+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 13:21:37 on 26-Nov-2001 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC400 in Pbca CELL 0.71073 14.1493 17.3003 17.4340 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0006 0.0007 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O UNIT 184 192 72 V = 4267.62 F(000) = 1872.0 Mu = 0.11 mm-1 Cell Wt = 3555.38 Rho = 1.383 SHEL 7 0.84 SIZE 0.2 0.2 0.1 TEMP -123 ACTA FMAP 2 PLAN 20 L.S. 4 WGHT 0.066000 FVAR 0.12458 C1 1 0.642009 -0.171953 -0.098848 11.00000 0.03554 0.04674 = 0.03721 -0.01834 0.00763 -0.00358 AFIX 137 H1A 2 0.658194 -0.126255 -0.129357 11.00000 -1.50000 H1B 2 0.614972 -0.211683 -0.132373 11.00000 -1.50000 H1C 2 0.699128 -0.192167 -0.074183 11.00000 -1.50000 AFIX 0 C2 1 0.376129 -0.105625 0.114186 11.00000 0.02614 0.03075 = 0.03394 -0.00241 0.00733 -0.00592 AFIX 137 H2A 2 0.401484 -0.111350 0.166187 11.00000 -1.50000 H2B 2 0.324505 -0.142588 0.106504 11.00000 -1.50000 H2C 2 0.352228 -0.052910 0.107322 11.00000 -1.50000 AFIX 0 C3 1 0.683866 -0.054609 0.008138 11.00000 0.02700 0.02623 = 0.01918 0.00167 0.00087 0.00163 AFIX 43 H3 2 0.733043 -0.069514 -0.025885 11.00000 -1.20000 AFIX 0 C4 1 0.598614 -0.093215 0.008550 11.00000 0.02717 0.02124 = 0.02028 0.00032 -0.00464 -0.00213 C5 1 0.527952 -0.074011 0.063218 11.00000 0.02221 0.02141 = 0.02121 0.00370 -0.00397 -0.00260 C6 1 0.540977 -0.013242 0.112896 11.00000 0.02435 0.02335 = 0.01866 0.00035 -0.00037 0.00245 AFIX 43 H6 2 0.493431 0.000263 0.148960 11.00000 -1.20000 AFIX 0 C7 1 0.625981 0.028465 0.109252 11.00000 0.02460 0.02232 = 0.01687 0.00341 -0.00425 0.00037 C8 1 0.696090 0.006881 0.058929 11.00000 0.02165 0.02586 = 0.01772 0.00392 -0.00339 -0.00274 C9 1 0.649627 0.104037 0.149410 11.00000 0.02905 0.02381 = 0.02109 0.00164 -0.00328 -0.00102 C10 1 0.623052 0.110169 0.233052 11.00000 0.02189 0.02362 = 0.02188 -0.00007 -0.00209 -0.00323 C11 1 0.597116 0.180075 0.265516 11.00000 0.03235 0.01900 = 0.02544 0.00326 -0.00091 -0.00229 AFIX 43 H11 2 0.590879 0.224466 0.233842 11.00000 -1.20000 AFIX 0 C12 1 0.580026 0.186217 0.344061 11.00000 0.03229 0.02018 = 0.02922 -0.00316 0.00005 0.00131 AFIX 43 H12 2 0.562756 0.234655 0.365566 11.00000 -1.20000 AFIX 0 C13 1 0.588182 0.121918 0.390670 11.00000 0.02399 0.02497 = 0.02107 -0.00390 0.00244 -0.00218 C14 1 0.610209 0.050141 0.357893 11.00000 0.02211 0.02293 = 0.02013 0.00290 -0.00117 -0.00113 C15 1 0.628288 0.044783 0.280455 11.00000 0.02119 0.02132 = 0.02177 -0.00304 -0.00024 -0.00091 AFIX 43 H15 2 0.644523 -0.003847 0.258847 11.00000 -1.20000 AFIX 0 C16 1 0.567584 0.195744 0.505094 11.00000 0.05631 0.02921 = 0.02823 -0.01171 0.01079 -0.00147 AFIX 137 H16A 2 0.622159 0.227593 0.490984 11.00000 -1.50000 H16B 2 0.566234 0.188804 0.560872 11.00000 -1.50000 H16C 2 0.509353 0.221407 0.488427 11.00000 -1.50000 AFIX 0 C17 1 0.612201 -0.086506 0.374734 11.00000 0.03632 0.02084 = 0.02951 -0.00030 -0.00274 0.00039 AFIX 137 H17A 2 0.559199 -0.091375 0.338873 11.00000 -1.50000 H17B 2 0.606052 -0.125404 0.415293 11.00000 -1.50000 H17C 2 0.671774 -0.094489 0.347176 11.00000 -1.50000 AFIX 0 C18 1 0.781970 0.058677 0.064524 11.00000 0.02625 0.03123 = 0.01820 0.00076 0.00038 -0.00462 AFIX 13 H18 2 0.790984 0.090206 0.017009 