++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 + + neal054 started at 16:25:48 on 18-Oct-2021 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: neal054 -a50000 -b3000 -c624 -g0 -m0 -t12 -a sets the approximate maximum number of atoms including hydrogens. -b sets the maximum number of full-matrix parameters (not used by CGLS). For example -b9000 allows refinement of 1000 anisotropic atoms or 3000 with BLOC 1. For a 32-bit version, -b times the square root of the number of threads should not exceed about 65500. -c sets the reflection buffer size. This depends on the CPU cache size but will rarely need changing. -g sets the number of reflection groups used for calculating R_complete, This must be greater than 1 but not greater than the total number of reflections for refinement. -m sets the current reflection group number. This may not be less than 1 nor greater than the number set by -g. These command line flags override other ways of defining free-R reflections. The -m value is also used as a seed for the WIGL pseudo-random shifts. -t sets the number of threads, otherwise it is set to the apparent number of CPUs. For optimal performance on hyperthreading systems, -t should be set to a little more than half the number of CPUs; e.g. -t4 or -t5 for an Intel i7 processor. Running 12 threads on 12 processors TITL neal054 in P21 #4 REM reset to P21 #4 CELL 1.54178 6.252 11.7415 13.0366 90 96.74 90 ZERR 2 0.0004 0.0007 0.0007 0 0.0024 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O I UNIT 34 46 4 8 2 V = 950.38 F(000) = 448.0 Mu = 13.43 mm-1 Cell Wt = 892.55 Rho = 1.559 L.S. 20 PLAN 10 SIZE 0.028 0.099 0.172 TEMP -173.15 BOND fmap 2 MORE -1 CONF WGHT 0.1 FVAR 0.5 REM REM REM I1 5 0.42510 0.04540 0.02910 11.00000 0.05000 C1 1 0.70980 0.04480 -0.08950 11.00000 0.05000 C2 1 0.57540 -0.01210 -0.52720 11.00000 0.05000 C3 1 0.57730 0.10270 -0.52840 11.00000 0.05000 HKLF 4 Covalent radii and connectivity table for neal054 in P21 #4 C 0.770 H 0.320 N 0.700 O 0.660 I 1.330 I1 - C1 C1 - I1 C2 - C3 C3 - C2 Floating origin restraints generated 9 Systematically absent reflections rejected 3177 Reflections read, of which 9 rejected -7 =< h =< 6, -13 =< k =< 11, -15 =< l =< 14, Max. 2-theta = 127.28 0 Systematic absence violations (I>3sig(I)) before merging 0 Inconsistent equivalents 2488 Unique reflections, of which 0 suppressed R(int) = 0.0310 R(sigma) = 0.0612 Friedel opposites not merged Maximum memory for data reduction = 491 / 25732 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.860A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 2488 2488 Unique reflections possible (point group) 3120 3427 Unique reflections found (Laue group) 1552 1552 Unique reflections possible (Laue group) 1646 1805 Unique Friedel pairs found 936 936 Unique Friedel pairs possible 1474 1622 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 34.00 6.00 H 46.00 0.00 N 4.00 0.00 O 8.00 0.00 I 2.00 2.00 Least-squares cycle 1 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.707242 before cycle 1 for 2488 data and 17 / 17 parameters GooF = S = 11.818; Restrained GooF = 11.816 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22067 0.00752 -37.168 OSF 5 0.04361 0.00190 -3.368 U11 I1 9 0.12653 0.01139 6.718 U11 C1 Mean shift/esd = 3.401 Maximum = -37.168 for OSF Max. shift = 0.159 A for C1 Max. dU = 