+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 12:16:16 on 17-Apr-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT039 in P2(1)/c CELL 0.71073 20.3034 10.1636 13.4570 90.000 104.057 90.000 ZERR 4.00 0.0011 0.0005 0.0006 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 120 76 28 40 V = 2693.77 F(000) = 1312.0 Mu = 0.12 mm-1 Cell Wt = 2550.09 Rho = 1.572 SHEL 7 0.84 HTAB N3 O2_$1 EQIV $1 -x-1, y-1/2, -z-1/2 HTAB N4 O7_$2 EQIV $2 -x, y+1/2, -z+1/2 FMAP 2 HTAB PLAN 20 SIZE 0.03 0.04 0.10 ACTA BOND L.S. 4 TEMP -153.00 WGHT 0.056300 EXTI 0.002129 FVAR 0.14796 MOLE 1 C1 1 -0.406690 1.037531 -0.205016 11.00000 0.02846 0.02861 = 0.02407 -0.00078 0.00664 -0.00214 AFIX 43 H1 2 -0.415133 0.978294 -0.261302 11.00000 -1.20000 AFIX 0 C2 1 -0.439918 1.155620 -0.212684 11.00000 0.02593 0.03380 = 0.02242 0.00799 0.00372 0.00093 C3 1 -0.427979 1.248349 -0.135504 11.00000 0.03191 0.02562 = 0.03099 0.00459 0.00804 0.00013 AFIX 43 H3 2 -0.449733 1.331774 -0.143283 11.00000 -1.20000 AFIX 0 C4 1 -0.382422 1.211634 -0.046572 11.00000 0.03093 0.02936 = 0.02409 -0.00460 0.00827 -0.00330 C5 1 -0.348627 1.092819 -0.031851 11.00000 0.02690 0.03032 = 0.01995 0.00199 0.00379 -0.00164 AFIX 43 H5 2 -0.318449 1.071624 0.031902 11.00000 -1.20000 AFIX 0 C6 1 -0.360280 1.005099 -0.113627 11.00000 0.02973 0.02551 = 0.02705 0.00094 0.00920 -0.00453 C7 1 -0.267618 0.845686 -0.048888 11.00000 0.02566 0.03311 = 0.01757 0.00492 0.00458 -0.00243 C8 1 -0.243264 0.715678 -0.070461 11.00000 0.02950 0.02381 = 0.01822 0.00140 0.00509 0.00218 C9 1 -0.261849 0.625464 -0.150503 11.00000 0.02504 0.02802 = 0.02196 0.00503 0.00191 -0.00024 C10 1 -0.216047 0.518840 -0.126907 11.00000 0.02648 0.02819 = 0.01884 0.00284 0.00316 -0.00148 C11 1 -0.170558 0.548352 -0.034823 11.00000 0.03140 0.02676 = 0.01912 0.00088 0.00497 0.00321 C12 1 -0.106386 0.486944 0.023432 11.00000 0.03118 0.03147 = 0.02298 0.00444 0.00521 0.00078 C13 1 -0.026390 0.307331 0.003105 11.00000 0.02949 0.02812 = 0.02094 0.00274 0.00396 -0.00011 C14 1 0.017806 0.310569 0.100032 11.00000 0.02937 0.02954 = 0.02026 -0.00063 0.00469 -0.00019 AFIX 43 H14 2 0.012146 0.373186 0.149712 11.00000 -1.20000 AFIX 0 C15 1 0.069851 0.220565 0.121749 11.00000 0.02636 0.02898 = 0.01946 0.00286 0.00266 -0.00032 C16 1 0.081260 0.126864 0.054284 11.00000 0.02617 0.02954 = 0.02449 0.00235 0.00716 -0.00046 AFIX 43 H16 2 0.117986 0.066510 0.071821 11.00000 -1.20000 AFIX 0 C17 1 0.036039 0.125953 -0.040487 11.00000 0.03363 0.02642 = 0.02248 -0.00301 0.01183 -0.00343 C18 1 -0.016297 0.214250 -0.067903 11.00000 0.02947 0.03280 = 0.02366 0.00165 0.00322 -0.00336 AFIX 43 H18 2 -0.045473 0.212040 -0.134787 11.00000 -1.20000 AFIX 0 C19 1 -0.317775 0.636056 -0.244527 11.00000 0.02714 0.02987 = 0.01963 -0.00086 0.00350 0.00494 C20 1 -0.368233 0.539619 -0.266631 11.00000 0.03462 0.02951 = 0.02316 -0.00033 0.00583 0.00282 AFIX 43 H20 2 -0.366705 0.467404 -0.221306 11.00000 -1.20000 AFIX 0 C21 1 -0.420287 0.548722 -0.353971 11.00000 0.03152 0.03520 = 0.02696 -0.00787 0.00052 -0.00318 AFIX 43 H21 2 -0.454218 0.482356 -0.368636 11.00000 -1.20000 AFIX 0 C22 1 -0.423427 0.653062 -0.419921 11.00000 0.03238 0.04267 = 0.02156 -0.00524 -0.00030 0.00752 AFIX 43 H22 2 -0.459616 0.658871 -0.479648 11.00000 -1.20000 AFIX 0 C23 1 -0.374278 0.749020 -0.399578 11.00000 0.03613 0.03512 = 0.02041 0.00341 0.00594 0.00619 AFIX 43 H23 2 -0.376663 0.821397 -0.444988 11.00000 -1.20000 AFIX 0 C24 1 -0.321381 0.740169 -0.313026 11.00000 0.02988 0.03311 = 0.01872 0.00159 0.00143 0.00176 AFIX 43 H24 2 -0.287067 0.805857 -0.300077 11.00000 -1.20000 AFIX 0 C25 1 -0.215483 0.396699 -0.187332 