+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:36:10 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SOT033 in P-1 CELL 0.71073 8.2480 10.7247 19.0148 80.4289 88.9465 71.6786 ZERR 4 0.0007 0.0009 0.0018 0.0053 0.0050 0.0046 LATT 1 SFAC C H O F UNIT 64 76 12 12 V = 1573.48 F(000) = 664.0 Mu = 0.11 mm-1 Cell Wt = 1265.25 Rho = 1.335 L.S. 4 TEMP -123 SIZE 0.1 0.05 0.02 SHEL 7 0.9 HTAB EQIV $1 X-1, Y+1, Z EQIV $2 X, Y-1, Z HTAB O1B O2A_$1 HTAB O1A O2B_$2 FMAP 2 PLAN 20 WGHT 0.000000 EXTI 0.012983 FVAR 0.12583 F2A 4 0.850882 0.707457 0.041347 11.00000 0.07166 0.05642 = 0.04012 0.00526 -0.01083 -0.01776 F1B 4 0.460358 1.041566 0.311841 11.00000 0.08492 0.06695 = 0.04573 0.00093 -0.01238 -0.04588 O2B 3 0.801204 1.318694 0.222734 11.00000 0.03718 0.03814 = 0.03242 -0.00520 0.01089 -0.01431 F1A 4 0.761920 0.544244 0.087174 11.00000 0.06073 0.05190 = 0.05257 -0.00334 -0.01298 -0.01819 O3A 3 1.322288 0.240312 0.114968 11.00000 0.03877 0.03404 = 0.03841 -0.00927 -0.00055 -0.00885 O1B 3 0.434493 1.279806 0.363657 11.00000 0.03809 0.05220 = 0.03491 -0.00080 0.00255 -0.01563 AFIX 147 H1B 2 0.390514 1.288695 0.322890 11.00000 -1.50000 AFIX 0 O1A 3 0.816345 0.587860 0.226122 11.00000 0.03966 0.04093 = 0.04396 -0.00890 0.00557 -0.00872 AFIX 147 H1A 2 0.806516 0.512936 0.224021 11.00000 -1.50000 AFIX 0 O2A 3 1.296943 0.328630 0.220371 11.00000 0.03517 0.04112 = 0.03138 -0.00423 0.00111 -0.00422 O3B 3 0.856485 1.148178 0.154945 11.00000 0.04707 0.04757 = 0.03695 -0.01535 0.00849 -0.02471 F2B 4 0.648628 0.927904 0.394759 11.00000 0.06719 0.04205 = 0.06717 0.00901 -0.00739 -0.01843 F3B 4 0.399990 1.044437 0.421694 11.00000 0.06449 0.07582 = 0.05712 0.01028 0.00672 -0.04146 F3A 4 0.636025 0.741282 0.109174 11.00000 0.04856 0.07012 = 0.06683 -0.01133 -0.01639 0.01045 C11B 1 0.693931 1.292817 0.276196 11.00000 0.02813 0.03838 = 0.03650 -0.01155 0.00592 -0.01249 AFIX 43 H11B 2 0.601413 1.366189 0.286017 11.00000 -1.20000 AFIX 0 C11A 1 1.142185 0.429123 0.216503 11.00000 0.02312 0.03897 = 0.03372 -0.00933 0.00715 -0.00813 AFIX 43 H11A 2 1.077791 0.433567 0.258476 11.00000 -1.20000 AFIX 0 C10B 1 0.709257 1.174657 0.314769 11.00000 0.03140 0.03394 = 0.02917 -0.00193 -0.00418 -0.00960 C3A 1 0.933629 0.758532 0.178375 11.00000 0.05252 0.03053 = 0.04519 -0.00249 0.00573 -0.00976 AFIX 23 H3A1 2 0.968087 0.801476 0.132944 11.00000 -1.20000 H3A2 2 0.823213 0.819237 0.190844 11.00000 -1.20000 AFIX 0 C2B 1 0.584531 1.166637 0.373850 11.00000 0.03322 0.04179 = 0.03091 0.00451 -0.00336 -0.00896 C2A 1 0.907368 0.626216 0.166801 11.00000 0.03896 0.03555 = 0.03206 -0.00109 -0.00099 -0.00567 C4A 1 1.065295 0.741516 0.235681 11.00000 0.04992 0.02682 = 0.04685 -0.01607 0.00381 -0.00726 C12B 1 0.929053 1.204070 0.202681 11.00000 0.03031 0.04342 = 0.04230 -0.01409 0.01205 -0.00815 AFIX 13 H12B 2 1.024643 1.232183 0.179450 11.00000 -1.20000 AFIX 0 C10A 1 1.075729 0.519327 0.159969 11.00000 0.03331 0.02848 = 0.03396 -0.00586 -0.00162 -0.01399 C14A 1 1.174964 0.523774 0.093200 