+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0860 started at 16:18:37 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0860 in P2(1)/n CELL 0.71073 13.2503 6.9083 16.9813 90.000 102.287 90.000 ZERR 4.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O S BR UNIT 56 32 8 8 8 V = 1518.81 F(000) = 840.0 Mu = 5.61 mm-1 Cell Wt = 1728.58 Rho = 1.890 MERG 2 OMIT -3.00 55.00 OMIT 1 1 0 FMAP 2 PLAN 20 SIZE 0.02 0.03 0.20 ACTA BOND WGHT 0.01240 2.28110 L.S. 4 TEMP -153.00 FVAR 0.34692 MOLE 1 C1 1 0.442700 0.315736 0.129112 11.00000 0.02427 0.01880 = 0.02119 0.00084 0.00601 -0.00091 C2 1 0.388120 0.191788 0.073894 11.00000 0.02201 0.02352 = 0.01952 -0.00048 0.00291 -0.00035 AFIX 43 H2 2 0.370558 0.215791 0.017545 11.00000 -1.20000 AFIX 0 C3 1 0.360797 0.021903 0.111384 11.00000 0.02206 0.01993 = 0.02091 -0.00291 0.00369 -0.00114 AFIX 43 H3 2 0.321613 -0.080359 0.082372 11.00000 -1.20000 AFIX 0 C4 1 0.396392 0.018854 0.193910 11.00000 0.01769 0.01792 = 0.02397 -0.00278 0.00473 -0.00106 C5 1 0.376483 -0.133198 0.246389 11.00000 0.01659 0.01766 = 0.02424 -0.00201 0.00498 -0.00129 AFIX 43 H5 2 0.338002 -0.239856 0.220347 11.00000 -1.20000 AFIX 0 C6 1 0.404702 -0.145847 0.327354 11.00000 0.01696 0.01482 = 0.02101 -0.00183 0.00417 0.00248 C7 1 0.370478 -0.315985 0.366551 11.00000 0.02312 0.02055 = 0.02474 -0.00189 0.00591 -0.00324 AFIX 43 H7 2 0.334076 -0.413994 0.332763 11.00000 -1.20000 AFIX 0 C8 1 0.462666 0.007497 0.380224 11.00000 0.02547 0.01384 = 0.01869 0.00217 0.00663 0.00057 C9 1 0.402263 0.167030 0.404974 11.00000 0.03092 0.01964 = 0.01787 0.00241 0.00311 0.00601 AFIX 43 H9 2 0.438119 0.266152 0.438429 11.00000 -1.20000 AFIX 0 C10 1 0.565322 0.005421 0.410557 11.00000 0.02581 0.01489 = 0.01728 0.00098 0.00340 -0.00166 AFIX 43 H10 2 0.591882 0.112173 0.443839 11.00000 -1.20000 AFIX 0 C11 1 0.640130 -0.137899 0.399043 11.00000 0.02231 0.01712 = 0.01901 -0.00138 0.00513 -0.00336 C12 1 0.743877 -0.130618 0.433281 11.00000 0.02447 0.02248 = 0.02530 -0.00002 0.00022 -0.00435 AFIX 43 H12 2 0.774682 -0.027847 0.467208 11.00000 -1.20000 AFIX 0 C13 1 0.800554 -0.290127 0.413377 11.00000 0.02012 0.03048 = 0.03050 0.00537 0.00399 0.00158 AFIX 43 H13 2 0.872964 -0.306254 0.431635 11.00000 -1.20000 AFIX 0 C14 1 0.738682 -0.416267 0.365202 11.00000 0.02316 0.02377 = 0.02592 0.00212 0.00797 0.00589 O1 3 0.308763 0.177674 0.384585 11.00000 0.03024 0.03635 = 0.03088 -0.00454 0.00312 0.01324 O2 3 0.385281 -0.340789 0.439120 11.00000 0.03693 0.02692 = 0.02293 0.00227 0.00611 -0.00612 S1 4 0.465122 0.229815 0.226142 11.00000 0.02884 0.01905 = 0.01822 -0.00144 0.00251 -0.00524 S2 4 