+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0010 started at 14:44:06 on 01-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0010 in P2(1)/c CELL 0.71073 15.3278 4.3325 15.1614 90.000 108.576 90.000 ZERR 4.00 0.0004 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S CL UNIT 40 32 4 4 4 4 V = 954.38 F(000) = 464.0 Mu = 0.58 mm-1 Cell Wt = 902.74 Rho = 1.571 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 SIZE 0.28 0.02 0.01 BOND $H EQIV $1 -x, -y + 1, -z + 1 HTAB O1 N1_$1 L.S. 6 ACTA DFIX 0.84 0.02 O1 H1O TEMP -153.00 WGHT 0.0326 3.6150 FVAR 0.64985 C1 1 0.095546 0.451251 0.394942 11.00000 0.02244 0.01717 = 0.02272 0.00265 0.00590 0.00457 C2 1 0.143310 0.435808 0.333463 11.00000 0.02373 0.02109 = 0.02367 0.00145 0.00533 0.00329 AFIX 43 H2 2 0.124878 0.322800 0.276818 11.00000 -1.20000 AFIX 0 C3 1 0.212319 0.753348 0.471234 11.00000 0.02362 0.01976 = 0.02013 0.00314 0.00597 0.00718 C4 1 0.270184 0.958903 0.544327 11.00000 0.02248 0.01716 = 0.02552 0.00463 0.00407 0.00126 C5 1 0.357668 1.048204 0.544056 11.00000 0.02522 0.02734 = 0.02436 0.00281 0.00801 0.00209 AFIX 43 H5 2 0.381392 0.976417 0.497029 11.00000 -1.20000 AFIX 0 C6 1 0.409306 1.243621 0.613690 11.00000 0.01948 0.02440 = 0.02971 0.00941 0.00257 -0.00108 C7 1 0.376966 1.353456 0.682767 11.00000 0.03451 0.02639 = 0.02411 0.00081 0.00383 -0.00178 AFIX 43 H7 2 0.413555 1.487716 0.729547 11.00000 -1.20000 AFIX 0 C8 1 0.290071 1.264468 0.682750 11.00000 0.03281 0.02812 = 0.02407 0.00058 0.00859 -0.00102 AFIX 43 H8 2 0.266681 1.338568 0.729764 11.00000 -1.20000 AFIX 0 C9 1 0.236888 1.066688 0.614016 11.00000 0.02866 0.02363 = 0.02680 0.00232 0.00805 0.00090 AFIX 43 H9 2 0.177630 1.005147 0.614732 11.00000 -1.20000 AFIX 0 C10 1 0.006361 0.289833 0.384092 11.00000 0.02388 0.02265 = 0.02640 -0.00201 0.00816 -0.00107 AFIX 23 H10A 2 -0.008572 0.152871 0.329012 11.00000 -1.20000 H10B 2 0.012934 0.159680 0.439508 11.00000 -1.20000 AFIX 0 N1 3 0.134715 0.631839 0.472978 11.00000 0.02143 0.01979 = 0.02112 -0.00022 0.00609 0.00138 O1 4 -0.066947 0.503055 0.373317 11.00000 0.02040 0.03177 = 0.02898 0.00440 0.00962 0.00191 S1 5 0.242308 0.652013 0.373724 11.00000 0.02267 0.02900 = 0.02426 -0.00047 0.00940 0.00041 CL1 6 0.517913 1.358344 0.613070 11.00000 0.02669 0.04194 = 0.03299 0.00220 0.00707 -0.00796 H1O 2 -0.087484 0.460321 0.416171 11.00000 0.04193 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2007may0010 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 C1 - C2 N1 C10 C2 - C1 S1 C3 - N1 C4 S1 C4 - C9 C5 C3 C5 - C6 C4 C6 - C7 C5 Cl1 C7 - C6 C8 C8 - C7 C9 C9 - C4 C8 C10 - O1 C1 N1 - C3 C1 O1 - C10 S1 - C2 C3 Cl1 - C6 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 10884 Reflections read, of which 963 rejected -19 =< h =< 17, -5 =< k =< 4, -19 =< l =< 19, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 2170 Unique reflections, of which 0 suppressed