+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1376 started at 13:37:47 on 24-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1376 in P-1 CELL 0.71073 5.3320 12.9425 20.2396 71.806 89.317 78.634 ZERR 2.00 0.0004 0.0009 0.0015 0.003 0.003 0.004 LATT 1 SFAC C H N S UNIT 56 64 4 8 V = 1299.02 F(000) = 556.0 Mu = 0.39 mm-1 Cell Wt = 1049.59 Rho = 1.342 MERG 2 OMIT -3.00 55.00 OMIT -5 1 0 FMAP 2 PLAN 10 SIZE 0.01 0.10 0.20 ACTA BOND WGHT 0.05450 4.16080 L.S. 4 TEMP -153.00 FVAR 0.52536 H1 2 0.892811 0.694455 -0.064319 11.00000 0.02499 H15 2 0.065597 -0.198836 0.043655 11.00000 0.03368 MOLE 1 C1 1 0.931800 0.616625 -0.038820 11.00000 0.02975 0.01767 = 0.03484 -0.01123 0.00586 -0.00489 C2 1 0.806765 0.569012 0.018981 11.00000 0.02562 0.01948 = 0.03262 -0.01353 0.00218 -0.00088 C3 1 0.869726 0.454162 0.058376 11.00000 0.02686 0.02089 = 0.03147 -0.01023 0.00297 -0.00507 C4 1 0.547765 0.504984 0.118889 11.00000 0.02832 0.01786 = 0.03277 -0.01121 0.00091 -0.00230 C5 1 0.357608 0.496243 0.170754 11.00000 0.03064 0.02314 = 0.03365 -0.01042 0.00579 -0.00639 C6 1 0.168153 0.578489 0.180169 11.00000 0.02912 0.02650 = 0.03245 -0.00928 0.00303 -0.00503 AFIX 43 H6 2 0.143953 0.653915 0.151700 11.00000 -1.20000 AFIX 0 C7 1 0.012167 0.540672 0.236155 11.00000 0.02670 0.02670 = 0.03696 -0.01543 0.00514 -0.00497 C8 1 0.086549 0.429712 0.268155 11.00000 0.03565 0.02725 = 0.04085 -0.01386 0.01407 -0.00510 AFIX 43 H8 2 0.004619 0.389277 0.306786 11.00000 -1.20000 AFIX 0 C9 1 -0.206724 0.617885 0.254858 11.00000 0.02602 0.02730 = 0.03958 -0.01361 0.00844 -0.00354 AFIX 23 H9A 2 -0.328673 0.652698 0.213796 11.00000 -1.20000 H9B 2 -0.138167 0.677978 0.264216 11.00000 -1.20000 AFIX 0 C10 1 -0.354623 0.566245 0.316987 11.00000 0.03221 0.02780 = 0.03772 -0.01187 0.00820 -0.00522 AFIX 23 H10A 2 -0.234355 0.528141 0.358153 11.00000 -1.20000 H10B 2 -0.436288 0.509968 0.306996 11.00000 -1.20000 AFIX 0 C11 1 -0.560205 0.653738 0.333368 11.00000 0.03095 0.02884 = 0.03698 -0.01471 0.00652 -0.00073 AFIX 23 H11A 2 -0.476757 0.710052 0.342668 11.00000 -1.20000 H11B 2 -0.678342 0.691756 0.291750 11.00000 -1.20000 AFIX 0 C12 1 -0.716009 0.608175 0.395109 11.00000 0.03319 0.03084 = 0.03878 -0.01459 0.00824 -0.00739 AFIX 23 H12A 2 -0.598846 0.567950 0.436683 11.00000 -1.20000 H12B 2 -0.807099 0.554483 0.385276 11.00000 -1.20000 AFIX 0 C13 1 -0.911187 0.700249 0.410654 11.00000 0.03720 0.03555 = 0.04398 -0.02020 0.01205 -0.00821 AFIX 23 H13A 2 -0.819146 0.754397 0.419502 11.00000 -1.20000 H13B 2 -1.028241 0.739816 0.368979 11.00000 -1.20000 AFIX 0 C14 1 -1.069640 0.658792 0.472669 11.00000 0.04754 0.04792 = 0.04631 -0.02412 0.01782 -0.01228 AFIX 137 H14A 2 -1.163251 0.605732 0.464222 11.00000 -1.50000 H14B 2 -1.191726 0.721756 0.479132 11.00000 -1.50000 H14C 2 -0.956115 0.622157 0.514638 11.00000 -1.50000 AFIX 0 N1 3 0.720385 0.421269 0.114687 11.00000 0.02663 0.02000 = 0.03410 -0.01127 0.00439 -0.00345 S1 4 0.551797 0.633895 0.056106 11.00000 0.02920 0.02082 = 0.03439 -0.00974 0.00852 -0.00063 S2 4 0.345074 0.369737 0.231452 11.00000 0.03978 0.02271 = 0.04080 -0.00931 0.01476 -0.00437 MOLE 2 C15 1 0.042830 -0.119095 0.025205 11.00000 0.03100 0.01871 = 0.03092 -0.00871 0.00234 -0.00161 C16 1 0.186013 -0.060627 0.051348 11.00000 0.02636 0.02106 = 0.02709 -0.00737 0.00276 0.00022 C17 1 0.145314 0.056559 0.026453 11.00000 0.02568 0.02085 = 0.03053 -0.01144 0.00690 -0.00521 C18 1 0.462348 