0.611559 -0.347064 0.341534 11.00000 0.02119 0.02049 = 0.02418 -0.00455 0.00247 0.00220 BR1 5 0.493219 0.560974 0.110489 11.00000 0.03645 0.01870 = 0.02555 0.00042 0.00890 -0.00482 BR2 5 0.779481 -0.643978 0.320839 11.00000 0.04237 0.03833 = 0.04470 -0.00953 0.00602 0.01976 HKLF 4 Covalent radii and connectivity table for 2007src0860 in P2(1)/n C 0.770 H 0.320 O 0.660 S 1.030 BR 1.140 C1 - C2 S1 Br1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 S1 C5 - C6 C4 C6 - C5 C7 C8 C7 - O2 C6 C8 - C10 C9 C6 C9 - O1 C8 C10 - C8 C11 C11 - C12 C10 S2 C12 - C11 C13 C13 - C14 C12 C14 - C13 S2 Br2 O1 - C9 O2 - C7 S1 - C1 C4 S2 - C14 C11 Br1 - C1 Br2 - C14 21132 Reflections read, of which 1055 rejected -17 =< h =< 17, -8 =< k =< 8, -22 =< l =< 22, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 3468 Unique reflections, of which 0 suppressed R(int) = 0.0571 R(sigma) = 0.0443 Friedel opposites merged Maximum memory for data reduction = 1526 / 34490 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 = 1992 / 225832 wR2 = 0.0697 before cycle 1 for 3468 data and 181 / 181 parameters GooF = S = 1.062; Restrained GooF = 1.062 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0124 * P )^2 + 2.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34691 0.00040 -0.031 OSF Mean shift/esd = 0.004 Maximum = -0.038 for U33 Br1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1992 / 225832 wR2 = 0.0697 before cycle 2 for 3468 data and 181 / 181 parameters GooF = S = 1.062; Restrained GooF = 1.062 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0124 * P )^2 + 2.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34690 0.00040 -0.013 OSF Mean shift/esd = 0.001 Maximum = -0.013 for U33 Br1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1992 / 225832 wR2 = 0.0697 before cycle 3 for 3468 data and 181 / 181 parameters GooF = S = 1.062; Restrained GooF = 1.062 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0124 * P )^2 + 2.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34690 0.00040 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C7 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1992 / 225832 wR2 = 0.0697 before cycle 4 for 3468 data and 181 / 181 parameters GooF = S = 1.062; Restrained GooF = 1.062 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0124 * P )^2 + 2.