920 ( 0.000029 0.000038 0.000088 ) -0.083609 -0.011756 -0.008052 ( 0.000020 0.000027 0.000062 ) -0.012083 0.033679 0.076907 ( 0.000020 0.000026 0.000060 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 8.364(2) 8.356(5) 8.360(6) 89.96(6) 90.04(4) 90.01(3) V = 584.3(5) unit cell: 8.3599(7) 8.3599(7) 8.3599(7) 90.0 90.0 90.0 V = 584.26(9) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) HKL list info: 272 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.007467 0.077024 -0.034920 ( 0.000029 0.000038 0.000088 ) -0.083609 -0.011756 -0.008052 ( 0.000020 0.000027 0.000062 ) -0.012083 0.033679 0.076907 ( 0.000020 0.000026 0.000060 ) M - matrix: 0.007192 0.000001 0.000005 ( 0.000003 0.000003 0.000006 ) 0.000001 0.007205 -0.000005 ( 0.000003 0.000006 0.000008 ) 0.000005 -0.000005 0.007199 ( 0.000006 0.000008 0.000011 ) Constraint UB - matrix: -0.007467 0.077024 -0.034920 ( 0.000029 0.000038 0.000088 ) -0.083609 -0.011756 -0.008052 ( 0.000020 0.000027 0.000062 ) -0.012083 0.033679 0.076907 ( 0.000020 0.000026 0.000060 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 8.364(2) 8.356(5) 8.360(6) 89.96(6) 90.04(4) 90.01(3) V = 584.3(5) unit cell: 8.3599(7) 8.3599(7) 8.3599(7) 90.0 90.0 90.0 V = 584.26(9) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007474 0.076818 -0.034804 ( 0.000005 0.000005 0.000005 ) -0.083561 -0.011760 -0.008070 ( 0.000004 0.000004 0.000004 ) -0.012176 0.033649 0.076926 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007172 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007474 0.076818 -0.034804 ( 0.000005 0.000005 0.000005 ) -0.083561 -0.011760 -0.008070 ( 0.000004 0.000004 0.000004 ) -0.012176 0.033649 0.076926 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 3202 obs out of 3209 (total:3209,skipped:0) (99.78%) unit cell: 8.3670(4) 8.3757(5) 8.3626(5) 90.079(5) 89.982(4) 89.990(4) V = 586.05(6) unit cell: 8.36844(14) 8.36844(14) 8.36844(14) 90.0 90.0 90.0 V = 586.049(17) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 79 reflections under beam stop or inside a detector rejection region 33 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_8.rrpprof 4254 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 14:57:46 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.947) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.006) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.006) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257029.0082 PROFFIT INFO: background sum: min=524.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11154.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7106245.5000 PROFFIT INFO: sig(Inet): min=187.5304 max=63736.9180 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.29 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 5 113 349 560 885 975 1784 2843 3878 4254 Percent 0.0 0.1 2.7 8.2 13.2 20.8 22.9 41.9 66.8 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4254 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 4254 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7106246- 1512296 425 2287240.95 134.20 100.00 1508872- 946371 425 1209521.36 106.02 100.00 946165- 299057 425 553219.11 92.91 100.00 298645- 203179 425 244032.11 67.18 100.00 203101- 155469 425 175680.80 47.11 100.00 155439- 122699 425 138014.89 36.81 100.00 122640- 91085 425 107762.80 28.97 100.00 91056- 5970 425 50712.30 19.84 100.00 5952- 3403 425 4397.72 4.81 80.24 3390- 531 429 2440.72 3.03 38.23 ------------------------------------------------------------------------------------ 7106246- 531 4254 476855.77 54.04 91.80 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 821482.55 86.46 100.00 1.41- 1.12 425 720422.06 69.88 98.82 1.12- 0.96 425 648593.15 75.44 98.35 0.96- 0.88 425 444320.12 57.65 93.88 0.88- 0.81 425 609013.13 67.98 97.18 0.81- 0.74 425 320023.13 40.16 91.76 0.74- 0.71 425 266621.78 36.54 89.18 0.71- 0.65 425 464064.68 47.99 95.29 0.65- 0.62 425 245758.45 29.20 73.18 0.62- 0.58 429 230576.55 29.33 80.42 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 476855.77 54.04 91.80 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:57:46 2018 Sorting 4254 observations 120 unique observations with > 7.00 F2/sig(F2) 4254 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 24 740 Total number of frames 740 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4254 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 3 111 Total number of frames 111 3418 observations > 7.00 F2/sig(F2) 3418 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 3 111 Total number of frames 111 Removing 'redundancy=1' reflections Average redundancy: 26.9 (Out of 3418 removed 5 = 3413, 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 3413 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 3 111 Total number of frames 111 127 unique data precomputed (should be 127) 127 unique data with 3413 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.9 (Out of 3413 removed 0 = 3413, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3413 observations RMS deviation of equivalent data = 0.22087 Rint = 0.18485 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18425, wR= 0.23416 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13436, wR= 0.17712, Acormin=0.669, Acormax=1.290, Acor_av=0.938 F test: Probability=1.000, F= 1.878 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10765, wR= 0.13826, Acormin=0.538, Acormax=1.353, Acor_av=0.907 F test: Probability=1.000, F= 1.556 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11585, wR= 0.15554, Acormin=0.627, Acormax=1.425, Acor_av=0.953 F test: Probability=0.000, F= 0.862 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08623, wR= 0.11436, Acormin=0.474, Acormax=1.482, Acor_av=0.923 F test: Probability=1.000, F= 1.554 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08181, wR= 0.10891, Acormin=0.458, Acormax=1.377, Acor_av=0.897 F test: Probability=0.998, F= 1.109 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10680, wR= 0.14364, Acormin=0.609, Acormax=1.630, Acor_av=0.919 F test: Probability=0.000, F= 0.586 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08219, wR= 0.10936, Acormin=0.478, Acormax=1.498, Acor_av=0.912 F test: Probability=0.000, F= 0.989 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07823, wR= 0.10372, Acormin=0.462, Acormax=1.426, Acor_av=0.886 F test: Probability=0.993, F= 1.089 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07374, wR= 0.09833, Acormin=0.418, Acormax=1.418, Acor_av=0.810 F test: Probability=0.999, F= 1.121 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08954, wR= 0.11293, Acormin=0.274, Acormax=1.423, Acor_av=0.795 F test: Probability=0.000, F= 0.679 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08232, wR= 0.10494, Acormin=0.359, Acormax=1.451, Acor_av=0.833 F test: Probability=0.000, F= 0.803 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07763, wR= 0.10022, Acormin=0.137, Acormax=0.445, Acor_av=0.258 F test: Probability=0.000, F= 0.901 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07043, wR= 0.09315, Acormin=0.159, Acormax=0.484, Acor_av=0.285 F test: Probability=0.993, F= 1.091 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06526, wR= 0.08825, Acormin=0.158, Acormax=0.509, Acor_av=0.298 F test: Probability=1.000, F= 1.264 Final absorption model (ne=6, no=5): Rint= 0.07374, Acormin=0.418, Acormax=1.418, Acor_av=0.810 Combined refinement in use Rint: 0.18498 There are 111 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: 6, max odd order: 5 (48 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22087 Using Levenberg-Marquardt: 0.00010 New wR= 0.05564 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18485 with corrections 0.04341 Rint for all data: 0.18498 with corrections 0.04363 3 observations identified as outliers and rejected Cycle 2 wR= 0.05539 Using Levenberg-Marquardt: 0.00001 New wR= 0.05120 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18432 with corrections 0.03926 Rint for all data: 0.18498 with corrections 0.03961 2 observations identified as outliers and rejected Cycle 3 wR= 0.05125 Using Levenberg-Marquardt: 0.00000 New wR= 0.05050 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18421 with corrections 0.03841 Rint for all data: 0.18498 with corrections 0.03876 1 observations identified as outliers and rejected Cycle 4 wR= 0.05053 Using Levenberg-Marquardt: 0.00000 New wR= 0.05027 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18399 with corrections 0.03802 Rint for all data: 0.18498 with corrections 0.03839 0 observations identified as outliers and rejected Cycle 5 wR= 0.05027 Using Levenberg-Marquardt: 0.00000 New wR= 0.05019 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18399 with corrections 0.03786 Rint for all data: 0.18498 with corrections 0.03824 0 observations identified as outliers and rejected Final wR= 0.05019 Final frame scales: Min= 0.7806 Max= 1.1932 Final absorption correction factors: Amin= 0.5933 Amax= 1.5958 PROFFIT INFO: Inet (after scale3 abspack): min=542.0707 max=5198501.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=152.5425 max=69199.1641 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4254 reflections read from tmp file 670 reflections are rejected (669 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 5 2 2 3 1 3 3 134 Initial Chi^2= 0.38104 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.86128 Current error model SIG(F2)^2 = 118.94*I_RAW + 0.00*I_BACK+(0.02130*)^2 Cycle 2, Chi^2= 1.00083 Current error model SIG(F2)^2 = 112.33*I_RAW + 0.00*I_BACK+(0.01731*)^2 Cycle 3, Chi^2= 0.99997 Current error model SIG(F2)^2 = 111.30*I_RAW + 0.00*I_BACK+(0.01757*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 111.45*I_RAW + 0.00*I_BACK+(0.01753*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 111.45*I_RAW + 0.00*I_BACK+(0.01753*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5198501- 1452990 425 2178703.27 51.13 100.00 1451628- 929962 425 1147302.36 42.31 100.00 929817- 300315 425 561616.87 40.41 100.00 299702- 188578 425 231415.97 33.11 100.00 188573- 156488 425 171900.99 25.96 100.00 156298- 117362 425 132461.56 20.39 100.00 117196- 93188 425 105440.81 17.41 100.00 93071- 5455 425 53918.51 12.94 100.00 5444- 3200 425 4087.44 4.39 94.12 3199- 542 429 2467.24 3.36 55.71 ------------------------------------------------------------------------------------ 5198501- 542 4254 458502.29 25.12 94.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 835396.25 39.77 100.00 1.41- 1.12 425 710837.80 31.18 99.06 1.12- 0.96 425 611199.22 30.16 97.88 0.96- 0.88 425 427006.91 25.16 96.94 0.88- 0.81 425 575858.72 29.62 98.12 0.81- 0.74 425 299727.28 20.01 96.00 0.74- 0.71 425 250622.17 19.36 93.88 0.71- 0.65 425 431130.96 23.61 96.71 0.65- 0.62 425 232179.02 15.94 82.59 0.62- 0.58 429 213371.70 16.47 88.34 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 458502.29 25.12 94.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 835396.25 39.77 100.00 4.82- 1.12 850 773117.02 35.48 99.53 4.82- 0.96 1275 719144.42 33.70 98.98 4.82- 0.88 1700 646110.04 31.57 98.47 4.82- 0.81 2125 632059.78 31.18 98.40 4.82- 0.74 2550 576671.03 29.32 98.00 4.82- 0.71 2975 530092.62 27.90 97.41 4.82- 0.65 3400 517722.41 27.36 97.32 4.82- 0.62 3825 485995.37 26.09 95.69 4.82- 0.58 4254 458502.29 25.12 94.95 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 458502.29 25.12 94.95 Scale applied to data: s=0.192363 (maximum obs:5198501.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.038; Rsigma 0.025: data 4254 -> merged 156 With outlier rejection... Rint 0.037; Rsigma 0.025: data 4244 -> merged 156 Rejected total: 10, method kkm 7, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585908, 4.831523 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 24.93 100.00 349 1.41 - 1.12 14 14 35.21 100.00 493 1.12 - 0.97 14 14 35.21 100.00 493 0.96 - 0.84 14 14 37.64 100.00 527 0.84 - 0.78 14 14 28.50 100.00 399 0.78 - 0.73 14 14 29.93 100.00 419 0.73 - 0.69 14 14 28.36 100.00 397 0.69 - 0.66 14 14 24.07 100.00 337 0.65 - 0.63 14 14 26.29 100.00 368 0.63 - 0.60 14 14 23.21 100.00 325 --------------------------------------------------------------- 8.36 - 0.60 140 140 29.34 100.00 4107 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:57:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366984 8.375708 8.362649 90.0785 89.9823 89.9903 4244 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2158 0 2843 2843 4244 N (int>3sigma) = 0 0 0 0 2158 0 2700 2694 4029 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.4 88.9 88.0 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 25.2 25.2 25.1 Lattice type: F chosen Volume: 586.05 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.914 5.914 5.916 90.03 119.95 119.93 Niggli form: a.a = 34.974 b.b = 34.974 c.c = 34.996 b.c = -0.018 a.c = -17.468 a.b = -17.451 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.037 [ 4088] Vol = 586.0 Cell: 8.367 8.376 8.363 90.08 89.98 89.99 Volume: 586.05 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.098 RHOMBOHEDRAL R-lattice R(int) = 0.042 [ 3806] Vol = 439.5 Cell: 5.920 5.914 14.502 89.99 90.07 120.03 Volume: 439.54 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.098 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1229] Vol = 439.5 Trigonal Cell: 5.920 5.914 14.502 89.99 90.07 120.03 Volume: 439.54 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.036 TETRAGONAL I-lattice R(int) = 0.037 [ 3838] Vol = 293.0 Cell: 5.919 5.920 8.363 89.96 89.93 89.94 Volume: 293.02 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.106 TETRAGONAL I-lattice R(int) = 0.037 [ 3838] Vol = 293.0 Cell: 5.920 5.919 8.363 90.07 90.04 89.94 Volume: 293.02 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.048 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3785] Vol = 293.0 Cell: 5.920 5.919 8.363 89.93 89.96 89.94 Volume: 293.02 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3780] Vol = 293.0 Cell: 5.914 8.367 5.922 89.99 89.91 90.02 Volume: 293.02 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) = 0.036 [ 3440] Vol = 293.0 Cell: 5.919 5.920 8.363 90.04 90.07 89.94 Volume: 293.02 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.075 MONOCLINIC I-lattice R(int) = 0.034 [ 3435] Vol = 293.0 Cell: 5.914 5.922 8.367 90.01 90.02 90.09 Volume: 293.02 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.025 MONOCLINIC I-lattice R(int) = 0.033 [ 3450] Vol = 293.0 Cell: 5.914 8.367 5.922 89.99 90.09 89.98 Volume: 293.02 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.034 [ 3433] Vol = 293.0 Cell: 8.367 5.914 5.922 90.09 90.01 90.02 Volume: 293.02 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.076 MONOCLINIC C-lattice R(int) = 0.034 [ 3436] Vol = 293.0 Cell: 10.250 5.914 5.916 90.03 125.20 89.93 Volume: 293.02 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2782] Vol = 146.5 Cell: 5.914 5.914 5.916 90.03 119.95 119.93 Volume: 146.51 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2158 0 2843 2843 4244 N (int>3sigma) = 0 0 0 0 2158 0 2700 2694 4029 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.4 88.9 88.0 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 25.2 25.2 25.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.188 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 44 44 341 941 N I>3s 34 34 287 941 0.8 0.8 0.7 39.6 7.5 7.5 4.9 28.4 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 0.037 3767 Fd-3m 1 1 227 C N N N N 37 2284 0.038 3806 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366984 8.375708 8.362649 90.0785 89.9823 89.9903 ZERR 3.00 0.000396 0.000521 0.000504 0.0050 0.0044 0.0045 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5099467- 1081551 682 679 26 26.1 1822752.66 48.32 0.033 0.043 1071652- 264466 672 667 26 25.7 640537.58 40.29 0.045 0.059 263585- 129845 977 976 26 37.5 182762.69 27.01 0.039 0.051 124641- 93689 706 706 26 27.2 110350.29 17.88 0.055 0.072 91260- 3718 628 627 26 24.1 29446.57 8.87 0.070 0.097 3707- 1812 589 589 26 22.7 2984.66 3.81 0.206 0.262 ------------------------------------------------------------------------------------------- 5099467- 1812 4254 4244 156 27.2 457443.98 25.09 0.037 0.049 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 799 795 26 30.6 695463.00 34.47 0.036 0.045 0.020 1.12-0.88 952 952 26 36.6 580165.20 28.99 0.031 0.043 0.023 0.85-0.75 789 788 26 30.3 442440.28 24.28 0.035 0.047 0.026 0.74-0.68 701 700 26 26.9 366771.74 21.77 0.042 0.052 0.030 0.67-0.63 678 678 26 26.1 223576.81 17.22 0.055 0.075 0.037 0.62-0.59 335 331 26 12.7 239316.26 16.37 0.054 0.059 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 4254 4244 156 27.2 457443.98 25.09 0.037 0.049 0.025 inf-0.60 4111 4105 139 29.5 467427.61 25.43 0.037 0.049 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 795 26 26 100.0 30.6 695463.00 207.02 0.036 0.005 1.12-0.88 952 26 26 100.0 36.6 580165.20 177.75 0.031 0.004 0.85-0.75 788 26 26 100.0 30.3 442440.28 141.38 0.035 0.005 0.74-0.68 700 26 26 100.0 26.9 366771.74 115.41 0.042 0.006 0.67-0.63 678 26 26 100.0 26.1 223576.81 87.77 0.055 0.007 0.62-0.59 331 27 26 96.3 12.7 239316.26 69.77 0.054 0.015 -------------------------------------------------------------------------------------------- inf-0.59 4244 157 156 99.4 27.2 457443.98 143.40 0.037 0.006 inf-0.60 4105 139 139 100.0 29.5 467427.61 146.61 0.037 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007474 0.076818 -0.034804 ( 0.000005 0.000005 0.000005 ) -0.083561 -0.011760 -0.008070 ( 0.000004 0.000004 0.000004 ) -0.012176 0.033649 0.076926 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007172 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007474 0.076818 -0.034804 ( 0.000005 0.000005 0.000005 ) -0.083561 -0.011760 -0.008070 ( 0.000004 0.000004 0.000004 ) -0.012176 0.033649 0.076926 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3670(4) 8.3757(5) 8.3627(5) 90.078(5) 89.982(4) 89.990(4) V = 586.05(6) unit cell: 8.36846(14) 8.36846(14) 8.36846(14) 90.0 90.0 90.0 V = 586.053(17) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.947) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.006) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.006) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257029.0082 PROFFIT INFO: background sum: min=524.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11154.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7106245.5000 PROFFIT INFO: sig(Inet): min=187.5304 max=63736.9180 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.29 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 10 226 698 1120 1770 1950 3568 5686 7756 8508 Percent 0.0 0.1 2.7 8.2 13.2 20.8 22.9 41.9 66.8 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4254 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 4254 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7106246- 1512296 425 2287240.95 134.20 100.00 1508872- 946371 425 1209521.36 106.02 100.00 946165- 299057 425 553219.11 92.91 100.00 298645- 203179 425 244032.11 67.18 100.00 203101- 155469 425 175680.80 47.11 100.00 155439- 122699 425 138014.89 36.81 100.00 122640- 91085 425 107762.80 28.97 100.00 91056- 5970 425 50712.30 19.84 100.00 5952- 3403 425 4397.72 4.81 80.24 3390- 531 429 2440.72 3.03 38.23 ------------------------------------------------------------------------------------ 7106246- 531 4254 476855.77 54.04 91.80 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 821482.55 86.46 100.00 1.41- 1.12 425 720422.06 69.88 98.82 1.12- 0.96 425 648593.15 75.44 98.35 0.96- 0.88 425 444320.12 57.65 93.88 0.88- 0.81 425 609013.13 67.98 97.18 0.81- 0.74 425 320023.13 40.16 91.76 0.74- 0.71 425 266621.78 36.54 89.18 0.71- 0.65 425 464064.68 47.99 95.29 0.65- 0.62 425 245758.45 29.20 73.18 0.62- 0.58 429 230576.55 29.33 80.42 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 476855.77 54.04 91.80 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 14:57:48 2018 Sorting 4254 observations 86 unique observations with > 7.00 F2/sig(F2) 4254 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 24 740 Total number of frames 740 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4254 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 12 60 6 0 11 72 7 0 10 83 8 0 2 86 Total number of frames 86 3418 observations > 7.00 F2/sig(F2) 3418 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 8 0 2 85 Total number of frames 85 Removing 'redundancy=1' reflections Average redundancy: 37.5 (Out of 3418 removed 4 = 3414, 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): 4/m3bar2/m 3414 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 8 0 2 85 Total number of frames 85 91 unique data precomputed (should be 91) 91 unique data with 3414 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 37.5 (Out of 3414 removed 0 = 3414, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3414 observations RMS deviation of equivalent data = 0.22175 Rint = 0.18544 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18483, wR= 0.23455 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13462, wR= 0.17778, Acormin=0.669, Acormax=1.288, Acor_av=0.938 F test: Probability=1.000, F= 1.882 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10789, wR= 0.13861, Acormin=0.538, Acormax=1.352, Acor_av=0.907 F test: Probability=1.000, F= 1.556 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11723, wR= 0.15734, Acormin=0.630, Acormax=1.415, Acor_av=0.952 F test: Probability=0.000, F= 0.845 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08723, wR= 0.11574, Acormin=0.473, Acormax=1.475, Acor_av=0.922 F test: Probability=1.000, F= 1.526 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08248, wR= 0.11015, Acormin=0.456, Acormax=1.386, Acor_av=0.895 F test: Probability=0.999, F= 1.116 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10823, wR= 0.14551, Acormin=0.605, Acormax=1.638, Acor_av=0.917 F test: Probability=0.000, F= 0.580 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08376, wR= 0.11098, Acormin=0.468, Acormax=1.504, Acor_av=0.910 F test: Probability=0.000, F= 0.968 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07897, wR= 0.10521, Acormin=0.459, Acormax=1.437, Acor_av=0.883 F test: Probability=0.991, F= 1.086 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07430, wR= 0.09938, Acormin=0.414, Acormax=1.421, Acor_av=0.808 F test: Probability=1.000, F= 1.126 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09066, wR= 0.11436, Acormin=0.287, Acormax=1.438, Acor_av=0.793 F test: Probability=0.000, F= 0.672 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08326, wR= 0.10620, Acormin=0.368, Acormax=1.466, Acor_av=0.831 F test: Probability=0.000, F= 0.797 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07798, wR= 0.10084, Acormin=0.136, Acormax=0.441, Acor_av=0.254 F test: Probability=0.000, F= 0.906 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07064, wR= 0.09344, Acormin=0.157, Acormax=0.481, Acor_av=0.281 F test: Probability=0.997, F= 1.101 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06543, wR= 0.08856, Acormin=0.156, Acormax=0.503, Acor_av=0.295 F test: Probability=1.000, F= 1.277 Final absorption model (ne=6, no=5): Rint= 0.07430, Acormin=0.414, Acormax=1.421, Acor_av=0.808 Combined refinement in use Rint: 0.18556 There are 85 active scales (one needs to be fixed) Refinement control: frame scale #35 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 132 pars with 8778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22175 Using Levenberg-Marquardt: 0.00010 New wR= 0.06102 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18544 with corrections 0.04718 Rint for all data: 0.18556 with corrections 0.04740 3 observations identified as outliers and rejected Cycle 2 wR= 0.06081 Using Levenberg-Marquardt: 0.00001 New wR= 0.05424 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18522 with corrections 0.04173 Rint for all data: 0.18556 with corrections 0.04205 4 observations identified as outliers and rejected Cycle 3 wR= 0.05370 Using Levenberg-Marquardt: 0.00000 New wR= 0.05214 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18539 with corrections 0.04000 Rint for all data: 0.18556 with corrections 0.04047 0 observations identified as outliers and rejected Cycle 4 wR= 0.05214 Using Levenberg-Marquardt: 0.00000 New wR= 0.05151 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18539 with corrections 0.03925 Rint for all data: 0.18556 with corrections 0.03971 1 observations identified as outliers and rejected Cycle 5 wR= 0.05148 Using Levenberg-Marquardt: 0.00000 New wR= 0.05109 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18539 with corrections 0.03864 Rint for all data: 0.18556 with corrections 0.03923 0 observations identified as outliers and rejected Final wR= 0.05109 Final frame scales: Min= 0.7979 Max= 1.1897 Final absorption correction factors: Amin= 0.5568 Amax= 1.6063 PROFFIT INFO: Inet (after scale3 abspack): min=548.0727 max=5254116.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=150.6555 max=66534.9063 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4254 reflections read from tmp file 670 reflections are rejected (670 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 4 2 1 3 1 1 2 95 Initial Chi^2= 0.33482 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93699 Current error model SIG(F2)^2 = 111.59*I_RAW + 0.00*I_BACK+(0.01804*)^2 Cycle 2, Chi^2= 0.99995 Current error model SIG(F2)^2 = 101.50*I_RAW + 0.00*I_BACK+(0.01810*)^2 Cycle 3, Chi^2= 1.00001 Current error model SIG(F2)^2 = 101.82*I_RAW + 0.00*I_BACK+(0.01803*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 101.79*I_RAW + 0.00*I_BACK+(0.01804*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 101.79*I_RAW + 0.00*I_BACK+(0.01804*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5254116- 1461767 425 2174783.11 50.41 100.00 1459611- 932010 425 1149623.65 42.47 100.00 931498- 302108 425 561619.56 40.67 100.00 301488- 189413 425 230803.15 33.56 100.00 189182- 156056 425 171783.88 26.70 100.00 156054- 117067 425 132548.17 21.06 100.00 117042- 93099 425 105550.96 18.13 100.00 93002- 5501 425 53845.51 13.49 100.00 5489- 3195 425 4082.67 4.56 97.18 3191- 548 429 2463.67 3.53 66.67 ------------------------------------------------------------------------------------ 5254116- 548 4254 458281.43 25.44 96.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 832608.66 39.62 100.00 1.41- 1.12 425 709570.68 31.27 100.00 1.12- 0.96 425 609690.49 30.37 99.06 0.96- 0.88 425 427366.13 25.52 98.35 0.88- 0.81 425 576293.47 29.98 98.59 0.81- 0.74 425 299468.52 20.43 96.94 0.74- 0.71 425 251216.60 19.87 95.06 0.71- 0.65 425 432638.98 24.07 97.65 0.65- 0.62 425 232386.06 16.36 86.35 0.62- 0.58 429 213874.96 16.96 91.61 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 458281.43 25.44 96.36 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 425 832608.66 39.62 100.00 4.82- 1.12 850 771089.67 35.45 100.00 4.82- 0.96 1275 717289.94 33.75 99.69 4.82- 0.88 1700 644808.99 31.70 99.35 4.82- 0.81 2125 631105.89 31.35 99.20 4.82- 0.74 2550 575832.99 29.53 98.82 4.82- 0.71 2975 529459.22 28.15 98.29 4.82- 0.65 3400 517356.69 27.64 98.21 4.82- 0.62 3825 485693.29 26.39 96.89 4.82- 0.58 4254 458281.43 25.44 96.36 ------------------------------------------------------------------------------------ 4.82- 0.58 4254 458281.43 25.44 96.36 Scale applied to data: s=0.190327 (maximum obs:5254116.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.025: data 4254 -> merged 109 With outlier rejection... Rint 0.039; Rsigma 0.025: data 4245 -> merged 109 Rejected total: 9, method kkm 7, method Blessing 2 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585910, 4.831534 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 26.20 100.00 262 1.61 - 1.21 10 10 39.70 100.00 397 1.17 - 1.01 10 10 50.80 100.00 508 0.99 - 0.89 10 10 49.80 100.00 498 0.88 - 0.81 10 10 48.30 100.00 483 0.81 - 0.74 10 10 40.80 100.00 408 0.73 - 0.71 10 10 46.00 100.00 460 0.70 - 0.66 10 10 36.90 100.00 369 0.66 - 0.64 10 10 37.00 100.00 370 0.63 - 0.60 10 10 35.30 100.00 353 --------------------------------------------------------------- 8.36 - 0.60 100 100 41.08 100.00 4108 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 14:57:47 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366984 8.375708 8.362649 90.0785 89.9823 89.9903 4244 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2158 0 2843 2843 4244 N (int>3sigma) = 0 0 0 0 2158 0 2700 2694 4029 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.4 88.9 88.0 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 25.2 25.2 25.1 Lattice type: F chosen Volume: 586.05 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.914 5.914 5.916 90.03 119.95 119.93 Niggli form: a.a = 34.974 b.b = 34.974 c.c = 34.996 b.c = -0.018 a.c = -17.468 a.b = -17.451 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.110 CUBIC F-lattice R(int) = 0.037 [ 4088] Vol = 586.0 Cell: 8.367 8.376 8.363 90.08 89.98 89.99 Volume: 586.05 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.098 RHOMBOHEDRAL R-lattice R(int) = 0.042 [ 3806] Vol = 439.5 Cell: 5.920 5.914 14.502 89.99 90.07 120.03 Volume: 439.54 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.098 RHOMBOHEDRAL R-lattice R(int) = 0.036 [ 1229] Vol = 439.5 Trigonal Cell: 5.920 5.914 14.502 89.99 90.07 120.03 Volume: 439.54 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.036 TETRAGONAL I-lattice R(int) = 0.037 [ 3838] Vol = 293.0 Cell: 5.919 5.920 8.363 89.96 89.93 89.94 Volume: 293.02 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.106 TETRAGONAL I-lattice R(int) = 0.037 [ 3838] Vol = 293.0 Cell: 5.920 5.919 8.363 90.07 90.04 89.94 Volume: 293.02 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.048 ORTHORHOMBIC I-lattice R(int) = 0.037 [ 3785] Vol = 293.0 Cell: 5.920 5.919 8.363 89.93 89.96 89.94 Volume: 293.02 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 3780] Vol = 293.0 Cell: 5.914 8.367 5.922 89.99 89.91 90.02 Volume: 293.02 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) = 0.036 [ 3440] Vol = 293.0 Cell: 5.919 5.920 8.363 90.04 90.07 89.94 Volume: 293.02 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.075 MONOCLINIC I-lattice R(int) = 0.034 [ 3435] Vol = 293.0 Cell: 5.914 5.922 8.367 90.01 90.02 90.09 Volume: 293.02 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.025 MONOCLINIC I-lattice R(int) = 0.033 [ 3450] Vol = 293.0 Cell: 5.914 8.367 5.922 89.99 90.09 89.98 Volume: 293.02 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.034 [ 3433] Vol = 293.0 Cell: 8.367 5.914 5.922 90.09 90.01 90.02 Volume: 293.02 Matrix: 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [10] err= 0.076 MONOCLINIC C-lattice R(int) = 0.034 [ 3436] Vol = 293.0 Cell: 10.250 5.914 5.916 90.03 125.20 89.93 Volume: 293.02 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.031 [ 2782] Vol = 146.5 Cell: 5.914 5.914 5.916 90.03 119.95 119.93 Volume: 146.51 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2158 0 2843 2843 4244 N (int>3sigma) = 0 0 0 0 2158 0 2700 2694 4029 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.4 88.9 88.0 Mean int/sigma = 0.0 0.0 0.0 0.0 25.2 0.0 25.2 25.2 25.