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/m for scaling Equivalent reflections defined by point group 2/m for error model Reading file rudi001_0m.raw Mean and maximum errors in direction cosine check function = 0.000 0.002 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 13.067 10.321 20.494 90.020 90.016 89.979 148.99 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3847 85.17 2 55.00 0.8927 51.50 3 -89.50 0.8001 85.65 4 -89.50 0.8001 82.32 5 -89.50 0.8012 80.27 6 -89.50 0.8006 82.30 7 58.94 0.8777 85.66 8 -89.50 0.8001 85.31 9 -89.50 0.8001 80.63 10 -89.50 0.8014 82.24 11 -74.50 0.8267 85.39 ============================================================================== 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 44485 Reflections of which 5933 unique; 12.77 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 254 365 450 539 541 510 516 603 2155 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 93 524 368 244 456 865 637 551 2195 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 38980 Reflections employed for parameter determination Effective data to parameter ratio = 9.62 wR2(int) = 0.1378 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1173 0.0961 0.8297 2 0.0906 0.0844 0.8684 3 0.0816 0.0787 0.8807 4 0.0772 0.0755 0.8862 5 0.0746 0.0737 0.8890 6 0.0732 0.0727 0.8906 7 0.0724 0.0721 0.8915 8 0.0719 0.0717 0.8920 9 0.0715 0.0715 0.8923 10 0.0714 0.0714 0.8925 11 0.0712 0.0713 0.8926 12 0.0712 0.0712 0.8927 13 0.0711 0.0712 0.8927 14 0.0711 0.0711 0.8927 15 0.0710 0.0711 0.8927 16 0.0710 0.0711 0.8928 17 0.0710 0.0711 0.8928 18 0.0710 0.0711 0.8928 19 0.0710 0.0711 0.8928 20 0.0710 0.0711 0.8928 21 0.0710 0.0711 0.8928 22 0.0710 0.0711 0.8928 23 0.0710 0.0711 0.8928 24 0.0710 0.0711 0.8928 25 0.0710 0.0711 0.8928 26 0.0710 0.0711 0.8928 27 0.0710 0.0711 0.8928 28 0.0710 0.0711 0.8928 29 0.0710 0.0711 0.8928 30 0.0710 0.0711 0.8928 31 0.0710 0.0711 0.8928 32 0.0710 0.0711 0.8928 33 0.0710 0.0711 0.8928 34 0.0710 0.0711 0.8928 35 0.0710 0.0711 0.8928 36 0.0710 0.0711 0.8928 37 0.0710 0.0711 0.8928 38 0.0710 0.0711 0.8928 39 0.0710 0.0711 0.8928 40 0.0710 0.0711 0.8928 41 0.0710 0.0711 0.8927 42 0.0710 0.0711 0.8927 43 0.0710 0.0711 0.8927 44 0.0710 0.0711 0.8927 45 0.0710 0.0711 0.8927 46 0.0710 0.0711 0.8927 47 0.0710 0.0711 0.8927 48 0.0710 0.0711 0.8927 49 0.0710 0.0711 0.8927 50 0.0710 0.0711 0.8927 wR2(int) = 0.0711 (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: 44485 total and 5933 unique reflections assuming Friedel's law Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 42778 total and 5932 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 0.0 0.0503 0.488 - 0.599 0.799 - 1.419 1.061 0.0564 17.7 2819 2479 2 55.0 0.1256 4.035 - 6.051 0.813 - 1.461 1.126 0.0564 17.7 2970 1648 3 -89.5 0.0407 0.556 - 0.786 0.799 - 1.421 0.886 0.0564 17.7 6147 5573 4 -89.5 0.0636 0.548 - 0.687 0.822 - 1.462 1.175 0.0564 17.7 2742 2299 5 -89.5 0.0493 0.681 - 0.746 0.805 - 1.462 0.984 0.0564 17.7 2752 2322 6 -89.5 0.0515 0.558 - 0.899 0.810 - 1.462 0.969 0.0564 17.7 2776 2417 7 58.9 0.0483 0.493 - 0.657 0.799 - 1.461 1.071 0.0564 17.7 4382 3895 8 -89.5 0.0386 0.646 - 0.866 0.799 - 1.425 0.868 0.0564 17.7 5746 5189 9 -89.5 0.0453 0.623 - 0.720 0.799 - 1.462 0.914 0.0564 17.7 2801 2396 10 -89.5 0.0517 0.668 - 0.825 0.826 - 1.462 1.012 0.0564 17.7 2693 2323 11 -74.5 0.0455 0.567 - 0.900 0.799 - 1.443 0.928 0.0564 17.7 6950 6237 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. Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3847 85.17 2 55.00 0.8927 51.50 3 -89.50 0.8001 85.65 4 -89.50 0.8001 82.32 5 -89.50 0.8012 80.27 6 -89.50 0.8006 82.30 7 58.94 0.8777 85.66 8 -89.50 0.8001 85.31 9 -89.50 0.8001 80.63 10 -89.50 0.8014 82.24 11 -74.50 0.8267 85.39 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 38446 Reflections of which 5931 unique; 11.04 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 270 402 514 625 599 594 591 659 1677 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 90 508 362 216 441 846 639 520 2309 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 37763 Reflections employed for parameter determination Effective data to parameter ratio = 9.28 wR2(int) = 0.1380 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1168 0.0951 0.8404 2 0.0897 0.0835 0.8792 3 0.0808 0.0778 0.8912 4 0.0763 0.0746 0.8967 5 0.0737 0.0727 0.8995 6 0.0722 0.0716 0.9012 7 0.0713 0.0709 0.9022 8 0.0707 0.0705 0.9028 9 0.0703 0.0702 0.9032 10 0.0701 0.0700 0.9035 11 0.0699 0.0699 0.9036 12 0.0698 0.0698 0.9037 13 0.0697 0.0697 0.9038 14 0.0697 0.0697 0.9039 15 0.0696 0.0697 0.9039 16 0.0696 0.0696 0.9039 17 0.0696 0.0696 0.9039 18 0.0696 0.0696 0.9040 19 0.0695 0.0696 0.9040 20 0.0695 0.0696 0.9040 21 0.0695 0.0696 0.9040 22 0.0695 0.0696 0.9040 23 0.0695 0.0696 0.9040 24 0.0695 0.0696 0.9040 25 0.0695 0.0696 0.9040 26 0.0695 0.0696 0.9040 27 0.0695 0.0696 0.9040 28 0.0695 0.0696 0.9040 29 0.0695 0.0696 0.9040 30 0.0695 0.0696 0.9040 31 0.0695 0.0696 0.9040 32 0.0695 0.0696 0.9040 33 0.0695 0.0696 0.9040 34 0.0695 0.0696 0.9040 35 0.0695 0.0696 0.9040 36 0.0695 0.0696 0.9040 37 0.0695 0.0696 0.9040 38 0.0695 0.0696 0.9040 39 0.0695 0.0696 0.9040 40 0.0695 0.0696 0.9040 41 0.0695 0.0696 0.9040 42 0.0695 0.0696 0.9040 43 0.0695 0.0696 0.9040 44 0.0695 0.0696 0.9040 45 0.0695 0.0696 0.9040 46 0.0695 0.0696 0.9040 47 0.0695 0.0696 0.9040 48 0.0695 0.0696 0.9040 49 0.0695 0.0696 0.9040 50 0.0695 0.0696 0.9040 wR2(int) = 0.0696 (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: 38446 total and 5931 unique reflections assuming Friedel's law plus 3973 total and 913 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) 37283 total and 5925 unique reflections left after |I-|/su test plus 3669 total and 907 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 0.0545 0.658 - 0.818 0.792 - 1.394 1.309 0.0554 18.0 2481 2147 2f 55.0 0.0793 0.618 - 0.909 0.820 - 1.398 1.167 0.0554 18.0 1188 836 3 -89.5 0.0396 0.662 - 0.937 0.791 - 1.407 0.888 0.0554 18.0 6196 5608 4 -89.5 0.0638 0.581 - 0.730 0.819 - 1.458 1.234 0.0554 18.0 2781 2316 5 -89.5 0.0489 0.661 - 0.729 0.799 - 1.458 1.012 0.0554 18.0 2788 2337 6 -89.5 0.0489 0.566 - 0.910 0.799 - 1.458 0.971 0.0554 18.0 2801 2438 7 58.9 0.0471 0.647 - 0.856 0.792 - 1.458 1.063 0.0554 18.0 4425 3931 8 -89.5 0.0381 0.643 - 0.869 0.792 - 1.426 0.871 0.0554 18.0 5801 5223 9 -89.5 0.0471 0.645 - 0.734 0.792 - 1.458 0.913 0.0554 18.0 2801 2395 10 -89.5 0.0508 0.659 - 0.816 0.820 - 1.458 1.009 0.0554 18.0 2713 2339 11 -74.5 0.0459 0.614 - 0.965 0.792 - 1.440 0.938 0.0554 18.0 6977 6242 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 rudi001.eps Reflections not merged 3 Overloads replaced by fast scan measurements 37286 Corrected reflections written to file rudi001_0m.hkl Estimated minimum and maximum transmission: 0.4058 0.7538 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000