11.00000 0.05177 0.03882 = 0.03360 -0.00328 0.00372 -0.01669 AFIX 23 H14A 2 1.160933 0.617564 0.072140 11.00000 -1.20000 H14B 2 1.130642 0.483184 0.057893 11.00000 -1.20000 AFIX 0 C1A 1 0.789847 0.654163 0.101117 11.00000 0.04368 0.04546 = 0.04602 -0.00809 0.00143 -0.00634 C4B 1 0.758949 1.259029 0.446874 11.00000 0.04500 0.04864 = 0.02404 -0.00697 0.00302 -0.01551 C12A 1 1.385126 0.314673 0.153710 11.00000 0.03278 0.04242 = 0.04428 -0.00412 0.00811 -0.00824 AFIX 13 H12A 2 1.509718 0.268137 0.164778 11.00000 -1.20000 AFIX 0 C3B 1 0.662283 1.160719 0.447839 11.00000 0.04395 0.05004 = 0.03083 -0.00094 0.00177 -0.01117 AFIX 23 H3B1 2 0.569599 1.179466 0.482188 11.00000 -1.20000 H3B2 2 0.740628 1.069608 0.464462 11.00000 -1.20000 AFIX 0 C5A 1 1.029227 0.723060 0.307461 11.00000 0.05574 0.03367 = 0.04703 -0.00633 0.00254 -0.01363 AFIX 43 H5A 2 0.918792 0.720494 0.321110 11.00000 -1.20000 AFIX 0 C9B 1 0.934411 1.216959 0.444680 11.00000 0.04563 0.07177 = 0.04194 -0.01879 0.00295 -0.02581 AFIX 43 H9B 2 0.993839 1.124491 0.447978 11.00000 -1.20000 AFIX 0 C1B 1 0.525391 1.045177 0.375091 11.00000 0.05253 0.05282 = 0.04340 0.00300 0.00444 -0.02749 C13B 1 0.998219 1.099206 0.267727 11.00000 0.03474 0.04706 = 0.05106 -0.01543 0.00683 -0.00930 AFIX 23 H13A 2 1.055808 1.135339 0.300840 11.00000 -1.20000 H13B 2 1.084173 1.021013 0.253077 11.00000 -1.20000 AFIX 0 C5B 1 0.675198 1.394723 0.442811 11.00000 0.05931 0.05355 = 0.04491 -0.01515 -0.00604 -0.00957 AFIX 43 H5B 2 0.554364 1.426339 0.445558 11.00000 -1.20000 AFIX 0 C13A 1 1.363001 0.448437 0.110192 11.00000 0.04300 0.05302 = 0.03968 -0.01189 0.01222 -0.01670 AFIX 23 H13C 2 1.424178 0.437773 0.065197 11.00000 -1.20000 H13D 2 1.413253 0.500130 0.136780 11.00000 -1.20000 AFIX 0 C8A 1 1.354337 0.721537 0.270364 11.00000 0.04808 0.06505 = 0.09968 -0.03340 0.01172 -0.02650 AFIX 43 H8A 2 1.466556 0.720206 0.257360 11.00000 -1.20000 AFIX 0 C14B 1 0.857124 1.055573 0.305977 11.00000 0.04519 0.04017 = 0.04269 -0.00410 -0.00103 -0.00996 AFIX 23 H14C 2 0.819455 0.998771 0.278139 11.00000 -1.20000 H14D 2 0.900849 1.002425 0.353407 11.00000 -1.20000 AFIX 0 C6A 1 1.151984 0.708360 0.359361 11.00000 0.07641 0.06023 = 0.04175 -0.00839 -0.00264 -0.02716 AFIX 43 H6A 2 1.124001 0.699362 0.408234 11.00000 -1.20000 AFIX 0 C9A 1 1.229040 0.738561 0.218334 11.00000 0.06829 0.05588 = 0.04777 -0.01706 0.00876 -0.02816 AFIX 43 H9A 2 1.257375 0.748407 0.169513 11.00000 -1.20000 AFIX 0 C7B 1 0.941582 1.438827 0.431615 11.00000 0.11342 0.08687 = 0.04968 -0.00247 -0.01806 -0.06639 AFIX 43 H7B 2 1.003361 1.500947 0.425070 11.00000 -1.20000 AFIX 0 C7A 1 1.312545 0.706693 0.340919 11.00000 0.06995 0.06332 = 0.07159 -0.00675 -0.01424 -0.02468 AFIX 43 H7A 2 1.396526 0.695185 0.377047 11.00000 -1.20000 AFIX 0 C8B 1 1.026476 1.305895 0.437793 11.00000 0.05602 0.11153 = 0.04557 -0.02452 0.00436 -0.03805 AFIX 43 H8B 2 1.147730 1.274582 0.437375 11.00000 -1.20000 AFIX 0 C6B 1 0.766191 1.483118 0.434859 11.00000 0.09617 0.06010 = 0.07127 -0.00636 -0.02433 -0.02596 AFIX 43 H6B 2 0.707718 1.575743 0.431558 11.00000 -1.20000 AFIX 0 C15A 1 1.374862 0.099664 0.143599 11.00000 0.03339 0.03695 = 0.04587 -0.00442 -0.00172 -0.00690 AFIX 23 H15A 2 1.320923 0.084038 0.189761 11.00000 -1.20000 H15B 2 1.500505 0.064824 0.151592 11.00000 -1.20000 AFIX 0 C16A 1 1.319741 0.030760 0.090456 11.00000 0.05861 0.04108 = 0.06232 -0.01279 -0.00211 -0.00946 AFIX 137 H16A 2 1.194819 0.062645 0.084830 11.00000 -1.50000 H16B 2 1.358749 -0.065646 0.107430 11.00000 -1.50000 H16C 2 1.369647 0.050267 0.044390 11.00000 -1.50000 AFIX 0 C15B 1 0.822483 1.226661 0.084361 11.00000 0.04576 0.05054 = 0.03945 -0.00335 0.00932 -0.02258 AFIX 23 H15C 2 0.926185 1.247395 0.066505 11.00000 -1.20000 H15D 2 0.729879 1.311554 0.085260 11.00000 -1.20000 AFIX 0 C16B 1 0.769968 1.146130 0.036824 11.00000 0.08681 0.08670 = 0.04497 -0.01836 0.00751 -0.05083 AFIX 137 H16D 2 0.862939 1.062785 0.036022 11.00000 -1.50000 H16E 2 0.745149 1.197184 -0.011665 11.00000 -1.50000 H16F 2 0.667582 1.125922 0.055124 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 99SOT033 in P-1 C 0.770 H 0.320 O 0.660 F 0.640 F2A - C1A F1B - C1B O2B - C11B C12B F1A - C1A O3A - C12A C15A O1B - C2B O1A - C2A O2A - C11A C12A O3B - C12B C15B F2B - C1B F3B - C1B F3A - C1A C11B - C10B O2B C11A - C10A O2A C10B - C11B C14B C2B C3A - C4A C2A C2B - O1B C10B C1B C3B C2A - O1A C10A C1A C3A C4A - C9A C5A C3A C12B - O3B O2B C13B C10A - C11A C14A C2A C14A - C10A C13A C1A - F1A F3A F2A C2A C4B - C9B C5B C3B C12A - O3A O2A C13A C3B - C4B C2B C5A - C6A C4A C9B - C4B C8B C1B - F1B F2B F3B C2B C13B - C12B C14B C5B - C6B C4B C13A - C12A C14A C8A - C7A C9A C14B - C10B C13B C6A - C7A C5A C9A - C4A C8A C7B - C8B C6B C7A - C6A C8A C8B - C7B C9B C6B - C5B C7B C15A - O3A C16A C16A - C15A C15B - O3B C16B C16B - C15B Operators for generating equivalent atoms: $1 x-1, y+1, z $2 x, y-1, z 14488 Reflections read, of which 1744 rejected -9 =< h =< 9, -11 =< k =< 11, -21 =< l =< 21, Max. 2-theta = 46.51 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 -10 1 0.75 0.41 2 4.83 8 8 1 0.41 0.41 2 4.80 9 3 2 6.21 0.83 3 7.92 8 7 3 2.47 0.70 3 7.47 -6 5 6 0.53 0.40 3 2.71 2 0 8 -0.17 0.10 2 0.88 6 1 8 0.35 0.07 3 0.47 -8 -1 9 1.62 0.84 3 6.47 8 2 9 0.29 0.20 3 1.26 3 -2 10 1.03 0.09 4 0.51 0 1 11 0.16 0.25 4 1.86 3 1 15 0.14 0.10 2 1.13 3 1 17 0.02 0.10 2 0.51 -4 4 17 2.61 0.81 3 6.72 14 Inconsistent equivalents 4495 Unique reflections, of which 0 suppressed R(int) = 0.1345 R(sigma) = 0.1646 Friedel opposites merged Maximum memory for data reduction = 3195 / 45413 Default effective X-H distances for T = -123.0 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 = 4353 / 515646 wR2 = 0.1165 before cycle 1 for 4495 data and 402 / 402 parameters GooF = S = 0.927; Restrained GooF = 0.927 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12583 0.00028 0.007 OSF 2 0.01298 0.00104 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.007 for OSF Max. shift = 0.000 A for H16E Max. dU = 0.000 for C15A