+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 01sot191 started at 15:17:36 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pbcn CELL 0.71073 32.2854 11.8982 19.8475 90.000 90.000 90.000 ZERR 8.00 0.0024 0.0006 0.0011 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 360 252 60 72 V = 7624.18 F(000) = 3408.0 Mu = 0.10 mm-1 Cell Wt = 6570.22 Rho = 1.431 SHEL 7 0.84 TEMP -153 SIZE 0.06 0.04 0.02 FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.032000 FVAR 0.03473 C37 1 0.573678 0.542579 0.265281 11.00000 0.03203 0.02894 = 0.01374 -0.00391 0.00181 0.00161 C38 1 0.534196 0.479897 0.255748 11.00000 0.01729 0.03371 = 0.02623 0.00891 0.00393 0.01414 C39 1 0.521912 0.366967 0.253162 11.00000 0.01886 0.02436 = 0.02382 0.00312 -0.00182 -0.00563 N6 3 0.775845 0.571069 0.301749 11.00000 0.03270 0.03616 = 0.05225 0.01325 0.00909 -0.00841 N7 3 0.606924 0.475665 0.280089 11.00000 0.02128 0.01856 = 0.04319 0.00833 -0.00691 -0.00270 AFIX 43 H7 2 0.601050 0.404024 0.285574 11.00000 -1.20000 AFIX 0 N8 3 0.500000 0.546463 0.250000 10.50000 0.02720 0.02341 = 0.02602 0.00000 0.00229 0.00000 AFIX 43 H8 2 0.500000 0.620424 0.250000 10.50000 -1.20000 AFIX 0 O7 4 0.799863 0.489288 0.302204 11.00000 0.03259 0.04019 = 0.08397 0.00602 -0.00989 0.00801 O8 4 0.787475 0.668774 0.303777 11.00000 0.04568 0.03182 = 0.05800 0.00525 -0.00723 -0.01047 O9 4 0.575114 0.644616 0.262130 11.00000 0.03481 0.02163 = 0.04207 -0.00068 -0.00551 -0.00588 C1 1 -0.200804 0.751166 0.456596 11.00000 0.02057 0.03056 = 0.04215 0.00389 -0.01233 -0.01194 C2 1 -0.207161 0.863916 0.464064 11.00000 0.02485 0.04121 = 0.02492 0.00183 0.00725 0.00054 AFIX 43 H2 2 -0.234028 0.892336 0.473594 11.00000 -1.20000 AFIX 0 C3 1 -0.173761 0.936157 0.457506 11.00000 0.02901 0.03378 = 0.02987 0.01074 0.00623 0.00200 AFIX 43 H3 2 -0.177539 1.015036 0.461666 11.00000 -1.20000 AFIX 0 C4 1 -0.134627 0.892059 0.444765 11.00000 0.02300 0.02755 = 0.02565 0.01487 -0.00195 -0.00103 C5 1 -0.128172 0.777792 0.436254 11.00000 0.03748 0.01546 = 0.04309 0.00824 0.00025 0.00302 AFIX 43 H5 2 -0.101336 0.748885 0.427024 11.00000 -1.20000 AFIX 0 C6 1 -0.162010 0.707224 0.441621 11.00000 0.04442 0.03082 = 0.04377 -0.00325 -0.00524 -0.00900 AFIX 43 H6 2 -0.158745 0.628630 0.435068 11.00000 -1.20000 AFIX 0 C7 1 -0.060510 0.947284 0.431721 11.00000 0.03410 0.04537 = 0.01072 -0.00831 0.00110 0.00217 C8 1 -0.032421 1.044977 0.426102 11.00000 0.02235 0.02173 = 0.03953 -0.00610 0.00364 -0.00407 C9 1 -0.035053 1.160911 0.428707 11.00000 0.03608 0.02422 = 0.00807 -0.01202 -0.00395 -0.00437 C10 1 0.005184 1.202587 0.415706 11.00000 0.02679 0.01485 = 0.01821 -0.00129 0.00671 -0.00431 C11 1 0.030885 1.111547 0.406907 11.00000 0.01939 0.01568 = 0.02834 -0.00030 0.00731 -0.00321 C12 1 0.075557 1.090268 0.393089 11.00000 0.02567 0.02565 = 0.01314 -0.00388 0.00390 -0.00163 C13 1 0.142888 1.190817 0.378556 11.00000 0.02184 0.05553 = 0.02048 0.00549 -0.00606 -0.01916 C14 1 0.168189 1.097695 0.375179 11.00000 0.01675 0.04195 = 0.03755 -0.00450 -0.00362 0.00807 AFIX 43 H14 2 0.156556 1.024504 0.377969 11.00000 -1.20000 AFIX 0 C15 1 0.210242 1.110675 0.367778 11.00000 0.02320 0.05245 = 0.03419 -0.00491 -0.00922 -0.00041 AFIX 43 H15 2 0.227776 1.046839 0.364165 11.00000 -1.20000 AFIX 0 C16 1 0.226535 1.216984 0.365681 11.00000 0.01075 0.05480 = 0.04049 0.00195 -0.00141 -0.01486 C17 1 0.201700 1.312402 0.367376 11.00000 0.04988 0.03796 = 0.02419 -0.00192 0.01160 -0.01627 AFIX 43 H17 2 0.213518 1.385263 0.363683 11.00000 -1.20000 AFIX 0 C18 1 0.159851 1.298919 0.374486 11.00000 0.01312 0.02501 = 0.05956 0.00506 0.00067 -0.00035 AFIX 43 H18 2 0.142295 1.362893 0.376661 11.00000 -1.20000 AFIX 0 C19 1 0.018938 1.322659 0.414499 11.00000 0.01910 0.02255 = 0.02834 0.00605 0.00850 -0.00197 C20 1 0.035113 1.371894 0.472176 11.00000 0.03979 0.03674 = 0.02478 -0.00506 0.00139 0.00243 AFIX 43 H20 2 0.035969 1.330655 0.513139 11.00000 -1.20000 AFIX 0 C21 1 0.049935 1.480455 0.470165 11.00000 0.04935 0.02553 = 0.04739 -0.00108 -0.01844 -0.02288 AFIX 43 H21 2 0.061043 1.514007 0.509662 11.00000 -1.20000 AFIX 0 C22 1 0.048612 1.540171 0.410810 11.00000 0.03585 0.02740 = 0.05817 0.00646 0.00263 -0.01404 AFIX 43 H22 2 0.059023 1.614810 0.409345 11.00000 -1.20000 AFIX 0 C23 1 0.032336 1.492418 0.353792 11.00000 0.04141 0.03584 = 0.01956 0.00770 -0.00094 0.00265 AFIX 43 H23 2 0.031184 1.534308 0.313087 11.00000 -1.20000 AFIX 0 C24 1 0.017463 1.382347 0.355494 11.00000 0.04410 0.00965 = 0.02843 0.00432 0.00049 -0.00768 AFIX 43 H24 2 0.006367 1.348944 0.315943 11.00000 -1.20000 AFIX 0 C25 1 -0.072827 1.228302 0.442063 11.00000 0.01584 0.02516 = 0.03010 -0.00255 0.00900 -0.00476 C26 1 -0.088499 1.303638 0.394145 11.00000 0.02578 0.04037 = 0.03051 -0.00144 0.00702 -0.00766 AFIX 43 H26 2 -0.074461 1.313990 0.352539 11.00000 -1.20000 AFIX 0 C27 1 -0.124457 1.362949 0.407511 11.00000 0.04288 0.03094 = 0.03007 0.00558 -0.00271 -0.00958 AFIX 43 H27 2 -0.134722 1.413864 0.374638 11.00000 -1.20000 AFIX 0 C28 1 -0.145668 