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34690 0.00040 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 Br2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C1 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 H2 0.3706 0.2158 0.0175 43 0.950 0.000 C2 C1 C3 H3 0.3216 -0.0804 0.0824 43 0.950 0.000 C3 C4 C2 H5 0.3380 -0.2399 0.2203 43 0.950 0.000 C5 C6 C4 H7 0.3341 -0.4140 0.3328 43 0.950 0.000 C7 O2 C6 H9 0.4381 0.2662 0.4384 43 0.950 0.000 C9 O1 C8 H10 0.5919 0.1122 0.4438 43 0.950 0.000 C10 C8 C11 H12 0.7747 -0.0279 0.4672 43 0.950 0.000 C12 C11 C13 H13 0.8730 -0.3063 0.4316 43 0.950 0.000 C13 C14 C12 2007src0860 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.44270 0.31574 0.12911 1.00000 0.02426 0.01880 0.02118 0.00084 0.00601 -0.00091 0.02124 0.00569 0.00023 0.00043 0.00018 0.00000 0.00157 0.00159 0.00161 0.00123 0.00125 0.00118 0.00064 C2 0.38812 0.19179 0.07389 1.00000 0.02201 0.02351 0.01951 -0.00048 0.00291 -0.00035 0.02190 0.00570 0.00022 0.00044 0.00019 0.00000 0.00155 0.00167 0.00160 0.00125 0.00122 0.00120 0.00065 H2 0.37056 0.21579 0.01754 1.00000 0.02628 0.00000 0.00000 C3 0.36080 0.02191 0.11138 1.00000 0.02206 0.01993 0.02090 -0.00291 0.00369 -0.00114 0.02109 0.00573 0.00023 0.00044 0.00018 0.00000 0.00151 0.00157 0.00161 0.00125 0.00123 0.00119 0.00064 H3 0.32161 -0.08036 0.08237 1.00000 0.02531 0.00000 0.00000 C4 0.39639 0.01885 0.19391 1.00000 0.01769 0.01791 0.02397 -0.00278 0.00473 -0.00106 0.01981 0.00551 0.00022 0.00043 0.00018 0.00000 0.00144 0.00153 0.00166 0.00124 0.00122 0.00113 0.00063 C5 0.37648 -0.13320 0.24639 1.00000 0.01658 0.01766 0.02424 -0.00201 0.00498 -0.00130 0.01940 0.00561 0.00021 0.00042 0.00018 0.00000 0.00141 0.00151 0.00165 0.00123 0.00121 0.00113 0.00062 H5 0.33800 -0.23986 0.22035 1.00000 0.02328 0.00000 0.00000 C6 0.40470 -0.14585 0.32735 1.00000 0.01695 0.01481 0.02100 -0.00183 0.00417 0.00247 0.01757 0.00547 0.00021 0.00042 0.00018 0.00000 0.00139 0.00145 0.00159 0.00118 0.00117 0.00110 0.00060 C7 0.37048 -0.31599 0.36655 1.00000 0.02311 0.02055 0.02474 -0.00189 0.00591 -0.00323 0.02268 0.00589 0.00023 0.00045 0.00019 0.00000 0.00158 0.00160 0.00178 0.00130 0.00128 0.00121 0.00066 H7 0.33407 -0.41400 0.33276 1.00000 0.02721 0.00000 0.00000 C8 0.46267 0.00750 0.38022 1.00000 0.02546 0.01384 0.01868 0.00217 0.00663 0.00057 0.01904 0.00564 0.00023 0.00042 0.00018 0.00000 0.00157 0.00143 0.00155 0.00118 0.00123 0.00117 0.00061 C9 0.40226 0.16703 0.40497 1.00000 0.03093 0.01964 0.01787 0.00241 0.00311 0.00601 0.02312 0.00614 0.00024 0.00044 0.00018 0.00000 0.00178 0.00160 0.00159 0.00127 0.00130 0.00129 0.00067 H9 0.43812 0.26615 0.43843 1.00000 0.02774 0.00000 0.00000 C10 0.56532 0.00542 0.41056 1.00000 0.02580 0.01489 0.01727 0.00098 0.00340 -0.00166 0.01950 0.00567 0.00023 0.00043 0.00018 0.00000 0.00157 0.00144 0.00152 0.00118 0.00122 0.00118 0.00061 H10 0.59188 0.11218 0.44384 1.00000 0.02340 