+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0648 started at 00:02:26 on 18-May-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0648 in Pnnm CELL 0.71073 11.5390 12.4271 9.9748 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0008 0.0005 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, 1/2 - Z SFAC C H N O P CL UNIT 20 40 12 8 12 16 V = 1430.35 F(000) = 760.0 Mu = 1.15 mm-1 Cell Wt = 1515.48 Rho = 1.759 MERG 2 OMIT -3.00 55.00 OMIT 1 2 0 OMIT 1 1 1 OMIT 5 0 1 TEMP -153 ACTA SIZE 0.6 0.15 0.13 FMAP 2 PLAN 10 BOND WGHT 0.04440 0.57670 L.S. 4 FVAR 0.61731 C1 1 0.475761 0.185792 0.129051 11.00000 0.01548 0.02328 = 0.01936 -0.00112 -0.00414 -0.00210 AFIX 23 H1A 2 0.493311 0.109818 0.119815 11.00000 -1.20000 H1B 2 0.522868 0.213755 0.201669 11.00000 -1.20000 AFIX 0 C2 1 0.509654 0.242961 0.000000 10.50000 0.01528 0.01449 = 0.02162 0.00000 0.00000 -0.00085 C3 1 0.464978 0.358713 0.000000 10.50000 0.03247 0.01532 = 0.04036 0.00000 0.00000 0.00137 AFIX 137 H3A 2 0.483847 0.392345 -0.083848 10.50000 -1.50000 H3B 2 0.500601 0.397921 0.071961 10.50000 -1.50000 H3C 2 0.382419 0.358593 0.011887 10.50000 -1.50000 AFIX 0 C4 1 0.642856 0.241444 0.000000 10.50000 0.01660 0.02912 = 0.03392 0.00000 0.00000 -0.00508 AFIX 137 H4A 2 0.669630 0.168816 -0.010778 10.50000 -1.50000 H4B 2 0.670964 0.269792 0.083414 10.50000 -1.50000 H4C 2 0.671162 0.284775 -0.072636 10.50000 -1.50000 AFIX 0 N1 3 0.138458 0.159266 0.136138 11.00000 0.01732 0.02966 = 0.01738 0.00202 0.00372 0.00566 N2 3 0.299335 0.043749 0.000000 10.50000 0.01500 0.01576 = 0.01806 0.00000 0.00000 -0.00157 O1 4 0.353601 0.197370 0.165264 11.00000 0.02035 0.02386 = 0.01705 -0.00534 0.00288 -0.00228 P1 5 0.264184 0.106716 0.132523 11.00000 0.01436 0.01878 = 0.01390 0.00283 0.00153 0.00061 P2 5 0.077860 0.188602 0.000000 10.50000 0.01263 0.01907 = 0.01929 0.00000 0.00000 0.00115 CL1 6 -0.081890 0.129407 0.000000 10.50000 0.01257 0.03023 = 0.05546 0.00000 0.00000 -0.00175 CL2 6 0.043351 0.347155 0.000000 10.50000 0.03791 0.01824 = 0.02356 0.00000 0.00000 0.00297 CL3 6 0.275692 0.002277 0.282717 11.00000 0.03150 0.03447 = 0.02354 0.01510 0.00499 0.00605 HKLF 4 1.0 0.00 1.00 0.00 0.00 0.00 1.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2005src0648 in Pnnm C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C1_$1 C1 C3 C4 C3 - C2 C4 - C2 N1 - P2 P1 N2 - P1 P1_$1 O1 - C1 P1 P1 - O1 N2 N1 Cl3 P1_$1 P2 - N1_$1 N1 Cl1 Cl2 Cl1 - P2 Cl2 - P2 Cl3 - P1 Operators for generating equivalent atoms: $1 x, y, -z h k l Fo^2 Sigma Why rejected 0 0 7 19.00 4.69 observed but should be systematically absent 14711 Reflections read, of which 773 rejected -14 =< h =< 14, -16 =< k =< 14, -12 =< l =< 12, Max. 2-theta = 54.99 1 Systematic absence violations 0 Inconsistent equivalents 1723 Unique reflections, of which 0 