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.188 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 44 44 341 941 N I>3s 34 34 287 941 0.8 0.8 0.7 39.6 7.5 7.5 4.9 28.4 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 0.037 3767 Fd-3m 1 1 227 C N N N N 37 2284 0.038 3806 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366984 8.375708 8.362649 90.0785 89.9823 89.9903 ZERR 3.00 0.000396 0.000521 0.000504 0.0050 0.0044 0.0045 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 5058548- 850262 947 945 27 35.0 1581556.11 45.46 0.036 0.048 805088- 144859 1262 1257 27 46.6 266341.52 32.80 0.041 0.051 134358- 49304 1045 1044 27 38.7 105319.20 18.24 0.057 0.075 20308- 1801 1000 999 28 35.7 4382.21 4.63 0.163 0.206 ------------------------------------------------------------------------------------------- 5058548- 1801 4254 4245 109 38.9 457878.18 25.41 0.039 0.050 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1079 1076 27 39.9 732770.80 35.33 0.035 0.048 0.021 1.01-0.78 1327 1327 28 47.4 432759.80 24.37 0.035 0.047 0.025 0.76-0.65 1104 1102 27 40.8 358998.09 21.81 0.043 0.053 0.029 0.65-0.59 744 740 27 27.4 250463.99 18.19 0.056 0.061 0.035 ------------------------------------------------------------------------------------------------------ inf-0.59 4254 4245 109 38.9 457878.18 25.41 0.039 0.050 0.025 inf-0.60 4111 4106 99 41.5 467677.01 25.74 0.038 0.050 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1076 27 27 100.0 39.9 732770.80 250.19 0.035 0.005 1.01-0.78 1327 28 28 100.0 47.4 432759.80 178.48 0.035 0.004 0.76-0.65 1102 27 27 100.0 40.8 358998.09 148.25 0.043 0.006 0.65-0.59 740 28 27 96.4 27.4 250463.99 111.73 0.056 0.010 -------------------------------------------------------------------------------------------- inf-0.59 4245 110 109 99.1 38.9 457878.18 177.17 0.039 0.005 inf-0.60 4106 99 99 100.0 41.5 467677.01 180.83 0.038 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 15:02:26 2018) ID: 2932; threads 39; handles 876; mem 516416.00 (1237728.00)kB; time: 1w 6d 0h 7m 56s MEMORY INFO: Memory PF:0.0, Ph:174.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:504.3,peak PF: 708.5, WS: 269.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:174.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.1,peak PF: 708.5, WS: 270.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 15:02:26 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000005 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) 8.37051 ( 0.00040 ) 8.37682 ( 0.00052 ) 8.35710 ( 0.00050 ) 90.12473 ( 0.00495 ) 89.98579 ( 0.00440 ) 90.00567 ( 0.00451 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 15:02:26 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000005 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007172 0.000010 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000010 0.007194 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(4) 90.006(4) V = 585.98(6) unit cell: 8.36846(14) 8.36846(14) 8.36846(14) 90.0 90.0 90.0 V = 586.053(17) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 452 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.32 | 45 | 0.995 ( 0.157) | 1.251 ( 0.669) | 1.326 ( 0.799) | 1.32- 1.12 | 45 | 1.095 ( 0.082) | 1.163 ( 0.164) | 1.167 ( 0.525) | 1.09- 0.97 | 45 | 1.119 ( 0.082) | 1.157 ( 0.136) | 1.183 ( 0.456) | 0.97- 0.88 | 45 | 1.138 ( 0.081) | 1.160 ( 0.121) | 1.171 ( 0.481) | 0.88- 0.81 | 45 | 1.157 ( 0.074) | 1.141 ( 0.133) | 1.245 ( 0.446) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.144 ( 0.121) | 1.203 ( 0.384) | 0.73- 0.70 | 45 | 1.197 ( 0.067) | 1.213 ( 0.155) | 1.196 ( 0.377) | 0.70- 0.66 | 45 | 1.207 ( 0.059) | 1.186 ( 0.162) | 1.180 ( 0.394) | 0.65- 0.62 | 45 | 1.224 ( 0.083) | 1.199 ( 0.162) | 1.208 ( 0.473) | 0.62- 0.59 | 44 | 1.225 ( 0.089) | 1.212 ( 0.231) | 1.341 ( 0.552) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 449 | 1.154 ( 0.111) | 1.183 ( 0.261) | 1.222 ( 0.506) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) OTKP changes: 94 1 1 1 UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) 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 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.307) HKL list info: 707 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 457 obs out of 487 (total:487,skipped:0) (93.84%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 1 of 419 peaks identified as outliers and rejected 418 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 418 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 418 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 42 | 1.093 ( 0.273) | 1.325 ( 0.679) | 1.498 ( 1.008) | 1.42- 1.17 | 42 | 1.077 ( 0.066) | 1.144 ( 0.405) | 1.094 ( 0.487) | 1.17- 0.99 | 42 | 1.098 ( 0.065) | 1.070 ( 0.105) | 1.114 ( 0.480) | 0.99- 0.92 | 42 | 1.140 ( 0.048) | 1.099 ( 0.110) | 1.080 ( 0.426) | 0.92- 0.82 | 42 | 1.171 ( 0.047) | 1.098 ( 0.111) | 1.244 ( 0.490) | 0.82- 0.76 | 42 | 1.178 ( 0.059) | 1.079 ( 0.121) | 1.263 ( 0.485) | 0.76- 0.71 | 42 | 1.207 ( 0.058) | 1.096 ( 0.157) | 1.313 ( 0.450) | 0.71- 0.67 | 42 | 1.212 ( 0.066) | 1.118 ( 0.133) | 1.335 ( 0.459) | 0.67- 0.63 | 42 | 1.213 ( 0.079) | 1.199 ( 0.128) | 1.310 ( 0.450) | 0.63- 0.59 | 40 | 1.251 ( 0.107) | 1.125 ( 0.120) | 1.547 ( 0.592) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 418 | 1.164 ( 0.122) | 1.135 ( 0.284) | 1.279 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 415 obs out of 418 (total:418,skipped:0) (99.28%) UB - matrix: -0.007354 0.076558 -0.034855 ( 0.000014 0.000017 0.000013 ) -0.083297 -0.011621 -0.008117 ( 0.000012 0.000014 0.000011 ) -0.011999 0.033378 0.076669 ( 0.000014 0.000017 0.000013 ) M - matrix: 0.007136 0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) 0.000004 0.007110 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000015 0.007159 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3964(12) 8.4117(16) 8.3831(14) 89.879(14) 90.100(12) 90.036(13) V = 592.08(17) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 703 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 3 of 420 peaks identified as outliers and rejected 417 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 417 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 417 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 42 | 1.065 ( 0.164) | 1.299 ( 0.681) | 1.465 ( 0.960) | 1.41- 1.17 | 42 | 1.085 ( 0.067) | 1.159 ( 0.376) | 1.063 ( 0.455) | 1.17- 0.98 | 42 | 1.104 ( 0.068) | 1.081 ( 0.108) | 1.141 ( 0.463) | 0.98- 0.92 | 42 | 1.145 ( 0.044) | 1.099 ( 0.103) | 1.097 ( 0.417) | 0.92- 0.82 | 42 | 1.172 ( 0.053) | 1.097 ( 0.119) | 1.207 ( 0.493) | 0.82- 0.76 | 42 | 1.182 ( 0.066) | 1.088 ( 0.124) | 1.323 ( 0.462) | 0.76- 0.71 | 42 | 1.209 ( 0.056) | 1.100 ( 0.155) | 1.304 ( 0.443) | 0.71- 0.67 | 42 | 1.214 ( 0.069) | 1.131 ( 0.134) | 1.371 ( 0.474) | 0.67- 0.62 | 42 | 1.225 ( 0.076) | 1.206 ( 0.140) | 1.310 ( 0.480) | 0.62- 0.59 | 39 | 1.253 ( 0.105) | 1.137 ( 0.127) | 1.584 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 417 | 1.165 ( 0.103) | 1.140 ( 0.279) | 1.284 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb PROFFITPEAK info: 476 peaks in the peak location table UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) UB - matrix: -0.007513 0.076972 -0.035007 ( 0.000038 0.000041 0.000067 ) -0.083579 -0.011683 -0.008079 ( 0.000031 0.000033 0.000054 ) -0.012101 0.033560 0.076841 ( 0.000037 0.000039 0.000064 ) M - matrix: 0.007188 -0.000008 0.000008 ( 0.000005 0.000004 0.000006 ) -0.000008 0.007188 -0.000021 ( 0.000004 0.000007 0.000007 ) 0.000008 -0.000021 0.007195 ( 0.000006 0.000007 0.000011 ) unit cell: 8.366(3) 8.366(5) 8.362(6) 89.83(5) 90.07(4) 89.94(4) V = 585.3(6) UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) UB - matrix: -0.007513 0.076972 -0.035007 ( 0.000038 0.000041 0.000067 ) -0.083579 -0.011683 -0.008079 ( 0.000031 0.000033 0.000054 ) -0.012101 0.033560 0.076841 ( 0.000037 0.000039 0.000064 ) M - matrix: 0.007188 -0.000008 0.000008 ( 0.000005 0.000004 0.000006 ) -0.000008 0.007188 -0.000021 ( 0.000004 0.000007 0.000007 ) 0.000008 -0.000021 0.007195 ( 0.000006 0.000007 0.000011 ) unit cell: 8.366(3) 8.366(5) 8.362(6) 89.83(5) 90.07(4) 89.94(4) V = 585.3(6) OTKP changes: 49 1 1 1 No constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007156 -0.000008 0.000010 ( 0.000005 0.000004 0.000005 ) -0.000008 0.007159 -0.000016 ( 0.000004 0.000007 0.000007 ) 0.000010 -0.000016 0.007159 ( 0.000005 0.000007 0.000011 ) Constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007153 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007153 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007153 ( 0.000000 0.000000 0.000001 ) UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) unit cell: 8.385(3) 8.383(5) 8.383(6) 89.87(5) 90.08(4) 89.93(4) V = 589.2(6) unit cell: 8.3836(8) 8.3836(8) 8.3836(8) 90.0 90.0 90.0 V = 589.24(10) UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007156 -0.000008 0.000010 ( 0.000005 0.000004 0.000005 ) -0.000008 0.007159 -0.000016 ( 0.000004 0.000007 0.000007 ) 0.000010 -0.000016 0.007159 ( 0.000005 0.000007 0.000011 ) unit cell: 8.385(3) 8.383(5) 8.383(6) 89.87(5) 90.08(4) 89.93(4) V = 589.2(6) OTKP changes: 49 1 1 1 No constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007156 -0.000008 0.000010 ( 0.000005 0.000004 0.000005 ) -0.000008 0.007159 -0.000016 ( 0.000004 0.000007 0.000007 ) 0.000010 -0.000016 0.007159 ( 0.000005 0.000007 0.000011 ) Constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007153 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007153 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007153 ( 0.000000 0.000000 0.000001 ) UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) unit cell: 8.385(3) 8.383(5) 8.383(6) 89.87(5) 90.08(4) 89.93(4) V = 589.2(6) unit cell: 8.3836(8) 8.3836(8) 8.3836(8) 90.0 90.0 90.0 V = 589.24(10) 242 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Run 8 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=53.129) HKL list info: 433 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007156 -0.000008 0.000010 ( 0.000005 0.000004 0.000005 ) -0.000008 0.007159 -0.000016 ( 0.000004 0.000007 0.000007 ) 0.000010 -0.000016 0.007159 ( 0.000005 0.000007 0.000011 ) Constraint UB - matrix: -0.007406 0.076802 -0.034921 ( 0.000039 0.000041 0.000068 ) -0.083387 -0.011618 -0.008204 ( 0.000030 0.000032 0.000053 ) -0.012166 0.033547 0.076632 ( 0.000036 0.000039 0.000064 ) M - matrix: 0.007153 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007153 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007153 ( 0.000000 0.000000 0.000001 ) UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) unit cell: 8.385(3) 8.383(5) 8.383(6) 89.87(5) 90.08(4) 89.93(4) V = 589.2(6) unit cell: 8.3836(8) 8.3836(8) 8.3836(8) 90.0 90.0 90.0 V = 589.24(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 242 (total:242,skipped:0) (94.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb 2 of 209 peaks identified as outliers and rejected 207 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 207 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 207 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.60 | 21 | 1.040 ( 0.311) | 1.161 ( 0.537) | 1.477 ( 1.507) | 1.60- 1.17 | 21 | 1.034 ( 0.071) | 1.107 ( 0.286) | 1.055 ( 0.449) | 1.17- 0.99 | 21 | 1.097 ( 0.058) | 1.081 ( 0.085) | 1.146 ( 0.544) | 0.99- 0.89 | 21 | 1.116 ( 0.062) | 1.080 ( 0.099) | 1.085 ( 0.522) | 0.89- 0.82 | 21 | 1.133 ( 0.057) | 1.089 ( 0.089) | 1.271 ( 0.456) | 0.82- 0.76 | 21 | 1.163 ( 0.072) | 1.091 ( 0.081) | 1.186 ( 0.358) | 0.75- 0.71 | 21 | 1.148 ( 0.064) | 1.120 ( 0.074) | 1.116 ( 0.406) | 0.71- 0.67 | 21 | 1.158 ( 0.062) | 1.083 ( 0.089) | 1.268 ( 0.427) | 0.67- 0.62 | 21 | 1.184 ( 0.073) | 1.152 ( 0.125) | 1.226 ( 0.496) | 0.62- 0.59 | 18 | 1.264 ( 0.111) | 1.097 ( 0.138) | 1.426 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 207 | 1.132 ( 0.135) | 1.106 ( 0.215) | 1.223 ( 0.670) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 206 obs out of 207 (total:207,skipped:0) (99.52%) UB - matrix: -0.007472 0.076817 -0.034923 ( 0.000015 0.000016 0.000025 ) -0.083516 -0.011696 -0.008130 ( 0.000018 0.000019 0.000032 ) -0.012209 0.033469 0.076773 ( 0.000018 0.000019 0.000031 ) M - matrix: 0.007180 -0.000006 0.000003 ( 0.000003 0.000002 0.000003 ) -0.000006 0.007158 -0.000018 ( 0.000002 0.000003 0.000003 ) 0.000003 -0.000018 0.007180 ( 0.000003 0.000003 0.000005 ) unit cell: 8.3709(19) 8.3838(19) 8.371(3) 89.86(2) 90.02(2) 89.954(19) V = 587.5(3) OTKP changes: 206 1 1 1 No constraint UB - matrix: -0.007500 0.076964 -0.035081 ( 0.000014 0.000015 0.000024 ) -0.083634 -0.011753 -0.008128 ( 0.000015 0.000016 0.000026 ) -0.012147 0.033766 0.076852 ( 0.000014 0.000015 0.000024 ) M - matrix: 0.007198 -0.000004 0.000009 ( 0.000003 0.000002 0.000003 ) -0.000004 0.007202 -0.000009 ( 0.000002 0.000003 0.000002 ) 0.000009 -0.000009 0.007203 ( 0.000003 0.000002 0.000004 ) Constraint UB - matrix: -0.007500 0.076964 -0.035081 ( 0.000014 0.000015 0.000024 ) -0.083634 -0.011753 -0.008128 ( 0.000015 0.000016 0.000026 ) -0.012147 0.033766 0.076852 ( 0.000014 0.000015 0.000024 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 207 (total:207,skipped:0) (99.52%) unit cell: 8.3601(16) 8.3582(18) 8.357(2) 89.925(19) 90.075(19) 89.965(16) V = 584.0(2) unit cell: 8.3586(3) 8.3586(3) 8.3586(3) 90.0 90.0 90.0 V = 583.98(4) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.891) HKL list info: 432 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007500 0.076964 -0.035081 ( 0.000014 0.000015 0.000024 ) -0.083634 -0.011753 -0.008128 ( 0.000015 0.000016 0.000026 ) -0.012147 0.033766 0.076852 ( 0.000014 0.000015 0.000024 ) M - matrix: 0.007198 -0.000004 0.000009 ( 0.000003 0.000002 0.000003 ) -0.000004 0.007202 -0.000009 ( 0.000002 0.000003 0.000002 ) 0.000009 -0.000009 0.007203 ( 0.000003 0.000002 0.000004 ) Constraint UB - matrix: -0.007500 0.076964 -0.035081 ( 0.000014 0.000015 0.000024 ) -0.083634 -0.011753 -0.008128 ( 0.000015 0.000016 0.000026 ) -0.012147 0.033766 0.076852 ( 0.000014 0.000015 0.000024 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 207 (total:207,skipped:0) (99.52%) unit cell: 8.3601(16) 8.3582(18) 8.357(2) 89.925(19) 90.075(19) 89.965(16) V = 584.0(2) unit cell: 8.3586(3) 8.3586(3) 8.3586(3) 90.0 90.0 90.0 V = 583.98(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 206 obs out of 207 (total:207,skipped:0) (99.52%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb 1 of 207 peaks identified as outliers and rejected 206 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 206 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 206 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.61 | 21 | 1.049 ( 0.319) | 1.300 ( 0.721) | 1.456 ( 1.109) | 1.60- 1.17 | 21 | 1.050 ( 0.072) | 1.134 ( 0.295) | 1.116 ( 0.399) | 1.17- 0.98 | 21 | 1.107 ( 0.063) | 1.094 ( 0.088) | 1.166 ( 0.605) | 0.98- 0.89 | 21 | 1.108 ( 0.065) | 1.076 ( 0.100) | 1.085 ( 0.434) | 0.89- 0.82 | 21 | 1.148 ( 0.067) | 1.095 ( 0.091) | 1.258 ( 0.426) | 0.82- 0.75 | 21 | 1.155 ( 0.068) | 1.107 ( 0.085) | 1.131 ( 0.335) | 0.75- 0.71 | 21 | 1.163 ( 0.054) | 1.124 ( 0.065) | 1.205 ( 0.476) | 0.71- 0.66 | 21 | 1.168 ( 0.078) | 1.074 ( 0.079) | 1.224 ( 0.450) | 0.66- 0.62 | 21 | 1.189 ( 0.068) | 1.164 ( 0.127) | 1.217 ( 0.485) | 0.62- 0.59 | 17 | 1.272 ( 0.116) | 1.107 ( 0.142) | 1.471 ( 0.572) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 206 | 1.138 ( 0.137) | 1.128 ( 0.271) | 1.228 ( 0.581) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 332 | 1.142 ( 0.110) | 1.237 ( 0.401) | 1.280 ( 0.623) | 13.0-18.7 | 332 | 1.136 ( 0.101) | 1.186 ( 0.308) | 1.279 ( 0.614) | 18.7-22.9 | 332 | 1.142 ( 0.089) | 1.187 ( 0.285) | 1.274 ( 0.664) | 22.9-27.2 | 332 | 1.132 ( 0.097) | 1.163 ( 0.285) | 1.227 ( 0.579) | 27.2-30.4 | 332 | 1.132 ( 0.100) | 1.148 ( 0.260) | 1.201 ( 0.454) | 30.4-33.6 | 332 | 1.145 ( 0.097) | 1.136 ( 0.214) | 1.194 ( 0.442) | 33.6-37.0 | 332 | 1.145 ( 0.097) | 1.114 ( 0.186) | 1.179 ( 0.437) | 37.0-39.7 | 332 | 1.151 ( 0.115) | 1.093 ( 0.196) | 1.247 ( 0.524) | 39.8-42.7 | 332 | 1.165 ( 0.112) | 1.104 ( 0.246) | 1.212 ( 0.524) | 42.7-50.5 | 328 | 1.213 ( 0.151) | 1.118 ( 0.251) | 1.235 ( 0.500) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.5 | 3316 | 1.150 ( 0.110) | 1.149 ( 0.273) | 1.233 ( 0.543) | Fitted profile normalization line parameters e1 dimension: a=0.0021 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0019 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464571 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 15:03:00 2018 PROFFITMAIN - Started at Wed Mar 28 15:03:00 2018 OTKP changes: 3300 2 4 7 OTKP changes: 3300 2 4 7 OTKP changes: 3300 2 4 7 No constraint UB - matrix: -0.007480 0.076864 -0.034840 ( 0.000005 0.000005 0.000005 ) -0.083580 -0.011767 -0.008063 ( 0.000004 0.000004 0.000004 ) -0.012137 0.033652 0.076988 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007179 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000000 0.000008 0.007206 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007480 0.076864 -0.034840 ( 0.000005 0.000005 0.000005 ) -0.083580 -0.011767 -0.008063 ( 0.000004 0.000004 0.000004 ) -0.012137 0.033652 0.076988 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007190 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007190 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007190 ( 0.000000 0.000000 0.000000 ) UB fit with 3306 obs out of 3316 (total:3316,skipped:0) (99.70%) unit cell: 8.3657(4) 8.3714(5) 8.3557(5) 90.061(5) 90.001(4) 90.001(4) V = 585.17(6) unit cell: 8.36425(13) 8.36425(13) 8.36425(13) 90.0 90.0 90.0 V = 585.170(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 OTKP changes: 449 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000013 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 449 obs out of 449 (total:449,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007134 0.076818 -0.034877 ( 0.000016 0.000011 0.000018 ) -0.083535 -0.011635 -0.008044 ( 0.000013 0.000009 0.000014 ) -0.012412 0.033806 0.076702 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007183 0.000004 -0.000031 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007179 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000031 0.000007 0.007164 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3691(13) 8.3713(13) 8.3801(15) 90.059(14) 89.750(14) 90.035(13) V = 587.11(17) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007220 0.076690 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011687 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076839 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007220 0.076690 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011687 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076839 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3678(13) 8.3771(12) 8.3623(15) 90.135(13) 89.822(13) 90.028(12) V = 586.18(16) unit cell: 8.3690(3) 8.3690(3) 8.3690(3) 90.0 90.0 90.0 V = 586.18(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.008) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007220 0.076690 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011687 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076839 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007185 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007169 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007195 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007220 0.076690 -0.035006 ( 0.000015 0.000010 0.000016 ) -0.083549 -0.011687 -0.008071 ( 0.000013 0.000009 0.000014 ) -0.012354 0.033930 0.076839 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3678(13) 8.3771(12) 8.3623(15) 90.135(13) 89.822(13) 90.028(12) V = 586.18(16) unit cell: 8.3690(3) 8.3690(3) 8.3690(3) 90.0 90.0 90.0 V = 586.18(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084641 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000011 0.084725 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084784 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007164 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007178 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007188 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084641 0.000110 -0.000191 ( 0.000016 0.000011 0.000017 ) 0.000011 0.084725 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084784 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3801(16) 8.3718(8) 8.3660(10) 90.058(10) 89.872(13) 90.082(11) V = 586.93(14) unit cell: 8.3726(3) 8.3726(3) 8.3726(3) 90.0 90.0 90.0 V = 586.93(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007576 0.076987 -0.034605 ( 0.000014 0.000013 0.000012 ) -0.083450 -0.011891 -0.008147 ( 0.000011 0.000011 0.000009 ) -0.012248 0.033277 0.076948 ( 0.000012 0.000012 0.000010 ) M - matrix: 0.007171 0.000002 -0.000000 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007176 -0.000007 ( 0.000001 0.000002 0.000001 ) -0.000000 -0.000007 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3758(11) 8.3733(13) 8.3680(11) 89.947(11) 89.997(11) 90.012(12) V = 586.88(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3698(11) 8.3736(12) 8.3701(10) 90.000(10) 90.053(10) 90.087(11) V = 586.62(13) unit cell: 8.3712(4) 8.3712(4) 8.3712(4) 90.0 90.0 90.0 V = 586.62(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.008) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3698(11) 8.3736(12) 8.3701(10) 90.000(10) 90.053(10) 90.087(11) V = 586.62(13) unit cell: 8.3712(4) 8.3712(4) 8.3712(4) 90.0 90.0 90.0 V = 586.62(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007182 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007175 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007181 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007569 0.076960 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083526 -0.011953 -0.008150 ( 0.000011 0.000010 0.000009 ) -0.012161 0.033308 0.076941 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3698(11) 8.3736(12) 8.3701(10) 90.000(10) 90.053(10) 90.087(11) V = 586.62(13) unit cell: 8.3712(4) 8.3712(4) 8.3712(4) 90.0 90.0 90.0 V = 586.62(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) UB - matrix: -0.007468 0.076669 -0.034978 ( 0.000013 0.000016 0.000012 ) -0.083544 -0.011732 -0.008154 ( 0.000011 0.000013 0.000010 ) -0.012244 0.033568 0.076823 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000003 0.000002 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007143 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000002 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3678(11) 8.3927(14) 8.3640(13) 89.942(13) 90.014(11) 89.973(12) V = 587.39(16) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 701 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.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= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 205 obs out of 206 (total:206,skipped:0) (99.51%) UB - matrix: -0.007584 0.076982 -0.034908 ( 0.000020 0.000021 0.000034 ) -0.083658 -0.011727 -0.008082 ( 0.000017 0.000017 0.000029 ) -0.012197 0.033620 0.076930 ( 0.000016 0.000017 0.000029 ) M - matrix: 0.007205 -0.000013 0.000003 ( 0.000003 0.000002 0.000003 ) -0.000013 0.007194 -0.000006 ( 0.000002 0.000003 0.000003 ) 0.000003 -0.000006 0.007202 ( 0.000003 0.000003 0.000005 ) unit cell: 8.3563(17) 8.363(2) 8.358(3) 89.95(2) 90.02(2) 89.898(19) V = 584.1(3) OTKP changes: 205 1 1 1 No constraint UB - matrix: -0.007494 0.076983 -0.035060 ( 0.000018 0.000019 0.000032 ) -0.083642 -0.011750 -0.008112 ( 0.000016 0.000017 0.000028 ) -0.012141 0.033759 0.076846 ( 0.000014 0.000015 0.000025 ) M - matrix: 0.007200 -0.000004 0.000008 ( 0.000003 0.000002 0.000003 ) -0.000004 0.007204 -0.000009 ( 0.000002 0.000003 0.000003 ) 0.000008 -0.000009 0.007200 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007494 0.076983 -0.035060 ( 0.000018 0.000019 0.000032 ) -0.083642 -0.011750 -0.008112 ( 0.000016 0.000017 0.000028 ) -0.012141 0.033759 0.076846 ( 0.000014 0.000015 0.000025 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 206 (total:206,skipped:0) (99.51%) unit cell: 8.3594(16) 8.357(2) 8.359(2) 89.92(2) 90.07(2) 89.969(18) V = 583.9(2) unit cell: 8.3584(4) 8.3584(4) 8.3584(4) 90.0 90.0 90.0 V = 583.94(5) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.896) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007494 0.076983 -0.035060 ( 0.000018 0.000019 0.000032 ) -0.083642 -0.011750 -0.008112 ( 0.000016 0.000017 0.000028 ) -0.012141 0.033759 0.076846 ( 0.000014 0.000015 0.000025 ) M - matrix: 0.007200 -0.000004 0.000008 ( 0.000003 0.000002 0.000003 ) -0.000004 0.007204 -0.000009 ( 0.000002 0.000003 0.000003 ) 0.000008 -0.000009 0.007200 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007494 0.076983 -0.035060 ( 0.000018 0.000019 0.000032 ) -0.083642 -0.011750 -0.008112 ( 0.000016 0.000017 0.000028 ) -0.012141 0.033759 0.076846 ( 0.000014 0.000015 0.000025 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 206 (total:206,skipped:0) (99.51%) unit cell: 8.3594(16) 8.357(2) 8.359(2) 89.92(2) 90.07(2) 89.969(18) V = 583.9(2) unit cell: 8.3584(4) 8.3584(4) 8.3584(4) 90.0 90.0 90.0 V = 583.94(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 206 (total:206,skipped:0) (99.51%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.084846 -0.000057 0.000080 ( 0.000015 0.000016 0.000026 ) 0.000005 0.084872 -0.000111 ( 0.000016 0.000017 0.000027 ) -0.000006 0.000005 0.084852 ( 0.000017 0.000018 0.000030 ) M - matrix: 0.007199 -0.000004 0.000006 ( 0.000003 0.000002 0.000003 ) -0.000004 0.007203 -0.000009 ( 0.000002 0.000003 0.000003 ) 0.000006 -0.000009 0.007200 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: 0.084846 -0.000057 0.000080 ( 0.000015 0.000016 0.000026 ) 0.000005 0.084872 -0.000111 ( 0.000016 0.000017 0.000027 ) -0.000006 0.000005 0.084852 ( 0.000017 0.000018 0.000030 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 206 (total:206,skipped:0) (99.51%) unit cell: 8.3598(15) 8.3573(16) 8.359(3) 89.93(2) 90.05(2) 89.965(15) V = 584.0(3) unit cell: 8.3588(4) 8.3588(4) 8.3588(4) 90.0 90.0 90.0 V = 584.02(5) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007464 0.076822 -0.034812 ( 0.000005 0.000005 0.000005 ) -0.083564 -0.011761 -0.008068 ( 0.000004 0.000004 0.000004 ) -0.012171 0.033654 0.076922 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000009 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007464 0.076822 -0.034812 ( 0.000005 0.000005 0.000005 ) -0.083564 -0.011761 -0.008068 ( 0.000004 0.000004 0.000004 ) -0.012171 0.033654 0.076922 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 3308 obs out of 3316 (total:3316,skipped:0) (99.76%) unit cell: 8.3668(4) 8.3752(5) 8.3627(5) 90.074(5) 89.982(4) 89.998(4) V = 586.00(6) unit cell: 8.36823(14) 8.36823(14) 8.36823(14) 90.0 90.0 90.0 V = 586.005(17) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 81 reflections under beam stop or inside a detector rejection region 33 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_8.rrpprof 4401 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 15:03:10 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.008) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.008) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.896) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256814.8281 PROFFIT INFO: background sum: min=302.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11117.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7105778.0000 PROFFIT INFO: sig(Inet): min=187.5275 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.28 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 6 119 369 587 916 1011 1858 2951 4019 4401 Percent 0.0 0.1 2.7 8.4 13.3 20.8 23.0 42.2 67.1 91.