1.350268 0.466859 11.00000 0.02935 0.03093 = 0.05237 -0.00710 0.00215 -0.00568 AFIX 43 H28 2 -0.170190 1.392165 0.475170 11.00000 -1.20000 AFIX 0 C29 1 -0.130725 1.275080 0.514737 11.00000 0.03878 0.03693 = 0.03959 -0.00299 0.01956 -0.00059 AFIX 43 H29 2 -0.144953 1.264547 0.556156 11.00000 -1.20000 AFIX 0 C30 1 -0.094262 1.215007 0.500836 11.00000 0.02967 0.01651 = 0.04079 -0.00098 -0.00308 -0.00190 AFIX 43 H30 2 -0.084167 1.163360 0.533437 11.00000 -1.20000 AFIX 0 C31 1 0.677151 0.416539 0.282891 11.00000 0.04899 0.01423 = 0.03340 -0.00130 -0.01425 0.00301 AFIX 43 H31 2 0.667776 0.341854 0.275545 11.00000 -1.20000 AFIX 0 C32 1 0.718643 0.437876 0.288477 11.00000 0.02543 0.03068 = 0.03534 -0.00173 0.00186 -0.00302 AFIX 43 H32 2 0.738301 0.378743 0.285023 11.00000 -1.20000 AFIX 0 C33 1 0.731285 0.546861 0.299207 11.00000 0.01940 0.03195 = 0.03190 0.00617 -0.00290 -0.01697 C34 1 0.703558 0.635494 0.306895 11.00000 0.01486 0.02298 = 0.05120 -0.00611 -0.00758 -0.00397 AFIX 43 H34 2 0.713040 0.709494 0.316126 11.00000 -1.20000 AFIX 0 C35 1 0.661985 0.612486 0.300697 11.00000 0.01523 0.02654 = 0.03786 -0.00154 0.00183 -0.00661 AFIX 43 H35 2 0.642249 0.671238 0.305159 11.00000 -1.20000 AFIX 0 C36 1 0.648817 0.503195 0.287892 11.00000 0.02154 0.03716 = 0.01788 -0.00121 -0.00851 -0.01680 C40 1 0.548855 0.268283 0.257676 11.00000 0.01694 0.02345 = 0.02903 -0.01316 -0.00592 0.01279 C41 1 0.581350 0.253405 0.212425 11.00000 0.03151 0.02696 = 0.03113 -0.00284 0.00184 0.00856 AFIX 43 H41 2 0.584737 0.305127 0.176379 11.00000 -1.20000 AFIX 0 C42 1 0.608821 0.164731 0.218922 11.00000 0.02889 0.03215 = 0.05563 -0.01718 0.00603 0.00614 AFIX 43 H42 2 0.631321 0.157131 0.188415 11.00000 -1.20000 AFIX 0 C43 1 0.603224 0.086095 0.270878 11.00000 0.02550 0.02306 = 0.06339 -0.00067 -0.00391 0.00240 AFIX 43 H43 2 0.622007 0.025352 0.276493 11.00000 -1.20000 AFIX 0 C44 1 0.570037 0.098901 0.313358 11.00000 0.02408 0.02289 = 0.04447 0.00170 -0.00540 0.00372 AFIX 43 H44 2 0.565449 0.044142 0.347384 11.00000 -1.20000 AFIX 0 C45 1 0.543196 0.188172 0.308414 11.00000 0.02177 0.04068 = 0.03229 0.00648 -0.00164 -0.00558 AFIX 43 H45 2 0.520892 0.195434 0.339330 11.00000 -1.20000 AFIX 0 N1 3 -0.235466 0.672525 0.464795 11.00000 0.03729 0.04327 = 0.03511 -0.01109 -0.00739 -0.00358 N2 3 -0.101502 0.969757 0.441414 11.00000 0.03390 0.02101 = 0.03539 0.00001 0.00641 0.00371 AFIX 43 H2A 2 -0.108144 1.041053 0.446147 11.00000 -1.20000 AFIX 0 N3 3 0.007368 1.017064 0.412965 11.00000 0.03311 0.02137 = 0.01640 -0.00244 0.00263 0.00231 AFIX 43 H3A 2 0.016707 0.947908 0.408920 11.00000 -1.20000 AFIX 0 N4 3 0.100090 1.185125 0.389767 11.00000 0.03626 0.01664 = 0.03210 -0.00642 -0.00323 -0.00406 AFIX 43 H4 2 0.087317 1.249791 0.395362 11.00000 -1.20000 AFIX 0 N5 3 0.271938 1.229945 0.361501 11.00000 0.03444 0.05733 = 0.02320 -0.00007 0.00449 -0.00792 O1 4 -0.269945 0.712813 0.477200 11.00000 0.02328 0.04909 = 0.08217 0.00103 0.00629 -0.00078 O2 4 -0.229353 0.571672 0.456256 11.00000 0.05669 0.02124 = 0.09118 0.00010 0.00714 -0.00810 O3 4 -0.046433 0.852645 0.426766 11.00000 0.02565 0.03000 = 0.03939 -0.00374 0.00427 0.00111 O4 4 0.088473 0.995372 0.386836 11.00000 0.03010 0.01819 = 0.04394 -0.00434 -0.00432 0.00333 O5 4 0.292738 1.143022 0.359188 11.00000 0.03963 0.06554 = 0.06692 -0.00808 -0.00033 0.01647 O6 4 0.286781 1.325469 0.360893 11.00000 0.04188 0.06113 = 0.06420 0.00796 -0.00018 -0.01246 HKLF 4 1.0 0.00 0.00 1.00 1.00 0.00 0.00 0.00 1.00 0.00 Covalent radii and connectivity table for s93 in Pbcn C 0.770 H 0.320 N 0.700 O 0.660 C37 - O9 N7 C38 C38 - N8 C39 C37 C39 - C38 C39_$1 C40 N6 - O8 O7 C33 N7 - C37 C36 N8 - C38_$1 C38 O7 - N6 O8 - N6 O9 - C37 C1 - C2 C6 N1 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 N2 C5 - C6 C4 C6 - C5 C1 C7 - O3 N2 C8 C8 - N3 C9 C7 C9 - C8 C10 C25 C10 - C11 C9 C19 C11 - N3 C10 C12 C12 - O4 N4 C11 C13 - C14 C18 N4 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 N5 C17 - C18 C16 C18 - C17 C13 C19 - C24 C20 C10 C20 - C21 C19 C21 - C22 C20 C22 - C23 C21 C23 - C22 C24 C24 - C19 C23 C25 - C30 C26 C9 C26 - C27 C25 C27 - C28 C26 C28 - C27 C29 C29 - C28 C30 C30 - C25 C29 C31 - C32 C36 C32 - C31 C33 C33 - C32 C34 N6 C34 - C35 C33 C35 - C34 C36 C36 - C31 C35 N7 C40 - C41 C45 C39 C41 - C42 C40 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 C45 - C44 C40 N1 - O2 O1 C1 N2 - C7 C4 N3 - C8 C11 N4 - C12 C13 N5 - O6 O5 C16 O1 - N1 O2 - N1 O3 - C7 O4 - C12 O5 - N5 O6 - N5 Operators for generating equivalent atoms: $1 -x+1, y, -z+1/2 44265 Reflections read, of which 3832 rejected -38 =< h =< 38, -14 =< k =< 13, -19 =< l =< 23, Max. 2-theta = 50.03 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 3 3 6.54 0.29 17 1.85 1 Inconsistent equivalents 5946 Unique reflections, of which 0 suppressed R(int) = 0.4075 R(sigma) = 0.4909 Friedel opposites merged Maximum memory for data reduction = 4343 / 61142 Special position constraints for N8 x = 0.5000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 5834 / 745605 wR2 = 0.1634 before cycle 1 for 5946 data and 555 / 555 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.03473 0.00007 0.025 OSF Mean shift/esd = 0.000 Maximum = 0.025 for OSF Max. shift = 0.000 A for C20 Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5834 / 745605 wR2 = 0.1634 before cycle 2 for 5946 data and 555 / 555 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.03473 0.00007 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x O9 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5834 / 745605 wR2 = 0.1634 before cycle 3 for 5946 data and 555 / 555 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.03473 0.00007 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 C6 Max. shift = 0.000 A for C34 Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5834 / 745605 wR2 = 0.1634 before cycle 4 for 5946 data and 555 / 555 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.03473 0.00007 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C31 Max. dU = 0.000 for C21 Largest correlation matrix elements 0.505 y O2 / y N1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 0.6011 0.4040 0.2856 43 0.880 0.000 N7 C37 C36 H8 0.5000 0.6204 0.2500 43 0.880 0.000 N8 C38_$1 C38 H2 -0.2340 0.8923 0.4736 43 0.950 0.000 C2 C1 C3 H3 -0.1775 1.0150 0.4617 43 0.950 0.000 C3 C2 C4 H5 -0.1013 0.7489 0.4270 43 0.950 0.000 C5 C6 C4 H6 -0.1587 0.6286 0.4351 43 0.950 0.000 C6 C5 C1 H14 0.1566 1.0245 0.3780 43 0.950 0.000 C14 C15 C13 H15 0.2278 1.0468 0.3642 43 0.950 0.000 C15 C16 C14 H17 0.2135 1.3853 0.3637 43 0.950 0.000 C17 C18 C16 H18 0.1423 1.3629 0.3767 43 0.950 0.000 C18 C17 C13 H20 0.0360 1.3307 0.5131 43 0.950 0.000 C20 C21 C19 H21 0.0610 1.5140 0.5097 43 0.950 0.000 C21 C22 C20 H22 0.0590 1.6148 0.4093 43 0.950 0.000 C22 C23 C21 H23 0.0312 1.5343 0.3131 43 0.950 0.000 C23 C22 C24 H24 0.0064 1.3489 0.3159 43 0.950 0.000 C24 C19 C23 H26 -0.0745 1.3140 0.3525 43 0.950 0.000 C26 C27 C25 H27 -0.1347 1.4139 0.3746 43 0.950 0.000 C27 C28 C26 H28 -0.1702 1.3922 0.4752 43 0.950 0.000 C28 C27 C29 H29 -0.1450 1.2645 0.5562 43 0.950 0.000 C29 C28 C30 H30 -0.0842 1.1634 0.5334 43 0.950 0.000 C30 C25 C29 H31 0.6678 0.3419 0.2755 43 0.950 0.000 C31 C32 C36 H32 0.7383 0.3787 0.2850 43 0.950 0.000 C32 C31 C33 H34 0.7130 0.7095 0.3161 43 0.950 0.000 C34 C35 C33 H35 0.6422 0.6712 0.3052 43 0.950 0.000 C35 C34 C36 H41 0.5847 0.3051 0.1764 43 0.950 0.000 C41 C42 C40 H42 0.6313 0.1571 0.1884 43 0.950 0.000 C42 C41 C43 H43 0.6220 0.0254 0.2765 43 0.950 0.000 C43 C44 C42 H44 0.5654 0.0441 0.3474 43 0.950 0.000 C44 C43 C45 H45 0.5209 0.1954 0.3393 43 0.950 0.000 C45 C44 C40 H2A -0.1081 1.0411 0.4461 43 0.880 0.000 N2 C7 C4 H3A 0.0167 0.9479 0.4089 43 0.880 0.000 N3 C8 C11 H4 0.0873 1.2498 0.3954 43 0.880 0.000 N4 C12 C13 s93 in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C37 0.57368 0.54258 0.26528 1.00000 0.03203 0.02894 0.01374 -0.00391 0.00181 0.00161 0.02490 0.01510 0.00029 0.00076 0.00038 0.00000 0.00704 0.00627 0.00537 0.00521 0.00506 0.00637 0.00238 C38 0.53420 0.47990 0.25575 1.00000 0.01729 0.03371 0.02623 0.00891 0.00393 0.01414 0.02574 0.01556 0.00026 0.00073 0.00037 0.00000 0.00567 0.00630 0.00580 0.00516 0.00493 0.00515 0.00232 C39 0.52191 0.36697 0.25316 1.00000 0.01886 0.02436 0.02382 0.00312 -0.00182 -0.00563 0.02235 0.01220 0.00020 0.00068 0.00038 0.00000 0.00540 0.00497 0.00499 0.00493 0.00534 0.00437 0.00221 N6 0.77584 0.57107 0.30175 1.00000 0.03270 0.03615 0.05225 0.01325 0.00909 -0.00841 0.04037 0.01407 0.00025 0.00070 0.00037 0.00000 0.00678 0.00610 0.00546 0.00531 0.00478 0.00527 0.00231 N7 0.60692 0.47567 0.28009 1.00000 0.02128 0.01855 0.04319 0.00833 -0.00691 -0.00270 0.02767 0.01072 0.00021 0.00053 0.00029 0.00000 0.00483 0.00461 0.00492 0.00379 0.00406 0.00413 0.00192 H7 0.60105 0.40402 0.28557 1.00000 0.03321 0.00000 0.00000 N8 0.50000 0.54646 0.25000 0.50000 0.02720 0.02341 0.02602 0.00000 0.00229 0.00000 0.02555 0.00885 0.00000 0.00074 0.00000 0.00000 0.00717 0.00654 0.00614 0.00000 0.00580 0.00000 0.00261 H8 0.50000 0.62042 0.25000 0.50000 0.03066 0.00000 0.00000 O7 0.79986 0.48929 0.30220 1.00000 0.03259 0.04019 0.08397 0.00602 -0.00989 0.00801 0.05225 0.00996 0.00018 0.00051 0.00031 0.00000 0.00456 0.00437 0.00489 0.00396 0.00396 0.00375 0.00193 O8 0.78747 0.66877 0.30378 1.00000 0.04568 0.03182 0.05800 0.00525 -0.00723 -0.01047 0.04516 0.00972 0.00017 0.00049 0.00027 0.00000 0.00472 0.00406 0.00418 0.00379 0.00355 0.00399 0.00182 O9 0.57511 0.64462 0.26213 1.00000 0.03481 0.02163 0.04207 -0.00068 -0.00551 -0.00588 0.03284 0.00882 0.00016 0.00046 0.00025 0.00000 0.00406 0.00361 0.00387 0.00340 0.00304 0.00346 0.00162 C1 -0.20080 0.75117 0.45660 1.00000 0.02057 0.03056 0.04215 0.00389 -0.01233 -0.01194 0.03110 0.01443 0.00029 0.00076 0.00041 0.00000 0.00645 0.00672 0.00628 0.00541 0.00555 0.00596 0.00242 C2 -0.20716 0.86392 0.46406 1.00000 0.02485 0.04121 0.02492 0.00183 0.00725 0.00054 0.03033 0.01462 0.00026 0.00075 0.00036 0.00000 0.00641 0.00651 0.00532 