TITL P2(1)/c CELL 1.54178 14.2677 13.7543 7.8890 90.000 90.259 90.000 ZERR 4.00 0.0007 0.0007 0.0004 0.000 0.002 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H O F UNIT 68 32 12 24 L.S. 10 ACTA BOND $H FMAP 2 WGHT 0.200000 0.000000 FVAR 0.217690 ... 13702 Reflections read, of which 1128 rejected -14 =< h =< 16, -16 =< k =< 16, -7 =< l =< 9, Max. 2-theta = 132.00 0 Systematic absence violations 0 Inconsistent equivalents 2619 Unique reflections, of which 0 suppressed R(int) = 0.0237 R(sigma) = 0.0189 Friedel opposites merged ... Total number of l.s. parameters = 235 Maximum vector length = 623 Memory required = 2995 / 28035 wR2 = 0.6050 before cycle 11 for 2619 data and 0 / 235 parameters GooF = S = 3.536; Restrained GooF = 3.536 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1890 for 2509 Fo > 4sig(Fo) and 0.1900 for all 2619 data wR2 = 0.6050, GooF = S = 3.536, Restrained GooF = 3.536 for all data ... Principal mean square atomic displacements U 0.1447 0.1013 0.0440 F1 0.2113 0.1021 0.0461 F2 0.1171 0.1098 0.0590 F3 0.1371 0.1073 0.0596 F4 0.1654 0.1116 0.0533 F5 0.2375 0.1159 0.0520 F6 0.0679 0.0543 0.0437 O2 0.0597 0.0587 0.0372 O3 0.1150 0.0892 0.0427 C1 0.1253 0.0771 0.0406 C2 0.0799 0.0565 0.0493 C3 0.0594 0.0426 0.0375 C4 0.0562 0.0448 0.0365 C5 0.0482 0.0415 0.0395 C6 0.0523 0.0460 0.0412 C7 0.0645 0.0591 0.0446 C8 0.0669 0.0611 0.0506 C9 0.0932 0.0710 0.0497 C10 0.0623 0.0557 0.0441 C11 0.0688 0.0550 0.0447 C12 0.0630 0.0495 0.0376 C13 0.0621 0.0472 0.0400 C14 0.0692 0.0540 0.0398 C15 0.0952 0.0838 0.0392 O1 0.1051 0.0704 0.0406 C17 0.1310 0.0669 0.0483 C18 ... Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.012 0.018 0.025 0.033 0.044 0.060 0.084 0.131 1.000 Number in group 285. 240. 269. 269. 260. 259. 258. 255. 262. 262. GooF 5.409 4.924 4.509 3.726 3.357 3.097 2.315 2.075 1.866 1.488 K 40.188 6.138 2.516 1.845 1.592 1.486 1.157 1.020 0.973 0.805 Resolution(A) 0.84 0.88 0.91 0.96 1.01 1.07 1.15 1.27 1.46 1.83 inf Number in group 278. 254. 263. 254. 260. 264. 259. 263. 261. 263. GooF 2.350 2.795 2.550 3.283 3.950 3.939 3.713 3.891 4.143 4.180 K 0.988 0.971 0.927 0.918 0.927 0.918 0.888 0.934 0.923 0.860 R1 0.184 0.189 0.189 0.213 0.210 0.197 0.194 0.178 0.181 0.188 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.2000 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. ... Most Disagreeable Reflections (* if suppressed or used for Rfree). Error/esd is calculated as sqrt(wD^2/) where w is given by the weight formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections. h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A) 1 2 1 1695.55 