Least-squares cycle 2 Maximum vector length = 511 Memory required = 4353 / 515646 wR2 = 0.1165 before cycle 2 for 4495 data and 402 / 402 parameters GooF = S = 0.927; Restrained GooF = 0.927 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12583 0.00028 0.000 OSF 2 0.01298 0.00104 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U12 F2A Max. shift = 0.000 A for H16E Max. dU = 0.000 for C15A Least-squares cycle 3 Maximum vector length = 511 Memory required = 4353 / 515646 wR2 = 0.1165 before cycle 3 for 4495 data and 402 / 402 parameters GooF = S = 0.927; Restrained GooF = 0.927 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12583 0.00028 0.000 OSF 2 0.01298 0.00104 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1A Max. dU = 0.000 for C16B Least-squares cycle 4 Maximum vector length = 511 Memory required = 4353 / 515646 wR2 = 0.1165 before cycle 4 for 4495 data and 402 / 402 parameters GooF = S = 0.927; Restrained GooF = 0.927 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12583 0.00028 0.000 OSF 2 0.01298 0.00104 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H16D Max. dU = 0.000 for C9A Largest correlation matrix elements 0.690 EXTI / OSF 0.548 x C6B / x C7B 0.528 y C8B / y C7B Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1B 0.3905 1.2887 0.3229 147 0.840 0.000 O1B C2B H1B H1A 0.8065 0.5129 0.2240 147 0.840 0.000 O1A C2A H1A H11B 0.6014 1.3662 0.2860 43 0.950 0.000 C11B C10B O2B H11A 1.0778 0.4336 0.2585 43 0.950 0.000 C11A C10A O2A H3A1 0.9681 0.8015 0.1329 23 0.990 0.000 C3A C4A C2A H3A2 0.8232 0.8192 0.1908 23 0.990 0.000 C3A C4A C2A H12B 1.0246 1.2322 0.1795 13 1.000 0.000 C12B O3B O2B C13B H14A 1.1609 0.6176 0.0721 23 0.990 0.000 C14A C10A C13A H14B 1.1306 0.4832 0.0579 23 0.990 0.000 C14A C10A C13A H12A 1.5097 0.2681 0.1648 13 1.000 0.000 C12A O3A O2A C13A H3B1 0.5696 1.1795 0.4822 23 0.990 0.000 C3B C4B C2B H3B2 0.7406 1.0696 0.4645 23 0.990 0.000 C3B C4B C2B H5A 0.9188 0.7205 0.3211 43 0.950 0.000 C5A C6A C4A H9B 0.9938 1.1245 0.4480 43 0.950 0.000 C9B C4B C8B H13A 1.0558 1.1353 0.3008 23 0.990 0.000 C13B C12B C14B H13B 1.0842 1.0210 0.2531 23 0.990 0.000 C13B C12B C14B H5B 0.5544 1.4263 0.4456 43 0.950 0.000 C5B C6B C4B H13C 1.4242 0.4378 0.0652 23 0.990 0.000 C13A C12A C14A H13D 1.4133 0.5001 0.1368 23 0.990 0.000 C13A C12A C14A H8A 1.4666 0.7202 0.2574 43 0.950 0.000 C8A C7A C9A H14C 0.8195 0.9988 0.2781 23 0.990 0.000 C14B C10B C13B H14D 0.9008 1.0024 0.3534 23 0.990 0.000 C14B C10B C13B H6A 1.1240 0.6994 0.4082 43 0.950 0.000 C6A C7A C5A H9A 1.2574 0.7484 0.1695 43 0.950 0.000 C9A C4A C8A H7B 1.0034 1.5009 0.4251 43 0.950 0.000 C7B C8B C6B H7A 1.3965 0.6952 0.3770 43 0.950 0.000 C7A C6A C8A H8B 1.1477 1.2746 0.4374 43 0.950 0.000 C8B C7B C9B H6B 0.7077 1.5757 0.4316 43 0.950 0.000 C6B C5B C7B H15A 1.3209 0.0840 0.1898 23 0.990 0.000 C15A O3A C16A H15B 1.5005 0.0648 0.1516 23 0.990 0.000 C15A O3A C16A H16A 1.1948 0.0626 0.0848 137 0.980 0.000 C16A C15A H16A H16B 1.3587 -0.0656 0.1074 137 0.980 