11.00000 -1.20000 AFIX 0 C19 1 0.872293 0.016495 0.087552 11.00000 0.02326 0.04063 = 0.02589 -0.00204 -0.00126 -0.00558 AFIX 23 H19A 2 0.872669 -0.037064 0.067559 11.00000 -1.20000 H19B 2 0.928934 0.043979 0.068380 11.00000 -1.20000 AFIX 0 C20 1 0.868897 0.017190 0.173219 11.00000 0.02001 0.04072 = 0.02944 0.00549 -0.00004 -0.00541 C21 1 0.759500 0.109485 0.134521 11.00000 0.02890 0.03019 = 0.01677 0.00278 -0.00249 -0.00663 C22 1 0.793761 0.192375 0.125394 11.00000 0.03393 0.03740 = 0.02684 -0.00449 0.00082 -0.01170 C23 1 0.818418 0.310812 0.187039 11.00000 0.15438 0.05040 = 0.05229 -0.01957 0.02404 -0.05939 AFIX 137 H23A 2 0.885505 0.313984 0.173424 11.00000 -1.50000 H23B 2 0.808153 0.335772 0.236807 11.00000 -1.50000 H23C 2 0.780633 0.337056 0.147781 11.00000 -1.50000 AFIX 0 O1 3 0.574261 -0.151091 -0.041200 11.00000 0.02952 0.02585 = 0.02640 -0.00636 0.00027 -0.00210 O2 3 0.449355 -0.120261 0.059519 11.00000 0.02450 0.02669 = 0.02939 -0.00559 0.00171 -0.00515 O3 3 0.574917 0.121657 0.468469 11.00000 0.03908 0.02585 = 0.02096 -0.00602 0.00387 -0.00025 O4 3 0.611591 -0.011405 0.407911 11.00000 0.03958 0.02179 = 0.02055 -0.00029 0.00027 -0.00015 O5 3 0.612330 0.168259 0.107053 11.00000 0.03355 0.02392 = 0.02824 0.00672 -0.00691 -0.00177 AFIX 83 H5 2 0.553305 0.164126 0.103913 11.00000 -1.50000 AFIX 0 O6 3 0.909986 -0.022916 0.218721 11.00000 0.03232 0.06041 = 0.03936 0.01170 -0.00376 0.00375 O7 3 0.809359 0.073776 0.198273 11.00000 0.02555 0.04146 = 0.01843 0.00254 -0.00216 -0.00309 O8 3 0.819178 0.220162 0.065790 11.00000 0.07090 0.03868 = 0.03191 0.00137 0.01437 -0.01987 O9 3 0.790426 0.230857 0.191602 11.00000 0.07755 0.04028 = 0.02960 -0.00923 0.01086 -0.03156 HKLF 4 Covalent radii and connectivity table for 01SRC400 in Pbca C 0.770 H 0.320 O 0.660 C1 - O1 C2 - O2 C3 - C4 C8 C4 - O1 C3 C5 C5 - O2 C6 C4 C6 - C5 C7 C7 - C8 C6 C9 C8 - C7 C3 C18 C9 - O5 C10 C7 C21 C10 - C11 C15 C9 C11 - C10 C12 C12 - C13 C11 C13 - O3 C12 C14 C14 - O4 C15 C13 C15 - C14 C10 C16 - O3 C17 - O4 C18 - C8 C19 C21 C19 - C20 C18 C20 - O6 O7 C19 C21 - O7 C22 C18 C9 C22 - O8 O9 C21 C23 - O9 O1 - C4 C1 O2 - C5 C2 O3 - C13 C16 O4 - C14 C17 O5 - C9 O6 - C20 O7 - C20 C21 O8 - C22 O9 - C22 C23 27115 Reflections read, of which 4771 rejected -15 =< h =< 16, -18 =< k =< 20, -20 =< l =< 20, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 12 7 0 16.48 0.72 3 10.33 11 4 1 19.89 0.47 7 2.59 9 2 2 16.13 0.29 6 2.52 8 1 3 21.24 0.28 8 2.11 3 2 4 77.53 0.31 8 10.30 11 0 6 39.34 0.50 4 20.31 12 0 6 28.75 0.50 4 14.49 5 3 8 19.06 0.35 7 2.11 7 2 9 13.35 0.29 7 2.01 10 0 10 13.08 0.58 4 5.78 10 Inconsistent equivalents 3776 Unique reflections, of which 0 suppressed R(int) = 0.0943 R(sigma) = 0.0678 Friedel opposites merged Maximum memory for data reduction = 2627 / 37435 Default effective X-H distances for T = -123.0 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 = 3449 / 366394 wR2 = 0.1213 before cycle 1 for 3776 data and 294 / 294 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12458 0.00027 -0.004 OSF Mean shift/esd = 0.002 Maximum = 0.005 for U12 O5 Max. shift = 0.000 A for H1C Max. dU = 0.000 for C18 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3449 / 366394 wR2 = 0.1213 before cycle 2 for 3776 data