0.026279 0.104118 11.00000 0.02721 0.02039 = 0.02960 -0.01068 0.00660 -0.00504 C19 1 0.648441 0.050713 0.144715 11.00000 0.02785 0.01837 = 0.03245 -0.00903 0.00396 -0.00438 C20 1 0.827376 -0.018673 0.195397 11.00000 0.02826 0.02146 = 0.03138 -0.00986 0.00328 -0.00326 AFIX 43 H20 2 0.850696 -0.097334 0.209858 11.00000 -1.20000 AFIX 0 C21 1 0.974649 0.038918 0.224168 11.00000 0.02673 0.02690 = 0.02875 -0.00888 0.00534 -0.00375 C22 1 0.904153 0.151760 0.192876 11.00000 0.02803 0.02516 = 0.03480 -0.01437 0.00405 -0.00544 AFIX 43 H22 2 0.982661 0.204011 0.204571 11.00000 -1.20000 AFIX 0 C23 1 1.179178 -0.019600 0.281298 11.00000 0.03517 0.02761 = 0.03679 -0.01086 -0.00007 -0.00588 AFIX 23 H23A 2 1.308891 -0.070914 0.264928 11.00000 -1.20000 H23B 2 1.100841 -0.065144 0.321763 11.00000 -1.20000 AFIX 0 C24 1 1.314714 0.056318 0.305553 11.00000 0.03246 0.03035 = 0.03578 -0.01240 0.00368 -0.00832 AFIX 23 H24A 2 1.185379 0.111920 0.318507 11.00000 -1.20000 H24B 2 1.408542 0.096735 0.266663 11.00000 -1.20000 AFIX 0 C25 1 1.502225 -0.007919 0.367703 11.00000 0.04156 0.03742 = 0.03718 -0.01071 -0.00170 -0.00883 AFIX 23 H25A 2 1.618943 -0.068829 0.356235 11.00000 -1.20000 H25B 2 1.404906 -0.042036 0.407829 11.00000 -1.20000 AFIX 0 C26 1 1.662329 0.063077 0.389122 11.00000 0.03947 0.05570 = 0.03914 -0.02201 0.00275 -0.01307 AFIX 23 H26A 2 1.795192 0.013483 0.424859 11.00000 -1.20000 H26B 2 1.751301 0.100608 0.348094 11.00000 -1.20000 AFIX 0 C27 1 1.511593 0.150733 0.417877 11.00000 0.04843 0.05246 = 0.03829 -0.01917 0.00649 -0.01857 AFIX 23 H27A 2 1.431448 0.113832 0.460876 11.00000 -1.20000 H27B 2 1.372997 0.198856 0.383416 11.00000 -1.20000 AFIX 0 C28 1 1.683381 0.222203 0.434148 11.00000 0.06140 0.07965 = 0.06915 -0.04698 0.02056 -0.03623 AFIX 137 H28A 2 1.819239 0.174869 0.468780 11.00000 -1.50000 H28B 2 1.580916 0.277561 0.452648 11.00000 -1.50000 H28C 2 1.760174 0.260018 0.391451 11.00000 -1.50000 AFIX 0 N2 3 0.304768 0.102984 0.057533 11.00000 0.02877 0.01846 = 0.03189 -0.01121 0.00310 -0.00431 S3 4 0.432799 -0.111505 0.115611 11.00000 0.03103 0.01937 = 0.03325 -0.00935 -0.00116 -0.00191 S4 4 0.659509 0.188455 0.130466 11.00000 0.03034 0.02077 = 0.03147 -0.00959 0.00163 -0.00396 HKLF 4 Covalent radii and connectivity table for 2007src1376 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 C1 - C2 C3_$1 C2 - C1 C3 S1 C3 - N1 C1_$1 C2 C4 - N1 C5 S1 C5 - C6 C4 S2 C6 - C5 C7 C7 - C8 C6 C9 C8 - C7 S2 C9 - C7 C10 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 N1 - C4 C3 S1 - C2 C4 S2 - C8 C5 C15 - C16 C17_$2 C16 - C15 C17 S3 C17 - N2 C15_$2 C16 C18 - N2 C19 S3 C19 - C20 C18 S4 C20 - C19 C21 C21 - C22 C20 C23 C22 - C21 S4 C23 - C21 C24 C24 - C23 C25 C25 - C24 C26 C26 - C27 C25 C27 - C26 C28 C28 - C27 N2 - C18 C17 S3 - C16 C18 S4 - C22 C19 Operators for generating equivalent atoms: $1 -x+2, -y+1, -z $2 -x, -y, -z 23476 Reflections read, of which 106 rejected -6 =< h =< 6, -16 =< k =< 16, -26 =< l =< 26, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 9 7 23.34 3.02 2 20.04 1 Inconsistent equivalents 5906 Unique reflections, of which 0 suppressed R(int) = 0.0661 R(sigma) = 0.0523 Friedel opposites merged Maximum memory for data reduction = 3044 / 58357 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 = 3958 / 398006 wR2 = 0.1825 before cycle 1 for 5906 data and 317 / 317 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 4.