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 rudi002_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.): 1.54163 14.169 14.278 21.327 89.758 72.195 74.865 149.06 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3789 85.16 2 55.00 0.8921 34.82 3 -89.50 0.8004 89.20 4 -89.50 0.8000 91.35 5 -89.50 0.8001 88.94 6 -89.50 0.8001 91.42 7 -89.50 0.8010 88.65 8 -89.50 0.8006 90.92 9 58.94 0.8743 91.71 10 -89.50 0.8000 89.36 11 58.94 0.8754 91.75 12 -74.50 0.8264 89.53 13 -89.50 0.8000 89.22 14 58.94 0.8749 90.28 15 58.94 0.8750 92.08 16 58.94 0.8741 91.85 17 58.94 0.8755 90.32 18 58.94 0.8758 91.39 19 58.94 0.8766 89.89 20 58.94 0.8761 90.93 21 58.94 0.8746 87.48 22 58.94 0.8749 90.01 23 58.94 0.8752 90.53 24 58.94 0.8758 92.20 25 58.94 0.8757 89.42 26 58.94 0.8763 91.19 27 58.94 0.8757 90.56 28 58.94 0.8750 90.98 ============================================================================== 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 148619 Reflections of which 15881 unique; 18.05 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 903 1000 1121 600 630 626 917 1116 8968 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 72 363 712 934 1755 3302 2161 1666 4916 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 139825 Reflections employed for parameter determination Effective data to parameter ratio = 15.14 wR2(int) = 0.1131 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1029 0.0951 0.8407 2 0.0932 0.0920 0.8496 3 0.0912 0.0909 0.8510 4 0.0905 0.0904 0.8514 5 0.0901 0.0902 0.8515 6 0.0899 0.0900 0.8516 7 0.0897 0.0899 0.8516 8 0.0896 0.0898 0.8517 9 0.0895 0.0897 0.8517 10 0.0895 0.0897 0.8517 11 0.0894 0.0896 0.8517 12 0.0894 0.0896 0.8516 13 0.0894 0.0896 0.8516 14 0.0893 0.0895 0.8516 15 0.0893 0.0895 0.8516 16 0.0893 0.0895 0.8516 17 0.0893 0.0895 0.8516 18 0.0893 0.0895 0.8515 19 0.0893 0.0895 0.8515 20 0.0893 0.0895 0.8515 21 0.0893 0.0895 0.8515 22 0.0893 0.0895 0.8515 23 0.0893 0.0895 0.8515 24 0.0892 0.0895 0.8515 25 0.0892 0.0895 0.8515 26 0.0892 0.0895 0.8515 27 0.0892 0.0894 0.8515 28 0.0892 0.0894 0.8515 29 0.0892 0.0894 0.8515 30 0.0892 0.0894 0.8515 31 0.0892 0.0894 0.8515 32 0.0892 0.0894 0.8515 33 0.0892 0.0894 0.8515 34 0.0892 0.0894 0.8515 35 0.0892 0.0894 0.8515 36 0.0892 0.0894 0.8515 37 0.0892 0.0894 0.8515 38 0.0892 0.0894 0.8515 39 0.0892 0.0894 0.8515 40 0.0892 0.0894 0.8515 41 0.0892 0.0894 0.8515 42 0.0892 0.0894 0.8515 43 0.0892 0.0894 0.8515 44 0.0892 0.0894 0.8515 45 0.0892 0.0894 0.8515 46 0.0892 0.0894 0.8515 47 0.0892 0.0894 0.8515 48 0.0892 0.0894 0.8515 49 0.0892 0.0894 0.8515 50 0.0892 0.0894 0.8515 wR2(int) = 0.0894 (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: 148619 total and 15881 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) 137355 total and 15875 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 0.0711 0.442 - 0.542 0.898 - 1.349 1.268 0.0637 15.7 3872 3336 2 55.0 0.2881 4.249 - 5.805 0.880 - 1.151 1.099 0.0637 15.7 4251 1755 3 -89.5 0.0595 0.588 - 0.766 0.879 - 1.349 1.154 0.0637 15.7 12606 11654 4 -89.5 0.0642 0.484 - 0.590 0.976 - 1.315 1.141 0.0637 15.7 3608 3380 5 -89.5 0.0700 0.675 - 0.749 0.879 - 1.138 1.200 0.0637 15.7 3730 3393 6 -89.5 0.0593 0.503 - 0.544 0.932 - 1.350 1.083 0.0637 15.7 3716 3508 7 -89.5 0.0658 0.573 - 