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 rudi005_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.): 1.54183 11.199 16.686 22.178 89.983 89.949 89.998 149.01 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3774 94.45 2 55.00 0.8922 46.36 3 -89.50 0.8000 96.06 4 -89.50 0.8003 93.89 5 -89.50 0.8004 93.77 6 58.94 0.8757 96.05 7 -89.50 0.8000 91.25 8 -89.50 0.8003 93.12 Fast scans: 1 2 These scans are used only to provide replacements for reflections missing in all other scans (e.g. overloads suppressed by SAINT) and do not otherwise contribute to the final reflection file. Fast scans truncated to 1.5000 Angstroms ============================================================================== 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 34915 Reflections of which 8294 unique; 17.12 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 499 1164 1507 1621 1389 1104 650 285 75 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 15 105 185 216 443 1262 1233 1210 3625 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 39262 Reflections employed for parameter determination Effective data to parameter ratio = 15.21 wR2(int) = 0.1454 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1317 0.1048 0.7854 2 0.0993 0.0923 0.8349 3 0.0910 0.0875 0.8531 4 0.0871 0.0848 0.8651 5 0.0848 0.0831 0.8742 6 0.0831 0.0818 0.8819 7 0.0816 0.0806 0.8871 8 0.0805 0.0799 0.8901 9 0.0798 0.0795 0.8919 10 0.0794 0.0792 0.8930 11 0.0792 0.0791 0.8936 12 0.0790 0.0790 0.8940 13 0.0789 0.0789 0.8943 14 0.0789 0.0789 0.8944 15 0.0788 0.0789 0.8945 16 0.0788 0.0789 0.8946 17 0.0788 0.0788 0.8946 18 0.0788 0.0788 0.8947 19 0.0788 0.0788 0.8947 20 0.0788 0.0788 0.8947 21 0.0788 0.0788 0.8947 22 0.0788 0.0788 0.8947 23 0.0788 0.0788 0.8947 24 0.0788 0.0788 0.8947 25 0.0788 0.0789 0.8947 26 0.0788 0.0789 0.8947 27 0.0788 0.0789 0.8947 28 0.0788 0.0789 0.8947 29 0.0788 0.0789 0.8947 30 0.0788 0.0789 0.8947 31 0.0788 0.0789 0.8948 32 0.0788 0.0789 0.8948 33 0.0788 0.0789 0.8948 34 0.0788 0.0789 0.8948 35 0.0788 0.0789 0.8948 36 0.0788 0.0789 0.8948 37 0.0788 0.0789 0.8948 38 0.0788 0.0789 0.8948 39 0.0788 0.0789 0.8948 40 0.0788 0.0789 0.8948 41 0.0788 0.0789 0.8948 42 0.0788 0.0789 0.8948 43 0.0788 0.0789 0.8948 44 0.0788 0.0789 0.8948 45 0.0788 0.0789 0.8948 46 0.0788 0.0789 0.8948 47 0.0788 0.0789 0.8948 48 0.0788 0.0789 0.8948 49 0.0788 0.0789 0.8948 50 0.0788 0.0789 0.8948 wR2(int) = 0.0789 (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: 34915 total and 8294 unique reflections. plus 6065 total and 1295 unique reflections in fast scans Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 32861 total and 8290 unique reflections left after |I-|/su test plus 5028 total and 1291 unique reflections in fast scans 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) 1f 0.0 0.0682 0.391 - 0.488 0.707 - 1.442 1.641 0.0623 16.1 3254 3024 2f 55.0 0.1331 4.091 - 5.982 0.724 - 1.475 1.434 0.0623 16.1 1774 1304 3 -89.5 0.0467 0.488 - 0.809 0.707 - 1.461 0.894 0.0623 16.1 9711 9522 4 -89.5 0.0513 0.558 - 0.675 0.760 - 1.629 1.015 0.0623 16.1 4209 4049 5 -89.5 0.0556 0.817 - 0.952 0.707 - 1.630 1.188 0.0623 16.1 4275 4055 6 58.9 0.0414 0.433 - 0.564 0.707 - 1.591 0.930 0.0623 16.1 6730 6584 7 -89.5 0.0797 0.761 - 1.114 0.755 - 1.630 1.510 0.0623 16.1 3778 3383 8 -89.5 0.0635 0.728 - 0.908 0.708 - 1.630 1.470 0.0623 16.1 4158 3853 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 rudi005.eps Reflections not merged 2 Overloads replaced by fast scan measurements 32863 Corrected reflections written to file rudi005_0m.hkl Estimated minimum and maximum transmission: 0.3257 0.7538 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000