0.00533 0.00503 0.00566 0.00235 H2 -0.23403 0.89234 0.47359 1.00000 0.03639 0.00000 0.00000 C3 -0.17376 0.93616 0.45751 1.00000 0.02901 0.03378 0.02987 0.01074 0.00623 0.00200 0.03089 0.01447 0.00028 0.00069 0.00036 0.00000 0.00665 0.00642 0.00573 0.00496 0.00533 0.00548 0.00245 H3 -0.17754 1.01504 0.46167 1.00000 0.03706 0.00000 0.00000 C4 -0.13463 0.89206 0.44477 1.00000 0.02300 0.02755 0.02565 0.01487 -0.00195 -0.00103 0.02540 0.01474 0.00028 0.00073 0.00038 0.00000 0.00655 0.00664 0.00558 0.00503 0.00486 0.00576 0.00233 C5 -0.12817 0.77779 0.43625 1.00000 0.03749 0.01546 0.04309 0.00823 0.00025 0.00302 0.03201 0.01431 0.00027 0.00066 0.00037 0.00000 0.00686 0.00573 0.00599 0.00498 0.00521 0.00554 0.00244 H5 -0.10134 0.74889 0.42702 1.00000 0.03841 0.00000 0.00000 C6 -0.16201 0.70722 0.44162 1.00000 0.04442 0.03081 0.04377 -0.00325 -0.00524 -0.00901 0.03967 0.01436 0.00031 0.00071 0.00038 0.00000 0.00733 0.00644 0.00613 0.00543 0.00589 0.00626 0.00259 H6 -0.15874 0.62863 0.43507 1.00000 0.04760 0.00000 0.00000 C7 -0.06051 0.94728 0.43172 1.00000 0.03410 0.04537 0.01073 -0.00831 0.00110 0.00217 0.03007 0.01533 0.00031 0.00083 0.00039 0.00000 0.00752 0.00735 0.00543 0.00547 0.00508 0.00628 0.00262 C8 -0.03242 1.04498 0.42610 1.00000 0.02235 0.02173 0.03953 -0.00610 0.00364 -0.00407 0.02787 0.01475 0.00029 0.00074 0.00040 0.00000 0.00646 0.00624 0.00653 0.00522 0.00520 0.00560 0.00244 C9 -0.03505 1.16091 0.42871 1.00000 0.03608 0.02422 0.00807 -0.01203 -0.00395 -0.00437 0.02279 0.01332 0.00029 0.00071 0.00035 0.00000 0.00688 0.00592 0.00499 0.00450 0.00473 0.00559 0.00223 C10 0.00518 1.20259 0.41571 1.00000 0.02679 0.01485 0.01821 -0.00129 0.00671 -0.00431 0.01995 0.01319 0.00026 0.00065 0.00035 0.00000 0.00623 0.00543 0.00514 0.00454 0.00466 0.00522 0.00218 C11 0.03089 1.11155 0.40691 1.00000 0.01939 0.01568 0.02834 -0.00029 0.00731 -0.00321 0.02113 0.01392 0.00027 0.00070 0.00037 0.00000 0.00586 0.00536 0.00534 0.00487 0.00464 0.00548 0.00217 C12 0.07556 1.09027 0.39309 1.00000 0.02567 0.02565 0.01314 -0.00388 0.00390 -0.00163 0.02148 0.01434 0.00027 0.00076 0.00036 0.00000 0.00652 0.00591 0.00511 0.00503 0.00468 0.00590 0.00222 C13 0.14289 1.19082 0.37856 1.00000 0.02184 0.05553 0.02048 0.00549 -0.00606 -0.01917 0.03262 0.01454 0.00029 0.00086 0.00038 0.00000 0.00635 0.00748 0.00542 0.00534 0.00505 0.00639 0.00255 C14 0.16819 1.09770 0.37518 1.00000 0.01674 0.04195 0.03755 -0.00450 -0.00362 0.00807 0.03208 0.01421 0.00027 0.00074 0.00037 0.00000 0.00612 0.00674 0.00596 0.00526 0.00518 0.00568 0.00246 H14 0.15656 1.02450 0.37797 1.00000 0.03850 0.00000 0.00000 C15 0.21024 1.11068 0.36778 1.00000 0.02320 0.05245 0.03419 -0.00491 -0.00922 -0.00041 0.03661 0.01440 0.00027 0.00077 0.00037 0.00000 0.00673 0.00723 0.00584 0.00568 0.00530 0.00595 0.00252 H15 0.22778 1.04684 0.36417 1.00000 0.04394 0.00000 0.00000 C16 0.22653 1.21698 0.36568 1.00000 0.01075 0.05480 0.04049 0.00194 -0.00141 -0.01486 0.03535 0.01523 0.00028 0.00087 0.00042 0.00000 0.00640 0.00741 0.00630 0.00636 0.00510 0.00627 0.00258 C17 0.20170 1.31240 0.36738 1.00000 0.04988 0.03796 0.02419 -0.00192 0.01160 -0.01627 0.03734 0.01440 0.00030 0.00075 0.00037 0.00000 0.00741 0.00648 0.00540 0.00524 0.00574 0.00661 0.00253 H17 0.21352 1.38526 0.36368 1.00000 0.04481 0.00000 0.00000 C18 0.15985 1.29892 0.37449 1.00000 0.01312 0.02501 0.05957 0.00507 0.00067 -0.00035 0.03256 0.01410 0.00026 0.00071 0.00038 0.00000 0.00598 0.00614 0.00666 0.00529 0.00540 0.00528 0.00244 H18 0.14230 1.36289 0.37666 1.00000 0.03907 0.00000 0.00000 C19 0.01894 1.32266 0.41450 1.00000 0.01910 0.02256 0.02834 0.00605 0.00850 -0.00197 0.02333 0.01474 0.00023 0.00065 0.00045 0.00000 0.00586 0.00559 0.00579 0.00568 0.00476 0.00456 0.00220 C20 0.03511 1.37189 0.47218 1.00000 0.03980 0.03674 0.02478 -0.00506 0.00139 0.00243 0.03377 0.01566 0.00024 0.00071 0.00042 0.00000 0.00655 0.00660 0.00588 0.00540 0.00501 0.00537 0.00243 H20 0.03597 1.33065 0.51314 1.00000 0.04053 0.00000 0.00000 C21 0.04994 1.48045 0.47016 1.00000 0.04935 0.02553 0.04739 -0.00108 -0.01844 -0.02288 0.04076 0.01394 0.00025 0.00071 0.00048 0.00000 0.00723 0.00628 0.00730 0.00576 0.00550 0.00545 0.00268 H21 0.06104 1.51401 0.50966 1.00000 0.04891 0.00000 0.00000 C22 0.04861 1.54017 0.41081 1.00000 0.03585 0.02740 0.05817 0.00645 0.00263 -0.01404 0.04047 0.01605 0.00025 0.00071 0.00052 0.00000 0.00686 0.00591 0.00712 0.00663 0.00603 0.00510 0.00261 H22 0.05902 1.61481 0.40935 1.00000 0.04857 0.00000 0.00000 C23 0.03234 1.49242 0.35379 1.00000 0.04141 0.03584 0.01956 0.00770 -0.00094 0.00265 0.03227 0.01619 0.00025 0.00070 0.00042 0.00000 0.00670 0.00646 0.00599 0.00531 0.00513 0.00561 0.00243 H23 0.03118 1.53431 0.31309 1.00000 0.03872 0.00000 0.00000 C24 0.01746 1.38235 0.35549 1.00000 0.04410 0.00965 0.02843 0.00432 0.00049 -0.00768 0.02739 0.01353 0.00023 0.00065 0.00041 0.00000 0.00656 0.00516 0.00606 0.00488 0.00478 0.00485 0.00231 H24 0.00637 1.34894 0.31594 1.00000 0.03287 0.00000 0.00000 C25 -0.07283 1.22830 0.44206 1.00000 0.01584 0.02516 0.03010 -0.00255 0.00900 -0.00476 0.02370 0.01274 0.00025 0.00068 0.00045 0.00000 0.00589 0.00590 0.00575 0.00515 0.00530 0.00488 0.00222 C26 -0.08850 1.30364 0.39415 1.00000 0.02578 0.04037 0.03051 -0.00144 0.00702 -0.00766 0.03222 0.01240 0.00027 0.00072 0.00041 0.00000 0.00645 0.00660 0.00594 0.00558 0.00521 0.00531 0.00246 H26 -0.07446 1.31399 0.35254 1.00000 0.03866 0.00000 0.00000 C27 -0.12446 1.36295 0.40751 1.00000 0.04288 0.03094 0.03007 0.00558 -0.00271 -0.00958 0.03463 0.01270 0.00030 0.00067 0.00044 0.00000 0.00720 0.00610 0.00627 0.00527 0.00555 0.00570 0.00247 H27 -0.13472 1.41386 0.37464 1.00000 0.04156 0.00000 0.00000 C28 -0.14567 1.35027 0.46686 1.00000 0.02935 0.03093 0.05237 -0.00710 0.00215 -0.00568 0.03755 0.01284 0.00025 0.00071 0.00049 0.00000 0.00653 0.00632 0.00667 0.00592 0.00613 0.00504 0.00252 H28 -0.17019 1.39217 0.47517 1.00000 0.04506 0.00000 0.00000 C29 -0.13072 1.27508 0.51474 1.00000 0.03878 0.03693 0.03960 -0.00299 0.01956 -0.00059 0.03843 0.01319 0.00028 0.00071 0.00042 0.00000 0.00710 0.00646 0.00606 0.00551 0.00551 0.00559 0.00255 H29 -0.14495 1.26455 0.55616 1.00000 0.04612 0.00000 0.00000 C30 -0.09426 1.21501 0.50084 1.00000 0.02967 0.01651 0.04079 -0.00098 -0.00308 -0.00190 0.02899 0.01234 0.00026 0.00063 0.00044 0.00000 0.00651 0.00564 0.00618 0.00496 0.00524 0.00509 0.00233 H30 -0.08417 1.16336 0.53344 1.00000 0.03479 0.00000 0.00000 C31 0.67715 0.41654 0.28289 1.00000 0.04899 0.01423 0.03340 -0.00130 -0.01425 0.00301 0.03221 0.01454 0.00031 0.00069 0.00037 0.00000 0.00739 0.00590 0.00565 0.00470 0.00551 0.00580 0.00250 H31 0.66778 0.34185 0.27554 1.00000 0.03865 0.00000 0.00000 C32 0.71864 0.43788 0.28848 1.00000 0.02542 0.03068 0.03534 -0.00172 0.00186 -0.00302 0.03048 0.01506 0.00028 0.00072 0.00037 0.00000 0.00652 0.00667 0.00603 0.00501 0.00502 0.00534 0.00251 H32 0.73830 0.37874 0.28502 1.00000 0.03658 0.00000 0.00000 C33 0.73128 0.54686 0.29921 1.00000 0.01940 0.03195 0.03191 0.00617 -0.00290 -0.01697 0.02775 0.01497 0.00029 0.00078 0.00039 0.00000 0.00625 0.00652 0.00579 0.00539 0.00513 0.00555 0.00242 C34 0.70356 0.63549 0.30690 1.00000 0.01486 0.02298 0.05120 -0.00611 -0.00758 -0.00396 0.02968 0.01345 0.00026 0.00068 0.00037 0.00000 0.00590 0.00573 0.00592 0.00492 0.00538 0.00520 0.00231 H34 0.71304 0.70949 0.31613 1.00000 0.03562 0.00000 0.00000 C35 0.66198 0.61249 0.30070 1.00000 0.01523 0.02655 0.03786 -0.00154 0.00183 -0.00661 0.02655 0.01402 0.00025 0.00070 0.00035 0.00000 0.00580 0.00612 0.00546 0.00490 0.00490 0.00512 0.00223 H35 0.64225 0.67124 0.30516 1.00000 0.03186 0.00000 0.00000 C36 0.64882 0.50319 0.28789 1.00000 0.02154 0.03716 0.01788 -0.00121 -0.00851 -0.01680 0.02553 0.01426 0.00027 0.00082 0.00037 0.00000 0.00618 0.00663 0.00540 0.00495 0.00469 0.00590 0.00237 C40 0.54886 0.26828 0.25768 1.00000 0.01694 0.02345 0.02903 -0.01315 -0.00592 0.01279 0.02314 0.01213 0.00025 0.00069 0.00042 0.00000 0.00595 0.00584 0.00575 0.00525 0.00490 0.00483 0.00222 C41 0.58135 0.25340 0.21243 1.00000 0.03151 0.02696 0.03113 -0.00284 0.00184 0.00856 0.02986 0.01222 0.00025 0.00068 0.00039 0.00000 0.00622 0.00609 0.00580 0.00483 0.00502 0.00518 0.00238 H41 0.58474 0.30513 0.17638 1.00000 0.03584 0.00000 0.00000 C42 0.60882 0.16473 0.21892 1.00000 0.02889 0.03214 0.05563 -0.01718 0.00603 0.00614 0.03889 0.01266 0.00025 0.00076 0.00043 0.00000 0.00644 0.00617 0.00695 0.00586 0.00523 0.00560 0.00255 H42 0.63132 0.15713 0.18842 1.00000 0.04667 0.00000 0.00000 C43 0.60322 0.08610 0.27088 1.00000 0.02550 0.02306 0.06339 -0.00067 -0.00390 0.00240 0.03732 0.01308 0.00027 0.00071 0.00047 0.00000 0.00661 0.00621 0.00712 0.00586 0.00557 0.00526 0.00256 H43 0.62201 0.02535 0.27649 1.00000 0.04478 0.00000 0.00000 C44 0.57004 0.09890 0.31336 1.00000 0.02408 0.02289 0.04447 0.00170 -0.00540 0.00372 0.03048 0.01259 0.00027 0.00069 0.00041 0.00000 0.00610 0.00609 0.00610 0.00522 0.00549 0.00530 0.00233 H44 0.56545 0.04414 0.34738 1.00000 0.03658 0.00000 0.00000 C45 0.54320 0.18817 0.30841 1.00000 0.02177 0.04068 0.03229 0.00648 -0.00164 -0.00558 0.03158 0.01227 0.00025 0.00074 0.00040 0.00000 0.00628 0.00636 0.00598 0.00566 0.00502 0.00542 0.00235 H45 0.52089 0.19543 0.33933 1.00000 0.03790 0.00000 0.00000 N1 -0.23547 0.67253 0.46479 1.00000 0.03729 0.04327 0.03511 -0.01109 -0.00738 -0.00358 0.03856 0.01278 0.00025 0.00074 0.00035 0.00000 0.00613 0.00614 0.00486 0.00510 0.00482 0.00570 0.00220 N2 -0.10150 0.96976 0.44141 1.00000 0.03390 0.02101 0.03539 0.00001 0.00641 0.00371 0.03010 0.01128 0.00023 0.00052 0.00030 0.00000 0.00549 0.00463 0.00473 0.00380 0.00450 0.00444 0.00196 H2A -0.10814 1.04105 0.44615 1.00000 0.03612 0.00000 0.00000 N3 0.00737 1.01706 0.41297 1.00000 0.03311 0.02138 0.01640 -0.00244 0.00263 0.00231 0.02363 0.01090 0.00021 0.00053 0.00029 0.00000 0.00536 0.00466 0.00406 0.00355 0.00371 0.00439 0.00183 H3A 0.01671 0.94791 0.40892 1.00000 0.02835 0.00000 0.00000 N4 0.10009 1.18512 0.38977 1.00000 