0.000 C16A C15A H16A H16C 1.3696 0.0503 0.0444 137 0.980 0.000 C16A C15A H16A H15C 0.9262 1.2474 0.0665 23 0.990 0.000 C15B O3B C16B H15D 0.7299 1.3116 0.0853 23 0.990 0.000 C15B O3B C16B H16D 0.8629 1.0628 0.0360 137 0.980 0.000 C16B C15B H16D H16E 0.7451 1.1972 -0.0117 137 0.980 0.000 C16B C15B H16D H16F 0.6676 1.1259 0.0551 137 0.980 0.000 C16B C15B H16D 99SOT033 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F2A 0.85088 0.70746 0.04135 1.00000 0.07166 0.05642 0.04012 0.00526 -0.01083 -0.01776 0.05809 0.00401 0.00034 0.00024 0.00014 0.00000 0.00194 0.00176 0.00179 0.00141 0.00151 0.00149 0.00081 F1B 0.46036 1.04157 0.31184 1.00000 0.08492 0.06695 0.04573 0.00093 -0.01238 -0.04588 0.06176 0.00415 0.00034 0.00024 0.00014 0.00000 0.00216 0.00186 0.00191 0.00148 0.00164 0.00160 0.00085 O2B 0.80120 1.31869 0.22273 1.00000 0.03718 0.03814 0.03242 -0.00520 0.01089 -0.01431 0.03556 0.00419 0.00034 0.00025 0.00014 0.00000 0.00179 0.00178 0.00187 0.00147 0.00148 0.00153 0.00079 F1A 0.76192 0.54424 0.08717 1.00000 0.06073 0.05190 0.05257 -0.00334 -0.01298 -0.01819 0.05543 0.00418 0.00032 0.00026 0.00013 0.00000 0.00182 0.00172 0.00186 0.00147 0.00141 0.00148 0.00080 O3A 1.32229 0.24031 0.11497 1.00000 0.03877 0.03404 0.03841 -0.00927 -0.00055 -0.00885 0.03729 0.00457 0.00034 0.00026 0.00015 0.00000 0.00184 0.00177 0.00194 0.00153 0.00151 0.00151 0.00081 O1B 0.43449 1.27981 0.36366 1.00000 0.03809 0.05220 0.03491 -0.00080 0.00255 -0.01563 0.04222 0.00462 0.00035 0.00028 0.00015 0.00000 0.00186 0.00193 0.00198 0.00159 0.00148 0.00160 0.00085 H1B 0.39051 1.28869 0.32289 1.00000 0.06332 0.00000 0.00000 O1A 0.81635 0.58786 0.22612 1.00000 0.03966 0.04093 0.04396 -0.00890 0.00557 -0.00872 0.04231 0.00471 0.00037 0.00026 0.00016 0.00000 0.00182 0.00193 0.00205 0.00163 0.00159 0.00170 0.00085 H1A 0.80652 0.51294 0.22402 1.00000 0.06346 0.00000 0.00000 O2A 1.29694 0.32863 0.22037 1.00000 0.03517 0.04112 0.03138 -0.00423 0.00111 -0.00422 0.03796 0.00420 0.00033 0.00025 0.00014 0.00000 0.00179 0.00180 0.00190 0.00147 0.00149 0.00152 0.00083 O3B 0.85649 1.14818 0.15494 1.00000 0.04707 0.04757 0.03695 -0.01535 0.00849 -0.02471 0.04067 0.00449 0.00035 0.00026 0.00016 0.00000 0.00202 0.00189 0.00208 0.00166 0.00162 0.00159 0.00083 F2B 0.64863 0.92790 0.39476 1.00000 0.06719 0.04205 0.06717 0.00901 -0.00739 -0.01843 0.06059 0.00407 0.00033 0.00024 0.00014 0.00000 0.00192 0.00157 0.00205 0.00144 0.00156 0.00147 0.00085 F3B 0.39999 1.04444 0.42169 1.00000 0.06449 0.07582 0.05712 0.01028 0.00672 -0.04146 0.06390 0.00422 0.00034 0.00025 0.00015 0.00000 0.00196 0.00203 0.00199 0.00156 0.00160 0.00159 0.00086 F3A 0.63602 0.74128 0.10917 1.00000 0.04856 0.07012 0.06683 -0.01133 -0.01639 0.01045 0.06851 0.00424 0.00032 0.00026 0.00014 0.00000 0.00175 0.00185 0.00205 0.00157 0.00151 0.00154 0.00093 C11B 0.69393 1.29282 0.27620 1.00000 0.02813 0.03838 0.03650 -0.01155 0.00592 -0.01249 0.03330 0.00611 0.00050 0.00041 0.00022 0.00000 0.00265 0.00284 0.00299 0.00243 0.00229 