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52536 0.00125 0.003 OSF Mean shift/esd = 0.001 Maximum = -0.009 for U13 S1 Max. shift = 0.000 A for H15 Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3958 / 398006 wR2 = 0.1825 before cycle 2 for 5906 data and 317 / 317 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 4.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52536 0.00125 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.004 for U12 S4 Max. shift = 0.000 A for H15 Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3958 / 398006 wR2 = 0.1825 before cycle 3 for 5906 data and 317 / 317 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 4.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52536 0.00125 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U23 S2 Max. shift = 0.000 A for H15 Max. dU = 0.000 for H15 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3958 / 398006 wR2 = 0.1825 before cycle 4 for 5906 data and 317 / 317 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 4.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52536 0.00125 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H14A Max. dU = 0.000 for H1 Largest correlation matrix elements -0.607 U23 C28 / U33 C28 -0.526 U12 C28 / U13 C28 -0.510 U23 C14 / U33 C14 -0.593 U23 C28 / U22 C28 -0.514 z C28 / y C28 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6 0.1440 0.6539 0.1517 43 0.950 0.000 C6 C5 C7 H8 0.0046 0.3893 0.3068 43 0.950 0.000 C8 C7 S2 H9A -0.3287 0.6527 0.2138 23 0.990 0.000 C9 C7 C10 H9B -0.1382 0.6780 0.2642 23 0.990 0.000 C9 C7 C10 H10A -0.2344 0.5281 0.3582 23 0.990 0.000 C10 C9 C11 H10B -0.4363 0.5100 0.3070 23 0.990 0.000 C10 C9 C11 H11A -0.4768 0.7101 0.3427 23 0.990 0.000 C11 C12 C10 H11B -0.6783 0.6918 0.2917 23 0.990 0.000 C11 C12 C10 H12A -0.5988 0.5680 0.4367 23 0.990 0.000 C12 C11 C13 H12B -0.8071 0.5545 0.3853 23 0.990 0.000 C12 C11 C13 H13A -0.8191 0.7544 0.4195 23 0.990 0.000 C13 C14 C12 H13B -1.0282 0.7398 0.3690 23 0.990 0.000 C13 C14 C12 H14A -1.1632 0.6057 0.4642 137 0.980 0.000 C14 C13 H14A H14B -1.1917 0.7218 0.4791 137 0.980 0.000 C14 C13 H14A H14C -0.9561 0.6222 0.5146 137 0.980 0.000 C14 C13 H14A H20 0.8507 -0.0973 0.2099 43 0.950 0.000 C20 C19 C21 H22 0.9827 0.2040 0.2046 43 0.950 0.000 C22 C21 S4 H23A 1.3089 -0.0709 0.2649 23 0.990 0.000 C23 C21 C24 H23B 1.1008 -0.0651 0.3218 23 0.990 0.000 C23 C21 C24 H24A 1.1854 0.1119 0.3185 23 0.990 0.000 C24 C23 C25 H24B 1.4085 0.0967 0.2667 23 0.990 0.000 C24 C23 C25 H25A 1.6189 -0.0688 0.3562 23 0.990 0.000 C25 C24 C26 H25B 1.4049 -0.0420 0.4078 23 0.990 0.000 C25 C24 C26 H26A 1.7952 0.0135 0.4249 23 0.990 0.000 C26 C27 C25 H26B 1.7513 0.1006 0.3481 23 0.990 0.000 C26 C27 C25 H27A 1.4314 0.1138 0.4609 23 0.990 0.000 C27 C26 C28 H27B 1.3730 0.1989 0.3834 23 0.990 0.000 C27 C26 C28 H28A 1.8192 0.1749 0.4688 137 0.980 0.000 C28 C27 H28A H28B 1.5809 0.2776 0.4526 137 0.980 0.000 C28 C27 H28A H28C 1.7602 0.2600 0.3915 137 0.980 0.000 C28 C27 H28A 2007src1376 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H1 0.89281 0.69445 -0.06432 1.00000 0.02499 0.05801 0.00733 0.00336 0.00200 0.00000 0.00977 H15 0.06560 -0.19883 0.04365 1.00000 0.03368 0.06374 0.00793 0.00366 0.00216 0.00000 0.01103 C1 0.93180 0.61663 -0.03882 1.00000 0.02975 0.01767 0.03484 -0.01123 0.00586 -0.00489 0.02676 0.00542 0.00069 0.00028 0.00019 0.00000 0.00181 0.00161 0.00191 0.00142 0.00144 0.00134 0.00073 C2 