0.03626 0.01664 0.03210 -0.00642 -0.00323 -0.00406 0.02833 0.01095 0.00022 0.00054 0.00028 0.00000 0.00551 0.00463 0.00445 0.00369 0.00410 0.00437 0.00189 H4 0.08732 1.24979 0.39536 1.00000 0.03400 0.00000 0.00000 N5 0.27194 1.22995 0.36150 1.00000 0.03444 0.05733 0.02320 -0.00007 0.00449 -0.00792 0.03833 0.01355 0.00026 0.00075 0.00035 0.00000 0.00660 0.00666 0.00474 0.00557 0.00446 0.00561 0.00225 O1 -0.26994 0.71281 0.47720 1.00000 0.02328 0.04909 0.08217 0.00103 0.00629 -0.00078 0.05151 0.01008 0.00018 0.00049 0.00031 0.00000 0.00426 0.00463 0.00470 0.00392 0.00386 0.00382 0.00193 O2 -0.22935 0.57167 0.45626 1.00000 0.05669 0.02124 0.09118 0.00010 0.00713 -0.00810 0.05637 0.01045 0.00018 0.00050 0.00032 0.00000 0.00504 0.00386 0.00531 0.00420 0.00394 0.00376 0.00209 O3 -0.04643 0.85265 0.42677 1.00000 0.02566 0.03000 0.03939 -0.00374 0.00427 0.00112 0.03168 0.00894 0.00016 0.00046 0.00025 0.00000 0.00415 0.00383 0.00391 0.00335 0.00310 0.00331 0.00167 O4 0.08847 0.99537 0.38684 1.00000 0.03010 0.01819 0.04394 -0.00434 -0.00432 0.00333 0.03074 0.00867 0.00015 0.00045 0.00026 0.00000 0.00410 0.00372 0.00409 0.00327 0.00307 0.00327 0.00163 O5 0.29274 1.14302 0.35919 1.00000 0.03963 0.06554 0.06692 -0.00808 -0.00033 0.01647 0.05736 0.01058 0.00019 0.00054 0.00031 0.00000 0.00485 0.00503 0.00465 0.00438 0.00395 0.00423 0.00210 O6 0.28678 1.32547 0.36089 1.00000 0.04188 0.06113 0.06419 0.00796 -0.00018 -0.01246 0.05573 0.01090 0.00018 0.00055 0.00030 0.00000 0.00492 0.00486 0.00459 0.00432 0.00381 0.00417 0.00203 Final Structure Factor Calculation for s93 in Pbcn Total number of l.s. parameters = 555 Maximum vector length = 511 Memory required = 5279 / 22995 wR2 = 0.1634 before cycle 5 for 5946 data and 0 / 555 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0941 for 1689 Fo > 4sig(Fo) and 0.3726 for all 5946 data wR2 = 0.1634, GooF = S = 0.958, Restrained GooF = 0.958 for all data Occupancy sum of asymmetric unit = 61.50 for non-hydrogen and 31.50 for hydrogen atoms Principal mean square atomic displacements U 0.0327 0.0294 0.0126 C37 0.0465 0.0217 0.0091 C38 0.0300 0.0217 0.0153 C39 0.0603 0.0422 0.0186 N6 0.0478 0.0193 0.0159 N7 0.0290 0.0242 0.0234 N8 0.0862 0.0453 0.0252 O7 0.0641 0.0452 0.0261 O8 0.0453 0.0342 0.0191 O9 0.0516 0.0314 0.0103 C1 0.0415 0.0318 0.0176 C2 0.0447 0.0285 0.0194 C3 0.0417 0.0228 0.0117 C4 0.0455 0.0377 0.0129 C5 0.0507 0.0435 0.0248 C6 0.0475 0.0339 0.0087 C7 0.0425 0.0234 0.0177 C8 0.0375 0.0301 0.0008 C9 0.0316 0.0151 0.0131 C10 0.0326 0.0180 0.0127 C11 0.0292 0.0240 0.0112 C12 0.0655 0.0206 0.0118 C13 0.0473 0.0348 0.0142 C14 0.0538 0.0383 0.0177 C15 0.0596 0.0402 0.0062 C16 0.0641 0.0295 0.0184 C17 0.0603 0.0243 0.0131 C18 0.0350 0.0233 0.0118 C19 0.0413 0.0374 0.0227 C20 0.0730 0.0408 0.0085 C21 0.0595 0.0461 0.0159 C22 0.0427 0.0377 0.0164 C23 0.0457 0.0293 0.0071 C24 0.0362 0.0241 0.0107 C25 0.0449 0.0325 0.0192 C26 0.0496 0.0310 0.0234 C27 0.0551 0.0336 0.0240 C28 0.0590 0.0368 0.0195 C29 0.0416 0.0292 0.0162 C30 0.0577 0.0250 0.0140 C31 0.0366 0.0309 0.0240 C32 0.0468 0.0289 0.0075 C33 0.0536 0.0244 0.0110 C34 0.0384 0.0291 0.0121 C35 0.0483 0.0226 0.0057 C36 0.0455 0.0176 0.0063 C40 0.0381 0.0321 0.0194 C41 0.0649 0.0346 0.0172 C42 0.0638 0.0266 0.0215 C43 0.0458 0.0268 0.0188 C44 0.0456 0.0289 0.0202 C45 0.0512 0.0417 0.0228 N1 0.0414 0.0291 0.0198 N2 0.0338 0.0223 0.0148 N3 0.0380 0.0337 0.0133 N4 0.0599 0.0337 0.0214 N5 0.0829 0.0491 0.0226 O1 0.0926 0.0570 0.0194 O2 0.0416 0.0298 0.0237 O3 0.0461 0.0292 0.0169 O4 0.0784 0.0624 0.0313 O5 0.0732 0.0586 0.0353 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.007 0.010 0.014 0.019 0.024 0.031 0.040 0.057 1.000 Number in group 732. 524. 535. 595. 667. 559. 603. 567. 578. 586. GooF 0.903 0.880 0.928 0.937 0.885 0.968 1.052 1.042 1.019 0.964 K 9.401 4.213 2.192 1.109 0.903 0.957 0.912 0.920 0.967 1.007 Resolution(A) 0.84 0.89 0.94 0.98 1.04 1.10 1.18 1.31 1.49 1.87 inf Number in group 599. 602. 590. 591. 598. 589. 598. 594. 591. 594. GooF 0.858 0.878 0.890 0.950 0.976 0.979 0.972 0.999 1.046 1.019 K 1.252 1.012 0.904 1.032 0.971 0.999 0.976 0.956 1.044 1.001 R1 0.719 0.655 0.593 0.506 0.354 0.289 0.262 0.235 0.137 0.051 Recommended weighting scheme: WGHT 0.0278 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) 14 2 2 3852.95 2420.45 4.50 0.049 2.10 15 4 8 2296.13 947.96 4.22 0.031 1.43 2 10 10 -683.62 1736.97 3.87 0.042 1.02 0 6 2 1925.96 927.86 3.68 0.030 1.94 3 8 5 2218.59 1005.47 3.64 0.032 1.38 4 3 13 1320.84 467.56 3.48 0.022 1.40 29 6 8 3491.58 12.08 3.36 0.003 0.90 20 3 4 -358.75 738.57 3.35 0.027 1.43 22 7 9 2541.82 1.94 3.26 0.001 0.99 15 0 8 2369.76 929.45 3.25 0.030 1.63 21 0 16 3823.25 11.10 3.21 0.003 0.97 7 2 11 1599.28 899.95 3.20 0.030 1.62 23 1 1 981.49 2260.77 3.19 0.047 1.39 9 5 1 2355.10 1441.75 3.12 0.038 1.97 15 7 10 2313.01 545.86 3.09 0.023 1.11 3 0 12 119699.52 106758.89 3.08 0.326 1.63 11 6 3 1621.20 504.28 3.08 0.022 1.59 19 7 12 -312.05 1449.00 3.03 0.038 0.97 3 7 4 