0.077 for C1 Least-squares cycle 2 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.591475 before cycle 2 for 2488 data and 17 / 17 parameters GooF = S = 5.697; Restrained GooF = 5.696 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17534 0.00429 -10.576 OSF 5 0.03487 0.00142 -6.155 U11 I1 Mean shift/esd = 1.910 Maximum = -10.576 for OSF Max. shift = 0.359 A for C1 Max. dU = 0.087 for C1 Least-squares cycle 3 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.575249 before cycle 3 for 2488 data and 17 / 17 parameters GooF = S = 4.970; Restrained GooF = 4.969 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16869 0.00376 -1.769 OSF 12 -0.57186 0.01141 -3.195 z C2 Mean shift/esd = 1.010 Maximum = -3.195 for z C2 Max. shift = 0.553 A for C2 Max. dU =-0.054 for C3 Least-squares cycle 4 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.569325 before cycle 4 for 2488 data and 17 / 17 parameters GooF = S = 4.931; Restrained GooF = 4.930 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16790 0.00356 -0.221 OSF 13 -0.00948 0.03555 -3.058 U11 C2 Mean shift/esd = 0.570 Maximum = -3.058 for U11 C2 Max. shift = 0.129 A for C1 Max. dU =-0.109 for C2 Least-squares cycle 5 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.559947 before cycle 5 for 2488 data and 17 / 17 parameters GooF = S = 4.826; Restrained GooF = 4.825 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16765 0.00345 -0.072 OSF Mean shift/esd = 0.523 Maximum = -2.304 for z C3 Max. shift = 0.151 A for C1 Max. dU = 0.051 for C1 Least-squares cycle 6 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.556840 before cycle 6 for 2488 data and 17 / 17 parameters GooF = S = 4.770; Restrained GooF = 4.769 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16762 0.00340 -0.009 OSF Mean shift/esd = 0.254 Maximum = -1.019 for U11 C2 Max. shift = 0.171 A for C1 Max. dU = 0.034 for C1 Least-squares cycle 7 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.556281 before cycle 7 for 2488 data and 17 / 17 parameters GooF = S = 4.761; Restrained GooF = 4.760 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16738 0.00335 -0.073 OSF Mean shift/esd = 0.205 Maximum = -1.253 for U11 C2 Max. shift = 0.147 A for C1 Max. dU = 0.039 for C1 Least-squares cycle 8 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.556030 before cycle 8 for 2488 data and 17 / 17 parameters GooF = S = 4.753; Restrained GooF = 4.752 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16714 0.00331 -0.072 OSF Mean shift/esd = 0.198 Maximum = -1.327 for U11 C2 Max. shift = 0.183 A for C1 Max. dU = 0.047 for C1 Least-squares cycle 9 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.555842 before cycle 9 for 2488 data and 17 / 17 parameters GooF = S = 4.750; Restrained GooF = 4.749 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16682 0.00328 -0.097 OSF Mean shift/esd = 0.219 Maximum = -1.366 for U11 C2 Max. shift = 0.328 A for C1 Max. dU = 0.061 for C1 Least-squares cycle 10 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.555593 before cycle 10 for 2488 data and 17 / 17 parameters GooF = S = 4.747; Restrained GooF = 4.746 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16645 0.00324 -0.117 OSF Mean shift/esd = 0.276 Maximum = -1.404 for U11 C2 Max. shift = 0.742 A for C1 Max. dU = 0.066 for C1 Least-squares cycle 11 