R(int) = 0.0483 R(sigma) = 0.0440 Friedel opposites merged Maximum memory for data reduction = 1371 / 21747 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 = 1718 / 167829 wR2 = 0.1425 before cycle 1 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65022 0.00192 0.194 OSF Mean shift/esd = 0.039 Maximum = 0.194 for OSF Max. shift = 0.003 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1718 / 167829 wR2 = 0.1425 before cycle 2 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65031 0.00192 0.046 OSF Mean shift/esd = 0.014 Maximum = 0.053 for U33 Cl1 Max. shift = 0.001 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1718 / 167829 wR2 = 0.1425 before cycle 3 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65032 0.00192 0.004 OSF Mean shift/esd = 0.001 Maximum = 0.006 for U33 C8 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1718 / 167829 wR2 = 0.1425 before cycle 4 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65032 0.00192 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x C4 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1718 / 167829 wR2 = 0.1425 before cycle 5 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65032 0.00192 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cl1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1718 / 167829 wR2 = 0.1425 before cycle 6 for 2170 data and 131 / 131 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.65032 0.00192 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cl1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Largest correlation matrix elements 0.765 z H1O / x H1O Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1249 0.3228 0.2768 43 0.950 0.000 C2 C1 S1 H5 0.3814 0.9765 0.4970 43 0.950 0.000 C5 C6 C4 H7 0.4135 1.4876 0.7295 43 0.950 0.000 C7 C6 C8 H8 0.2667 1.3384 0.7298 43 0.950 0.000 C8 C7 C9 H9 0.1777 1.0051 0.6147 43 0.950 0.000 C9 C4 C8 H10A -0.0086 0.1529 0.3290 23 0.990 0.000 C10 O1 C1 H10B 0.0129 0.1597 0.4395 23 0.990 0.000 C10 O1 C1 2007may0010 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09552 0.45135 0.39492 1.00000 0.02239 0.01726 0.02262 0.00258 0.00586 0.00458 0.02107 0.00706 0.00023 0.00085 0.00024 0.00000 0.00164 0.00168 0.00165 0.00141 0.00135 0.00144 0.00072 C2 0.14331 0.43584 0.33348 1.00000 0.02373 0.02104 0.02375 0.00137 0.00529 0.00324 0.02338 0.00725 0.00024 0.00089 0.00025 0.00000 0.00169 0.00187 0.00174 0.00145 0.00140 0.00149 0.00077 H2 0.12488 0.32278 0.27685 1.00000 0.02805 0.00000 0.00000 C3 0.21234 0.75339 0.47123 1.00000 0.02357 0.01972 0.02023 0.00323 0.00600 0.00717 0.02140 0.00713 0.00023 0.00086 0.00024 0.00000 0.00170 0.00180 0.00165 0.00139 0.00136 0.00147 0.00074 C4 0.27019 0.95887 0.54433 1.00000 0.02236 0.01727 0.02553 0.00477 0.00405 0.00132 0.02257 0.00710 0.00024 0.00086 0.00025 0.00000 0.00165 0.00174 0.00176 0.00146 0.00136 0.00147 0.00074 C5 0.35769 1.04824 