0.80677 0.56901 0.01898 1.00000 0.02562 0.01948 0.03262 -0.01353 0.00218 -0.00088 0.02520 0.00523 0.00067 0.00028 0.00019 0.00000 0.00167 0.00159 0.00183 0.00137 0.00136 0.00127 0.00070 C3 0.86973 0.45416 0.05838 1.00000 0.02686 0.02089 0.03147 -0.01023 0.00297 -0.00507 0.02593 0.00528 0.00068 0.00028 0.00019 0.00000 0.00173 0.00162 0.00181 0.00137 0.00137 0.00132 0.00071 C4 0.54776 0.50498 0.11889 1.00000 0.02832 0.01786 0.03277 -0.01121 0.00091 -0.00230 0.02590 0.00523 0.00067 0.00028 0.00019 0.00000 0.00176 0.00154 0.00186 0.00136 0.00142 0.00129 0.00071 C5 0.35761 0.49624 0.17075 1.00000 0.03064 0.02314 0.03365 -0.01042 0.00579 -0.00639 0.02871 0.00562 0.00071 0.00029 0.00019 0.00000 0.00185 0.00170 0.00192 0.00145 0.00147 0.00141 0.00075 C6 0.16815 0.57849 0.18017 1.00000 0.02912 0.02650 0.03245 -0.00928 0.00303 -0.00503 0.02947 0.00561 0.00070 0.00031 0.00019 0.00000 0.00183 0.00179 0.00191 0.00148 0.00145 0.00143 0.00076 H6 0.14395 0.65392 0.15170 1.00000 0.03536 0.00000 0.00000 C7 0.01217 0.54067 0.23615 1.00000 0.02670 0.02670 0.03696 -0.01543 0.00514 -0.00497 0.02895 0.00555 0.00069 0.00030 0.00020 0.00000 0.00179 0.00177 0.00199 0.00152 0.00146 0.00140 0.00076 C8 0.08655 0.42971 0.26816 1.00000 0.03565 0.02725 0.04085 -0.01386 0.01406 -0.00510 0.03414 0.00633 0.00076 0.00032 0.00022 0.00000 0.00204 0.00185 0.00216 0.00161 0.00165 0.00153 0.00085 H8 0.00462 0.38928 0.30679 1.00000 0.04097 0.00000 0.00000 C9 -0.20672 0.61788 0.25486 1.00000 0.02602 0.02730 0.03958 -0.01361 0.00844 -0.00354 0.03058 0.00601 0.00070 0.00031 0.00021 0.00000 0.00178 0.00180 0.00207 0.00155 0.00150 0.00142 0.00078 H9A -0.32867 0.65270 0.21380 1.00000 0.03670 0.00000 0.00000 H9B -0.13817 0.67798 0.26422 1.00000 0.03670 0.00000 0.00000 C10 -0.35462 0.56624 0.31699 1.00000 0.03221 0.02780 0.03772 -0.01187 0.00819 -0.00522 0.03240 0.00622 0.00074 0.00031 0.00021 0.00000 0.00195 0.00186 0.00208 0.00157 0.00157 0.00151 0.00081 H10A -0.23436 0.52814 0.35815 1.00000 0.03889 0.00000 0.00000 H10B -0.43629 0.50997 0.30700 1.00000 0.03889 0.00000 0.00000 C11 -0.56020 0.65374 0.33337 1.00000 0.03095 0.02884 0.03698 -0.01471 0.00652 -0.00073 0.03206 0.00615 0.00073 0.00032 0.00020 0.00000 0.00191 0.00187 0.00206 0.00158 0.00154 0.00149 0.00081 H11A -0.47676 0.71005 0.34267 1.00000 0.03847 0.00000 0.00000 H11B -0.67834 0.69176 0.29175 1.00000 0.03847 0.00000 0.00000 C12 -0.71601 0.60818 0.39511 1.00000 0.03320 0.03084 0.03878 -0.01459 0.00824 -0.00739 0.03335 0.00617 0.00075 0.00032 0.00021 0.00000 0.00200 0.00195 0.00211 0.00163 0.00160 0.00156 0.00083 H12A -0.59885 0.56795 0.43668 1.00000 0.04002 0.00000 0.00000 H12B -0.80710 0.55448 0.38528 1.00000 0.04002 0.00000 0.00000 C13 -0.91119 0.70025 0.41065 1.00000 0.03720 0.03555 0.04398 -0.02020 0.01205 -0.00821 0.03708 0.00655 0.00079 0.00034 0.00022 0.00000 0.00214 0.00212 0.00231 0.00180 0.00175 0.00170 0.00090 H13A -0.81915 0.75440 0.41950 1.00000 0.04449 0.00000 0.00000 H13B -1.02824 0.73982 0.36898 1.00000 0.04449 0.00000 0.00000 C14 -1.06964 0.65879 0.47267 1.00000 0.04754 0.04792 0.04631 -0.02412 0.01782 -0.01228 0.04484 0.00731 0.00090 0.00040 0.00024 0.00000 0.00255 0.00257 0.00252 0.00207 0.00200 0.00204 0.00105 H14A -1.16325 0.60573 0.46422 1.00000 0.06726 0.00000 0.00000 H14B -1.19173 0.72176 0.47913 1.00000 0.06726 0.00000 0.00000 H14C -0.95611 0.62216 0.51464 1.00000 0.06726 0.00000 0.00000 N1 0.72039 0.42127 0.11469 