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4401 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 4401 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7105778- 1489103 440 2263954.25 133.59 100.00 1487697- 924045 440 1189842.12 104.81 100.00 923088- 296873 440 539775.24 92.41 100.00 295924- 200511 440 240412.30 65.96 100.00 200409- 153007 440 172455.65 47.05 100.00 152933- 120393 440 135531.81 36.32 100.00 120319- 88472 440 105504.93 29.07 100.00 88224- 5853 440 48891.58 19.55 100.00 5852- 3342 440 4342.21 4.76 79.09 3331- 531 441 2385.65 3.03 37.19 ------------------------------------------------------------------------------------ 7105778- 531 4401 470203.25 53.64 91.62 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 809472.62 85.48 100.00 1.41- 1.12 440 690030.61 68.97 98.41 1.12- 0.96 440 659850.10 75.45 97.73 0.96- 0.88 440 437285.70 57.22 93.64 0.88- 0.81 440 598558.74 67.31 97.27 0.81- 0.74 440 303501.86 39.23 91.36 0.74- 0.71 440 278244.84 37.40 89.09 0.71- 0.65 440 457745.39 47.53 95.45 0.65- 0.62 440 241119.51 28.86 73.18 0.62- 0.58 441 226776.40 29.04 80.05 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 470203.25 53.64 91.62 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:03:10 2018 Sorting 4401 observations 120 unique observations with > 7.00 F2/sig(F2) 4401 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 48 764 Total number of frames 764 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4401 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 6 114 Total number of frames 114 3534 observations > 7.00 F2/sig(F2) 3534 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 6 114 Total number of frames 114 Removing 'redundancy=1' reflections Average redundancy: 27.8 (Out of 3534 removed 5 = 3529, 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 3529 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 6 114 Total number of frames 114 127 unique data precomputed (should be 127) 127 unique data with 3529 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.8 (Out of 3529 removed 0 = 3529, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3529 observations RMS deviation of equivalent data = 0.24028 Rint = 0.19536 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19527, wR= 0.25696 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14180, wR= 0.19182, Acormin=0.642, Acormax=1.310, Acor_av=0.942 F test: Probability=1.000, F= 1.894 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11553, wR= 0.15264, Acormin=0.518, Acormax=1.364, Acor_av=0.913 F test: Probability=1.000, F= 1.505 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12299, wR= 0.16723, Acormin=0.615, Acormax=1.546, Acor_av=0.956 F test: Probability=0.000, F= 0.881 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09415, wR= 0.12728, Acormin=0.461, Acormax=1.481, Acor_av=0.929 F test: Probability=1.000, F= 1.502 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09023, wR= 0.11918, Acormin=0.449, Acormax=1.562, Acor_av=0.899 F test: Probability=0.992, F= 1.087 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11283, wR= 0.15448, Acormin=0.604, Acormax=1.728, Acor_av=0.927 F test: Probability=0.000, F= 0.639 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08949, wR= 0.11984, Acormin=0.454, Acormax=1.632, Acor_av=0.921 F test: Probability=0.666, F= 1.015 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08552, wR= 0.11320, Acormin=0.452, Acormax=1.630, Acor_av=0.889 F test: Probability=0.999, F= 1.109 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07811, wR= 0.10256, Acormin=0.403, Acormax=1.620, Acor_av=0.807 F test: Probability=1.000, F= 1.195 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09387, wR= 0.11858, Acormin=0.224, Acormax=1.553, Acor_av=0.800 F test: Probability=0.000, F= 0.693 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08904, wR= 0.11345, Acormin=0.283, Acormax=1.581, Acor_av=0.825 F test: Probability=0.000, F= 0.770 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08652, wR= 0.11086, Acormin=0.100, Acormax=0.393, Acor_av=0.206 F test: Probability=0.000, F= 0.813 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07583, wR= 0.09903, Acormin=0.125, Acormax=0.483, Acor_av=0.238 F test: Probability=0.941, F= 1.056 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06884, wR= 0.09194, Acormin=0.129, Acormax=0.511, Acor_av=0.254 F test: Probability=1.000, F= 1.275 Final absorption model (ne=6, no=5): Rint= 0.07811, Acormin=0.403, Acormax=1.620, Acor_av=0.807 Combined refinement in use Rint: 0.19549 There are 114 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: 6, max odd order: 5 (48 parameters) Refinement control: 161 pars with 13041 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24028 Using Levenberg-Marquardt: 0.00010 New wR= 0.05656 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19536 with corrections 0.04402 Rint for all data: 0.19549 with corrections 0.04424 4 observations identified as outliers and rejected Cycle 2 wR= 0.05630 Using Levenberg-Marquardt: 0.00001 New wR= 0.05252 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19488 with corrections 0.04037 Rint for all data: 0.19549 with corrections 0.04073 1 observations identified as outliers and rejected Cycle 3 wR= 0.05257 Using Levenberg-Marquardt: 0.00000 New wR= 0.05174 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19481 with corrections 0.03952 Rint for all data: 0.19549 with corrections 0.03988 1 observations identified as outliers and rejected Cycle 4 wR= 0.05177 Using Levenberg-Marquardt: 0.00000 New wR= 0.05145 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19466 with corrections 0.03915 Rint for all data: 0.19549 with corrections 0.03954 0 observations identified as outliers and rejected Cycle 5 wR= 0.05145 Using Levenberg-Marquardt: 0.00000 New wR= 0.05133 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19466 with corrections 0.03900 Rint for all data: 0.19549 with corrections 0.03939 0 observations identified as outliers and rejected Final wR= 0.05133 Final frame scales: Min= 0.7704 Max= 1.1984 Final absorption correction factors: Amin= 0.3846 Amax= 1.6213 PROFFIT INFO: Inet (after scale3 abspack): min=529.9942 max=5079788.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=150.3773 max=68791.7266 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4401 reflections read from tmp file 698 reflections are rejected (697 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 7 1 1 3 2 3 2 135 Initial Chi^2= 0.38126 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.85646 Current error model SIG(F2)^2 = 114.67*I_RAW + 0.00*I_BACK+(0.02266*)^2 Cycle 2, Chi^2= 1.00164 Current error model SIG(F2)^2 = 111.13*I_RAW + 0.00*I_BACK+(0.01763*)^2 Cycle 3, Chi^2= 0.99997 Current error model SIG(F2)^2 = 109.25*I_RAW + 0.00*I_BACK+(0.01812*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 109.63*I_RAW + 0.00*I_BACK+(0.01803*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 109.56*I_RAW + 0.00*I_BACK+(0.01805*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 109.56*I_RAW + 0.00*I_BACK+(0.01805*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5079789- 1410126 440 2135497.62 49.94 100.00 1409691- 906958 440 1120320.39 41.64 100.00 905420- 293106 440 545378.20 39.77 100.00 291918- 184596 440 226042.72 32.68 100.00 184545- 152451 440 167857.37 25.85 100.00 152234- 114768 440 129341.84 20.23 100.00 114563- 90770 440 102913.63 17.44 100.00 90768- 5311 440 52215.93 12.87 100.00 5304- 3134 440 3991.97 4.38 93.41 3132- 530 441 2411.11 3.36 58.73 ------------------------------------------------------------------------------------ 5079789- 530 4401 448495.69 24.81 95.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 826138.91 38.93 100.00 1.41- 1.12 440 681433.66 30.53 98.86 1.12- 0.96 440 611078.22 29.81 97.95 0.96- 0.88 440 416061.64 24.92 97.27 0.88- 0.81 440 561060.33 29.20 98.41 0.81- 0.74 440 281424.30 19.65 95.68 0.74- 0.71 440 258278.48 19.64 94.09 0.71- 0.65 440 419700.80 23.33 96.82 0.65- 0.62 440 224399.64 15.77 83.41 0.62- 0.58 441 205932.24 16.35 89.57 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 448495.69 24.81 95.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 826138.91 38.93 100.00 4.82- 1.12 880 753786.28 34.73 99.43 4.82- 0.96 1320 706216.93 33.09 98.94 4.82- 0.88 1760 633678.11 31.05 98.52 4.82- 0.81 2200 619154.55 30.68 98.50 4.82- 0.74 2640 562866.18 28.84 98.03 4.82- 0.71 3080 519353.65 27.53 97.47 4.82- 0.65 3520 506897.04 27.00 97.39 4.82- 0.62 3960 475508.44 25.75 95.83 4.82- 0.58 4401 448495.69 24.81 95.21 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 448495.69 24.81 95.21 Scale applied to data: s=0.196858 (maximum obs:5079788.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.026: data 4401 -> merged 156 With outlier rejection... Rint 0.039; Rsigma 0.026: data 4389 -> merged 156 Rejected total: 12, method kkm 9, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585893, 4.831400 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 26.00 100.00 364 1.41 - 1.12 14 14 36.57 100.00 512 1.12 - 0.97 14 14 36.50 100.00 511 0.96 - 0.84 14 14 38.86 100.00 544 0.84 - 0.78 14 14 29.36 100.00 411 0.78 - 0.73 14 14 30.93 100.00 433 0.73 - 0.69 14 14 29.43 100.00 412 0.69 - 0.66 14 14 24.79 100.00 347 0.65 - 0.63 14 14 27.21 100.00 381 0.63 - 0.60 14 14 23.93 100.00 335 --------------------------------------------------------------- 8.36 - 0.60 140 140 30.36 100.00 4250 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:03:11 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366827 8.375171 8.362708 90.0740 89.9824 89.9980 4389 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2234 0 2936 2940 4389 N (int>3sigma) = 0 0 0 0 2234 0 2794 2799 4178 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.6 89.6 88.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.0 0.0 24.9 24.9 24.8 Lattice type: F chosen Volume: 586.00 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.914 5.914 5.916 119.95 90.03 119.94 Niggli form: a.a = 34.974 b.b = 34.974 c.c = 34.995 b.c = -17.467 a.c = -0.017 a.b = -17.455 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.077 CUBIC F-lattice R(int) = 0.039 [ 4233] Vol = 586.0 Cell: 8.363 8.375 8.367 90.00 89.98 90.07 Volume: 586.00 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.074 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 3951] Vol = 439.5 Cell: 5.914 5.914 14.502 90.01 90.06 119.94 Volume: 439.50 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.074 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1277] Vol = 439.5 Trigonal Cell: 5.914 5.914 14.502 90.01 90.06 119.94 Volume: 439.50 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.138 TETRAGONAL I-lattice R(int) = 0.038 [ 3983] Vol = 293.0 Cell: 5.919 5.919 8.363 89.94 90.04 90.06 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.100 TETRAGONAL I-lattice R(int) = 0.038 [ 3983] Vol = 293.0 Cell: 5.919 5.919 8.363 89.94 90.04 90.06 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.038 [ 3930] Vol = 293.0 Cell: 5.919 8.363 5.919 89.94 89.94 89.96 Volume: 293.00 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.035 MONOCLINIC I-lattice R(int) = 0.037 [ 3585] Vol = 293.0 Cell: 8.363 5.919 5.919 90.06 90.06 89.96 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.036 MONOCLINIC I-lattice R(int) = 0.035 [ 3580] Vol = 293.0 Cell: 5.916 5.914 8.375 89.95 90.05 89.97 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.096 MONOCLINIC C-lattice R(int) = 0.035 [ 3600] Vol = 293.0 Cell: 8.363 8.375 5.914 89.95 134.98 90.07 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 2926] Vol = 146.5 Cell: 5.914 5.914 5.916 119.95 90.03 119.94 Volume: 146.50 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2234 0 2918 2940 4389 N (int>3sigma) = 0 0 0 0 2234 0 2783 2799 4178 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 90.9 89.6 88.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.0 0.0 25.0 24.9 24.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.187 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 350 983 N I>3s 36 36 300 983 0.8 0.8 0.7 39.5 7.5 7.5 4.9 28.0 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 0.038 3903 Fd-3m 1 1 227 C N N N N 37 2284 0.039 3942 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362708 8.375171 8.366827 89.9980 89.9824 90.0740 ZERR 3.00 0.000494 0.000514 0.000385 0.0044 0.0043 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4970186- 1051617 706 703 26 27.0 1783957.79 47.27 0.034 0.044 1044547- 258352 695 689 26 26.5 624433.08 39.62 0.046 0.061 256631- 126642 1013 1012 26 38.9 178579.81 26.81 0.040 0.054 121548- 91301 728 728 26 28.0 107745.98 17.86 0.056 0.073 88619- 3656 654 652 26 25.1 28530.55 8.81 0.071 0.095 3621- 1763 605 605 26 23.3 2924.46 3.81 0.206 0.263 ------------------------------------------------------------------------------------------- 4970186- 1763 4401 4389 156 28.1 447457.23 24.77 0.039 0.051 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 832 827 26 31.8 685251.56 33.82 0.037 0.046 0.021 1.12-0.88 984 984 26 37.8 564942.55 28.55 0.032 0.044 0.023 0.85-0.75 817 816 26 31.4 428633.62 23.93 0.036 0.048 0.027 0.74-0.68 723 722 26 27.8 362922.13 21.71 0.044 0.053 0.030 0.67-0.63 700 700 26 26.9 215949.07 17.08 0.057 0.076 0.038 0.62-0.59 345 340 26 13.1 230365.00 16.17 0.054 0.059 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 4401 4389 156 28.1 447457.23 24.77 0.039 0.051 0.026 inf-0.60 4255 4248 139 30.6 457106.98 25.10 0.038 0.050 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 827 26 26 100.0 31.8 685251.56 206.93 0.037 0.005 1.12-0.88 984 26 26 100.0 37.8 564942.55 177.87 0.032 0.004 0.85-0.75 816 26 26 100.0 31.4 428633.62 141.78 0.036 0.005 0.74-0.68 722 26 26 100.0 27.8 362922.13 117.22 0.044 0.006 0.67-0.63 700 26 26 100.0 26.9 215949.07 88.34 0.057 0.007 0.62-0.59 340 27 26 96.3 13.1 230365.00 69.58 0.054 0.014 -------------------------------------------------------------------------------------------- inf-0.59 4389 157 156 99.4 28.1 447457.23 143.99 0.039 0.006 inf-0.60 4248 139 139 100.0 30.6 457106.98 147.17 0.038 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007465 0.076822 -0.034812 ( 0.000005 0.000005 0.000005 ) -0.083564 -0.011761 -0.008068 ( 0.000004 0.000004 0.000004 ) -0.012171 0.033654 0.076922 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000009 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007465 0.076822 -0.034812 ( 0.000005 0.000005 0.000005 ) -0.083564 -0.011761 -0.008068 ( 0.000004 0.000004 0.000004 ) -0.012171 0.033654 0.076922 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3668(4) 8.3752(5) 8.3628(5) 90.074(5) 89.983(4) 89.998(4) V = 586.01(6) unit cell: 8.36825(14) 8.36825(14) 8.36825(14) 90.0 90.0 90.0 V = 586.008(17) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.008) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.008) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.896) PROFFIT INFO: signal sum: min=159.0000 max=22704656.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256814.8281 PROFFIT INFO: background sum: min=302.0000 max=17454.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11117.0000 PROFFIT INFO: num of signal pixels: min=56 max=888 PROFFIT INFO: Inet: min=530.6313 max=7105778.0000 PROFFIT INFO: sig(Inet): min=187.5275 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.28 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 12 238 738 1174 1832 2022 3716 5902 8038 8802 Percent 0.0 0.1 2.7 8.4 13.3 20.8 23.0 42.2 67.1 91.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4401 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 4401 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7105778- 1489103 440 2263954.25 133.59 100.00 1487697- 924045 440 1189842.12 104.81 100.00 923088- 296873 440 539775.24 92.41 100.00 295924- 200511 440 240412.30 65.96 100.00 200409- 153007 440 172455.65 47.05 100.00 152933- 120393 440 135531.81 36.32 100.00 120319- 88472 440 105504.93 29.07 100.00 88224- 5853 440 48891.58 19.55 100.00 5852- 3342 440 4342.21 4.76 79.09 3331- 531 441 2385.65 3.03 37.19 ------------------------------------------------------------------------------------ 7105778- 531 4401 470203.25 53.64 91.62 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 809472.62 85.48 100.00 1.41- 1.12 440 690030.61 68.97 98.41 1.12- 0.96 440 659850.10 75.45 97.73 0.96- 0.88 440 437285.70 57.22 93.64 0.88- 0.81 440 598558.74 67.31 97.27 0.81- 0.74 440 303501.86 39.23 91.36 0.74- 0.71 440 278244.84 37.40 89.09 0.71- 0.65 440 457745.39 47.53 95.45 0.65- 0.62 440 241119.51 28.86 73.18 0.62- 0.58 441 226776.40 29.04 80.05 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 470203.25 53.64 91.62 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:03:12 2018 Sorting 4401 observations 86 unique observations with > 7.00 F2/sig(F2) 4401 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 48 764 Total number of frames 764 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4401 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 12 60 6 0 11 72 7 0 10 83 8 0 5 89 Total number of frames 89 3534 observations > 7.00 F2/sig(F2) 3534 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 8 0 5 88 Total number of frames 88 Removing 'redundancy=1' reflections Average redundancy: 38.8 (Out of 3534 removed 4 = 3530, 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): 4/m3bar2/m 3530 observations in 8 runs Run # start # end # total # 1 0 11 12 2 0 12 25 3 0 10 36 4 0 10 47 5 0 11 59 6 0 11 71 7 0 10 82 8 0 5 88 Total number of frames 88 91 unique data precomputed (should be 91) 91 unique data with 3530 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 38.8 (Out of 3530 removed 0 = 3530, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3530 observations RMS deviation of equivalent data = 0.24105 Rint = 0.19568 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19523, wR= 0.25676 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14183, wR= 0.19251, Acormin=0.643, Acormax=1.308, Acor_av=0.942 F test: Probability=1.000, F= 1.892 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11569, wR= 0.15297, Acormin=0.518, Acormax=1.364, Acor_av=0.913 F test: Probability=1.000, F= 1.502 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12431, wR= 0.16880, Acormin=0.616, Acormax=1.538, Acor_av=0.954 F test: Probability=0.000, F= 0.865 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09504, wR= 0.12835, Acormin=0.460, Acormax=1.482, Acor_av=0.928 F test: Probability=1.000, F= 1.478 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09073, wR= 0.12010, Acormin=0.448, Acormax=1.559, Acor_av=0.897 F test: Probability=0.996, F= 1.095 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11376, wR= 0.15566, Acormin=0.596, Acormax=1.731, Acor_av=0.925 F test: Probability=0.000, F= 0.635 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09047, wR= 0.12076, Acormin=0.447, Acormax=1.639, Acor_av=0.920 F test: Probability=0.545, F= 1.004 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08586, wR= 0.11410, Acormin=0.444, Acormax=1.631, Acor_av=0.888 F test: Probability=0.999, F= 1.112 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07835, wR= 0.10324, Acormin=0.399, Acormax=1.620, Acor_av=0.807 F test: Probability=1.000, F= 1.197 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09458, wR= 0.11948, Acormin=0.235, Acormax=1.558, Acor_av=0.799 F test: Probability=0.000, F= 0.687 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08960, wR= 0.11421, Acormin=0.292, Acormax=1.586, Acor_av=0.825 F test: Probability=0.000, F= 0.765 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08676, wR= 0.11133, Acormin=0.099, Acormax=0.390, Acor_av=0.204 F test: Probability=0.000, F= 0.814 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07617, wR= 0.09933, Acormin=0.124, Acormax=0.480, Acor_av=0.237 F test: Probability=0.933, F= 1.053 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06904, wR= 0.09218, Acormin=0.128, Acormax=0.509, Acor_av=0.252 F test: Probability=1.000, F= 1.276 Final absorption model (ne=6, no=5): Rint= 0.07835, Acormin=0.399, Acormax=1.620, Acor_av=0.807 Combined refinement in use Rint: 0.19581 There are 88 active scales (one needs to be fixed) Refinement control: frame scale #35 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 135 pars with 9180 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24105 Using Levenberg-Marquardt: 0.00010 New wR= 0.06178 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19568 with corrections 0.04811 Rint for all data: 0.19581 with corrections 0.04833 2 observations identified as outliers and rejected Cycle 2 wR= 0.06165 Using Levenberg-Marquardt: 0.00001 New wR= 0.05553 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19557 with corrections 0.04316 Rint for all data: 0.19581 with corrections 0.04341 5 observations identified as outliers and rejected Cycle 3 wR= 0.05507 Using Levenberg-Marquardt: 0.00000 New wR= 0.05344 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19569 with corrections 0.04136 Rint for all data: 0.19581 with corrections 0.04183 2 observations identified as outliers and rejected Cycle 4 wR= 0.05352 Using Levenberg-Marquardt: 0.00000 New wR= 0.05286 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19586 with corrections 0.04066 Rint for all data: 0.19581 with corrections 0.04111 2 observations identified as outliers and rejected Cycle 5 wR= 0.05291 Using Levenberg-Marquardt: 0.00000 New wR= 0.05252 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19589 with corrections 0.04022 Rint for all data: 0.19581 with corrections 0.04068 1 observations identified as outliers and rejected Final wR= 0.05252 Final frame scales: Min= 0.8036 Max= 1.2144 Final absorption correction factors: Amin= 0.3815 Amax= 1.6270 PROFFIT INFO: Inet (after scale3 abspack): min=529.8425 max=5143337.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=147.2401 max=70247.2578 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4401 reflections read from tmp file 719 reflections are rejected (719 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 1 3 2 1 1 2 95 Initial Chi^2= 0.33667 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.91678 Current error model SIG(F2)^2 = 108.51*I_RAW + 0.00*I_BACK+(0.01922*)^2 Cycle 2, Chi^2= 1.00017 Current error model SIG(F2)^2 = 102.50*I_RAW + 0.00*I_BACK+(0.01772*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 102.30*I_RAW + 0.00*I_BACK+(0.01777*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 102.30*I_RAW + 0.00*I_BACK+(0.01777*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5143337- 1413030 440 2130450.48 50.94 100.00 1405948- 911518 440 1123089.42 42.62 100.00 911103- 293342 440 545566.03 40.78 100.00 293158- 185043 440 225430.36 33.52 100.00 184918- 152427 440 167671.17 26.57 100.00 152358- 114412 440 129420.72 20.95 100.00 114406- 90773 440 102957.68 18.01 100.00 90750- 5341 440 52300.34 13.30 100.00 5340- 3129 440 3988.91 4.52 95.00 3128- 530 441 2410.87 3.49 65.76 ------------------------------------------------------------------------------------ 5143337- 530 4401 448227.28 25.47 96.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 822704.58 39.78 100.00 1.41- 1.12 440 680430.79 31.29 99.55 1.12- 0.96 440 609095.60 30.54 98.64 0.96- 0.88 440 416057.54 25.59 97.95 0.88- 0.81 440 561356.98 29.96 98.64 0.81- 0.74 440 281415.69 20.21 96.36 0.74- 0.71 440 258980.58 20.22 94.77 0.71- 0.65 440 421226.30 23.99 97.50 0.65- 0.62 440 224942.99 16.24 86.14 0.62- 0.58 441 206610.86 16.85 91.16 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 448227.28 25.47 96.07 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 440 822704.58 39.78 100.00 4.82- 1.12 880 751567.68 35.53 99.77 4.82- 0.96 1320 704076.99 33.87 99.39 4.82- 0.88 1760 632072.13 31.80 99.03 4.82- 0.81 2200 617929.10 31.43 98.95 4.82- 0.74 2640 561843.53 29.56 98.52 4.82- 0.71 3080 518577.39 28.23 97.99 4.82- 0.65 3520 506408.51 27.70 97.93 4.82- 0.62 3960 475134.56 26.42 96.62 4.82- 0.58 4401 448227.28 25.47 96.07 ------------------------------------------------------------------------------------ 4.82- 0.58 4401 448227.28 25.47 96.07 Scale applied to data: s=0.194426 (maximum obs:5143337.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.041; Rsigma 0.025: data 4401 -> merged 109 With outlier rejection... Rint 0.040; Rsigma 0.025: data 4392 -> merged 109 Rejected total: 9, method kkm 7, method Blessing 2 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585895, 4.831411 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 27.40 100.00 274 1.61 - 1.21 10 10 41.30 100.00 413 1.17 - 1.01 10 10 52.60 100.00 526 0.99 - 0.89 10 10 51.50 100.00 515 0.88 - 0.81 10 10 49.80 100.00 498 0.81 - 0.74 10 10 42.40 100.00 424 0.73 - 0.71 10 10 47.50 100.00 475 0.70 - 0.66 10 10 38.00 100.00 380 0.66 - 0.64 10 10 38.40 100.00 384 0.63 - 0.60 10 10 36.30 100.00 363 --------------------------------------------------------------- 8.36 - 0.60 100 100 42.52 100.00 4252 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:03:11 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.366827 8.375171 8.362708 90.0740 89.9824 89.9980 4389 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2234 0 2936 2940 4389 N (int>3sigma) = 0 0 0 0 2234 0 2794 2799 4178 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.6 89.6 88.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.0 0.0 24.9 24.9 24.8 Lattice type: F chosen Volume: 586.00 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.914 5.914 5.916 119.95 90.03 119.94 Niggli form: a.a = 34.974 b.b = 34.974 c.c = 34.995 b.c = -17.467 a.c = -0.017 a.b = -17.455 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.077 CUBIC F-lattice R(int) = 0.039 [ 4233] Vol = 586.0 Cell: 8.363 8.375 8.367 90.00 89.98 90.07 Volume: 586.00 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.074 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 3951] Vol = 439.5 Cell: 5.914 5.914 14.502 90.01 90.06 119.94 Volume: 439.50 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.074 RHOMBOHEDRAL R-lattice R(int) = 0.037 [ 1277] Vol = 439.5 Trigonal Cell: 5.914 5.914 14.502 90.01 90.06 119.94 Volume: 439.50 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.138 TETRAGONAL I-lattice R(int) = 0.038 [ 3983] Vol = 293.0 Cell: 5.919 5.919 8.363 89.94 90.04 90.06 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.100 TETRAGONAL I-lattice R(int) = 0.038 [ 3983] Vol = 293.0 Cell: 5.919 5.919 8.363 89.94 90.04 90.06 Volume: 293.00 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.038 [ 3930] Vol = 293.0 Cell: 5.919 8.363 5.919 89.94 89.94 89.96 Volume: 293.00 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.035 MONOCLINIC I-lattice R(int) = 0.037 [ 3585] Vol = 293.0 Cell: 8.363 5.919 5.919 90.06 90.06 89.96 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.036 MONOCLINIC I-lattice R(int) = 0.035 [ 3580] Vol = 293.0 Cell: 5.916 5.914 8.375 89.95 90.05 89.97 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.096 MONOCLINIC C-lattice R(int) = 0.035 [ 3600] Vol = 293.0 Cell: 8.363 8.375 5.914 89.95 134.98 90.07 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 2926] Vol = 146.5 Cell: 5.914 5.914 5.916 119.95 90.03 119.94 Volume: 146.50 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2234 0 2918 2940 4389 N (int>3sigma) = 0 0 0 0 2234 0 2783 2799 4178 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 90.9 89.6 88.1 Mean int/sigma = 0.0 0.0 0.0 0.0 25.0 0.0 25.0 24.9 24.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.187 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 350 983 N I>3s 36 36 300 983 0.8 0.8 0.7 39.5 7.5 7.5 4.9 28.0 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 0.038 3903 Fd-3m 1 1 227 C N N N N 37 2284 0.039 3942 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362708 8.375171 8.366827 89.9980 89.9824 90.0740 ZERR 3.00 0.000494 0.000514 0.000385 0.0044 0.0043 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4927322- 829894 980 978 27 36.2 1547850.93 45.80 0.038 0.050 786075- 141876 1308 1303 27 48.3 259342.29 32.74 0.042 0.052 130629- 48084 1079 1078 27 39.9 102795.99 18.12 0.059 0.077 19742- 1758 1034 1033 28 36.9 4289.19 4.59 0.163 0.210 ------------------------------------------------------------------------------------------- 4927322- 1758 4401 4392 109 40.3 447852.01 25.44 0.040 0.052 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1120 1117 27 41.4 718083.55 35.48 0.036 0.049 0.021 1.01-0.78 1337 1337 27 49.5 433740.23 24.95 0.037 0.050 0.025 0.78-0.65 1144 1142 27 42.3 350185.03 21.75 0.045 0.056 0.029 0.65-0.59 800 796 28 28.4 232468.20 17.47 0.058 0.062 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 4401 4392 109 40.3 447852.01 25.44 0.040 0.052 0.025 inf-0.60 4255 4250 99 42.9 457380.69 25.77 0.040 0.052 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1117 27 27 100.0 41.4 718083.55 254.38 0.036 0.005 1.01-0.78 1337 27 27 100.0 49.5 433740.23 185.68 0.037 0.004 0.78-0.65 1142 27 27 100.0 42.3 350185.03 149.82 0.045 0.005 0.65-0.59 796 29 28 96.6 28.4 232468.20 108.63 0.058 0.009 -------------------------------------------------------------------------------------------- inf-0.59 4392 110 109 99.1 40.3 447852.01 179.86 0.040 0.005 inf-0.60 4250 99 99 100.0 42.9 457380.69 183.55 0.040 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 15:07:45 2018) ID: 2932; threads 39; handles 878; mem 517240.00 (1237728.00)kB; time: 1w 6d 0h 13m 15s MEMORY INFO: Memory PF:10.0, Ph:181.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.1,peak PF: 708.5, WS: 269.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:13.0, Ph:181.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.9,peak PF: 708.5, WS: 271.