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 -1 for scaling Equivalent reflections defined by point group -1 for error model Reading file rudi004_0m.raw Mean and maximum errors in direction cosine check function = 0.001 0.003 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.): 1.54173 11.935 13.017 19.202 93.964 98.585 97.103 148.91 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3935 89.46 2 55.00 0.8929 53.65 3 -89.50 0.8001 79.83 4 -89.50 0.8004 78.25 5 -89.50 0.8003 78.81 6 -89.50 0.8003 76.34 7 -89.50 0.8006 74.99 8 -89.50 0.8004 76.47 9 58.94 0.8744 81.49 10 -89.50 0.8003 81.47 11 58.94 0.8752 78.05 12 -89.50 0.8001 79.97 13 -74.50 0.8271 82.22 14 58.94 0.8749 79.20 15 58.94 0.8790 78.75 16 58.94 0.8773 77.60 17 58.94 0.8750 82.45 18 58.94 0.8757 78.54 19 58.94 0.8770 79.56 20 58.94 0.8752 77.85 21 -59.50 0.8794 77.32 22 58.94 0.8767 77.70 23 58.94 0.8778 77.99 24 58.94 0.8750 77.34 ============================================================================== 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 100300 Reflections of which 11745 unique; 25.30 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 635 742 869 511 621 605 837 1033 5892 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 263 1051 782 689 1072 2173 1501 1043 3171 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 86389 Reflections employed for parameter determination Effective data to parameter ratio = 19.09 wR2(int) = 0.1477 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1291 0.1046 0.7886 2 0.1001 0.0934 0.8338 3 0.0906 0.0868 0.8509 4 0.0847 0.0825 0.8591 5 0.0812 0.0801 0.8631 6 0.0793 0.0788 0.8650 7 0.0783 0.0781 0.8659 8 0.0777 0.0777 0.8664 9 0.0774 0.0774 0.8667 10 0.0772 0.0773 0.8668 11 0.0771 0.0772 0.8669 12 0.0770 0.0771 0.8670 13 0.0769 0.0771 0.8670 14 0.0769 0.0770 0.8671 15 0.0768 0.0770 0.8671 16 0.0768 0.0770 0.8671 17 0.0768 0.0770 0.8671 18 0.0768 0.0770 0.8671 19 0.0768 0.0770 0.8671 20 0.0768 0.0770 0.8671 21 0.0768 0.0770 0.8671 22 0.0768 0.0770 0.8672 23 0.0768 0.0770 0.8672 24 0.0768 0.0770 0.8672 25 0.0768 0.0770 0.8672 26 0.0768 0.0770 0.8672 27 0.0768 0.0770 0.8672 28 0.0768 0.0770 0.8672 29 0.0768 0.0770 0.8672 30 0.0768 0.0770 0.8672 31 0.0768 0.0770 0.8672 32 0.0768 0.0770 0.8672 33 0.0768 0.0770 0.8671 34 0.0768 0.0770 0.8671 35 0.0768 0.0770 0.8671 36 0.0768 0.0770 0.8671 37 0.0768 0.0770 0.8671 38 0.0768 0.0770 0.8671 39 0.0768 0.0770 0.8671 40 0.0768 0.0770 0.8671 41 0.0768 0.0770 0.8671 42 0.0768 0.0770 0.8671 43 0.0768 0.0770 0.8671 44 0.0768 0.0770 0.8671 45 0.0768 0.0770 0.8671 46 0.0768 0.0770 0.8671 47 0.0768 0.0770 0.8671 48 0.0768 0.0770 0.8671 49 0.0768 0.0770 0.8671 50 0.0768 0.0770 0.8671 wR2(int) = 0.0770 (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: 100300 total and 11745 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) 96336 total and 11740 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 0.0534 0.527 - 0.671 0.782 - 1.520 1.190 0.0568 17.6 2892 2599 2 55.0 0.1364 5.488 - 6.981 0.772 - 1.520 1.057 0.0568 17.6 3041 1789 3 -89.5 0.0440 0.542 - 0.849 0.772 - 1.525 0.888 0.0568 17.6 9936 8520 4 -89.5 0.0642 0.598 - 0.841 0.773 - 1.525 1.163 0.0568 17.6 2993 2435 5 -89.5 0.0776 0.594 - 0.645 0.799 - 1.525 1.271 0.0568 17.6 2843 2256 6 -89.5 0.0561 0.633 - 0.722 0.772 - 1.525 1.057 0.0568 17.6 2966 2395 7 -89.5 0.0645 0.699 - 0.838 0.773 - 1.525 1.057 0.0568 17.6 2897 2309 8 -89.5 0.0613 0.630 - 0.728 0.782 - 1.519 1.062 0.0568 17.6 2928 2365 9 58.9 0.0486 0.504 - 0.690 0.773 - 1.524 0.967 0.0568 17.6 8459 7308 10 -89.5 0.0447 0.553 - 0.966 0.772 - 1.525 0.867 0.0568 17.6 7626 6630 11 58.9 0.0732 0.561 - 0.815 0.791 - 1.526 1.192 0.0568 17.6 2154 1709 12 -89.5 0.0453 0.552 - 0.902 0.772 - 1.526 0.872 0.0568 17.6 9978 8568 13 -74.5 0.0498 0.547 - 0.966 0.772 - 1.525 0.969 0.0568 17.6 7451 6421 14 58.9 0.0582 0.549 - 0.666 0.772 - 1.524 1.010 0.0568 17.6 2240 1873 15 58.9 0.0752 0.548 - 0.673 0.825 - 1.524 1.201 0.0568 17.6 2146 1731 16 58.9 0.0637 0.611 - 0.748 0.783 - 1.527 1.069 0.0568 17.6 2199 1793 17 58.9 0.0466 0.499 - 0.761 0.772 - 1.525 0.942 0.0568 17.6 8787 7671 18 58.9 0.0565 0.556 - 0.656 0.772 - 1.524 1.044 0.0568 17.6 2199 1820 19 58.9 0.0677 0.570 - 0.618 0.782 - 1.527 1.189 0.0568 17.6 2115 1719 20 58.9 0.0702 0.673 - 0.788 0.788 - 1.526 1.255 0.0568 17.6 2147 1692 21 -59.5 0.0647 0.725 - 0.870 0.783 - 1.527 1.146 0.0568 17.6 1882 1501 22 58.9 0.0657 0.571 - 0.791 0.781 - 1.526 1.136 0.0568 17.6 2107 1687 23 58.9 0.0546 0.575 - 0.668 0.773 - 1.517 1.047 0.0568 17.6 2242 1858 24 58.9 0.0662 0.632 - 0.786 0.773 - 1.524 1.140 0.0568 17.6 2108 1689 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 1.3935 89.46 2 55.00 0.8929 53.65 3 -89.50 0.8001 79.83 4 -89.50 0.8004 78.25 5 -89.50 0.8003 78.81 6 -89.50 0.8003 76.34 7 -89.50 0.8006 74.99 8 -89.50 0.8004 76.47 9 58.94 0.8744 81.49 10 -89.50 0.8003 81.47 11 58.94 0.8752 78.05 12 -89.50 0.8001 79.97 13 -74.50 0.8271 82.22 14 58.94 0.8749 79.20 15 58.94 0.8790 78.75 16 58.94 0.8773 77.60 17 58.94 0.8750 82.45 18 58.94 0.8757 78.54 19 58.94 0.8770 79.56 20 58.94 0.8752 77.85 21 -59.50 0.8794 77.32 22 58.94 0.8767 77.70 23 58.94 0.8778 77.99 24 58.94 0.8750 77.34 Fast scans: 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 97139 Reflections of which 11745 unique; 24.51 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 635 742 870 522 650 647 936 1110 5633 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 261 1044 769 683 1053 2163 1493 1029 3250 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 85366 Reflections employed for parameter determination Effective data to parameter ratio = 18.83 wR2(int) = 0.1477 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1290 0.1044 0.7918 2 0.0999 0.0933 0.8370 3 0.0904 0.0866 0.8542 4 0.0845 0.0823 0.8625 5 0.0810 0.0798 0.8665 6 0.0791 0.0785 0.8684 7 0.0780 0.0778 0.8693 8 0.0774 0.0773 0.8698 9 0.0771 0.0771 0.8701 10 0.0769 0.0769 0.8703 11 0.0767 0.0768 0.8704 12 0.0767 0.0768 0.8704 13 0.0766 0.0767 0.8705 14 0.0766 0.0767 0.8705 15 0.0765 0.0767 0.8705 16 0.0765 0.0767 0.8705 17 0.0765 0.0767 0.8706 18 0.0765 0.0767 0.8706 19 0.0765 0.0767 0.8706 20 0.0765 0.0767 0.8706 