+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:29:51 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SOT062 in P-1 CELL 0.71073 10.6612 11.8523 13.5014 76.852 81.352 72.116 ZERR 4.00 0.0021 0.0024 0.0027 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 56 84 12 12 4 V = 1575.06 F(000) = 664.0 Mu = 0.22 mm-1 Cell Wt = 1245.59 Rho = 1.313 L.S. 4 BOND FMAP 2 PLAN 10 OMIT -3 52 OMIT 0 0 1 OMIT 0 -6 1 OMIT -2 1 4 EXTI WGHT 0.100000 FVAR 0.39963 S1 5 0.262814 0.264329 0.360407 11.00000 0.03698 0.02316 = 0.02167 -0.00250 -0.00599 -0.00328 S2 5 0.585957 0.237106 0.776243 11.00000 0.02111 0.02229 = 0.03829 -0.00094 -0.00134 -0.00358 O1 4 0.049471 0.346021 0.626450 11.00000 0.02558 0.02027 = 0.02899 -0.00751 0.00497 -0.00726 O2 4 0.035539 0.386495 0.820056 11.00000 0.02056 0.03220 = 0.02867 -0.00435 -0.00396 -0.00342 O3 4 -0.187143 0.463747 0.820713 11.00000 0.02046 0.03138 = 0.02306 -0.00903 -0.00091 -0.00479 N1 3 0.329751 0.068364 0.506391 11.00000 0.01900 0.00575 = 0.00627 -0.00053 -0.00204 -0.00124 AFIX 43 H1 2 0.340490 0.035476 0.569391 11.00000 -1.20000 AFIX 0 N2 3 0.296761 0.238332 0.557147 11.00000 0.02730 0.01759 = 0.01759 -0.00185 -0.00149 -0.00274 AFIX 43 H2 2 0.321323 0.190952 0.613586 11.00000 -1.20000 AFIX 0 N3 3 0.347908 0.424361 0.517357 11.00000 0.02960 0.02377 = 0.02394 -0.00445 -0.00098 -0.00726 N4 3 0.383935 0.437146 0.768714 11.00000 0.00636 0.00382 = 0.01766 -0.00151 0.00202 -0.00003 AFIX 43 H4 2 0.301205 0.472653 0.780180 11.00000 -1.20000 AFIX 0 N5 3 0.326135 0.268817 0.809702 11.00000 0.02004 0.01702 = 0.02500 -0.00098 -0.00012 -0.00223 AFIX 43 H5 2 0.246967 0.316584 0.810592 11.00000 -1.20000 AFIX 0 N6 3 0.358245 0.086147 0.756730 11.00000 0.02336 0.02564 = 0.02226 -0.00389 -0.00172 -0.00791 O5 4 0.086795 0.123723 1.064317 11.00000 0.02725 0.03725 = 0.03075 0.00192 -0.00882 -0.00610 O4 4 0.332254 0.150893 1.007314 11.00000 0.02938 0.02125 = 0.01950 -0.00393 0.00099 -0.00839 O6 4 0.146350 0.023840 1.222082 11.00000 0.02267 0.02941 = 0.02345 -0.00204 0.00081 -0.00949 C1 1 0.297107 0.188967 0.477393 11.00000 0.01697 0.02250 = 0.02404 -0.00578 0.00054 -0.00540 C2 1 0.346903 -0.006487 0.431217 11.00000 0.03287 0.02473 = 0.02244 -0.01027 0.00209 -0.00989 AFIX 23 H2A 2 0.427371 -0.005459 0.387057 11.00000 -1.20000 H2B 2 0.272695 0.023241 0.389434 11.00000 -1.20000 AFIX 0 C3 1 0.354765 -0.131999 0.488652 11.00000 0.03693 0.02386 = 0.03219 -0.00822 0.00010 -0.00759 AFIX 137 H3A 2 0.425875 -0.158855 0.532150 11.00000 -1.50000 H3B 2 0.370531 -0.185161 0.441217 11.00000 -1.50000 H3C 2 0.272931 -0.132495 0.529435 11.00000 -1.50000 AFIX 0 C4 1 0.257833 0.365347 0.553571 11.00000 0.02621 0.01960 = 0.01733 -0.00278 -0.00311 -0.00507 C5 1 0.311664 0.543312 0.516608 11.00000 0.03163 0.02599 = 0.02479 -0.00450 0.00033 -0.01312 AFIX 43 H5A 2 0.373250 0.586122 0.490928 11.00000 -1.20000 AFIX 0 C6 1 0.186722 0.605151 0.552345 11.00000 0.03487 0.01803 = 0.02546 -0.00460 -0.00546 -0.00516 AFIX 43 H6 2 0.165164 0.687861 0.550094 11.00000 -1.20000 AFIX 0 C7 1 0.094240 0.542892 0.591420 11.00000 0.02734 0.02364 = 0.02207 -0.00421 -0.00101 -0.00480 AFIX 43 H7 2 0.010129 0.582339 0.617011 11.00000 -1.20000 AFIX 0 C8 1 0.129947 0.420365 0.591507 11.00000 0.02452 0.02107 = 0.01723 -0.00235 -0.00284 -0.00686 C9 1 -0.076725 0.396898 0.675046 11.00000 0.01940 0.02437 = 0.02752 -0.00694 0.00256 -0.00605 AFIX 23 H9A 2 -0.132299 0.344307 0.679795 11.00000 -1.20000 H9B 2 -0.118405 0.474423 0.633962 11.00000 -1.20000 AFIX 0 C10 1 -0.066240 0.413807 0.780257 11.00000 0.01925 0.01834 = 0.02465 -0.00225 -0.00050 -0.00517 C11 1 -0.206632 0.500771 0.921256 11.00000 0.02585 0.04202 = 0.02235 -0.01098 -0.00241 -0.00621 C12 1 -0.170803 0.388210 1.003724 11.00000 0.04042 0.05399 = 0.02651 -0.00119 -0.00130 -0.02077 AFIX 137 H12A 2 -0.221527 0.335186 0.999950 11.00000 -1.50000 H12B 2 -0.190007 0.410656 1.069536 11.00000 -1.50000 H12C 2 -0.078216 0.347608 0.993836 11.00000 -1.50000 AFIX 0 C13 1 -0.352764 0.565098 0.930382 11.00000 0.02617 0.07513 = 0.03504 -0.02771 0.00201 -0.00190 AFIX 137 H13A 2 -0.374114 0.628710 0.871896 11.00000 -1.50000 H13B 2 -0.374854 0.598761 0.991180 11.00000 -1.50000 H13C 2 -0.402248 0.508727 0.933874 11.00000 -1.50000 AFIX 0 C14 1 -0.127497 0.588246 0.917314 11.00000 0.03524 0.03270 = 0.03458 -0.01252 -0.00922 -0.00218 AFIX 137 H14A 2 -0.034978 0.545560 0.916165 11.00000 -1.50000 H14B 2 -0.153687 0.624998 0.976447 11.00000 -1.50000 H14C 2 -0.143605 0.649693 0.856828 11.00000 -1.50000 AFIX 0 C15 1 0.428065 0.316705 0.785142 11.00000 0.02656 0.02188 = 0.01647 -0.00322 -0.00222 -0.00790 C16 1 0.477463 0.507461 0.731220 11.00000 0.02973 0.02360 = 0.03021 -0.00366 0.00072 -0.01440 AFIX 23 H16A 2 0.509924 0.500975 0.661071 11.00000 -1.20000 H16B 2 0.552277 0.477846 0.772385 11.00000 -1.20000 AFIX 0 C17 1 0.406651 0.635925 0.737784 11.00000 0.03613 0.02421 = 0.03817 -0.00396 -0.00445 -0.01177 AFIX 137 H17A 2 0.331373 0.663532 0.698414 11.00000 -1.50000 H17B 2 0.465392 0.685109 0.711386 11.00000 -1.50000 H17C 2 0.377681 0.641693 0.807771 11.00000 -1.50000 AFIX 0 C18 1 0.344035 0.142240 0.834281 11.00000 0.01603 0.01961 = 0.02218 -0.00293 0.00003 -0.00458 C19 1 0.374247 -0.032830 0.777096 11.00000 0.02482 0.02511 = 0.02756 -0.00844 0.00023 -0.00912 AFIX 43 H19 2 0.385712 -0.072795 0.723129 11.00000 -1.20000 AFIX 0 C20 1 0.374314 -0.098576 0.875984 11.00000 0.02543 0.01834 = 0.03282 -0.00316 -0.00225 -0.00649 AFIX 43 H20 2 0.385297 -0.181320 0.887767 11.00000 -1.20000 AFIX 0 C21 1 0.358058 -0.041018 0.956866 11.00000 0.02271 0.02247 = 0.02419 0.00037 -0.00176 -0.00781 AFIX 43 H21 2 0.356812 -0.083846 1.023731 11.00000 -1.20000 AFIX 0 C22 1 0.343551 0.082497 0.936375 11.00000 0.01707 0.02141 = 0.02345 -0.00447 -0.00056 -0.00516 C23 1 0.304299 0.097366 1.110727 11.00000 0.02397 0.02339 = 0.01873 -0.00295 -0.00173 -0.00563 AFIX 23 H23A 2 0.313352 0.147231 1.155585 11.00000 -1.20000 H23B 2 0.367339 0.018432 1.127327 11.00000 -1.20000 AFIX 0 C24 1 0.164827 0.084486 1.127547 11.00000 0.02504 0.01978 = 0.02394 -0.00481 -0.00148 -0.00340 C25 1 0.017902 -0.002815 1.257854 11.00000 0.02116 0.03379 = 0.03332 -0.00617 0.00286 -0.01243 C26 1 -0.007086 -0.079096 1.191171 11.00000 0.03408 0.03916 = 0.03954 -0.00781 -0.00317 -0.01663 AFIX 137 H26A 2 -0.035900 -0.028840 1.127531 11.00000 -1.50000 H26B 2 -0.074301 -0.116256 1.225238 11.00000 -1.50000 H26C 2 0.073089 -0.140591 1.178435 11.00000 -1.50000 AFIX 0 C27 1 -0.090123 0.115753 1.260270 11.00000 0.02649 0.04821 = 0.05442 -0.02102 0.00810 -0.00936 AFIX 137 H27A 2 -0.061693 0.165277 1.294315 11.00000 -1.50000 H27B 2 -0.169370 0.099481 1.296318 11.00000 -1.50000 H27C 2 -0.107422 0.157267 1.191699 11.00000 -1.50000 AFIX 0 C28 1 0.042494 -0.075832 1.365061 11.00000 0.04568 0.06076 = 0.02893 -0.00151 0.00299 -0.02958 AFIX 137 H28A 2 0.121801 -0.141496 1.362280 11.00000 -1.50000 H28B 2 -0.031013 -0.107291 1.392909 11.00000 -1.50000 H28C 2 0.052201 -0.024752 1.407599 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 99SOT062 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - C1 S2 - C15 O1 - C8 C9 O2 - C10 O3 - C10 C11 N1 - C1 C2 N2 - C1 C4 N3 - C4 C5 N4 - C15 C16 N5 - C15 C18 N6 - C18 C19 O5 - C24 O4 - C22 C23 O6 - C24 C25 C1 - N2 N1 S1 C2 - N1 C3 C3 - C2 C4 - N3 C8 N2 C5 - N3 C6 C6 - C7 C5 C7 - C6 C8 C8 - O1 C7 C4 C9 - O1 C10 C10 - O2 O3 C9 C11 - O3 C13 C14 C12 C12 - C11 C13 - C11 C14 - C11 C15 - N4 N5 S2 C16 - N4 C17 C17 - C16 C18 - N6 C22 N5 C19 - N6 C20 C20 - C21 C19 C21 - C20 C22 C22 - O4 C21 C18 C23 - O4 C24 C24 - O5 O6 C23 C25 - O6 C26 C28 C27 C26 - C25 C27 - C25 C28 - C25 21965 Reflections read, of which 1362 rejected -13 =< h =< 13, -14 =< k =< 14, -16 =< l =< 16, Max. 2-theta = 52.