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 15:07:45 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000005 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) 8.37051 ( 0.00039 ) 8.37682 ( 0.00051 ) 8.35710 ( 0.00049 ) 90.12473 ( 0.00487 ) 89.98579 ( 0.00429 ) 90.00567 ( 0.00441 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\plots_red\xs1715a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1715a\xs1715a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1715a\xs1715a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1715a\xs1715a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1715a\xs1715a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1715a\xs1715a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1715a\xs1715a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1715a\xs1715a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 15:07:45 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000005 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000009 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000009 0.007194 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(4) 90.006(4) V = 585.98(6) unit cell: 8.36825(14) 8.36825(14) 8.36825(14) 90.0 90.0 90.0 V = 586.008(17) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.092 ( 0.069) | 1.152 ( 0.108) | 1.302 ( 0.618) | 1.09- 0.96 | 45 | 1.129 ( 0.127) | 1.237 ( 0.340) | 1.202 ( 0.557) | 0.96- 0.85 | 45 | 1.142 ( 0.052) | 1.145 ( 0.122) | 1.270 ( 0.487) | 0.85- 0.81 | 45 | 1.164 ( 0.058) | 1.193 ( 0.131) | 1.146 ( 0.404) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.150 ( 0.148) | 1.275 ( 0.430) | 0.73- 0.70 | 45 | 1.184 ( 0.046) | 1.188 ( 0.146) | 1.276 ( 0.444) | 0.70- 0.66 | 45 | 1.193 ( 0.056) | 1.196 ( 0.163) | 1.224 ( 0.416) | 0.66- 0.62 | 45 | 1.199 ( 0.083) | 1.224 ( 0.171) | 1.249 ( 0.501) | 0.62- 0.59 | 42 | 1.206 ( 0.067) | 1.208 ( 0.199) | 1.346 ( 0.507) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 447 | 1.147 ( 0.103) | 1.195 ( 0.271) | 1.266 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) OTKP changes: 94 1 1 1 UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) 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 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.307) HKL list info: 707 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 457 obs out of 487 (total:487,skipped:0) (93.84%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 1 of 419 peaks identified as outliers and rejected 418 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 418 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 418 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 42 | 1.093 ( 0.273) | 1.325 ( 0.679) | 1.498 ( 1.008) | 1.42- 1.17 | 42 | 1.077 ( 0.066) | 1.144 ( 0.405) | 1.094 ( 0.487) | 1.17- 0.99 | 42 | 1.098 ( 0.065) | 1.070 ( 0.105) | 1.114 ( 0.480) | 0.99- 0.92 | 42 | 1.140 ( 0.048) | 1.099 ( 0.110) | 1.080 ( 0.426) | 0.92- 0.82 | 42 | 1.171 ( 0.047) | 1.098 ( 0.111) | 1.244 ( 0.490) | 0.82- 0.76 | 42 | 1.178 ( 0.059) | 1.079 ( 0.121) | 1.263 ( 0.485) | 0.76- 0.71 | 42 | 1.207 ( 0.058) | 1.096 ( 0.157) | 1.313 ( 0.450) | 0.71- 0.67 | 42 | 1.212 ( 0.066) | 1.118 ( 0.133) | 1.335 ( 0.459) | 0.67- 0.63 | 42 | 1.213 ( 0.079) | 1.199 ( 0.128) | 1.310 ( 0.450) | 0.63- 0.59 | 40 | 1.251 ( 0.107) | 1.125 ( 0.120) | 1.547 ( 0.592) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 418 | 1.164 ( 0.122) | 1.135 ( 0.284) | 1.279 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 415 obs out of 418 (total:418,skipped:0) (99.28%) UB - matrix: -0.007354 0.076558 -0.034855 ( 0.000014 0.000017 0.000013 ) -0.083297 -0.011621 -0.008117 ( 0.000012 0.000014 0.000011 ) -0.011999 0.033378 0.076669 ( 0.000014 0.000017 0.000013 ) M - matrix: 0.007136 0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) 0.000004 0.007110 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000015 0.007159 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3964(12) 8.4117(16) 8.3831(14) 89.879(14) 90.100(12) 90.036(13) V = 592.08(17) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 703 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 3 of 420 peaks identified as outliers and rejected 417 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 417 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 417 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 42 | 1.065 ( 0.164) | 1.299 ( 0.681) | 1.465 ( 0.960) | 1.41- 1.17 | 42 | 1.085 ( 0.067) | 1.159 ( 0.376) | 1.063 ( 0.455) | 1.17- 0.98 | 42 | 1.104 ( 0.068) | 1.081 ( 0.108) | 1.141 ( 0.463) | 0.98- 0.92 | 42 | 1.145 ( 0.044) | 1.099 ( 0.103) | 1.097 ( 0.417) | 0.92- 0.82 | 42 | 1.172 ( 0.053) | 1.097 ( 0.119) | 1.207 ( 0.493) | 0.82- 0.76 | 42 | 1.182 ( 0.066) | 1.088 ( 0.124) | 1.323 ( 0.462) | 0.76- 0.71 | 42 | 1.209 ( 0.056) | 1.100 ( 0.155) | 1.304 ( 0.443) | 0.71- 0.67 | 42 | 1.214 ( 0.069) | 1.131 ( 0.134) | 1.371 ( 0.474) | 0.67- 0.62 | 42 | 1.225 ( 0.076) | 1.206 ( 0.140) | 1.310 ( 0.480) | 0.62- 0.59 | 39 | 1.253 ( 0.105) | 1.137 ( 0.127) | 1.584 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 417 | 1.165 ( 0.103) | 1.140 ( 0.279) | 1.284 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 *** 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\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb PROFFITPEAK info: 703 peaks in the peak location table UB fit with 346 obs out of 365 (total:365,skipped:0) (94.79%) UB - matrix: -0.007523 0.076926 -0.035116 ( 0.000028 0.000029 0.000035 ) -0.083621 -0.011649 -0.008171 ( 0.000031 0.000031 0.000037 ) -0.012207 0.033716 0.076677 ( 0.000030 0.000030 0.000036 ) M - matrix: 0.007198 -0.000016 0.000011 ( 0.000005 0.000004 0.000004 ) -0.000016 0.007190 -0.000021 ( 0.000004 0.000005 0.000004 ) 0.000011 -0.000021 0.007179 ( 0.000004 0.000004 0.000006 ) unit cell: 8.360(3) 8.365(3) 8.371(3) 89.83(3) 90.09(3) 89.87(3) V = 585.4(4) UB fit with 346 obs out of 365 (total:365,skipped:0) (94.79%) UB - matrix: -0.007523 0.076926 -0.035116 ( 0.000028 0.000029 0.000035 ) -0.083621 -0.011649 -0.008171 ( 0.000031 0.000031 0.000037 ) -0.012207 0.033716 0.076677 ( 0.000030 0.000030 0.000036 ) M - matrix: 0.007198 -0.000016 0.000011 ( 0.000005 0.000004 0.000004 ) -0.000016 0.007190 -0.000021 ( 0.000004 0.000005 0.000004 ) 0.000011 -0.000021 0.007179 ( 0.000004 0.000004 0.000006 ) unit cell: 8.360(3) 8.365(3) 8.371(3) 89.83(3) 90.09(3) 89.87(3) V = 585.4(4) 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 346 obs out of 365 (total:365,skipped:0) (94.79%) UB - matrix: -0.007529 0.076929 -0.035142 ( 0.000029 0.000029 0.000035 ) -0.083622 -0.011642 -0.008173 ( 0.000031 0.000031 0.000038 ) -0.012209 0.033717 0.076661 ( 0.000029 0.000030 0.000036 ) M - matrix: 0.007198 -0.000017 0.000012 ( 0.000005 0.000004 0.000004 ) -0.000017 0.007190 -0.000023 ( 0.000004 0.000005 0.000004 ) 0.000012 -0.000023 0.007179 ( 0.000004 0.000004 0.000006 ) unit cell: 8.360(3) 8.365(3) 8.372(3) 89.81(3) 90.10(3) 89.86(3) V = 585.4(4) 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 1 365 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Run 8 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.971) HKL list info: 574 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007529 0.076929 -0.035142 ( 0.000029 0.000029 0.000035 ) -0.083623 -0.011642 -0.008173 ( 0.000031 0.000031 0.000038 ) -0.012209 0.033717 0.076661 ( 0.000029 0.000030 0.000036 ) M - matrix: 0.007198 -0.000017 0.000012 ( 0.000005 0.000004 0.000004 ) -0.000017 0.007190 -0.000024 ( 0.000004 0.000005 0.000004 ) 0.000012 -0.000024 0.007179 ( 0.000004 0.000004 0.000006 ) Constraint UB - matrix: -0.007529 0.076929 -0.035142 ( 0.000029 0.000029 0.000035 ) -0.083623 -0.011642 -0.008173 ( 0.000031 0.000031 0.000038 ) -0.012209 0.033717 0.076661 ( 0.000029 0.000030 0.000036 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 346 obs out of 365 (total:365,skipped:0) (94.79%) unit cell: 8.360(3) 8.365(3) 8.372(3) 89.81(3) 90.10(3) 89.86(3) V = 585.4(4) unit cell: 8.3655(7) 8.3655(7) 8.3655(7) 90.0 90.0 90.0 V = 585.43(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 346 obs out of 365 (total:365,skipped:0) (94.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb 3 of 326 peaks identified as outliers and rejected 323 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 323 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 323 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.60 | 32 | 1.040 ( 0.284) | 1.300 ( 0.759) | 1.641 ( 1.398) | 1.60- 1.17 | 32 | 1.052 ( 0.067) | 1.090 ( 0.203) | 1.075 ( 0.501) | 1.17- 1.01 | 32 | 1.097 ( 0.066) | 1.065 ( 0.098) | 1.144 ( 0.553) | 0.98- 0.91 | 32 | 1.114 ( 0.058) | 1.082 ( 0.097) | 1.163 ( 0.480) | 0.91- 0.82 | 32 | 1.131 ( 0.058) | 1.078 ( 0.096) | 1.249 ( 0.536) | 0.82- 0.76 | 32 | 1.148 ( 0.068) | 1.081 ( 0.081) | 1.190 ( 0.395) | 0.76- 0.72 | 32 | 1.179 ( 0.051) | 1.111 ( 0.072) | 1.186 ( 0.409) | 0.72- 0.67 | 32 | 1.160 ( 0.059) | 1.087 ( 0.076) | 1.200 ( 0.410) | 0.67- 0.64 | 32 | 1.175 ( 0.062) | 1.156 ( 0.135) | 1.154 ( 0.410) | 0.64- 0.59 | 35 | 1.218 ( 0.111) | 1.102 ( 0.133) | 1.369 ( 0.553) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 323 | 1.132 ( 0.124) | 1.115 ( 0.272) | 1.238 ( 0.650) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 322 obs out of 323 (total:323,skipped:0) (99.69%) UB - matrix: -0.007608 0.076948 -0.035194 ( 0.000017 0.000017 0.000020 ) -0.083770 -0.011723 -0.008133 ( 0.000017 0.000017 0.000020 ) -0.012228 0.033620 0.076843 ( 0.000020 0.000021 0.000024 ) M - matrix: 0.007225 -0.000015 0.000009 ( 0.000003 0.000002 0.000002 ) -0.000015 0.007189 -0.000029 ( 0.000002 0.000003 0.000002 ) 0.000009 -0.000029 0.007210 ( 0.000002 0.000002 0.000004 ) unit cell: 8.3449(17) 8.3658(19) 8.354(2) 89.77(2) 90.074(19) 89.885(17) V = 583.2(2) OTKP changes: 322 1 1 1 No constraint UB - matrix: -0.007528 0.076902 -0.035226 ( 0.000016 0.000016 0.000018 ) -0.083643 -0.011771 -0.008230 ( 0.000015 0.000015 0.000017 ) -0.012265 0.033920 0.076729 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007203 -0.000010 0.000012 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007203 -0.000009 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000009 0.007196 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007528 0.076902 -0.035226 ( 0.000016 0.000016 0.000018 ) -0.083643 -0.011771 -0.008230 ( 0.000015 0.000015 0.000017 ) -0.012265 0.033920 0.076729 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 322 obs out of 323 (total:323,skipped:0) (99.69%) unit cell: 8.3574(14) 8.3574(16) 8.3616(15) 89.925(15) 90.099(14) 89.918(15) V = 584.02(18) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.899) HKL list info: 574 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007528 0.076902 -0.035226 ( 0.000016 0.000016 0.000018 ) -0.083643 -0.011771 -0.008230 ( 0.000015 0.000015 0.000017 ) -0.012265 0.033920 0.076729 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007203 -0.000010 0.000012 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007203 -0.000009 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000009 0.007196 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007528 0.076902 -0.035226 ( 0.000016 0.000016 0.000018 ) -0.083643 -0.011771 -0.008230 ( 0.000015 0.000015 0.000017 ) -0.012265 0.033920 0.076729 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 322 obs out of 323 (total:323,skipped:0) (99.69%) unit cell: 8.3574(14) 8.3574(16) 8.3616(15) 89.925(15) 90.099(14) 89.918(15) V = 584.02(18) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 322 obs out of 323 (total:323,skipped:0) (99.69%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb 2 of 326 peaks identified as outliers and rejected 324 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 324 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 324 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.61 | 32 | 1.073 ( 0.321) | 1.356 ( 0.808) | 1.640 ( 1.253) | 1.60- 1.20 | 32 | 1.052 ( 0.072) | 1.084 ( 0.148) | 1.120 ( 0.480) | 1.17- 1.02 | 32 | 1.098 ( 0.070) | 1.062 ( 0.104) | 1.184 ( 0.553) | 1.02- 0.92 | 32 | 1.112 ( 0.061) | 1.090 ( 0.080) | 1.188 ( 0.513) | 0.92- 0.84 | 32 | 1.128 ( 0.061) | 1.069 ( 0.107) | 1.248 ( 0.535) | 0.82- 0.78 | 32 | 1.166 ( 0.115) | 1.088 ( 0.086) | 1.165 ( 0.391) | 0.76- 0.72 | 32 | 1.175 ( 0.057) | 1.109 ( 0.084) | 1.186 ( 0.420) | 0.72- 0.67 | 32 | 1.164 ( 0.063) | 1.089 ( 0.073) | 1.132 ( 0.367) | 0.67- 0.64 | 32 | 1.177 ( 0.065) | 1.152 ( 0.132) | 1.187 ( 0.426) | 0.64- 0.59 | 36 | 1.219 ( 0.111) | 1.108 ( 0.134) | 1.329 ( 0.573) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 324 | 1.137 ( 0.135) | 1.121 ( 0.286) | 1.239 ( 0.619) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 343 | 1.142 ( 0.109) | 1.233 ( 0.395) | 1.289 ( 0.625) | 13.1-18.7 | 343 | 1.135 ( 0.100) | 1.182 ( 0.304) | 1.290 ( 0.615) | 18.7-22.9 | 343 | 1.143 ( 0.090) | 1.194 ( 0.318) | 1.287 ( 0.677) | 22.9-27.2 | 343 | 1.132 ( 0.095) | 1.160 ( 0.281) | 1.228 ( 0.576) | 27.2-30.4 | 343 | 1.131 ( 0.100) | 1.146 ( 0.256) | 1.193 ( 0.452) | 30.4-33.6 | 343 | 1.143 ( 0.098) | 1.130 ( 0.203) | 1.191 ( 0.440) | 33.6-37.0 | 344 | 1.145 ( 0.096) | 1.115 ( 0.183) | 1.168 ( 0.431) | 37.0-39.7 | 343 | 1.148 ( 0.114) | 1.088 ( 0.196) | 1.240 ( 0.519) | 39.7-42.7 | 343 | 1.165 ( 0.116) | 1.103 ( 0.243) | 1.208 ( 0.523) | 42.7-50.5 | 346 | 1.211 ( 0.157) | 1.120 ( 0.264) | 1.244 ( 0.549) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.5 | 3434 | 1.150 ( 0.111) | 1.147 ( 0.275) | 1.234 ( 0.548) | Fitted profile normalization line parameters e1 dimension: a=0.0021 b=0.96 e2 dimension: a=-0.0011 b=1.02 e3 dimension: a=-0.0021 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464571 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 15:08:20 2018 PROFFITMAIN - Started at Wed Mar 28 15:08:20 2018 OTKP changes: 3418 2 4 7 OTKP changes: 3418 2 4 7 OTKP changes: 3418 2 4 7 No constraint UB - matrix: -0.007469 0.076864 -0.034856 ( 0.000006 0.000005 0.000005 ) -0.083574 -0.011762 -0.008072 ( 0.000004 0.000004 0.000004 ) -0.012124 0.033658 0.076967 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 0.000001 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007179 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000006 0.007204 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007469 0.076864 -0.034856 ( 0.000006 0.000005 0.000005 ) -0.083574 -0.011762 -0.008072 ( 0.000004 0.000004 0.000004 ) -0.012124 0.033658 0.076967 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000000 ) UB fit with 3424 obs out of 3434 (total:3434,skipped:0) (99.71%) unit cell: 8.3665(4) 8.3713(5) 8.3568(5) 90.051(5) 90.014(4) 90.006(4) V = 585.30(6) unit cell: 8.36488(13) 8.36488(13) 8.36488(13) 90.0 90.0 90.0 V = 585.301(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3654(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.007479 0.076932 -0.034754 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011768 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076913 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076932 -0.034754 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011768 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076913 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3655(9) 8.3668(12) 8.3657(11) 90.054(11) 89.992(10) 89.991(10) V = 585.54(13) unit cell: 8.3660(3) 8.3660(3) 8.3660(3) 90.0 90.0 90.0 V = 585.54(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076932 -0.034754 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011768 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076913 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076932 -0.034754 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011768 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076913 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3655(9) 8.3668(12) 8.3657(11) 90.054(11) 89.992(10) 89.991(10) V = 585.54(13) unit cell: 8.3660(3) 8.3660(3) 8.3660(3) 90.0 90.0 90.0 V = 585.54(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084799 -0.000003 0.000000 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084779 ( 0.000011 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084799 -0.000003 0.000000 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084779 ( 0.000011 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3644(9) 8.3692(13) 8.3664(9) 90.023(11) 90.002(9) 89.992(11) V = 585.68(13) unit cell: 8.3667(3) 8.3667(3) 8.3667(3) 90.0 90.0 90.0 V = 585.68(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 432 obs out of 435 (total:435,skipped:0) (99.31%) UB - matrix: -0.007136 0.076810 -0.034883 ( 0.000016 0.000011 0.000017 ) -0.083534 -0.011634 -0.008048 ( 0.000013 0.000009 0.000014 ) -0.012409 0.033814 0.076700 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007183 0.000004 -0.000031 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007179 0.000008 ( 0.000002 0.000002 0.000002 ) -0.000031 0.000008 0.007165 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3692(13) 8.3717(13) 8.3799(15) 90.062(13) 89.756(13) 90.034(13) V = 587.13(16) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 No constraint UB - matrix: -0.007216 0.076684 -0.035003 ( 0.000015 0.000010 0.000016 ) -0.083543 -0.011682 -0.008069 ( 0.000013 0.000009 0.000014 ) -0.012351 0.033929 0.076833 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007184 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007168 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007194 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007216 0.076684 -0.035003 ( 0.000015 0.000010 0.000016 ) -0.083543 -0.011682 -0.008069 ( 0.000013 0.000009 0.000014 ) -0.012351 0.033929 0.076833 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3685(13) 8.3778(12) 8.3630(15) 90.135(13) 89.822(13) 90.029(12) V = 586.32(16) unit cell: 8.3697(3) 8.3697(3) 8.3697(3) 90.0 90.0 90.0 V = 586.32(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.016) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007216 0.076684 -0.035003 ( 0.000015 0.000010 0.000016 ) -0.083543 -0.011682 -0.008069 ( 0.000013 0.000009 0.000014 ) -0.012351 0.033929 0.076833 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007184 0.000004 -0.000022 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007168 0.000017 ( 0.000001 0.000002 0.000002 ) -0.000022 0.000017 0.007194 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007216 0.076684 -0.035003 ( 0.000015 0.000010 0.000016 ) -0.083543 -0.011682 -0.008069 ( 0.000013 0.000009 0.000014 ) -0.012351 0.033929 0.076833 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3685(13) 8.3778(12) 8.3630(15) 90.135(13) 89.822(13) 90.029(12) V = 586.32(16) unit cell: 8.3697(3) 8.3697(3) 8.3697(3) 90.0 90.0 90.0 V = 586.32(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084634 0.000112 -0.000191 ( 0.000016 0.000011 0.000018 ) 0.000009 0.084718 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084776 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007163 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007177 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000007 0.007187 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084634 0.000112 -0.000191 ( 0.000016 0.000011 0.000018 ) 0.000009 0.084718 0.000087 ( 0.000012 0.000008 0.000013 ) 0.000001 -0.000002 0.084776 ( 0.000009 0.000006 0.000010 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000000 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3808(16) 8.3725(8) 8.3667(10) 90.058(10) 89.872(13) 90.082(11) V = 587.07(14) unit cell: 8.3733(3) 8.3733(3) 8.3733(3) 90.0 90.0 90.0 V = 587.07(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007580 0.076983 -0.034607 ( 0.000014 0.000013 0.000012 ) -0.083455 -0.011897 -0.008142 ( 0.000012 0.000011 0.000009 ) -0.012247 0.033280 0.076940 ( 0.000012 0.000012 0.000010 ) M - matrix: 0.007172 0.000002 -0.000000 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007176 -0.000007 ( 0.000001 0.000002 0.000001 ) -0.000000 -0.000007 0.007184 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3754(11) 8.3734(13) 8.3687(11) 89.946(11) 89.996(11) 90.015(12) V = 586.90(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007174 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007180 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3705(11) 8.3743(12) 8.3708(10) 89.999(10) 90.053(10) 90.086(11) V = 586.77(13) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.77(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.016) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007174 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007180 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3705(11) 8.3743(12) 8.3708(10) 89.999(10) 90.053(10) 90.086(11) V = 586.77(13) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.77(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007181 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007174 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007180 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007565 0.076953 -0.034566 ( 0.000013 0.000012 0.000011 ) -0.083519 -0.011950 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076934 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3705(11) 8.3743(12) 8.3708(10) 89.999(10) 90.053(10) 90.086(11) V = 586.77(13) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.77(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) UB - matrix: -0.007468 0.076669 -0.034978 ( 0.000013 0.000016 0.000012 ) -0.083544 -0.011732 -0.008154 ( 0.000011 0.000013 0.000010 ) -0.012244 0.033568 0.076823 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000003 0.000002 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007143 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000002 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3678(11) 8.3927(14) 8.3640(13) 89.942(13) 90.014(11) 89.973(12) V = 587.39(16) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 701 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.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= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 322 obs out of 324 (total:324,skipped:0) (99.38%) UB - matrix: -0.007659 0.076910 -0.035058 ( 0.000018 0.000018 0.000021 ) -0.083707 -0.011701 -0.008165 ( 0.000015 0.000015 0.000017 ) -0.012338 0.033724 0.076849 ( 0.000018 0.000018 0.000021 ) M - matrix: 0.007218 -0.000026 0.000004 ( 0.000003 0.000002 0.000002 ) -0.000026 0.007189 -0.000009 ( 0.000002 0.000003 0.000002 ) 0.000004 -0.000009 0.007202 ( 0.000002 0.000002 0.000004 ) unit cell: 8.3489(15) 8.3654(19) 8.358(2) 89.927(19) 90.030(17) 89.796(16) V = 583.8(2) OTKP changes: 322 1 1 1 No constraint UB - matrix: -0.007533 0.076918 -0.035229 ( 0.000016 0.000017 0.000019 ) -0.083655 -0.011765 -0.008229 ( 0.000014 0.000015 0.000017 ) -0.012265 0.033928 0.076730 ( 0.000014 0.000014 0.000016 ) M - matrix: 0.007205 -0.000011 0.000013 ( 0.000002 0.000002 0.000002 ) -0.000011 0.007206 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000010 0.007196 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007533 0.076918 -0.035229 ( 0.000016 0.000017 0.000019 ) -0.083655 -0.011765 -0.008229 ( 0.000014 0.000015 0.000017 ) -0.012265 0.033928 0.076730 ( 0.000014 0.000014 0.000016 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 323 obs out of 324 (total:324,skipped:0) (99.69%) unit cell: 8.3562(14) 8.3558(17) 8.3613(16) 89.924(16) 90.101(15) 89.910(15) V = 583.81(19) unit cell: 8.3578(4) 8.3578(4) 8.3578(4) 90.0 90.0 90.0 V = 583.81(4) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) HKL list info: 573 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007533 0.076918 -0.035229 ( 0.000016 0.000017 0.000019 ) -0.083655 -0.011765 -0.008229 ( 0.000014 0.000015 0.000017 ) -0.012265 0.033928 0.076730 ( 0.000014 0.000014 0.000016 ) M - matrix: 0.007205 -0.000011 0.000013 ( 0.000002 0.000002 0.000002 ) -0.000011 0.007206 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000010 0.007196 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007533 0.076918 -0.035229 ( 0.000016 0.000017 0.000019 ) -0.083655 -0.011765 -0.008229 ( 0.000014 0.000015 0.000017 ) -0.012265 0.033928 0.076730 ( 0.000014 0.000014 0.000016 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 323 obs out of 324 (total:324,skipped:0) (99.69%) unit cell: 8.3562(14) 8.3558(17) 8.3613(16) 89.924(16) 90.101(15) 89.910(15) V = 583.81(19) unit cell: 8.3578(4) 8.3578(4) 8.3578(4) 90.0 90.0 90.0 V = 583.81(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 323 obs out of 324 (total:324,skipped:0) (99.69%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.084905 -0.000178 0.000146 ( 0.000015 0.000015 0.000017 ) 0.000006 0.084870 -0.000102 ( 0.000014 0.000015 0.000017 ) 0.000002 -0.000005 0.084843 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007209 -0.000015 0.000013 ( 0.000002 0.000002 0.000002 ) -0.000015 0.007203 -0.000009 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000009 0.007198 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.084905 -0.000178 0.000146 ( 0.000015 0.000015 0.000017 ) 0.000006 0.084870 -0.000102 ( 0.000014 0.000015 0.000017 ) 0.000002 -0.000005 0.084843 ( 0.000013 0.000014 0.000016 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 323 obs out of 324 (total:324,skipped:0) (99.69%) unit cell: 8.3541(14) 8.3575(14) 8.3602(16) 89.928(15) 90.099(15) 89.884(14) V = 583.70(18) unit cell: 8.3573(4) 8.3573(4) 8.3573(4) 90.0 90.0 90.0 V = 583.70(4) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007450 0.076827 -0.034836 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008077 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033669 0.076906 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007185 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007174 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000008 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007450 0.076827 -0.034836 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008077 ( 0.000004 0.000004 0.000004 ) -0.012165 0.033669 0.076906 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 3425 obs out of 3434 (total:3434,skipped:0) (99.74%) unit cell: 8.3678(4) 8.3742(5) 8.3630(5) 90.064(5) 89.991(4) 90.004(4) V = 586.03(6) unit cell: 8.36835(14) 8.36835(14) 8.36835(14) 90.0 90.0 90.0 V = 586.030(17) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 83 reflections under beam stop or inside a detector rejection region 33 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_8.rrpprof 4548 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 15:08:30 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.016) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.016) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) PROFFIT INFO: signal sum: min=155.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256928.1970 PROFFIT INFO: background sum: min=345.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11267.0000 PROFFIT INFO: num of signal pixels: min=56 max=899 PROFFIT INFO: Inet: min=530.6313 max=7106025.5000 PROFFIT INFO: sig(Inet): min=187.7506 max=63739.8086 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 5 122 390 614 951 1051 1943 3061 4159 4548 Percent 0.0 0.1 2.7 8.6 13.5 20.9 23.1 42.7 67.3 91.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4548 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 4548 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7106026- 1478477 454 2251000.68 133.41 100.00 1478318- 907119 454 1177528.40 104.56 100.00 906923- 293251 454 531399.94 91.92 100.00 292896- 198881 454 238487.93 65.84 100.00 198854- 151032 454 170634.29 46.59 100.00 150922- 118449 454 133809.46 35.90 100.00 118430- 86507 454 103455.24 28.84 100.00 86503- 5845 454 47942.02 19.37 100.00 5843- 3303 454 4316.90 4.76 79.07 3302- 531 462 2351.62 3.02 36.15 ------------------------------------------------------------------------------------ 7106026- 531 4548 465276.92 53.33 91.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 810717.46 84.87 100.00 1.41- 1.12 454 674714.99 68.98 98.24 1.12- 0.96 454 660734.30 75.27 97.80 0.96- 0.88 454 433770.18 57.06 93.17 0.88- 0.81 454 589173.13 66.70 97.14 0.81- 0.74 454 293705.12 38.62 90.97 0.74- 0.71 454 283401.08 37.88 88.77 0.71- 0.65 454 449451.91 46.77 94.93 0.65- 0.62 454 238521.64 28.78 73.13 0.62- 0.58 462 222851.20 28.83 80.30 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 465276.92 53.33 91.42 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:08:30 2018 Sorting 4548 observations 120 unique observations with > 7.00 F2/sig(F2) 4548 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 73 789 Total number of frames 789 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4548 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 10 118 Total number of frames 118 3648 observations > 7.00 F2/sig(F2) 3648 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 10 118 Total number of frames 118 Removing 'redundancy=1' reflections Average redundancy: 28.7 (Out of 3648 removed 5 = 3643, 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 3643 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 10 118 Total number of frames 118 127 unique data precomputed (should be 127) 127 unique data with 3643 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 28.7 (Out of 3643 removed 0 = 3643, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3643 observations RMS deviation of equivalent data = 0.24622 Rint = 0.20133 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20083, wR= 0.26355 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14437, wR= 0.19289, Acormin=0.635, Acormax=1.325, Acor_av=0.947 F test: Probability=1.000, F= 1.932 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11635, wR= 0.15219, Acormin=0.515, Acormax=1.420, Acor_av=0.925 F test: Probability=1.000, F= 1.538 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12618, wR= 0.16946, Acormin=0.614, Acormax=1.568, Acor_av=0.959 F test: Probability=0.000, F= 0.849 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09547, wR= 0.12732, Acormin=0.451, Acormax=1.494, Acor_av=0.938 F test: Probability=1.000, F= 1.482 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08950, wR= 0.11769, Acormin=0.454, Acormax=1.557, Acor_av=0.916 F test: Probability=1.000, F= 1.136 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11705, wR= 0.15788, Acormin=0.601, Acormax=1.737, Acor_av=0.930 F test: Probability=0.000, F= 0.584 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09082, wR= 0.11980, Acormin=0.448, Acormax=1.641, Acor_av=0.930 F test: Probability=0.000, F= 0.969 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08470, wR= 0.11146, Acormin=0.456, Acormax=1.641, Acor_av=0.906 F test: Probability=0.999, F= 1.112 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07846, wR= 0.10191, Acormin=0.406, Acormax=1.612, Acor_av=0.819 F test: Probability=1.000, F= 1.162 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09692, wR= 0.12156, Acormin=0.206, Acormax=1.555, Acor_av=0.803 F test: Probability=0.000, F= 0.656 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09097, wR= 0.11499, Acormin=0.272, Acormax=1.590, Acor_av=0.834 F test: Probability=0.000, F= 0.744 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08705, wR= 0.11056, Acormin=0.095, Acormax=0.382, Acor_av=0.202 F test: Probability=0.000, F= 0.811 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07601, wR= 0.09885, Acormin=0.120, Acormax=0.468, Acor_av=0.235 F test: Probability=0.957, F= 1.060 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06914, wR= 0.09164, Acormin=0.125, Acormax=0.489, Acor_av=0.250 F test: Probability=1.000, F= 1.276 Final absorption model (ne=6, no=5): Rint= 0.07846, Acormin=0.406, Acormax=1.612, Acor_av=0.819 Combined refinement in use Rint: 0.20146 There are 118 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: 6, max odd order: 5 (48 parameters) Refinement control: 165 pars with 13695 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24622 Using Levenberg-Marquardt: 0.00010 New wR= 0.05629 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20133 with corrections 0.04379 Rint for all data: 0.20146 with corrections 0.04401 4 observations identified as outliers and rejected Cycle 2 wR= 0.05579 Using Levenberg-Marquardt: 0.00001 New wR= 0.05224 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20128 with corrections 0.04050 Rint for all data: 0.20146 with corrections 0.04093 1 observations identified as outliers and rejected Cycle 3 wR= 0.05219 Using Levenberg-Marquardt: 0.00000 New wR= 0.05139 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20122 with corrections 0.03943 Rint for all data: 0.20146 with corrections 0.04002 0 observations identified as outliers and rejected Cycle 4 wR= 0.05139 Using Levenberg-Marquardt: 0.00000 New wR= 0.05102 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20122 with corrections 0.03895 Rint for all data: 0.20146 with corrections 0.03957 0 observations identified as outliers and rejected Cycle 5 wR= 0.05102 Using Levenberg-Marquardt: 0.00000 New wR= 0.05083 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20122 with corrections 0.03870 Rint for all data: 0.20146 with corrections 0.03932 0 observations identified as outliers and rejected Final wR= 0.05083 Final frame scales: Min= 0.7593 Max= 1.1702 Final absorption correction factors: Amin= 0.4002 Amax= 1.5819 PROFFIT INFO: Inet (after scale3 abspack): min=513.6133 max=4984479.