suppressed R(int) = 0.0267 R(sigma) = 0.0170 Friedel opposites merged Maximum memory for data reduction = 1284 / 16936 Special position constraints for C2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C3 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C4 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl1 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl2 z = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1557 / 121294 wR2 = 0.0694 before cycle 1 for 1723 data and 90 / 90 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0444 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61941 0.00118 1.783 OSF Mean shift/esd = 0.289 Maximum = 1.783 for OSF Max. shift = 0.005 A for H4C Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1557 / 121294 wR2 = 0.0690 before cycle 2 for 1723 data and 90 / 90 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0444 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61962 0.00117 0.179 OSF Mean shift/esd = 0.098 Maximum = 0.374 for z N1 Max. shift = 0.001 A for H3A Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1557 / 121294 wR2 = 0.0690 before cycle 3 for 1723 data and 90 / 90 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0444 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61961 0.00117 -0.003 OSF Mean shift/esd = 0.004 Maximum = -0.022 for tors H4A Max. shift = 0.001 A for H4C Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1557 / 121294 wR2 = 0.0690 before cycle 4 for 1723 data and 90 / 90 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0444 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61961 0.00117 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.007 for y C4 Max. shift = 0.000 A for H4C Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4938 0.1082 0.1197 23 0.990 0.000 C1 O1 C2 H1B 0.5239 0.2143 0.2033 23 0.990 0.000 C1 O1 C2 H3A 0.4845 0.3930 -0.0856 137 0.980 0.000 C3 C2 H3A H3B 0.5017 0.3987 0.0734 137 0.980 0.000 C3 C2 H3A H3C 0.3809 0.3587 0.0122 137 0.980 0.000 C3 C2 H3A H4A 0.6703 0.1674 -0.0113 137 0.980 0.000 C4 C2 H4A H4B 0.6716 0.2703 0.0853 137 0.980 0.000 C4 C2 H4A H4C 0.6718 0.2859 -0.0740 137 0.980 0.000 C4 C2 H4A 2005src0648 in Pnnm ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.47586 0.18573 0.12916 1.00000 0.01537 0.02358 0.01931 -0.00088 -0.00387 -0.00246 0.01942 0.00233 0.00011 0.00011 0.00014 0.00000 0.00060 0.00067 0.00067 0.00054 0.00049 0.00051 0.00028 H1A 0.49376 0.10819 0.11971 1.00000 0.02330 0.00000 0.00000 H1B 0.52392 0.21427 0.20329 1.00000 0.02330 0.00000 0.00000 C2 0.50964 0.24301 0.00000 0.50000 0.01534 0.01464 0.02214 0.00000 0.00000 -0.00102 0.01737 0.00256 0.00016 0.00015 0.00000 0.00000 0.00083 0.00085 0.00098 0.00000 0.00000 0.00067 0.00038 C3 0.46522 0.35868 0.00000 0.50000 0.03255 0.01526 0.04014 0.00000 0.00000 