0.00000 0.00000 C11 0.64013 -0.13790 0.39904 1.00000 0.02230 0.01711 0.01900 -0.00139 0.00513 -0.00335 0.01936 0.00551 0.00022 0.00042 0.00018 0.00000 0.00149 0.00150 0.00157 0.00121 0.00121 0.00117 0.00061 C12 0.74388 -0.13062 0.43328 1.00000 0.02447 0.02247 0.02530 -0.00002 0.00023 -0.00436 0.02483 0.00592 0.00023 0.00046 0.00019 0.00000 0.00160 0.00168 0.00174 0.00133 0.00131 0.00127 0.00068 H12 0.77468 -0.02785 0.46721 1.00000 0.02980 0.00000 0.00000 C13 0.80055 -0.29013 0.41338 1.00000 0.02012 0.03048 0.03049 0.00537 0.00399 0.00158 0.02724 0.00627 0.00024 0.00048 0.00020 0.00000 0.00156 0.00183 0.00187 0.00146 0.00134 0.00130 0.00072 H13 0.87297 -0.30625 0.43163 1.00000 0.03269 0.00000 0.00000 C14 0.73868 -0.41626 0.36520 1.00000 0.02316 0.02376 0.02591 0.00212 0.00798 0.00589 0.02387 0.00614 0.00023 0.00046 0.00019 0.00000 0.00158 0.00167 0.00174 0.00132 0.00132 0.00126 0.00068 O1 0.30876 0.17768 0.38458 1.00000 0.03024 0.03635 0.03087 -0.00454 0.00312 0.01325 0.03299 0.00449 0.00017 0.00035 0.00014 0.00000 0.00131 0.00142 0.00134 0.00108 0.00103 0.00104 0.00056 O2 0.38528 -0.34079 0.43912 1.00000 0.03693 0.02691 0.02293 0.00227 0.00611 -0.00612 0.02896 0.00422 0.00017 0.00032 0.00013 0.00000 0.00131 0.00126 0.00127 0.00099 0.00100 0.00099 0.00052 S1 0.46512 0.22982 0.22614 1.00000 0.02884 0.01905 0.01822 -0.00144 0.00251 -0.00524 0.02241 0.00140 0.00006 0.00011 0.00005 0.00000 0.00041 0.00039 0.00039 0.00030 0.00031 0.00031 0.00017 S2 0.61156 -0.34706 0.34153 1.00000 0.02119 0.02048 0.02418 -0.00455 0.00247 0.00220 0.02230 0.00144 0.00006 0.00011 0.00005 0.00000 0.00037 0.00039 0.00042 0.00032 0.00030 0.00029 0.00017 Br1 0.49322 0.56097 0.11049 1.00000 0.03645 0.01870 0.02554 0.00042 0.00890 -0.00482 0.02655 0.00060 0.00003 0.00004 0.00002 0.00000 0.00019 0.00017 0.00018 0.00013 0.00014 0.00013 0.00010 Br2 0.77948 -0.64398 0.32084 1.00000 0.04236 0.03833 0.04469 -0.00953 0.00602 0.01976 0.04228 0.00077 0.00003 0.00006 0.00002 0.00000 0.00022 0.00023 0.00024 0.00017 0.00017 0.00017 0.00012 Final Structure Factor Calculation for 2007src0860 in P2(1)/n Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 1811 / 24017 wR2 = 0.0697 before cycle 5 for 3468 data and 0 / 181 parameters GooF = S = 1.062; Restrained GooF = 1.062 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0124 * P )^2 + 2.