1.00000 0.02663 0.02000 0.03410 -0.01127 0.00439 -0.00345 0.02648 0.00452 0.00056 0.00024 0.00016 0.00000 0.00150 0.00139 0.00163 0.00120 0.00120 0.00114 0.00062 S1 0.55180 0.63389 0.05611 1.00000 0.02920 0.02082 0.03439 -0.00974 0.00852 -0.00063 0.02860 0.00147 0.00017 0.00007 0.00005 0.00000 0.00046 0.00041 0.00048 0.00035 0.00035 0.00033 0.00022 S2 0.34507 0.36974 0.23145 1.00000 0.03978 0.02271 0.04080 -0.00931 0.01476 -0.00437 0.03499 0.00168 0.00020 0.00008 0.00005 0.00000 0.00054 0.00044 0.00055 0.00038 0.00042 0.00037 0.00025 C15 0.04283 -0.11910 0.02521 1.00000 0.03100 0.01871 0.03092 -0.00871 0.00234 -0.00161 0.02717 0.00559 0.00070 0.00029 0.00019 0.00000 0.00185 0.00162 0.00185 0.00138 0.00143 0.00135 0.00073 C16 0.18601 -0.06063 0.05135 1.00000 0.02636 0.02106 0.02709 -0.00737 0.00276 0.00022 0.02563 0.00552 0.00067 0.00028 0.00018 0.00000 0.00170 0.00162 0.00173 0.00133 0.00132 0.00129 0.00070 C17 0.14531 0.05656 0.02645 1.00000 0.02568 0.02085 0.03053 -0.01144 0.00690 -0.00521 0.02488 0.00531 0.00066 0.00028 0.00018 0.00000 0.00168 0.00162 0.00179 0.00136 0.00134 0.00129 0.00069 C18 0.46235 0.02628 0.10412 1.00000 0.02721 0.02039 0.02960 -0.01068 0.00660 -0.00504 0.02510 0.00536 0.00067 0.00028 0.00018 0.00000 0.00170 0.00159 0.00177 0.00134 0.00136 0.00130 0.00070 C19 0.64844 0.05071 0.14471 1.00000 0.02785 0.01837 0.03245 -0.00903 0.00396 -0.00438 0.02605 0.00541 0.00068 0.00028 0.00019 0.00000 0.00174 0.00155 0.00184 0.00135 0.00140 0.00130 0.00071 C20 0.82738 -0.01867 0.19540 1.00000 0.02826 0.02146 0.03138 -0.00986 0.00328 -0.00326 0.02695 0.00542 0.00068 0.00029 0.00019 0.00000 0.00177 0.00163 0.00184 0.00139 0.00140 0.00134 0.00072 H20 0.85070 -0.09733 0.20986 1.00000 0.03234 0.00000 0.00000 C21 0.97465 0.03892 0.22417 1.00000 0.02673 0.02690 0.02875 -0.00888 0.00534 -0.00375 0.02772 0.00562 0.00068 0.00030 0.00019 0.00000 0.00175 0.00176 0.00180 0.00142 0.00139 0.00139 0.00074 C22 0.90415 0.15176 0.19288 1.00000 0.02803 0.02516 0.03480 -0.01437 0.00405 -0.00544 0.02819 0.00553 0.00069 0.00030 0.00019 0.00000 0.00178 0.00174 0.00194 0.00149 0.00144 0.00139 0.00074 H22 0.98266 0.20401 0.20457 1.00000 0.03383 0.00000 0.00000 C23 1.17918 -0.01960 0.28130 1.00000 0.03517 0.02761 0.03679 -0.01086 -0.00007 -0.00588 0.03309 0.00574 0.00076 0.00031 0.00021 0.00000 0.00204 0.00186 0.00207 0.00157 0.00160 0.00154 0.00082 H23A 1.30889 -0.07091 0.26493 1.00000 0.03970 0.00000 0.00000 H23B 1.10084 -0.06514 0.32176 1.00000 0.03970 0.00000 0.00000 C24 1.31471 0.05632 0.30555 1.00000 0.03246 0.03035 0.03578 -0.01240 0.00368 -0.00833 0.03214 0.00569 0.00074 0.00032 0.00020 0.00000 0.00195 0.00189 0.00204 0.00157 0.00155 0.00152 0.00080 H24A 1.18538 0.11192 0.31851 1.00000 0.03857 0.00000 0.00000 H24B 1.40854 0.09673 0.26666 1.00000 0.03857 0.00000 0.00000 C25 1.50222 -0.00792 0.36770 1.00000 0.04157 0.03742 0.03718 -0.01071 -0.00170 -0.00883 0.03883 0.00614 0.00082 0.00035 0.00022 0.00000 0.00230 0.00220 0.00219 0.00175 0.00174 0.00179 0.00092 H25A 1.61894 -0.06883 0.35623 1.00000 0.04660 0.00000 0.00000 H25B 1.40491 -0.04204 0.40783 1.00000 0.04660 0.00000 0.00000 C26 1.66233 0.06308 0.38912 1.00000 0.03947 0.05570 0.03914 -0.02201 0.00275 -0.01307 0.04263 0.00638 0.00085 0.00040 0.00023 0.00000 0.00229 0.00273 0.00231 0.00203 0.00178 0.00199 0.00099 H26A 1.79519 0.01348 0.42486 1.00000 0.05116 0.00000 0.00000 H26B 1.75130 0.10061 0.34809 1.00000 