0.00221 0.00117 H11B 0.60141 1.36619 0.28602 1.00000 0.03996 0.00000 0.00000 C11A 1.14218 0.42912 0.21650 1.00000 0.02312 0.03897 0.03372 -0.00933 0.00715 -0.00813 0.03203 0.00610 0.00047 0.00038 0.00023 0.00000 0.00252 0.00265 0.00288 0.00227 0.00213 0.00217 0.00115 H11A 1.07779 0.43357 0.25848 1.00000 0.03844 0.00000 0.00000 C10B 0.70926 1.17466 0.31477 1.00000 0.03140 0.03394 0.02917 -0.00193 -0.00418 -0.00960 0.03202 0.00627 0.00050 0.00040 0.00023 0.00000 0.00270 0.00269 0.00275 0.00224 0.00216 0.00224 0.00115 C3A 0.93363 0.75853 0.17837 1.00000 0.05252 0.03053 0.04519 -0.00249 0.00573 -0.00976 0.04406 0.00700 0.00056 0.00039 0.00024 0.00000 0.00315 0.00270 0.00321 0.00238 0.00260 0.00241 0.00132 H3A1 0.96809 0.80148 0.13294 1.00000 0.05288 0.00000 0.00000 H3A2 0.82321 0.81924 0.19084 1.00000 0.05288 0.00000 0.00000 C2B 0.58453 1.16664 0.37385 1.00000 0.03322 0.04179 0.03091 0.00451 -0.00336 -0.00896 0.03721 0.00696 0.00052 0.00042 0.00023 0.00000 0.00277 0.00286 0.00294 0.00227 0.00230 0.00244 0.00123 C2A 0.90737 0.62622 0.16680 1.00000 0.03896 0.03555 0.03206 -0.00109 -0.00099 -0.00567 0.03749 0.00686 0.00054 0.00040 0.00023 0.00000 0.00281 0.00282 0.00296 0.00232 0.00244 0.00236 0.00123 C4A 1.06529 0.74152 0.23568 1.00000 0.04992 0.02682 0.04685 -0.01607 0.00381 -0.00726 0.04119 0.00729 0.00062 0.00040 0.00026 0.00000 0.00327 0.00263 0.00350 0.00239 0.00280 0.00239 0.00128 C12B 0.92905 1.20407 0.20268 1.00000 0.03031 0.04342 0.04230 -0.01409 0.01205 -0.00815 0.03882 0.00721 0.00053 0.00041 0.00023 0.00000 0.00268 0.00285 0.00315 0.00252 0.00237 0.00234 0.00123 H12B 1.02464 1.23218 0.17945 1.00000 0.04659 0.00000 0.00000 C10A 1.07573 0.51933 0.15997 1.00000 0.03331 0.02848 0.03396 -0.00586 -0.00162 -0.01399 0.03081 0.00612 0.00050 0.00037 0.00022 0.00000 0.00262 0.00249 0.00292 0.00225 0.00227 0.00215 0.00113 C14A 1.17496 0.52377 0.09320 1.00000 0.05177 0.03882 0.03360 -0.00328 0.00372 -0.01669 0.04121 0.00679 0.00053 0.00040 0.00022 0.00000 0.00310 0.00276 0.00304 0.00228 0.00246 0.00241 0.00127 H14A 1.16093 0.61756 0.07214 1.00000 0.04945 0.00000 0.00000 H14B 1.13064 0.48318 0.05789 1.00000 0.04945 0.00000 0.00000 C1A 0.78985 0.65416 0.10112 1.00000 0.04368 0.04546 0.04602 -0.00809 0.00143 -0.00634 0.04683 0.00803 0.00061 0.00050 0.00026 0.00000 0.00329 0.00324 0.00369 0.00289 0.00275 0.00280 0.00136 C4B 0.75895 1.25903 0.44687 1.00000 0.04500 0.04864 0.02404 -0.00697 0.00302 -0.01551 0.03898 0.00716 0.00061 0.00046 0.00022 0.00000 0.00315 0.00319 0.00281 0.00231 0.00229 0.00269 0.00123 C12A 1.38513 0.31467 0.15371 1.00000 0.03278 0.04242 0.04428 -0.00412 0.00811 -0.00824 0.04116 0.00768 0.00055 0.00043 0.00025 0.00000 0.00280 0.00301 0.00336 0.00263 0.00251 0.00235 0.00129 H12A 1.50972 0.26814 0.16478 1.00000 0.04939 0.00000 0.00000 C3B 0.66228 1.16072 0.44784 1.00000 0.04395 0.05004 0.03083 -0.00094 0.00177 -0.01117 0.04318 0.00703 0.00055 0.00042 0.00022 0.00000 0.00289 0.00302 0.00302 0.00238 0.00235 0.00255 0.00130 H3B1 0.56960 