727.99 57.06 3.01 0.008 1.59 11 6 15 1861.29 3.23 3.00 0.002 1.03 29 7 1 2527.28 14.42 2.97 0.004 0.93 3 5 7 1376.22 485.02 2.96 0.022 1.80 13 3 3 20278.89 17618.94 2.95 0.133 2.01 13 3 9 -283.53 473.97 2.93 0.022 1.52 1 11 3 -210.87 1377.91 2.92 0.037 1.07 22 8 6 2783.02 603.47 2.91 0.025 1.00 20 1 9 -447.33 738.91 2.90 0.027 1.29 24 8 0 7847.85 3718.48 2.90 0.061 1.00 19 9 2 1768.04 4069.40 2.89 0.064 1.04 23 7 2 -701.59 1723.18 2.87 0.041 1.08 26 3 11 2120.17 24.43 2.85 0.005 0.99 10 5 1 2810.76 2125.61 2.83 0.046 1.91 6 4 15 1376.93 55.58 2.83 0.007 1.18 12 6 11 1768.98 3339.03 2.83 0.058 1.20 29 4 4 -357.62 1698.61 2.82 0.041 1.02 6 8 9 1343.95 58.61 2.81 0.008 1.20 0 0 12 44920.57 39359.24 2.79 0.198 1.65 5 5 8 676.98 43.42 2.78 0.007 1.66 28 6 5 2672.89 43.41 2.78 0.007 0.97 10 6 14 1648.61 68.26 2.77 0.008 1.09 24 2 14 -430.93 1822.94 2.77 0.043 0.96 15 1 1 2845.19 2192.64 2.77 0.047 2.11 7 3 20 3445.37 6.89 2.75 0.003 0.94 14 2 20 4103.42 14.15 2.73 0.004 0.90 1 8 9 -393.05 584.35 2.72 0.024 1.23 16 0 10 2057.04 733.15 2.71 0.027 1.41 1 2 1 6882.50 7624.68 2.71 0.087 5.61 2 10 11 1442.13 11.58 2.71 0.003 0.99 31 6 9 4065.30 117.05 2.70 0.011 0.85 7 1 17 1055.56 67.46 2.68 0.008 1.13 Bond lengths and angles C37 - Distance Angles O9 1.2165 (0.0081) N7 1.3684 (0.0088) 124.18 (0.88) C38 1.4889 (0.0103) 121.73 (0.86) 114.04 (0.76) C37 - O9 N7 C38 - Distance Angles N8 1.3635 (0.0078) C39 1.4019 (0.0093) 108.94 (0.80) C37 1.4889 (0.0103) 114.39 (0.76) 136.63 (0.75) C38 - N8 C39 C39 - Distance Angles C38 1.4019 (0.0093) C39_$1 1.4205 (0.0128) 106.56 (0.44) C40 1.4640 (0.0089) 126.75 (0.66) 126.67 (0.41) C39 - C38 C39_$1 N6 - Distance Angles O8 1.2223 (0.0073) O7 1.2443 (0.0077) 123.51 (0.83) C33 1.4681 (0.0093) 119.26 (0.82) 117.23 (0.77) N6 - O8 O7 N7 - Distance Angles C37 1.3684 (0.0087) C36 1.4002 (0.0082) 130.19 (0.77) N7 - C37 N8 - Distance Angles C38_$1 1.3635 (0.0078) C38 1.3635 (0.0079) 108.98 (1.03) N8 - C38_$1 O7 - Distance Angles N6 1.2443 (0.0077) O7 - O8 - Distance Angles N6 1.2223 (0.0073) O8 - O9 - Distance Angles C37 1.2165 (0.0081) O9 - C1 - Distance Angles C2 1.3652 (0.0093) C6 1.3894 (0.0094) 121.91 (0.87) N1 1.4678 (0.0095) 119.99 (0.90) 118.11 (0.87) C1 - C2 C6 C2 - Distance Angles C1 1.3652 (0.0093) C3 1.3851 (0.0091) 118.85 (0.83) C2 - C1 C3 - Distance Angles C2 1.3851 (0.0091) C4 1.3913 (0.0092) 119.34 (0.81) C3 - C2 C4 - Distance Angles C5 1.3858 (0.0089) C3 1.3913 (0.0092) 121.92 (0.84) N2 1.4152 (0.0085) 121.43 (0.80) 116.64 (0.78) C4 - C5 C3 C5 - Distance Angles C6 1.3820 (0.0090) C4 1.3858 (0.0089) 117.89 (0.82) C5 - C6 C6 - Distance Angles C5 1.3820 (0.0090) C1 1.3894 (0.0094) 120.03 (0.83) C6 - C5 C7 - Distance Angles O3 1.2183 (0.0087) N2 1.3638 (0.0091) 123.68 (0.91) C8 1.4785 (0.0103) 119.46 (0.89) 116.85 (0.86) C7 - O3 N2 C8 - Distance Angles N3 1.3522 (0.0084) C9 1.3830 (0.0095) 108.09 (0.79) C7 1.4785 (0.0103) 113.84 (0.80) 138.04 (0.93) C8 - N3 C9 C9 - Distance Angles C8 1.3830 (0.0095) C10 1.4142 (0.0094) 106.65 (0.79) C25 1.4834 (0.0095) 126.61 (0.85) 126.75 (0.75) C9 - C8 C10 C10 - Distance Angles C11 1.3756 (0.0093) C9 1.4142 (0.0093) 107.53 (0.72) C19 1.4962 (0.0093) 124.81 (0.80) 127.61 (0.75) C10 - C11 C9 C11 - Distance Angles N3 1.3619 (0.0080) C10 1.3756 (0.0093) 107.61 (0.74) C12 1.4897 (0.0096) 114.56 (0.76) 137.83 (0.86) C11 - N3 C10 C12 - Distance Angles O4 1.2100 (0.0079) N4 1.3804 (0.0087) 124.07 (0.83) C11 1.4897 (0.0096) 120.74 (0.82) 115.17 (0.78) C12 - O4 N4 C13 - Distance Angles C14 1.3782 (0.0100) C18 1.4003 (0.0098) 120.26 (0.85) N4 1.4012 (0.0087) 123.60 (0.86) 116.05 (0.89) C13 - C14 C18 C14 - Distance Angles C15 1.3743 (0.0093) C13 1.3782 (0.0100) 120.03 (0.89) C14 - C15 C15 - Distance Angles C16 1.3705 (0.0100) C14 1.3743 (0.0093) 119.09 (0.88) C15 - C16 C16 - Distance Angles C15 1.3705 (0.0100) C17 1.3903 (0.0100) 122.11 (0.85) N5 1.4763 (0.0097) 118.63 (0.93) 119.25 (0.92) C16 - C15 C17 C17 - Distance Angles C18 1.3679 (0.0092) C16 1.3903 (0.0101) 118.45 (0.85) C17 - C18 C18 - Distance Angles C17 1.3679 (0.0092) C13 1.4003 (0.0098) 120.00 (0.84) C18 - C17 C19 - Distance Angles C24 1.3704 (0.0092) C20 1.3879 (0.0091) 119.95 (0.73) C10 1.4962 (0.0093) 119.88 (0.80) 120.10 (0.79) C19 - C24 C20 C20 - Distance Angles C21 1.3781 (0.0090) C19 1.3879 (0.0091) 120.16 (0.81) C20 - C21 C21 - Distance Angles C22 1.3764 (0.0097) C20 1.3781 (0.0090) 119.86 (0.83) C21 - C22 C22 - Distance Angles C23 1.3710 (0.0093) C21 1.3764 (0.0097) 120.30 (0.80) C22 - C23 C23 - Distance Angles C22 1.3710 (0.0093) C24 1.3953 (0.0086) 120.06 (0.80) C23 - C22 C24 - Distance Angles C19 1.3704 (0.0092) C23 1.3953 (0.0086) 119.68 (0.77) C24 - C19 C25 - Distance Angles C30 1.3655 (0.0094) C26 1.4014 (0.0095) 118.09 (0.78) C9 1.4834 (0.0095) 120.44 (0.84) 121.42 (0.80) C25 - C30 C26 C26 - Distance Angles C27 1.3843 (0.0090) C25 1.4014 (0.0095) 119.92 (0.78) C26 - C27 C27 - Distance Angles C28 1.3708 (0.0093) C26 1.3843 (0.0090) 121.84 (0.84) C27 - C28 C28 - Distance