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 20.33 0.55 3 6.22 1 1 0 14.59 0.07 4 257.36 6 1 0 381.02 1.67 6 55.47 -7 0 1 51.65 0.80 6 6.37 1 0 1 3.18 0.09 4 0.79 0 1 1 725.49 13.98 2 494.07 5 1 4 2.13 0.20 4 1.36 -2 8 4 151.42 3.26 4 27.91 1 0 7 62.94 1.58 4 8.22 9 Inconsistent equivalents 6191 Unique reflections, of which 0 suppressed R(int) = 0.0465 R(sigma) = 0.0479 Friedel opposites merged Maximum memory for data reduction = 3636 / 62154 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 4771 / 496795 wR2 = 0.1655 before cycle 1 for 6191 data and 388 / 388 parameters GooF = S = 1.194; Restrained GooF = 1.194 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40077 0.00106 1.074 OSF 2 0.00545 0.00202 2.697 EXTI Mean shift/esd = 0.070 Maximum = 2.697 for EXTI Max. shift = 0.001 A for H27B Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4771 / 496795 wR2 = 0.1653 before cycle 2 for 6191 data and 388 / 388 parameters GooF = S = 1.192; Restrained GooF = 1.192 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40115 0.00108 0.347 OSF 2 0.00733 0.00236 0.799 EXTI Mean shift/esd = 0.023 Maximum = 0.799 for EXTI Max. shift = 0.000 A for H28C Max. dU = 0.000 for C28 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4771 / 496795 wR2 = 0.1652 before cycle 3 for 6191 data and 388 / 388 parameters GooF = S = 1.192; Restrained GooF = 1.192 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40113 0.00108 -0.012 OSF 2 0.00722 0.00247 -0.046 EXTI Mean shift/esd = 0.001 Maximum = -0.046 for EXTI Max. shift = 0.000 A for H27C Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4771 / 496795 wR2 = 0.1652 before cycle 4 for 6191 data and 388 / 388 parameters GooF = S = 1.192; Restrained GooF = 1.192 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40112 0.00108 -0.010 OSF 2 0.00712 0.00247 -0.039 EXTI Mean shift/esd = 0.001 Maximum = -0.039 for EXTI Max. shift = 0.000 A for H27C Max. dU = 0.000 for N4 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 H1 0.3405 0.0355 0.5694 43 0.860 0.000 N1 C1 C2 H2 0.3213 0.1910 0.6136 43 0.860 0.000 N2 C1 C4 H4 0.3012 0.4727 0.7802 43 0.860 0.000 N4 C15 C16 H5 0.2470 0.3166 0.8106 43 0.860 0.000 N5 C15 C18 H2A 0.4274 -0.0055 0.3871 23 0.970 0.000 C2 N1 C3 H2B 0.2727 0.0232 0.3894 23 0.970 0.000 C2 N1 C3 H3A 0.4259 -0.1588 0.5321 137 0.960 0.000 C3 C2 H3A H3B 0.3705 -0.1852 0.4412 137 0.960 0.000 C3 C2 H3A H3C 0.2729 -0.1325 0.5294 137 0.960 0.000 C3 C2 H3A H5A 0.3733 0.5861 0.4909 43 0.930 0.000 C5 N3 C6 H6 0.1652 0.6879 0.5501 43 0.930 0.000 C6 C7 C5 H7 0.0101 0.5823 0.6170 43 0.930 0.000 C7 C6 C8 H9A -0.1323 0.3443 0.6798 23 0.970 0.000 C9 O1 C10 H9B -0.1184 0.4744 0.6340 23 0.970 0.000 C9 O1 C10 H12A -0.2215 0.3352 0.9999 137 0.960 0.000 C12 C11 H12A H12B -0.1900 0.4107 1.0695 137 0.960 0.000 C12 C11 H12A H12C -0.0782 0.3476 0.9939 137 0.960 0.000 C12 C11 H12A H13A -0.3741 0.6287 0.8719 137 0.960 0.000 C13 C11 H13A H13B -0.3748 0.5988 0.9912 137 0.960 0.000 C13 C11 H13A H13C -0.4022 0.5087 0.9339 137 0.960 0.000 C13 C11 H13A H14A -0.0350 0.5455 0.9162 137 0.960 0.000 C14 C11 H14A H14B -0.1537 0.6250 0.9764 137 0.960 0.000 C14 C11 H14A H14C -0.1436 0.6497 0.8568 137 0.960 0.000 C14 C11 H14A H16A 0.5099 0.5010 0.6611 23 0.970 0.000 C16 N4 C17 H16B 0.5523 0.4778 0.7724 23 0.970 0.000 C16 N4 C17 H17A 0.3313 0.6635 0.6984 137 0.960 0.000 C17 C16 H17A H17B 0.4654 0.6851 0.7114 137 0.960 0.000 C17 C16 H17A H17C 0.3777 0.6417 0.8078 137 0.960 0.000 C17 C16 H17A H19 0.3857 -0.0728 0.7231 43 0.930 0.000 C19 N6 C20 H20 0.3853 -0.1813 0.8878 43 0.930 0.000 C20 C21 C19 H21 0.3568 -0.0838 1.0237 43 0.930 0.000 C21 C20 C22 H23A 0.3134 0.1472 1.1556 23 0.970 0.000 C23 O4 C24 H23B 0.3673 0.0184 1.1273 23 0.970 0.000 C23 O4 C24 H26A -0.0359 -0.0288 1.1275 137 0.960 0.000 C26 C25 H26A H26B -0.0743 -0.1162 1.2252 137 0.960 0.000 C26 C25 H26A H26C 0.0731 -0.1406 1.1785 137 0.960 0.000 C26 C25 H26A H27A -0.0617 0.1653 1.2943 137 0.960 0.000 C27 C25 H27A H27B -0.1693 0.0995 1.2964 137 0.960 0.000 C27 C25 H27A H27C -0.1075 0.1572 1.1917 137 0.960 0.000 C27 C25 H27A H28A 0.1218 -0.1415 1.3623 137 0.960 0.000 C28 C25 H28A H28B -0.0310 -0.1074 1.3929 137 0.960 0.000 C28 C25 H28A H28C 0.0521 -0.0247 1.4076 137 0.960 0.000 C28 C25 H28A 99SOT062 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.26281 0.26433 0.36041 1.00000 0.03717 0.02333 0.02184 -0.00253 -0.00601 -0.00333 0.02859 0.00085 0.00006 0.00005 0.00004 0.00000 0.00034 0.00033 0.00033 0.00023 0.00023 0.00024 0.00019 S2 0.58596 0.23711 0.77624 1.00000 0.02129 0.02247 0.03847 -0.00097 -0.00136 -0.00363 0.02896 0.00088 0.00005 0.00005 0.00005 0.00000 0.00030 0.00032 0.00038 0.00024 0.00023 0.00022 0.00019 O1 0.04947 0.34602 0.62645 1.00000 0.02576 0.02047 0.02916 -0.00754 0.00494 -0.00732 0.02529 0.00218 0.00014 0.00013 0.00012 0.00000 0.00076 0.00079 0.00087 0.00062 0.00061 0.00061 0.00036 O2 0.03554 0.38649 0.82005 1.00000 0.02073 0.03238 0.02884 -0.00438 -0.00397 -0.00347 0.02831 0.00231 0.00014 0.00014 0.00012 0.00000 0.00077 0.00090 0.00089 0.00067 0.00062 0.00062 0.00038 O3 -0.18714 0.46374 0.82071 1.00000 0.02065 0.03155 0.02325 -0.00907 -0.00094 -0.00484 0.02521 0.00212 0.00013 0.00013 0.00011 0.00000 0.00073 0.00088 0.00084 0.00066 0.00058 0.00062 0.00036 N1 0.32975 0.06836 0.50639 1.00000 0.01916 0.00591 0.00642 -0.00054 -0.00206 -0.00128 0.01103 0.00217 0.00014 0.00013 0.00011 0.00000 0.00078 0.00075 0.00077 0.00056 0.00058 0.00059 0.00033 H1 0.34049 0.03547 0.56939 1.00000 0.01323 0.00000 0.00000 N2 0.29676 0.23833 0.55714 1.00000 0.02744 0.01776 0.01776 -0.00186 -0.00150 -0.00277 0.02214 0.00258 0.00016 0.00015 0.00013 0.00000 0.00092 0.00092 0.00094 0.00069 0.00069 0.00070 0.00040 H2 0.32133 0.19095 0.61358 1.00000 0.02657 0.00000 0.00000 N3 0.34790 0.42436 0.51736 1.00000 0.02977 0.02397 0.02411 -0.00447 -0.00099 -0.00730 0.02620 0.00273 0.00017 0.00016 0.00014 0.00000 0.00097 0.00101 0.00102 0.00076 0.00075 0.00077 0.00043 N4 0.38394 0.43715 0.76871 1.00000 0.00650 0.00396 0.01784 -0.00154 0.00200 -0.00007 0.01019 0.00217 0.00014 0.00013 0.00012 0.00000 0.00068 0.00072 0.00085 0.00058 0.00055 0.00054 0.00033 H4 0.30121 0.47266 0.78018 1.00000 0.01223 0.00000 0.00000 N5 0.32614 0.26881 0.80970 1.00000 0.02020 0.01722 0.02517 -0.00103 -0.00013 -0.00228 0.02227 0.00259 0.00016 0.00015 0.00013 0.00000 0.00086 0.00091 0.00100 0.00072 0.00068 0.00067 0.00041 H5 0.24697 0.31658 0.81059 1.00000 0.02673 0.00000 0.00000 N6 0.35824 0.08615 0.75673 1.00000 0.02354 0.02583 0.02242 -0.00393 -0.00173 -0.00797 0.02386 0.00258 0.00016 0.00016 0.00014 0.00000 0.00091 0.00102 0.00100 0.00075 0.00071 0.00074 0.00042 O5 0.08680 0.12372 1.06432 1.00000 0.02742 0.03742 0.03094 0.00186 -0.00886 -0.00613 0.03336 0.00246 0.00015 0.00015 0.00013 0.00000 0.00082 0.00098 0.00097 0.00073 0.00068 0.00069 0.00041 O4 0.33225 0.15089 1.00732 1.00000 0.02955 0.02144 0.01968 -0.00396 0.00097 -0.00843 0.02362 0.00212 0.00014 0.00013 0.00011 0.00000 0.00078 0.00079 0.00079 0.00060 0.00058 0.00061 0.00035 O6 0.14635 0.02384 1.22208 1.00000 0.02286 0.02961 0.02362 -0.00207 0.00079 -0.00954 0.02569 0.00220 0.00013 0.00013 0.00011 0.00000 0.00075 0.00085 0.00085 0.00064 0.00059 0.00062 0.00036 C1 0.29710 0.18897 0.47740 1.00000 0.01712 0.02266 0.02424 -0.00582 0.00054 -0.00544 0.02142 0.00305 0.00019 0.00019 0.00016 0.00000 0.00098 0.00112 0.00117 0.00087 0.00078 0.00081 0.00046 C2 0.34691 -0.00649 0.43122 1.00000 0.03300 0.02493 0.02263 -0.01032 0.00207 -0.00995 0.02598 0.00322 0.00022 0.00019 0.00017 0.00000 0.00117 0.00118 0.00118 0.00089 0.00088 0.00091 0.00049 H2A 0.42738 -0.00547 0.38706 1.00000 0.03118 0.00000 0.00000 H2B 0.27270 0.02323 0.38943 1.00000 0.03118 0.00000 0.00000 C3 0.35476 -0.13199 0.48865 1.00000 0.03709 0.02406 0.03238 -0.00827 0.00008 -0.00764 0.03128 0.00356 0.00023 0.00020 0.00018 0.00000 0.00127 0.00124 0.00135 0.00098 0.00099 0.00098 0.00054 H3A 0.42588 -0.15885 0.53214 1.00000 0.04692 0.00000 0.00000 H3B 0.37052 -0.18515 0.44121 1.00000 0.04692 0.00000 0.00000 H3C 0.27293 -0.13248 0.52943 1.00000 0.04692 0.00000 0.00000 C4 0.25784 0.36535 0.55358 1.00000 0.02637 0.01978 0.01750 -0.00281 -0.00313 -0.00512 0.02154 0.00305 0.00020 0.00019 0.00016 0.00000 0.00108 0.00109 0.00110 0.00082 0.00081 0.00085 0.00046 C5 0.31167 0.54331 0.51661 1.00000 0.03180 0.02619 0.02493 -0.00452 0.00031 -0.01317 0.02687 0.00328 0.00021 0.00020 0.00017 0.00000 0.00117 