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 gore001_0m.raw Mean and maximum errors in direction cosine check function = 0.000 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.): 1.54181 5.309 18.173 6.266 90.024 98.857 89.996 144.20 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.3928 99.05 2 0.00 1.3506 94.11 3 -84.57 0.8102 99.07 4 -84.57 0.8100 99.70 5 -84.57 0.8108 99.82 6 -84.57 0.8116 98.75 7 -84.57 0.8102 100.00 8 -84.57 0.8102 99.60 9 -84.57 0.8112 99.83 10 62.55 0.8492 100.00 11 62.55 0.8476 99.88 12 62.55 0.8463 99.76 ============================================================================== 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 8469 Reflections of which 2322 unique; 7.96 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 264 464 533 512 230 100 60 65 94 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 4 2 2 1 4 18 25 35 2231 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 8161 Reflections employed for parameter determination Effective data to parameter ratio = 5.54 wR2(int) = 0.1141 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.0960 0.0804 0.9016 2 0.0770 0.0752 0.9133 3 0.0737 0.0731 0.9157 4 0.0718 0.0716 0.9174 5 0.0709 0.0709 0.9181 6 0.0705 0.0705 0.9186 7 0.0701 0.0703 0.9189 8 0.0699 0.0701 0.9192 9 0.0698 0.0700 0.9194 10 0.0697 0.0699 0.9194 11 0.0697 0.0699 0.9195 12 0.0697 0.0698 0.9196 13 0.0696 0.0698 0.9197 14 0.0696 0.0698 0.9198 15 0.0696 0.0698 0.9198 16 0.0696 0.0698 0.9198 17 0.0696 0.0697 0.9199 18 0.0696 0.0697 0.9199 19 0.0695 0.0697 0.9199 20 0.0695 0.0697 0.9199 21 0.0695 0.0697 0.9199 22 0.0695 0.0697 0.9199 23 0.0695 0.0696 0.9198 24 0.0695 0.0696 0.9198 25 0.0695 0.0697 0.9198 26 0.0695 0.0697 0.9198 27 0.0695 0.0697 0.9198 28 0.0695 0.0697 0.9198 29 0.0695 0.0697 0.9198 30 0.0695 0.0697 0.9199 31 0.0695 0.0697 0.9199 32 0.0695 0.0697 0.9199 33 0.0695 0.0697 0.9199 34 0.0695 0.0697 0.9199 35 0.0695 0.0697 0.9199 36 0.0695 0.0697 0.9199 37 0.0695 0.0697 0.9199 38 0.0695 0.0697 0.9199 39 0.0695 0.0697 0.9199 40 0.0695 0.0697 0.9199 41 0.0695 0.0697 0.9199 42 0.0695 0.0697 0.9199 43 0.0695 0.0697 0.9199 44 0.0695 0.0697 0.9199 45 0.0695 0.0697 0.9199 46 0.0696 0.0697 0.9199 47 0.0696 0.0697 0.9199 48 0.0696 0.0697 0.9199 49 0.0696 0.0697 0.9199 50 0.0696 0.0697 0.9199 wR2(int) = 0.0697 (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: 8469 total and 2322 unique reflections. Reflections rejected for which |I-|/su > 4.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 7899 total and 2282 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 0.0376 0.599 - 0.678 0.912 - 1.159 2.078 0.0591 16.9 615 610 2 0.0 0.0476 6.812 - 8.090 0.907 - 1.164 1.407 0.0591 16.9 683 643 3 -84.6 0.0420 0.624 - 0.713 0.965 - 1.143 3.933 0.0591 16.9 393 389 4 -84.6 0.0446 0.570 - 0.737 0.907 - 1.168 5.040 0.0591 16.9 1236 1221 5 -84.6 0.0549 0.553 - 0.662 0.960 - 1.167 5.794 0.0591 16.9 485 481 6 -84.6 0.0550 0.640 - 0.789 0.933 - 1.168 6.827 0.0591 16.9 495 480 7 -84.6 0.0441 0.600 - 0.646 0.914 - 1.168 4.367 0.0591 16.9 505 503 8 -84.6 0.0424 0.468 - 0.770 0.907 - 1.167 2.388 0.0591 16.9 1427 1422 9 -84.6 0.0527 0.645 - 0.767 0.909 - 1.167 6.931 0.0591 16.9 512 496 10 62.6 0.0392 0.624 - 0.734 0.964 - 1.168 1.878 0.0591 16.9 374 374 11 62.6 0.0379 0.611 - 0.703 0.912 - 1.167 2.609 0.0591 16.9 793 792 12 62.6 0.0420 0.661 - 0.726 0.964 - 1.168 2.963 0.0591 16.9 381 379 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 