11.00000 0.02340 0.02838 = 0.02423 0.00271 0.00268 0.00448 C26 1 -0.227023 0.274991 -0.146097 11.00000 0.02896 0.03655 = 0.01889 0.00291 0.00511 0.00105 AFIX 43 H26 2 -0.239295 0.272174 -0.082355 11.00000 -1.20000 AFIX 0 C27 1 -0.220910 0.158903 -0.196314 11.00000 0.03751 0.02638 = 0.03345 0.00257 0.00844 0.00031 AFIX 43 H27 2 -0.228368 0.076938 -0.166918 11.00000 -1.20000 AFIX 0 C28 1 -0.203858 0.162707 -0.289700 11.00000 0.03464 0.03100 = 0.03741 -0.00875 0.00717 -0.00070 AFIX 43 H28 2 -0.199134 0.083104 -0.324319 11.00000 -1.20000 AFIX 0 C29 1 -0.193656 0.282393 -0.332841 11.00000 0.04131 0.04054 = 0.02445 -0.00470 0.01233 -0.00231 AFIX 43 H29 2 -0.182727 0.284886 -0.397569 11.00000 -1.20000 AFIX 0 C30 1 -0.199383 0.398483 -0.281643 11.00000 0.03296 0.03229 = 0.02642 0.00317 0.00474 -0.00562 AFIX 43 H30 2 -0.192187 0.480251 -0.311546 11.00000 -1.20000 AFIX 0 N1 3 -0.491551 1.183594 -0.307377 11.00000 0.03116 0.03802 = 0.03445 0.00740 0.00631 0.00013 N2 3 -0.370428 1.305104 0.039368 11.00000 0.04105 0.03932 = 0.03374 -0.00455 0.00760 0.00755 N3 3 -0.329032 0.881951 -0.109992 11.00000 0.03098 0.02379 = 0.02377 -0.00336 -0.00096 0.00122 AFIX 43 H3A 2 -0.351310 0.821273 -0.151517 11.00000 -1.20000 AFIX 0 N4 3 -0.188309 0.665925 -0.001699 11.00000 0.02890 0.03368 = 0.01477 -0.00164 -0.00107 0.00282 AFIX 43 H4 2 -0.167389 0.704537 0.055851 11.00000 -1.20000 AFIX 0 N5 3 -0.082283 0.390080 -0.029242 11.00000 0.03073 0.03652 = 0.01886 -0.00137 -0.00452 0.00764 AFIX 43 H5A 2 -0.105530 0.378391 -0.092903 11.00000 -1.20000 AFIX 0 N6 3 0.116746 0.219725 0.224714 11.00000 0.02752 0.02936 = 0.02793 0.00446 0.00447 0.00191 N7 3 0.042810 0.021700 -0.113600 11.00000 0.03601 0.03163 = 0.02805 -0.00071 0.01238 -0.00310 O1 4 -0.503157 1.099901 -0.375340 11.00000 0.04708 0.04265 = 0.03060 -0.00292 -0.00643 0.00885 O2 4 -0.521563 1.289025 -0.313184 11.00000 0.04588 0.03774 = 0.04280 0.00732 0.00429 0.01430 O3 4 -0.369974 1.422198 0.019070 11.00000 0.08852 0.02649 = 0.05557 -0.00489 0.00270 0.00271 O4 4 -0.361566 1.260219 0.125547 11.00000 0.05015 0.04814 = 0.03155 -0.00566 0.00794 0.00554 O5 4 -0.233931 0.916970 0.017823 11.00000 0.03364 0.03448 = 0.03013 -0.00735 -0.00532 0.00233 O6 4 -0.077200 0.524992 0.107788 11.00000 0.03741 0.04200 = 0.02231 -0.00502 -0.00658 0.00809 O7 4 0.106742 0.296822 0.288985 11.00000 0.04294 0.04098 = 0.02276 -0.00877 0.00013 0.00833 O8 4 0.163903 0.141304 0.240500 11.00000 0.03180 0.03825 = 0.03584 0.00215 0.00076 0.00981 O9 4 0.089165 -0.057598 -0.085432 11.00000 0.03915 0.03598 = 0.03936 -0.00127 0.01211 0.00586 O10 4 0.000395 0.017683 -0.196084 11.00000 0.04318 0.04311 = 0.02090 -0.00288 0.00241 -0.00506 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 02SOT039 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 C2 - C1 C3 N1 C3 - C4 C2 C4 - C3 C5 N2 C5 - C4 C6 C6 - C5 C1 N3 C7 - O5 N3 C8 C8 - N4 C9 C7 C9 - C8 C10 C19 C10 - C11 C9 C25 C11 - N4 C10 C12 C12 - O6 N5 C11 C13 - C14 N5 C18 C14 - C15 C13 C15 - C16 C14 N6 C16 - C15 C17 C17 - C18 C16 N7 C18 - C17 C13 C19 - C24 C20 C9 C20 - C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 C24 - C23 C19 C25 - C30 C26 C10 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 C29 - C28 C30 C30 - C29 C25 N1 - O2 O1 C2 N2 - O4 O3 C4 N3 - C7 C6 N4 - C11 C8 N5 - C12 C13 N6 - O7 O8 C15 N7 - O9 O10 C17 O1 - N1 O2 - N1 O3 - N2 O4 - N2 O5 - C7 O6 - C12 O7 - N6 O8 - N6 O9 - N7 O10 - N7 Operators for generating equivalent atoms: $1 -x-1, y-1/2, -z-1/2 $2 -x, y+1/2, -z+1/2 21623 Reflections read, of which 3645 rejected -24 =< h =< 24, -12 =< k =< 12, -16 =< l =< 15, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 