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.555122 before cycle 11 for 2488 data and 17 / 17 parameters GooF = S = 4.740; Restrained GooF = 4.739 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16675 0.00320 0.094 OSF Mean shift/esd = 0.314 Maximum = -1.388 for U11 C2 Max. shift = 1.018 A for C1 Max. dU =-0.128 for C1 Least-squares cycle 12 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.554708 before cycle 12 for 2488 data and 17 / 17 parameters GooF = S = 4.741; Restrained GooF = 4.740 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16694 0.00319 0.062 OSF Mean shift/esd = 0.325 Maximum = -1.366 for U11 C2 Max. shift = 0.699 A for C1 Max. dU =-0.207 for C1 Least-squares cycle 13 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.555132 before cycle 13 for 2488 data and 17 / 17 parameters GooF = S = 4.746; Restrained GooF = 4.745 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16686 0.00319 -0.027 OSF Mean shift/esd = 0.234 Maximum = -1.341 for U11 C2 Max. shift = 0.146 A for C1 Max. dU = 0.056 for C1 Least-squares cycle 14 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.554784 before cycle 14 for 2488 data and 17 / 17 parameters GooF = S = 4.741; Restrained GooF = 4.740 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16674 0.00319 -0.036 OSF Mean shift/esd = 0.221 Maximum = -1.335 for U11 C2 Max. shift = 0.281 A for C1 Max. dU = 0.028 for C1 Least-squares cycle 15 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.554419 before cycle 15 for 2488 data and 17 / 17 parameters GooF = S = 4.735; Restrained GooF = 4.734 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16679 0.00319 0.015 OSF Mean shift/esd = 0.252 Maximum = -1.328 for U11 C2 Max. shift = 0.328 A for C1 Max. dU =-0.082 for C1 Least-squares cycle 16 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.554017 before cycle 16 for 2488 data and 17 / 17 parameters GooF = S = 4.731; Restrained GooF = 4.730 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16681 0.00318 0.007 OSF Mean shift/esd = 0.230 Maximum = -1.347 for U11 C2 Max. shift = 0.152 A for C1 Max. dU =-0.070 for C1 Least-squares cycle 17 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.553937 before cycle 17 for 2488 data and 17 / 17 parameters GooF = S = 4.731; Restrained GooF = 4.730 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16679 0.00318 -0.009 OSF Mean shift/esd = 0.165 Maximum = -1.363 for U11 C2 Max. shift = 0.068 A for C1 Max. dU =-0.009 for C2 Least-squares cycle 18 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.553831 before cycle 18 for 2488 data and 17 / 17 parameters GooF = S = 4.729; Restrained GooF = 4.728 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16682 0.00318 0.011 OSF Mean shift/esd = 0.169 Maximum = -1.368 for U11 C2 Max. shift = 0.073 A for C1 Max. dU =-0.009 for C2 Least-squares cycle 19 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.553708 before cycle 19 for 2488 data and 17 / 17 parameters GooF = S = 4.728; Restrained GooF = 4.727 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16690 0.00318 0.023 OSF Mean shift/esd = 0.177 Maximum = -1.367 for U11 C2 Max. shift = 0.083 A for C1 Max. dU =-0.009 for C2 Least-squares cycle 20 Maximum vector length = 623 Memory required = 12 / 532 / 50650 wR2 = 0.553548 before cycle 20 for 2488 data and 17 / 17 parameters GooF = S = 