+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 12:40:21 on 19-Jan-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT005 in C2/c CELL 0.71073 16.1333 10.3709 37.6445 90.000 97.982 90.000 ZERR 8.00 0.0005 0.0003 0.0012 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O FE UNIT 320 280 24 16 16 V = 6237.54 F(000) = 2912.0 Mu = 0.97 mm-1 Cell Wt = 5611.28 Rho = 1.494 ACTA TEMP -153 SIZE 0.15 0.1 0.03 HTAB N2 O2_$1 EQIV $1 -x+1/2, -y+1/2, -z SHEL 7 0.84 HTAB FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.017500 FVAR 0.05977 C1 1 0.234168 0.448535 0.231835 11.00000 0.02918 0.03577 = 0.02189 -0.00717 0.00038 0.01646 AFIX 43 H1 2 0.183410 0.454932 0.215789 11.00000 -1.20000 AFIX 0 C2 1 0.250220 0.362598 0.260195 11.00000 0.03348 0.02510 = 0.03010 -0.00373 0.02098 -0.00052 AFIX 43 H2 2 0.212303 0.299945 0.266880 11.00000 -1.20000 AFIX 0 C3 1 0.331815 0.383907 0.277293 11.00000 0.04079 0.04981 = 0.01240 -0.00142 0.00546 0.02479 AFIX 43 H3 2 0.359213 0.338229 0.297452 11.00000 -1.20000 AFIX 0 C4 1 0.365558 0.484781 0.259241 11.00000 0.03292 0.05732 = 0.03724 -0.03478 0.01359 -0.01085 AFIX 43 H4 2 0.419959 0.520393 0.265221 11.00000 -1.20000 AFIX 0 C5 1 0.305760 0.524252 0.230954 11.00000 0.07783 0.01354 = 0.03841 -0.00073 0.03790 0.00528 AFIX 43 H5 2 0.312395 0.590476 0.214142 11.00000 -1.20000 AFIX 0 C6 1 0.394669 0.164359 0.221651 11.00000 0.02696 0.01955 = 0.01204 0.00251 0.00625 0.00623 AFIX 43 H6 2 0.415433 0.109722 0.241124 11.00000 -1.20000 AFIX 0 C7 1 0.314070 0.158157 0.201266 11.00000 0.02502 0.01072 = 0.02343 -0.00332 0.00583 -0.00619 AFIX 43 H7 2 0.271191 0.098360 0.204571 11.00000 -1.20000 AFIX 0 C8 1 0.308793 0.257076 0.175058 11.00000 0.01648 0.01581 = 0.01081 -0.00382 0.00069 0.00195 AFIX 43 H8 2 0.261526 0.274606 0.157716 11.00000 -1.20000 AFIX 0 C9 1 0.385959 0.325915 0.178972 11.00000 0.01977 0.01028 = 0.01061 -0.00313 0.00736 -0.00006 C10 1 0.439008 0.267253 0.207704 11.00000 0.01593 0.02187 = 0.01783 -0.00319 0.00574 0.00187 AFIX 43 H10 2 0.494850 0.292440 0.216226 11.00000 -1.20000 AFIX 0 C11 1 0.406458 0.439638 0.157271 11.00000 0.02191 0.01630 = 0.01400 -0.00481 0.00664 -0.00177 AFIX 23 H11A 2 0.354652 0.489707 0.149956 11.00000 -1.20000 H11B 2 0.446119 0.496079 0.172535 11.00000 -1.20000 AFIX 0 C12 1 0.394611 0.351528 0.096898 11.00000 0.01353 0.01193 = 0.01535 0.00380 0.00243 0.00480 C13 1 0.432268 0.322195 0.063981 11.00000 0.01357 0.01042 = 0.01138 0.00000 -0.00046 -0.00020 C14 1 0.511083 0.334796 0.053083 11.00000 0.01322 0.00527 = 0.01392 0.00164 0.00134 0.00009 C15 1 0.504479 0.282358 0.018018 11.00000 0.01567 0.00943 = 0.01119 0.00390 0.00176 0.00340 C16 1 0.422019 0.242831 0.008512 11.00000 0.01496 0.01136 = 0.01242 -0.00062 0.00518 0.00120 C17 1 0.373270 0.178195 -0.022781 11.00000 0.01784 0.00721 = 0.01583 0.00285 0.00199 0.00139 C18 1 0.365723 0.068204 -0.079544 11.00000 0.01679 0.02875 = 0.01328 -0.00337 0.00148 -0.00130 AFIX 23 H18A 2 0.320452 0.123550 -0.091723 11.00000 -1.20000 H18B 2 0.338981 -0.005988 -0.069093 11.00000 -1.20000 AFIX 0 C19 1 0.415812 0.018834 -0.106877 11.00000 0.01503 0.01194 = 0.01723 -0.00081 0.00447 -0.00043 C20 1 0.379861 -0.010511 -0.142397 11.00000 0.01262 0.01687 = 0.02072 -0.00133 0.00036 -0.00190 AFIX 43 H20 2 0.323570 0.005750 -0.152529 11.00000 -1.20000 AFIX 0 C21 1 0.442329 -0.068513 -0.160367 11.00000 0.02283 0.01622 = 0.01927 -0.00354 0.00308 -0.00065 AFIX 43 H21 2 0.435100 -0.097980 -0.184494 11.00000 -1.20000 AFIX 0 C22 1 0.516923 -0.074429 -0.135939 11.00000 0.01694 0.01619 = 0.02484 0.00004 0.00813 -0.00086 AFIX 43 H22 2 0.568848 -0.108217 -0.140882 11.00000 -1.20000 AFIX 0 C23 1 0.501365 -0.021445 -0.102756 11.00000 0.01462 0.01484 = 0.02129 0.00324 -0.00019 -0.00036 AFIX 43 H23 2 0.540710 -0.014057 -0.081604 11.00000 -1.20000 AFIX 0 C24 1 0.437208 0.283230 -0.164412 11.00000 0.02298 0.03734 = 0.16855 0.06195 0.02505 0.01489 AFIX 43 H24 2 0.380314 0.307247 -0.170961 11.00000 -1.20000 AFIX 0 C25 1 0.488010 0.224399 -0.186316 11.00000 0.07352 0.05523 = 0.02857 0.02044 -0.01022 -0.03736 AFIX 43 H25 2 0.471812 0.199703 -0.210589 11.00000 -1.20000 AFIX 0 C26 1 0.564990 0.207997 -0.167182 11.00000 0.03098 0.02853 = 0.05637 0.00691 0.02120 -0.00620 AFIX 43 H26 2 0.611706 0.170461 -0.176099 11.00000 -1.20000 AFIX 0 C27 1 0.565053 0.253506 -0.133288 11.00000 0.07894 0.03287 = 0.03973 0.02117 -0.02016 -0.03318 AFIX 43 H27 2 0.611210 0.253160 -0.114632 11.00000 -1.20000 AFIX 0 C28 1 0.484982 0.300831 -0.130877 11.00000 0.14170 0.01123 = 0.09620 -0.01012 0.10103 -0.00599 AFIX 43 H28 2 0.466482 0.338014 -0.110292 11.00000 -1.20000 AFIX 0 C29 1 0.587733 0.387788 0.074440 11.00000 0.00624 0.01288 = 0.01660 -0.00198 0.00329 -0.00017 C30 1 0.622965 0.502681 0.063958 11.00000 0.01396 0.01645 = 0.01954 -0.00095 0.00320 -0.00065 AFIX 43 H30 2 0.597563 0.546424 0.043071 11.00000 -1.20000 AFIX 0 C31 1 0.694570 0.553389 0.083733 11.00000 0.02527 0.01474 = 0.02794 -0.00124 0.00973 -0.00523 AFIX 43 H31 2 0.718231 0.630837 0.076154 11.00000 -1.20000 AFIX 0 C32 1 0.731564 0.491530 0.114427 11.00000 0.01343 0.03217 = 0.02650 -0.01193 0.00720 -0.00462 AFIX 43 H32 2 0.780217 0.526705 0.128119 11.00000 -1.20000 AFIX 0 C33 1 0.697383 0.378552 0.125014 11.00000 0.01633 0.03734 = 0.01392 0.00199 0.00032 0.00467 AFIX 43 H33 2 0.722785 0.335472 0.146013 11.00000 -1.20000 AFIX 0 C34 1 0.626111 0.327319 0.105201 11.00000 0.01598 0.01809 = 0.01765 -0.00135 0.00453 -0.00162 AFIX 43 H34 2 0.603203 0.249386 0.112858 11.00000 -1.20000 AFIX 0 C35 1 0.573064 0.267499 -0.004076 11.00000 0.00946 0.01680 = 0.01558 -0.00435 0.00075 -0.00066 C36 1 0.605470 0.371773 -0.021028 11.00000 0.01466 0.01549 = 0.01893 0.00250 0.00207 0.00332 AFIX 43 H36 2 0.582565 0.455337 -0.018875 11.00000 -1.20000 AFIX 0 C37 1 0.670692 0.355105 -0.040990 11.00000 0.01726 0.02414 = 0.01825 0.00532 0.00426 -0.00707 AFIX 43 H37 2 0.693182 0.427488 -0.051821 11.00000 -1.20000 AFIX 0 C38 1 0.703265 0.233086 -0.045216 11.00000 0.01202 0.03500 = 0.01610 -0.00169 0.00714 0.00190 AFIX 43 H38 2 0.746809 0.221487 -0.059509 11.00000 -1.20000 AFIX 0 C39 1 0.672289 0.129115 -0.028644 11.00000 0.01828 0.02614 = 0.02414 -0.00655 0.00212 0.00744 AFIX 43 H39 2 0.695257 0.045732 -0.031037 11.00000 -1.20000 AFIX 0 C40 1 0.607661 0.145860 -0.008476 11.00000 0.01421 0.02069 = 0.01939 0.00080 0.00120 -0.00385 AFIX 43 H40 2 0.586306 0.073128 0.002631 11.00000 -1.20000 AFIX 0 N1 3 0.443204 0.404630 0.125113 11.00000 0.01156 0.01706 = 0.01671 -0.00169 0.00702 -0.00342 AFIX 43 H1A 2 0.496724 0.418226 0.124240 11.00000 -1.20000 AFIX 0 N2 3 0.380024 0.269070 0.036641 11.00000 0.00439 0.01667 = 0.01876 0.00225 0.00399 -0.00209 AFIX 43 H2A 2 0.326505 0.253676 0.036998 11.00000 -1.20000 AFIX 0 N3 3 0.412692 0.142070 -0.050296 11.00000 0.01250 0.01811 = 0.01338 -0.00487 0.00202 -0.00284 AFIX 43 H3A 2 0.465509 0.162308 -0.050742 11.00000 -1.20000 AFIX 0 O1 4 0.320607 0.326600 0.097870 11.00000 0.00992 0.04542 = 0.01684 -0.00056 0.00392 0.00113 O2 4 0.298441 0.155011 -0.022383 11.00000 0.00991 0.02508 = 0.02065 -0.00647 0.00353 -0.00190 FE1 5 0.333434 0.336017 0.224944 11.00000 0.01983 0.01644 = 0.01429 -0.00169 0.00603 0.00034 FE2 5 0.478142 0.112097 -0.143026 11.00000 0.01826 0.01397 = 0.02099 0.00169 0.00584 0.00026 HKLF 4 Covalent radii and connectivity table for 01SOT005 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 C1 - C2 C5 Fe1 C2 - C1 C3 Fe1 C3 - C4 C2 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C7 C9 Fe1 C9 - C10 C8 C11 Fe1 C10 - C9 C6 Fe1 C11 - N1 C9 C12 - O1 N1 C13 C13 - N2 C14 C12 C14 - C13 C15 C29 C15 - C16 C14 C35 C16 - N2 C15 C17 C17 - O2 N3 C16 C18 - N3 C19 C19 - C20 C23 C18 Fe2 C20 - C19 C21 Fe2 C21 - C22 C20 Fe2 C22 - C21 C23 Fe2 C23 - C22 C19 Fe2 C24 - C25 C28 Fe2 C25 - C26 C24 Fe2 C26 - C25 C27 Fe2 C27 - C26 C28 Fe2 C28 - C27 C24 Fe2 C29 - C34 C30 C14 C30 - C31 C29 C31 - C32 C30 C32 - C33 C31 C33 - C32 C34 C34 - C29 C33 C35 - C36 C40 C15 C36 - C37 C35 C37 - C36 C38 C38 - C39 C37 C39 - C38 C40 C40 - C39 C35 N1 - C12 C11 N2 - C13 C16 N3 - C17 C18 O1 - C12 O2 - C17 Fe1 - C5 C1 C4 C9 C2 C10 C3 C8 C6 C7 Fe2 - C28 C24 C27 C25 C26 C20 C22 C21 C19 C23 Operators for generating equivalent atoms: $1 -x+1/2, -y+1/2, -z 13862 Reflections read, of which 2430 rejected -19 =< h =< 18, -10 =< k =< 12, -42 =< l =< 44, 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) 7 3 3 36.43 0.98 3 12.63 1 Inconsistent equivalents 5096 Unique reflections, of which 0 suppressed R(int) = 0.0706 R(sigma) = 0.1100 Friedel opposites merged Maximum memory for data reduction = 4130 / 62598 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 = 5328 / 548293 wR2 = 0.0938 before cycle 1 for 5096 data and 424 / 424 parameters GooF = S = 0.984; Restrained GooF = 0.984 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05977 0.00007 -0.067 OSF Mean