0.74 4.31 0.006 4.87 8 10 2 64.02 0.04 4.31 0.001 1.05 -4 2 3 1049.97 0.72 4.30 0.005 2.03 9 0 2 146.31 0.52 4.29 0.005 1.47 3 5 1 1255.97 3.46 4.29 0.012 2.28 8 3 2 112.04 0.91 4.28 0.006 1.53 -6 1 4 31.06 0.01 4.27 0.001 1.51 -6 2 4 80.84 0.22 4.27 0.003 1.49 7 1 3 68.12 0.18 4.24 0.003 1.60 5 4 2 355.91 3.80 4.20 0.012 1.92 9 2 4 104.90 0.03 4.20 0.001 1.21 2 7 1 53.76 0.85 4.18 0.006 1.84 10 1 1 103.01 2.06 4.10 0.009 1.40 -8 3 3 47.88 0.90 4.01 0.006 1.41 5 11 3 30.66 0.28 4.01 0.003 1.05 7 2 4 85.23 2.04 4.01 0.009 1.39 8 4 6 44.08 0.84 3.98 0.006 1.01 -12 3 1 105.32 2.16 3.97 0.009 1.14 3 3 3 54.47 1.91 3.94 0.009 2.05 11 1 3 127.51 1.92 3.89 0.009 1.16 -2 7 3 339.92 12.68 3.86 0.023 1.54 -2 1 4 889.23 34.13 3.83 0.037 1.89 10 12 1 26.22 0.44 3.82 0.004 0.89 -10 4 3 19.91 0.19 3.81 0.003 1.18 8 7 4 41.51 1.19 3.79 0.007 1.10 -10 9 1 42.47 0.66 3.78 0.005 1.03 -2 1 2 4372.37 206.15 3.78 0.092 3.35 1 6 6 53.80 2.02 3.75 0.009 1.14 -4 1 2 693.32 35.40 3.74 0.038 2.60 4 2 1 90.30 4.50 3.73 0.014 2.93 -12 4 1 51.22 1.78 3.73 0.009 1.11 9 4 5 91.84 4.97 3.69 0.014 1.06 6 11 4 25.99 0.87 3.68 0.006 0.96 10 5 4 31.02 1.62 3.67 0.008 1.06 3 9 1 152.99 9.03 3.67 0.019 1.43 2 5 7 56.61 1.38 3.65 0.008 1.03 2 3 7 65.00 0.83 3.64 0.006 1.08 -13 2 2 37.10 2.05 3.64 0.009 1.05 -2 3 2 961.08 50.19 3.64 0.045 2.76 3 9 4 12.31 0.14 3.63 0.002 1.17 10 3 5 88.60 4.71 3.61 0.014 1.03 1 9 2 64.18 4.26 3.59 0.013 1.42 5 1 4 286.04 16.16 3.58 0.026 1.61 -1 8 2 43.90 2.99 3.57 0.011 1.57 -15 1 3 26.28 1.15 3.54 0.007 0.89 8 0 2 360.13 26.43 3.52 0.033 1.62 9 5 3 27.06 1.59 3.51 0.008 1.22 -2 7 4 166.26 12.43 3.50 0.023 1.37 -2 5 3 387.35 29.88 3.49 0.035 1.84 -6 11 1 63.04 3.54 3.49 0.012 1.10 ... Bond lengths and angles F4 - Distance Angles C18 1.3257 (0.0154) F4 - F5 - Distance Angles C18 1.3351 (0.0126) F5 - F6 - Distance Angles C18 1.3455 (0.0126) F6 - O2 - Distance Angles C12 1.3992 (0.0089) C5 1.4147 (0.0081) 112.27 (0.49) O2 - C12 O3 - Distance Angles C13 1.3681 (0.0095) C5 1.4554 (0.0078) 110.35 (0.53) O3 - C13 C1 - Distance Angles C10 1.3864 (0.0149) C2 1.4048 (0.0186) 122.38 (0.83) H1 0.9300 118.81 118.81 C1 - C10 C2 C2 - Distance Angles C3 1.3720 (0.0144) C1 1.4048 (0.0185) 119.27 (0.84) H7 0.9300 120.37 120.37 C2 - C3 C1 C3 - Distance Angles C2 1.3720 (0.0144) C4 1.3746 (0.0104) 119.71 (0.91) H8 0.9300 120.14 120.14 C3 - C2 C4 ... Electron density synthesis with coefficients Fo-Fc Highest peak 0.67 at 0.5733 0.6362 0.1161 [ 1.34 A from H7 ] Deepest hole -0.90 at 0.3161 0.5786 0.1348 [ 0.20 A from C18 ] Mean = 0.00, Rms deviation from mean = 0.17, Highest memory used = 3214 / 18099