4.726; Restrained GooF = 4.725 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16699 0.00318 0.030 OSF 13 -0.00968 0.00639 -1.359 U11 C2 Mean shift/esd = 0.181 Maximum = -1.359 for U11 C2 Max. shift = 0.093 A for C1 Max. dU =-0.009 for C2 Largest correlation matrix elements 0.892 U11 I1 / OSF neal054 in P21 #4 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq I1 0.42777 0.03392 0.02921 1.00000 0.03201 0.00344 0.00036 0.00002 0.00018 0.00000 0.00126 C1 0.65052 0.24960 -0.23827 1.00000 0.17042 0.39295 0.03061 0.01729 0.01724 0.00000 0.06772 C2 0.61779 -0.00310 -0.55530 1.00000 -0.00100 0.05525 0.00508 0.00256 0.00252 0.00000 0.00639 C3 0.58601 0.09186 -0.50641 1.00000 -0.00100 0.06252 0.00509 0.00296 0.00276 0.00000 0.00612 Final Structure Factor Calculation for neal054 in P21 #4 Total number of l.s. parameters = 17 Maximum vector length = 623 Memory required = 12 / 515 / 29281 wR2 = 0.553350 before cycle 21 for 2488 data and 0 / 17 parameters GooF = S = 4.723; Restrained GooF = 4.722 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.553350, GooF = S = 4.72327, Restrained GooF = 4.72232 for all data R1 = 0.241587 for 2418 Fo > 4sig(Fo) and 0.243771 for all 2488 data Flack x = 0.125(155) by classical fit to all intensities 0.114(88) from 774 selected quotients (Parsons' method) Occupancy sum of asymmetric unit = 4.00 for non-hydrogen and 0.00 for H and D atoms Principal mean square atomic displacements U -0.0010 -0.0010 -0.0010 C2 ** NON POSITIVE DEFINITE ** -0.0010 -0.0010 -0.0010 C3 ** NON POSITIVE DEFINITE ** ** Warning: 0 atoms may be split and 2 atoms NPD ** Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.062 0.108 0.152 0.189 0.222 0.258 0.302 0.361 0.459 1.000 Number in group 251. 250. 245. 251. 247. 249. 252. 246. 247. 250. GooF 5.131 5.767 5.313 4.840 4.192 4.414 4.707 4.038 4.160 4.501 K 5.778 2.616 1.815 1.509 1.246 1.333 1.286 1.226 1.277 1.301 Resolution(A) 0.86 0.91 0.96 1.01 1.08 1.15 1.24 1.37 1.56 1.98 inf Number in group 252. 249. 251. 253. 240. 252. 245. 252. 244. 250. GooF 3.885 3.771 3.873 4.822 4.097 4.803 4.775 4.929 5.500 6.300 K 1.222 1.286 1.294 1.339 1.227 1.288 1.276 1.244 1.398 1.376 R1 0.248 0.223 0.224 0.272 0.219 0.245 0.234 0.214 0.245 0.276 Recommended weighting scheme: WGHT 0.2000 0.0000 [Weight parameters refined to 0.3860 146.97 but appear excessive] 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 -1 3 1273.13 63.55 3.64 0.071 3.23 -2 2 4 1342.88 92.03 3.46 0.086 2.21 1 -5 4 2006.02 286.93 3.32 0.151 1.78 -2 -4 2 3298.91 341.93 3.29 0.165 2.08 -3 -4 2 1598.71 143.28 3.25 0.107 1.68 -2 4 2 3446.04 407.99 3.21 0.180 2.08 1 0 0 176.25 12587.65 3.12 1.000 6.21 -3 4 2 1507.31 127.98 3.06 0.101 1.68 2 -5 6 684.08 58.59 3.05 0.068 1.37 0 0 7 6523.02 254.45 3.00 0.142 1.85 -2 0 1 34.27 1018.38 3.00 0.284 3.10 2 3 2 29.99 830.46 2.98 0.257 2.21 -1 -6 8 3.57 365.82 2.96 0.170 1.24 2 -4 0 96.04 1851.40 2.93 0.384 2.13 -1 0 4 75.69 1412.08 2.92 0.335 3.02 1 1 2 1323.46 65.05 2.92 0.072 3.99 -1 -4 9 2788.63 447.30 2.89 0.189 1.29 -2 -4 9 74.47 1281.71 2.89 0.319 1.24 4 -4 7 20.71 705.14 2.89 0.237 1.05 -2 0 2 3205.18 561.96 2.88 0.211 2.94 -3 0 2 1455.06 225.57 2.88 0.134 2.04 -1 6 4 34.63 454.46 2.77 0.190 1.64 1 -5 1 2120.21 413.81 2.76 0.181 2.15 4 0 1 180.12 6.70 2.76 0.023 1.52 1 3 5 92.11 1083.03 2.75 0.293 1.98 3 2 0 957.12 159.62 2.70 0.113 