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.3517 max=66050.3203 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4548 reflections read from tmp file 711 reflections are rejected (710 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 5 2 2 1 3 2 1 138 Initial Chi^2= 0.36150 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.95196 Current error model SIG(F2)^2 = 103.97*I_RAW + 0.00*I_BACK+(0.01920*)^2 Cycle 2, Chi^2= 1.00018 Current error model SIG(F2)^2 = 101.60*I_RAW + 0.00*I_BACK+(0.01808*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 101.27*I_RAW + 0.00*I_BACK+(0.01817*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 101.32*I_RAW + 0.00*I_BACK+(0.01816*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 101.32*I_RAW + 0.00*I_BACK+(0.01816*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4984480- 1388165 454 2108329.97 49.98 100.00 1387076- 897651 454 1104972.47 42.06 100.00 896677- 285645 454 536976.97 40.25 100.00 285334- 181496 454 221545.50 33.18 100.00 181398- 150442 454 165106.93 26.35 100.00 150434- 112633 454 127472.08 20.83 100.00 112532- 89633 454 101316.14 17.95 100.00 89360- 5274 454 51625.64 13.25 99.78 5274- 3089 454 3946.41 4.52 93.61 3085- 514 462 2387.15 3.53 65.80 ------------------------------------------------------------------------------------ 4984480- 514 4548 441593.99 25.15 95.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 820010.99 39.08 100.00 1.41- 1.12 454 667936.01 30.77 99.78 1.12- 0.96 454 604824.63 30.15 98.46 0.96- 0.88 454 409718.59 25.34 97.36 0.88- 0.81 454 550434.54 29.58 98.46 0.81- 0.74 454 269634.93 19.95 96.04 0.74- 0.71 454 263708.64 20.34 94.27 0.71- 0.65 454 409909.75 23.52 97.36 0.65- 0.62 454 222272.25 16.18 85.90 0.62- 0.58 462 201716.51 16.75 91.13 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 441593.99 25.15 95.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 820010.99 39.08 100.00 4.82- 1.12 908 743973.50 34.93 99.89 4.82- 0.96 1362 697590.54 33.34 99.41 4.82- 0.88 1816 625622.56 31.34 98.90 4.82- 0.81 2270 610584.95 30.99 98.81 4.82- 0.74 2724 553759.95 29.15 98.35 4.82- 0.71 3178 512324.05 27.89 97.77 4.82- 0.65 3632 499522.26 27.34 97.71 4.82- 0.62 4086 468716.71 26.10 96.40 4.82- 0.58 4548 441593.99 25.15 95.87 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 441593.99 25.15 95.87 Scale applied to data: s=0.200623 (maximum obs:4984479.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.039; Rsigma 0.025: data 4548 -> merged 156 With outlier rejection... Rint 0.039; Rsigma 0.025: data 4537 -> merged 156 Rejected total: 11, method kkm 10, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585902, 4.831469 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 27.07 100.00 379 1.41 - 1.12 14 14 37.71 100.00 528 1.12 - 0.97 14 14 37.64 100.00 527 0.96 - 0.84 14 14 40.14 100.00 562 0.84 - 0.78 14 14 30.50 100.00 427 0.78 - 0.73 14 14 31.79 100.00 445 0.73 - 0.69 14 14 30.64 100.00 429 0.69 - 0.66 14 14 25.50 100.00 357 0.65 - 0.63 14 14 28.07 100.00 393 0.63 - 0.60 14 14 24.79 100.00 347 --------------------------------------------------------------- 8.36 - 0.60 140 140 31.39 100.00 4394 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:08:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367809 8.374212 8.363038 90.0635 89.9912 90.0040 4537 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2307 0 3039 3040 4537 N (int>3sigma) = 0 0 0 0 2307 0 2908 2915 4349 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.9 89.8 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 25.5 0.0 25.2 25.3 25.1 Lattice type: F chosen Volume: 586.03 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.914 5.915 5.916 90.03 119.95 119.95 Niggli form: a.a = 34.978 b.b = 34.985 c.c = 34.996 b.c = -0.020 a.c = -17.467 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.039 [ 4381] Vol = 586.0 Cell: 8.368 8.374 8.363 90.06 89.99 90.00 Volume: 586.03 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 4099] Vol = 439.5 Cell: 5.919 5.915 14.501 90.00 90.06 120.03 Volume: 439.52 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1324] Vol = 439.5 Trigonal Cell: 5.919 5.915 14.501 90.00 90.06 120.03 Volume: 439.52 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.027 TETRAGONAL I-lattice R(int) = 0.038 [ 4130] Vol = 293.0 Cell: 5.919 5.919 8.363 89.96 89.95 89.96 Volume: 293.01 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.078 TETRAGONAL I-lattice R(int) = 0.038 [ 4130] Vol = 293.0 Cell: 5.919 5.919 8.363 90.05 90.04 89.96 Volume: 293.01 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.037 ORTHORHOMBIC I-lattice R(int) = 0.038 [ 4077] Vol = 293.0 Cell: 5.919 5.919 8.363 89.95 89.96 89.96 Volume: 293.01 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 4075] Vol = 293.0 Cell: 5.914 8.368 5.921 89.99 89.92 90.00 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.028 MONOCLINIC I-lattice R(int) = 0.037 [ 3731] Vol = 293.0 Cell: 5.919 5.919 8.363 90.04 90.05 89.96 Volume: 293.01 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.067 MONOCLINIC I-lattice R(int) = 0.035 [ 3728] Vol = 293.0 Cell: 5.914 5.921 8.368 90.01 90.00 90.08 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.011 MONOCLINIC I-lattice R(int) = 0.034 [ 3743] Vol = 293.0 Cell: 5.914 8.368 5.921 89.99 90.08 90.00 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.033 MONOCLINIC I-lattice R(int) = 0.035 [ 3724] Vol = 293.0 Cell: 5.921 5.914 8.368 90.00 90.01 89.92 Volume: 293.01 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.035 [ 3726] Vol = 293.0 Cell: 10.249 5.915 5.916 90.03 125.21 89.95 Volume: 293.01 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 3072] Vol = 146.5 Cell: 5.914 5.915 5.916 90.03 119.95 119.95 Volume: 146.51 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2307 0 3039 3040 4537 N (int>3sigma) = 0 0 0 0 2307 0 2908 2915 4349 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.9 89.8 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 25.5 0.0 25.2 25.3 25.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 47 47 364 1009 N I>3s 40 40 324 1009 0.7 0.7 0.7 39.6 7.8 7.8 5.1 28.6 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 0.038 4037 Fd-3m 1 1 227 C N N N N 37 2284 0.039 4076 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367809 8.374212 8.363038 90.0635 89.9912 90.0040 ZERR 3.00 0.000387 0.000532 0.000503 0.0050 0.0044 0.0045 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4873503- 1041658 730 727 26 28.0 1759585.32 47.43 0.034 0.044 1030358- 252627 714 710 26 27.3 613839.51 40.11 0.046 0.061 251608- 125015 1047 1046 26 40.2 175600.80 27.39 0.039 0.053 119863- 89946 749 749 26 28.8 106149.70 18.37 0.056 0.073 84557- 3671 684 682 26 26.2 28167.13 9.06 0.073 0.090 3565- 1709 624 623 26 24.0 2876.79 3.94 0.206 0.261 ------------------------------------------------------------------------------------------- 4873503- 1709 4548 4537 156 29.1 440650.51 25.13 0.039 0.051 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 860 857 26 33.0 678128.69 34.11 0.037 0.047 0.021 1.12-0.88 1018 1017 26 39.1 554595.27 28.91 0.032 0.044 0.023 0.85-0.75 843 842 26 32.4 421918.29 24.31 0.036 0.048 0.026 0.74-0.68 747 746 26 28.7 355858.22 22.04 0.043 0.052 0.030 0.67-0.63 724 724 26 27.8 211874.78 17.47 0.056 0.076 0.037 0.62-0.59 356 351 26 13.5 227717.71 16.56 0.053 0.058 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 4548 4537 156 29.1 440650.51 25.13 0.039 0.051 0.025 inf-0.60 4398 4392 139 31.6 450022.69 25.45 0.038 0.050 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 857 26 26 100.0 33.0 678128.69 211.89 0.037 0.005 1.12-0.88 1017 26 26 100.0 39.1 554595.27 182.65 0.032 0.004 0.85-0.75 842 26 26 100.0 32.4 421918.29 146.21 0.036 0.005 0.74-0.68 746 26 26 100.0 28.7 355858.22 120.75 0.043 0.006 0.67-0.63 724 26 26 100.0 27.8 211874.78 91.85 0.056 0.007 0.62-0.59 351 27 26 96.3 13.5 227717.71 72.00 0.053 0.014 -------------------------------------------------------------------------------------------- inf-0.59 4537 157 156 99.4 29.1 440650.51 148.18 0.039 0.006 inf-0.60 4392 139 139 100.0 31.6 450022.69 151.40 0.038 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007450 0.076826 -0.034836 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008077 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033668 0.076906 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007185 0.000000 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007174 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000008 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007450 0.076826 -0.034836 ( 0.000006 0.000005 0.000005 ) -0.083556 -0.011758 -0.008077 ( 0.000004 0.000004 0.000004 ) -0.012164 0.033668 0.076906 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3678(4) 8.3743(5) 8.3631(5) 90.063(5) 89.991(4) 90.004(4) V = 586.04(6) unit cell: 8.36838(14) 8.36838(14) 8.36838(14) 90.0 90.0 90.0 V = 586.036(17) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.016) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.016) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.900) PROFFIT INFO: signal sum: min=155.0000 max=22702712.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3256928.1970 PROFFIT INFO: background sum: min=345.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11267.0000 PROFFIT INFO: num of signal pixels: min=56 max=899 PROFFIT INFO: Inet: min=530.6313 max=7106025.5000 PROFFIT INFO: sig(Inet): min=187.7506 max=63739.8086 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 10 244 780 1228 1902 2102 3886 6122 8318 9096 Percent 0.0 0.1 2.7 8.6 13.5 20.9 23.1 42.7 67.3 91.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4548 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 4548 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7106026- 1478477 454 2251000.68 133.41 100.00 1478318- 907119 454 1177528.40 104.56 100.00 906923- 293251 454 531399.94 91.92 100.00 292896- 198881 454 238487.93 65.84 100.00 198854- 151032 454 170634.29 46.59 100.00 150922- 118449 454 133809.46 35.90 100.00 118430- 86507 454 103455.24 28.84 100.00 86503- 5845 454 47942.02 19.37 100.00 5843- 3303 454 4316.90 4.76 79.07 3302- 531 462 2351.62 3.02 36.15 ------------------------------------------------------------------------------------ 7106026- 531 4548 465276.92 53.33 91.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 810717.46 84.87 100.00 1.41- 1.12 454 674714.99 68.98 98.24 1.12- 0.96 454 660734.30 75.27 97.80 0.96- 0.88 454 433770.18 57.06 93.17 0.88- 0.81 454 589173.13 66.70 97.14 0.81- 0.74 454 293705.12 38.62 90.97 0.74- 0.71 454 283401.08 37.88 88.77 0.71- 0.65 454 449451.91 46.77 94.93 0.65- 0.62 454 238521.64 28.78 73.13 0.62- 0.58 462 222851.20 28.83 80.30 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 465276.92 53.33 91.42 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:08:32 2018 Sorting 4548 observations 86 unique observations with > 7.00 F2/sig(F2) 4548 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 73 789 Total number of frames 789 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4548 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 7 81 Total number of frames 81 3648 observations > 7.00 F2/sig(F2) 3648 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 7 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 40.0 (Out of 3648 removed 4 = 3644, 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): 4/m3bar2/m 3644 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 7 81 Total number of frames 81 91 unique data precomputed (should be 91) 91 unique data with 3644 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 40.0 (Out of 3644 removed 0 = 3644, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3644 observations RMS deviation of equivalent data = 0.24668 Rint = 0.20154 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20145, wR= 0.26523 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14448, wR= 0.19364, Acormin=0.635, Acormax=1.324, Acor_av=0.947 F test: Probability=1.000, F= 1.941 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11672, wR= 0.15264, Acormin=0.515, Acormax=1.421, Acor_av=0.925 F test: Probability=1.000, F= 1.531 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12722, wR= 0.17077, Acormin=0.616, Acormax=1.565, Acor_av=0.958 F test: Probability=0.000, F= 0.840 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09637, wR= 0.12844, Acormin=0.451, Acormax=1.495, Acor_av=0.937 F test: Probability=1.000, F= 1.463 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09010, wR= 0.11873, Acormin=0.453, Acormax=1.554, Acor_av=0.915 F test: Probability=1.000, F= 1.142 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11772, wR= 0.15890, Acormin=0.597, Acormax=1.741, Acor_av=0.929 F test: Probability=0.000, F= 0.585 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09172, wR= 0.12062, Acormin=0.442, Acormax=1.650, Acor_av=0.929 F test: Probability=0.000, F= 0.963 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08513, wR= 0.11228, Acormin=0.448, Acormax=1.647, Acor_av=0.905 F test: Probability=0.999, F= 1.116 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07879, wR= 0.10252, Acormin=0.403, Acormax=1.611, Acor_av=0.818 F test: Probability=1.000, F= 1.164 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09756, wR= 0.12302, Acormin=0.216, Acormax=1.560, Acor_av=0.802 F test: Probability=0.000, F= 0.653 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09155, wR= 0.11600, Acormin=0.282, Acormax=1.595, Acor_av=0.833 F test: Probability=0.000, F= 0.741 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08739, wR= 0.11104, Acormin=0.094, Acormax=0.379, Acor_av=0.200 F test: Probability=0.000, F= 0.812 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07630, wR= 0.09902, Acormin=0.119, Acormax=0.464, Acor_av=0.233 F test: Probability=0.960, F= 1.061 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06927, wR= 0.09166, Acormin=0.124, Acormax=0.486, Acor_av=0.248 F test: Probability=1.000, F= 1.282 Final absorption model (ne=6, no=5): Rint= 0.07879, Acormin=0.403, Acormax=1.611, Acor_av=0.818 Combined refinement in use Rint: 0.20166 There are 81 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24668 Using Levenberg-Marquardt: 0.00010 New wR= 0.06340 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20154 with corrections 0.04910 Rint for all data: 0.20166 with corrections 0.04932 4 observations identified as outliers and rejected Cycle 2 wR= 0.06279 Using Levenberg-Marquardt: 0.00001 New wR= 0.05719 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20148 with corrections 0.04463 Rint for all data: 0.20166 with corrections 0.04510 4 observations identified as outliers and rejected Cycle 3 wR= 0.05718 Using Levenberg-Marquardt: 0.00000 New wR= 0.05567 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20152 with corrections 0.04326 Rint for all data: 0.20166 with corrections 0.04374 1 observations identified as outliers and rejected Cycle 4 wR= 0.05562 Using Levenberg-Marquardt: 0.00000 New wR= 0.05493 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20146 with corrections 0.04242 Rint for all data: 0.20166 with corrections 0.04306 0 observations identified as outliers and rejected Cycle 5 wR= 0.05493 Using Levenberg-Marquardt: 0.00000 New wR= 0.05453 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20146 with corrections 0.04202 Rint for all data: 0.20166 with corrections 0.04266 0 observations identified as outliers and rejected Final wR= 0.05453 Final frame scales: Min= 0.8310 Max= 1.2028 Final absorption correction factors: Amin= 0.4218 Amax= 1.6218 PROFFIT INFO: Inet (after scale3 abspack): min=516.9444 max=4983461.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.7593 max=65585.1484 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4548 reflections read from tmp file 785 reflections are rejected (785 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 4 0 1 2 2 1 3 95 Initial Chi^2= 0.34841 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.92607 Current error model SIG(F2)^2 = 111.85*I_RAW + 0.00*I_BACK+(0.01997*)^2 Cycle 2, Chi^2= 0.99999 Current error model SIG(F2)^2 = 101.84*I_RAW + 0.00*I_BACK+(0.01959*)^2 Cycle 3, Chi^2= 1.00001 Current error model SIG(F2)^2 = 102.14*I_RAW + 0.00*I_BACK+(0.01953*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 102.14*I_RAW + 0.00*I_BACK+(0.01953*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4983461- 1395073 454 2101214.32 47.08 100.00 1393648- 900743 454 1108055.16 40.25 100.00 899358- 286005 454 536691.36 38.48 100.00 285617- 181923 454 221154.05 32.11 100.00 181908- 150251 454 165066.98 25.78 100.00 150229- 112631 454 127734.45 20.56 100.00 112387- 89111 454 101542.92 17.69 100.00 88947- 5292 454 51589.54 13.13 99.78 5290- 3097 454 3949.12 4.48 93.61 3097- 517 462 2384.50 3.53 65.37 ------------------------------------------------------------------------------------ 4983461- 517 4548 441165.06 24.27 95.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 816294.75 37.12 100.00 1.41- 1.12 454 665498.20 29.46 99.56 1.12- 0.96 454 602501.54 28.93 98.46 0.96- 0.88 454 409904.27 24.49 97.36 0.88- 0.81 454 550428.92 28.53 98.46 0.81- 0.74 454 269606.52 19.41 96.04 0.74- 0.71 454 264387.33 19.86 94.27 0.71- 0.65 454 411486.00 22.84 97.14 0.65- 0.62 454 223146.53 15.81 85.90 0.62- 0.58 462 202600.34 16.43 91.13 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 441165.06 24.27 95.82 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 454 816294.75 37.12 100.00 4.82- 1.12 908 740896.47 33.29 99.78 4.82- 0.96 1362 694764.83 31.83 99.34 4.82- 0.88 1816 623549.69 30.00 98.84 4.82- 0.81 2270 608925.53 29.71 98.77 4.82- 0.74 2724 552372.37 27.99 98.31 4.82- 0.71 3178 511231.65 26.83 97.73 4.82- 0.65 3632 498763.44 26.33 97.66 4.82- 0.62 4086 468139.34 25.16 96.35 4.82- 0.58 4548 441165.06 24.27 95.82 ------------------------------------------------------------------------------------ 4.82- 0.58 4548 441165.06 24.27 95.82 Scale applied to data: s=0.200664 (maximum obs:4983461.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.043; Rsigma 0.027: data 4548 -> merged 109 With outlier rejection... Rint 0.042; Rsigma 0.027: data 4541 -> merged 109 Rejected total: 7, method kkm 6, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585904, 4.831487 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 28.40 100.00 284 1.61 - 1.21 10 10 42.70 100.00 427 1.17 - 1.01 10 10 54.30 100.00 543 0.99 - 0.89 10 10 53.30 100.00 533 0.88 - 0.81 10 10 51.40 100.00 514 0.81 - 0.74 10 10 43.80 100.00 438 0.73 - 0.71 10 10 49.30 100.00 493 0.70 - 0.66 10 10 39.20 100.00 392 0.66 - 0.64 10 10 39.60 100.00 396 0.63 - 0.60 10 10 37.60 100.00 376 --------------------------------------------------------------- 8.36 - 0.60 100 100 43.96 100.00 4396 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:08:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.367809 8.374212 8.363038 90.0635 89.9912 90.0040 4537 Reflections read from file xs1715a.hkl; mean (I/sigma) = 25.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2307 0 3039 3040 4537 N (int>3sigma) = 0 0 0 0 2307 0 2908 2915 4349 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.9 89.8 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 25.5 0.0 25.2 25.3 25.1 Lattice type: F chosen Volume: 586.03 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.914 5.915 5.916 90.03 119.95 119.95 Niggli form: a.a = 34.978 b.b = 34.985 c.c = 34.996 b.c = -0.020 a.c = -17.467 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.039 [ 4381] Vol = 586.0 Cell: 8.368 8.374 8.363 90.06 89.99 90.00 Volume: 586.03 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 4099] Vol = 439.5 Cell: 5.919 5.915 14.501 90.00 90.06 120.03 Volume: 439.52 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1324] Vol = 439.5 Trigonal Cell: 5.919 5.915 14.501 90.00 90.06 120.03 Volume: 439.52 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.0000 0.5000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.027 TETRAGONAL I-lattice R(int) = 0.038 [ 4130] Vol = 293.0 Cell: 5.919 5.919 8.363 89.96 89.95 89.96 Volume: 293.01 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.078 TETRAGONAL I-lattice R(int) = 0.038 [ 4130] Vol = 293.0 Cell: 5.919 5.919 8.363 90.05 90.04 89.96 Volume: 293.01 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.037 ORTHORHOMBIC I-lattice R(int) = 0.038 [ 4077] Vol = 293.0 Cell: 5.919 5.919 8.363 89.95 89.96 89.96 Volume: 293.01 Matrix:-0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.036 [ 4075] Vol = 293.0 Cell: 5.914 8.368 5.921 89.99 89.92 90.00 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.028 MONOCLINIC I-lattice R(int) = 0.037 [ 3731] Vol = 293.0 Cell: 5.919 5.919 8.363 90.04 90.05 89.96 Volume: 293.01 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.067 MONOCLINIC I-lattice R(int) = 0.035 [ 3728] Vol = 293.0 Cell: 5.914 5.921 8.368 90.01 90.00 90.08 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.011 MONOCLINIC I-lattice R(int) = 0.034 [ 3743] Vol = 293.0 Cell: 5.914 8.368 5.921 89.99 90.08 90.00 Volume: 293.01 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [27] err= 0.033 MONOCLINIC I-lattice R(int) = 0.035 [ 3724] Vol = 293.0 Cell: 5.921 5.914 8.368 90.00 90.01 89.92 Volume: 293.01 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.035 [ 3726] Vol = 293.0 Cell: 10.249 5.915 5.916 90.03 125.21 89.95 Volume: 293.01 Matrix: 0.5000 1.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 3072] Vol = 146.5 Cell: 5.914 5.915 5.916 90.03 119.95 119.95 Volume: 146.51 Matrix: 0.0000 0.5000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2307 0 3039 3040 4537 N (int>3sigma) = 0 0 0 0 2307 0 2908 2915 4349 Mean intensity = 0.0 0.0 0.0 0.0 33.7 0.0 88.9 89.8 88.4 Mean int/sigma = 0.0 0.0 0.0 0.0 25.5 0.0 25.2 25.3 25.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 47 47 364 1009 N I>3s 40 40 324 1009 0.7 0.7 0.7 39.6 7.8 7.8 5.1 28.6 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 0.038 4037 Fd-3m 1 1 227 C N N N N 37 2284 0.039 4076 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.367809 8.374212 8.363038 90.0635 89.9912 90.0040 ZERR 3.00 0.000387 0.000532 0.000503 0.0050 0.0044 0.0045 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4782032- 824127 1012 1010 27 37.4 1526214.86 42.79 0.040 0.052 776040- 140116 1349 1345 27 49.8 254501.25 31.36 0.045 0.057 129218- 47076 1114 1114 27 41.3 101400.36 17.81 0.061 0.081 19429- 1708 1073 1072 28 38.3 4223.66 4.56 0.167 0.213 ------------------------------------------------------------------------------------------- 4782032- 1708 4548 4541 109 41.7 440711.07 24.25 0.042 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-1.02 1157 1155 27 42.8 708417.22 33.36 0.038 0.051 0.022 1.01-0.78 1350 1350 27 50.0 435549.61 24.31 0.038 0.052 0.026 0.78-0.65 1180 1178 27 43.6 344494.65 20.95 0.048 0.058 0.031 0.65-0.59 861 858 28 30.6 220559.90 16.42 0.061 0.069 0.037 ------------------------------------------------------------------------------------------------------ inf-0.59 4548 4541 109 41.7 440711.07 24.25 0.042 0.054 0.027 inf-0.60 4398 4394 99 44.4 450018.75 24.55 0.042 0.054 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1155 27 27 100.0 42.8 708417.22 243.29 0.038 0.005 1.01-0.78 1350 27 27 100.0 50.0 435549.61 183.98 0.038 0.004 0.78-0.65 1178 27 27 100.0 43.6 344494.65 147.16 0.048 0.006 0.65-0.59 858 29 28 96.6 30.6 220559.90 103.79 0.061 0.009 -------------------------------------------------------------------------------------------- inf-0.59 4541 110 109 99.1 41.7 440711.07 174.36 0.042 0.005 inf-0.60 4394 99 99 100.0 44.4 450018.75 177.87 0.042 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Mar 28 15:13:02 2018) ID: 2932; threads 39; handles 878; mem 517044.00 (1237728.00)kB; time: 1w 6d 0h 18m 32s MEMORY INFO: Memory PF:0.0, Ph:175.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:504.9,peak PF: 708.5, WS: 269.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:176.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.7,peak PF: 708.5, WS: 271.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.6 (#1110),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Wed Mar 28 15:13:02 2018 Experiment file name: D:\Data\xs1715a\xs1715a Output file name: D:\Data\xs1715a\xs1715a Data reduction with automatic settings UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) 8.37051 ( 0.00039 ) 8.37682 ( 0.00053 ) 8.35710 ( 0.00050 ) 90.12473 ( 0.00499 ) 89.98579 ( 0.00435 ) 90.00567 ( 0.00451 ) V = 585.98 Selected cell (from UM rr/UM ttt/UM f): 1 8.3705 8.3768 8.3571 90.1247 89.9858 90.0057 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\xs1715a\plots_red\xs1715a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1715a\plots_red\xs1715a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1715a\plots_red\xs1715a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1715a\xs1715a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.97 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 Mar 28 15:13:02 2018 Experiment file name: D:\Data\xs1715a\xs1715a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.007494 0.076803 -0.034768 ( 0.000006 0.000005 0.000005 ) -0.083527 -0.011793 -0.008060 ( 0.000004 0.000004 0.000004 ) -0.012149 0.033645 0.077005 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007185 0.000000 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007174 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000008 0.007193 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3705(4) 8.3768(5) 8.3571(5) 90.125(5) 89.986(4) 90.006(4) V = 585.98(6) unit cell: 8.36838(14) 8.36838(14) 8.36838(14) 90.0 90.0 90.0 V = 586.036(17) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007544 0.076952 -0.034724 ( 0.000026 0.000032 0.000025 ) -0.083462 -0.011734 -0.008082 ( 0.000018 0.000022 0.000017 ) -0.012060 0.033612 0.076940 ( 0.000024 0.000030 0.000023 ) M - matrix: 0.007168 -0.000007 0.000009 ( 0.000003 0.000003 0.000003 ) -0.000007 0.007189 0.000009 ( 0.000003 0.000005 0.000003 ) 0.000009 0.000009 0.007191 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3777(18) 8.366(3) 8.364(2) 90.07(3) 90.07(2) 89.95(2) V = 586.2(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) UB - matrix: -0.007501 0.076824 -0.034708 ( 0.000026 0.000032 0.000025 ) -0.083415 -0.011774 -0.008047 ( 0.000017 0.000021 0.000016 ) -0.012138 0.033571 0.076829 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007162 -0.000002 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000002 0.007168 0.000008 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000008 0.007172 ( 0.000002 0.000003 0.000004 ) unit cell: 8.3815(17) 8.378(3) 8.375(2) 90.06(3) 89.99(2) 89.99(2) V = 588.1(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.989) HKL list info: 803 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007504 0.076816 -0.034712 ( 0.000026 0.000032 0.000025 ) -0.083404 -0.011780 -0.008039 ( 0.000017 0.000022 0.000017 ) -0.012136 0.033568 0.076825 ( 0.000023 0.000029 0.000022 ) M - matrix: 0.007160 -0.000001 -0.000001 ( 0.000003 0.000003 0.000002 ) -0.000001 0.007166 0.000007 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000007 0.007172 ( 0.000002 0.000003 0.000004 ) UB fit with 537 obs out of 600 (total:600,skipped:0) (89.50%) unit cell: 8.3826(17) 8.379(3) 8.376(2) 90.06(3) 89.99(2) 89.99(2) V = 588.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 529 obs out of 600 (total:600,skipped:0) (88.