0.678 0.880 - 1.166 1.229 0.0637 15.7 3574 3214 8 -89.5 0.0686 0.588 - 0.673 0.924 - 1.151 1.242 0.0637 15.7 3808 3508 9 58.9 0.0578 0.431 - 0.579 0.879 - 1.349 1.180 0.0637 15.7 10405 9772 10 -89.5 0.0524 0.661 - 0.885 0.879 - 1.349 0.945 0.0637 15.7 10099 9549 11 58.9 0.0551 0.498 - 0.566 0.976 - 1.349 0.977 0.0637 15.7 3009 2868 12 -74.5 0.0614 0.701 - 0.909 0.879 - 1.349 1.071 0.0637 15.7 9481 8815 13 -89.5 0.0564 0.637 - 0.853 0.879 - 1.349 0.979 0.0637 15.7 13583 12759 14 58.9 0.0606 0.505 - 0.546 0.881 - 1.138 1.170 0.0637 15.7 2791 2568 15 58.9 0.0560 0.476 - 0.544 0.933 - 1.138 1.046 0.0637 15.7 2895 2738 16 58.9 0.0612 0.493 - 0.580 0.976 - 1.200 1.129 0.0637 15.7 2864 2675 17 58.9 0.0530 0.508 - 0.699 0.879 - 1.348 1.113 0.0637 15.7 11102 10358 18 58.9 0.0561 0.492 - 0.527 0.880 - 1.138 1.027 0.0637 15.7 2988 2825 19 58.9 0.0566 0.487 - 0.602 0.926 - 1.151 1.139 0.0637 15.7 2886 2659 20 58.9 0.0627 0.516 - 0.578 0.979 - 1.341 1.218 0.0637 15.7 2894 2683 21 58.9 0.0562 0.587 - 0.808 0.927 - 1.292 1.183 0.0637 15.7 2695 2433 22 58.9 0.0631 0.561 - 0.596 0.880 - 1.145 1.219 0.0637 15.7 2981 2739 23 58.9 0.0516 0.519 - 0.595 0.968 - 1.349 0.985 0.0637 15.7 3035 2884 24 58.9 0.0555 0.501 - 0.558 0.922 - 1.145 1.060 0.0637 15.7 3064 2918 25 58.9 0.0501 0.532 - 0.598 0.903 - 1.301 1.084 0.0637 15.7 2642 2447 26 58.9 0.0622 0.506 - 0.610 0.976 - 1.231 1.142 0.0637 15.7 2904 2712 27 58.9 0.0588 0.530 - 0.571 0.947 - 1.349 1.182 0.0637 15.7 2874 2654 28 58.9 0.0557 0.502 - 0.579 0.880 - 1.146 1.109 0.0637 15.7 2998 2804 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 1.3789 85.16 2 55.00 0.8921 34.82 3 -89.50 0.8004 89.20 4 -89.50 0.8000 91.35 5 -89.50 0.8001 88.94 6 -89.50 0.8001 91.42 7 -89.50 0.8010 88.65 8 -89.50 0.8006 90.92 9 58.94 0.8743 91.71 10 -89.50 0.8000 89.36 11 58.94 0.8754 91.75 12 -74.50 0.8264 89.53 13 -89.50 0.8000 89.22 14 58.94 0.8749 90.28 15 58.94 0.8750 92.08 16 58.94 0.8741 91.85 17 58.94 0.8755 90.32 18 58.94 0.8758 91.39 19 58.94 0.8766 89.89 20 58.94 0.8761 90.93 21 58.94 0.8746 87.48 22 58.94 0.8749 90.01 23 58.94 0.8752 90.53 24 58.94 0.8758 92.20 25 58.94 0.8757 89.42 26 58.94 0.8763 91.19 27 58.94 0.8757 90.56 28 58.94 0.8750 90.98 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 139905 Reflections of which 15881 unique; 16.99 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 903 1000 1122 609 648 687 1013 1227 8672 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 71 359 693 905 1721 3257 2150 1634 5091 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 138600 Reflections employed for parameter determination Effective data to parameter ratio = 14.99 wR2(int) = 0.1120 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1020 0.0943 0.8467 2 0.0924 0.0912 0.8551 3 0.0905 0.0902 0.8564 4 0.0898 0.0897 0.8568 5 0.0894 0.0894 0.8569 6 0.0892 0.0893 0.8570 7 0.0890 0.0892 0.8570 8 0.0889 0.0891 0.8570 9 0.0889 0.0890 0.8570 10 0.0888 0.0890 0.8570 11 0.0888 0.0889 0.8570 12 0.0887 0.0889 0.8570 13 0.0887 0.0889 0.8570 14 0.0887 0.0889 0.8569 15 0.0887 0.0888 0.8569 16 0.0886 0.0888 0.8569 17 0.0886 0.0888 0.8569 18 0.0886 0.0888 0.8569 19 0.0886 0.0888 0.8569 20 0.0886 0.0888 0.8569 21 0.0886 0.0888 0.8569 22 0.0886 0.0888 0.8569 23 0.0886 0.0888 0.8569 24 0.0886 0.0888 0.8569 25 