0.54407 1.00000 0.02528 0.02727 0.02441 0.00293 0.00798 0.00221 0.02564 0.00747 0.00025 0.00094 0.00025 0.00000 0.00174 0.00199 0.00177 0.00157 0.00143 0.00161 0.00079 H5 0.38142 0.97651 0.49705 1.00000 0.03076 0.00000 0.00000 C6 0.40928 1.24357 0.61369 1.00000 0.01951 0.02435 0.02963 0.00950 0.00253 -0.00106 0.02575 0.00747 0.00024 0.00092 0.00026 0.00000 0.00165 0.00194 0.00187 0.00157 0.00143 0.00152 0.00081 C7 0.37695 1.35337 0.68276 1.00000 0.03465 0.02633 0.02408 0.00091 0.00389 -0.00166 0.02964 0.00785 0.00027 0.00100 0.00026 0.00000 0.00198 0.00204 0.00178 0.00166 0.00151 0.00180 0.00084 H7 0.41354 1.48765 0.72953 1.00000 0.03557 0.00000 0.00000 C8 0.29007 1.26441 0.68277 1.00000 0.03275 0.02796 0.02439 0.00079 0.00847 -0.00094 0.02851 0.00766 0.00026 0.00095 0.00026 0.00000 0.00196 0.00212 0.00184 0.00158 0.00155 0.00171 0.00085 H8 0.26668 1.33844 0.72979 1.00000 0.03422 0.00000 0.00000 C9 0.23693 1.06668 0.61402 1.00000 0.02853 0.02370 0.02661 0.00233 0.00797 0.00091 0.02647 0.00749 0.00026 0.00092 0.00025 0.00000 0.00185 0.00200 0.00185 0.00156 0.00151 0.00158 0.00082 H9 0.17767 1.00514 0.61472 1.00000 0.03177 0.00000 0.00000 C10 0.00636 0.28985 0.38409 1.00000 0.02383 0.02280 0.02627 -0.00198 0.00810 -0.00104 0.02427 0.00718 0.00024 0.00089 0.00026 0.00000 0.00172 0.00197 0.00182 0.00152 0.00143 0.00153 0.00078 H10A -0.00856 0.15285 0.32902 1.00000 0.02913 0.00000 0.00000 H10B 0.01295 0.15973 0.43952 1.00000 0.02913 0.00000 0.00000 N1 0.13471 0.63186 0.47298 1.00000 0.02132 0.01976 0.02114 -0.00006 0.00605 0.00148 0.02091 0.00573 0.00019 0.00074 0.00019 0.00000 0.00138 0.00154 0.00140 0.00124 0.00112 0.00126 0.00062 O1 -0.06696 0.50308 0.37330 1.00000 0.02055 0.03177 0.02896 0.00441 0.00976 0.00199 0.02665 0.00527 0.00017 0.00067 0.00018 0.00000 0.00122 0.00157 0.00139 0.00123 0.00106 0.00118 0.00060 S1 0.24231 0.65199 0.37372 1.00000 0.02271 0.02903 0.02432 -0.00043 0.00942 0.00040 0.02490 0.00186 0.00006 0.00024 0.00006 0.00000 0.00043 0.00050 0.00044 0.00040 0.00034 0.00040 0.00024 Cl1 0.51791 1.35836 0.61307 1.00000 0.02675 0.04201 0.03309 0.00220 0.00712 -0.00799 0.03452 0.00195 0.00006 0.00027 0.00007 0.00000 0.00046 0.00062 0.00051 0.00046 0.00037 0.00045 0.00028 H1O -0.08747 0.46113 0.41620 1.00000 0.04234 0.09608 0.00302 0.01202 0.00241 0.00000 0.01391 Final Structure Factor Calculation for 2007may0010 in P2(1)/c Total number of l.s. parameters = 131 Maximum vector length = 511 Memory required = 1587 / 25039 wR2 = 0.1425 before cycle 7 for 2170 data and 0 / 131 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.112 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 3.