shift/esd = 0.001 Maximum = -0.067 for OSF Max. shift = 0.000 A for C27 Max. dU = 0.000 for C31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5328 / 548293 wR2 = 0.0938 before cycle 2 for 5096 data and 424 / 424 parameters GooF = S = 0.984; Restrained GooF = 0.984 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05977 0.00007 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.006 for z Fe2 Max. shift = 0.000 A for C27 Max. dU = 0.000 for C31 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5328 / 548293 wR2 = 0.0938 before cycle 3 for 5096 data and 424 / 424 parameters GooF = S = 0.984; Restrained GooF = 0.984 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05977 0.00007 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5328 / 548293 wR2 = 0.0938 before cycle 4 for 5096 data and 424 / 424 parameters GooF = S = 0.984; Restrained GooF = 0.984 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05977 0.00007 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Fe2 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C28 Largest correlation matrix elements 0.670 U12 C28 / U23 C28 0.579 U13 C28 / U33 C28 0.536 x C28 / z C24 0.588 z C28 / x C28 0.579 U13 C28 / U11 C28 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1 0.1834 0.4549 0.2158 43 0.950 0.000 C1 C2 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.2123 0.2999 0.2669 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.3592 0.3382 0.2975 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.4200 0.5204 0.2652 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.3124 0.5905 0.2141 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.4154 0.1097 0.2411 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.2712 0.0984 0.2046 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.2615 0.2746 0.1577 43 0.950 0.000 C8 C7 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.4948 0.2924 0.2162 43 0.950 0.000 C10 C9 C6 H11A 0.3547 0.4897 0.1500 23 0.990 0.000 C11 N1 C9 H11B 0.4461 0.4961 0.1725 23 0.990 0.000 C11 N1 C9 H18A 0.3205 0.1236 -0.0917 23 0.990 0.000 C18 N3 C19 H18B 0.3390 -0.0060 -0.0691 23 0.990 0.000 C18 N3 C19 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C20 ** H20 0.3236 0.0057 -0.1525 43 0.950 0.000 C20 C19 C21 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C21 ** H21 0.4351 -0.0980 -0.1845 43 0.950 0.000 C21 C22 C20 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C22 ** H22 0.5688 -0.1082 -0.1409 43 0.950 0.000 C22 C21 C23 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C23 ** H23 0.5407 -0.0141 -0.0816 43 0.950 0.000 C23 C22 C19 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C24 ** H24 0.3803 0.3072 -0.1710 43 0.950 0.000 C24 C25 C28 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C25 ** H25 0.4718 0.1997 -0.2106 43 0.950 0.000 C25 C26 C24 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C26 ** H26 0.6117 0.1705 -0.1761 43 0.950 0.000 C26 C25 C27 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C27 ** H27 0.6112 0.2532 -0.1146 43 0.950 0.000 C27 C26 C28 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C28 ** H28 0.4665 0.3380 -0.1103 43 0.950 0.000 C28 C27 C24 H30 0.5976 0.5464 0.0431 43 0.950 0.000 C30 C31 C29 H31 0.7182 0.6308 0.0762 43 0.950 0.000 C31 C32 C30 H32 0.7802 0.5267 0.1281 43 0.950 0.000 C32 C33 C31 H33 0.7228 0.3355 0.1460 43 0.950 0.000 C33 C32 C34 H34 0.6032 0.2494 0.1129 43 0.950 0.000 C34 C29 C33 H36 0.5826 0.4553 -0.0189 43 0.950 0.000 C36 C37 C35 H37 0.6932 0.4275 -0.0518 43 0.950 0.000 C37 C36 C38 H38 0.7468 0.2215 -0.0595 43 0.950 0.000 C38 C39 C37 H39 0.6953 0.0457 -0.0310 43 0.950 0.000 C39 C38 C40 H40 0.5863 0.0731 0.0026 43 0.950 0.000 C40 C39 C35 H1A 0.4967 0.4182 0.1242 43 0.880 0.000 N1 C12 C11 H2A 0.3265 0.2537 0.0370 43 0.880 0.000 N2 C13 C16 H3A 0.4655 0.1623 -0.0507 43 0.880 0.000 N3 C17 C18 01SOT005 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.23417 0.44854 0.23184 1.00000 0.02917 0.03577 0.02189 -0.00717 0.00038 0.01646 0.02924 0.00750 0.00025 0.00040 0.00011 0.00000 0.00256 0.00277 0.00276 0.00223 0.00205 0.00235 0.00109 H1 0.18341 0.45493 0.21579 1.00000 0.03509 0.00000 0.00000 C2 0.25022 0.36260 0.26020 1.00000 0.03348 0.02510 0.03010 -0.00373 0.02098 -0.00052 0.02800 0.00740 0.00025 0.00038 0.00011 0.00000 0.00262 0.00260 0.00282 0.00215 0.00217 0.00217 0.00108 H2 0.21230 0.29994 0.26688 1.00000 0.03360 0.00000 0.00000 C3 0.33182 