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0341 for 2828 Fo > 4sig(Fo) and 0.0495 for all 3468 data wR2 = 0.0697, GooF = S = 1.062, Restrained GooF = 1.062 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0245 0.0211 0.0181 C1 0.0236 0.0231 0.0190 C2 0.0234 0.0225 0.0173 C3 0.0251 0.0179 0.0165 C4 0.0248 0.0177 0.0157 C5 0.0218 0.0184 0.0125 C6 0.0265 0.0233 0.0183 C7 0.0257 0.0185 0.0129 C8 0.0341 0.0202 0.0151 C9 0.0267 0.0175 0.0143 C10 0.0240 0.0187 0.0154 C11 0.0325 0.0238 0.0182 C12 0.0360 0.0259 0.0198 C13 0.0307 0.0237 0.0172 C14 0.0505 0.0292 0.0193 O1 0.0404 0.0258 0.0206 O2 0.0320 0.0196 0.0157 S1 0.0296 0.0203 0.0170 S2 0.0377 0.0249 0.0171 Br1 0.0672 0.0419 0.0177 Br2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.029 0.043 0.059 0.077 0.095 0.119 0.153 0.218 1.000 Number in group 366. 355. 338. 334. 347. 345. 344. 347. 344. 348. GooF 0.997 0.985 1.113 1.119 1.139 1.146 1.041 0.958 0.985 1.131 K 1.937 1.036 0.981 0.990 0.979 0.969 0.997 1.002 1.018 0.996 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 357. 342. 345. 348. 352. 337. 348. 345. 354. 340. GooF 1.054 0.974 1.110 1.032 0.934 0.990 0.984 0.923 1.017 1.502 K 0.996 0.998 0.988 0.994 1.007 1.013 1.019 1.020 1.013 0.982 R1 0.144 0.114 0.102 0.064 0.049 0.043 0.033 0.026 0.021 0.022 Recommended weighting scheme: WGHT 0.0124 2.2859 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) -3 2 3 203.64 83.34 5.87 0.031 2.56 -7 1 1 304.25 178.35 4.44 0.045 1.82 3 1 1 4143.05 4744.67 4.28 0.232 3.45 -12 0 2 12.50 117.69 3.86 0.036 1.10 -2 4 16 229.23 428.91 3.85 0.070 0.90 -6 1 19 336.11 567.74 3.77 0.080 0.87 3 0 1 80587.04 88347.29 3.66 1.000 3.98 0 1 2 1214.82 990.37 3.59 0.106 5.31 -3 1 3 785.61 622.87 3.52 0.084 3.34 1 2 1 3791.36 4304.29 3.45 0.221 3.24 1 8 3 181.68 9.95 3.36 0.011 0.85 -2 4 1 1719.62 1439.00 3.28 0.128 1.67 4 2 3 172.98 99.06 3.28 0.033 2.06 2 1 7 1501.96 1254.75 3.27 0.119 2.00 -2 2 5 2804.07 2467.31 3.21 0.167 2.37 0 7 10 277.02 440.97 3.18 0.071 0.85 -1 7 10 -227.50 501.43 3.14 0.075 0.85 3 3 2 841.92 1015.14 3.10 0.107 1.93 1 2 5 9050.38 9921.40 3.09 0.335 2.29 3 2 2 2033.87 2311.87 3.04 0.162 2.47 6 0 0 143.34 70.84 3.03 0.028 2.16 -10 5 5 627.74 803.44 3.03 0.095 0.95 1 2 6 2787.89 3136.49 3.03 0.188 2.07 -4 4 17 98.74 212.65 2.98 0.049 0.86 -5 4 13 434.30 574.10 2.93 0.081 1.02 4 0 0 5337.42 5890.61 2.90 0.258 3.24 12 6 2 227.28 76.35 2.87 0.029 0.77 -5 4 16 861.09 1094.20 2.86 0.111 0.89 5 1 1 226.22 310.86 2.81 0.059 2.33 -4 2 6 1628.92 1429.34 2.81 0.127 1.95 -5 5 9 58.00 120.21 2.81 0.037 1.07 -8 2 17 614.68 791.32 2.80 0.095 0.90 -4 5 13 52.90 132.69 2.79 0.039 0.94 -8 3 17 -20.39 62.45 2.79 0.027 0.86 2 5 13 135.45 26.52 2.72 0.017 0.91 6 7 9 443.55 744.73 2.70 0.092 0.78 -9 6 7 300.13 510.74 2.70 0.076 0.88 -1 1 3 10910.48 11778.86 2.68 0.365 4.32 3 7 11 329.52 494.77 2.67 0.075 0.79 2 5 15 522.36 248.76 2.65 0.053 0.84 8 0 