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 6 of 455 peaks identified as outliers and rejected 449 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 449 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 449 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.33 | 45 | 1.015 ( 0.204) | 1.300 ( 0.665) | 1.482 ( 1.179) | 1.33- 1.11 | 45 | 1.080 ( 0.077) | 1.141 ( 0.127) | 1.179 ( 0.514) | 1.09- 0.97 | 45 | 1.132 ( 0.072) | 1.253 ( 0.457) | 1.183 ( 0.528) | 0.97- 0.86 | 45 | 1.144 ( 0.065) | 1.150 ( 0.121) | 1.282 ( 0.484) | 0.85- 0.81 | 45 | 1.163 ( 0.054) | 1.205 ( 0.132) | 1.140 ( 0.386) | 0.81- 0.75 | 45 | 1.172 ( 0.052) | 1.132 ( 0.154) | 1.296 ( 0.388) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.188 ( 0.145) | 1.300 ( 0.459) | 0.70- 0.67 | 45 | 1.189 ( 0.059) | 1.210 ( 0.162) | 1.214 ( 0.376) | 0.66- 0.62 | 45 | 1.203 ( 0.083) | 1.219 ( 0.173) | 1.210 ( 0.469) | 0.62- 0.59 | 44 | 1.199 ( 0.068) | 1.205 ( 0.198) | 1.335 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 449 | 1.148 ( 0.106) | 1.200 ( 0.294) | 1.262 ( 0.582) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 448 obs out of 449 (total:449,skipped:0) (99.78%) UB - matrix: -0.007357 0.076781 -0.034782 ( 0.000014 0.000015 0.000013 ) -0.083512 -0.011819 -0.008058 ( 0.000010 0.000010 0.000009 ) -0.012261 0.033584 0.076726 ( 0.000012 0.000013 0.000011 ) M - matrix: 0.007179 0.000010 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000010 0.007163 0.000001 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000001 0.007162 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3716(10) 8.3808(14) 8.3816(12) 90.011(12) 89.905(11) 90.083(12) V = 588.05(15) OTKP changes: 448 1 1 1 No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.948) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007186 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007469 0.076928 -0.034750 ( 0.000012 0.000013 0.000011 ) -0.083576 -0.011771 -0.008081 ( 0.000009 0.000010 0.000008 ) -0.012187 0.033611 0.076906 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) unit cell: 8.3654(9) 8.3672(12) 8.3665(11) 90.054(11) 89.982(10) 89.997(10) V = 585.61(13) unit cell: 8.3664(3) 8.3664(3) 8.3664(3) 90.0 90.0 90.0 V = 585.61(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 449 (total:449,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb 7 of 455 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" 448 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1.tabbin file 448 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 45 | 0.997 ( 0.154) | 1.263 ( 0.649) | 1.378 ( 0.877) | 1.32- 1.09 | 45 | 1.088 ( 0.070) | 1.142 ( 0.118) | 1.299 ( 0.621) | 1.09- 0.96 | 45 | 1.131 ( 0.127) | 1.240 ( 0.339) | 1.200 ( 0.558) | 0.96- 0.87 | 45 | 1.138 ( 0.052) | 1.142 ( 0.122) | 1.248 ( 0.484) | 0.85- 0.81 | 45 | 1.166 ( 0.060) | 1.190 ( 0.128) | 1.168 ( 0.413) | 0.81- 0.74 | 45 | 1.166 ( 0.049) | 1.152 ( 0.151) | 1.272 ( 0.432) | 0.74- 0.71 | 45 | 1.182 ( 0.045) | 1.187 ( 0.144) | 1.269 ( 0.446) | 0.70- 0.66 | 45 | 1.194 ( 0.056) | 1.205 ( 0.162) | 1.205 ( 0.392) | 0.66- 0.62 | 45 | 1.202 ( 0.083) | 1.219 ( 0.175) | 1.275 ( 0.516) | 0.62- 0.59 | 43 | 1.204 ( 0.068) | 1.208 ( 0.197) | 1.337 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 1.147 ( 0.103) | 1.195 ( 0.272) | 1.265 ( 0.545) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) UB fit with 543 obs out of 605 (total:605,skipped:0) (89.75%) UB - matrix: -0.007573 0.077045 -0.034582 ( 0.000030 0.000030 0.000023 ) -0.083428 -0.011792 -0.008067 ( 0.000021 0.000021 0.000016 ) -0.012075 0.033426 0.076960 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007163 -0.000003 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000003 0.007192 0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000003 0.007184 ( 0.000003 0.000003 0.000003 ) unit cell: 8.381(2) 8.364(3) 8.369(2) 90.03(2) 90.05(2) 89.97(2) V = 586.6(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) UB - matrix: -0.007610 0.076822 -0.034550 ( 0.000029 0.000029 0.000022 ) -0.083316 -0.011807 -0.007986 ( 0.000021 0.000021 0.000016 ) -0.012126 0.033409 0.076789 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000006 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007157 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000003 0.000006 0.007154 ( 0.000003 0.000003 0.000003 ) unit cell: 8.390(2) 8.384(3) 8.386(2) 90.04(2) 89.98(2) 89.95(2) V = 589.9(3) OTKP changes: 109 1 1 1 UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 818 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007612 0.076813 -0.034548 ( 0.000029 0.000029 0.000022 ) -0.083314 -0.011803 -0.007993 ( 0.000021 0.000021 0.000016 ) -0.012132 0.033413 0.076777 ( 0.000026 0.000026 0.000020 ) M - matrix: 0.007146 -0.000007 -0.000002 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007156 0.000006 ( 0.000003 0.000005 0.000003 ) -0.000002 0.000006 0.007152 ( 0.000003 0.000003 0.000003 ) UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) unit cell: 8.390(2) 8.385(3) 8.387(2) 90.05(2) 89.98(2) 89.95(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 544 obs out of 605 (total:605,skipped:0) (89.92%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 4 of 455 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 451 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 451 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.37 | 45 | 0.985 ( 0.154) | 1.244 ( 0.735) | 1.229 ( 0.768) | 1.33- 1.12 | 45 | 1.083 ( 0.089) | 1.131 ( 0.115) | 1.122 ( 0.502) | 1.12- 0.97 | 45 | 1.115 ( 0.083) | 1.140 ( 0.112) | 1.309 ( 0.544) | 0.97- 0.88 | 45 | 1.145 ( 0.081) | 1.174 ( 0.118) | 1.135 ( 0.434) | 0.88- 0.81 | 45 | 1.160 ( 0.077) | 1.144 ( 0.124) | 1.242 ( 0.455) | 0.81- 0.75 | 45 | 1.184 ( 0.063) | 1.142 ( 0.120) | 1.158 ( 0.400) | 0.74- 0.71 | 45 | 1.196 ( 0.069) | 1.222 ( 0.143) | 1.165 ( 0.375) | 0.71- 0.67 | 45 | 1.198 ( 0.057) | 1.201 ( 0.170) | 1.156 ( 0.400) | 0.66- 0.63 | 45 | 1.222 ( 0.080) | 1.190 ( 0.151) | 1.146 ( 0.431) | 0.63- 0.59 | 46 | 1.224 ( 0.088) | 1.217 ( 0.228) | 1.299 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 451 | 1.152 ( 0.113) | 1.181 ( 0.274) | 1.196 ( 0.499) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) UB - matrix: -0.007583 0.076667 -0.034653 ( 0.000016 0.000014 0.000011 ) -0.083484 -0.011773 -0.008006 ( 0.000011 0.000010 0.000008 ) -0.012184 0.033516 0.076672 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007175 -0.000007 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000007 0.007140 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000007 0.007144 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3735(11) 8.3944(13) 8.3922(11) 90.058(12) 89.976(11) 89.945(12) V = 589.88(14) OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 OTKP changes: 451 1 1 1 No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 817 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007168 -0.000006 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000006 0.007170 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007626 0.076864 -0.034657 ( 0.000014 0.000013 0.000010 ) -0.083446 -0.011818 -0.008035 ( 0.000010 0.000009 0.000007 ) -0.012120 0.033499 0.076867 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) unit cell: 8.3776(10) 8.3767(12) 8.3742(9) 90.048(10) 90.025(10) 89.952(11) V = 587.67(13) unit cell: 8.3762(3) 8.3762(3) 8.3762(3) 90.0 90.0 90.0 V = 587.67(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 451 obs out of 451 (total:451,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb 3 of 453 peaks identified as outliers and rejected 450 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" 450 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2.tabbin file 450 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.36 | 45 | 0.992 ( 0.159) | 1.248 ( 0.670) | 1.312 ( 0.800) | 1.32- 1.12 | 45 | 1.092 ( 0.083) | 1.159 ( 0.165) | 1.180 ( 0.527) | 1.12- 0.97 | 45 | 1.120 ( 0.082) | 1.158 ( 0.136) | 1.179 ( 0.457) | 0.97- 0.88 | 45 | 1.139 ( 0.081) | 1.163 ( 0.120) | 1.183 ( 0.474) | 0.88- 0.81 | 45 | 1.154 ( 0.075) | 1.139 ( 0.134) | 1.234 ( 0.455) | 0.81- 0.74 | 45 | 1.189 ( 0.061) | 1.141 ( 0.119) | 1.201 ( 0.384) | 0.74- 0.71 | 45 | 1.195 ( 0.067) | 1.208 ( 0.148) | 1.199 ( 0.377) | 0.70- 0.66 | 45 | 1.210 ( 0.059) | 1.191 ( 0.168) | 1.185 ( 0.391) | 0.66- 0.62 | 45 | 1.221 ( 0.083) | 1.202 ( 0.162) | 1.188 ( 0.467) | 0.62- 0.59 | 45 | 1.225 ( 0.088) | 1.211 ( 0.229) | 1.351 ( 0.550) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 450 | 1.154 ( 0.112) | 1.182 ( 0.261) | 1.221 ( 0.505) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) UB fit with 498 obs out of 525 (total:525,skipped:0) (94.86%) UB - matrix: -0.007282 0.076716 -0.035005 ( 0.000024 0.000017 0.000024 ) -0.083572 -0.011755 -0.008084 ( 0.000032 0.000023 0.000032 ) -0.012379 0.033910 0.076863 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007191 0.000004 -0.000021 ( 0.000005 0.000003 0.000003 ) 0.000004 0.007173 0.000016 ( 0.000003 0.000003 0.000003 ) -0.000021 0.000016 0.007199 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(3) 8.3747(19) 8.360(2) 90.13(2) 89.83(3) 90.03(2) V = 585.6(3) OTKP changes: 99 1 1 1 UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) UB - matrix: -0.007143 0.076563 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083362 -0.011573 -0.008134 ( 0.000032 0.000023 0.000032 ) -0.012297 0.033807 0.076634 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007151 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007139 0.000003 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000003 0.007166 ( 0.000003 0.000003 0.000004 ) unit cell: 8.388(3) 8.3950(19) 8.379(2) 90.02(2) 89.89(3) 90.02(2) V = 590.0(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007140 0.076561 -0.035034 ( 0.000023 0.000017 0.000023 ) -0.083355 -0.011569 -0.008131 ( 0.000032 0.000023 0.000032 ) -0.012295 0.033797 0.076633 ( 0.000025 0.000018 0.000025 ) M - matrix: 0.007150 0.000002 -0.000014 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007138 0.000002 ( 0.000003 0.000003 0.000003 ) -0.000014 0.000002 0.007166 ( 0.000003 0.000003 0.000004 ) UB fit with 501 obs out of 525 (total:525,skipped:0) (95.43%) unit cell: 8.388(3) 8.3956(19) 8.379(2) 90.01(2) 89.89(3) 90.02(2) V = 590.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 497 obs out of 525 (total:525,skipped:0) (94.67%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 4 of 443 peaks identified as outliers and rejected 439 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 439 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 439 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.48 | 44 | 1.046 ( 0.251) | 1.216 ( 0.707) | 1.314 ( 0.998) | 1.48- 1.17 | 44 | 1.095 ( 0.152) | 1.085 ( 0.160) | 1.224 ( 0.700) | 1.16- 0.99 | 44 | 1.110 ( 0.077) | 1.082 ( 0.084) | 1.163 ( 0.471) | 0.99- 0.92 | 44 | 1.143 ( 0.066) | 1.106 ( 0.084) | 1.126 ( 0.367) | 0.92- 0.82 | 44 | 1.179 ( 0.068) | 1.107 ( 0.087) | 1.178 ( 0.406) | 0.82- 0.75 | 44 | 1.203 ( 0.052) | 1.098 ( 0.097) | 1.289 ( 0.381) | 0.75- 0.71 | 44 | 1.219 ( 0.054) | 1.088 ( 0.115) | 1.282 ( 0.503) | 0.71- 0.67 | 44 | 1.250 ( 0.054) | 1.133 ( 0.148) | 1.301 ( 0.502) | 0.67- 0.63 | 44 | 1.240 ( 0.063) | 1.117 ( 0.157) | 1.479 ( 0.553) | 0.63- 0.59 | 43 | 1.293 ( 0.070) | 1.112 ( 0.179) | 1.308 ( 0.548) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 439 | 1.178 ( 0.132) | 1.114 ( 0.258) | 1.266 ( 0.579) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 435 obs out of 439 (total:439,skipped:0) (99.09%) UB - matrix: -0.007177 0.076614 -0.035044 ( 0.000014 0.000010 0.000015 ) -0.083509 -0.011618 -0.008175 ( 0.000014 0.000010 0.000015 ) -0.012327 0.034019 0.076649 ( 0.000015 0.000011 0.000016 ) M - matrix: 0.007177 0.000001 -0.000011 ( 0.000002 0.000001 0.000002 ) 0.000001 0.007162 0.000018 ( 0.000001 0.000002 0.000002 ) -0.000011 0.000018 0.007170 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3724(14) 8.3813(12) 8.3767(14) 90.141(13) 89.915(14) 90.008(12) V = 587.81(16) OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 OTKP changes: 437 1 1 1 No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007165 0.000004 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007155 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000007 0.007168 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.007118 0.076641 -0.035011 ( 0.000015 0.000010 0.000015 ) -0.083439 -0.011585 -0.008103 ( 0.000014 0.000010 0.000015 ) -0.012325 0.033865 0.076660 ( 0.000014 0.000010 0.000015 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) unit cell: 8.3798(14) 8.3855(12) 8.3777(13) 90.053(12) 89.844(13) 90.030(13) V = 588.69(16) unit cell: 8.3810(4) 8.3810(4) 8.3810(4) 90.0 90.0 90.0 V = 588.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 437 obs out of 439 (total:439,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb 3 of 438 peaks identified as outliers and rejected 435 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" 435 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3.tabbin file 435 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 44 | 1.056 ( 0.252) | 1.239 ( 0.738) | 1.418 ( 1.089) | 1.48- 1.16 | 44 | 1.070 ( 0.073) | 1.068 ( 0.084) | 1.120 ( 0.507) | 1.12- 0.99 | 44 | 1.121 ( 0.068) | 1.095 ( 0.079) | 1.160 ( 0.444) | 0.99- 0.89 | 44 | 1.152 ( 0.063) | 1.107 ( 0.078) | 1.128 ( 0.367) | 0.89- 0.82 | 44 | 1.178 ( 0.069) | 1.112 ( 0.088) | 1.190 ( 0.412) | 0.82- 0.75 | 44 | 1.208 ( 0.054) | 1.098 ( 0.093) | 1.313 ( 0.388) | 0.75- 0.71 | 44 | 1.218 ( 0.055) | 1.087 ( 0.117) | 1.242 ( 0.512) | 0.71- 0.67 | 44 | 1.243 ( 0.069) | 1.140 ( 0.148) | 1.306 ( 0.501) | 0.67- 0.63 | 44 | 1.252 ( 0.055) | 1.120 ( 0.151) | 1.513 ( 0.518) | 0.63- 0.59 | 39 | 1.290 ( 0.066) | 1.095 ( 0.186) | 1.291 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 435 | 1.178 ( 0.125) | 1.116 ( 0.264) | 1.268 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007464 0.076787 -0.035019 ( 0.000022 0.000029 0.000028 ) -0.083587 -0.011763 -0.008161 ( 0.000021 0.000029 0.000027 ) -0.012123 0.033826 0.076874 ( 0.000019 0.000025 0.000024 ) M - matrix: 0.007189 0.000000 0.000012 ( 0.000004 0.000003 0.000003 ) 0.000000 0.007179 0.000007 ( 0.000003 0.000005 0.000003 ) 0.000012 0.000007 0.007203 ( 0.000003 0.000003 0.000004 ) unit cell: 8.365(2) 8.371(3) 8.358(2) 90.06(2) 90.09(2) 90.00(2) V = 585.3(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) UB - matrix: -0.007478 0.076764 -0.035056 ( 0.000021 0.000029 0.000027 ) -0.083541 -0.011737 -0.008148 ( 0.000021 0.000029 0.000027 ) -0.012066 0.033803 0.076848 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000001 0.000016 ( 0.000004 0.000003 0.000003 ) -0.000001 0.007173 0.000002 ( 0.000003 0.000005 0.000003 ) 0.000016 0.000002 0.007201 ( 0.000003 0.000003 0.000004 ) unit cell: 8.370(2) 8.375(3) 8.359(2) 90.02(2) 90.12(2) 89.99(2) V = 585.9(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 744 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007492 0.076770 -0.035061 ( 0.000021 0.000029 0.000027 ) -0.083543 -0.011736 -0.008139 ( 0.000021 0.000029 0.000027 ) -0.012052 0.033799 0.076841 ( 0.000019 0.000026 0.000024 ) M - matrix: 0.007181 -0.000002 0.000017 ( 0.000004 0.000003 0.000003 ) -0.000002 0.007174 0.000001 ( 0.000003 0.000005 0.000003 ) 0.000017 0.000001 0.007200 ( 0.000003 0.000003 0.000004 ) UB fit with 519 obs out of 575 (total:575,skipped:0) (90.26%) unit cell: 8.370(2) 8.374(3) 8.359(2) 90.01(2) 90.13(2) 89.98(2) V = 586.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 514 obs out of 575 (total:575,skipped:0) (89.39%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 8 of 453 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 445 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 445 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 45 | 1.073 ( 0.295) | 1.226 ( 0.598) | 1.309 ( 0.949) | 1.40- 1.14 | 45 | 1.086 ( 0.095) | 1.263 ( 0.494) | 1.037 ( 0.480) | 1.12- 0.98 | 45 | 1.085 ( 0.083) | 1.127 ( 0.210) | 1.135 ( 0.554) | 0.98- 0.89 | 45 | 1.118 ( 0.076) | 1.127 ( 0.090) | 1.131 ( 0.427) | 0.89- 0.81 | 45 | 1.143 ( 0.078) | 1.152 ( 0.102) | 1.214 ( 0.399) | 0.81- 0.75 | 45 | 1.182 ( 0.072) | 1.121 ( 0.116) | 1.151 ( 0.473) | 0.75- 0.71 | 45 | 1.171 ( 0.067) | 1.161 ( 0.120) | 1.176 ( 0.391) | 0.71- 0.66 | 45 | 1.188 ( 0.065) | 1.106 ( 0.114) | 1.372 ( 0.528) | 0.66- 0.62 | 45 | 1.220 ( 0.070) | 1.171 ( 0.162) | 1.256 ( 0.423) | 0.62- 0.59 | 40 | 1.248 ( 0.087) | 1.104 ( 0.210) | 1.304 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 445 | 1.150 ( 0.132) | 1.156 ( 0.284) | 1.207 ( 0.542) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 441 obs out of 445 (total:445,skipped:0) (99.10%) UB - matrix: -0.007609 0.076885 -0.034986 ( 0.000011 0.000016 0.000016 ) -0.083724 -0.011719 -0.008062 ( 0.000010 0.000014 0.000015 ) -0.012051 0.033823 0.076865 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007213 -0.000011 0.000015 ( 0.000002 0.000001 0.000001 ) -0.000011 0.007193 0.000004 ( 0.000001 0.000003 0.000002 ) 0.000015 0.000004 0.007197 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3518(10) 8.3635(15) 8.3608(12) 90.035(13) 90.119(12) 89.909(12) V = 584.00(15) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007190 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076773 -0.035007 ( 0.000010 0.000014 0.000015 ) -0.083596 -0.011653 -0.008125 ( 0.000009 0.000013 0.000014 ) -0.012070 0.033779 0.076899 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) unit cell: 8.3648(9) 8.3761(14) 8.3564(12) 90.037(13) 90.110(11) 89.922(11) V = 585.48(14) unit cell: 8.3657(4) 8.3657(4) 8.3657(4) 90.0 90.0 90.0 V = 585.48(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 445 (total:445,skipped:0) (99.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb 9 of 450 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" 441 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4.tabbin file 441 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.41 | 44 | 1.055 ( 0.226) | 1.176 ( 0.497) | 1.209 ( 0.730) | 1.41- 1.14 | 44 | 1.077 ( 0.076) | 1.305 ( 0.557) | 1.072 ( 0.477) | 1.12- 0.98 | 44 | 1.081 ( 0.080) | 1.117 ( 0.153) | 1.165 ( 0.512) | 0.98- 0.89 | 44 | 1.124 ( 0.074) | 1.127 ( 0.094) | 1.185 ( 0.461) | 0.89- 0.82 | 44 | 1.146 ( 0.074) | 1.152 ( 0.111) | 1.139 ( 0.378) | 0.82- 0.76 | 44 | 1.170 ( 0.083) | 1.130 ( 0.152) | 1.171 ( 0.384) | 0.75- 0.71 | 44 | 1.176 ( 0.069) | 1.164 ( 0.122) | 1.194 ( 0.421) | 0.71- 0.67 | 44 | 1.189 ( 0.061) | 1.128 ( 0.136) | 1.382 ( 0.518) | 0.67- 0.63 | 44 | 1.212 ( 0.071) | 1.166 ( 0.149) | 1.259 ( 0.425) | 0.63- 0.59 | 45 | 1.234 ( 0.079) | 1.122 ( 0.209) | 1.248 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.147 ( 0.116) | 1.159 ( 0.274) | 1.202 ( 0.491) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) UB fit with 537 obs out of 566 (total:566,skipped:0) (94.88%) UB - matrix: -0.007583 0.076983 -0.034576 ( 0.000030 0.000029 0.000025 ) -0.083561 -0.011987 -0.008104 ( 0.000020 0.000019 0.000016 ) -0.012164 0.033312 0.076985 ( 0.000026 0.000025 0.000021 ) M - matrix: 0.007188 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007180 -0.000000 ( 0.000003 0.000005 0.000003 ) 0.000003 -0.000000 0.007188 ( 0.000003 0.000003 0.000004 ) unit cell: 8.366(2) 8.371(3) 8.366(2) 90.00(2) 90.02(2) 90.10(2) V = 585.9(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) OTKP changes: 108 1 1 1 UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 790 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007563 0.076786 -0.034569 ( 0.000030 0.000029 0.000025 ) -0.083436 -0.011928 -0.008194 ( 0.000019 0.000019 0.000016 ) -0.012160 0.033290 0.076805 ( 0.000024 0.000024 0.000020 ) M - matrix: 0.007167 0.000010 0.000011 ( 0.000003 0.000003 0.000003 ) 0.000010 0.007147 0.000000 ( 0.000003 0.000005 0.000003 ) 0.000011 0.000000 0.007161 ( 0.000003 0.000003 0.000004 ) UB fit with 539 obs out of 566 (total:566,skipped:0) (95.23%) unit cell: 8.3786(19) 8.390(3) 8.382(2) 90.00(2) 90.09(2) 90.08(2) V = 589.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 540 obs out of 566 (total:566,skipped:0) (95.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 5 of 477 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 472 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 472 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.41 | 47 | 1.016 ( 0.147) | 1.188 ( 0.546) | 1.381 ( 1.135) | 1.41- 1.17 | 47 | 1.084 ( 0.105) | 1.194 ( 0.453) | 1.055 ( 0.469) | 1.16- 0.99 | 47 | 1.087 ( 0.065) | 1.178 ( 0.375) | 1.202 ( 0.517) | 0.98- 0.92 | 47 | 1.125 ( 0.049) | 1.111 ( 0.105) | 1.100 ( 0.425) | 0.92- 0.82 | 47 | 1.158 ( 0.044) | 1.101 ( 0.100) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.172 ( 0.046) | 1.102 ( 0.111) | 1.251 ( 0.465) | 0.75- 0.71 | 47 | 1.172 ( 0.031) | 1.073 ( 0.125) | 1.238 ( 0.488) | 0.71- 0.67 | 47 | 1.195 ( 0.050) | 1.121 ( 0.141) | 1.199 ( 0.401) | 0.67- 0.63 | 47 | 1.183 ( 0.072) | 1.159 ( 0.154) | 1.186 ( 0.480) | 0.63- 0.59 | 49 | 1.227 ( 0.071) | 1.143 ( 0.181) | 1.232 ( 0.523) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 472 | 1.142 ( 0.097) | 1.137 ( 0.280) | 1.205 ( 0.583) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 469 obs out of 472 (total:472,skipped:0) (99.36%) UB - matrix: -0.007661 0.076944 -0.034660 ( 0.000014 0.000013 0.000012 ) -0.083527 -0.011998 -0.008029 ( 0.000012 0.000011 0.000010 ) -0.012250 0.033326 0.076825 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007186 0.000004 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007175 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000005 -0.000010 0.007168 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3676(12) 8.3738(12) 8.3779(11) 89.918(11) 89.960(11) 90.036(12) V = 587.03(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.094) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007167 0.000006 0.000008 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007157 -0.000003 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000003 0.007170 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007567 0.076856 -0.034598 ( 0.000013 0.000012 0.000011 ) -0.083436 -0.011905 -0.008180 ( 0.000010 0.000009 0.000008 ) -0.012180 0.033299 0.076851 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007165 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007165 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007165 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) unit cell: 8.3783(10) 8.3840(12) 8.3766(10) 89.979(11) 90.066(10) 90.049(11) V = 588.40(13) unit cell: 8.3796(4) 8.3796(4) 8.3796(4) 90.0 90.0 90.0 V = 588.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb 4 of 470 peaks identified as outliers and rejected 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" 466 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5.tabbin file 466 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.41 | 47 | 1.014 ( 0.148) | 1.155 ( 0.520) | 1.304 ( 1.083) | 1.41- 1.17 | 47 | 1.070 ( 0.082) | 1.184 ( 0.407) | 1.103 ( 0.638) | 1.17- 0.99 | 47 | 1.090 ( 0.075) | 1.195 ( 0.404) | 1.193 ( 0.533) | 0.99- 0.92 | 47 | 1.129 ( 0.048) | 1.113 ( 0.107) | 1.074 ( 0.409) | 0.92- 0.82 | 47 | 1.155 ( 0.051) | 1.115 ( 0.115) | 1.172 ( 0.487) | 0.82- 0.75 | 47 | 1.172 ( 0.041) | 1.087 ( 0.095) | 1.275 ( 0.456) | 0.75- 0.71 | 47 | 1.173 ( 0.033) | 1.085 ( 0.130) | 1.200 ( 0.423) | 0.71- 0.67 | 47 | 1.192 ( 0.050) | 1.136 ( 0.152) | 1.161 ( 0.381) | 0.67- 0.62 | 47 | 1.194 ( 0.073) | 1.168 ( 0.159) | 1.199 ( 0.479) | 0.62- 0.59 | 43 | 1.225 ( 0.072) | 1.145 ( 0.178) | 1.288 ( 0.574) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 466 | 1.141 ( 0.097) | 1.138 ( 0.273) | 1.196 ( 0.584) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 45 | 0.995 ( 0.138) | 1.194 ( 0.672) | 1.218 ( 0.727) | 1.41- 1.17 | 45 | 1.059 ( 0.066) | 1.210 ( 0.429) | 1.136 ( 0.493) | 1.17- 1.02 | 45 | 1.091 ( 0.060) | 1.092 ( 0.095) | 1.061 ( 0.436) | 1.02- 0.92 | 45 | 1.099 ( 0.078) | 1.063 ( 0.127) | 1.140 ( 0.418) | 0.92- 0.84 | 45 | 1.137 ( 0.065) | 1.099 ( 0.100) | 1.172 ( 0.458) | 0.84- 0.76 | 45 | 1.160 ( 0.076) | 1.113 ( 0.125) | 1.151 ( 0.435) | 0.76- 0.72 | 45 | 1.170 ( 0.039) | 1.108 ( 0.114) | 1.209 ( 0.405) | 0.72- 0.67 | 45 | 1.180 ( 0.037) | 1.097 ( 0.137) | 1.305 ( 0.496) | 0.67- 0.63 | 45 | 1.188 ( 0.051) | 1.117 ( 0.150) | 1.256 ( 0.449) | 0.63- 0.59 | 49 | 1.205 ( 0.064) | 1.094 ( 0.152) | 1.338 ( 0.509) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 454 | 1.129 ( 0.096) | 1.118 ( 0.279) | 1.200 ( 0.497) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) UB fit with 445 obs out of 487 (total:487,skipped:0) (91.38%) UB - matrix: -0.007446 0.076768 -0.035036 ( 0.000029 0.000037 0.000026 ) -0.083568 -0.011786 -0.008055 ( 0.000021 0.000027 0.000019 ) -0.012156 0.033570 0.076810 ( 0.000025 0.000032 0.000023 ) M - matrix: 0.007187 0.000005 0.000000 ( 0.000004 0.000003 0.000003 ) 0.000005 0.007159 -0.000016 ( 0.000003 0.000006 0.000004 ) 0.000000 -0.000016 0.007192 ( 0.000003 0.000004 0.000004 ) unit cell: 8.367(2) 8.383(3) 8.364(3) 89.87(3) 90.00(2) 90.04(3) V = 586.6(3) OTKP changes: 94 1 1 1 UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) 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 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.307) HKL list info: 707 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.007338 0.076440 -0.034773 ( 0.000028 0.000035 0.000025 ) -0.083234 -0.011572 -0.008110 ( 0.000021 0.000026 0.000019 ) -0.012191 0.033290 0.076520 ( 0.000023 0.000029 0.000021 ) M - matrix: 0.007130 -0.000004 -0.000003 ( 0.000004 0.000003 0.000003 ) -0.000004 0.007085 -0.000017 ( 0.000003 0.000006 0.000003 ) -0.000003 -0.000017 0.007130 ( 0.000003 0.000003 0.000004 ) UB fit with 455 obs out of 487 (total:487,skipped:0) (93.43%) unit cell: 8.400(2) 8.427(3) 8.400(2) 89.86(3) 89.98(2) 89.97(2) V = 594.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 457 obs out of 487 (total:487,skipped:0) (93.84%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 1 of 419 peaks identified as outliers and rejected 418 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 418 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 418 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.42 | 42 | 1.093 ( 0.273) | 1.325 ( 0.679) | 1.498 ( 1.008) | 1.42- 1.17 | 42 | 1.077 ( 0.066) | 1.144 ( 0.405) | 1.094 ( 0.487) | 1.17- 0.99 | 42 | 1.098 ( 0.065) | 1.070 ( 0.105) | 1.114 ( 0.480) | 0.99- 0.92 | 42 | 1.140 ( 0.048) | 1.099 ( 0.110) | 1.080 ( 0.426) | 0.92- 0.82 | 42 | 1.171 ( 0.047) | 1.098 ( 0.111) | 1.244 ( 0.490) | 0.82- 0.76 | 42 | 1.178 ( 0.059) | 1.079 ( 0.121) | 1.263 ( 0.485) | 0.76- 0.71 | 42 | 1.207 ( 0.058) | 1.096 ( 0.157) | 1.313 ( 0.450) | 0.71- 0.67 | 42 | 1.212 ( 0.066) | 1.118 ( 0.133) | 1.335 ( 0.459) | 0.67- 0.63 | 42 | 1.213 ( 0.079) | 1.199 ( 0.128) | 1.310 ( 0.450) | 0.63- 0.59 | 40 | 1.251 ( 0.107) | 1.125 ( 0.120) | 1.547 ( 0.592) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 418 | 1.164 ( 0.122) | 1.135 ( 0.284) | 1.279 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 415 obs out of 418 (total:418,skipped:0) (99.28%) UB - matrix: -0.007354 0.076558 -0.034855 ( 0.000014 0.000017 0.000013 ) -0.083297 -0.011621 -0.008117 ( 0.000012 0.000014 0.000011 ) -0.011999 0.033378 0.076669 ( 0.000014 0.000017 0.000013 ) M - matrix: 0.007136 0.000004 0.000012 ( 0.000002 0.000002 0.000001 ) 0.000004 0.007110 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000012 -0.000015 0.007159 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3964(12) 8.4117(16) 8.3831(14) 89.879(14) 90.100(12) 90.036(13) V = 592.08(17) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=53.002) HKL list info: 703 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007141 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000007 0.007191 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007473 0.076663 -0.034970 ( 0.000013 0.000016 0.000012 ) -0.083541 -0.011726 -0.008149 ( 0.000012 0.000014 0.000011 ) -0.012251 0.033560 0.076821 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) unit cell: 8.3679(12) 8.3937(15) 8.3646(13) 89.943(13) 90.008(12) 89.965(13) V = 587.51(16) unit cell: 8.3754(3) 8.3754(3) 8.3754(3) 90.0 90.0 90.0 V = 587.