0.0886 0.0888 0.8569 26 0.0886 0.0888 0.8569 27 0.0886 0.0888 0.8569 28 0.0886 0.0888 0.8569 29 0.0886 0.0888 0.8569 30 0.0886 0.0888 0.8569 31 0.0886 0.0888 0.8569 32 0.0886 0.0888 0.8569 33 0.0886 0.0888 0.8568 34 0.0886 0.0888 0.8568 35 0.0886 0.0888 0.8568 36 0.0886 0.0888 0.8568 37 0.0886 0.0888 0.8568 38 0.0886 0.0888 0.8568 39 0.0886 0.0888 0.8568 40 0.0886 0.0888 0.8568 41 0.0886 0.0888 0.8568 42 0.0886 0.0888 0.8568 43 0.0886 0.0888 0.8568 44 0.0886 0.0888 0.8568 45 0.0886 0.0888 0.8568 46 0.0886 0.0888 0.8568 47 0.0886 0.0888 0.8568 48 0.0886 0.0888 0.8568 49 0.0886 0.0888 0.8568 50 0.0886 0.0888 0.8568 wR2(int) = 0.0888 (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: 139905 total and 15881 unique reflections assuming Friedel's law plus 5774 total and 2189 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) 130012 total and 15876 unique reflections left after |I-|/su test plus 5157 total and 2147 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 0.0725 0.522 - 0.642 0.897 - 1.324 1.386 0.0639 15.7 3438 2981 2f 55.0 0.1443 0.592 - 0.805 0.879 - 1.148 1.216 0.0639 15.7 1719 1111 3 -89.5 0.0594 0.575 - 0.744 0.878 - 1.324 1.140 0.0639 15.7 12719 11767 4 -89.5 0.0639 0.566 - 0.690 0.978 - 1.297 1.175 0.0639 15.7 3635 3391 5 -89.5 0.0701 0.607 - 0.674 0.878 - 1.145 1.213 0.0639 15.7 3751 3406 6 -89.5 0.0596 0.601 - 0.652 0.935 - 1.324 1.124 0.0639 15.7 3705 3488 7 -89.5 0.0658 0.595 - 0.706 0.879 - 1.160 1.264 0.0639 15.7 3600 3221 8 -89.5 0.0686 0.563 - 0.653 0.927 - 1.148 1.226 0.0639 15.7 3796 3500 9 58.9 0.0571 0.543 - 0.727 0.878 - 1.324 1.180 0.0639 15.7 10513 9860 10 -89.5 0.0526 0.572 - 0.762 0.878 - 1.324 0.932 0.0639 15.7 10167 9618 11 58.9 0.0556 0.583 - 0.669 0.977 - 1.323 0.995 0.0639 15.7 3009 2866 12 -74.5 0.0610 0.557 - 0.724 0.878 - 1.323 1.089 0.0639 15.7 9513 8829 13 -89.5 0.0559 0.545 - 0.728 0.878 - 1.324 0.978 0.0639 15.7 13724 12892 14 58.9 0.0609 0.595 - 0.642 0.880 - 1.145 1.176 0.0639 15.7 2811 2587 15 58.9 0.0555 0.582 - 0.666 0.932 - 1.140 1.092 0.0639 15.7 2911 2740 16 58.9 0.0603 0.570 - 0.672 0.977 - 1.175 1.128 0.0639 15.7 2884 2696 17 58.9 0.0539 0.545 - 0.751 0.878 - 1.323 1.112 0.0639 15.7 11209 10448 18 58.9 0.0556 0.607 - 0.650 0.879 - 1.140 1.009 0.0639 15.7 3003 2840 19 58.9 0.0561 0.524 - 0.644 0.926 - 1.148 1.120 0.0639 15.7 2882 2660 20 58.9 0.0633 0.579 - 0.648 0.984 - 1.317 1.233 0.0639 15.7 2888 2673 21 58.9 0.0547 0.510 - 0.699 0.927 - 1.263 1.138 0.0639 15.7 2691 2441 22 58.9 0.0623 0.602 - 0.639 0.878 - 1.148 1.160 0.0639 15.7 2998 2770 23 58.9 0.0517 0.576 - 0.668 0.971 - 1.323 0.975 0.0639 15.7 3037 2886 24 58.9 0.0552 0.590 - 0.663 0.922 - 1.150 1.014 0.0639 15.7 3085 2948 25 58.9 0.0498 0.564 - 0.639 0.903 - 1.285 1.095 0.0639 15.7 2677 2477 26 58.9 0.0612 0.564 - 0.685 0.977 - 1.209 1.163 0.0639 15.7 2925 2728 27 58.9 0.0594 0.591 - 0.637 0.951 - 1.323 1.196 0.0639 15.7 2867 2643 28 58.9 0.0554 0.577 - 0.666 0.879 - 1.147 1.055 0.0639 15.7 3012 2829 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 rudi002.eps Reflections not merged 0 Overloads replaced by fast scan measurements 130012 Corrected reflections written to file rudi002_0m.hkl Estimated minimum and maximum transmission: 0.4934 0.7538 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000