0.38391 0.27729 1.00000 0.04079 0.04981 0.01240 -0.00142 0.00546 0.02479 0.03417 0.00816 0.00027 0.00044 0.00011 0.00000 0.00285 0.00325 0.00250 0.00230 0.00213 0.00262 0.00118 H3 0.35921 0.33823 0.29745 1.00000 0.04100 0.00000 0.00000 C4 0.36556 0.48478 0.25924 1.00000 0.03292 0.05732 0.03724 -0.03478 0.01359 -0.01085 0.04167 0.00783 0.00027 0.00046 0.00013 0.00000 0.00284 0.00361 0.00328 0.00273 0.00246 0.00269 0.00134 H4 0.41996 0.52039 0.26522 1.00000 0.05000 0.00000 0.00000 C5 0.30576 0.52425 0.23095 1.00000 0.07783 0.01354 0.03841 -0.00073 0.03790 0.00528 0.04045 0.00903 0.00031 0.00039 0.00013 0.00000 0.00376 0.00249 0.00336 0.00223 0.00289 0.00266 0.00131 H5 0.31240 0.59048 0.21414 1.00000 0.04854 0.00000 0.00000 C6 0.39467 0.16436 0.22165 1.00000 0.02696 0.01955 0.01204 0.00251 0.00624 0.00623 0.01918 0.00670 0.00022 0.00036 0.00010 0.00000 0.00228 0.00227 0.00226 0.00183 0.00181 0.00203 0.00093 H6 0.41543 0.10972 0.24112 1.00000 0.02302 0.00000 0.00000 C7 0.31407 0.15816 0.20127 1.00000 0.02502 0.01072 0.02343 -0.00332 0.00583 -0.00619 0.01949 0.00660 0.00023 0.00035 0.00010 0.00000 0.00224 0.00215 0.00253 0.00186 0.00186 0.00192 0.00094 H7 0.27119 0.09836 0.20457 1.00000 0.02339 0.00000 0.00000 C8 0.30879 0.25708 0.17506 1.00000 0.01648 0.01581 0.01081 -0.00382 0.00069 0.00195 0.01448 0.00615 0.00021 0.00032 0.00009 0.00000 0.00204 0.00228 0.00221 0.00173 0.00166 0.00182 0.00089 H8 0.26153 0.27461 0.15772 1.00000 0.01738 0.00000 0.00000 C9 0.38596 0.32591 0.17897 1.00000 0.01977 0.01028 0.01061 -0.00313 0.00736 -0.00006 0.01306 0.00627 0.00021 0.00033 0.00009 0.00000 0.00210 0.00208 0.00218 0.00170 0.00167 0.00183 0.00085 C10 0.43901 0.26725 0.20770 1.00000 0.01593 0.02187 0.01783 -0.00319 0.00574 0.00187 0.01822 0.00669 0.00022 0.00034 0.00010 0.00000 0.00207 0.00233 0.00240 0.00189 0.00177 0.00193 0.00092 H10 0.49485 0.29244 0.21623 1.00000 0.02187 0.00000 0.00000 C11 0.40646 0.43964 0.15727 1.00000 0.02191 0.01630 0.01400 -0.00481 0.00664 -0.00177 0.01701 0.00651 0.00022 0.00035 0.00010 0.00000 0.00216 0.00215 0.00230 0.00181 0.00174 0.00187 0.00090 H11A 0.35465 0.48971 0.14996 1.00000 0.02041 0.00000 0.00000 H11B 0.44612 0.49608 0.17253 1.00000 0.02041 0.00000 0.00000 C12 0.39461 0.35153 0.09690 1.00000 0.01353 0.01193 0.01535 0.00380 0.00243 0.00480 0.01356 0.00675 0.00022 0.00034 0.00010 0.00000 0.00208 0.00215 0.00231 0.00173 0.00171 0.00175 0.00087 C13 0.43227 0.32220 0.06398 1.00000 0.01357 0.01042 0.01138 0.00000 -0.00046 -0.00020 0.01200 0.00632 0.00021 0.00033 0.00010 0.00000 0.00193 0.00212 0.00217 0.00165 0.00163 0.00175 0.00084 C14 0.51108 0.33480 0.05308 1.00000 0.01322 0.00527 0.01392 0.00164 0.00134 0.00009 0.01086 0.00620 0.00021 0.00032 0.00010 0.00000 0.00192 0.00193 0.00216 0.00166 0.00159 0.00173 0.00082 C15 0.50448 0.28236 0.01802 1.00000 0.01567 0.00943 0.01119 0.00390 0.00176 0.00340 0.01211 0.00638 0.00021 0.00033 0.00010 0.00000 0.00202 0.00201 0.00220 0.00170 0.00162 0.00174 0.00084 C16 0.42202 0.24283 0.00851 1.00000 0.01496 0.01136 0.01242 -0.00062 0.00518 0.00120 0.01260 0.00638 0.00021 0.00033 0.00010 0.00000 0.00197 0.00215 0.00218 0.00167 0.00166 0.00175 0.00085 C17 0.37327 0.17819 -0.02278 1.00000 0.01784 0.00721 0.01583 0.00285 0.00199 0.00139 0.01366 0.00654 0.00022 0.00033 0.00010 0.00000 0.00212 0.00210 0.00232 0.00172 0.00173 0.00180 0.00086 C18 0.36572 0.06820 -0.07954 1.00000 0.01679 0.02875 0.01328 -0.00337 0.00148 -0.00130 0.01966 0.00635 0.00021 0.00037 0.00010 0.00000 0.00209 0.00240 0.00230 0.00190 0.00171 0.00193 0.00093 H18A 0.32045 0.12355 -0.09172 1.00000 0.02360 0.00000 0.00000 H18B 0.33898 -0.00599 -0.06909 1.00000 0.02360 0.00000 0.00000 C19 0.41581 0.01883 -0.10688 1.00000 0.01503 0.01194 0.01723 -0.00081 0.00447 -0.00043 0.01453 0.00636 0.00021 0.00033 0.00010 0.00000 0.00205 0.00217 0.00238 0.00173 0.00172 0.00174 0.00089 C20 0.37986 -0.01051 -0.14240 1.00000 0.01262 0.01687 0.02072 -0.00133 0.00036 -0.00190 0.01692 0.00637 0.00022 0.00033 0.00010 0.00000 0.00200 0.00225 0.00249 0.00180 0.00176 0.00178 0.00092 H20 0.32357 0.00575 -0.15253 1.00000 0.02031 0.00000 0.00000 C21 0.44233 -0.06851 -0.16037 1.00000 0.02283 0.01622 0.01927 -0.00354 0.00308 -0.00065 0.01942 0.00666 0.00022 0.00035 0.00010 0.00000 0.00224 0.00224 0.00244 0.00187 0.00188 0.00192 0.00094 H21 0.43510 -0.09798 -0.18449 1.00000 0.02331 0.00000 0.00000 C22 0.51692 -0.07443 -0.13594 