0.05116 0.00000 0.00000 C27 1.51159 0.15073 0.41788 1.00000 0.04843 0.05246 0.03829 -0.01917 0.00649 -0.01857 0.04409 0.00659 0.00091 0.00040 0.00023 0.00000 0.00255 0.00267 0.00232 0.00200 0.00189 0.00211 0.00102 H27A 1.43145 0.11383 0.46088 1.00000 0.05291 0.00000 0.00000 H27B 1.37300 0.19886 0.38342 1.00000 0.05291 0.00000 0.00000 C28 1.68338 0.22220 0.43415 1.00000 0.06140 0.07965 0.06915 -0.04698 0.02056 -0.03623 0.06152 0.00744 0.00108 0.00051 0.00030 0.00000 0.00329 0.00390 0.00351 0.00312 0.00270 0.00296 0.00147 H28A 1.81924 0.17487 0.46878 1.00000 0.09228 0.00000 0.00000 H28B 1.58092 0.27756 0.45265 1.00000 0.09228 0.00000 0.00000 H28C 1.76017 0.26002 0.39145 1.00000 0.09228 0.00000 0.00000 N2 0.30477 0.10298 0.05753 1.00000 0.02877 0.01846 0.03189 -0.01122 0.00310 -0.00431 0.02569 0.00440 0.00057 0.00023 0.00016 0.00000 0.00152 0.00135 0.00158 0.00117 0.00119 0.00114 0.00061 S3 0.43280 -0.11150 0.11561 1.00000 0.03103 0.01937 0.03325 -0.00935 -0.00116 -0.00191 0.02808 0.00137 0.00018 0.00007 0.00005 0.00000 0.00046 0.00041 0.00048 0.00034 0.00035 0.00033 0.00022 S4 0.65951 0.18846 0.13047 1.00000 0.03034 0.02077 0.03147 -0.00959 0.00163 -0.00396 0.02739 0.00136 0.00017 0.00007 0.00005 0.00000 0.00046 0.00041 0.00046 0.00034 0.00034 0.00033 0.00021 Final Structure Factor Calculation for 2007src1376 in P-1 Total number of l.s. parameters = 317 Maximum vector length = 511 Memory required = 3641 / 22995 wR2 = 0.1825 before cycle 5 for 5906 data and 0 / 317 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 4.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0727 for 4840 Fo > 4sig(Fo) and 0.0902 for all 5906 data wR2 = 0.1825, GooF = S = 1.076, Restrained GooF = 1.076 for all data Occupancy sum of asymmetric unit = 34.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0371 0.0276 0.0156 C1 0.0334 0.0278 0.0144 C2 0.0318 0.0265 0.0195 C3 0.0331 0.0291 0.0155 C4 0.0364 0.0276 0.0221 C5 0.0333 0.0288 0.0262 C6 0.0384 0.0272 0.0213 C7 0.0510 0.0298 0.0216 C8 0.0422 0.0291 0.0205 C9 0.0422 0.0298 0.0253 C10 0.0397 0.0360 0.0204 C11 0.0426 0.0307 0.0268 C12 0.0508 0.0353 0.0251 C13 0.0621 0.0450 0.0275 C14 0.0349 0.0267 0.0178 N1 0.0412 0.0274 0.0171 S1 0.0556 0.0274 0.0220 S2 0.0335 0.0305 0.0176 C15 0.0322 0.0263 0.0184 C16 0.0338 0.0230 0.0179 C17 0.0335 0.0238 0.0181 C18 0.0337 0.0269 0.0175 C19 0.0323 0.0285 0.0201 C20 0.0330 0.0274 0.0228 C21 0.0360 0.0278 0.0208 C22 0.0382 0.0340 0.0270 C23 0.0367 0.0317 0.0280 C24 0.0444 0.0371 0.0351 C25 0.0568 0.0389 0.0323 C26 0.0579 0.0400 0.0344 C27 0.1016 0.0468 0.0361 C28 0.0324 0.0286 0.0161 N2 0.0356 0.0303 0.0184 S3 0.0315 0.0309 0.0198 S4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.017 0.027 0.036 0.046 0.059 0.076 0.098 0.144 1.000 Number in group 592. 614. 608. 592. 564. 576. 598. 577. 598. 587. GooF 1.339 1.175 1.086 1.020 0.987 0.969 1.027 0.998 0.985 1.109 K 7.102 1.577 1.162 1.055 0.980 1.005 1.001 0.998 1.012 1.019 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 595. 601. 583. 593. 580. 593. 596. 590. 581. 