1.17947 0.48219 1.00000 0.05182 0.00000 0.00000 H3B2 0.74063 1.06961 0.46446 1.00000 0.05182 0.00000 0.00000 C5A 1.02923 0.72306 0.30746 1.00000 0.05574 0.03367 0.04703 -0.00633 0.00254 -0.01363 0.04566 0.00762 0.00062 0.00039 0.00026 0.00000 0.00325 0.00276 0.00356 0.00246 0.00289 0.00242 0.00135 H5A 0.91879 0.72049 0.32111 1.00000 0.05480 0.00000 0.00000 C9B 0.93441 1.21696 0.44468 1.00000 0.04563 0.07177 0.04194 -0.01879 0.00295 -0.02581 0.05031 0.00774 0.00064 0.00052 0.00024 0.00000 0.00335 0.00367 0.00339 0.00278 0.00259 0.00306 0.00140 H9B 0.99384 1.12449 0.44798 1.00000 0.06037 0.00000 0.00000 C1B 0.52539 1.04518 0.37509 1.00000 0.05253 0.05282 0.04340 0.00300 0.00444 -0.02749 0.04840 0.00820 0.00064 0.00048 0.00028 0.00000 0.00354 0.00349 0.00365 0.00278 0.00299 0.00298 0.00135 C13B 0.99822 1.09921 0.26773 1.00000 0.03474 0.04706 0.05106 -0.01543 0.00683 -0.00930 0.04435 0.00716 0.00054 0.00041 0.00024 0.00000 0.00280 0.00294 0.00338 0.00257 0.00249 0.00241 0.00132 H13A 1.05581 1.13534 0.30084 1.00000 0.05322 0.00000 0.00000 H13B 1.08417 1.02101 0.25308 1.00000 0.05322 0.00000 0.00000 C5B 0.67520 1.39472 0.44281 1.00000 0.05931 0.05355 0.04491 -0.01514 -0.00604 -0.00957 0.05361 0.00812 0.00067 0.00050 0.00025 0.00000 0.00360 0.00347 0.00340 0.00278 0.00276 0.00321 0.00149 H5B 0.55436 1.42634 0.44556 1.00000 0.06434 0.00000 0.00000 C13A 1.36300 0.44844 0.11019 1.00000 0.04300 0.05302 0.03968 -0.01189 0.01222 -0.01670 0.04452 0.00700 0.00051 0.00040 0.00023 0.00000 0.00302 0.00309 0.00309 0.00256 0.00241 0.00253 0.00132 H13C 1.42418 0.43777 0.06520 1.00000 0.05343 0.00000 0.00000 H13D 1.41325 0.50013 0.13678 1.00000 0.05343 0.00000 0.00000 C8A 1.35434 0.72154 0.27036 1.00000 0.04808 0.06505 0.09968 -0.03340 0.01172 -0.02650 0.06668 0.00885 0.00067 0.00048 0.00036 0.00000 0.00358 0.00375 0.00525 0.00373 0.00371 0.00291 0.00167 H8A 1.46656 0.72021 0.25736 1.00000 0.08001 0.00000 0.00000 C14B 0.85712 1.05557 0.30598 1.00000 0.04519 0.04017 0.04269 -0.00410 -0.00103 -0.00996 0.04383 0.00713 0.00052 0.00040 0.00024 0.00000 0.00307 0.00281 0.00315 0.00239 0.00250 0.00249 0.00132 H14C 0.81945 0.99877 0.27814 1.00000 0.05259 0.00000 0.00000 H14D 0.90085 1.00242 0.35341 1.00000 0.05259 0.00000 0.00000 C6A 1.15198 0.70836 0.35936 1.00000 0.07641 0.06023 0.04175 -0.00839 -0.00264 -0.02716 0.05811 0.00838 0.00075 0.00046 0.00028 0.00000 0.00414 0.00357 0.00356 0.00271 0.00331 0.00317 0.00151 H6A 1.12400 0.69936 0.40823 1.00000 0.06973 0.00000 0.00000 C9A 1.22904 0.73856 0.21833 1.00000 0.06829 0.05588 0.04777 -0.01706 0.00876 -0.02816 0.05438 0.00809 0.00070 0.00044 0.00027 0.00000 0.00393 0.00344 0.00364 0.00273 0.00320 0.00296 0.00146 H9A 1.25737 0.74841 0.16951 1.00000 0.06526 0.00000 0.00000 C7B 0.94158 1.43883 0.43161 1.00000 0.11342 0.08687 0.04969 -0.00247 -0.01806 -0.06639 0.07593 0.00834 0.00094 0.00066 0.00027 0.00000 0.00588 0.00504 0.00392 0.00348 0.00392 0.00445 0.00189 H7B 1.00336 1.50095 0.42507 1.00000 0.09112 0.00000 0.00000 C7A 1.31255 