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 xray072_0m.raw Mean and maximum errors in direction cosine check function = 0.000 0.004 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 8.090 7.049 8.221 89.993 103.023 90.003 144.22 Scan 2-theta high res %[I>3sig(I)] 1 0.00 1.4077 98.40 2 0.00 1.3362 91.15 3 -84.57 0.8104 99.77 4 -84.57 0.8113 99.76 5 -84.57 0.8101 100.00 6 -84.57 0.8101 100.00 7 -84.57 0.8129 99.60 8 -84.57 0.8101 99.79 9 54.57 0.8760 99.81 10 62.55 0.8463 100.00 11 62.55 0.8516 100.00 12 -84.57 0.8105 98.95 13 62.55 0.8503 98.86 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 5931 Reflections of which 954 unique; 1.84 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 53 76 97 97 101 89 100 122 219 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 0 0 0 1 6 27 29 26 865 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 6793 Reflections employed for parameter determination Effective data to parameter ratio = 1.80 wR2(int) = 0.1573 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.1434 0.1227 0.7118 2 0.1169 0.1116 0.7812 3 0.1084 0.1066 0.8078 4 0.1052 0.1044 0.8184 5 0.1035 0.1032 0.8246 6 0.1025 0.1023 0.8289 7 0.1018 0.1017 0.8322 8 0.1013 0.1013 0.8348 9 0.1010 0.1011 0.8370 10 0.1008 0.1011 0.8392 11 0.1008 0.1009 0.8416 12 0.1004 0.1005 0.8432 13 0.1001 0.1004 0.8442 14 0.1001 0.1004 0.8452 15 0.1001 0.1004 0.8462 16 0.1000 0.1003 0.8470 17 0.1000 0.1003 0.8476 18 0.0999 0.1002 0.8481 19 0.0998 0.1001 0.8485 20 0.0997 0.1000 0.8487 21 0.0997 0.1000 0.8490 22 0.0997 0.0999 0.8493 23 0.0996 0.0999 0.8494 24 0.0995 0.0998 0.8496 25 0.0995 0.0998 0.8497 26 0.0995 0.0998 0.8498 27 0.0994 0.0997 0.8498 28 0.0994 0.0997 0.8499 29 0.0994 0.0997 0.8500 30 0.0994 0.0997 0.8501 31 0.0994 0.0997 0.8501 32 0.0994 0.0997 0.8502 33 0.0994 0.0997 0.8502 34 0.0994 0.0997 0.8503 35 0.0994 0.0997 0.8505 36 0.0993 0.0997 0.8505 37 0.0993 0.0997 0.8506 38 0.0993 0.0997 0.8506 39 0.0993 0.0997 0.8507 40 0.0993 0.0997 0.8507 41 0.0993 0.0997 0.8507 42 0.0993 0.0997 0.8507 43 0.0993 0.0997 0.8508 44 0.0993 0.0997 0.8508 45 0.0993 0.0997 0.8508 46 0.0993 0.0997 0.8508 47 0.0993 0.0997 0.8508 48 0.0993 0.0997 0.8508 49 0.0993 0.0997 0.8508 50 0.0993 0.0997 0.8509 wR2(int) = 0.0997 (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: 5931 total and 954 unique reflections assuming Friedel's law plus 929 total and 152 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) 4918 total and 948 unique reflections left after |I-|/su test plus 575 total and 147 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 0.0791 0.338 - 0.445 0.670 - 1.598 3.755 0.0780 12.8 255 240 2f 0.0 0.0826 2.936 - 3.578 0.684 - 1.626 2.348 0.0780 12.8 320 279 3 -84.6 0.0567 0.323 - 0.416 0.666 - 1.573 1.284 0.0780 12.8 376 375 4 -84.6 0.0590 0.312 - 0.482 0.681 - 1.618 1.841 0.0780 12.8 702 700 5 -84.6 0.0602 0.390 - 0.458 0.751 - 1.584 2.135 0.0780 12.8 375 372 6 -84.6 0.0597 0.384 - 0.445 0.667 - 1.586 1.797 0.0780 12.8 419 418 7 -84.6 0.0552 0.340 - 0.424 0.668 - 1.607 1.467 0.0780 12.8 456 454 8 -84.6 0.0576 0.370 - 0.409 0.669 - 1.477 1.477 0.0780 12.8 449 448 9 54.6 0.0599 0.318 - 0.690 0.666 - 1.600 1.899 0.0780 12.8 769 769 10 62.6 0.0613 0.559 - 0.826 0.666 - 1.429 2.070 0.0780 12.8 264 264 11 62.6 0.0660 0.501 - 0.656 0.666 - 1.458 2.431 0.0780 12.8 295 293 12 -84.6 0.0592 0.388 - 0.547 0.740 - 1.632 1.970 0.0780 12.8 534 527 13 62.6 0.0648 0.470 - 0.545 0.717 - 1.530 4.125 0.0780 12.8 279 262 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 xray072.eps Reflections not merged 65 Overloads replaced by fast scan measurements 4983 Corrected reflections written to file xray072_0m.hkl Estimated minimum and maximum transmission: 0.3083 0.7535 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000