3 2 95.77 1.91 7 32.88 -10 5 3 27.37 0.92 7 6.79 -11 5 5 26.92 0.94 6 9.34 3 Inconsistent equivalents 4716 Unique reflections, of which 0 suppressed R(int) = 0.0965 R(sigma) = 0.1142 Friedel opposites merged Maximum memory for data reduction = 3235 / 47732 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 = 4338 / 548720 wR2 = 0.1308 before cycle 1 for 4716 data and 425 / 425 parameters GooF = S = 0.928; Restrained GooF = 0.928 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14796 0.00033 0.001 OSF 2 0.00213 0.00053 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for U12 O6 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4338 / 548720 wR2 = 0.1308 before cycle 2 for 4716 data and 425 / 425 parameters GooF = S = 0.928; Restrained GooF = 0.928 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14796 0.00033 0.000 OSF 2 0.00213 0.00053 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U12 O6 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4338 / 548720 wR2 = 0.1308 before cycle 3 for 4716 data and 425 / 425 parameters GooF = S = 0.928; Restrained GooF = 0.928 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14796 0.00033 0.000 OSF 2 0.00213 0.00053 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O3 Max. dU = 0.000 for C26 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4338 / 548720 wR2 = 0.1308 before cycle 4 for 4716 data and 425 / 425 parameters GooF = S = 0.928; Restrained GooF = 0.928 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14796 0.00033 0.000 OSF 2 0.00213 0.00053 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for C24 Max. dU = 0.000 for C2 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 -0.4151 0.9783 -0.2613 43 0.950 0.000 C1 C2 C6 H3 -0.4497 1.3318 -0.1433 43 0.950 0.000 C3 C4 C2 H5 -0.3184 1.0716 0.0319 43 0.950 0.000 C5 C4 C6 H14 0.0121 0.3732 0.1497 43 0.950 0.000 C14 C15 C13 H16 0.1180 0.0665 0.0718 43 0.950 0.000 C16 C15 C17 H18 -0.0455 0.2120 -0.1348 43 0.950 0.000 C18 C17 C13 H20 -0.3667 0.4674 -0.2213 43 0.950 0.000 C20 C21 C19 H21 -0.4542 0.4824 -0.3686 43 0.950 0.000 C21 C22 C20 H22 -0.4596 0.6589 -0.4796 43 0.950 0.000 C22 C21 C23 H23 -0.3767 0.8214 -0.4450 43 0.950 0.000 C23 C22 C24 H24 -0.2871 0.8059 -0.3001 43 0.950 0.000 C24 C23 C19 H26 -0.2393 0.2722 -0.0824 43 0.950 0.000 C26 C27 C25 H27 -0.2284 0.0769 -0.1669 43 0.950 0.000 C27 C26 C28 H28 -0.1991 0.0831 -0.3243 43 0.950 0.000 C28 C27 C29 H29 -0.1827 0.2849 -0.3976 43 0.950 0.000 C29 C28 C30 H30 -0.1922 0.4803 -0.3115 43 0.950 0.000 C30 C29 C25 H3A -0.3513 0.8213 -0.1515 43 0.880 0.000 N3 C7 C6 H4 -0.1674 0.7045 0.0559 43 0.880 0.000 N4 C11 C8 H5A -0.1055 0.3784 -0.0929 43 0.880 0.000 N5 C12 C13 02SOT039 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.40669 1.03753 -0.20502 1.00000 0.02846 0.02861 0.02407 -0.00078 0.00664 -0.00214 0.02700 0.00563 0.00014 0.00027 0.00023 0.00000 0.00173 0.00170 0.00190 0.00140 0.00153 0.00140 0.00073 H1 -0.41513 0.97829 -0.26130 1.00000 0.03240 0.00000 0.00000 C2 -0.43992 1.15562 -0.21268 1.00000 0.02593 0.03380 0.02242 0.00799 0.00372 0.00093 0.02775 0.00574 0.00015 0.00029 0.00023 0.00000 0.00168 0.00181 0.00185 0.00151 0.00145 0.00140 0.00074 C3 -0.42798 1.24835 -0.13550 1.00000 0.03191 0.02562 0.03099 0.00459 0.00804 0.00013 0.02944 0.00575 0.00015 0.00029 0.00024 0.00000 0.00180 0.00167 0.00206 0.00154 0.00161 0.00140 0.00077 H3 -0.44973 1.33177 -0.14328 1.00000 0.03532 0.00000 0.00000 C4 -0.38242 1.21163 -0.04657 1.00000 0.03093 0.02936 0.02409 -0.00460 0.00827 -0.00330 0.02785 0.00559 0.00015 0.00028 0.00023 0.00000 0.00175 0.00174 0.00193 0.00149 0.00154 0.00145 