21 0.0765 0.0766 0.8706 22 0.0765 0.0766 0.8706 23 0.0765 0.0766 0.8706 24 0.0765 0.0766 0.8706 25 0.0765 0.0766 0.8706 26 0.0765 0.0766 0.8706 27 0.0765 0.0766 0.8706 28 0.0765 0.0766 0.8706 29 0.0765 0.0766 0.8706 30 0.0765 0.0766 0.8706 31 0.0765 0.0766 0.8706 32 0.0765 0.0766 0.8706 33 0.0765 0.0766 0.8706 34 0.0765 0.0766 0.8706 35 0.0765 0.0766 0.8706 36 0.0765 0.0766 0.8706 37 0.0765 0.0766 0.8706 38 0.0765 0.0766 0.8706 39 0.0765 0.0766 0.8706 40 0.0765 0.0766 0.8706 41 0.0765 0.0766 0.8706 42 0.0765 0.0766 0.8706 43 0.0765 0.0766 0.8706 44 0.0765 0.0766 0.8706 45 0.0765 0.0766 0.8706 46 0.0765 0.0766 0.8706 47 0.0765 0.0766 0.8706 48 0.0765 0.0766 0.8706 49 0.0765 0.0766 0.8706 50 0.0765 0.0766 0.8706 wR2(int) = 0.0766 (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: 97139 total and 11745 unique reflections assuming Friedel's law plus 1289 total and 1180 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) 93369 total and 11739 unique reflections left after |I-|/su test plus 1208 total and 1122 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) 1 0.0 0.0531 0.604 - 0.770 0.781 - 1.518 1.181 0.0560 17.8 2887 2597 2f 55.0 0.0798 0.645 - 0.828 0.772 - 1.517 1.135 0.0560 17.8 1208 930 3 -89.5 0.0438 0.598 - 0.938 0.772 - 1.523 0.888 0.0560 17.8 9957 8538 4 -89.5 0.0644 0.560 - 0.788 0.773 - 1.523 1.175 0.0560 17.8 2993 2431 5 -89.5 0.0774 0.566 - 0.615 0.798 - 1.523 1.270 0.0560 17.8 2840 2254 6 -89.5 0.0560 0.597 - 0.680 0.773 - 1.523 1.051 0.0560 17.8 2969 2397 7 -89.5 0.0643 0.651 - 0.781 0.773 - 1.523 1.051 0.0560 17.8 2896 2312 8 -89.5 0.0613 0.600 - 0.694 0.781 - 1.517 1.114 0.0560 17.8 2928 2347 9 58.9 0.0488 0.577 - 0.790 0.773 - 1.522 0.972 0.0560 17.8 8468 7309 10 -89.5 0.0445 0.587 - 1.026 0.772 - 1.523 0.865 0.0560 17.8 7639 6640 11 58.9 0.0735 0.480 - 0.696 0.790 - 1.524 1.212 0.0560 17.8 2154 1703 12 -89.5 0.0450 0.598 - 0.977 0.772 - 1.523 0.877 0.0560 17.8 9996 8575 13 -74.5 0.0497 0.586 - 1.036 0.772 - 1.523 0.951 0.0560 17.8 7455 6441 14 58.9 0.0581 0.589 - 0.715 0.773 - 1.521 1.025 0.0560 17.8 2242 1871 15 58.9 0.0738 0.549 - 0.674 0.825 - 1.522 1.155 0.0560 17.8 2141 1739 16 58.9 0.0630 0.564 - 0.691 0.781 - 1.525 1.052 0.0560 17.8 2198 1795 17 58.9 0.0466 0.577 - 0.881 0.773 - 1.523 0.942 0.0560 17.8 8799 7676 18 58.9 0.0568 0.582 - 0.687 0.773 - 1.522 1.001 0.0560 17.8 2199 1836 19 58.9 0.0676 0.612 - 0.662 0.781 - 1.524 1.195 0.0560 17.8 2117 1720 20 58.9 0.0702 0.584 - 0.685 0.788 - 1.524 1.242 0.0560 17.8 2145 1694 21 -59.5 0.0652 0.668 - 0.802 0.782 - 1.524 1.137 0.0560 17.8 1883 1506 22 58.9 0.0653 0.512 - 0.710 0.781 - 1.524 1.135 0.0560 17.8 2111 1692 23 58.9 0.0546 0.577 - 0.670 0.773 - 1.516 1.044 0.0560 17.8 2245 1859 24 58.9 0.0656 0.585 - 0.729 0.774 - 1.522 1.156 0.0560 17.8 2107 1683 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 rudi004.eps Reflections not merged 0 Overloads replaced by fast scan measurements 93369 Corrected reflections written to file rudi004_0m.hkl Estimated minimum and maximum transmission: 0.3773 0.7538 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000