1.3928 99.05 2 0.00 1.3506 94.11 3 -84.57 0.8102 99.07 4 -84.57 0.8100 99.70 5 -84.57 0.8108 99.82 6 -84.57 0.8116 98.75 7 -84.57 0.8102 100.00 8 -84.57 0.8102 99.60 9 -84.57 0.8112 99.83 10 62.55 0.8492 100.00 11 62.55 0.8476 99.88 12 62.55 0.8463 99.76 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 7139 Reflections of which 2202 unique; 6.72 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 311 461 547 494 210 89 38 34 18 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 4 2 2 0 5 14 23 32 2120 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 8018 Reflections employed for parameter determination Effective data to parameter ratio = 5.43 wR2(int) = 0.1148 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.0950 0.0795 0.9063 2 0.0764 0.0745 0.9166 3 0.0732 0.0727 0.9186 4 0.0714 0.0713 0.9202 5 0.0706 0.0706 0.9209 6 0.0701 0.0701 0.9213 7 0.0697 0.0698 0.9216 8 0.0695 0.0697 0.9219 9 0.0694 0.0696 0.9221 10 0.0693 0.0695 0.9222 11 0.0693 0.0695 0.9223 12 0.0692 0.0694 0.9225 13 0.0692 0.0694 0.9226 14 0.0692 0.0694 0.9227 15 0.0692 0.0693 0.9228 16 0.0691 0.0693 0.9229 17 0.0691 0.0692 0.9229 18 0.0690 0.0692 0.9229 19 0.0690 0.0692 0.9230 20 0.0690 0.0692 0.9230 21 0.0690 0.0692 0.9230 22 0.0690 0.0692 0.9230 23 0.0690 0.0692 0.9231 24 0.0690 0.0692 0.9232 25 0.0690 0.0692 0.9232 26 0.0691 0.0692 0.9232 27 0.0691 0.0692 0.9232 28 0.0691 0.0692 0.9232 29 0.0691 0.0692 0.9232 30 0.0691 0.0692 0.9232 31 0.0691 0.0692 0.9232 32 0.0691 0.0692 0.9232 33 0.0691 0.0692 0.9232 34 0.0691 0.0693 0.9232 35 0.0691 0.0693 0.9232 36 0.0691 0.0693 0.9232 37 0.0691 0.0693 0.9232 38 0.0691 0.0693 0.9232 39 0.0691 0.0693 0.9232 40 0.0691 0.0693 0.9232 41 0.0691 0.0693 0.9232 42 0.0691 0.0693 0.9231 43 0.0691 0.0693 0.9231 44 0.0691 0.0693 0.9231 45 0.0691 0.0693 0.9231 46 0.0691 0.0693 0.9231 47 0.0691 0.0693 0.9231 48 0.0691 0.0693 0.9231 49 0.0691 0.0693 0.9231 50 0.0691 0.0693 0.9231 wR2(int) = 0.0693 (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: 7139 total and 2202 unique reflections. plus 1182 total and 385 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) 6610 total and 2161 unique reflections left after |I-|/su test plus 1089 total and 376 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 0.0444 0.701 - 0.818 0.939 - 1.172 3.841 0.0593 16.8 508 497 2f 0.0 0.0514 0.676 - 0.838 0.907 - 1.179 1.968 0.0593 16.8 581 546 3 -84.6 0.0398 0.710 - 0.809 0.951 - 1.156 3.742 0.0593 16.8 396 392 4 -84.6 0.0412 0.743 - 0.947 0.907 - 1.178 4.884 0.0593 16.8 1233 1221 5 -84.6 0.0509 0.704 - 0.840 0.947 - 1.176 4.846 0.0593 16.8 490 487 6 -84.6 0.0536 0.631 - 0.779 0.943 - 1.181 6.935 0.0593 16.8 498 483 7 -84.6 0.0395 0.706 - 0.764 0.914 - 1.180 3.702 0.0593 16.8 506 504 8 -84.6 0.0396 0.654 - 1.075 0.907 - 1.180 2.363 0.0593 16.8 1430 1425 9 -84.6 0.0516 0.607 - 0.723 0.914 - 1.181 5.189 0.0593 16.8 512 502 10 62.6 0.0395 0.659 - 0.775 0.961 - 1.180 2.627 0.0593 16.8 373 372 11 62.6 0.0354 0.732 - 0.857 0.919 - 1.181 2.586 0.0593 16.8 793 792 12 62.6 0.0427 0.661 - 0.726 0.958 - 1.181 2.751 0.0593 16.8 379 377 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 gore001.eps ** R(int) could not be plotted for 1 scans - insufficient common reflections Reflections not merged 184 Overloads replaced by fast scan measurements 6794 Corrected reflections written to file gore001_0m.hkl Estimated minimum and maximum transmission: 0.5739 0.7536 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000