8 132.53 270.80 2.62 0.055 1.16 4 2 6 610.77 740.61 2.62 0.092 1.67 1 1 16 185.01 312.44 2.62 0.059 1.01 1 1 7 364.06 271.91 2.60 0.055 2.14 -5 1 19 32.96 122.65 2.59 0.037 0.88 13 3 5 70.43 168.30 2.58 0.044 0.84 3 6 11 102.42 20.69 2.58 0.015 0.87 7 8 1 442.24 606.76 2.58 0.083 0.78 9 6 8 73.86 226.74 2.56 0.051 0.79 -6 8 5 315.07 185.39 2.55 0.046 0.79 Bond lengths and angles C1 - Distance Angles C2 1.3590 (0.0042) S1 1.7167 (0.0031) 113.73 (0.23) Br1 1.8731 (0.0030) 127.61 (0.24) 118.67 (0.17) C1 - C2 S1 C2 - Distance Angles C1 1.3590 (0.0042) C3 1.4184 (0.0042) 111.15 (0.28) C2 - C1 C3 - Distance Angles C4 1.3804 (0.0042) C2 1.4184 (0.0042) 113.80 (0.27) C3 - C4 C4 - Distance Angles C3 1.3804 (0.0042) C5 1.4378 (0.0041) 124.91 (0.27) S1 1.7438 (0.0030) 110.41 (0.22) 124.65 (0.23) C4 - C3 C5 C5 - Distance Angles C6 1.3487 (0.0042) C4 1.4378 (0.0041) 129.17 (0.28) C5 - C6 C6 - Distance Angles C5 1.3487 (0.0042) C7 1.4692 (0.0041) 117.93 (0.27) C8 1.4915 (0.0041) 124.27 (0.27) 117.68 (0.26) C6 - C5 C7 C7 - Distance Angles O2 1.2180 (0.0037) C6 1.4692 (0.0041) 124.90 (0.29) C7 - O2 C8 - Distance Angles C10 1.3482 (0.0041) C9 1.4748 (0.0040) 117.62 (0.28) C6 1.4915 (0.0041) 124.81 (0.27) 117.46 (0.26) C8 - C10 C9 C9 - Distance Angles O1 1.2156 (0.0037) C8 1.4748 (0.0040) 123.10 (0.30) C9 - O1 C10 - Distance Angles C8 1.3482 (0.0041) C11 1.4435 (0.0040) 128.44 (0.28) C10 - C8 C11 - Distance Angles C12 1.3748 (0.0041) C10 1.4435 (0.0040) 124.84 (0.28) S2 1.7400 (0.0030) 110.26 (0.23) 124.89 (0.23) C11 - C12 C10 C12 - Distance Angles C11 1.3748 (0.0041) C13 1.4144 (0.0044) 113.85 (0.29) C12 - C11 C13 - Distance Angles C14 1.3473 (0.0046) C12 1.4144 (0.0044) 111.32 (0.28) C13 - C14 C14 - Distance Angles C13 1.3473 (0.0046) S2 1.7144 (0.0030) 113.74 (0.24) Br2 1.8729 (0.0031) 126.66 (0.24) 119.55 (0.18) C14 - C13 S2 O1 - Distance Angles C9 1.2156 (0.0037) O1 - O2 - Distance Angles C7 1.2180 (0.0037) O2 - S1 - Distance Angles C1 1.7167 (0.0031) C4 1.7438 (0.0030) 90.89 (0.15) S1 - C1 S2 - Distance Angles C14 1.7144 (0.0030) C11 1.7400 (0.0030) 90.83 (0.15) S2 - C14 Br1 - Distance Angles C1 1.8731 (0.0030) Br1 - Br2 - Distance Angles C14 1.8729 (0.0031) Br2 - FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0469 for 3468 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.8617 0.0686 0.2287 [ 1.44 A from S2 ] Deepest hole -0.62 at 0.7577 0.7822 0.1831 [ 0.70 A from BR2 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 1855 / 19071 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6383 -0.4314 0.2713 1.00000 0.05 0.38 1.44 S2 1.85 C14 2.39 BR2 2.88 BR2 Q2 1 0.3851 0.1020 