0.00157 0.02932 0.00322 0.00021 0.00017 0.00000 0.00000 0.00116 0.00092 0.00134 0.00000 0.00000 0.00085 0.00049 H3A 0.48452 0.39298 -0.08560 0.50000 0.04397 0.00000 0.00000 H3B 0.50166 0.39866 0.07345 0.50000 0.04397 0.00000 0.00000 H3C 0.38094 0.35869 0.01216 0.50000 0.04397 0.00000 0.00000 C4 0.64293 0.24152 0.00000 0.50000 0.01668 0.02898 0.03427 0.00000 0.00000 -0.00530 0.02664 0.00289 0.00017 0.00018 0.00000 0.00000 0.00092 0.00108 0.00122 0.00000 0.00000 0.00081 0.00046 H4A 0.67028 0.16741 -0.01127 0.50000 0.03997 0.00000 0.00000 H4B 0.67161 0.27027 0.08526 0.50000 0.03997 0.00000 0.00000 H4C 0.67182 0.28594 -0.07399 0.50000 0.03997 0.00000 0.00000 N1 0.13854 0.15920 0.13630 1.00000 0.01725 0.02977 0.01752 0.00225 0.00378 0.00555 0.02151 0.00222 0.00010 0.00010 0.00012 0.00000 0.00055 0.00064 0.00059 0.00049 0.00042 0.00049 0.00026 N2 0.29940 0.04383 0.00000 0.50000 0.01511 0.01557 0.01797 0.00000 0.00000 -0.00115 0.01622 0.00217 0.00014 0.00012 0.00000 0.00000 0.00072 0.00072 0.00081 0.00000 0.00000 0.00061 0.00032 O1 0.35355 0.19742 0.16522 1.00000 0.02020 0.02382 0.01749 -0.00541 0.00294 -0.00237 0.02051 0.00166 0.00008 0.00008 0.00010 0.00000 0.00047 0.00050 0.00048 0.00040 0.00038 0.00038 0.00022 P1 0.26420 0.10673 0.13252 1.00000 0.01451 0.01880 0.01393 0.00283 0.00157 0.00061 0.01574 0.00062 0.00003 0.00003 0.00004 0.00000 0.00018 0.00019 0.00019 0.00013 0.00011 0.00012 0.00011 P2 0.07786 0.18859 0.00000 0.50000 0.01274 0.01907 0.01948 0.00000 0.00000 0.00119 0.01710 0.00068 0.00004 0.00004 0.00000 0.00000 0.00023 0.00025 0.00026 0.00000 0.00000 0.00017 0.00013 Cl1 -0.08185 0.12938 0.00000 0.50000 0.01268 0.03021 0.05577 0.00000 0.00000 -0.00161 0.03289 0.00073 0.00004 0.00005 0.00000 0.00000 0.00023 0.00029 0.00039 0.00000 0.00000 0.00019 0.00015 Cl2 0.04336 0.34716 0.00000 0.50000 0.03813 0.01823 0.02354 0.00000 0.00000 0.00301 0.02664 0.00076 0.00005 0.00004 0.00000 0.00000 0.00030 0.00024 0.00027 0.00000 0.00000 0.00020 0.00014 Cl3 0.27570 0.00229 0.28273 1.00000 0.03168 0.03450 0.02365 0.01518 0.00502 0.00618 0.02994 0.00076 0.00003 0.00003 0.00004 0.00000 0.00022 0.00023 0.00021 0.00015 0.00014 0.00015 0.00013 Final Structure Factor Calculation for 2005src0648 in Pnnm Total number of l.s. parameters = 90 Maximum vector length = 511 Memory required = 1467 / 25039 wR2 = 0.0690 before cycle 5 for 1723 data and 0 / 90 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0444 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0232 for 1587 Fo > 4sig(Fo) and 0.0261 for all 1723 data wR2 = 0.0690, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 8.50 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0243 0.0216 0.0124 C1 0.0221 0.0161 0.0139 C2 0.0401 0.0327 0.0151 C3 0.0343 0.0309 0.0147 C4 0.0327 0.0187 0.0131 N1 0.0180 0.0165 0.0142 N2 0.0285 0.0190 0.0140 O1 0.0204 0.0148 0.0120 P1 0.0195 0.0193 0.0125 P2 0.0558 0.0304 0.0125 Cl1 0.0386 0.0235 0.0178 Cl2 0.0489 0.0280 0.0129 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.041 0.061 0.089 0.113 0.141 0.176 0.225 0.317 1.000 Number in group 173. 