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 2 for scaling Equivalent reflections defined by point group 2 for error model Reading file neal054_0m.raw Mean and maximum errors in direction cosine check function = 0.001 0.005 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.): 1.54172 6.250 11.761 13.023 90.009 96.678 90.013 127.36 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3970 95.18 2 62.44 0.8651 99.27 3 77.43 0.8603 98.52 4 62.44 0.8642 98.58 5 62.44 0.8618 97.82 6 77.43 0.8604 98.35 7 58.94 0.8797 98.16 8 77.43 0.8601 98.35 9 58.94 0.8846 98.86 10 77.43 0.8609 98.31 11 77.43 0.8601 98.10 12 62.44 0.8642 98.45 13 58.94 0.8787 96.85 14 58.94 0.8798 97.41 15 58.94 0.8778 98.16 16 77.43 0.8610 98.06 17 77.43 0.8610 97.23 18 47.44 0.9351 94.98 19 58.94 0.8800 96.41 20 77.43 0.8604 97.91 21 47.44 0.9346 95.53 22 47.44 0.9327 93.19 23 77.43 0.8600 97.94 24 77.43 0.8600 98.03 Fast scans: 1 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 19548 Reflections of which 3132 unique; 8.03 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 98 203 335 377 384 367 337 298 733 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 8 14 23 29 67 194 204 166 2427 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 20176 Reflections employed for parameter determination Effective data to parameter ratio = 6.94 wR2(int) = 0.1209 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1070 0.0957 0.8609 2 0.0914 0.0893 0.8791 3 0.0880 0.0873 0.8845 4 0.0867 0.0865 0.8869 5 0.0859 0.0859 0.8884 6 0.0853 0.0854 0.8895 7 0.0849 0.0851 0.8903 8 0.0846 0.0848 0.8908 9 0.0844 0.0847 0.8912 10 0.0843 0.0845 0.8915 11 0.0842 0.0844 0.8917 12 0.0841 0.0844 0.8919 13 0.0841 0.0843 0.8921 14 0.0840 0.0843 0.8922 15 0.0840 0.0842 0.8923 16 0.0839 0.0842 0.8924 17 0.0839 0.0842 0.8924 18 0.0839 0.0842 0.8925 19 0.0839 0.0841 0.8925 20 0.0839 0.0841 0.8925 21 0.0838 0.0841 0.8926 22 0.0838 0.0841 0.8926 23 0.0838 0.0841 0.8927 24 0.0838 0.0841 0.8927 25 0.0838 0.0841 0.8927 26 0.0838 0.0841 0.8927 27 0.0838 0.0841 0.8927 28 0.0838 0.0841 0.8928 29 0.0838 0.0841 0.8928 30 0.0838 0.0841 0.8928 31 0.0838 0.0841 0.8928 32 0.0838 0.0841 0.8928 33 0.0838 0.0841 0.8928 34 0.0838 0.0841 0.8928 35 0.0838 0.0841 0.8928 36 0.0838 0.0841 0.8928 37 0.0838 0.0841 0.8928 38 0.0838 0.0841 0.8928 39 0.0838 0.0841 0.8928 40 0.0838 0.0840 0.8928 41 0.0838 0.0840 0.8928 42 0.0838 0.0840 0.8928 43 0.0838 0.0840 0.8928 44 0.0838 0.0840 0.8929 45 0.0838 0.0840 0.8929 46 0.0838 0.0840 0.8929 47 0.0838 0.0840 0.8929 48 0.0838 0.0840 0.8929 49 0.0838 0.0840 0.8929 50 0.0838 0.0840 0.8929 wR2(int) = 0.0840 (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: 19548 total and 3132 unique reflections. plus 972 total and 570 unique reflections in fast scans Reflections rejected for which |I-|/su > 4.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 18124 total and 3130 unique reflections left after |I-|/su test plus 914 total and 558 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 0.0756 0.618 - 0.800 0.886 - 1.320 2.280 0.0676 14.8 914 848 2 62.4 0.0727 0.397 - 0.449 0.883 - 1.319 3.405 0.0676 14.8 577 554 3 77.4 0.0712 0.426 - 0.598 0.898 - 1.348 2.637 0.0676 14.8 790 771 4 62.4 0.0810 0.428 - 0.509 0.892 - 1.330 3.874 0.0676 14.8 575 544 5 62.4 0.0669 0.431 - 0.540 0.894 - 1.348 2.386 0.0676 14.8 604 583 6 77.4 0.0625 0.471 - 0.636 0.885 - 1.348 1.585 0.0676 14.8 802 789 7 58.9 0.0607 0.500 - 0.575 0.882 - 1.345 2.172 0.0676 14.8 648 632 8 77.4 0.0639 0.485 - 0.599 0.885 - 1.349 3.142 0.0676 14.8 751 718 9 58.9 0.0563 0.605 - 0.724 0.884 - 1.340 1.535 0.0676 14.8 670 662 10 77.4 0.0482 0.568 - 0.693 0.910 - 1.348 1.525 0.0676 14.8 766 752 11 77.4 0.0446 0.598 - 0.823 0.897 - 1.341 1.487 0.0676 14.8 801 786 12 62.4 0.0505 0.690 - 0.804 0.885 - 1.349 1.294 0.0676 14.8 687 679 13 58.9 0.0423 0.663 - 0.792 0.883 - 1.349 1.272 0.0676 14.8 772 753 14 58.9 0.0506 0.612 - 0.721 0.892 - 1.330 1.754 0.0676 14.8 675 655 15 58.9 0.0481 0.619 - 0.723 0.883 - 1.321 1.547 0.0676 14.8 681 668 16 77.4 0.0442 0.636 - 0.864 0.883 - 1.349 1.358 0.0676 14.8 800 788 17 77.4 0.0604 0.679 - 0.891 0.911 - 1.346 1.854 0.0676 14.8 816 786 18 47.4 0.0546 0.734 - 0.828 0.883 - 1.349 1.582 0.0676 14.8 685 649 19 58.9 0.0465 0.728 - 0.877 0.922 - 1.342 1.829 0.0676 14.8 655 624 20 77.4 0.0631 0.804 - 1.053 0.883 - 1.346 1.810 0.0676 14.8 755 733 21 47.4 0.0593 0.825 - 0.988 0.884 - 1.349 2.053 0.0676 14.8 694 650 22 47.4 0.0506 0.675 - 0.928 0.894 - 1.348 1.897 0.0676 14.8 655 599 23 77.4 0.0570 0.743 - 1.273 0.883 - 1.327 1.808 0.0676 14.8 2272 2217 24 77.4 0.0585 0.928 - 1.127 0.882 - 1.296 1.857 0.0676 14.8 993 972 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 neal054.eps Reflections not merged 0 Overloads replaced by fast scan measurements 18124 Corrected reflections written to file neal054_0m.hkl Estimated minimum and maximum transmission: 0.4887 0.7524 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000