1.00000 0.01694 0.01619 0.02484 0.00004 0.00813 -0.00086 0.01883 0.00657 0.00022 0.00035 0.00010 0.00000 0.00211 0.00228 0.00256 0.00189 0.00185 0.00185 0.00094 H22 0.56885 -0.10822 -0.14088 1.00000 0.02260 0.00000 0.00000 C23 0.50136 -0.02145 -0.10276 1.00000 0.01462 0.01484 0.02129 0.00324 -0.00019 -0.00036 0.01717 0.00651 0.00021 0.00033 0.00010 0.00000 0.00208 0.00222 0.00252 0.00182 0.00176 0.00179 0.00093 H23 0.54071 -0.01406 -0.08160 1.00000 0.02061 0.00000 0.00000 C24 0.43721 0.28323 -0.16441 1.00000 0.02298 0.03734 0.16855 0.06195 0.02505 0.01489 0.07518 0.01390 0.00031 0.00053 0.00023 0.00000 0.00300 0.00365 0.00778 0.00449 0.00401 0.00276 0.00242 H24 0.38031 0.30725 -0.17096 1.00000 0.09022 0.00000 0.00000 C25 0.48801 0.22440 -0.18632 1.00000 0.07352 0.05523 0.02857 0.02044 -0.01021 -0.03736 0.05407 0.00873 0.00036 0.00050 0.00013 0.00000 0.00414 0.00373 0.00324 0.00273 0.00301 0.00337 0.00158 H25 0.47181 0.19970 -0.21059 1.00000 0.06488 0.00000 0.00000 C26 0.56499 0.20800 -0.16718 1.00000 0.03098 0.02853 0.05637 0.00691 0.02120 -0.00620 0.03720 0.00891 0.00028 0.00040 0.00014 0.00000 0.00275 0.00282 0.00377 0.00260 0.00260 0.00234 0.00122 H26 0.61171 0.17046 -0.17610 1.00000 0.04463 0.00000 0.00000 C27 0.56505 0.25351 -0.13329 1.00000 0.07895 0.03287 0.03973 0.02117 -0.02016 -0.03318 0.05320 0.00852 0.00035 0.00046 0.00014 0.00000 0.00415 0.00331 0.00365 0.00266 0.00316 0.00312 0.00160 H27 0.61121 0.25316 -0.11463 1.00000 0.06384 0.00000 0.00000 C28 0.48498 0.30083 -0.13088 1.00000 0.14170 0.01123 0.09620 -0.01012 0.10103 -0.00599 0.07507 0.01366 0.00050 0.00045 0.00019 0.00000 0.00646 0.00283 0.00569 0.00325 0.00505 0.00368 0.00231 H28 0.46648 0.33801 -0.11029 1.00000 0.09008 0.00000 0.00000 C29 0.58773 0.38779 0.07444 1.00000 0.00624 0.01288 0.01660 -0.00198 0.00329 -0.00017 0.01175 0.00612 0.00019 0.00033 0.00010 0.00000 0.00186 0.00207 0.00225 0.00177 0.00159 0.00173 0.00084 C30 0.62296 0.50268 0.06396 1.00000 0.01396 0.01645 0.01954 -0.00095 0.00320 -0.00065 0.01657 0.00636 0.00021 0.00033 0.00010 0.00000 0.00209 0.00228 0.00245 0.00182 0.00177 0.00186 0.00093 H30 0.59756 0.54642 0.04307 1.00000 0.01988 0.00000 0.00000 C31 0.69457 0.55339 0.08373 1.00000 0.02527 0.01474 0.02794 -0.00124 0.00973 -0.00523 0.02208 0.00686 0.00023 0.00037 0.00011 0.00000 0.00233 0.00224 0.00269 0.00202 0.00197 0.00204 0.00097 H31 0.71823 0.63084 0.07615 1.00000 0.02649 0.00000 0.00000 C32 0.73156 0.49153 0.11443 1.00000 0.01343 0.03217 0.02650 -0.01193 0.00720 -0.00462 0.02362 0.00712 0.00023 0.00038 0.00011 0.00000 0.00214 0.00275 0.00272 0.00214 0.00190 0.00204 0.00103 H32 0.78022 0.52670 0.12812 1.00000 0.02834 0.00000 0.00000 C33 0.69738 0.37855 0.12501 1.00000 0.01633 0.03734 0.01392 0.00199 0.00032 0.00467 0.02270 0.00689 0.00022 0.00039 0.00010 0.00000 0.00213 0.00278 0.00234 0.00205 0.00176 0.00213 0.00099 H33 0.72279 0.33547 0.14601 1.00000 0.02724 0.00000 0.00000 C34 0.62611 0.32732 0.10520 1.00000 0.01598 0.01809 0.01765 -0.00135 0.00453 -0.00162 0.01703 0.00643 0.00021 0.00036 0.00010 0.00000 0.00207 0.00228 0.00234 0.00185 0.00175 0.00188 0.00091 H34 0.60320 0.24939 0.11286 1.00000 0.02044 0.00000 0.00000 C35 0.57306 0.26750 -0.00408 1.00000 0.00946 0.01680 0.01558 -0.00435 0.00075 -0.00066 0.01404 0.00616 0.00020 0.00034 0.00010 0.00000 0.00192 0.00224 0.00227 0.00180 0.00163 0.00181 0.00088 C36 0.60547 0.37177 -0.02103 1.00000 0.01466 0.01549 0.01893 0.00250 0.00207 0.00332 0.01638 0.00626 0.00021 0.00035 0.00010 0.00000 0.00202 0.00226 0.00240 0.00179 0.00172 0.00177 0.00091 H36 0.58256 0.45534 -0.01887 1.00000 0.01966 0.00000 0.00000 C37 0.67069 0.35510 -0.04099 1.00000 0.01726 0.02414 0.01825 0.00532 0.00426 -0.00707 0.01971 0.00641 0.00021 0.00037 0.00010 0.00000 0.00212 0.00248 0.00243 0.00187 0.00177 0.00192 0.00096 H37 0.69318 0.42749 -0.05182 1.00000 0.02366 0.00000 0.00000 C38 0.70327 0.23309 -0.04522 1.00000 0.01202 0.03500 0.01610 -0.00169 0.00714 0.00190 0.02055 0.00659 0.00021 0.00038 0.00010 0.00000 0.00205 0.00266 0.00243 0.00203 0.00174 0.00201 0.00096 H38 0.74681 0.22149 -0.05951 1.00000 0.02466 0.00000 0.00000 C39 0.67229 0.12912 -0.02864 1.00000 0.01828 0.02614 0.02414 -0.00655 0.00212 0.00744 0.02293 0.00661 0.00022 0.00037 0.00010 0.00000 0.00218 0.00252 0.00258 0.00201 0.00186 0.00198 0.00100 H39 0.69526 0.04573 -0.03104 1.00000 0.02752 0.00000 0.00000 C40 0.60766 0.14586 -0.00848 1.00000 