0.00124 0.00122 0.00092 0.00090 0.00096 0.00050 H5A 0.37326 0.58612 0.49093 1.00000 0.03224 0.00000 0.00000 C6 0.18672 0.60515 0.55235 1.00000 0.03510 0.01819 0.02563 -0.00464 -0.00548 -0.00519 0.02647 0.00326 0.00022 0.00020 0.00017 0.00000 0.00123 0.00110 0.00121 0.00088 0.00091 0.00090 0.00050 H6 0.16516 0.68786 0.55009 1.00000 0.03177 0.00000 0.00000 C7 0.09425 0.54289 0.59142 1.00000 0.02752 0.02383 0.02221 -0.00424 -0.00103 -0.00486 0.02524 0.00323 0.00021 0.00019 0.00017 0.00000 0.00110 0.00115 0.00116 0.00087 0.00084 0.00088 0.00049 H7 0.01013 0.58233 0.61701 1.00000 0.03028 0.00000 0.00000 C8 0.12995 0.42037 0.59151 1.00000 0.02471 0.02126 0.01738 -0.00237 -0.00285 -0.00693 0.02114 0.00302 0.00019 0.00018 0.00016 0.00000 0.00105 0.00111 0.00107 0.00082 0.00079 0.00084 0.00046 C9 -0.07672 0.39690 0.67505 1.00000 0.01957 0.02456 0.02771 -0.00698 0.00254 -0.00611 0.02416 0.00319 0.00020 0.00020 0.00017 0.00000 0.00101 0.00114 0.00122 0.00090 0.00082 0.00083 0.00048 H9A -0.13230 0.34431 0.67980 1.00000 0.02899 0.00000 0.00000 H9B -0.11840 0.47442 0.63396 1.00000 0.02899 0.00000 0.00000 C10 -0.06624 0.41381 0.78026 1.00000 0.01942 0.01849 0.02483 -0.00226 -0.00052 -0.00523 0.02142 0.00312 0.00019 0.00018 0.00016 0.00000 0.00104 0.00107 0.00116 0.00083 0.00083 0.00082 0.00046 C11 -0.20663 0.50077 0.92125 1.00000 0.02607 0.04219 0.02252 -0.01100 -0.00241 -0.00626 0.03022 0.00341 0.00021 0.00022 0.00018 0.00000 0.00113 0.00142 0.00120 0.00100 0.00087 0.00098 0.00054 C12 -0.17080 0.38821 1.00372 1.00000 0.04058 0.05416 0.02670 -0.00125 -0.00133 -0.02081 0.04004 0.00401 0.00025 0.00025 0.00019 0.00000 0.00139 0.00169 0.00137 0.00115 0.00103 0.00121 0.00062 H12A -0.22149 0.33517 0.99993 1.00000 0.06007 0.00000 0.00000 H12B -0.19004 0.41066 1.06954 1.00000 0.06007 0.00000 0.00000 H12C -0.07820 0.34763 0.99385 1.00000 0.06007 0.00000 0.00000 C13 -0.35276 0.56509 0.93038 1.00000 0.02638 0.07532 0.03517 -0.02773 0.00199 -0.00198 0.04615 0.00410 0.00023 0.00029 0.00021 0.00000 0.00127 0.00206 0.00152 0.00139 0.00102 0.00124 0.00073 H13A -0.37411 0.62870 0.87190 1.00000 0.06923 0.00000 0.00000 H13B -0.37485 0.59875 0.99118 1.00000 0.06923 0.00000 0.00000 H13C -0.40224 0.50872 0.93388 1.00000 0.06923 0.00000 0.00000 C14 -0.12750 0.58823 0.91732 1.00000 0.03538 0.03289 0.03476 -0.01256 -0.00923 -0.00223 0.03438 0.00353 0.00023 0.00022 0.00020 0.00000 0.00128 0.00134 0.00143 0.00106 0.00102 0.00102 0.00057 H14A -0.03498 0.54554 0.91618 1.00000 0.05158 0.00000 0.00000 H14B -0.15370 0.62500 0.97644 1.00000 0.05158 0.00000 0.00000 H14C -0.14359 0.64967 0.85682 1.00000 0.05158 0.00000 0.00000 C15 0.42806 0.31670 0.78514 1.00000 0.02679 0.02206 0.01661 -0.00326 -0.00224 -0.00796 0.02162 0.00299 0.00020 0.00018 0.00016 0.00000 0.00110 0.00114 0.00107 0.00083 0.00080 0.00088 0.00047 C16 0.47747 0.50746 0.73122 1.00000 0.02992 0.02379 0.03036 -0.00367 0.00069 -0.01445 0.02706 0.00332 0.00021 0.00019 0.00018 0.00000 0.00115 0.00118 0.00128 0.00093 0.00091 0.00092 0.00050 H16A 0.50992 0.50097 0.66107 1.00000 0.03247 0.00000 0.00000 H16B 0.55228 0.47784 0.77238 1.00000 0.03247 0.00000 0.00000 C17 0.40665 0.63593 0.73778 1.00000 0.03630 0.02441 0.03833 -0.00398 -0.00449 -0.01181 0.03248 0.00354 0.00023 0.00020 0.00020 0.00000 0.00128 0.00123 0.00145 0.00100 0.00102 0.00098 0.00055 H17A 0.33135 0.66352 0.69844 1.00000 0.04872 0.00000 0.00000 H17B 0.46538 0.68511 0.71135 1.00000 0.04872 0.00000 0.00000 H17C 0.37773 0.64170 0.80778 1.00000 0.04872 0.00000 0.00000 C18 0.34403 0.14224 0.83428 1.00000 0.01619 0.01979 0.02233 -0.00295 0.00002 -0.00462 0.01992 0.00307 0.00019 0.00018 0.00016 0.00000 0.00094 0.00107 0.00113 0.00083 0.00076 0.00077 0.00045 C19 0.37424 -0.03282 0.77709 1.00000 0.02496 0.02530 0.02773 -0.00847 0.00022 -0.00918 0.02523 0.00322 0.00020 0.00019 0.00017 0.00000 0.00108 0.00121 0.00125 0.00093 0.00087 0.00089 0.00049 H19 0.38570 -0.07279 0.72313 1.00000 0.03028 0.00000 0.00000 C20 0.37431 -0.09857 0.87599 1.00000 0.02559 0.01851 0.03300 -0.00320 -0.00226 -0.00653 0.02596 0.00327 0.00020 0.00019 0.00018 0.00000 0.00109 0.00110 0.00132 0.00092 0.00089 0.00086 0.00050 H20 0.38529 -0.18131 0.88777 1.00000 0.03116 0.00000 0.00000 C21 0.35806 -0.04102 0.95686 1.00000 0.02285 0.02266 0.02436 0.00035 -0.00178 -0.00787 0.02381 0.00320 0.00019 0.00019 0.00017 0.00000 0.00105 0.00115 0.00118 0.00087 0.00082 0.00084 0.00048 H21 0.35683 -0.08385 1.02373 1.00000 0.02857 0.00000 0.00000 C22 0.34355 0.08250 0.93638 1.00000 0.01724 0.02160 0.02362 -0.00451 -0.00057 -0.00521 0.02100 0.00307 0.00019 0.00019 0.00016 0.00000 0.00097 0.00110 0.00116 0.00085 0.00077 0.00079 0.00046 C23 0.30430 0.09736 1.11072 1.00000 0.02413 0.02357 0.01893 -0.00301 -0.00173 -0.00566 0.02266 0.00316 0.00020 0.00019 0.00016 0.00000 0.00105 0.00113 0.00111 0.00084 0.00080 0.00084 0.00047 H23A 0.31336 0.14722 1.15559 1.00000 0.02720 0.00000 0.00000 H23B 0.36734 0.01842 1.12732 1.00000 0.02720 0.00000 0.00000 C24 0.16483 0.08448 1.12755 1.00000 0.02522 0.01991 0.02411 -0.00484 -0.00150 -0.00344 0.02373 0.00320 0.00020 0.00019 0.00017 0.00000 0.00108 0.00110 0.00120 0.00087 0.00087 0.00085 0.00048 C25 0.01791 -0.00282 1.25785 1.00000 0.02134 0.03395 0.03350 -0.00618 0.00285 -0.01246 0.02915 0.00344 0.00020 0.00021 0.00019 0.00000 0.00107 0.00131 0.00133 0.00100 0.00089 0.00092 0.00052 C26 -0.00708 -0.07909 1.19118 1.00000 0.03426 0.03934 0.03973 -0.00784 -0.00319 -0.01668 0.03630 0.00354 0.00024 0.00023 0.00020 0.00000 0.00129 0.00146 0.00152 0.00112 0.00105 0.00108 0.00059 H26A -0.03586 -0.02884 1.12753 1.00000 0.05444 0.00000 0.00000 H26B -0.07432 -0.11622 1.22523 1.00000 0.05444 0.00000 0.00000 H26C 0.07309 -0.14061 1.17847 1.00000 0.05444 0.00000 0.00000 C27 -0.09012 0.11574 1.26028 1.00000 0.02667 0.04840 0.05464 -0.02106 0.00805 -0.00941 0.04292 0.00416 0.00023 0.00024 0.00023 0.00000 0.00127 0.00167 0.00176 0.00134 0.00111 0.00113 0.00067 H27A -0.06166 0.16529 1.29428 1.00000 0.06438 0.00000 0.00000 H27B -0.16934 0.09947 1.29638 1.00000 0.06438 0.00000 0.00000 H27C -0.10748 0.15724 1.19171 1.00000 0.06438 0.00000 0.00000 C28 0.04249 -0.07584 1.36506 1.00000 0.04586 0.06095 0.02912 -0.00152 0.00297 -0.02962 0.04384 0.00410 0.00026 0.00026 0.00020 0.00000 0.00149 0.00186 0.00144 0.00125 0.00110 0.00135 0.00068 H28A 0.12184 -0.14147 1.36229 1.00000 0.06575 0.00000 0.00000 H28B -0.03098 -0.10736 1.39288 1.00000 0.06575 0.00000 0.00000 H28C 0.05212 -0.02475 1.40762 1.00000 0.06575 0.00000 0.00000 Final Structure Factor Calculation for 99SOT062 in P-1 Total number of l.s. parameters = 388 Maximum vector length = 511 Memory required = 4383 / 24017 wR2 = 0.1652 before cycle 5 for 6191 data and 0 / 388 parameters GooF = S = 1.192; Restrained GooF = 1.192 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0522 for 4949 Fo > 4sig(Fo) and 0.0681 for all 6191 data wR2 = 0.1652, GooF = S = 1.192, Restrained GooF = 1.192 for all data Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 42.00 for hydrogen atoms Principal mean square atomic displacements U 0.0411 0.0249 0.0198 S1 0.0427 0.0245 0.0197 S2 0.0358 0.0212 0.0189 O1 0.0360 0.0291 0.0198 O2 0.0336 0.0224 0.0197 O3 0.0206 0.0070 0.0055 N1 0.0310 0.0192 0.0163 N2 0.0307 0.0242 0.0237 N3 0.0200 0.0071 0.0035 N4 0.0303 0.0207 0.0159 N5 0.0262 0.0232 0.0222 N6 0.0458 0.0332 0.0211 O5 0.0308 0.0211 0.0189 O4 0.0318 0.0262 0.0190 O6 0.0252 0.0224 0.0166 C1 0.0353 0.0261 0.0165 C2 0.0395 0.0319 0.0225 C3 0.0273 0.0202 0.0171 C4 0.0340 0.0255 0.0211 C5 0.0368 0.0246 0.0180 C6 0.0305 0.0232 0.0220 C7 0.0248 0.0216 0.0171 C8 0.0302 0.0244 0.0178 C9 0.0269 0.0192 0.0182 C10 0.0445 0.0260 0.0201 C11 0.0579 0.0368 0.0254 C12 0.0849 0.0334 0.0201 C13 0.0483 0.0288 0.0261 C14 0.0268 0.0215 0.0165 C15 0.0340 0.0306 0.0166 C16 0.0396 0.0356 0.0222 C17 0.0243 0.0196 0.0159 C18 0.0307 0.0237 0.0213 C19 0.0340 0.0257 0.0183 C20 0.0298 0.0231 0.0186 C21 0.0241 0.0218 0.0171 C22 0.0260 0.0231 0.0188 C23 0.0281 0.0241 0.0190 C24 0.0360 0.0342 0.0173 C25 0.0422 0.0397 0.0270 C26 0.0625 0.0431 0.0231 C27 0.0675 0.0406 0.0234 C28 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.034 0.047 0.061 0.078 0.100 0.131 0.186 1.000 Number in group 644. 