174. 174. 170. 174. 168. 174. 174. 172. 170. GooF 1.168 1.272 1.137 1.133 0.988 0.989 0.905 0.846 0.745 1.035 K 1.171 1.003 0.977 0.978 0.992 1.003 1.007 1.016 1.012 0.979 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 180. 168. 172. 172. 174. 167. 172. 173. 172. 173. GooF 0.837 0.821 0.883 0.840 0.843 0.860 0.994 0.831 0.980 1.927 K 0.986 1.005 1.016 1.018 1.025 1.020 1.022 1.006 0.996 0.956 R1 0.042 0.033 0.031 0.029 0.023 0.023 0.023 0.014 0.017 0.034 Recommended weighting scheme: WGHT 0.0299 0.8790 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) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 4 4 136.69 77.57 6.45 0.054 1.92 5 2 0 686.64 488.13 6.31 0.134 2.16 4 6 0 61.96 31.02 5.25 0.034 1.68 3 3 2 -1.01 9.04 5.00 0.018 2.45 4 5 0 238.33 171.72 4.69 0.080 1.88 1 3 3 624.62 798.73 4.36 0.172 2.53 3 2 1 10.18 25.48 4.22 0.031 3.11 6 0 0 6774.66 8307.93 4.05 0.555 1.92 4 0 4 13.67 31.35 4.00 0.034 1.89 4 4 0 115.72 78.83 3.94 0.054 2.11 3 1 4 1032.10 857.38 3.68 0.178 2.06 0 5 1 18.30 35.67 3.63 0.036 2.41 4 4 1 170.54 131.03 3.42 0.070 2.07 7 4 0 15.28 6.65 3.39 0.016 1.46 0 2 2 20846.18 24530.53 3.38 0.953 3.89 3 2 4 61.34 41.58 3.36 0.039 1.98 1 7 0 372.58 307.72 3.12 0.107 1.75 3 3 6 21.34 10.88 3.11 0.020 1.43 1 5 7 377.49 311.52 3.11 0.107 1.23 3 1 3 784.10 920.47 2.99 0.185 2.47 1 6 0 791.82 676.82 2.98 0.158 2.04 1 4 2 674.24 574.67 2.97 0.146 2.57 2 2 3 395.18 331.81 2.93 0.111 2.61 2 5 0 311.98 258.87 2.91 0.098 2.28 4 2 7 12.82 5.05 2.89 0.014 1.25 1 0 3 11880.93 13588.61 2.85 0.709 3.19 10 3 1 45.40 30.73 2.79 0.034 1.10 4 5 2 6.86 14.98 2.78 0.024 1.76 8 3 9 33.63 52.82 2.77 0.044 0.86 6 1 0 266.84 221.18 2.73 0.090 1.90 2 4 6 5.92 0.96 2.70 0.006 1.42 2 4 2 72.91 54.85 2.68 0.045 2.40 0 3 1 14527.58 16467.81 2.66 0.781 3.83 2 5 8 96.54 123.04 2.62 0.067 1.09 9 1 4 3.63 0.04 2.62 0.001 1.14 1 10 9 63.13 42.01 2.61 0.039 0.83 0 7 7 216.32 177.97 2.58 0.081 1.11 7 11 6 212.32 262.95 2.53 0.099 0.81 6 9 0 56.35 76.13 2.50 0.053 1.12 5 1 0 20487.23 23045.45 2.45 0.924 2.27 9 4 0 15.87 7.90 2.41 0.017 1.19 8 10 5 143.55 180.22 2.41 0.082 0.85 1 3 0 443.52 384.56 2.40 0.119 3.90 0 4 10 413.39 347.02 2.38 0.113 0.95 1 7 2 14.45 23.39 2.38 0.029 1.66 12 2 0 407.11 349.24 2.37 0.114 0.95 13 5 5 33.72 52.61 2.35 0.044 0.77 4 0 2 2779.77 3117.53 2.35 0.340 2.50 4 3 8 20.45 31.57 2.35 0.034 1.10 5 10 3 11.02 4.81 2.34 0.013 1.04 Bond lengths and angles C1 - Distance Angles O1 1.4637 (0.0016) C2 1.5226 (0.0017) 114.10 (0.12) C1 - O1 C2 - Distance Angles C1_$1 1.5226 (0.0017) C1 