0.01421 0.02069 0.01939 0.00080 0.00120 -0.00385 0.01820 0.00625 0.00021 0.00036 0.00010 0.00000 0.00204 0.00239 0.00242 0.00184 0.00172 0.00183 0.00093 H40 0.58631 0.07313 0.00263 1.00000 0.02185 0.00000 0.00000 N1 0.44320 0.40463 0.12511 1.00000 0.01156 0.01706 0.01671 -0.00169 0.00702 -0.00342 0.01463 0.00514 0.00017 0.00027 0.00008 0.00000 0.00162 0.00189 0.00194 0.00147 0.00142 0.00146 0.00074 H1A 0.49672 0.41823 0.12424 1.00000 0.01756 0.00000 0.00000 N2 0.38002 0.26907 0.03664 1.00000 0.00439 0.01667 0.01876 0.00225 0.00399 -0.00209 0.01305 0.00502 0.00016 0.00026 0.00008 0.00000 0.00151 0.00179 0.00195 0.00149 0.00137 0.00142 0.00072 H2A 0.32651 0.25368 0.03700 1.00000 0.01566 0.00000 0.00000 N3 0.41269 0.14207 -0.05030 1.00000 0.01250 0.01811 0.01338 -0.00487 0.00202 -0.00284 0.01464 0.00502 0.00017 0.00026 0.00008 0.00000 0.00161 0.00182 0.00186 0.00143 0.00137 0.00144 0.00073 H3A 0.46551 0.16231 -0.05074 1.00000 0.01757 0.00000 0.00000 O1 0.32061 0.32660 0.09787 1.00000 0.00992 0.04542 0.01684 -0.00056 0.00392 0.00113 0.02387 0.00445 0.00014 0.00025 0.00007 0.00000 0.00138 0.00190 0.00165 0.00134 0.00116 0.00138 0.00067 O2 0.29844 0.15501 -0.02238 1.00000 0.00991 0.02508 0.02065 -0.00647 0.00353 -0.00190 0.01841 0.00417 0.00014 0.00024 0.00006 0.00000 0.00136 0.00158 0.00165 0.00122 0.00115 0.00126 0.00063 Fe1 0.33343 0.33602 0.22494 1.00000 0.01983 0.01644 0.01429 -0.00169 0.00603 0.00034 0.01651 0.00095 0.00003 0.00005 0.00001 0.00000 0.00031 0.00032 0.00033 0.00026 0.00024 0.00027 0.00016 Fe2 0.47814 0.11210 -0.14303 1.00000 0.01826 0.01397 0.02099 0.00169 0.00584 0.00026 0.01745 0.00097 0.00003 0.00005 0.00001 0.00000 0.00031 0.00032 0.00035 0.00026 0.00024 0.00027 0.00016 Final Structure Factor Calculation for 01SOT005 in C2/c Total number of l.s. parameters = 424 Maximum vector length = 511 Memory required = 4904 / 24017 wR2 = 0.0938 before cycle 5 for 5096 data and 0 / 424 parameters GooF = S = 0.984; Restrained GooF = 0.984 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0474 for 3383 Fo > 4sig(Fo) and 0.0929 for all 5096 data wR2 = 0.0938, GooF = S = 0.984, Restrained GooF = 0.984 for all data Occupancy sum of asymmetric unit = 47.00 for non-hydrogen and 35.00 for hydrogen atoms Principal mean square atomic displacements U 0.0525 0.0212 0.0140 C1 0.0468 0.0253 0.0120 C2 0.0708 0.0210 0.0107 C3 0.0853 0.0292 0.0105 C4 0.0905 0.0195 0.0113 C5 0.0310 0.0160 0.0106 C6 0.0289 0.0213 0.0083 C7 0.0200 0.0147 0.0087 C8 0.0216 0.0120 0.0055 C9 0.0237 0.0196 0.0115 C10 0.0246 0.0171 0.0093 C11 0.0193 0.0141 0.0073 C12 0.0153 0.0105 0.0102 C13 0.0145 0.0131 0.0050 C14 0.0174 0.0131 0.0058 C15 0.0169 0.0120 0.0089 C16 0.0180 0.0167 0.0063 C17 0.0295 0.0170 0.0125 C18 0.0185 0.0133 0.0118 C19 0.0216 0.0175 0.0116 C20 0.0229 0.0215 0.0139 C21 0.0268 0.0164 0.0133 C22 0.0239 0.0144 0.0133 C23 0.1933 0.0224 0.0098 C24 0.1156 0.0308 0.0158 C25 0.0621 0.0345 0.0150 C26 0.1189 0.0293 0.0114 C27 0.1967 0.0200 0.0085 C28 0.0175 0.0121 0.0057 C29 0.0199 0.0162 0.0136 C30 0.0329 0.0210 0.0123 C31 0.0423 0.0172 0.0113 C32 0.0384 0.0171 0.0126 C33 0.0205 0.0166 0.0140 C34 0.0207 0.0123 0.0092 C35 0.0204 0.0172 0.0115 C36 0.0303 0.0194 0.0094 C37 0.0353 0.0190 0.0074 C38 0.0351 0.0212 0.0124 C39 0.0232 0.0190 0.0124 C40 0.0214 0.0153 0.0072 N1 0.0202 0.0159 0.0031 N2 0.0216 0.0125 0.0099 N3 0.0455 0.0172 0.0090 O1 0.0298 0.0160 0.0094 O2 0.0212 0.0170 0.0113 Fe1 0.0229 0.0160 0.0134 Fe2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.025 0.039 0.051 0.066 0.083 0.104 0.132 0.177 1.000 Number in group 513. 508. 545. 489. 497. 528. 502. 491. 513. 510. GooF 0.809 0.883 0.935 1.018 0.947 1.090 1.089 0.976 1.015 1.041 K 3.009 1.017 0.948 1.003 1.007 1.019 1.014 1.004 1.006 1.012 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.16 1.28 1.45 1.83 inf Number in group 519. 514. 503. 508. 511. 510. 502. 508. 510. 