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 cu_marc004_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.): 1.54185 19.915 11.315 22.114 89.980 90.066 90.007 150.77 Scan 2-theta high res %[I>3sig(I)] 1 -73.90 0.9796 81.43 2 118.90 0.7968 72.28 3 -58.14 1.1030 83.56 4 118.90 0.7974 73.25 5 118.90 0.7969 73.45 6 118.90 0.7977 69.26 7 -28.85 1.4908 87.71 8 103.90 0.8332 77.15 9 -73.14 0.9817 80.56 10 -73.90 0.9779 82.72 11 118.90 0.7973 72.30 12 118.90 0.7967 72.02 13 118.90 0.7981 71.01 14 118.90 0.7985 70.43 15 118.90 0.7980 73.25 16 91.47 0.8803 79.07 17 118.90 0.7983 69.48 18 118.90 0.7977 75.21 ============================================================================== 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 36843 Reflections of which 5378 unique; 12.85 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 182 418 491 544 601 633 543 522 1444 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 157 586 333 224 392 797 593 453 1843 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 30337 Reflections employed for parameter determination Effective data to parameter ratio = 8.92 wR2(int) = 0.0622 (selected reflections only, before parameter refinement) Cycle wR2(incid) wR2(diffr) Mean wt. 1 0.0518 0.0497 0.9332 2 0.0489 0.0487 0.9336 3 0.0486 0.0486 0.9336 4 0.0485 0.0485 0.9336 5 0.0484 0.0485 0.9336 6 0.0484 0.0484 0.9337 7 0.0484 0.0484 0.9337 8 0.0484 0.0484 0.9337 9 0.0484 0.0484 0.9337 10 0.0484 0.0484 0.9336 11 0.0484 0.0484 0.9336 12 0.0484 0.0484 0.9337 13 0.0484 0.0484 0.9337 14 0.0484 0.0484 0.9337 15 0.0484 0.0484 0.9337 16 0.0484 0.0484 0.9337 17 0.0484 0.0484 0.9337 18 0.0484 0.0484 0.9337 19 0.0484 0.0484 0.9337 20 0.0484 0.0484 0.9337 21 0.0484 0.0484 0.9337 22 0.0484 0.0484 0.9337 23 0.0484 0.0484 0.9337 24 0.0484 0.0484 0.9337 25 0.0484 0.0484 0.9337 26 0.0484 0.0484 0.9337 27 0.0484 0.0484 0.9337 28 0.0484 0.0484 0.9337 29 0.0484 0.0484 0.9337 30 0.0484 0.0484 0.9337 31 0.0484 0.0484 0.9337 32 0.0484 0.0484 0.9337 33 0.0484 0.0484 0.9337 34 0.0484 0.0484 0.9337 35 0.0484 0.0484 0.9337 36 0.0484 0.0484 0.9337 37 0.0484 0.0484 0.9337 38 0.0484 0.0484 0.9337 39 0.0484 0.0484 0.9337 40 0.0484 0.0484 0.9337 41 0.0484 0.0484 0.9337 42 0.0484 0.0484 0.9337 43 0.0484 0.0484 0.9337 44 0.0484 0.0484 0.9337 45 0.0484 0.0484 0.9337 46 0.0484 0.0484 0.9337 47 0.0484 0.0484 0.9337 48 0.0484 0.0484 0.9337 49 0.0484 0.0484 0.9337 50 0.0484 0.0484 0.9337 wR2(int) = 0.0484 (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: 36843 total and 5378 unique reflections assuming Friedel's law Reflections rejected for which |I-|/su > 4.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 36740 total and 5375 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 -73.9 0.0274 0.798 - 0.910 0.981 - 1.026 0.721 0.0355 28.2 2222 1955 2 118.9 0.0427 0.833 - 0.936 0.975 - 1.026 0.888 0.0355 28.2 2055 1609 3 -58.1 0.0281 0.877 - 0.991 0.975 - 1.025 0.695 0.0355 28.2 1970 1766 4 118.9 0.0425 0.803 - 0.998 0.975 - 1.024 0.734 0.0355 28.2 2024 1649 5 118.9 0.0404 0.891 - 1.017 0.975 - 1.027 0.699 0.0355 28.2 2055 1691 6 118.9 0.0449 0.847 - 0.984 0.980 - 1.025 0.989 0.0355 28.2 2031 1508 7 -28.9 0.0253 0.813 - 0.976 0.981 - 1.027 0.758 0.0355 28.2 1114 1016 8 103.9 0.0317 0.779 - 0.901 0.981 - 1.027 0.658 0.0355 28.2 2243 1912 9 -73.1 0.0259 0.830 - 0.963 0.975 - 1.027 0.632 0.0355 28.2 2228 1957 10 -73.9 0.0263 0.851 - 0.919 0.981 - 1.027 0.655 0.0355 28.2 2246 1992 11 118.9 0.0400 0.866 - 0.984 0.975 - 1.027 0.740 0.0355 28.2 2041 1663 12 118.9 0.0458 0.862 - 1.131 0.975 - 1.025 0.825 0.0355 28.2 2037 1603 13 118.9 0.0392 0.828 - 1.012 0.975 - 1.025 0.799 0.0355 28.2 2024 1593 14 118.9 0.0401 0.784 - 0.901 0.981 - 1.026 0.767 0.0355 28.2 2040 1619 15 118.9 0.0386 0.804 - 0.987 0.975 - 1.025 0.729 0.0355 28.2 2026 1644 16 91.5 0.0335 0.833 - 0.995 0.981 - 1.027 0.677 0.0355 28.2 2329 2011 17 118.9 0.0407 0.766 - 0.847 0.981 - 1.026 0.745 0.0355 28.2 2020 1612 18 118.9 0.0348 0.802 - 0.896 0.981 - 1.027 0.730 0.0355 28.2 2035 1700 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 cu_marc004.eps Reflections not merged 36740 Corrected reflections written to file cu_marc004_0m.hkl Estimated minimum and maximum transmission: 0.7072 0.7539 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000