and 294 / 294 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12458 0.00027 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U12 O7 Max. shift = 0.000 A for H17B Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3449 / 366394 wR2 = 0.1213 before cycle 3 for 3776 data and 294 / 294 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12458 0.00027 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H23C Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3449 / 366394 wR2 = 0.1213 before cycle 4 for 3776 data and 294 / 294 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12458 0.00027 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H18 Max. dU = 0.000 for C13 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 0.6582 -0.1263 -0.1294 137 0.980 0.000 C1 O1 H1A H1B 0.6150 -0.2117 -0.1324 137 0.980 0.000 C1 O1 H1A H1C 0.6991 -0.1922 -0.0742 137 0.980 0.000 C1 O1 H1A H2A 0.4015 -0.1113 0.1662 137 0.980 0.000 C2 O2 H2A H2B 0.3245 -0.1426 0.1065 137 0.980 0.000 C2 O2 H2A H2C 0.3522 -0.0529 0.1073 137 0.980 0.000 C2 O2 H2A H3 0.7330 -0.0695 -0.0259 43 0.950 0.000 C3 C4 C8 H6 0.4934 0.0003 0.1490 43 0.950 0.000 C6 C5 C7 H11 0.5909 0.2245 0.2338 43 0.950 0.000 C11 C10 C12 H12 0.5628 0.2347 0.3656 43 0.950 0.000 C12 C13 C11 H15 0.6445 -0.0038 0.2588 43 0.950 0.000 C15 C14 C10 H16A 0.6222 0.2276 0.4910 137 0.980 0.000 C16 O3 H16A H16B 0.5662 0.1888 0.5609 137 0.980 0.000 C16 O3 H16A H16C 0.5094 0.2214 0.4884 137 0.980 0.000 C16 O3 H16A H17A 0.5592 -0.0914 0.3389 137 0.980 0.000 C17 O4 H17A H17B 0.6061 -0.1254 0.4153 137 0.980 0.000 C17 O4 H17A H17C 0.6718 -0.0945 0.3472 137 0.980 0.000 C17 O4 H17A H18 0.7910 0.0902 0.0170 13 1.000 0.000 C18 C8 C19 C21 H19A 0.8727 -0.0371 0.0676 23 0.990 0.000 C19 C20 C18 H19B 0.9289 0.0440 0.0684 23 0.990 0.000 C19 C20 C18 H23A 0.8855 0.3140 0.1734 137 0.980 0.000 C23 O9 H23A H23B 0.8082 0.3358 0.2368 137 0.980 0.000 C23 O9 H23A H23C 0.7806 0.3371 0.1478 137 0.980 0.000 C23 O9 H23A H5 0.5533 0.1641 0.1039 83 0.840 0.000 O5 C9 H5 01SRC400 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.64201 -0.17195 -0.09885 1.00000 0.03554 0.04674 0.03721 -0.01834 0.00763 -0.00358 0.03983 0.00438 0.00018 0.00016 0.00014 0.00000 0.00139 0.00172 0.00153 0.00132 0.00120 0.00122 0.00067 H1A 0.65819 -0.12625 -0.12936 1.00000 0.05975 0.00000 0.00000 H1B 0.61497 -0.21168 -0.13237 1.00000 0.05975 0.00000 0.00000 H1C 0.69913 -0.19217 -0.07418 1.00000 0.05975 0.00000 0.00000 C2 0.37613 -0.10563 0.11419 1.00000 0.02614 0.03075 0.03394 -0.00241 0.00733 -0.00592 0.03028 0.00404 0.00015 0.00014 0.00014 0.00000 0.00125 0.00144 0.00140 0.00113 0.00108 0.00104 0.00058 H2A 0.40148 -0.11135 0.16619 1.00000 0.04541 0.00000 0.00000 H2B 0.32450 -0.14259 0.10650 1.00000 0.04541 0.00000 0.00000 H2C 0.35223 -0.05291 0.10732 1.00000 0.04541 0.00000 0.00000 C3 0.68387 -0.05461 0.00814 1.00000 0.02700 0.02623 0.01918 0.00167 0.00087 0.00163 0.02414 0.00372 0.00015 0.00013 0.00012 0.00000 0.00120 0.00139 0.00118 0.00107 0.00096 0.00099 0.00054 H3 0.73304 -0.06951 -0.02589 1.00000 0.02896 0.00000 0.00000 C4 0.59861 -0.09322 0.00855 1.00000 0.02717 0.02124 0.02028 0.00032 -0.00464 -0.00213 0.02290 0.00364 0.00015 0.00012 0.00012 0.00000 0.00126 0.00127 0.00122 0.00100 0.00099 