0.00074 C5 -0.34863 1.09282 -0.03185 1.00000 0.02690 0.03032 0.01995 0.00199 0.00379 -0.00164 0.02605 0.00549 0.00014 0.00028 0.00023 0.00000 0.00167 0.00172 0.00178 0.00143 0.00141 0.00138 0.00072 H5 -0.31845 1.07162 0.03190 1.00000 0.03126 0.00000 0.00000 C6 -0.36028 1.00510 -0.11363 1.00000 0.02973 0.02551 0.02705 0.00094 0.00920 -0.00453 0.02703 0.00547 0.00014 0.00027 0.00023 0.00000 0.00177 0.00168 0.00194 0.00153 0.00152 0.00138 0.00073 C7 -0.26762 0.84569 -0.04889 1.00000 0.02566 0.03311 0.01757 0.00492 0.00458 -0.00243 0.02556 0.00589 0.00015 0.00028 0.00023 0.00000 0.00174 0.00177 0.00177 0.00148 0.00151 0.00143 0.00071 C8 -0.24326 0.71568 -0.07046 1.00000 0.02950 0.02381 0.01822 0.00140 0.00509 0.00218 0.02396 0.00538 0.00014 0.00026 0.00022 0.00000 0.00174 0.00162 0.00176 0.00139 0.00145 0.00135 0.00070 C9 -0.26185 0.62546 -0.15050 1.00000 0.02504 0.02802 0.02196 0.00503 0.00191 -0.00024 0.02566 0.00543 0.00014 0.00027 0.00022 0.00000 0.00165 0.00165 0.00181 0.00142 0.00142 0.00136 0.00072 C10 -0.21605 0.51884 -0.12691 1.00000 0.02648 0.02819 0.01884 0.00284 0.00316 -0.00148 0.02491 0.00536 0.00014 0.00027 0.00022 0.00000 0.00169 0.00170 0.00177 0.00138 0.00143 0.00135 0.00072 C11 -0.17056 0.54835 -0.03482 1.00000 0.03140 0.02676 0.01912 0.00088 0.00497 0.00321 0.02596 0.00555 0.00015 0.00027 0.00022 0.00000 0.00180 0.00169 0.00178 0.00137 0.00151 0.00137 0.00073 C12 -0.10639 0.48694 0.02343 1.00000 0.03118 0.03147 0.02298 0.00444 0.00521 0.00078 0.02878 0.00604 0.00015 0.00029 0.00025 0.00000 0.00187 0.00179 0.00194 0.00155 0.00160 0.00146 0.00075 C13 -0.02639 0.30733 0.00311 1.00000 0.02949 0.02812 0.02094 0.00274 0.00396 -0.00011 0.02656 0.00557 0.00015 0.00028 0.00023 0.00000 0.00176 0.00165 0.00185 0.00145 0.00151 0.00139 0.00073 C14 0.01781 0.31057 0.10003 1.00000 0.02937 0.02954 0.02026 -0.00063 0.00469 -0.00019 0.02662 0.00546 0.00014 0.00028 0.00022 0.00000 0.00177 0.00167 0.00187 0.00140 0.00151 0.00139 0.00073 H14 0.01215 0.37319 0.14971 1.00000 0.03195 0.00000 0.00000 C15 0.06985 0.22056 0.12175 1.00000 0.02636 0.02898 0.01946 0.00286 0.00266 -0.00032 0.02543 0.00548 0.00014 0.00028 0.00022 0.00000 0.00171 0.00174 0.00182 0.00142 0.00145 0.00137 0.00072 C16 0.08126 0.12686 0.05428 1.00000 0.02617 0.02954 0.02449 0.00235 0.00716 -0.00046 0.02656 0.00550 0.00014 0.00028 0.00023 0.00000 0.00169 0.00172 0.00189 0.00144 0.00150 0.00136 0.00073 H16 0.11799 0.06651 0.07182 1.00000 0.03187 0.00000 0.00000 C17 0.03604 0.12595 -0.04049 1.00000 0.03363 0.02642 0.02248 -0.00301 0.01183 -0.00343 0.02664 0.00551 0.00015 0.00027 0.00023 0.00000 0.00182 0.00166 0.00186 0.00143 0.00156 0.00143 0.00073 C18 -0.01630 0.21425 -0.06790 1.00000 0.02947 0.03280 0.02366 0.00165 0.00322 -0.00336 0.02920 0.00568 0.00015 0.00028 0.00024 0.00000 0.00181 0.00178 0.00188 0.00153 0.00147 0.00148 0.00075 H18 -0.04547 0.21204 -0.13479 1.00000 0.03504 0.00000 0.00000 C19 -0.31778 0.63606 -0.24453 1.00000 0.02714 0.02987 0.01963 -0.00086 0.00350 0.00494 0.02592 0.00544 0.00014 0.00028 0.00022 0.00000 0.00169 0.00169 0.00177 0.00144 0.00144 0.00140 0.00072 C20 -0.36823 0.53962 -0.26663 1.00000 0.03462 0.02951 0.02316 -0.00033 0.00583 0.00282 0.02930 0.00562 0.00015 0.00029 0.00023 0.00000 0.00188 0.00170 0.00187 0.00141 0.00158 0.00145 0.00076 H20 -0.36670 0.46740 -0.22131 1.00000 0.03516 0.00000 0.00000 C21 -0.42029 0.54872 -0.35397 1.00000 0.03152 0.03520 0.02696 -0.00787 0.00052 -0.00318 0.03236 0.00570 0.00015 0.00031 0.00023 0.00000 0.00187 0.00188 0.00201 0.00161 0.00163 0.00146 0.00080 H21 -0.45422 0.48236 -0.36864 1.00000 0.03883 0.00000 0.00000 C22 -0.42343 0.65306 -0.41992 1.00000 0.03238 0.04267 0.02156 -0.00524 -0.00030 0.00752 0.03338 0.00594 0.00016 0.00031 0.00024 0.00000 0.00189 0.00198 0.00187 0.00165 0.00153 0.00159 0.00080 H22 -0.45962 0.65887 -0.47965 1.00000 0.04005 0.00000 0.00000 C23 -0.37428 0.74902 -0.39958 1.00000 0.03613 0.03512 0.02041 0.00341 0.00594 0.00619 0.03071 0.00583 0.00015 0.00030 0.00023 0.00000 0.00194 0.00181 0.00192 0.00146 0.00160 0.00157 0.00078 H23 -0.37666 0.82140 -0.44499 1.00000 0.03685 0.00000 0.00000 C24 -0.32138 0.74017 -0.31303 1.00000 0.02988 0.03311 0.01872 0.00159 0.00143 0.00176 0.02801 0.00566 0.00015 0.00029 0.00022 0.00000 0.00178 0.00176 0.00183 0.00145 0.00152 0.00140 0.00075 H24 -0.28707 0.80586 -0.30008 1.00000 0.03361 0.00000 0.00000 C25 -0.21548 0.39670 -0.18733 1.00000 0.02340 0.02838 0.02423 0.00271 0.00268 0.00448 0.02587 0.00539 0.00014 0.00027 0.00023 0.00000 0.00169 0.00176 0.00190 0.00144 0.00144 0.00132 0.00073 C26 -0.22702 0.27499 -0.14610 1.00000 0.02896 0.03655 0.01889 0.00291 0.00511 0.00105 0.02825 0.00551 0.00014 0.00028 0.00023 0.00000 0.00177 0.00197 0.00180 0.00148 0.00142 0.00140 0.00075 H26 -0.23929 0.27217 -0.08236 1.00000 0.03390 0.00000 0.00000 C27 -0.22091 0.15890 -0.19631 1.00000 0.03751 0.02638 0.03345 0.00257 0.00844 0.00031 0.03248 0.00573 0.00015 0.00029 0.00024 0.00000 0.00195 0.00175 0.00211 0.00153 0.00166 0.00142 0.00079 H27 -0.22837 0.07694 -0.16692 1.00000 0.03897 0.00000 0.00000 C28 -0.20386 0.16271 -0.28970 1.00000 0.03464 0.03100 0.03741 -0.00875 0.00717 -0.00070 0.03462 0.00573 0.00015 0.00030 0.00025 0.00000 0.00192 0.00184 0.00219 0.00162 0.00168 0.00145 0.00082 H28 -0.19913 0.08310 -0.32432 1.00000 0.04155 0.00000 0.00000 C29 -0.19366 0.28239 -0.33284 1.00000 0.04131 0.04054 0.02445 -0.00470 0.01233 -0.00231 0.03469 0.00583 0.00016 0.00030 0.00025 0.00000 0.00199 0.00208 0.00192 0.00161 0.00156 0.00155 0.00081 H29 -0.18273 0.28489 -0.39757 1.00000 0.04162 0.00000 0.00000 C30 -0.19938 0.39848 -0.28164 1.00000 0.03296 0.03229 0.02642 0.00317 0.00474 -0.00562 0.03098 0.00548 0.00014 0.00030 0.00023 0.00000 0.00185 0.00179 0.00199 0.00153 0.00156 0.00145 0.00077 H30 -0.19219 0.48025 -0.31155 1.00000 0.03718 0.00000 0.00000 N1 -0.49155 1.18359 -0.30738 1.00000 0.03116 0.03802 0.03445 0.00740 0.00631 0.00013 0.03483 0.00533 0.00013 0.00028 0.00022 0.00000 0.00160 0.00168 0.00183 0.00152 0.00140 0.00138 0.00066 N2 -0.37043 1.30510 0.03937 1.00000 0.04105 0.03932 0.03374 -0.00455 0.00760 0.00755 0.03829 0.00517 0.00013 0.00028 0.00023 0.00000 0.00175 0.00182 0.00197 0.00155 0.00146 0.00137 0.00069 N3 -0.32903 0.88195 -0.10999 1.00000 0.03098 0.02379 0.02377 -0.00336 -0.00096 0.00122 0.02749 0.00443 0.00012 0.00022 0.00018 0.00000 0.00147 0.00136 0.00150 0.00112 0.00122 0.00114 0.00061 H3A -0.35131 0.82127 -0.15152 1.00000 0.03299 0.00000 0.00000 N4 -0.18831 0.66592 -0.00170 1.00000 0.02890 0.03368 0.01477 -0.00164 -0.00107 0.00282 0.02688 0.00445 0.00012 0.00022 0.00018 0.00000 0.00143 0.00147 0.00138 0.00119 0.00120 0.00117 0.00060 H4 -0.16739 0.70454 0.05585 1.00000 0.03226 0.00000 0.00000 N5 -0.08228 0.39008 -0.02924 1.00000 0.03073 0.03652 0.01886 -0.00137 -0.00452 0.00764 0.03052 0.00452 0.00012 0.00023 0.00018 0.00000 0.00146 0.00149 0.00148 0.00124 0.00121 0.00124 0.00064 H5A -0.10553 0.37839 -0.09290 1.00000 0.03662 0.00000 0.00000 N6 0.11675 0.21972 0.22471 1.00000 0.02752 0.02936 0.02793 0.00446 0.00447 0.00191 0.02866 0.00476 0.00013 0.00024 0.00020 0.00000 0.00150 0.00152 0.00174 0.00132 0.00131 0.00125 0.00062 N7 0.04281 0.02170 -0.11360 1.00000 0.03601 0.03163 0.02805 -0.00071 0.01238 -0.00310 0.03110 0.00502 0.00014 