Angles C27 1.3708 (0.0093) C29 1.3914 (0.0093) 118.97 (0.83) C28 - C27 C29 - Distance Angles C28 1.3914 (0.0093) C30 1.4046 (0.0092) 118.92 (0.78) C29 - C28 C30 - Distance Angles C25 1.3655 (0.0094) C29 1.4046 (0.0092) 122.25 (0.81) C30 - C25 C31 - Distance Angles C32 1.3679 (0.0092) C36 1.3819 (0.0096) 120.26 (0.81) C31 - C32 C32 - Distance Angles C31 1.3679 (0.0092) C33 1.3760 (0.0095) 118.55 (0.85) C32 - C31 C33 - Distance Angles C32 1.3760 (0.0095) C34 1.3917 (0.0096) 122.70 (0.85) N6 1.4681 (0.0093) 118.74 (0.89) 118.55 (0.82) C33 - C32 C34 C34 - Distance Angles C35 1.3754 (0.0086) C33 1.3917 (0.0096) 117.85 (0.80) C34 - C35 C35 - Distance Angles C34 1.3754 (0.0086) C36 1.3915 (0.0097) 120.03 (0.81) C35 - C34 C36 - Distance Angles C31 1.3819 (0.0096) C35 1.3915 (0.0097) 120.54 (0.81) N7 1.4002 (0.0082) 117.19 (0.85) 122.27 (0.86) C36 - C31 C35 C40 - Distance Angles C41 1.3923 (0.0087) C45 1.3986 (0.0093) 118.44 (0.77) C39 1.4640 (0.0089) 120.68 (0.83) 120.87 (0.79) C40 - C41 C45 C41 - Distance Angles C42 1.3843 (0.0091) C40 1.3923 (0.0086) 121.30 (0.81) C41 - C42 C42 - Distance Angles C41 1.3843 (0.0091) C43 1.4041 (0.0095) 119.59 (0.82) C42 - C41 C43 - Distance Angles C44 1.3719 (0.0094) C42 1.4041 (0.0095) 118.55 (0.82) C43 - C44 C44 - Distance Angles C43 1.3719 (0.0094) C45 1.3743 (0.0090) 122.30 (0.83) C44 - C43 C45 - Distance Angles C44 1.3743 (0.0090) C40 1.3986 (0.0093) 119.72 (0.80) C45 - C44 N1 - Distance Angles O2 1.2278 (0.0075) O1 1.2367 (0.0073) 123.43 (0.85) C1 1.4678 (0.0095) 119.02 (0.81) 117.47 (0.84) N1 - O2 O1 N2 - Distance Angles C7 1.3638 (0.0091) C4 1.4152 (0.0085) 127.72 (0.76) N2 - C7 N3 - Distance Angles C8 1.3522 (0.0084) C11 1.3619 (0.0080) 110.12 (0.72) N3 - C8 N4 - Distance Angles C12 1.3804 (0.0087) C13 1.4012 (0.0087) 127.80 (0.76) N4 - C12 N5 - Distance Angles O6 1.2335 (0.0076) O5 1.2340 (0.0077) 124.09 (0.87) C16 1.4763 (0.0097) 118.85 (0.88) 117.06 (0.85) N5 - O6 O5 O1 - Distance Angles N1 1.2367 (0.0074) O1 - O2 - Distance Angles N1 1.2278 (0.0075) O2 - O3 - Distance Angles C7 1.2183 (0.0087) O3 - O4 - Distance Angles C12 1.2100 (0.0079) O4 - O5 - Distance Angles N5 1.2340 (0.0077) O5 - O6 - Distance Angles N5 1.2335 (0.0076) O6 - FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 24 -2 1.316 1 2 R1 = 0.3725 for 5946 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.2992 0.6402 0.0304 [ 1.29 A from O1 ] Deepest hole -0.32 at 0.3672 0.1223 0.1967 [ 1.23 A from C43 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 5494 / 45581 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2992 0.6402 0.4696 1.00000 0.05 0.30 1.29 O1 1.67 H3 2.10 N1 2.41 O2 Q2 1 -0.1292 1.0581 0.4263 1.00000 0.05 0.28 0.81 H2A 1.41 N2 1.79 H3 2.02 C4 Q3 1 -0.0443 0.8968 0.3567 1.00000 0.05 0.28 1.49 O3 1.69 C7 2.21 C39 2.26 C38 Q4 1 0.2100 1.4802 0.2916 1.00000 0.05 0.28 1.83 H17 1.89 O7 2.19 N6 2.36 O5 Q5 1 -0.1785 1.4652 0.3940 1.00000 0.05 0.27 1.59 H27 1.85 H28 1.97 O7 2.14 C27 Q6 1 0.0010 1.2253 0.4598 1.00000 0.05 0.27 0.93 C10 1.52 C9 1.58 C19 1.97 C11 Q7 1 0.1220 1.1555 0.4644 1.00000 0.05 0.26 1.68 N4 1.88 C13 1.93 C4 2.10 H4 Q8 1 -0.0024 0.7947 0.4647 1.00000 0.05 0.26 1.75 O3 1.90 H20 2.22 H3A 2.38 C10 Q9 1 -0.2096 0.4667 0.4469 1.00000 0.05 0.25 1.41 O2 1.65 H28 2.09 H2 2.52 C28 Q10 1 0.1582 0.9211 0.3795 1.00000 0.05 0.25 1.23 H14 2.13 C14 2.14 O6 2.42 O4 Q11 1 0.6556 0.3374 0.2350 1.00000 0.05 0.25 0.90 H31 1.51 C31 2.18 H7 2.25 C36 Q12 1 0.0435 1.3593 0.4072 1.00000 0.05 0.25 0.92 C19 1.33 C20 1.36 C24 1.92 C21 Q13 1 -0.1686 1.3575 0.3793 1.00000 0.05 0.25 1.29 H27 1.53 C27 1.89 C28 1.95 H28 Q14 1 0.6014 -0.0856 0.2778 1.00000 0.05 0.25 1.48 H43 2.05 C43 2.09 H26 2.20 H27 Q15 1 0.7422 0.2913 0.2546 1.00000 0.05 0.25 1.21 H32 2.00 O8 2.02 C32 2.13 H34 Q16 1 0.6079 0.3152 0.2638 1.00000 0.05 0.24 1.16 H7 1.52 C41 1.89 H41 1.94 N7 Q17 1 0.5704 0.3086 0.1544 1.00000 0.05 0.24 0.64 H41 1.37 C41 2.22 C40 2.44 O4 Q18 1 0.0607 1.2792 0.4707 1.00000 0.05 0.24 1.31 H20 1.38 C20 1.76 H4 1.82 C19 Q19 1 -0.1577 1.3725 0.3026 1.00000 0.05 0.24 1.68 H27 1.95 O7 2.21 H43 2.35 C27 Q20 1 0.5488 0.0225 0.3338 1.00000 0.05 0.24 0.66 H44 1.21 C44 2.04 C45 2.25 H45 Shortest distances between peaks (including symmetry equivalents) 5 13 1.35 5 9 1.45 6 8 1.52 13 19 1.57 11 16 1.66 12 18 1.67 14 19 1.95 6 18 2.04 5 19 2.23 9 13 2.29 6 12 2.35 14 20 2.40 8 18 2.44 7 18 2.47 10 11 2.48 16 17 2.49 1 2 2.65 3 8 2.81 4 19 2.83 11 15 2.87 4 15 2.88 3 16 2.92 Time profile in seconds ----------------------- 0.23: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 6.30: Read intensity data, sort/merge etc. 0.02: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.84: Structure factors and derivatives 11.94: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 2.00: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.14: Peaksearch 0.03: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 01sot191 finished at 15:18:06 Total CPU time: 28.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++