0.0907 1.00000 0.05 0.36 0.69 C2 0.76 C3 1.45 H2 1.50 H3 Q3 1 0.5570 -0.4384 0.2502 1.00000 0.05 0.35 1.69 S2 2.34 BR1 2.59 S1 2.76 C14 Q4 1 0.7797 -0.2041 0.4172 1.00000 0.05 0.35 0.66 C13 0.78 C12 1.40 H13 1.49 H12 Q5 1 0.6008 -0.0546 0.3994 1.00000 0.05 0.33 0.68 C10 0.78 C11 1.40 H10 1.84 C8 Q6 1 0.3380 -0.3589 0.2937 1.00000 0.05 0.33 0.78 H7 1.26 C7 1.49 H5 1.75 C6 Q7 1 0.8239 -0.5412 0.3109 1.00000 0.05 0.33 0.96 BR2 1.82 C14 2.52 C13 2.59 H13 Q8 1 0.1971 -0.1302 0.0243 1.00000 0.05 0.33 1.77 H3 2.05 O1 2.15 H9 2.41 C9 Q9 1 0.9402 -0.5010 0.4553 1.00000 0.05 0.32 1.62 H13 2.14 H2 2.34 C13 2.62 C2 Q10 1 0.6526 -0.4132 0.2367 1.00000 0.05 0.32 2.02 S2 2.24 C14 2.37 BR2 2.53 BR2 Q11 1 0.2548 -0.0767 0.2879 1.00000 0.05 0.32 1.93 C5 2.01 C6 2.08 H5 2.41 O1 Q12 1 0.4297 0.0636 0.3885 1.00000 0.05 0.32 0.62 C8 0.87 C9 1.63 H9 1.77 C6 Q13 1 0.3859 -0.2543 0.4956 1.00000 0.05 0.31 1.13 O2 1.41 H10 2.20 C7 2.34 C10 Q14 1 0.4001 -0.3664 0.4832 1.00000 0.05 0.31 0.75 O2 1.97 C7 2.14 H10 2.37 H9 Q15 1 0.2997 0.2174 -0.0036 1.00000 0.05 0.31 0.93 H2 1.57 C2 2.21 H12 2.37 C3 Q16 1 0.3804 0.1597 0.0360 1.00000 0.05 0.30 0.50 H2 0.67 C2 1.66 C3 1.95 C1 Q17 1 0.4845 0.3369 0.1171 1.00000 0.05 0.30 0.65 C1 1.56 BR1 1.67 C2 2.06 S1 Q18 1 0.6664 -0.6584 0.2168 1.00000 0.05 0.30 2.06 BR2 2.51 C13 2.67 H13 2.73 C14 Q19 1 0.7395 -0.6271 0.2095 1.00000 0.05 0.30 1.86 BR2 2.33 C13 2.42 C14 2.48 C12 Q20 1 0.5824 0.2941 0.2529 1.00000 0.05 0.30 1.59 S1 2.49 C1 2.66 BR2 2.88 S2 Shortest distances between peaks (including symmetry equivalents) 1 10 0.67 13 14 0.83 2 16 1.00 18 19 1.02 1 3 1.06 15 16 1.20 3 10 1.35 18 20 1.42 10 18 1.74 3 20 1.88 1 18 1.90 2 15 1.93 7 19 1.94 9 9 1.95 10 19 1.99 1 20 2.04 9 16 2.04 2 17 2.08 16 17 2.12 4 19 2.18 8 14 2.22 6 11 2.23 6 11 2.23 3 18 2.25 10 20 2.27 1 19 2.31 5 12 2.38 17 20 2.41 19 20 2.41 7 18 2.48 10 19 2.50 13 15 2.50 7 10 2.51 1 7 2.52 4 5 2.54 4 18 2.55 4 8 2.58 9 15 2.60 9 16 2.60 7 9 2.62 1 19 2.63 17 18 2.63 2 9 2.65 2 9 2.69 7 18 2.69 7 10 2.73 3 17 2.74 11 12 2.75 5 13 2.76 14 15 2.80 8 13 2.81 8 15 2.85 9 17 2.91 4 9 2.93 7 20 2.94 10 18 2.94 3 19 2.96 15 17 2.96 2 8 2.98 7 19 2.98 12 13 2.99 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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 0.01: Analyse other restraints etc. 2.89: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.00: Structure factors and derivatives 1.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.04: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0860 finished at 16:18:49 Total CPU time: 5.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++