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0623 for 1669 Fo > 4sig(Fo) and 0.0884 for all 2170 data wR2 = 0.1425, GooF = S = 1.112, Restrained GooF = 1.112 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0253 0.0236 0.0143 C1 0.0276 0.0241 0.0185 C2 0.0291 0.0213 0.0138 C3 0.0306 0.0223 0.0148 C4 0.0295 0.0250 0.0225 C5 0.0409 0.0196 0.0168 C6 0.0399 0.0260 0.0230 C7 0.0335 0.0279 0.0241 C8 0.0292 0.0278 0.0224 C9 0.0272 0.0239 0.0218 C10 0.0229 0.0209 0.0189 N1 0.0350 0.0257 0.0192 O1 0.0291 0.0251 0.0205 S1 0.0475 0.0327 0.0233 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.033 0.046 0.062 0.081 0.103 0.134 0.193 1.000 Number in group 232. 214. 213. 215. 219. 220. 210. 215. 215. 217. GooF 1.230 1.244 1.228 1.156 1.103 1.059 0.981 0.919 1.009 1.131 K 4.728 1.723 1.157 1.022 0.990 0.997 0.993 1.002 1.014 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 220. 216. 215. 223. 214. 217. 213. 219. 216. 217. GooF 1.257 1.165 1.118 1.189 0.971 0.949 0.918 0.916 1.074 1.439 K 1.128 1.057 1.032 1.019 0.999 1.013 1.009 0.997 0.998 1.010 R1 0.219 0.180 0.150 0.128 0.094 0.082 0.058 0.050 0.050 0.043 Recommended weighting scheme: WGHT 0.0315 3.5924 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) -6 1 19 40.77 155.64 4.45 0.081 0.78 -1 3 14 57.46 3.42 3.78 0.012 0.85 10 3 6 56.75 0.01 3.45 0.001 0.87 -5 0 10 807.84 1071.67 3.43 0.211 1.49 2 2 1 67.74 17.47 3.31 0.027 2.03 -5 0 2 446.43 624.49 3.26 0.161 3.05 -1 3 15 54.60 5.84 3.13 0.016 0.81 5 0 4 449.33 613.69 3.05 0.160 1.97 -4 4 1 32.94 0.06 3.04 0.002 1.04 -4 3 12 35.12 96.36 3.03 0.063 0.95 -5 1 3 23.49 1.31 3.00 0.007 2.43 -5 3 16 56.02 0.96 3.00 0.006 0.79 -1 1 3 3714.84 3176.52 2.96 0.364 3.29 11 1 9 -26.18 37.23 2.96 0.039 0.87 0 5 7 46.36 5.11 2.91 0.015 0.80 -7 1 17 -6.00 33.11 2.91 0.037 0.87 14 0 8 -9.01 61.31 2.87 0.051 0.80 3 2 1 25.20 0.19 2.83 0.003 1.93 1 5 6 50.20 11.55 2.77 0.022 0.81 2 1 11 22.90 0.37 2.76 0.004 1.17 -9 3 13 69.94 13.38 2.70 0.024 0.87 4 0 6 1025.50 825.15 2.69 0.185 1.76 1 1 7 75.11 35.06 2.66 0.038 1.78 2 3 2 33.20 0.72 2.65 0.005 1.37 1 1 5 3.53 32.19 2.63 0.037 2.27 4 1 3 601.45 762.15 2.62 0.178 2.19 -8 2 1 33.08 2.36 2.60 0.010 1.42 -14 2 8 31.33 4.38 2.58 0.014 0.95 1 5 7 38.52 1.31 2.57 0.007 0.79 6 2 9 38.31 10.80 2.54 0.021 1.03 12 2 3 -10.15 14.26 2.53 0.024 0.98 2 5 5 29.98 0.18 2.50 0.003 0.82 7 3 10 44.84 3.29 2.50 0.012 0.84 6 0 4 783.79 628.83 2.50 0.162 1.76 9 1 11 33.27 82.12 2.48 0.059 0.87 5 2 0 1115.01 926.27 2.46 0.197 1.74 -6 2 10 25.45 4.52 2.46 0.014 1.21 -1 0 4 22.78 3.35 2.45 0.012 3.78 -3 1 5 505.78 393.47 2.44 0.128 2.42 -3 4 6 23.15 1.77 2.43 0.009 0.99 2 1 15 -1.95 34.81 2.42 0.038 0.89 3 1 2 918.63 1106.44 2.41 0.215 2.74 -6 1 9 28.12 5.15 2.40 0.015 1.49 1 0 4 161.81 237.36 2.40 0.099 3.25 -1 1 1 140.17 211.52 2.40 0.094 4.09 -8 2 15 103.92 171.76 2.39 0.085 0.90 14 0 6 -7.98 19.41 2.39 0.028 0.86 -13 1 13 19.15 0.54 2.38 0.005 0.93 -2 0 8 102.18 57.09 2.38 0.049 1.89 7 4 9 80.23 4.53 2.38 0.014 0.77 Bond lengths and angles C1 - Distance Angles C2 1.3577 (0.0049) N1 1.3857 (0.0046) 115.60 (0.32) C10 1.4970 (0.0049) 125.08 (0.33) 