0.00099 0.00053 C5 0.52795 -0.07401 0.06322 1.00000 0.02221 0.02141 0.02121 0.00370 -0.00397 -0.00260 0.02161 0.00359 0.00014 0.00013 0.00012 0.00000 0.00113 0.00128 0.00119 0.00102 0.00095 0.00096 0.00051 C6 0.54098 -0.01324 0.11290 1.00000 0.02435 0.02335 0.01866 0.00035 -0.00037 0.00245 0.02212 0.00364 0.00015 0.00012 0.00012 0.00000 0.00118 0.00127 0.00116 0.00101 0.00095 0.00098 0.00051 H6 0.49343 0.00026 0.14896 1.00000 0.02655 0.00000 0.00000 C7 0.62598 0.02846 0.10925 1.00000 0.02460 0.02232 0.01687 0.00341 -0.00425 0.00037 0.02126 0.00361 0.00014 0.00012 0.00012 0.00000 0.00118 0.00127 0.00115 0.00095 0.00097 0.00095 0.00051 C8 0.69609 0.00688 0.05893 1.00000 0.02165 0.02586 0.01772 0.00392 -0.00339 -0.00274 0.02174 0.00363 0.00014 0.00013 0.00012 0.00000 0.00111 0.00132 0.00116 0.00101 0.00093 0.00095 0.00051 C9 0.64963 0.10404 0.14941 1.00000 0.02905 0.02381 0.02109 0.00164 -0.00328 -0.00102 0.02465 0.00375 0.00015 0.00013 0.00012 0.00000 0.00123 0.00134 0.00123 0.00103 0.00101 0.00099 0.00054 C10 0.62305 0.11017 0.23305 1.00000 0.02189 0.02362 0.02188 -0.00007 -0.00209 -0.00323 0.02246 0.00356 0.00014 0.00012 0.00012 0.00000 0.00115 0.00129 0.00122 0.00100 0.00096 0.00095 0.00052 C11 0.59712 0.18008 0.26552 1.00000 0.03235 0.01900 0.02544 0.00326 -0.00091 -0.00229 0.02560 0.00373 0.00015 0.00013 0.00013 0.00000 0.00123 0.00129 0.00134 0.00103 0.00104 0.00102 0.00054 H11 0.59088 0.22447 0.23384 1.00000 0.03072 0.00000 0.00000 C12 0.58003 0.18622 0.34406 1.00000 0.03229 0.02018 0.02922 -0.00316 0.00005 0.00131 0.02723 0.00384 0.00015 0.00013 0.00013 0.00000 0.00133 0.00131 0.00139 0.00110 0.00107 0.00100 0.00056 H12 0.56276 0.23465 0.36557 1.00000 0.03267 0.00000 0.00000 C13 0.58818 0.12192 0.39067 1.00000 0.02399 0.02497 0.02107 -0.00390 0.00244 -0.00218 0.02334 0.00369 0.00015 0.00013 0.00013 0.00000 0.00120 0.00136 0.00125 0.00107 0.00097 0.00097 0.00053 C14 0.61021 0.05014 0.35789 1.00000 0.02211 0.02293 0.02013 0.00290 -0.00117 -0.00113 0.02172 0.00364 0.00014 0.00012 0.00012 0.00000 0.00110 0.00127 0.00121 0.00103 0.00093 0.00095 0.00051 C15 0.62829 0.04478 0.28046 1.00000 0.02119 0.02132 0.02177 -0.00304 -0.00024 -0.00091 0.02143 0.00349 0.00014 0.00012 0.00012 0.00000 0.00114 0.00127 0.00121 0.00099 0.00093 0.00092 0.00051 H15 0.64452 -0.00385 0.25885 1.00000 0.02571 0.00000 0.00000 C16 0.56758 0.19574 0.50509 1.00000 0.05631 0.02921 0.02823 -0.01171 0.01079 -0.00147 0.03792 0.00432 0.00019 0.00014 0.00014 0.00000 0.00169 0.00148 0.00143 0.00116 0.00125 0.00121 0.00065 H16A 0.62216 0.22759 0.49098 1.00000 0.05688 0.00000 0.00000 H16B 0.56623 0.18880 0.56087 1.00000 0.05688 0.00000 0.00000 H16C 0.50935 0.22141 0.48843 1.00000 0.05688 0.00000 0.00000 C17 0.61220 -0.08651 0.37473 1.00000 0.03632 0.02084 0.02951 -0.00030 -0.00274 0.00039 0.02889 0.00385 0.00016 0.00013 0.00014 0.00000 0.00135 0.00132 0.00135 0.00107 0.00109 0.00106 0.00056 H17A 0.55920 -0.09138 0.33887 1.00000 0.04333 0.00000 0.00000 H17B 0.60605 -0.12540 0.41529 1.00000 0.04333 0.00000 0.00000 H17C 0.67177 -0.09449 0.34718 1.00000 0.04333 0.00000 0.00000 C18 0.78197 0.05868 0.06452 1.00000 0.02625 0.03123 0.01820 0.00076 0.00038 -0.00462 0.02522 0.00370 0.00015 0.00014 0.00012 0.00000 0.00118 0.00139 