1.5226 (0.0017) 115.59 (0.15) C3 1.5262 (0.0027) 110.75 (0.10) 110.75 (0.10) C4 1.5381 (0.0026) 104.50 (0.10) 104.50 (0.10) 110.32 (0.17) C2 - C1_$1 C1 C3 C3 - Distance Angles C2 1.5262 (0.0027) C3 - C4 - Distance Angles C2 1.5381 (0.0026) C4 - N1 - Distance Angles P2 1.5723 (0.0012) P1 1.5904 (0.0012) 118.73 (0.07) N1 - P2 N2 - Distance Angles P1 1.5884 (0.0009) P1_$1 1.5884 (0.0009) 112.64 (0.10) N2 - P1 O1 - Distance Angles C1 1.4637 (0.0016) P1 1.5619 (0.0010) 120.90 (0.08) O1 - C1 P1 - Distance Angles O1 1.5619 (0.0010) N2 1.5884 (0.0009) 111.10 (0.07) N1 1.5904 (0.0012) 107.52 (0.06) 117.04 (0.07) Cl3 1.9868 (0.0005) 105.65 (0.04) 106.80 (0.05) 108.11 (0.05) P1_$1 2.6437 (0.0007) 102.05 (0.04) 33.68 (0.05) 91.36 (0.04) 138.95 (0.02) P1 - O1 N2 N1 Cl3 P2 - Distance Angles N1_$1 1.5723 (0.0012) N1 1.5723 (0.0012) 119.70 (0.09) Cl1 1.9843 (0.0007) 109.11 (0.05) 109.11 (0.05) Cl2 2.0104 (0.0007) 108.41 (0.05) 108.41 (0.05) 100.34 (0.03) P2 - N1_$1 N1 Cl1 Cl1 - Distance Angles P2 1.9843 (0.0007) Cl1 - Cl2 - Distance Angles P2 2.0104 (0.0007) Cl2 - Cl3 - Distance Angles P1 1.9868 (0.0005) Cl3 - FMAP and GRID set by program FMAP 2 3 14 GRID -2.273 -2 -1 2.273 2 1 R1 = 0.0260 for 1723 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.5658 0.2403 0.0000 [ 0.65 A from C2 ] Deepest hole -0.43 at 0.0724 0.1332 0.0000 [ 0.69 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1788 / 19099 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5658 0.2403 0.0000 0.50000 0.05 0.27 0.65 C2 0.89 C4 1.51 H4A 1.53 H4B Q2 1 0.1837 0.1305 0.1368 1.00000 0.05 0.26 0.63 N1 0.98 P1 1.97 P2 2.15 O1 Q3 1 0.4973 0.2806 0.0000 0.50000 0.05 0.25 0.49 C2 1.04 C3 1.64 H3B 1.64 H3A Q4 1 0.4961 0.2229 0.0602 1.00000 0.05 0.23 0.67 C2 0.86 C1 1.47 H1B 1.54 H1A Q5 1 0.2968 0.0717 0.0481 1.00000 0.05 0.22 0.59 N2 1.02 P1 1.89 P1 2.06 O1 Q6 1 0.2020 0.0219 0.1810 1.00000 0.05 0.21 1.35 CL3 1.36 P1 1.91 N1 2.14 N2 Q7 1 0.3366 0.0530 0.0000 0.50000 0.05 0.21 0.44 N2 1.70 P1 2.28 H1A 2.44 O1 Q8 1 -0.0242 0.0815 0.1366 1.00000 0.05 0.19 1.63 CL1 2.11 N1 2.24 P2 2.79 H3A Q9 1 0.2132 0.0814 0.2488 1.00000 0.05 0.18 1.27 CL3 1.34 P1 1.71 N1 2.32 O1 Q10 1 0.2741 0.0163 0.0000 0.50000 0.05 0.18 0.45 N2 1.74 P1 2.37 H4A 2.73 N1 Shortest distances between peaks (including symmetry equivalents) 5 7 0.70 7 10 0.85 5 10 0.88 1 3 0.94 3 4 0.94 5 5 0.96 6 9 1.01 1 4 1.03 4 4 1.20 2 9 1.32 2 6 1.44 2 5 1.74 5 6 1.83 6 10 1.99 8 8 2.10 5 9 2.22 2 10 2.23 2 5 2.37 6 7 2.41 2 7 2.43 6 8 2.46 2 8 2.47 5 6 2.61 9 10 2.70 8 8 2.72 2 2 2.73 6 8 2.75 4 7 2.86 7 9 2.88 8 9 2.96 4 5 2.97 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.49: Structure factors and derivatives 0.17: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0648 finished at 00:02:28 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++