511. GooF 0.914 0.906 0.878 0.969 0.936 0.914 0.922 0.961 1.103 1.270 K 1.034 1.038 1.027 1.010 1.015 1.019 1.012 1.011 1.004 1.004 R1 0.218 0.177 0.145 0.143 0.115 0.094 0.073 0.054 0.038 0.028 Recommended weighting scheme: WGHT 0.0165 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) -8 0 2 11940.80 14005.63 4.24 0.162 2.02 8 2 4 600.05 1246.65 3.93 0.048 1.78 -4 0 14 11425.38 13791.86 3.89 0.161 2.37 -5 3 13 2654.89 1882.06 3.84 0.059 1.91 -1 5 9 7402.24 6144.30 3.58 0.107 1.86 6 2 12 60.13 499.49 3.46 0.031 1.78 -4 2 6 2496.04 3006.25 3.43 0.075 2.95 10 4 26 3779.81 2372.66 3.39 0.067 0.93 8 0 6 8724.59 10410.78 3.38 0.140 1.83 -4 2 10 22345.02 19423.59 3.37 0.191 2.56 1 1 11 6857.85 7999.07 3.36 0.123 3.08 -7 3 6 450.39 923.52 3.33 0.042 1.88 9 1 26 4219.08 2323.73 3.31 0.066 1.04 -4 8 19 302.36 1143.41 3.30 0.046 1.06 -3 1 12 3137.09 2543.72 3.26 0.069 2.76 -1 3 13 3939.79 4524.05 3.26 0.092 2.22 -3 1 34 3551.73 1578.42 3.24 0.054 1.10 -1 5 23 1733.82 2345.94 3.17 0.066 1.28 8 0 4 753.11 115.95 3.16 0.015 1.90 10 0 0 28595.89 24114.49 3.15 0.213 1.60 -3 3 33 2715.66 4496.90 3.11 0.092 1.08 -5 3 3 2435.88 2899.96 3.11 0.074 2.35 -4 6 26 2903.08 4768.86 3.08 0.095 1.09 -10 4 6 747.51 142.88 3.03 0.016 1.36 3 5 0 5277.42 4535.28 3.03 0.092 1.93 -7 1 41 5953.13 3280.70 2.98 0.079 0.88 2 4 1 10336.16 9295.25 2.98 0.132 2.45 10 0 4 0.00 847.74 2.97 0.040 1.54 -1 3 12 3321.03 2707.14 2.97 0.071 2.32 -5 5 8 64369.98 58377.80 2.97 0.331 1.67 -15 1 19 4439.69 6471.28 2.96 0.110 0.99 9 5 20 1876.28 1025.26 2.95 0.044 1.04 -17 1 15 9181.01 6212.34 2.94 0.108 0.92 5 5 0 23945.69 20591.33 2.93 0.197 1.74 -4 8 5 499.89 1023.88 2.92 0.044 1.23 7 1 3 22136.93 20047.09 2.92 0.194 2.14 -12 2 35 19810.34 13988.96 2.91 0.162 0.88 2 6 33 4072.01 1737.67 2.91 0.057 0.93 -11 1 14 701.05 1221.63 2.90 0.048 1.35 14 0 16 3916.71 6402.37 2.90 0.110 0.97 -6 2 14 8093.39 7083.75 2.90 0.115 1.89 7 1 11 4495.24 5266.91 2.90 0.099 1.76 -2 6 6 32577.52 28982.73 2.87 0.233 1.64 -17 3 22 2343.95 3680.65 2.87 0.083 0.85 6 0 0 20608.36 22940.65 2.85 0.208 2.66 -1 9 17 2053.23 707.96 2.84 0.036 1.02 -10 10 9 6609.98 4094.53 2.83 0.088 0.86 -14 8 8 2262.58 352.18 2.83 0.026 0.86 0 2 19 7015.90 5835.39 2.81 0.105 1.84 3 5 24 1105.55 1905.08 2.81 0.060 1.18 Bond lengths and angles C1 - Distance Angles C2 1.3872 (0.0053) C5 1.4009 (0.0054) 108.18 (0.37) Fe1 2.0271 (0.0037) 70.26 (0.23) 69.57 (0.22) C1 - C2 C5 C2 - Distance Angles C1 1.3872 (0.0053) C3 1.4002 (0.0053) 108.39 (0.38) Fe1 2.0333 (0.0038) 69.78 (0.24) 69.98 (0.22) C2 - C1 C3 C3 - Distance Angles C4 1.3983 (0.0058) C2 1.4002 (0.0053) 107.41 (0.39) Fe1 2.0360 (0.0040) 69.75 (0.25) 69.77 (0.23) C3 - C4 C2 C4 - Distance Angles C5 1.3953 (0.0059) C3 1.3983 (0.0058) 108.41 (0.39) Fe1 2.0322 (0.0042) 69.49 (0.25) 70.04 (0.25) C4 - C5 C3 C5 - Distance Angles C4 1.3953 (0.0059) C1 1.4009 (0.0054) 107.60 (0.39) Fe1 2.0223 (0.0039) 70.26 (0.25) 69.95 (0.23) C5 - C4 C1 C6 - Distance Angles C7 1.4166 (0.0048) C10 1.4249 (0.0048) 107.73 (0.34) Fe1 2.0481 (0.0037) 70.00 (0.21) 69.05 (0.21) C6 - C7 C10 C7 - Distance Angles C6 1.4166 (0.0048) C8 1.4177 (0.0047) 107.82 (0.33) Fe1 2.0536 (0.0036) 69.59 (0.21) 69.08 (0.20) C7 - C6 C8 C8 - Distance Angles C7 1.4177 (0.0047) C9 1.4249 (0.0044) 108.87 (0.31) Fe1 2.0366 (0.0035) 70.37 (0.21) 69.35 (0.19) C8 - C7 C9 C9 - Distance Angles C10 1.4197 (0.0047) C8 1.4249 (0.0043) 106.84 (0.31) C11 1.4976 (0.0047) 126.70 (0.32) 126.45 (0.32) Fe1 2.0326 (0.0035) 69.63 (0.21) 69.65 (0.20) 125.00 (0.25) C9 - C10 C8 C11 C10 - Distance Angles C9 1.4197 (0.0047) C6 1.4249 (0.0048) 108.74 (0.31) Fe1 2.0342 (0.0035) 69.51 (0.20) 70.10 (0.20) C10 - C9 C6 C11 - Distance Angles N1 1.4656 (0.0041) C9 1.4976 (0.0047) 113.63 (0.29) C11 - N1 C12 - Distance Angles O1 1.2271 (0.0038) N1 1.3471 (0.0042) 121.65 (0.34) C13 1.4853 (0.0047) 119.61 (0.33) 118.74 (0.31) C12 - O1 N1 C13 - Distance Angles N2 1.3536 (0.0041) C14 1.3954 (0.0044) 108.13 (0.31) C12 1.4853 (0.0047) 115.72 (0.30) 136.14 (0.33) C13 - N2 C14 C14 - Distance Angles C13 1.3954 (0.0044) C15 1.4179 (0.0047) 106.50 (0.30) C29 1.4837 (0.0045) 126.89 (0.32) 126.56 (0.31) C14 - C13 C15 C15 - Distance Angles C16 1.3906 (0.0045) C14 1.4179 (0.0047) 107.35 (0.31) C35 1.4817 (0.0046) 125.96 (0.32) 126.66 (0.31) C15 - C16 C14 C16 - Distance Angles N2 1.3615 (0.0041) C15 1.3906 (0.0045) 107.61 (0.30) C17 1.4827 (0.0048) 116.23 (0.30) 136.11 (0.33) C16 - N2 C15 C17 - Distance Angles O2 1.2331 (0.0038) N3 1.3419 (0.0042) 121.65 (0.34) C16 1.4827 (0.0048) 119.39 (0.33) 118.92 (0.31) C17 - O2 N3 C18 - Distance Angles N3 1.4634 (0.0042) C19 1.4848 (0.0046) 115.28 (0.29) C18 - N3 C19 - Distance Angles C20 1.4148 (0.0047) C23 1.4298 (0.0044) 107.61 (0.32) C18 1.4848 (0.0046) 122.54 (0.32) 129.47 (0.34) Fe2 2.0442 (0.0036) 69.37 (0.21) 69.74 (0.20) 131.57 (0.26) C19 - C20 C23 C18 C20 - Distance Angles C19 1.4148 (0.0047) C21 1.4228 (0.0046) 108.41 (0.31) Fe2 