0.00118 0.00105 0.00096 0.00103 0.00053 H18 0.79098 0.09021 0.01701 1.00000 0.03027 0.00000 0.00000 C19 0.87229 0.01650 0.08755 1.00000 0.02326 0.04063 0.02589 -0.00204 -0.00126 -0.00558 0.02993 0.00392 0.00015 0.00015 0.00013 0.00000 0.00119 0.00153 0.00130 0.00113 0.00102 0.00107 0.00058 H19A 0.87267 -0.03706 0.06756 1.00000 0.03591 0.00000 0.00000 H19B 0.92893 0.04398 0.06838 1.00000 0.03591 0.00000 0.00000 C20 0.86890 0.01719 0.17322 1.00000 0.02001 0.04072 0.02944 0.00549 -0.00004 -0.00541 0.03006 0.00400 0.00015 0.00015 0.00014 0.00000 0.00116 0.00153 0.00137 0.00123 0.00110 0.00113 0.00057 C21 0.75950 0.10949 0.13452 1.00000 0.02890 0.03019 0.01677 0.00278 -0.00249 -0.00663 0.02529 0.00372 0.00015 0.00013 0.00013 0.00000 0.00125 0.00142 0.00118 0.00107 0.00099 0.00101 0.00055 C22 0.79376 0.19237 0.12539 1.00000 0.03393 0.03740 0.02684 -0.00449 0.00082 -0.01170 0.03273 0.00400 0.00016 0.00015 0.00014 0.00000 0.00139 0.00156 0.00148 0.00126 0.00113 0.00115 0.00061 C23 0.81842 0.31081 0.18704 1.00000 0.15438 0.05040 0.05229 -0.01957 0.02404 -0.05939 0.08569 0.00554 0.00031 0.00019 0.00019 0.00000 0.00367 0.00219 0.00211 0.00174 0.00223 0.00221 0.00132 H23A 0.88551 0.31398 0.17342 1.00000 0.12853 0.00000 0.00000 H23B 0.80815 0.33577 0.23681 1.00000 0.12853 0.00000 0.00000 H23C 0.78063 0.33706 0.14778 1.00000 0.12853 0.00000 0.00000 O1 0.57426 -0.15109 -0.04120 1.00000 0.02952 0.02585 0.02640 -0.00636 0.00027 -0.00210 0.02726 0.00247 0.00010 0.00009 0.00008 0.00000 0.00086 0.00093 0.00089 0.00075 0.00071 0.00068 0.00039 O2 0.44936 -0.12026 0.05952 1.00000 0.02450 0.02669 0.02939 -0.00559 0.00171 -0.00515 0.02686 0.00245 0.00010 0.00008 0.00009 0.00000 0.00082 0.00093 0.00092 0.00072 0.00069 0.00068 0.00039 O3 0.57492 0.12166 0.46847 1.00000 0.03908 0.02585 0.02096 -0.00602 0.00387 -0.00025 0.02863 0.00257 0.00011 0.00009 0.00009 0.00000 0.00095 0.00095 0.00086 0.00073 0.00073 0.00070 0.00040 O4 0.61159 -0.01140 0.40791 1.00000 0.03958 0.02178 0.02055 -0.00029 0.00027 -0.00015 0.02730 0.00249 0.00011 0.00008 0.00008 0.00000 0.00094 0.00089 0.00085 0.00073 0.00070 0.00070 0.00039 O5 0.61233 0.16826 0.10705 1.00000 0.03355 0.02392 0.02824 0.00672 -0.00691 -0.00177 0.02857 0.00253 0.00010 0.00008 0.00008 0.00000 0.00090 0.00090 0.00091 0.00073 0.00072 0.00071 0.00040 H5 0.55330 0.16413 0.10391 1.00000 0.04285 0.00000 0.00000 O6 0.90999 -0.02292 0.21872 1.00000 0.03232 0.06041 0.03936 0.01170 -0.00376 0.00375 0.04403 0.00312 0.00012 0.00011 0.00010 0.00000 0.00093 0.00129 0.00110 0.00097 0.00084 0.00088 0.00049 O7 0.80936 0.07378 0.19827 1.00000 0.02555 0.04146 0.01843 0.00254 -0.00216 -0.00309 0.02848 0.00254 0.00010 0.00009 0.00008 0.00000 0.00079 0.00105 0.00082 0.00076 0.00067 0.00074 0.00040 O8 0.81918 0.22016 0.06579 1.00000 0.07090 0.03868 0.03191 0.00137 0.01437 -0.01987 0.04716 0.00305 0.00013 0.00010 0.00010 0.00000 0.00132 0.00116 0.00106 0.00088 0.00096 0.00093 0.00051 O9 0.79043 0.23086 0.19160 1.00000 0.07755 0.04028 0.02960 -0.00923 0.01086 -0.03156 0.04914 0.00287 0.00014 0.00010 0.00010 0.00000 0.00132 0.00116 0.00102 0.00088 0.00093 0.00098 0.00052 Final Structure Factor Calculation for 01SRC400 in Pbca Total number of l.s. parameters = 294 Maximum vector length = 511 