SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction -------------------------------------------------------------------------- Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10. Equivalent reflections defined by point group 222 for scaling Equivalent reflections defined by point group 222 for error model Reading file cu_bilm001_0m.raw Mean and maximum errors in direction cosine check function = 0.000 0.000 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Approximate wavelength, cell and maximum 2-theta (from cosines etc.): 1.54184 6.978 12.497 16.170 89.984 90.000 90.009 150.53 Scan 2-theta high res %[I>3sig(I)] 1 -73.14 0.9812 94.33 2 118.90 0.7974 87.53 3 118.90 0.7985 82.20 4 -28.85 1.4780 94.69 5 118.90 0.7991 86.69 6 -73.14 0.9792 93.74 7 118.90 0.7972 88.42 8 118.90 0.7982 88.95 9 -58.14 1.1047 95.61 ============================================================================== PART 1 - Refinement of parameters to model systematic errors Thresholds should now be specified for excluding reflections from the parameter refinement; these reflections may still be corrected and included in the final output .hkl file 10235 Reflections of which 2913 unique; 5.51 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 266 735 648 499 357 209 113 56 30 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 26 117 80 88 169 515 471 359 1088 Settings for parameter refinement: Maximum resolution = 0.1000 A (Intensity/sigma) threshold = 1.500 Restraint esd for equal adjacent scale factors = 0.0050 Maximum odd and even orders for spherical harmonics = 3 6 9339 Reflections employed for parameter determination Effective data to parameter ratio = 3.62 wR2(int) = 0.0787 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.0490 0.0431 0.9590 2 0.0414 0.0407 0.9607 3 0.0403 0.0401 0.9609 4 0.0400 0.0399 0.9610 5 0.0398 0.0397 0.9610 6 0.0397 0.0396 0.9611 7 0.0396 0.0396 0.9611 8 0.0395 0.0395 0.9611 9 0.0395 0.0395 0.9612 10 0.0395 0.0395 0.9612 11 0.0395 0.0395 0.9612 12 0.0394 0.0394 0.9612 13 0.0394 0.0394 0.9612 14 0.0394 0.0394 0.9612 15 0.0394 0.0394 0.9612 16 0.0394 0.0394 0.9612 17 0.0394 0.0394 0.9612 18 0.0394 0.0394 0.9612 19 0.0394 0.0394 0.9612 20 0.0394 0.0394 0.9612 21 0.0394 0.0394 0.9612 22 0.0394 0.0394 0.9612 23 0.0394 0.0394 0.9612 24 0.0394 0.0394 0.9612 25 0.0394 0.0394 0.9612 26 0.0394 0.0394 0.9612 27 0.0394 0.0394 0.9612 28 0.0394 0.0394 0.9612 29 0.0394 0.0394 0.9612 30 0.0394 0.0394 0.9612 31 0.0394 0.0394 0.9612 32 0.0394 0.0394 0.9612 33 0.0394 0.0394 0.9612 34 0.0394 0.0394 0.9612 35 0.0394 0.0394 0.9612 36 0.0394 0.0394 0.9612 37 0.0394 0.0394 0.9612 38 0.0394 0.0394 0.9612 39 0.0394 0.0394 0.9612 40 0.0394 0.0394 0.9612 41 0.0394 0.0394 0.9612 42 0.0394 0.0394 0.9612 43 0.0394 0.0394 0.9612 44 0.0394 0.0394 0.9612 45 0.0394 0.0394 0.9612 46 0.0394 0.0394 0.9612 47 0.0394 0.0394 0.9612 48 0.0394 0.0394 0.9612 49 0.0394 0.0394 0.9612 50 0.0394 0.0394 0.9612 wR2(int) = 0.0394 (selected reflections only, after parameter refinement) ============================================================================== PART 2 - Reject outliers and establish error model Rejected reflections are ignored in the statistics and Postscript plots (except the detector diagnostics) and in the output .hkl file Before applying rejections there are: 10235 total and 2913 unique reflections. Reflections rejected for which |I-|/su > 4.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 10229 total and 2913 unique reflections left after |I-|/su test su^2 = [K*sigma(I)]^2 + [g]^2 where sigma(I) is from SAINT Error model 5: refine all K and overall g Run 2theta R(int) Incid. factors Diffr. factors K g I/s(lim) Total I>2sig(I) 1 -73.1 0.0211 0.695 - 0.907 0.977 - 1.037 0.675 0.0278 36.0 1269 1227 2 118.9 0.0387 0.709 - 1.083 0.977 - 1.034 0.912 0.0278 36.0 1175 1066 3 118.9 0.0320 0.949 - 1.071 0.977 - 1.039 0.775 0.0278 36.0 1180 1059 4 -28.9 0.0215 0.937 - 1.079 0.977 - 1.038 0.818 0.0278 36.0 659 634 5 118.9 0.0390 0.937 - 1.048 0.977 - 1.042 0.816 0.0278 36.0 1172 1079 6 -73.1 0.0211 0.783 - 1.081 0.977 - 1.041 0.577 0.0278 36.0 1278 1232 7 118.9 0.0343 0.896 - 1.103 0.977 - 1.040 0.843 0.0278 36.0 1182 1095 8 118.9 0.0386 0.833 - 1.054 0.977 - 1.041 0.957 0.0278 36.0 1176 1080 9 -58.1 0.0220 0.772 - 0.943 0.977 - 1.036 0.646 0.0278 36.0 1138 1107 I/s(lim) is the limiting value of I/sigma(I) for a reflection of infinite intensity, and may be used as a criterion for data quality (Diederichs(2010), Acta Cryst, D66, 733-740. The above statistics are based on all non-rejected data, ignoring reflections without equivalents when estimating R(int) and K. ============================================================================== PART 3 - Output Postscript diagnostics and corrected data Diagnostic plots written to Postscript file cu_bilm001.eps Reflections not merged 10229 Corrected reflections written to file cu_bilm001_0m.hkl Estimated minimum and maximum transmission: 0.7009 0.7539 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000