619. 598. 625. 608. 621. 633. 609. 624. 610. GooF 1.024 1.240 1.405 1.418 1.410 1.272 1.126 1.038 0.964 0.885 K 1.410 1.057 1.005 1.004 0.983 0.987 0.996 1.020 1.053 1.015 Resolution(A) 0.81 0.84 0.87 0.91 0.96 1.02 1.10 1.21 1.39 1.74 inf Number in group 621. 645. 590. 631. 613. 623. 622. 611. 614. 621. GooF 0.990 0.995 1.096 1.032 0.947 0.959 0.898 1.100 1.713 1.796 K 1.011 1.029 1.021 1.025 1.044 1.055 1.062 1.054 1.037 0.985 R1 0.154 0.118 0.110 0.077 0.062 0.053 0.045 0.047 0.058 0.051 Recommended weighting scheme: WGHT 0.0854 0.8272 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) -5 2 2 1.78 13.15 5.55 0.024 1.68 1 3 8 11.47 38.44 5.45 0.041 1.65 3 -5 2 5.01 16.62 5.22 0.027 1.56 3 -1 1 25.16 52.21 5.18 0.047 2.94 0 -4 1 21.29 45.62 5.16 0.044 2.61 -2 5 0 2.19 19.38 5.13 0.029 1.84 0 1 2 4.40 12.61 5.09 0.023 6.18 2 -2 7 15.46 4.34 5.03 0.014 1.59 6 4 0 10.49 0.56 4.94 0.005 1.66 0 -2 7 38.91 85.57 4.92 0.061 1.68 -2 4 0 31.34 11.37 4.91 0.022 2.18 0 3 3 26.28 53.68 4.91 0.048 3.13 3 1 4 5.45 19.28 4.89 0.029 2.60 1 1 0 105.91 11488.06 4.88 0.703 8.81 5 -3 4 56.79 112.27 4.80 0.069 1.42 -3 1 3 12.65 32.96 4.79 0.038 2.44 3 0 1 72.69 39.59 4.73 0.041 3.33 -7 -3 2 95.59 53.17 4.70 0.048 1.41 -2 -2 3 0.21 5.67 4.69 0.016 2.80 -3 2 1 95.66 55.45 4.67 0.049 2.54 4 2 4 95.33 178.62 4.65 0.088 2.24 -2 -3 1 125.86 230.90 4.59 0.100 3.18 -3 -1 6 231.24 137.23 4.56 0.077 1.74 -3 3 3 59.11 32.79 4.50 0.038 2.01 -4 0 4 26.53 11.77 4.47 0.022 1.92 -5 1 0 191.39 118.15 4.14 0.071 1.90 3 -2 1 2.40 11.01 4.14 0.022 2.51 5 2 2 113.22 70.21 4.13 0.055 2.10 -2 4 2 86.04 52.21 4.11 0.047 2.14 -5 2 1 6.71 0.16 4.06 0.003 1.73 4 1 5 90.87 55.58 3.99 0.049 2.00 -3 3 1 228.31 144.83 3.99 0.079 2.19 -1 -1 3 8.97 0.47 3.91 0.004 3.60 6 -2 2 19.00 37.85 3.87 0.040 1.47 3 -1 5 50.99 23.00 3.85 0.031 2.00 4 -4 1 171.83 107.00 3.84 0.068 1.62 3 2 6 9.77 2.46 3.81 0.010 2.02 -6 0 1 18.82 9.94 3.75 0.021 1.65 2 5 8 40.61 76.55 3.69 0.057 1.51 -5 2 0 81.62 130.95 3.66 0.075 1.75 0 -3 4 20.49 7.92 3.66 0.018 2.24 5 7 4 13.12 28.92 3.62 0.035 1.47 6 -1 4 -0.26 6.99 3.60 0.017 1.47 2 -7 1 24.34 49.57 3.58 0.046 1.37 -7 0 4 27.69 13.08 3.58 0.024 1.28 -6 1 0 31.37 17.41 3.56 0.027 1.60 0 4 8 50.34 27.98 3.55 0.035 1.55 0 7 2 7.46 16.49 3.53 0.027 1.61 -4 3 0 16.63 8.71 3.48 0.019 1.85 2 -2 5 110.46 174.32 3.46 0.087 1.99 Bond lengths and angles S1 - Distance Angles C1 1.6606 (0.0022) S1 - S2 - Distance Angles C15 1.6594 (0.0021) S2 - O1 - Distance Angles C8 1.3743 (0.0026) C9 1.4213 (0.0025) 117.13 (0.16) O1 - C8 O2 - Distance Angles C10 1.2046 (0.0025) O2 - O3 - Distance Angles C10 1.3329 (0.0025) C11 1.4862 (0.0028) 120.81 (0.16) O3 - C10 N1 - Distance Angles C1 1.3411 (0.0026) C2 1.4508 (0.0026) 119.84 (0.17) N1 - C1 N2 - Distance Angles C1 1.3363 (0.0028) C4 1.4248 (0.0027) 123.44 (0.18) N2 - C1 N3 - Distance Angles C4 1.3289 (0.0029) C5 1.3405 (0.0029) 117.46 (0.19) N3 - C4 N4 - Distance Angles C15 1.3354 (0.0026) C16 1.4531 (0.0026) 119.16 (0.16) N4 - C15 N5 - Distance Angles C15 1.3408 (0.0027) C18 1.4190 (0.0027) 122.45 (0.17) N5 - C15 N6 - Distance Angles C18 1.3298 (0.0029) C19 1.3353 (0.0028) 118.55 (0.19) N6 - C18 O5 - Distance Angles C24 1.1969 (0.0026) O5 - O4 - Distance Angles C22 1.3592 (0.0026) C23 1.4243 (0.0026) 116.34 (0.16) O4 - C22 O6 - Distance Angles C24 1.3335 (0.0026) C25 1.4852 (0.0025) 119.88 (0.16) O6 - C24 C1 - Distance Angles N2 1.3363 (0.0028) N1 1.3411 (0.0026) 109.35 (0.18) S1 1.6606 (0.0022) 125.64 (0.16) 125.00 (0.17) C1 - N2 N1 C2 - Distance Angles N1 1.4508 (0.0026) C3 1.4963 (0.0031) 107.07 (0.18) C2 - N1 C3 - Distance Angles C2 1.4963 (0.0031) C3 - C4 - Distance Angles N3 1.3289 (0.0029) C8 1.3937 (0.0029) 123.45 (0.20) N2 1.4248 (0.0027) 117.74 (0.18) 118.77 (0.18) C4 - N3 C8 C5 - Distance Angles N3 1.3405 (0.0029) C6 1.3829 (0.0031) 122.88 (0.21) C5 - N3 C6 - Distance Angles C7 