Memory required = 3155 / 21973 wR2 = 0.1213 before cycle 5 for 3776 data and 0 / 294 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0468 for 2464 Fo > 4sig(Fo) and 0.0881 for all 3776 data wR2 = 0.1213, GooF = S = 0.968, Restrained GooF = 0.968 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0630 0.0347 0.0218 C1 0.0411 0.0296 0.0201 C2 0.0286 0.0250 0.0188 C3 0.0300 0.0209 0.0178 C4 0.0285 0.0192 0.0171 C5 0.0263 0.0214 0.0186 C6 0.0268 0.0233 0.0137 C7 0.0294 0.0206 0.0153 C8 0.0306 0.0238 0.0196 C9 0.0264 0.0224 0.0185 C10 0.0330 0.0263 0.0174 C11 0.0325 0.0302 0.0191 C12 0.0293 0.0223 0.0185 C13 0.0255 0.0214 0.0183 C14 0.0246 0.0214 0.0183 C15 0.0609 0.0371 0.0158 C16 0.0373 0.0285 0.0208 C17 0.0340 0.0236 0.0181 C18 0.0424 0.0264 0.0210 C19 0.0440 0.0276 0.0185 C20 0.0369 0.0229 0.0161 C21 0.0482 0.0275 0.0224 C22 0.1880 0.0481 0.0210 C23 0.0332 0.0289 0.0196 O1 0.0357 0.0252 0.0197 O2 0.0400 0.0294 0.0165 O3 0.0396 0.0218 0.0205 O4 0.0401 0.0271 0.0184 O5 0.0657 0.0382 0.0281 O6 0.0424 0.0253 0.0177 O7 0.0834 0.0362 0.0218 O8 0.0984 0.0279 0.0211 O9 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.032 0.042 0.054 0.070 0.092 0.138 1.000 Number in group 420. 346. 378. 375. 382. 386. 375. 364. 371. 379. GooF 0.780 0.830 0.929 0.972 1.065 1.043 1.068 0.957 0.955 1.041 K 0.982 1.270 0.936 0.950 0.965 0.979 1.000 1.002 1.009 0.993 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.25 1.43 1.79 inf Number in group 392. 367. 380. 379. 369. 386. 368. 380. 378. 377. GooF 0.898 0.855 0.858 0.977 0.956 0.977 0.916 0.935 1.032 1.222 K 1.047 0.986 1.000 0.991 1.004 1.008 1.026 1.027 1.041 0.967 R1 0.301 0.207 0.158 0.142 0.083 0.070 0.057 0.050 0.047 0.037 Recommended weighting scheme: WGHT 0.0620 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) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 4 6 59.46 123.94 5.34 0.034 2.15 13 1 9 35.11 159.74 4.56 0.038 0.95 0 8 7 499.20 731.13 4.08 0.082 1.63 5 3 4 48.58 106.21 3.92 0.031 2.19 2 9 3 495.35 363.47 3.80 0.058 1.77 1 2 16 23.95 136.49 3.47 0.035 1.08 11 7 12 212.74 3.90 3.33 0.006 0.90 2 7 10 140.21 228.97 3.32 0.046 1.40 10 12 5 59.32 203.57 3.26 0.043 0.97 2 4 6 1236.22 1000.54 3.24 0.095 2.28 6 7 18 881.57 525.17 3.19 0.069 0.84 1 2 19 3.13 137.56 3.18 0.035 0.91 8 6 2 165.62 116.60 3.14 0.033 1.49 8 2 3 267.74 342.51 3.12 0.056 1.66 0 0 16 2194.61 1530.19 3.12 0.118 1.09 12 1 11 112.64 229.73 3.04 0.046 0.94 5 1 3 458.41 621.78 3.04 0.075 2.52 12 9 3 41.44 147.21 2.97 0.037 0.99 4 6 3 801.60 660.56 2.92 0.078 2.09 1 1 12 409.99 536.15 2.90 0.070 1.44 4 4 11 547.66 429.62 2.88 0.063 1.37 1 2 9 64.85 17.17 2.86 0.013 1.87 12 3 1 61.38 119.92 2.85 0.033 1.15 5 2 14 224.00 313.72 2.83 0.053 1.13 1 15 7 787.21 1008.56 2.83 0.096 1.04 4 2 7 739.70 606.63 2.82 0.074 1.98 3 2 7 1387.96 1157.01 2.80 0.103 2.13 0 0 10 2937.78 3592.96 2.80 0.181 1.74 3 1 2 1393.94 1679.80 2.76 0.124 4.03 5 2 7 418.07 566.79 2.75 0.072 1.83 0 0 4 30297.88 36700.77 2.74 0.578 4.36 12 4 4 764.10 957.10 2.74 0.093 1.10 0 8 4 1606.02 1322.15 2.73 0.110 1.94 11 11 5 232.29 99.00 2.69 0.030 0.96 1 10 3 127.86 70.57 2.67 0.025 1.65 13 7 10 1345.72 965.20 2.65 0.094 0.86 4 4 13 540.97 410.10 2.63 0.061 1.20 6 18 1 -0.95 131.51 2.63 0.035 