1.95 1 1 3 842.91 66.23 2.69 0.073 3.23 -2 -2 4 1182.08 106.03 2.65 0.092 2.21 -2 -4 6 84.82 763.92 2.64 0.246 1.58 1 -11 2 251.39 14.96 2.64 0.034 1.04 -3 0 7 211.35 1901.65 2.64 0.389 1.47 0 7 1 8.78 138.73 2.63 0.105 1.66 0 0 1 822.56 6576.26 2.61 0.723 12.95 -4 0 11 36.42 542.47 2.60 0.208 1.00 2 1 4 638.34 41.86 2.60 0.058 2.09 4 8 1 489.74 30.28 2.59 0.049 1.06 -3 -6 1 519.81 18.15 2.59 0.038 1.43 -3 0 14 23.04 262.84 2.59 0.145 0.88 1 7 1 4.28 153.54 2.56 0.110 1.60 1 -3 5 149.95 1173.73 2.55 0.305 1.98 -2 -3 11 476.38 57.54 2.53 0.068 1.10 -3 -1 13 740.73 135.15 2.52 0.104 0.94 4 -2 1 442.34 7.29 2.51 0.024 1.47 4 4 0 1106.44 216.75 2.49 0.131 1.37 -1 0 7 866.48 65.22 2.48 0.072 1.83 2 -3 2 145.13 933.16 2.47 0.272 2.21 1 0 7 171.37 1212.29 2.47 0.310 1.72 3 1 6 489.23 64.83 2.45 0.072 1.40 1 7 2 550.87 29.63 2.45 0.049 1.56 -4 5 6 1392.72 126.00 2.43 0.100 1.16 Bond lengths and angles I1 - Distance Angles C1 4.6532 (0.1990) I1 C1 - Distance Angles I1 4.6532 (0.1990) C1 C2 - Distance Angles C3 1.3110 (0.0461) C2 C3 - Distance Angles C2 1.3110 (0.0461) C3 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.245782 for 1552 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 9.52 at 0.4279 0.0349 0.0312 [ 0.03 A from I1 ] Deepest hole -3.50 at 0.2662 0.5348 0.0770 [ 2.49 A from I1 ] Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.9111 -0.1778 -0.5598 1.00000 0.05 6.38 2.76 C2 3.87 C3 4.11 C1 4.28 C3 Q2 1 0.9449 -0.0825 -0.3938 1.00000 0.05 6.12 2.91 C2 3.26 C3 4.86 C1 5.08 C3 Q3 1 0.9137 0.2476 -0.5598 1.00000 0.05 6.09 2.89 C3 3.48 C2 4.29 C2 4.68 C1 Q4 1 0.9410 0.1539 -0.3949 1.00000 0.05 5.87 2.61 C3 3.10 C1 3.30 C2 4.97 C2 Q5 1 1.0188 0.3741 -0.1735 1.00000 0.05 5.63 2.77 C1 4.01 I1 4.65 C2 5.28 I1 Q6 1 0.9428 -0.1214 -0.5586 1.00000 0.05 5.57 2.47 C2 3.47 C3 4.17 C1 4.49 C3 Q7 1 0.4985 -0.0811 -0.5588 1.00000 0.05 5.41 1.18 C2 2.19 C3 3.35 C1 3.98 C3 Q8 1 -0.0208 0.1944 0.1715 1.00000 0.05 5.36 4.01 I1 5.01 C2 5.25 C3 5.26 I1 Q9 1 0.9449 0.1869 -0.5579 1.00000 0.05 5.30 2.66 C3 3.03 C2 4.69 C2 4.81 C1 Q10 1 0.4971 0.1511 -0.5603 1.00000 0.05 5.27 1.09 C3 1.96 C2 4.35 C1 4.42 C2 Shortest distances between peaks (including symmetry equivalents) 1 6 0.69 3 9 0.74 1 3 2.00 4 9 2.16 2 6 2.20 3 6 2.29 1 4 2.29 2 3 2.29 1 9 2.32 3 4 2.40 1 2 2.42 7 10 2.73 6 9 2.76 2 4 2.78 6 7 2.82 1 7 2.82 4 6 2.82 9 10 2.83 3 10 2.84 2 9 2.88 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX and DANG restraints 0.00: Analyse SAME, SADI and NCSY restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU and RIGU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Analyse electron density 0.00: Analyse other restraints etc. 0.04: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.20: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.10: Structure factors and derivatives 0.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.01: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist ** WARNING: These times are only approximate for multiple threads. To get better estimates run with -t1 ** Please cite: G.M. Sheldrick (2015) "Crystal structure refinement with SHELXL", Acta Cryst., C71, 3-8 (Open Access) if SHELXL proves useful. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + neal054 finished at 16:25:48 Total elapsed time: 0.55 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++