119.32 (0.30) C1 - C2 N1 C2 - Distance Angles C1 1.3577 (0.0049) S1 1.7211 (0.0037) 109.71 (0.28) H2 0.9500 125.14 125.14 C2 - C1 S1 C3 - Distance Angles N1 1.3092 (0.0045) C4 1.4768 (0.0051) 124.03 (0.32) S1 1.7385 (0.0035) 113.81 (0.27) 122.16 (0.27) C3 - N1 C4 C4 - Distance Angles C9 1.3920 (0.0052) C5 1.3971 (0.0050) 119.55 (0.35) C3 1.4768 (0.0051) 119.62 (0.33) 120.83 (0.34) C4 - C9 C5 C5 - Distance Angles C6 1.3870 (0.0055) C4 1.3971 (0.0050) 118.82 (0.35) H5 0.9500 120.59 120.59 C5 - C6 C4 C6 - Distance Angles C7 1.3781 (0.0055) C5 1.3870 (0.0055) 122.21 (0.35) Cl1 1.7406 (0.0036) 118.79 (0.30) 119.00 (0.31) C6 - C7 C5 C7 - Distance Angles C6 1.3781 (0.0055) C8 1.3864 (0.0055) 118.82 (0.36) H7 0.9500 120.59 120.59 C7 - C6 C8 C8 - Distance Angles C7 1.3864 (0.0055) C9 1.3939 (0.0054) 120.21 (0.37) H8 0.9500 119.89 119.89 C8 - C7 C9 C9 - Distance Angles C4 1.3920 (0.0052) C8 1.3939 (0.0054) 120.39 (0.36) H9 0.9500 119.81 119.81 C9 - C4 C8 C10 - Distance Angles O1 1.4234 (0.0044) C1 1.4970 (0.0049) 111.65 (0.31) H10A 0.9900 109.29 109.29 H10B 0.9900 109.29 109.29 107.95 C10 - O1 C1 H10A N1 - Distance Angles C3 1.3092 (0.0046) C1 1.3857 (0.0046) 111.05 (0.29) N1 - C3 O1 - Distance Angles C10 1.4234 (0.0044) H1O 0.8277 (0.0191) 104.53 (3.52) O1 - C10 S1 - Distance Angles C2 1.7211 (0.0038) C3 1.7385 (0.0035) 89.83 (0.18) S1 - C2 Cl1 - Distance Angles C6 1.7406 (0.0036) Cl1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.828(19) 2.07(2) 2.897(4) 178(5) O1-H1O...N1_$1 FMAP and GRID set by program FMAP 2 2 24 GRID -4.762 -1 -1 4.762 1 1 R1 = 0.0880 for 2170 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.43 at 0.2997 0.0948 0.2488 [ 0.57 A from H8 ] Deepest hole -0.40 at 0.4599 0.7480 0.4031 [ 0.66 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2166 / 35997 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2997 1.4052 0.7488 1.00000 0.05 1.43 0.57 H8 1.14 C8 1.79 C7 1.89 H7 Q2 1 0.3305 1.2551 0.6590 1.00000 0.05 0.45 0.81 C7 0.81 C8 1.57 C6 1.60 C9 Q3 1 0.2481 1.0561 0.5694 1.00000 0.05 0.40 0.72 C4 0.75 C9 1.47 H9 1.84 C5 Q4 1 0.1881 0.5727 0.3356 1.00000 0.05 0.39 0.90 C2 0.91 S1 1.53 H2 1.98 C1 Q5 1 0.2485 0.8057 0.5290 1.00000 0.05 0.38 0.75 C4 0.90 C3 1.77 C9 1.84 N1 Shortest distances between peaks (including symmetry equivalents) 3 5 1.25 1 2 1.70 2 3 1.76 2 5 2.77 4 5 2.96 1 3 2.99 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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 0.01: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 0.59: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.88: Structure factors and derivatives 1.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.26: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.23: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0010 finished at 14:44:22 Total CPU time: 3.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++