0.00024 0.00021 0.00000 0.00167 0.00154 0.00174 0.00134 0.00144 0.00134 0.00064 O1 -0.50316 1.09990 -0.37534 1.00000 0.04708 0.04265 0.03060 -0.00292 -0.00643 0.00885 0.04284 0.00428 0.00011 0.00022 0.00017 0.00000 0.00143 0.00137 0.00144 0.00121 0.00118 0.00114 0.00061 O2 -0.52156 1.28902 -0.31318 1.00000 0.04588 0.03774 0.04280 0.00732 0.00429 0.01430 0.04325 0.00419 0.00011 0.00021 0.00017 0.00000 0.00145 0.00133 0.00156 0.00116 0.00119 0.00117 0.00062 O3 -0.36997 1.42220 0.01907 1.00000 0.08852 0.02649 0.05557 -0.00489 0.00270 0.00271 0.05941 0.00448 0.00014 0.00022 0.00019 0.00000 0.00201 0.00138 0.00176 0.00126 0.00151 0.00129 0.00075 O4 -0.36157 1.26022 0.12555 1.00000 0.05015 0.04814 0.03155 -0.00566 0.00794 0.00554 0.04362 0.00423 0.00011 0.00022 0.00019 0.00000 0.00152 0.00143 0.00156 0.00121 0.00121 0.00115 0.00062 O5 -0.23393 0.91697 0.01782 1.00000 0.03364 0.03448 0.03013 -0.00735 -0.00532 0.00233 0.03500 0.00385 0.00010 0.00020 0.00016 0.00000 0.00125 0.00120 0.00136 0.00108 0.00109 0.00101 0.00056 O6 -0.07720 0.52499 0.10779 1.00000 0.03741 0.04200 0.02231 -0.00502 -0.00658 0.00809 0.03629 0.00394 0.00010 0.00020 0.00016 0.00000 0.00130 0.00131 0.00133 0.00105 0.00108 0.00104 0.00056 O7 0.10674 0.29682 0.28898 1.00000 0.04294 0.04098 0.02276 -0.00877 0.00013 0.00833 0.03691 0.00394 0.00010 0.00021 0.00016 0.00000 0.00138 0.00127 0.00133 0.00112 0.00108 0.00108 0.00056 O8 0.16390 0.14130 0.24050 1.00000 0.03180 0.03825 0.03584 0.00215 0.00076 0.00981 0.03658 0.00383 0.00010 0.00020 0.00016 0.00000 0.00126 0.00126 0.00140 0.00106 0.00109 0.00107 0.00056 O9 0.08917 -0.05760 -0.08543 1.00000 0.03915 0.03598 0.03936 -0.00127 0.01211 0.00586 0.03772 0.00396 0.00011 0.00020 0.00016 0.00000 0.00133 0.00127 0.00148 0.00108 0.00116 0.00110 0.00057 O10 0.00039 0.01768 -0.19608 1.00000 0.04318 0.04311 0.02090 -0.00288 0.00241 -0.00506 0.03666 0.00404 0.00011 0.00020 0.00017 0.00000 0.00138 0.00130 0.00131 0.00106 0.00114 0.00109 0.00056 Final Structure Factor Calculation for 02SOT039 in P2(1)/c Total number of l.s. parameters = 425 Maximum vector length = 511 Memory required = 3913 / 22995 wR2 = 0.1308 before cycle 5 for 4716 data and 0 / 425 parameters GooF = S = 0.928; Restrained GooF = 0.928 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0550 for 2684 Fo > 4sig(Fo) and 0.1256 for all 4716 data wR2 = 0.1308, GooF = S = 0.928, Restrained GooF = 0.928 for all data Occupancy sum of asymmetric unit = 47.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0307 0.0265 0.0239 C1 0.0382 0.0269 0.0182 C2 0.0336 0.0318 0.0228 C3 0.0344 0.0278 0.0213 C4 0.0320 0.0266 0.0195 C5 0.0327 0.0275 0.0209 C6 0.0358 0.0249 0.0160 C7 0.0305 0.0235 0.0179 C8 0.0326 0.0259 0.0184 C9 0.0310 0.0258 0.0180 C10 0.0335 0.0254 0.0190 C11 0.0335 0.0318 0.0211 C12 0.0313 0.0285 0.0199 C13 0.0301 0.0296 0.0202 C14 0.0307 0.0272 0.0183 C15 0.0305 0.0264 0.0227 C16 0.0362 0.0251 0.0187 C17 0.0366 0.0282 0.0228 C18 0.0346 0.0237 0.0194 C19 0.0365 0.0283 0.0231 C20 0.0410 0.0363 0.0198 C21 0.0509 0.0299 0.0193 C22 0.0419 0.0306 0.0197 C23 0.0342 0.0321 0.0178 C24 0.0310 0.0276 0.0190 C25 0.0370 0.0293 0.0184 C26 0.0376 0.0343 0.0255 C27 0.0442 0.0348 0.0249 C28 0.0442 0.0387 0.0211 C29 0.0407 0.0274 0.0248 C30 0.0444 0.0316 0.0285 N1 0.0503 0.0353 0.0292 N2 0.0390 0.0242 0.0193 N3 0.0372 0.0299 0.0135 N4 0.0467 0.0303 0.0145 N5 0.0334 0.0295 0.0231 N6 0.0385 0.0305 0.0243 N7 0.0662 0.0384 0.0239 O1 0.0577 0.0476 0.0244 O2 0.0994 0.0532 0.0256 O3 0.0574 0.0440 0.0295 O4 0.0526 0.0323 0.0202 O5 0.0576 0.0345 0.0168 O6 0.0579 0.0337 0.0192 O7 0.0481 0.0389 0.0227 O8 0.0437 0.0398 0.0297 O9 0.0493 0.0406 0.0201 O10 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.027 0.036 0.045 0.057 0.076 0.110 1.000 Number in group 526. 