2.0352 (0.0034) 70.05 (0.20) 69.77 (0.20) C20 - C19 C21 C21 - Distance Angles C22 1.4108 (0.0047) C20 1.4228 (0.0046) 107.75 (0.35) Fe2 2.0405 (0.0037) 69.72 (0.22) 69.37 (0.20) C21 - C22 C20 C22 - Distance Angles C21 1.4108 (0.0047) C23 1.4186 (0.0048) 108.54 (0.33) Fe2 2.0392 (0.0037) 69.82 (0.22) 70.07 (0.21) C22 - C21 C23 C23 - Distance Angles C22 1.4186 (0.0048) C19 1.4298 (0.0044) 107.69 (0.32) Fe2 2.0491 (0.0036) 69.32 (0.21) 69.37 (0.21) C23 - C22 C19 C24 - Distance Angles C25 1.3826 (0.0074) C28 1.3967 (0.0078) 107.36 (0.47) Fe2 2.0215 (0.0048) 70.25 (0.29) 69.27 (0.30) C24 - C25 C28 C25 - Distance Angles C26 1.3571 (0.0060) C24 1.3826 (0.0074) 108.26 (0.50) Fe2 2.0272 (0.0045) 70.70 (0.27) 69.81 (0.30) C25 - C26 C24 C26 - Distance Angles C25 1.3571 (0.0060) C27 1.3603 (0.0062) 109.62 (0.46) Fe2 2.0330 (0.0041) 70.24 (0.26) 70.18 (0.27) C26 - C25 C27 C27 - Distance Angles C26 1.3603 (0.0062) C28 1.3966 (0.0070) 107.62 (0.47) Fe2 2.0269 (0.0043) 70.67 (0.26) 69.09 (0.28) C27 - C26 C28 C28 - Distance Angles C27 1.3966 (0.0070) C24 1.3967 (0.0078) 107.14 (0.49) Fe2 2.0096 (0.0047) 70.43 (0.27) 70.19 (0.31) C28 - C27 C24 C29 - Distance Angles C34 1.3851 (0.0046) C30 1.4003 (0.0046) 117.97 (0.32) C14 1.4837 (0.0045) 121.84 (0.31) 120.19 (0.33) C29 - C34 C30 C30 - Distance Angles C31 1.3880 (0.0046) C29 1.4003 (0.0046) 120.76 (0.36) C30 - C31 C31 - Distance Angles C32 1.3825 (0.0050) C30 1.3880 (0.0046) 120.20 (0.36) C31 - C32 C32 - Distance Angles C33 1.3772 (0.0050) C31 1.3825 (0.0050) 119.53 (0.36) C32 - C33 C33 - Distance Angles C32 1.3772 (0.0050) C34 1.3866 (0.0046) 120.39 (0.38) C33 - C32 C34 - Distance Angles C29 1.3851 (0.0046) C33 1.3866 (0.0046) 121.15 (0.35) C34 - C29 C35 - Distance Angles C36 1.3938 (0.0047) C40 1.3986 (0.0046) 117.67 (0.34) C15 1.4817 (0.0046) 122.22 (0.33) 120.11 (0.33) C35 - C36 C40 C36 - Distance Angles C37 1.3861 (0.0045) C35 1.3938 (0.0047) 120.84 (0.35) C36 - C37 C37 - Distance Angles C36 1.3861 (0.0045) C38 1.3878 (0.0049) 120.26 (0.35) C37 - C36 C38 - Distance Angles C39 1.3741 (0.0050) C37 1.3878 (0.0049) 119.74 (0.35) C38 - C39 C39 - Distance Angles C38 1.3741 (0.0050) C40 1.3833 (0.0047) 120.00 (0.36) C39 - C38 C40 - Distance Angles C39 1.3833 (0.0047) C35 1.3986 (0.0046) 121.46 (0.36) C40 - C39 N1 - Distance Angles C12 1.3471 (0.0042) C11 1.4656 (0.0041) 119.65 (0.28) N1 - C12 N2 - Distance Angles C13 1.3536 (0.0041) C16 1.3615 (0.0041) 110.37 (0.28) N2 - C13 N3 - Distance Angles C17 1.3419 (0.0042) C18 1.4634 (0.0042) 118.39 (0.29) N3 - C17 O1 - Distance Angles C12 1.2271 (0.0038) O1 - O2 - Distance Angles C17 1.2331 (0.0038) O2 - Fe1 - Distance Angles C5 2.0223 (0.0040) C1 2.0271 (0.0037) 40.48 (0.16) C4 2.0322 (0.0042) 40.26 (0.17) 67.54 (0.16) C9 2.0326 (0.0035) 105.64 (0.16) 124.67 (0.16) 118.71 (0.17) C2 2.0333 (0.0038) 67.67 (0.16) 39.95 (0.15) 67.40 (0.16) 162.52 (0.16) C10 2.0342 (0.0035) 125.58 (0.17) 162.56 (0.17) 108.53 (0.16) 40.86 (0.13) 156.03 (0.16) C3 2.0360 (0.0040) 67.88 (0.18) 67.61 (0.16) 40.21 (0.17) 154.11 (0.17) 40.25 (0.15) 121.21 (0.16) C8 2.0366 (0.0035) 118.25 (0.17) 107.03 (0.15) 152.99 (0.18) 41.00 (0.13) 126.46 (0.15) 68.27 (0.14) 164.47 (0.17) C6 2.0481 (0.0037) 164.09 (0.18) 154.75 (0.17) 128.01 (0.18) 69.02 (0.14) 121.68 (0.16) 40.86 (0.13) 109.98 (0.16) C7 2.0536 (0.0036) 153.25 (0.19) 119.82 (0.16) 165.39 (0.19) 68.93 (0.14) 109.31 (0.15) 68.30 (0.14) 128.14 (0.18) Fe1 - C5 C1 C4 C9 C2 C10 C3 Fe2 - Distance Angles C28 2.0096 (0.0047) C24 2.0215 (0.0048) 40.54 (0.23) C27 2.0269 (0.0043) 40.48 (0.21) 67.44 (0.21) C25 2.0272 (0.0045) 67.38 (0.22) 39.94 (0.22) 66.43 (0.18) C26 2.0330 (0.0041) 66.79 (0.19) 66.40 (0.19) 39.15 (0.18) 39.05 (0.17) C20 2.0352 (0.0034) 128.62 (0.22) 109.95 (0.18) 166.04 (0.21) 121.10 (0.17) 153.81 (0.18) C22 2.0392 (0.0037) 152.63 (0.27) 164.22 (0.28) 118.08 (0.19) 126.39 (0.21) 107.73 (0.16) 68.36 (0.14) C21 2.0405 (0.0037) 166.18 (0.27) 128.04 (0.25) 151.65 (0.21) 108.70 (0.19) 119.22 (0.17) 40.86 (0.13) 40.46 (0.13) C19 2.0442 (0.0036) 109.02 (0.18) 121.12 (0.21) 127.87 (0.19) 155.20 (0.19) 164.27 (0.18) 40.58 (0.13) 68.56 (0.14) C23 2.0491 (0.0036) 119.43 (0.23) 154.70 (0.27) 107.72 (0.16) 163.00 (0.21) 126.51 (0.16) 68.40 (0.14) 40.61 (0.13) Fe2 - C28 C24 C27 C25 C26 C20 C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.23 2.961(3) 140.9 N2-H2A...O2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)