1.3814 (0.0033) C5 1.3829 (0.0031) 119.36 (0.21) C6 - C7 C7 - Distance Angles C6 1.3814 (0.0033) C8 1.3833 (0.0030) 118.30 (0.20) C7 - C6 C8 - Distance Angles O1 1.3743 (0.0026) C7 1.3833 (0.0030) 125.50 (0.18) C4 1.3937 (0.0029) 115.96 (0.18) 118.54 (0.19) C8 - O1 C7 C9 - Distance Angles O1 1.4213 (0.0025) C10 1.5039 (0.0032) 111.66 (0.17) C9 - O1 C10 - Distance Angles O2 1.2046 (0.0025) O3 1.3329 (0.0025) 126.47 (0.21) C9 1.5039 (0.0032) 124.87 (0.19) 108.66 (0.17) C10 - O2 O3 C11 - Distance Angles O3 1.4862 (0.0028) C13 1.5096 (0.0032) 102.69 (0.18) C14 1.5125 (0.0036) 109.32 (0.19) 110.00 (0.22) C12 1.5181 (0.0034) 108.76 (0.20) 111.64 (0.22) 113.81 (0.20) C11 - O3 C13 C14 C12 - Distance Angles C11 1.5181 (0.0034) C12 - C13 - Distance Angles C11 1.5096 (0.0032) C13 - C14 - Distance Angles C11 1.5125 (0.0036) C14 - C15 - Distance Angles N4 1.3354 (0.0026) N5 1.3408 (0.0027) 110.19 (0.17) S2 1.6594 (0.0021) 125.18 (0.16) 124.63 (0.16) C15 - N4 N5 C16 - Distance Angles N4 1.4531 (0.0026) C17 1.4939 (0.0031) 107.60 (0.18) C16 - N4 C17 - Distance Angles C16 1.4939 (0.0031) C17 - C18 - Distance Angles N6 1.3298 (0.0029) C22 1.3991 (0.0030) 122.98 (0.19) N5 1.4190 (0.0027) 116.93 (0.18) 120.08 (0.19) C18 - N6 C22 C19 - Distance Angles N6 1.3353 (0.0028) C20 1.3844 (0.0031) 122.09 (0.21) C19 - N6 C20 - Distance Angles C21 1.3774 (0.0032) C19 1.3844 (0.0031) 119.77 (0.20) C20 - C21 C21 - Distance Angles C20 1.3774 (0.0032) C22 1.3903 (0.0030) 118.56 (0.20) C21 - C20 C22 - Distance Angles O4 1.3592 (0.0026) C21 1.3903 (0.0030) 125.54 (0.19) C18 1.3991 (0.0030) 116.41 (0.18) 118.03 (0.20) C22 - O4 C21 C23 - Distance Angles O4 1.4243 (0.0026) C24 1.5192 (0.0030) 110.48 (0.17) C23 - O4 C24 - Distance Angles O5 1.1969 (0.0026) O6 1.3335 (0.0026) 127.17 (0.20) C23 1.5192 (0.0030) 123.92 (0.20) 108.91 (0.17) C24 - O5 O6 C25 - Distance Angles O6 1.4852 (0.0025) C26 1.5128 (0.0035) 109.58 (0.19) C28 1.5225 (0.0035) 102.10 (0.17) 110.49 (0.21) C27 1.5224 (0.0033) 108.87 (0.19) 113.77 (0.21) 111.37 (0.23) C25 - O6 C26 C28 C26 - Distance Angles C25 1.5128 (0.0035) C26 - C27 - Distance Angles C25 1.5224 (0.0033) C27 - C28 - Distance Angles C25 1.5225 (0.0035) C28 - FMAP and GRID set by program FMAP 2 3 33 GRID -1.667 -2 -2 1.667 2 2 R1 = 0.0679 for 6191 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.66 at 0.6369 0.5485 0.2314 [ 0.23 A from N4 ] Deepest hole -0.92 at 0.6625 0.9698 0.4161 [ 0.19 A from H1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 4053 / 27753 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4206 0.4195 0.7801 1.00000 0.05 0.65 0.42 N4 1.18 C15 1.23 H4 1.36 C16 Q2 1 -0.0404 0.0584 1.2661 1.00000 0.05 0.31 0.72 C27 0.81 C25 1.34 H27B 1.35 H27A Q3 1 0.0420 -0.0361 1.2898 1.00000 0.05 0.31 0.55 C25 1.02 C28 1.51 H28A 1.57 O6 Q4 1 0.6141 0.3371 0.7223 1.00000 0.05 0.29 1.34 S2 1.84 H16B 1.98 H16A 2.10 C15 Q5 1 0.2277 0.5798 0.5611 1.00000 0.05 0.28 0.46 C6 1.03 C5 1.24 H6 1.58 C7 Q6 1 0.5018 0.5053 0.6014 1.00000 0.05 0.26 0.81 H16A 1.74 C16 1.93 H5A 2.04 H5A Q7 1 0.5377 0.3565 0.7631 1.00000 0.05 0.25 1.33 S2 1.36 C15 1.53 H16B 1.62 N4 Q8 1 0.3229 0.6795 0.7988 1.00000 0.05 0.25 0.63 H17C 1.20 C17 1.40 H17A 1.79 H17B Q9 1 -0.0974 0.1000 1.3507 1.00000 0.05 0.24 1.07 H27A 1.14 H27B 1.19 C27 1.93 H28C Q10 1 0.5256 0.4403 0.8217 1.00000 0.05 0.24 0.78 H16B 1.37 C16 1.78 N4 2.14 H16A Shortest distances between peaks (including symmetry equivalents) 4 7 0.91 2 3 1.20 1 7 1.26 2 9 1.33 7 10 1.37 1 10 1.43 4 10 1.96 3 9 2.06 1 4 2.11 4 6 2.39 6 7 2.47 1 6 2.53 6 6 2.78 5 6 2.88 6 10 2.93 8 10 2.97 1 8 2.99 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.02: 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 0.02: Analyse other restraints etc. 3.17: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.13: Structure factors and derivatives 6.80: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.92: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:30:07 Total CPU time: 14.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++