0.89 1 3 3 4889.13 5799.89 2.62 0.230 3.93 6 9 11 647.30 502.37 2.61 0.068 1.09 10 3 3 56.81 98.02 2.61 0.030 1.34 7 10 10 203.12 278.31 2.60 0.050 1.05 0 2 9 5816.71 4914.64 2.57 0.212 1.89 3 12 10 271.39 379.06 2.56 0.059 1.08 7 4 10 133.48 189.49 2.55 0.042 1.26 11 5 14 508.87 263.73 2.55 0.049 0.87 8 2 15 260.24 378.18 2.54 0.059 0.97 13 1 5 96.19 143.75 2.54 0.036 1.04 2 7 8 1386.02 1653.03 2.54 0.123 1.59 4 2 6 34.45 8.45 2.53 0.009 2.17 Bond lengths and angles C1 - Distance Angles O1 1.4350 (0.0027) C1 - C2 - Distance Angles O2 1.4304 (0.0026) C2 - C3 - Distance Angles C4 1.3788 (0.0030) C8 1.3949 (0.0031) 118.33 (0.20) C3 - C4 C4 - Distance Angles O1 1.3688 (0.0025) C3 1.3788 (0.0030) 124.84 (0.20) C5 1.4207 (0.0030) 114.77 (0.18) 120.39 (0.20) C4 - O1 C3 C5 - Distance Angles O2 1.3715 (0.0024) C6 1.3745 (0.0030) 125.77 (0.19) C4 1.4207 (0.0030) 113.74 (0.18) 120.48 (0.19) C5 - O2 C6 C6 - Distance Angles C5 1.3745 (0.0030) C7 1.4040 (0.0030) 118.65 (0.20) C6 - C5 C7 - Distance Angles C8 1.3759 (0.0030) C6 1.4040 (0.0030) 120.46 (0.20) C9 1.5203 (0.0030) 111.61 (0.18) 127.56 (0.19) C7 - C8 C6 C8 - Distance Angles C7 1.3759 (0.0030) C3 1.3949 (0.0031) 121.49 (0.19) C18 1.5130 (0.0029) 112.16 (0.19) 126.31 (0.19) C8 - C7 C3 C9 - Distance Angles O5 1.4347 (0.0025) C10 1.5096 (0.0030) 110.56 (0.17) C7 1.5203 (0.0030) 110.37 (0.17) 116.77 (0.18) C21 1.5790 (0.0030) 103.37 (0.16) 113.57 (0.17) 101.09 (0.17) C9 - O5 C10 C7 C10 - Distance Angles C11 1.3848 (0.0030) C15 1.4029 (0.0030) 118.52 (0.20) C9 1.5096 (0.0030) 121.48 (0.20) 119.95 (0.19) C10 - C11 C15 C11 - Distance Angles C10 1.3848 (0.0030) C12 1.3946 (0.0031) 120.92 (0.21) C11 - C10 C12 - Distance Angles C13 1.3824 (0.0031) C11 1.3946 (0.0031) 120.09 (0.21) C12 - C13 C13 - Distance Angles O3 1.3693 (0.0026) C12 1.3824 (0.0031) 124.99 (0.20) C14 1.4020 (0.0030) 115.55 (0.19) 119.45 (0.20) C13 - O3 C12 C14 - Distance Angles O4 1.3764 (0.0025) C15 1.3772 (0.0029) 124.50 (0.20) C13 1.4020 (0.0030) 115.47 (0.18) 120.03 (0.20) C14 - O4 C15 C15 - Distance Angles C14 1.3772 (0.0029) C10 1.4029 (0.0030) 120.89 (0.20) C15 - C14 C16 - Distance Angles O3 1.4357 (0.0027) C16 - C17 - Distance Angles O4 1.4222 (0.0025) C17 - C18 - Distance Angles C8 1.5130 (0.0029) C19 1.5255 (0.0031) 113.98 (0.20) C21 1.5372 (0.0031) 102.93 (0.17) 103.76 (0.17) C18 - C8 C19 C19 - Distance Angles C20 1.4943 (0.0032) C18 1.5255 (0.0031) 103.43 (0.19) C19 - C20 C20 - Distance Angles O6 1.2036 (0.0027) O7 1.3634 (0.0028) 120.08 (0.22) C19 1.4943 (0.0032) 129.68 (0.23) 110.23 (0.20) C20 - O6 O7 C21 - Distance Angles O7 1.4542 (0.0026) C22 1.5221 (0.0033) 109.00 (0.17) C18 1.5372 (0.0031) 105.28 (0.17) 112.95 (0.19) C9 1.5790 (0.0030) 109.06 (0.16) 112.77 (0.18) 107.46 (0.17) C21 - O7 C22 C18 C22 - Distance Angles O8 1.2001 (0.0028) O9 1.3334 (0.0029) 124.07 (0.23) C21 1.5221 (0.0033) 124.29 (0.22) 111.63 (0.20) C22 - O8 O9 C23 - Distance Angles O9 1.4410 (0.0033) C23 - O1 - Distance Angles C4 1.3688 (0.0025) C1 1.4350 (0.0027) 117.36 (0.17) O1 - C4 O2 - Distance Angles C5 1.3715 (0.0024) C2 1.4304 (0.0026) 116.92 (0.16) O2 - C5 O3 - Distance Angles C13 1.3693 (0.0026) C16 1.4357 (0.0027) 116.58 (0.17) O3 - C13 O4 - Distance Angles C14 1.3764 (0.0025) C17 1.4222 (0.0025) 116.69 (0.16) O4 - C14 O5 - Distance Angles C9 1.4347 (0.0025) O5 - O6 - Distance Angles C20 1.2036 (0.0027) O6 - O7 - Distance Angles C20 1.3634 (0.0028) C21 1.4542 (0.0026) 111.10 (0.17) O7 - C20 O8 - Distance Angles C22 1.2001 (0.0028) O8 - O9 - Distance Angles C22 1.3334 (0.0029) C23 1.4410 (0.0033) 114.95 (0.21) O9 - C22 FMAP and GRID set by program FMAP 2 2 20 GRID -1.471 24 -2 1.471 1 2 R1 = 0.0880 for 3776 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.0733 0.1523 0.4365 [ 0.79 A from H5 ] Deepest hole -0.37 at 0.0387 0.1681 0.3909 [ 0.24 A from H5 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3338 / 30155 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5733 0.1523 0.0635 1.00000 0.05 0.26 0.79 H5 0.98 O5 2.03 C9 2.12 O1 Q2 1 0.7536 0.3555 0.2345 1.00000 0.05 0.21 0.85 H23B 1.46 C23 1.59 H23C 2.27 H23A Q3 1 0.7067 0.1044 0.1463 1.00000 0.05 0.20 0.78 C21 0.81 C9 1.79 O7 1.86 C7 Q4 1 0.5989 -0.1915 -0.1411 1.00000 0.05 0.18 0.44 H1B 1.02 C1 1.42 H1A 1.84 H1C Q5 1 0.5380 -0.1523 -0.1719 1.00000 0.05 0.18 1.65 H1B 1.77 H5 1.91 H1A 1.98 C1 Q6 1 0.6404 0.1739 0.3427 1.00000 0.05 0.17 0.88 C12 1.43 C13 1.48 C11 1.57 H12 Q7 1 0.6072 -0.0271 0.2374 1.00000 0.05 0.17 0.76 H15 1.48 C15 2.20 H17A 2.28 H6 Q8 1 0.4649 0.0226 0.1697 1.00000 0.05 0.17 0.66 H6 1.59 C6 2.24 O6 2.33 H2C Q9 1 0.6369 0.0595 0.1207 1.00000 0.05 0.17 0.59 C7 0.94 C9 1.64 C8 1.86 C6 Q10 1 0.6655 0.1271 0.0702 1.00000 0.05 0.17 1.22 O5 1.46 C9 1.77 C21 1.81 H5 Q11 1 0.9029 0.1458 0.0929 1.00000 0.05 0.17 1.81 O8 1.83 C22 1.85 H19B 2.24 C21 Q12 1 0.4421 0.0845 0.1659 1.00000 0.05 0.17 1.65 H6 1.72 H1A 2.25 C1 2.35 H5 Q13 1 0.9063 0.0338 0.0792 1.00000 0.05 0.17 0.41 H19B 0.58 C19 1.33 H19A 1.75 C20 Q14 1 0.3846 0.0335 0.1796 1.00000 0.05 0.16 1.73 H6 1.93 H1A 2.01 H2C 2.06 O6 Q15 1 0.5855 0.0282 0.0985 1.00000 0.05 0.16 0.60 C7 0.99 C6 1.64 H6 1.75 C8 Q16 1 0.3552 -0.0117 0.1094 1.00000 0.05 0.16 0.72 H2C 1.65 C2 2.08 H6 2.09 H2A Q17 1 0.6036 -0.0546 0.1314 1.00000 0.05 0.16 1.18 C6 1.52 C7 1.63 C5 1.85 H6 Q18 1 0.7800 -0.1520 -0.0562 1.00000 0.05 0.16 1.38 H1C 1.66 H3 2.08 H16A 2.12 C1 Q19 1 0.6849 0.2691 0.5353 1.00000 0.05 0.16 1.38 H16A 1.95 O5 1.98 O8 2.15 C16 Q20 1 0.4346 0.0184 0.1159 1.00000 0.05 0.15 1.06 H6 1.60 C6 1.70 H2C 2.27 C5 Shortest distances between peaks (including symmetry equivalents) 9 15 0.99 8 20 1.03 8 12 1.12 8 14 1.16 5 12 1.21 4 5 1.22 12 14 1.22 16 20 1.24 3 9 1.33 14 20 1.34 1 10 1.38 12 20 1.44 3 10 1.50 14 16 1.51 9 10 1.52 15 17 1.56 7 17 1.91 10 19 1.92 11 13 1.95 8 16 1.97 4 12 1.99 9 17 2.04 1 9 2.09 10 15 2.11 8 15 2.11 6 18 2.12 1 19 2.14 15 20 2.16 1 15 2.24 5 8 2.25 12 16 2.29 3 15 2.32 5 14 2.33 1 5 2.46 8 17 2.47 7 8 2.49 1 3 2.52 12 15 2.54 5 20 2.54 7 9 2.56 7 15 2.62 18 19 2.63 8 9 2.66 17 20 2.72 4 14 2.82 1 12 2.83 2 7 2.83 1 4 2.87 9 12 2.90 3 19 2.94 9 20 2.95 Time profile in seconds ----------------------- 0.11: 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 0.00: Analyse other restraints etc. 0.60: 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 2.28: Structure factors and derivatives 2.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:21:43 Total elapsed time: 6.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++