420. 486. 456. 513. 451. 463. 464. 466. 471. GooF 0.747 0.821 0.853 0.958 0.954 0.999 0.925 0.996 0.931 1.068 K 3.294 0.946 0.996 0.919 0.990 0.994 0.996 0.998 0.998 1.023 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.79 inf Number in group 482. 463. 469. 474. 483. 458. 474. 475. 465. 473. GooF 0.827 0.845 0.875 0.911 0.932 0.946 0.892 0.944 0.975 1.106 K 1.077 1.066 1.035 1.023 0.982 1.000 1.014 1.001 1.048 1.008 R1 0.346 0.357 0.259 0.197 0.137 0.093 0.075 0.075 0.053 0.038 Recommended weighting scheme: WGHT 0.0473 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) -18 0 2 -26.11 64.00 3.88 0.025 1.12 9 10 4 375.13 161.53 3.54 0.040 0.86 -1 5 3 1367.09 1108.77 3.36 0.105 1.85 -6 7 7 -27.35 62.35 3.34 0.025 1.14 -9 4 12 -22.90 169.00 3.33 0.041 1.00 8 1 3 5109.75 4215.67 3.31 0.204 1.91 17 5 1 344.08 470.31 3.26 0.068 0.99 4 6 10 1736.20 1269.02 3.25 0.112 0.97 5 6 8 -15.02 59.82 3.24 0.024 1.08 -7 2 1 173.35 229.61 3.16 0.048 2.52 -6 1 7 161.10 97.30 3.07 0.031 1.79 7 1 5 1213.55 1000.61 3.04 0.099 1.69 -4 5 9 90.75 20.34 3.02 0.014 1.20 3 1 1 2489.58 3001.27 3.00 0.172 4.74 -12 1 10 129.97 67.12 2.96 0.026 1.16 -3 6 12 181.57 12.92 2.96 0.011 0.93 12 6 3 261.67 184.09 2.93 0.043 1.09 0 8 9 458.64 103.45 2.90 0.032 0.96 4 5 0 274.08 220.62 2.88 0.047 1.88 -6 6 6 -15.22 52.08 2.87 0.023 1.31 -7 4 5 382.69 478.31 2.86 0.069 1.66 11 1 0 1517.41 1243.84 2.85 0.111 1.76 3 6 3 3048.83 2581.43 2.83 0.160 1.50 -7 10 7 897.33 672.38 2.83 0.082 0.88 -6 6 2 178.92 244.16 2.83 0.049 1.50 2 5 0 890.00 755.13 2.83 0.086 1.99 6 3 2 357.26 290.93 2.82 0.054 2.10 0 0 2 502.04 642.33 2.80 0.080 6.53 -16 1 9 71.17 8.13 2.80 0.009 1.07 -2 5 8 9.10 59.78 2.79 0.024 1.29 -6 1 6 705.35 576.38 2.79 0.075 2.02 -13 6 7 2289.56 1874.77 2.77 0.136 1.05 3 3 7 161.19 214.06 2.77 0.046 1.51 12 9 4 812.05 565.14 2.77 0.075 0.86 -15 3 4 277.29 352.26 2.76 0.059 1.24 1 1 3 711.82 833.52 2.75 0.091 3.76 -5 6 5 18.38 68.79 2.74 0.026 1.40 3 2 9 345.46 469.16 2.74 0.068 1.30 5 10 0 -23.24 136.49 2.74 0.037 0.98 -17 3 8 492.21 340.47 2.73 0.058 1.03 -3 1 3 1264.10 1471.95 2.70 0.121 3.82 1 8 6 269.42 350.39 2.68 0.059 1.09 4 3 12 1285.29 952.25 2.67 0.097 0.97 -3 0 2 897.36 1057.49 2.66 0.102 5.32 0 0 14 450.42 131.95 2.65 0.036 0.93 -5 3 2 4423.00 8091.80 2.64 0.283 2.53 -4 4 13 370.27 190.43 2.64 0.043 0.96 -8 4 5 655.52 855.68 2.62 0.092 1.60 -2 7 1 473.04 559.82 2.60 0.074 1.43 -13 9 5 11.39 144.94 2.59 0.038 0.90 Bond lengths and angles C1 - Distance Angles C2 1.3684 (0.0039) C6 1.3950 (0.0039) 119.26 (0.28) C1 - C2 C2 - Distance Angles C1 1.3684 (0.0039) C3 1.3796 (0.0041) 123.31 (0.28) N1 1.4679 (0.0038) 118.06 (0.28) 118.62 (0.27) C2 - C1 C3 C3 - Distance Angles C4 1.3745 (0.0041) C2 1.3796 (0.0041) 115.34 (0.27) C3 - C4 C4 - Distance Angles C3 1.3745 (0.0041) C5 1.3792 (0.0040) 124.67 (0.28) N2 1.4705 (0.0039) 117.21 (0.26) 118.10 (0.27) C4 - C3 C5 C5 - Distance Angles C4 1.3792 (0.0040) C6 1.3912 (0.0039) 117.67 (0.27) C5 - C4 C6 - Distance Angles C5 1.3912 (0.0039) C1 1.3950 (0.0039) 119.64 (0.26) N3 1.3987 (0.0035) 123.87 (0.27) 116.47 (0.25) C6 - C5 C1 C7 - Distance Angles O5 1.2249 (0.0033) N3 1.3670 (0.0035) 123.14 (0.27) C8 1.4644 (0.0040) 121.58 (0.26) 115.25 (0.26) C7 - O5 N3 C8 - Distance Angles N4 1.3621 (0.0034) C9 1.3949 (0.0039) 107.69 (0.24) C7 1.4644 (0.0040) 117.43 (0.25) 134.84 (0.27) C8 - N4 C9 C9 - Distance Angles C8 1.3949 (0.0039) C10 1.4130 (0.0038) 106.90 (0.25) C19 1.4846 (0.0039) 128.16 (0.25) 124.93 (0.26) C9 - C8 C10 C10 - Distance Angles C11 1.3866 (0.0037) C9 1.4130 (0.0038) 107.10 (0.25) C25 1.4856 (0.0040) 125.30 (0.25) 127.59 (0.26) C10 - C11 C9 C11 - Distance Angles N4 1.3545 (0.0035) C10 1.3866 (0.0037) 108.19 (0.24) C12 1.4851 (0.0040) 117.81 (0.26) 133.58 (0.27) C11 - N4 C10 C12 - Distance Angles O6 1.2094 (0.0034) N5 1.3710 (0.0037) 124.05 (0.27) C11 1.4851 (0.0040) 121.88 (0.28) 113.98 (0.26) C12 - O6 N5 C13 - Distance Angles C14 1.3925 (0.0039) N5 1.3945 (0.0035) 124.65 (0.26) C18 1.3947 (0.0040) 119.29 (0.26) 116.04 (0.26) C13 - C14 N5 C14 - Distance Angles C15 1.3743 (0.0038) C13 1.3925 (0.0039) 118.08 (0.27) C14 - C15 C15 - Distance Angles C16 1.3737 (0.0040) C14 1.3743 (0.0038) 124.42 (0.28) N6 1.4784 (0.0038) 116.22 (0.25) 119.34 (0.26) C15 - C16 C14 C16 - Distance Angles C15 1.3737 (0.0040) C17 1.3787 (0.0039) 115.77 (0.26) C16 - C15 C17 - Distance Angles C18 1.3712 (0.0040) C16 1.3787 (0.0039) 122.88 (0.27) N7 1.4749 (0.0037) 118.84 (0.27) 118.22 (0.26) C17 - C18 C16 C18 - Distance Angles C17 1.3712 (0.0040) C13 1.3947 (0.0040) 119.53 (0.28) C18 - C17 C19 - Distance Angles C24 1.3936 (0.0039) C20 1.3967 (0.0040) 118.30 (0.27) C9 1.4846 (0.0039) 121.68 (0.25) 120.02 (0.26) C19 - C24 C20 C20 - Distance Angles C21 1.3797 (0.0039) C19 1.3967 (0.0040) 120.32 (0.28) C20 - C21 C21 - Distance Angles C22 1.3743 (0.0042) C20 1.3797 (0.0039) 120.51 (0.28) C21 - C22 C22 - Distance Angles C21 1.3743 (0.0042) C23 1.3745 (0.0041) 120.09 (0.29) C22 - C21 C23 - Distance Angles C22 1.3745 (0.0041) C24 1.3822 (0.0039) 119.97 (0.28) C23 - C22 C24 - Distance Angles C23 1.3822 (0.0039) C19 1.3936 (0.0039) 120.80 (0.27) C24 - C23 C25 - Distance Angles C30 1.3854 (0.0040) C26 1.3986 (0.0040) 118.33 (0.28) C10 1.4856 (0.0040) 121.69 (0.27) 119.84 (0.27) C25 - C30 C26 C26 - Distance Angles C27 1.3802 (0.0041) C25 1.3986 (0.0040) 121.21 (0.29) C26 - C27 C27 - Distance Angles C26 1.3802 (0.0041) C28 1.3827 (0.0043) 119.55 (0.29) C27 - C26 C28 - Distance Angles C27 1.3827 (0.0043) C29 1.3850 (0.0043) 120.10 (0.29) C28 - C27 C29 - Distance Angles C28 1.3850 (0.0043) C30 1.3854 (0.0042) 120.03 (0.30) C29 - C28 C30 - Distance Angles C29 1.3854 (0.0042) C25 1.3854 (0.0040) 120.76 (0.29) C30 - C29 N1 - Distance Angles O2 1.2258 (0.0031) O1 1.2292 (0.0032) 123.71 (0.26) C2 1.4679 (0.0038) 117.63 (0.27) 118.64 (0.26) N1 - O2 O1 N2 - Distance Angles O4 1.2182 (0.0032) O3 1.2216 (0.0033) 124.77 (0.28) C4 1.4705 (0.0039) 117.69 (0.27) 117.54 (0.28) N2 - O4 O3 N3 - Distance Angles C7 1.3670 (0.0036) C6 1.3987 (0.0035) 127.02 (0.24) N3 - C7 N4 - Distance Angles C11 1.3545 (0.0035) C8 1.3621 (0.0034) 110.09 (0.23) N4 - C11 N5 - Distance Angles C12 1.3710 (0.0037) C13 1.3945 (0.0035) 129.59 (0.25) N5 - C12 N6 - Distance Angles O7 1.2201 (0.0029) O8 1.2240 (0.0029) 123.58 (0.25) C15 1.4784 (0.0038) 118.72 (0.24) 117.71 (0.25) N6 - O7 O8 N7 - Distance Angles O9 1.2271 (0.0030) O10 1.2292 (0.0030) 125.01 (0.25) C17 1.4749 (0.0037) 117.04 (0.26) 117.90 (0.25) N7 - O9 O10 O1 - Distance Angles N1 1.2292 (0.0032) O1 - O2 - Distance Angles N1 1.2258 (0.0031) O2 - O3 - Distance Angles N2 1.2216 (0.0033) O3 - O4 - Distance Angles N2 1.2182 (0.0032) O4 - O5 - Distance Angles C7 1.2249 (0.0033) O5 - O6 - Distance Angles C12 1.2094 (0.0034) O6 - O7 - Distance Angles N6 1.2201 (0.0029) O7 - O8 - Distance Angles N6 1.2240 (0.0029) O8 - O9 - Distance Angles N7 1.2271 (0.0030) O9 - O10 - Distance Angles N7 1.2292 (0.0030) O10 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.53 3.105(3) 123.6 N3-H3A...O2_$1 0.88 2.35 3.225(3) 176.5 N4-H4...O7_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)