594. GooF 1.214 1.118 1.129 1.064 1.071 1.088 1.035 1.092 0.835 1.072 K 1.089 1.057 1.051 1.035 1.024 1.022 0.999 0.991 1.002 1.023 R1 0.192 0.167 0.143 0.121 0.119 0.095 0.077 0.065 0.046 0.041 Recommended weighting scheme: WGHT 0.0544 4.1603 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 6 10 316.73 794.18 6.25 0.151 1.14 2 -6 18 24.20 198.83 6.09 0.076 0.77 -2 5 10 240.86 601.95 6.01 0.131 1.42 0 6 0 75.50 0.80 5.97 0.005 2.01 4 4 3 94.24 0.47 5.39 0.004 1.29 0 0 3 65.82 4.87 5.36 0.012 6.40 -2 7 10 216.44 486.28 5.11 0.118 1.26 -3 2 13 1575.22 2484.37 4.92 0.267 1.16 -2 6 13 971.28 1634.84 4.74 0.217 1.20 -3 5 9 2494.90 3633.36 4.47 0.323 1.22 3 4 11 275.79 531.73 4.42 0.124 1.28 -2 8 10 1129.80 1829.46 4.36 0.229 1.18 -2 10 7 55.11 168.60 4.28 0.070 1.06 3 8 6 292.69 123.15 4.07 0.059 1.29 6 2 1 131.37 43.11 3.97 0.035 0.89 -2 14 0 128.26 303.41 3.94 0.093 0.77 -5 1 3 206.36 62.93 3.86 0.042 1.02 3 6 12 1732.24 2614.08 3.80 0.274 1.20 3 -7 5 1257.87 2070.94 3.80 0.244 1.01 -5 5 5 47.19 0.75 3.79 0.005 0.90 4 5 2 48.94 4.45 3.77 0.011 1.27 4 7 8 501.81 804.16 3.68 0.152 1.12 6 9 5 95.24 24.14 3.63 0.026 0.81 -5 2 3 46.57 0.75 3.59 0.005 1.00 -2 8 9 463.35 724.20 3.53 0.144 1.20 5 3 3 51.11 0.60 3.51 0.004 1.06 0 16 14 29.89 107.18 3.51 0.055 0.77 -4 -10 12 88.98 21.33 3.50 0.025 0.77 -4 11 7 113.63 34.55 3.46 0.031 0.79 0 11 16 142.66 273.03 3.45 0.089 0.98 -2 10 9 166.09 324.82 3.44 0.097 1.04 6 2 3 32.78 2.43 3.41 0.008 0.88 -5 8 6 72.83 20.15 3.40 0.024 0.80 5 6 3 106.08 31.76 3.37 0.030 1.02 4 11 8 75.36 174.14 3.33 0.071 0.95 5 11 6 45.56 2.07 3.29 0.008 0.86 5 8 9 40.61 1.69 3.25 0.007 0.92 5 -2 4 28.10 0.14 3.20 0.002 0.96 6 -1 4 30.32 0.16 3.19 0.002 0.83 -5 6 3 35.14 1.93 3.18 0.007 0.87 -4 6 2 82.98 24.34 3.18 0.026 1.02 6 6 5 111.30 215.21 3.16 0.079 0.86 3 1 0 46.88 11.80 3.16 0.018 1.77 -3 10 2 295.29 471.05 3.14 0.116 0.93 1 0 23 46.97 0.54 3.13 0.004 0.82 6 9 3 97.14 219.29 3.11 0.079 0.82 1 -11 3 108.82 206.48 3.09 0.077 0.97 6 7 1 62.53 2.95 3.08 0.009 0.85 6 10 6 16.45 86.22 3.07 0.050 0.79 -6 -6 3 52.32 128.16 3.07 0.061 0.85 Bond lengths and angles C1 - Distance Angles C2 1.3733 (0.0050) C3_$1 1.3965 (0.0047) 116.40 (0.32) C1 - C2 C2 - Distance Angles C1 1.3733 (0.0050) C3 1.4239 (0.0047) 123.58 (0.32) S1 1.7429 (0.0035) 127.59 (0.27) 108.84 (0.26) C2 - C1 C3 C3 - Distance Angles N1 1.3868 (0.0046) C1_$1 1.3965 (0.0047) 124.76 (0.32) C2 1.4239 (0.0047) 115.22 (0.30) 120.02 (0.33) C3 - N1 C1_$1 C4 - Distance Angles N1 1.3004 (0.0043) C5 1.4451 (0.0050) 123.73 (0.33) S1 1.7574 (0.0036) 116.24 (0.27) 120.03 (0.26) C4 - N1 C5 C5 - Distance Angles C6 1.3741 (0.0050) C4 1.4451 (0.0050) 128.67 (0.34) S2 1.7261 (0.0037) 110.57 (0.28) 120.75 (0.27) C5 - C6 C4 C6 - Distance Angles C5 1.3741 (0.0050) C7 1.4167 (0.0052) 113.94 (0.33) C6 - C5 C7 - Distance Angles C8 1.3564 (0.0052) C6 1.4167 (0.0052) 111.23 (0.33) C9 1.5067 (0.0047) 126.63 (0.35) 122.14 (0.33) C7 - C8 C6 C8 - Distance Angles C7 1.3564 (0.0053) S2 1.7229 (0.0038) 112.99 (0.29) C8 - C7 C9 - Distance Angles C7 1.5067 (0.0048) C10 1.5196 (0.0052) 116.43 (0.32) C9 - C7 C10 - Distance Angles C9 1.5196 (0.0052) C11 1.5265 (0.0049) 111.46 (0.31) C10 - C9 C11 - Distance Angles C12 1.5191 (0.0053) C10 1.5265 (0.0049) 114.46 (0.32) C11 - C12 C12 - Distance Angles C11 1.5191 (0.0053) C13 1.5296 (0.0052) 111.97 (0.32) C12 - C11 C13 - Distance Angles C14 1.5198 (0.0057) C12 1.5296 (0.0052) 113.90 (0.35) C13 - C14 C14 - Distance Angles C13 1.5198 (0.0057) C14 - N1 - Distance Angles C4 1.3004 (0.0043) C3 1.3868 (0.0046) 110.68 (0.30) N1 - C4 S1 - Distance Angles C2 1.7429 (0.0035) C4 1.7574 (0.0036) 89.02 (0.17) S1 - C2 S2 - Distance Angles C8 1.7229 (0.0038) C5 1.7261 (0.0037) 91.26 (0.18) S2 - C8 C15 - Distance Angles C16 1.3867 (0.0051) C17_$2 