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 418 obs out of 418 (total:418,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.rpb 3 of 420 peaks identified as outliers and rejected 417 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" 417 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7.tabbin file 417 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 42 | 1.065 ( 0.164) | 1.299 ( 0.681) | 1.465 ( 0.960) | 1.41- 1.17 | 42 | 1.085 ( 0.067) | 1.159 ( 0.376) | 1.063 ( 0.455) | 1.17- 0.98 | 42 | 1.104 ( 0.068) | 1.081 ( 0.108) | 1.141 ( 0.463) | 0.98- 0.92 | 42 | 1.145 ( 0.044) | 1.099 ( 0.103) | 1.097 ( 0.417) | 0.92- 0.82 | 42 | 1.172 ( 0.053) | 1.097 ( 0.119) | 1.207 ( 0.493) | 0.82- 0.76 | 42 | 1.182 ( 0.066) | 1.088 ( 0.124) | 1.323 ( 0.462) | 0.76- 0.71 | 42 | 1.209 ( 0.056) | 1.100 ( 0.155) | 1.304 ( 0.443) | 0.71- 0.67 | 42 | 1.214 ( 0.069) | 1.131 ( 0.134) | 1.371 ( 0.474) | 0.67- 0.62 | 42 | 1.225 ( 0.076) | 1.206 ( 0.140) | 1.310 ( 0.480) | 0.62- 0.59 | 39 | 1.253 ( 0.105) | 1.137 ( 0.127) | 1.584 ( 0.582) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 417 | 1.165 ( 0.103) | 1.140 ( 0.279) | 1.284 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 8 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1715a\tmp\xs1715a_back_8_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1715a\tmp\xs1715a_back_8_76.rpb PROFFITPEAK info: 984 peaks in the peak location table UB fit with 473 obs out of 503 (total:503,skipped:0) (94.04%) UB - matrix: -0.007523 0.076859 -0.035184 ( 0.000023 0.000024 0.000022 ) -0.083592 -0.011681 -0.008141 ( 0.000028 0.000029 0.000027 ) -0.012291 0.033845 0.076634 ( 0.000024 0.000024 0.000023 ) M - matrix: 0.007195 -0.000018 0.000003 ( 0.000005 0.000003 0.000003 ) -0.000018 0.007189 -0.000016 ( 0.000003 0.000004 0.000003 ) 0.000003 -0.000016 0.007177 ( 0.000003 0.000003 0.000004 ) unit cell: 8.362(3) 8.365(2) 8.373(2) 89.88(2) 90.03(2) 89.86(2) V = 585.7(3) UB fit with 473 obs out of 503 (total:503,skipped:0) (94.04%) UB - matrix: -0.007523 0.076859 -0.035184 ( 0.000023 0.000024 0.000022 ) -0.083592 -0.011681 -0.008141 ( 0.000028 0.000029 0.000027 ) -0.012291 0.033845 0.076634 ( 0.000024 0.000024 0.000023 ) M - matrix: 0.007195 -0.000018 0.000003 ( 0.000005 0.000003 0.000003 ) -0.000018 0.007189 -0.000016 ( 0.000003 0.000004 0.000003 ) 0.000003 -0.000016 0.007177 ( 0.000003 0.000003 0.000004 ) unit cell: 8.362(3) 8.365(2) 8.373(2) 89.88(2) 90.03(2) 89.86(2) V = 585.7(3) OTKP changes: 97 1 1 1 No constraint UB - matrix: -0.007386 0.076613 -0.035093 ( 0.000022 0.000022 0.000021 ) -0.083285 -0.011683 -0.008308 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033845 0.076390 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007145 -0.000012 0.000004 ( 0.000005 0.000003 0.000003 ) -0.000012 0.007151 -0.000006 ( 0.000003 0.000004 0.000003 ) 0.000004 -0.000006 0.007136 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007386 0.076613 -0.035093 ( 0.000022 0.000022 0.000021 ) -0.083285 -0.011683 -0.008308 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033845 0.076390 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007141 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007141 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007141 ( 0.000000 0.000000 0.000001 ) UB fit with 476 obs out of 503 (total:503,skipped:0) (94.63%) unit cell: 8.392(3) 8.387(2) 8.397(2) 89.95(2) 90.03(2) 89.90(2) V = 591.0(3) unit cell: 8.3919(5) 8.3919(5) 8.3919(5) 90.0 90.0 90.0 V = 590.98(7) UB fit with 476 obs out of 503 (total:503,skipped:0) (94.63%) UB - matrix: -0.007386 0.076613 -0.035093 ( 0.000022 0.000022 0.000021 ) -0.083285 -0.011683 -0.008308 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033845 0.076390 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007145 -0.000012 0.000004 ( 0.000005 0.000003 0.000003 ) -0.000012 0.007151 -0.000006 ( 0.000003 0.000004 0.000003 ) 0.000004 -0.000006 0.007136 ( 0.000003 0.000003 0.000004 ) unit cell: 8.392(3) 8.387(2) 8.397(2) 89.95(2) 90.03(2) 89.90(2) V = 591.0(3) OTKP changes: 97 1 1 1 No constraint UB - matrix: -0.007378 0.076607 -0.035090 ( 0.000022 0.000022 0.000021 ) -0.083271 -0.011679 -0.008314 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033846 0.076375 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007142 -0.000012 0.000004 ( 0.000005 0.000003 0.000003 ) -0.000012 0.007151 -0.000006 ( 0.000003 0.000004 0.000003 ) 0.000004 -0.000006 0.007133 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007378 0.076607 -0.035090 ( 0.000022 0.000022 0.000021 ) -0.083271 -0.011679 -0.008314 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033846 0.076375 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007139 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007139 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007139 ( 0.000000 0.000000 0.000001 ) UB fit with 476 obs out of 503 (total:503,skipped:0) (94.63%) unit cell: 8.393(3) 8.388(2) 8.398(2) 89.95(2) 90.04(2) 89.90(2) V = 591.2(3) unit cell: 8.3930(5) 8.3930(5) 8.3930(5) 90.0 90.0 90.0 V = 591.22(7) 503 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Run 8 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=53.207) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007378 0.076607 -0.035090 ( 0.000022 0.000022 0.000021 ) -0.083271 -0.011679 -0.008314 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033846 0.076375 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007142 -0.000012 0.000004 ( 0.000005 0.000003 0.000003 ) -0.000012 0.007151 -0.000006 ( 0.000003 0.000004 0.000003 ) 0.000004 -0.000006 0.007133 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.007378 0.076607 -0.035090 ( 0.000022 0.000022 0.000021 ) -0.083271 -0.011679 -0.008314 ( 0.000029 0.000029 0.000027 ) -0.012397 0.033846 0.076375 ( 0.000023 0.000023 0.000022 ) M - matrix: 0.007139 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007139 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007139 ( 0.000000 0.000000 0.000001 ) UB fit with 476 obs out of 503 (total:503,skipped:0) (94.63%) unit cell: 8.393(3) 8.388(2) 8.398(2) 89.95(2) 90.04(2) 89.90(2) V = 591.2(3) unit cell: 8.3930(5) 8.3930(5) 8.3930(5) 90.0 90.0 90.0 V = 591.22(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 478 obs out of 503 (total:503,skipped:0) (95.03%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_76.rpb 4 of 441 peaks identified as outliers and rejected 437 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 437 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 437 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.60 | 44 | 1.035 ( 0.245) | 1.275 ( 0.738) | 1.495 ( 1.020) | 1.60- 1.17 | 44 | 1.057 ( 0.062) | 1.111 ( 0.258) | 1.096 ( 0.470) | 1.17- 0.99 | 44 | 1.106 ( 0.061) | 1.074 ( 0.087) | 1.098 ( 0.496) | 0.99- 0.92 | 44 | 1.122 ( 0.063) | 1.096 ( 0.093) | 1.185 ( 0.509) | 0.92- 0.82 | 44 | 1.138 ( 0.063) | 1.082 ( 0.102) | 1.190 ( 0.498) | 0.82- 0.76 | 44 | 1.175 ( 0.081) | 1.075 ( 0.096) | 1.216 ( 0.409) | 0.76- 0.71 | 44 | 1.174 ( 0.056) | 1.107 ( 0.086) | 1.207 ( 0.473) | 0.71- 0.67 | 44 | 1.167 ( 0.067) | 1.055 ( 0.074) | 1.192 ( 0.395) | 0.66- 0.63 | 44 | 1.198 ( 0.072) | 1.124 ( 0.135) | 1.222 ( 0.499) | 0.63- 0.59 | 41 | 1.239 ( 0.120) | 1.108 ( 0.155) | 1.317 ( 0.510) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 437 | 1.140 ( 0.120) | 1.111 ( 0.272) | 1.221 ( 0.565) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 434 obs out of 437 (total:437,skipped:0) (99.31%) UB - matrix: -0.007453 0.076634 -0.035128 ( 0.000012 0.000013 0.000011 ) -0.083453 -0.011702 -0.008296 ( 0.000012 0.000013 0.000011 ) -0.012405 0.033715 0.076550 ( 0.000014 0.000015 0.000013 ) M - matrix: 0.007174 -0.000013 0.000005 ( 0.000002 0.000002 0.000002 ) -0.000013 0.007146 -0.000014 ( 0.000002 0.000002 0.000002 ) 0.000005 -0.000014 0.007163 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3744(12) 8.3905(13) 8.3810(13) 89.888(13) 90.036(12) 89.898(12) V = 588.89(15) OTKP changes: 434 1 1 1 No constraint UB - matrix: -0.007527 0.076827 -0.035277 ( 0.000011 0.000012 0.000011 ) -0.083597 -0.011815 -0.008239 ( 0.000012 0.000013 0.000011 ) -0.012345 0.033989 0.076679 ( 0.000013 0.000014 0.000012 ) M - matrix: 0.007198 -0.000010 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007197 -0.000007 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000007 0.007192 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007527 0.076827 -0.035277 ( 0.000011 0.000012 0.000011 ) -0.083597 -0.011815 -0.008239 ( 0.000012 0.000013 0.000011 ) -0.012345 0.033989 0.076679 ( 0.000013 0.000014 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) unit cell: 8.3606(12) 8.3608(12) 8.3638(12) 89.948(12) 90.061(11) 89.919(11) V = 584.64(14) unit cell: 8.3617(3) 8.3617(3) 8.3617(3) 90.0 90.0 90.0 V = 584.64(4) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.931) HKL list info: 738 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007527 0.076827 -0.035277 ( 0.000011 0.000012 0.000011 ) -0.083597 -0.011815 -0.008239 ( 0.000012 0.000013 0.000011 ) -0.012345 0.033989 0.076679 ( 0.000013 0.000014 0.000012 ) M - matrix: 0.007198 -0.000010 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007197 -0.000007 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000007 0.007192 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007527 0.076827 -0.035277 ( 0.000011 0.000012 0.000011 ) -0.083597 -0.011815 -0.008239 ( 0.000012 0.000013 0.000011 ) -0.012345 0.033989 0.076679 ( 0.000013 0.000014 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) unit cell: 8.3606(12) 8.3608(12) 8.3638(12) 89.948(12) 90.061(11) 89.919(11) V = 584.64(14) unit cell: 8.3617(3) 8.3617(3) 8.3617(3) 90.0 90.0 90.0 V = 584.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_76.rpb 3 of 435 peaks identified as outliers and rejected 432 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" 432 peaks saved into the D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8.tabbin file 432 profiles saved into the file D:\Data\xs1715a\tmp\xs1715a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.60 | 43 | 1.061 ( 0.292) | 1.314 ( 0.751) | 1.553 ( 1.124) | 1.60- 1.17 | 43 | 1.067 ( 0.063) | 1.141 ( 0.328) | 1.095 ( 0.461) | 1.17- 1.02 | 43 | 1.107 ( 0.067) | 1.077 ( 0.094) | 1.110 ( 0.495) | 1.02- 0.92 | 43 | 1.120 ( 0.062) | 1.102 ( 0.086) | 1.158 ( 0.520) | 0.92- 0.82 | 43 | 1.141 ( 0.069) | 1.064 ( 0.099) | 1.213 ( 0.485) | 0.82- 0.76 | 43 | 1.171 ( 0.079) | 1.088 ( 0.098) | 1.223 ( 0.413) | 0.76- 0.72 | 43 | 1.188 ( 0.059) | 1.107 ( 0.093) | 1.188 ( 0.496) | 0.72- 0.67 | 43 | 1.174 ( 0.069) | 1.067 ( 0.079) | 1.151 ( 0.378) | 0.67- 0.64 | 43 | 1.188 ( 0.073) | 1.129 ( 0.128) | 1.246 ( 0.473) | 0.64- 0.59 | 45 | 1.236 ( 0.114) | 1.082 ( 0.145) | 1.372 ( 0.567) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 432 | 1.146 ( 0.128) | 1.117 ( 0.284) | 1.232 ( 0.592) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.1 | 354 | 1.143 ( 0.107) | 1.230 ( 0.389) | 1.279 ( 0.624) | 13.1-18.6 | 354 | 1.135 ( 0.100) | 1.179 ( 0.300) | 1.274 ( 0.608) | 18.6-22.8 | 354 | 1.145 ( 0.091) | 1.197 ( 0.324) | 1.294 ( 0.676) | 22.8-27.1 | 354 | 1.132 ( 0.096) | 1.157 ( 0.277) | 1.222 ( 0.572) | 27.2-30.3 | 354 | 1.132 ( 0.101) | 1.143 ( 0.253) | 1.198 ( 0.454) | 30.4-33.6 | 354 | 1.145 ( 0.097) | 1.129 ( 0.214) | 1.199 ( 0.444) | 33.6-37.0 | 354 | 1.144 ( 0.097) | 1.117 ( 0.197) | 1.162 ( 0.429) | 37.0-39.7 | 354 | 1.149 ( 0.113) | 1.087 ( 0.194) | 1.240 ( 0.516) | 39.7-42.7 | 354 | 1.166 ( 0.112) | 1.100 ( 0.240) | 1.213 ( 0.524) | 42.7-50.5 | 357 | 1.212 ( 0.157) | 1.118 ( 0.264) | 1.248 ( 0.548) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.5 | 3543 | 1.150 ( 0.111) | 1.146 ( 0.275) | 1.233 ( 0.547) | Fitted profile normalization line parameters e1 dimension: a=0.0021 b=0.96 e2 dimension: a=-0.0012 b=1.02 e3 dimension: a=-0.0021 b=1.10 Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_peakhunt_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_peakhunt" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7173 lp-corr: 5347 Maximum peak integral for reflections I/sig<= 100 - raw: 464571 lp-corr: 681622 Maximum peak integral for reflections I/sig<= 10000 - raw: 22003060 lp-corr: 2856462 PROFFITPEAK - Finished at Wed Mar 28 15:13:38 2018 PROFFITMAIN - Started at Wed Mar 28 15:13:38 2018 OTKP changes: 3527 2 4 7 OTKP changes: 3527 2 4 7 OTKP changes: 3527 2 4 7 No constraint UB - matrix: -0.007467 0.076862 -0.034876 ( 0.000006 0.000006 0.000005 ) -0.083574 -0.011759 -0.008081 ( 0.000004 0.000004 0.000004 ) -0.012119 0.033668 0.076938 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007187 0.000001 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007180 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000005 0.007201 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007467 0.076862 -0.034876 ( 0.000006 0.000006 0.000005 ) -0.083574 -0.011759 -0.008081 ( 0.000004 0.000004 0.000004 ) -0.012119 0.033668 0.076938 ( 0.000006 0.000005 0.000005 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000000 ) UB fit with 3532 obs out of 3543 (total:3543,skipped:0) (99.69%) unit cell: 8.3666(4) 8.3711(5) 8.3586(5) 90.038(5) 90.027(4) 90.007(5) V = 585.41(6) unit cell: 8.36541(13) 8.36541(13) 8.36541(13) 90.0 90.0 90.0 V = 585.411(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= -30.93 ka= -77.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) UB - matrix: -0.007471 0.076921 -0.034752 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011772 -0.008084 ( 0.000009 0.000010 0.000008 ) -0.012186 0.033611 0.076900 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000000 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000000 0.007185 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000002 0.000007 0.007187 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3653(9) 8.3678(12) 8.3669(11) 90.053(11) 89.985(10) 89.997(10) V = 585.68(13) OTKP changes: 447 1 1 1 No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007189 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007187 0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 0.000007 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007479 0.076933 -0.034755 ( 0.000012 0.000013 0.000011 ) -0.083577 -0.011769 -0.008082 ( 0.000009 0.000010 0.000008 ) -0.012176 0.033614 0.076915 ( 0.000011 0.000012 0.000010 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3654(9) 8.3667(12) 8.3655(11) 90.053(11) 89.991(10) 89.992(10) V = 585.51(13) unit cell: 8.3659(3) 8.3659(3) 8.3659(3) 90.0 90.0 90.0 V = 585.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007191 -0.000001 0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007183 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000000 0.000003 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084800 -0.000003 -0.000002 ( 0.000009 0.000010 0.000008 ) -0.000009 0.084752 0.000064 ( 0.000012 0.000013 0.000011 ) 0.000002 -0.000030 0.084781 ( 0.000010 0.000011 0.000009 ) M - matrix: 0.007188 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007188 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007188 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 448 (total:448,skipped:0) (99.78%) unit cell: 8.3643(9) 8.3691(13) 8.3662(9) 90.023(11) 90.000(9) 89.992(11) V = 585.65(13) unit cell: 8.3666(3) 8.3666(3) 8.3666(3) 90.0 90.0 90.0 V = 585.65(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -30.93 ka= -77.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) UB - matrix: -0.007620 0.076874 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083451 -0.011820 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012123 0.033502 0.076869 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007172 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3771(11) 8.3756(13) 8.3741(10) 90.048(11) 90.021(10) 89.956(12) V = 587.56(13) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007169 -0.000006 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000006 0.007171 0.000006 ( 0.000002 0.000002 0.000001 ) 0.000003 0.000006 0.007174 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007619 0.076871 -0.034657 ( 0.000016 0.000014 0.000011 ) -0.083452 -0.011819 -0.008034 ( 0.000011 0.000010 0.000007 ) -0.012124 0.033503 0.076865 ( 0.000012 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 450 (total:450,skipped:0) (100.00%) unit cell: 8.3770(11) 8.3759(13) 8.3744(10) 90.048(11) 90.021(10) 89.956(12) V = 587.59(13) unit cell: 8.3758(4) 8.3758(4) 8.3758(4) 90.0 90.0 90.0 V = 587.59(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_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= -30.93 ka= -77.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_2_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_2_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_2_85.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) UB - matrix: -0.007134 0.076648 -0.035001 ( 0.000014 0.000010 0.000015 ) -0.083450 -0.011578 -0.008110 ( 0.000014 0.000010 0.000015 ) -0.012327 0.033870 0.076670 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007167 0.000002 -0.000019 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007156 0.000008 ( 0.000001 0.000002 0.000002 ) -0.000019 0.000008 0.007169 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3785(13) 8.3848(12) 8.3773(14) 90.064(12) 89.851(13) 90.015(12) V = 588.52(16) OTKP changes: 433 1 1 1 OTKP changes: 433 1 1 1 OTKP changes: 433 1 1 1 No constraint UB - matrix: -0.007131 0.076659 -0.034992 ( 0.000014 0.000010 0.000015 ) -0.083451 -0.011579 -0.008102 ( 0.000014 0.000010 0.000015 ) -0.012331 0.033858 0.076672 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007167 0.000002 -0.000020 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007157 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000020 0.000007 0.007169 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007131 0.076659 -0.034992 ( 0.000014 0.000010 0.000015 ) -0.083451 -0.011579 -0.008102 ( 0.000014 0.000010 0.000015 ) -0.012331 0.033858 0.076672 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007163 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007163 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007163 ( 0.000000 0.000000 0.000001 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3785(13) 8.3843(12) 8.3775(14) 90.058(12) 89.842(13) 90.018(12) V = 588.50(16) unit cell: 8.3801(4) 8.3801(4) 8.3801(4) 90.0 90.0 90.0 V = 588.50(4) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) HKL list info: 729 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007131 0.076659 -0.034992 ( 0.000014 0.000010 0.000015 ) -0.083451 -0.011579 -0.008102 ( 0.000014 0.000010 0.000015 ) -0.012331 0.033858 0.076672 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007167 0.000002 -0.000020 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007157 0.000007 ( 0.000001 0.000002 0.000002 ) -0.000020 0.000007 0.007169 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.007131 0.076659 -0.034992 ( 0.000014 0.000010 0.000015 ) -0.083451 -0.011579 -0.008102 ( 0.000014 0.000010 0.000015 ) -0.012331 0.033858 0.076672 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007163 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007163 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007163 ( 0.000000 0.000000 0.000001 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3785(13) 8.3843(12) 8.3775(14) 90.058(12) 89.842(13) 90.018(12) V = 588.50(16) unit cell: 8.3801(4) 8.3801(4) 8.3801(4) 90.0 90.0 90.0 V = 588.50(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: 0.084530 0.000134 -0.000188 ( 0.000016 0.000011 0.000017 ) -0.000010 0.084641 0.000000 ( 0.000012 0.000009 0.000013 ) 0.000002 0.000000 0.084643 ( 0.000009 0.000007 0.000010 ) M - matrix: 0.007145 0.000010 -0.000016 ( 0.000003 0.000001 0.000002 ) 0.000010 0.007164 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000016 0.000000 0.007164 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.084530 0.000134 -0.000188 ( 0.000016 0.000011 0.000017 ) -0.000010 0.084641 0.000000 ( 0.000012 0.000009 0.000013 ) 0.000002 0.000000 0.084643 ( 0.000009 0.000007 0.000010 ) M - matrix: 0.007163 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007163 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007163 ( 0.000000 0.000000 0.000001 ) UB fit with 433 obs out of 435 (total:435,skipped:0) (99.54%) unit cell: 8.3912(16) 8.3801(8) 8.3799(10) 90.000(10) 89.874(13) 90.084(11) V = 589.27(14) unit cell: 8.3837(4) 8.3837(4) 8.3837(4) 90.0 90.0 90.0 V = 589.27(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -60.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_3_76.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) UB - matrix: -0.007509 0.076770 -0.035010 ( 0.000009 0.000013 0.000014 ) -0.083603 -0.011659 -0.008128 ( 0.000009 0.000013 0.000014 ) -0.012075 0.033778 0.076899 ( 0.000008 0.000012 0.000012 ) M - matrix: 0.007192 -0.000010 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000010 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007205 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3641(9) 8.3764(13) 8.3561(12) 90.037(12) 90.111(11) 89.923(11) V = 585.44(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) HKL list info: 734 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007192 -0.000009 0.000014 ( 0.000002 0.000001 0.000001 ) -0.000009 0.007171 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000014 0.000005 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007504 0.076770 -0.035008 ( 0.000009 0.000013 0.000014 ) -0.083605 -0.011659 -0.008133 ( 0.000010 0.000014 0.000015 ) -0.012081 0.033779 0.076903 ( 0.000008 0.000012 0.000013 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 441 (total:441,skipped:0) (99.77%) unit cell: 8.3638(10) 8.3763(13) 8.3559(12) 90.040(12) 90.108(11) 89.924(11) V = 585.40(14) unit cell: 8.3653(4) 8.3653(4) 8.3653(4) 90.0 90.0 90.0 V = 585.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007191 -0.000008 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000008 0.007176 0.000008 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000008 0.007206 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.084797 -0.000093 0.000204 ( 0.000009 0.000014 0.000014 ) -0.000000 0.084711 0.000096 ( 0.000010 0.000014 0.000015 ) -0.000005 0.000001 0.084890 ( 0.000006 0.000009 0.000009 ) M - matrix: 0.007189 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007189 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007189 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 441 (total:441,skipped:0) (99.55%) unit cell: 8.3647(9) 8.3732(14) 8.3555(9) 90.066(12) 90.134(11) 89.937(11) V = 585.21(13) unit cell: 8.3644(4) 8.3644(4) 8.3644(4) 90.0 90.0 90.0 V = 585.21(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 56.87 ph= 90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_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\xs1715a\tmp\xs1715a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_4_76.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) UB - matrix: -0.007585 0.076981 -0.034611 ( 0.000014 0.000013 0.000012 ) -0.083462 -0.011905 -0.008133 ( 0.000012 0.000011 0.000010 ) -0.012247 0.033284 0.076932 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007173 0.000002 -0.000001 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007176 -0.000007 ( 0.000001 0.000002 0.000001 ) -0.000001 -0.000007 0.007183 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3746(11) 8.3734(13) 8.3693(11) 89.944(11) 89.993(11) 90.017(12) V = 586.89(14) OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 OTKP changes: 465 1 1 1 No constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007180 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007173 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007179 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3711(11) 8.3749(12) 8.3714(10) 89.999(11) 90.052(10) 90.086(11) V = 586.89(13) unit cell: 8.3724(4) 8.3724(4) 8.3724(4) 90.0 90.0 90.0 V = 586.89(4) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.022) HKL list info: 780 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007180 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007173 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007179 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3711(11) 8.3749(12) 8.3714(10) 89.999(11) 90.052(10) 90.086(11) V = 586.89(13) unit cell: 8.3724(4) 8.3724(4) 8.3724(4) 90.0 90.0 90.0 V = 586.89(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007180 0.000011 0.000007 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007173 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000000 0.007179 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.007563 0.076947 -0.034567 ( 0.000013 0.000012 0.000011 ) -0.083514 -0.011947 -0.008149 ( 0.000011 0.000010 0.000009 ) -0.012160 0.033309 0.076927 ( 0.000012 0.000011 0.000010 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 465 obs out of 466 (total:466,skipped:0) (99.79%) unit cell: 8.3711(11) 8.3749(12) 8.3714(10) 89.999(11) 90.052(10) 90.086(11) V = 586.89(13) unit cell: 8.3724(4) 8.3724(4) 8.3724(4) 90.0 90.0 90.0 V = 586.89(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_5_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_5_85.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_5_85.rpb Run 6 has been already processed *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) UB - matrix: -0.007468 0.076669 -0.034978 ( 0.000013 0.000016 0.000012 ) -0.083544 -0.011732 -0.008154 ( 0.000011 0.000013 0.000010 ) -0.012244 0.033568 0.076823 ( 0.000013 0.000015 0.000012 ) M - matrix: 0.007185 -0.000003 0.000002 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007143 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000002 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3678(11) 8.3927(14) 8.3640(13) 89.942(13) 90.014(11) 89.973(12) V = 587.39(16) OTKP changes: 417 1 1 1 No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) HKL list info: 701 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007189 -0.000004 0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007145 -0.000007 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007474 0.076678 -0.034983 ( 0.000013 0.000016 0.000012 ) -0.083562 -0.011737 -0.008172 ( 0.000011 0.000013 0.000010 ) -0.012255 0.033581 0.076818 ( 0.000012 0.000015 0.000011 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000001 ) UB fit with 417 obs out of 417 (total:417,skipped:0) (100.00%) unit cell: 8.3657(11) 8.3913(14) 8.3641(12) 89.944(13) 90.023(11) 89.969(12) V = 587.15(16) unit cell: 8.3737(3) 8.3737(3) 8.3737(3) 90.0 90.0 90.0 V = 587.15(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= -150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=94, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=70, end=94, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_7_70.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_7_70.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_7_70.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= 30.66 ka= -57.13 ph= 120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" UB fit with 431 obs out of 432 (total:432,skipped:0) (99.77%) UB - matrix: -0.007528 0.076839 -0.035274 ( 0.000013 0.000014 0.000012 ) -0.083614 -0.011811 -0.008240 ( 0.000012 0.000013 0.000011 ) -0.012346 0.033992 0.076683 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.007200 -0.000011 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000011 0.007199 -0.000006 ( 0.000002 0.000002 0.000002 ) 0.000008 -0.000006 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3590(12) 8.3597(13) 8.3636(12) 89.948(12) 90.061(12) 89.916(12) V = 584.44(15) OTKP changes: 431 1 1 1 OTKP changes: 431 1 1 1 OTKP changes: 431 1 1 1 OTKP changes: 431 1 1 1 OTKP changes: 431 1 1 1 OTKP changes: 431 1 1 1 Run 8 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.931) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.007528 0.076839 -0.035274 ( 0.000013 0.000014 0.000012 ) -0.083614 -0.011811 -0.008240 ( 0.000012 0.000013 0.000011 ) -0.012346 0.033992 0.076683 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.007200 -0.000011 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000011 0.007199 -0.000006 ( 0.000002 0.000002 0.000002 ) 0.000008 -0.000006 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007528 0.076839 -0.035274 ( 0.000013 0.000014 0.000012 ) -0.083614 -0.011811 -0.008240 ( 0.000012 0.000013 0.000011 ) -0.012346 0.033992 0.076683 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 431 obs out of 432 (total:432,skipped:0) (99.77%) unit cell: 8.3590(12) 8.3597(13) 8.3636(12) 89.948(12) 90.061(12) 89.916(12) V = 584.44(15) unit cell: 8.3608(3) 8.3608(3) 8.3608(3) 90.0 90.0 90.0 V = 584.44(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 431 obs out of 432 (total:432,skipped:0) (99.77%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.007528 0.076839 -0.035274 ( 0.000013 0.000014 0.000012 ) -0.083614 -0.011811 -0.008240 ( 0.000012 0.000013 0.000011 ) -0.012346 0.033992 0.076683 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.007200 -0.000011 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000011 0.007199 -0.000006 ( 0.000002 0.000002 0.000002 ) 0.000008 -0.000006 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.007528 0.076839 -0.035274 ( 0.000013 0.000014 0.000012 ) -0.083614 -0.011811 -0.008240 ( 0.000012 0.000013 0.000011 ) -0.012346 0.033992 0.076683 ( 0.000012 0.000013 0.000012 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 431 obs out of 432 (total:432,skipped:0) (99.77%) unit cell: 8.3590(12) 8.3597(13) 8.3636(12) 89.948(12) 90.061(12) 89.916(12) V = 584.44(15) unit cell: 8.3608(3) 8.3608(3) 8.3608(3) 90.0 90.0 90.0 V = 584.44(4) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.66 ka= -57.13 ph= 120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1715a\tmp\xs1715a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1715a\tmp\xs1715a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1715a\tmp\xs1715a_back_8_76.rpb Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1715a\tmp\xs1715a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.007441 0.076825 -0.034862 ( 0.000006 0.000006 0.000006 ) -0.083537 -0.011733 -0.008083 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033663 0.076875 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007182 -0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007173 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000004 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007441 0.076825 -0.034862 ( 0.000006 0.000006 0.000006 ) -0.083537 -0.011733 -0.008083 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033663 0.076875 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) UB fit with 3534 obs out of 3543 (total:3543,skipped:0) (99.75%) unit cell: 8.3697(4) 8.3749(5) 8.3647(5) 90.035(5) 89.993(5) 89.990(5) V = 586.33(6) unit cell: 8.36977(16) 8.36977(16) 8.36977(16) 90.0 90.0 90.0 V = 586.327(19) Writing tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" Discarded reflections: 83 reflections under beam stop or inside a detector rejection region 34 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1715a\tmp\xs1715a_1.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_2.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_3.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_4.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_5.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_6.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_7.rrpprof Adding file D:\Data\xs1715a\tmp\xs1715a_8.rrpprof 4688 reflections saved to the file D:\Data\xs1715a\xs1715a.rrpprof PROFFITMAIN - Finished at Wed Mar 28 15:13:49 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1715a\xs1715a.rrpprof OUTPUT: D:\Data\xs1715a\xs1715a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.022) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.931) PROFFIT INFO: signal sum: min=155.0000 max=22696260.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257434.6945 PROFFIT INFO: background sum: min=354.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11007.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7107130.5000 PROFFIT INFO: sig(Inet): min=185.8710 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 8 129 411 636 977 1080 2001 3159 4284 4687 Percent 0.0 0.2 2.8 8.8 13.6 20.8 23.0 42.7 67.4 91.