1.3897 (0.0050) 116.63 (0.32) C15 - C16 C16 - Distance Angles C15 1.3867 (0.0051) C17 1.4131 (0.0047) 121.95 (0.33) S3 1.7382 (0.0036) 128.80 (0.27) 109.25 (0.27) C16 - C15 C17 C17 - Distance Angles N2 1.3891 (0.0045) C15_$2 1.3897 (0.0050) 123.40 (0.31) C16 1.4131 (0.0047) 115.17 (0.31) 121.43 (0.33) C17 - N2 C15_$2 C18 - Distance Angles N2 1.2985 (0.0045) C19 1.4370 (0.0050) 122.79 (0.31) S3 1.7635 (0.0035) 115.79 (0.27) 121.42 (0.26) C18 - N2 C19 C19 - Distance Angles C20 1.3709 (0.0050) C18 1.4370 (0.0050) 130.59 (0.32) S4 1.7277 (0.0035) 111.46 (0.27) 117.95 (0.26) C19 - C20 C18 C20 - Distance Angles C19 1.3709 (0.0050) C21 1.4227 (0.0051) 113.26 (0.32) C20 - C19 C21 - Distance Angles C22 1.3737 (0.0050) C20 1.4227 (0.0051) 111.15 (0.33) C23 1.5025 (0.0051) 126.05 (0.34) 122.80 (0.32) C21 - C22 C20 C22 - Distance Angles C21 1.3737 (0.0050) S4 1.7156 (0.0038) 112.95 (0.28) C22 - C21 C23 - Distance Angles C21 1.5025 (0.0051) C24 1.5226 (0.0052) 115.08 (0.32) C23 - C21 C24 - Distance Angles C23 1.5226 (0.0052) C25 1.5240 (0.0054) 112.11 (0.33) C24 - C23 C25 - Distance Angles C24 1.5240 (0.0054) C26 1.5257 (0.0058) 113.91 (0.36) C25 - C24 C26 - Distance Angles C27 1.5210 (0.0062) C25 1.5257 (0.0058) 114.88 (0.37) C26 - C27 C27 - Distance Angles C26 1.5210 (0.0062) C28 1.5279 (0.0064) 111.48 (0.40) C27 - C26 C28 - Distance Angles C27 1.5279 (0.0063) C28 - N2 - Distance Angles C18 1.2985 (0.0046) C17 1.3891 (0.0045) 110.85 (0.29) N2 - C18 S3 - Distance Angles C16 1.7382 (0.0036) C18 1.7635 (0.0035) 88.94 (0.17) S3 - C16 S4 - Distance Angles C22 1.7156 (0.0038) C19 1.7277 (0.0035) 91.18 (0.17) S4 - C22 FMAP and GRID set by program FMAP 2 1 28 GRID -4.000 -2 -1 4.000 2 1 R1 = 0.0897 for 5906 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.8531 0.1794 0.1284 [ 1.02 A from S4 ] Deepest hole -0.46 at 0.2583 0.4263 0.2229 [ 0.75 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3950 / 45473 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8531 0.1794 0.1284 1.00000 0.05 0.51 1.02 S4 1.26 C22 1.84 H22 2.11 C19 Q2 1 0.6839 0.2095 0.0808 1.00000 0.05 0.50 0.97 S4 2.10 C19 2.40 C22 2.75 H1 Q3 1 0.6129 -0.1192 0.1096 1.00000 0.05 0.48 0.96 S3 1.87 C18 2.44 C16 2.52 H20 Q4 1 0.1624 0.3807 0.2388 1.00000 0.05 0.48 0.97 S2 1.02 C8 1.63 H8 2.05 C7 Q5 1 0.4463 -0.0859 0.0620 1.00000 0.05 0.46 1.04 S3 1.37 C16 1.91 C18 2.13 C17 Q6 1 0.5668 0.6543 -0.0009 1.00000 0.05 0.46 1.11 S1 1.48 C2 2.11 C1 2.20 H1 Q7 1 0.5077 0.2026 0.1408 1.00000 0.05 0.46 0.83 S4 1.94 C19 2.25 C22 2.53 H1 Q8 1 0.2742 -0.1015 0.1299 1.00000 0.05 0.46 0.89 S3 1.56 C16 2.03 C18 2.42 C17 Q9 1 0.3636 0.6394 0.0588 1.00000 0.05 0.44 0.99 S1 1.87 C4 2.24 H6 2.30 H15 Q10 1 0.5327 0.3623 0.2248 1.00000 0.05 0.43 1.00 S2 1.81 C5 2.37 C4 2.40 N1 Shortest distances between peaks (including symmetry equivalents) 3 5 1.23 1 2 1.24 2 7 1.52 6 9 1.60 5 8 1.62 3 8 1.83 1 7 1.83 4 10 1.97 2 6 2.20 6 7 2.84 2 9 2.87 5 5 2.93 Time profile in seconds ----------------------- 0.08: 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. 3.16: 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 2.46: Structure factors and derivatives 5.74: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.62: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.24: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1376 finished at 13:38:10 Total CPU time: 12.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++