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4688 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 4688 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7107131- 1480788 468 2244297.94 133.31 100.00 1480283- 901135 468 1173791.41 104.36 100.00 900356- 294991 468 533116.49 91.91 100.00 294269- 198751 468 238595.36 66.09 100.00 198524- 150311 468 170403.57 46.54 100.00 150308- 118053 468 133203.34 35.87 100.00 117913- 86440 468 102917.31 28.74 100.00 86329- 5845 468 48223.72 19.41 100.00 5841- 3253 468 4291.25 4.81 79.27 3252- 531 475 2316.74 2.97 33.89 ------------------------------------------------------------------------------------ 7107131- 531 4687 464424.52 53.33 91.23 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805312.74 84.92 100.00 1.41- 1.12 468 668827.45 68.21 98.29 1.12- 0.96 468 672104.02 75.94 97.44 0.96- 0.88 468 426465.89 56.57 93.16 0.88- 0.81 468 592233.79 67.09 96.37 0.81- 0.75 468 289314.71 38.42 90.81 0.75- 0.71 468 288170.46 38.47 89.10 0.71- 0.65 468 445586.23 46.35 93.80 0.65- 0.62 468 237048.25 28.73 72.86 0.62- 0.58 475 222795.80 28.92 80.63 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 464424.52 53.33 91.23 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:13:49 2018 Sorting 4687 observations 120 unique observations with > 7.00 F2/sig(F2) 4687 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 98 814 Total number of frames 814 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4687 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 14 122 Total number of frames 122 3762 observations > 7.00 F2/sig(F2) 3762 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 14 122 Total number of frames 122 Removing 'redundancy=1' reflections Average redundancy: 29.6 (Out of 3762 removed 5 = 3757, 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 3757 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 15 32 3 0 14 47 4 0 14 62 5 0 15 78 6 0 14 93 7 0 13 107 8 0 14 122 Total number of frames 122 127 unique data precomputed (should be 127) 127 unique data with 3757 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 29.6 (Out of 3757 removed 0 = 3757, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 3757 observations RMS deviation of equivalent data = 0.24635 Rint = 0.20179 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20131, wR= 0.26325 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14410, wR= 0.19255, Acormin=0.631, Acormax=1.318, Acor_av=0.955 F test: Probability=1.000, F= 1.949 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11861, wR= 0.15474, Acormin=0.529, Acormax=1.406, Acor_av=0.942 F test: Probability=1.000, F= 1.475 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12705, wR= 0.17028, Acormin=0.631, Acormax=1.558, Acor_av=0.958 F test: Probability=0.000, F= 0.870 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09481, wR= 0.12678, Acormin=0.453, Acormax=1.508, Acor_av=0.945 F test: Probability=1.000, F= 1.561 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08936, wR= 0.11714, Acormin=0.463, Acormax=1.565, Acor_av=0.932 F test: Probability=1.000, F= 1.123 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11626, wR= 0.15727, Acormin=0.607, Acormax=1.741, Acor_av=0.936 F test: Probability=0.000, F= 0.590 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08999, wR= 0.11944, Acormin=0.461, Acormax=1.644, Acor_av=0.940 F test: Probability=0.000, F= 0.985 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08478, wR= 0.11099, Acormin=0.465, Acormax=1.644, Acor_av=0.924 F test: Probability=0.999, F= 1.107 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07871, wR= 0.10201, Acormin=0.411, Acormax=1.628, Acor_av=0.834 F test: Probability=1.000, F= 1.157 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09634, wR= 0.12159, Acormin=0.199, Acormax=1.558, Acor_av=0.808 F test: Probability=0.000, F= 0.668 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09064, wR= 0.11490, Acormin=0.270, Acormax=1.588, Acor_av=0.839 F test: Probability=0.000, F= 0.754 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08773, wR= 0.11134, Acormin=0.093, Acormax=0.381, Acor_av=0.202 F test: Probability=0.000, F= 0.804 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07656, wR= 0.09997, Acormin=0.117, Acormax=0.461, Acor_av=0.234 F test: Probability=0.935, F= 1.052 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06970, wR= 0.09272, Acormin=0.122, Acormax=0.480, Acor_av=0.248 F test: Probability=1.000, F= 1.264 Final absorption model (ne=6, no=5): Rint= 0.07871, Acormin=0.411, Acormax=1.628, Acor_av=0.834 Combined refinement in use Rint: 0.20192 There are 122 active scales (one needs to be fixed) Refinement control: frame scale #86 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 169 pars with 14365 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24635 Using Levenberg-Marquardt: 0.00010 New wR= 0.05721 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20179 with corrections 0.04460 Rint for all data: 0.20192 with corrections 0.04483 4 observations identified as outliers and rejected Cycle 2 wR= 0.05647 Using Levenberg-Marquardt: 0.00001 New wR= 0.05284 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20160 with corrections 0.04130 Rint for all data: 0.20192 with corrections 0.04190 0 observations identified as outliers and rejected Cycle 3 wR= 0.05284 Using Levenberg-Marquardt: 0.00000 New wR= 0.05188 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20160 with corrections 0.04033 Rint for all data: 0.20192 with corrections 0.04092 0 observations identified as outliers and rejected Cycle 4 wR= 0.05188 Using Levenberg-Marquardt: 0.00000 New wR= 0.05144 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20160 with corrections 0.03987 Rint for all data: 0.20192 with corrections 0.04047 0 observations identified as outliers and rejected Cycle 5 wR= 0.05144 Using Levenberg-Marquardt: 0.00000 New wR= 0.05120 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20160 with corrections 0.03963 Rint for all data: 0.20192 with corrections 0.04022 0 observations identified as outliers and rejected Final wR= 0.05120 Final frame scales: Min= 0.7825 Max= 1.1850 Final absorption correction factors: Amin= 0.4256 Amax= 1.5499 PROFFIT INFO: Inet (after scale3 abspack): min=513.5839 max=4935952.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=144.6558 max=65427.2422 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4687 reflections read from tmp file 746 reflections are rejected (746 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 6 0 2 3 4 0 3 136 Initial Chi^2= 0.36232 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.92651 Current error model SIG(F2)^2 = 103.65*I_RAW + 0.00*I_BACK+(0.02124*)^2 Cycle 2, Chi^2= 1.00064 Current error model SIG(F2)^2 = 104.13*I_RAW + 0.00*I_BACK+(0.01839*)^2 Cycle 3, Chi^2= 0.99998 Current error model SIG(F2)^2 = 103.65*I_RAW + 0.00*I_BACK+(0.01853*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 103.70*I_RAW + 0.00*I_BACK+(0.01851*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 103.70*I_RAW + 0.00*I_BACK+(0.01851*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4935953- 1389448 468 2087909.77 49.14 100.00 1388426- 893387 468 1105190.45 41.34 100.00 893288- 284995 468 538755.77 39.58 100.00 284758- 181017 468 220742.42 32.77 100.00 180957- 150056 468 164321.53 25.93 100.00 149901- 112690 468 127371.71 20.56 100.00 112627- 89818 468 101431.05 17.72 100.00 89813- 5231 468 52045.87 13.13 99.79 5221- 3052 468 3907.28 4.49 92.09 3051- 514 475 2357.88 3.46 61.89 ------------------------------------------------------------------------------------ 4935953- 514 4687 439749.16 24.78 95.33 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805918.01 38.41 100.00 1.41- 1.12 468 659015.60 30.21 98.72 1.12- 0.96 468 610568.56 29.79 98.50 0.96- 0.88 468 402594.33 24.88 97.01 0.88- 0.81 468 553353.66 29.19 98.08 0.81- 0.75 468 263657.45 19.58 95.73 0.75- 0.71 468 272332.73 20.34 94.02 0.71- 0.65 468 407692.52 22.97 95.94 0.65- 0.62 468 222632.11 15.94 84.83 0.62- 0.58 475 203263.75 16.59 90.53 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 439749.16 24.78 95.33 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805918.01 38.41 100.00 4.82- 1.12 936 732466.81 34.31 99.36 4.82- 0.96 1404 691834.06 32.81 99.07 4.82- 0.88 1872 619524.13 30.82 98.56 4.82- 0.81 2340 606290.03 30.50 98.46 4.82- 0.75 2808 549184.60 28.68 98.01 4.82- 0.71 3276 509634.33 27.49 97.44 4.82- 0.65 3744 496891.61 26.92 97.25 4.82- 0.62 4212 466418.33 25.70 95.87 4.82- 0.58 4687 439749.16 24.78 95.33 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 439749.16 24.78 95.33 Scale applied to data: s=0.202595 (maximum obs:4935952.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.040; Rsigma 0.026: data 4687 -> merged 156 With outlier rejection... Rint 0.039; Rsigma 0.026: data 4676 -> merged 156 Rejected total: 11, method kkm 10, method Blessing 1 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586001, 4.832287 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 27.79 100.00 389 1.41 - 1.12 14 14 39.00 100.00 546 1.12 - 0.97 14 14 39.00 100.00 546 0.96 - 0.84 14 14 41.36 100.00 579 0.84 - 0.78 14 14 31.64 100.00 443 0.78 - 0.73 14 14 32.86 100.00 460 0.73 - 0.69 14 14 31.50 100.00 441 0.69 - 0.66 14 14 26.21 100.00 367 0.65 - 0.63 14 14 29.00 100.00 406 0.63 - 0.60 14 14 25.36 100.00 355 --------------------------------------------------------------- 8.36 - 0.60 140 140 32.37 100.00 4532 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:13:50 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.369679 8.374885 8.364739 90.0354 89.9927 89.9901 4676 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2377 0 3128 3129 4676 N (int>3sigma) = 0 0 0 0 2377 0 2976 2982 4457 Mean intensity = 0.0 0.0 0.0 0.0 33.9 0.0 89.4 90.3 88.8 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 24.8 24.9 24.7 Lattice type: F chosen Volume: 586.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.916 5.917 5.917 119.97 90.03 119.95 Niggli form: a.a = 35.001 b.b = 35.005 c.c = 35.010 b.c = -17.487 a.c = -0.021 a.b = -17.476 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.039 [ 4520] Vol = 586.3 Cell: 8.365 8.375 8.370 89.99 89.99 90.04 Volume: 586.33 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 4237] Vol = 439.7 Cell: 5.917 5.916 14.500 89.99 90.05 119.95 Volume: 439.75 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1373] Vol = 439.7 Trigonal Cell: 5.917 5.916 14.500 89.99 90.05 119.95 Volume: 439.75 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.070 TETRAGONAL I-lattice R(int) = 0.039 [ 4270] Vol = 293.2 Cell: 5.921 5.920 8.365 89.97 90.02 90.04 Volume: 293.16 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.054 TETRAGONAL I-lattice R(int) = 0.039 [ 4270] Vol = 293.2 Cell: 5.921 5.920 8.365 89.97 90.02 90.04 Volume: 293.16 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.039 [ 4217] Vol = 293.2 Cell: 5.921 8.365 5.920 89.97 89.96 89.98 Volume: 293.16 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.037 [ 3871] Vol = 293.2 Cell: 8.365 5.921 5.920 90.04 90.03 89.98 Volume: 293.16 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.032 MONOCLINIC I-lattice R(int) = 0.035 [ 3865] Vol = 293.2 Cell: 5.917 5.916 8.375 89.97 90.02 89.97 Volume: 293.16 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.048 MONOCLINIC C-lattice R(int) = 0.035 [ 3885] Vol = 293.2 Cell: 8.365 8.375 5.916 89.97 134.98 90.04 Volume: 293.16 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 3211] Vol = 146.6 Cell: 5.916 5.917 5.917 119.97 90.03 119.95 Volume: 146.58 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2377 0 3118 3129 4676 N (int>3sigma) = 0 0 0 0 2377 0 2975 2982 4457 Mean intensity = 0.0 0.0 0.0 0.0 33.9 0.0 92.2 90.3 88.8 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 25.0 24.9 24.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 48 48 380 1043 N I>3s 39 39 324 1043 0.7 0.7 0.7 39.7 7.3 7.3 4.9 28.2 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 0.039 4160 Fd-3m 1 1 227 C N N N N 37 2284 0.039 4199 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364739 8.374885 8.369679 89.9901 89.9927 90.0354 ZERR 3.00 0.000510 0.000550 0.000418 0.0048 0.0046 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4804861- 1033758 761 758 26 29.2 1734783.46 46.54 0.035 0.045 1033157- 250121 730 725 26 27.9 609609.86 39.44 0.047 0.058 249937- 124850 1084 1083 26 41.7 174458.86 26.96 0.039 0.053 119615- 89442 770 770 26 29.6 105931.66 18.10 0.058 0.074 84400- 3647 696 694 26 26.7 28155.35 8.93 0.074 0.089 3551- 1702 646 646 26 24.8 2853.47 3.91 0.207 0.265 ------------------------------------------------------------------------------------------- 4804861- 1702 4687 4676 156 30.0 438157.08 24.75 0.039 0.050 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 888 884 26 34.0 665199.74 33.50 0.037 0.045 0.021 1.12-0.88 1051 1051 26 40.4 549529.65 28.41 0.032 0.044 0.024 0.85-0.75 870 870 26 33.5 424842.90 24.02 0.038 0.051 0.027 0.74-0.68 771 770 26 29.6 354034.06 21.65 0.045 0.055 0.030 0.67-0.63 745 745 26 28.7 213529.73 17.24 0.058 0.079 0.037 0.62-0.59 362 356 26 13.7 230143.42 16.40 0.056 0.051 0.036 ------------------------------------------------------------------------------------------------------ inf-0.59 4687 4676 156 30.0 438157.08 24.75 0.039 0.050 0.026 inf-0.60 4535 4530 139 32.6 447218.51 25.06 0.039 0.051 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 884 26 26 100.0 34.0 665199.74 212.12 0.037 0.005 1.12-0.88 1051 26 26 100.0 40.4 549529.65 182.54 0.032 0.004 0.85-0.75 870 26 26 100.0 33.5 424842.90 146.81 0.038 0.005 0.74-0.68 770 26 26 100.0 29.6 354034.06 119.85 0.045 0.006 0.67-0.63 745 26 26 100.0 28.7 213529.73 91.81 0.058 0.007 0.62-0.59 356 27 26 96.3 13.7 230143.42 72.13 0.056 0.014 -------------------------------------------------------------------------------------------- inf-0.59 4676 157 156 99.4 30.0 438157.08 148.30 0.039 0.006 inf-0.60 4530 139 139 100.0 32.6 447218.51 151.45 0.039 0.005 Reading tabbin file: "D:\Data\xs1715a\xs1715a_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: -0.007441 0.076825 -0.034861 ( 0.000006 0.000006 0.000006 ) -0.083537 -0.011733 -0.008083 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033663 0.076875 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007182 -0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007173 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000004 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.007441 0.076825 -0.034861 ( 0.000006 0.000006 0.000006 ) -0.083537 -0.011733 -0.008083 ( 0.000004 0.000004 0.000004 ) -0.012170 0.033663 0.076875 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3697(4) 8.3750(5) 8.3647(5) 90.036(5) 89.993(4) 89.990(5) V = 586.33(6) unit cell: 8.36979(16) 8.36979(16) 8.36979(16) 90.0 90.0 90.0 V = 586.333(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-120.000 (rot geo dd=52.946) Run 2 Omega scan: (-107.000 - 2.000,109 frames, 5.500 sec, 1.000 deg) at th=-30.795, ka=-77.000,ph=-150.000 (rot geo dd=53.051) Run 3 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-60.000 (rot geo dd=53.126) Run 4 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=90.000 (rot geo dd=52.971) Run 5 Omega scan: (-2.000 - 107.000,109 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=77.000,ph=150.000 (rot geo dd=53.022) Run 6 Omega scan: (3.000 - 103.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=57.000,ph=0.000 (rot geo dd=52.968) Run 7 Omega scan: (-41.000 - 53.000,94 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=-150.000 (rot geo dd=52.995) Run 8 Omega scan: (-41.000 - 59.000,100 frames, 5.500 sec, 1.000 deg) at th=30.795, ka=-57.000,ph=120.000 (rot geo dd=52.931) PROFFIT INFO: signal sum: min=155.0000 max=22696260.0000 PROFFIT INFO: signal sum lp corr: min=243.2060 max=3257434.6945 PROFFIT INFO: background sum: min=354.0000 max=17359.0000 PROFFIT INFO: background sum sig2: min=550.0000 max=11007.0000 PROFFIT INFO: num of signal pixels: min=56 max=882 PROFFIT INFO: Inet: min=530.6313 max=7107130.5000 PROFFIT INFO: sig(Inet): min=185.8710 max=63736.6172 PROFFIT INFO: Inet/sig(Inet): min=0.49 max=309.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 16 258 822 1272 1954 2160 4002 6318 8568 9374 Percent 0.0 0.2 2.8 8.8 13.6 20.8 23.0 42.7 67.4 91.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4688 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 4688 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 7107131- 1480788 468 2244297.94 133.31 100.00 1480283- 901135 468 1173791.41 104.36 100.00 900356- 294991 468 533116.49 91.91 100.00 294269- 198751 468 238595.36 66.09 100.00 198524- 150311 468 170403.57 46.54 100.00 150308- 118053 468 133203.34 35.87 100.00 117913- 86440 468 102917.31 28.74 100.00 86329- 5845 468 48223.72 19.41 100.00 5841- 3253 468 4291.25 4.81 79.27 3252- 531 475 2316.74 2.97 33.89 ------------------------------------------------------------------------------------ 7107131- 531 4687 464424.52 53.33 91.23 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805312.74 84.92 100.00 1.41- 1.12 468 668827.45 68.21 98.29 1.12- 0.96 468 672104.02 75.94 97.44 0.96- 0.88 468 426465.89 56.57 93.16 0.88- 0.81 468 592233.79 67.09 96.37 0.81- 0.75 468 289314.71 38.42 90.81 0.75- 0.71 468 288170.46 38.47 89.10 0.71- 0.65 468 445586.23 46.35 93.80 0.65- 0.62 468 237048.25 28.73 72.86 0.62- 0.58 475 222795.80 28.92 80.63 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 464424.52 53.33 91.23 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\xs1715a\plots_red\xs1715a_absscale.dat Started at Wed Mar 28 15:13:51 2018 Sorting 4687 observations 86 unique observations with > 7.00 F2/sig(F2) 4687 observations in 8 runs Run # start # end # total # 1 1 107 107 2 1 108 215 3 0 98 314 4 0 98 413 5 0 108 522 6 0 99 622 7 0 92 715 8 0 98 814 Total number of frames 814 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4687 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 9 83 Total number of frames 83 3762 observations > 7.00 F2/sig(F2) 3762 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 9 83 Total number of frames 83 Removing 'redundancy=1' reflections Average redundancy: 41.3 (Out of 3762 removed 4 = 3758, 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): 4/m3bar2/m 3758 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 9 32 4 0 9 42 5 0 10 53 6 0 9 63 7 0 9 73 8 0 9 83 Total number of frames 83 91 unique data precomputed (should be 91) 91 unique data with 3758 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 41.3 (Out of 3758 removed 0 = 3758, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 3758 observations RMS deviation of equivalent data = 0.24688 Rint = 0.20205 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20164, wR= 0.26401 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14417, wR= 0.19345, Acormin=0.632, Acormax=1.316, Acor_av=0.955 F test: Probability=1.000, F= 1.953 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11900, wR= 0.15537, Acormin=0.529, Acormax=1.406, Acor_av=0.942 F test: Probability=1.000, F= 1.466 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12824, wR= 0.17184, Acormin=0.633, Acormax=1.553, Acor_av=0.957 F test: Probability=0.000, F= 0.860 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09587, wR= 0.12805, Acormin=0.452, Acormax=1.506, Acor_av=0.944 F test: Probability=1.000, F= 1.537 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09028, wR= 0.11841, Acormin=0.464, Acormax=1.561, Acor_av=0.931 F test: Probability=1.000, F= 1.126 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11689, wR= 0.15802, Acormin=0.601, Acormax=1.745, Acor_av=0.935 F test: Probability=0.000, F= 0.596 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09105, wR= 0.12032, Acormin=0.455, Acormax=1.653, Acor_av=0.938 F test: Probability=0.000, F= 0.982 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08523, wR= 0.11190, Acormin=0.464, Acormax=1.649, Acor_av=0.922 F test: Probability=1.000, F= 1.118 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07917, wR= 0.10271, Acormin=0.408, Acormax=1.630, Acor_av=0.833 F test: Probability=1.000, F= 1.155 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09688, wR= 0.12215, Acormin=0.209, Acormax=1.566, Acor_av=0.807 F test: Probability=0.000, F= 0.669 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09123, wR= 0.11540, Acormin=0.277, Acormax=1.597, Acor_av=0.839 F test: Probability=0.000, F= 0.753 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08800, wR= 0.11163, Acormin=0.093, Acormax=0.379, Acor_av=0.201 F test: Probability=0.000, F= 0.808 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07685, wR= 0.10015, Acormin=0.116, Acormax=0.458, Acor_av=0.232 F test: Probability=0.950, F= 1.056 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06995, wR= 0.09288, Acormin=0.121, Acormax=0.477, Acor_av=0.246 F test: Probability=1.000, F= 1.270 Final absorption model (ne=6, no=5): Rint= 0.07917, Acormin=0.408, Acormax=1.630, Acor_av=0.833 Combined refinement in use Rint: 0.20218 There are 83 active scales (one needs to be fixed) Refinement control: frame scale #31 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 130 pars with 8515 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24688 Using Levenberg-Marquardt: 0.00010 New wR= 0.06356 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20205 with corrections 0.04937 Rint for all data: 0.20218 with corrections 0.04960 2 observations identified as outliers and rejected Cycle 2 wR= 0.06293 Using Levenberg-Marquardt: 0.00001 New wR= 0.05734 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20189 with corrections 0.04485 Rint for all data: 0.20218 with corrections 0.04528 3 observations identified as outliers and rejected Cycle 3 wR= 0.05732 Using Levenberg-Marquardt: 0.00000 New wR= 0.05575 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20188 with corrections 0.04341 Rint for all data: 0.20218 with corrections 0.04383 2 observations identified as outliers and rejected Cycle 4 wR= 0.05542 Using Levenberg-Marquardt: 0.00000 New wR= 0.05472 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20172 with corrections 0.04240 Rint for all data: 0.20218 with corrections 0.04312 0 observations identified as outliers and rejected Cycle 5 wR= 0.05472 Using Levenberg-Marquardt: 0.00000 New wR= 0.05438 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20172 with corrections 0.04202 Rint for all data: 0.20218 with corrections 0.04275 0 observations identified as outliers and rejected Final wR= 0.05438 Final frame scales: Min= 0.8295 Max= 1.2054 Final absorption correction factors: Amin= 0.4450 Amax= 1.6349 PROFFIT INFO: Inet (after scale3 abspack): min=518.3713 max=4957910.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.0824 max=64555.4922 ****************************************************************************** * 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\xs1715a\xs1715a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4687 reflections read from tmp file 808 reflections are rejected (808 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 4 1 1 2 2 1 3 95 Initial Chi^2= 0.35367 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93130 Current error model SIG(F2)^2 = 106.68*I_RAW + 0.00*I_BACK+(0.02097*)^2 Cycle 2, Chi^2= 1.00030 Current error model SIG(F2)^2 = 102.97*I_RAW + 0.00*I_BACK+(0.01943*)^2 Cycle 3, Chi^2= 0.99998 Current error model SIG(F2)^2 = 102.21*I_RAW + 0.00*I_BACK+(0.01960*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 102.39*I_RAW + 0.00*I_BACK+(0.01956*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 102.39*I_RAW + 0.00*I_BACK+(0.01956*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4957910- 1389406 468 2086654.52 47.01 100.00 1388670- 898473 468 1106368.90 40.15 100.00 898433- 284831 468 539142.53 38.36 100.00 283555- 181667 468 220625.13 32.08 100.00 181572- 149324 468 164488.86 25.80 100.00 149073- 112456 468 127362.59 20.48 100.00 112394- 89644 468 101546.65 17.64 100.00 89464- 5244 468 51962.90 13.14 99.79 5240- 3055 468 3910.47 4.53 93.38 3052- 518 475 2355.40 3.48 62.95 ------------------------------------------------------------------------------------ 4957910- 518 4687 439787.52 24.24 95.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805150.88 37.04 100.00 1.41- 1.12 468 659303.78 29.35 98.93 1.12- 0.96 468 609968.00 28.97 98.50 0.96- 0.88 468 402389.68 24.37 97.22 0.88- 0.81 468 553506.69 28.53 98.50 0.81- 0.75 468 263733.69 19.30 95.94 0.75- 0.71 468 272226.01 20.09 94.23 0.71- 0.65 468 408212.30 22.59 95.94 0.65- 0.62 468 223047.85 15.78 85.26 0.62- 0.58 475 203865.04 16.46 91.16 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 439787.52 24.24 95.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 468 805150.88 37.04 100.00 4.82- 1.12 936 732227.33 33.20 99.47 4.82- 0.96 1404 691474.22 31.79 99.15 4.82- 0.88 1872 619203.08 29.93 98.66 4.82- 0.81 2340 606063.81 29.65 98.63 4.82- 0.75 2808 549008.79 27.93 98.18 4.82- 0.71 3276 509468.39 26.81 97.62 4.82- 0.65 3744 496811.38 26.28 97.41 4.82- 0.62 4212 466393.21 25.11 96.06 4.82- 0.58 4687 439787.52 24.24 95.56 ------------------------------------------------------------------------------------ 4.82- 0.58 4687 439787.52 24.24 95.56 Scale applied to data: s=0.201698 (maximum obs:4957910.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.043; Rsigma 0.027: data 4687 -> merged 109 With outlier rejection... Rint 0.042; Rsigma 0.027: data 4680 -> merged 109 Rejected total: 7, method kkm 6, method Blessing 1 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586003, 4.832302 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 29.30 100.00 293 1.61 - 1.21 10 10 44.10 100.00 441 1.17 - 1.01 10 10 56.20 100.00 562 0.99 - 0.89 10 10 54.90 100.00 549 0.88 - 0.81 10 10 53.10 100.00 531 0.81 - 0.74 10 10 45.20 100.00 452 0.73 - 0.71 10 10 50.80 100.00 508 0.70 - 0.66 10 10 40.20 100.00 402 0.66 - 0.64 10 10 41.10 100.00 411 0.63 - 0.60 10 10 38.40 100.00 384 --------------------------------------------------------------- 8.36 - 0.60 100 100 45.33 100.00 4533 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1715a\xs1715a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1715a\xs1715a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Mar 28 15:13:50 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.369679 8.374885 8.364739 90.0354 89.9927 89.9901 4676 Reflections read from file xs1715a.hkl; mean (I/sigma) = 24.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2377 0 3128 3129 4676 N (int>3sigma) = 0 0 0 0 2377 0 2976 2982 4457 Mean intensity = 0.0 0.0 0.0 0.0 33.9 0.0 89.4 90.3 88.8 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 24.8 24.9 24.7 Lattice type: F chosen Volume: 586.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Unitcell: 5.916 5.917 5.917 119.97 90.03 119.95 Niggli form: a.a = 35.001 b.b = 35.005 c.c = 35.010 b.c = -17.487 a.c = -0.021 a.b = -17.476 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.039 [ 4520] Vol = 586.3 Cell: 8.365 8.375 8.370 89.99 89.99 90.04 Volume: 586.33 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 4237] Vol = 439.7 Cell: 5.917 5.916 14.500 89.99 90.05 119.95 Volume: 439.75 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.038 [ 1373] Vol = 439.7 Trigonal Cell: 5.917 5.916 14.500 89.99 90.05 119.95 Volume: 439.75 Matrix: 0.0000 -0.5000 -0.5000 -0.5000 0.0000 0.5000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.070 TETRAGONAL I-lattice R(int) = 0.039 [ 4270] Vol = 293.2 Cell: 5.921 5.920 8.365 89.97 90.02 90.04 Volume: 293.16 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.054 TETRAGONAL I-lattice R(int) = 0.039 [ 4270] Vol = 293.2 Cell: 5.921 5.920 8.365 89.97 90.02 90.04 Volume: 293.16 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.039 [ 4217] Vol = 293.2 Cell: 5.921 8.365 5.920 89.97 89.96 89.98 Volume: 293.16 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.037 [ 3871] Vol = 293.2 Cell: 8.365 5.921 5.920 90.04 90.03 89.98 Volume: 293.16 Matrix: 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.032 MONOCLINIC I-lattice R(int) = 0.035 [ 3865] Vol = 293.2 Cell: 5.917 5.916 8.375 89.97 90.02 89.97 Volume: 293.16 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.048 MONOCLINIC C-lattice R(int) = 0.035 [ 3885] Vol = 293.2 Cell: 8.365 8.375 5.916 89.97 134.98 90.04 Volume: 293.16 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.032 [ 3211] Vol = 146.6 Cell: 5.916 5.917 5.917 119.97 90.03 119.95 Volume: 146.58 Matrix:-0.5000 0.0000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2377 0 3118 3129 4676 N (int>3sigma) = 0 0 0 0 2377 0 2975 2982 4457 Mean intensity = 0.0 0.0 0.0 0.0 33.9 0.0 92.2 90.3 88.8 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 25.0 24.9 24.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.190 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 48 48 380 1043 N I>3s 39 39 324 1043 0.7 0.7 0.7 39.7 7.3 7.3 4.9 28.2 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 0.039 4160 Fd-3m 1 1 227 C N N N N 37 2284 0.039 4199 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1715a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364739 8.374885 8.369679 89.9901 89.9927 90.0354 ZERR 3.00 0.000510 0.000550 0.000418 0.0048 0.0046 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 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.p4pgral! Back-up copy of original file: D:\Data\xs1715a\xs1715a.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 --------------------------------------------------------------------------------------------- 4746202- 817696 1046 1044 27 38.7 1516955.38 42.69 0.040 0.052 777853- 138929 1392 1388 27 51.4 253531.02 31.28 0.045 0.057 128267- 46737 1147 1147 27 42.5 101087.00 17.75 0.061 0.080 19244- 1703 1102 1101 28 39.3 4179.26 4.53 0.168 0.213 ------------------------------------------------------------------------------------------- 4746202- 1703 4687 4680 109 42.9 439348.42 24.22 0.042 0.055 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1196 1194 27 44.2 702668.45 33.29 0.038 0.051 0.022 1.01-0.78 1466 1466 28 52.4 412373.77 23.20 0.038 0.052 0.027 0.76-0.65 1241 1239 28 44.3 337288.26 20.51 0.048 0.058 0.031 0.65-0.59 784 781 26 30.0 249327.02 18.10 0.061 0.068 0.037 ------------------------------------------------------------------------------------------------------ inf-0.59 4687 4680 109 42.9 439348.42 24.22 0.042 0.055 0.027 inf-0.60 4535 4531 99 45.8 448349.57 24.51 0.042 0.055 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1194 27 27 100.0 44.2 702668.45 246.99 0.038 0.005 1.01-0.78 1466 28 28 100.0 52.4 412373.77 178.45 0.038 0.004 0.76-0.65 1239 28 28 100.0 44.3 337288.26 145.63 0.048 0.006 0.65-0.59 781 27 26 96.3 30.0 249327.02 116.01 0.061 0.009 -------------------------------------------------------------------------------------------- inf-0.59 4680 110 109 99.1 42.9 439348.42 176.83 0.042 0.005 inf-0.60 4531 99 99 100.0 45.8 448349.57 180.34 0.042 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1715a\struct\olex2_xs1715a\.olex\originals\*.*) ? Olex report: D:\Data\xs1715a\struct\olex2_xs1715a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1715a\struct\olex2_xs1715a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1715a\struct\olex2_xs1715a\xs1715a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1715a\xs1715a_proffitpeak" WD P/CAL INFO: D:\Data\xs1715a\xs1715a_cracker.par written Instrument model: dd: 52.97, x0: 1027.95, y0: 1024.61, beam: 0.04, o0: 0.06, t0: -0.14, k0: -0.13