0.70669 0.34092 1.00000 0.06995 0.06332 0.07159 -0.00675 -0.01424 -0.02468 0.06777 0.00895 0.00078 0.00049 0.00034 0.00000 0.00438 0.00379 0.00475 0.00334 0.00360 0.00326 0.00168 H7A 1.39653 0.69518 0.37705 1.00000 0.08132 0.00000 0.00000 C8B 1.02648 1.30589 0.43779 1.00000 0.05602 0.11153 0.04557 -0.02452 0.00436 -0.03805 0.06699 0.00866 0.00071 0.00069 0.00026 0.00000 0.00380 0.00516 0.00375 0.00365 0.00292 0.00406 0.00169 H8B 1.14773 1.27458 0.43738 1.00000 0.08038 0.00000 0.00000 C6B 0.76619 1.48312 0.43486 1.00000 0.09617 0.06010 0.07127 -0.00636 -0.02433 -0.02597 0.07575 0.00958 0.00093 0.00057 0.00029 0.00000 0.00523 0.00392 0.00453 0.00323 0.00398 0.00406 0.00193 H6B 0.70772 1.57574 0.43156 1.00000 0.09090 0.00000 0.00000 C15A 1.37486 0.09966 0.14360 1.00000 0.03339 0.03695 0.04587 -0.00442 -0.00172 -0.00690 0.03999 0.00676 0.00052 0.00038 0.00024 0.00000 0.00268 0.00282 0.00321 0.00245 0.00237 0.00226 0.00127 H15A 1.32092 0.08404 0.18976 1.00000 0.04799 0.00000 0.00000 H15B 1.50050 0.06482 0.15159 1.00000 0.04799 0.00000 0.00000 C16A 1.31974 0.03076 0.09046 1.00000 0.05861 0.04108 0.06232 -0.01279 -0.00211 -0.00946 0.05494 0.00726 0.00058 0.00041 0.00025 0.00000 0.00350 0.00289 0.00374 0.00274 0.00287 0.00261 0.00150 H16A 1.19482 0.06265 0.08483 1.00000 0.08241 0.00000 0.00000 H16B 1.35875 -0.06565 0.10743 1.00000 0.08241 0.00000 0.00000 H16C 1.36965 0.05027 0.04439 1.00000 0.08241 0.00000 0.00000 C15B 0.82248 1.22666 0.08436 1.00000 0.04576 0.05054 0.03945 -0.00335 0.00932 -0.02258 0.04412 0.00701 0.00056 0.00042 0.00023 0.00000 0.00298 0.00309 0.00321 0.00262 0.00248 0.00250 0.00130 H15C 0.92618 1.24739 0.06650 1.00000 0.05295 0.00000 0.00000 H15D 0.72988 1.31155 0.08526 1.00000 0.05295 0.00000 0.00000 C16B 0.76997 1.14613 0.03682 1.00000 0.08681 0.08670 0.04497 -0.01836 0.00751 -0.05083 0.06649 0.00745 0.00065 0.00048 0.00025 0.00000 0.00427 0.00395 0.00355 0.00310 0.00303 0.00336 0.00161 H16D 0.86294 1.06278 0.03602 1.00000 0.09974 0.00000 0.00000 H16E 0.74515 1.19718 -0.01167 1.00000 0.09974 0.00000 0.00000 H16F 0.66758 1.12592 0.05512 1.00000 0.09974 0.00000 0.00000 Final Structure Factor Calculation for 99SOT033 in P-1 Total number of l.s. parameters = 402 Maximum vector length = 511 Memory required = 3951 / 22995 wR2 = 0.1165 before cycle 5 for 4495 data and 0 / 402 parameters GooF = S = 0.927; Restrained GooF = 0.927 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0568 for 2058 Fo > 4sig(Fo) and 0.1592 for all 4495 data wR2 = 0.1165, GooF = S = 0.927, Restrained GooF = 0.927 for all data Occupancy sum of asymmetric unit = 44.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0767 0.0645 0.0330 F2A 0.1018 0.0441 0.0394 F1B 0.0446 0.0384 0.0236 O2B 0.0729 0.0517 0.0416 F1A 0.0434 0.0367 0.0317 O3A 0.0561 0.0384 0.0322 O1B 0.0480 0.0440 0.0349 O1A 0.0508 0.0321 0.0310 O2A 0.0574 0.0343 0.0302 O3B 0.0828 0.0642 0.0348 F2B 0.0963 0.0654 0.0300 F3B 0.1061 0.0678 0.0317 F3A 0.0423 0.0319 0.0257 C11B 0.0404 0.0356 0.0200 C11A 0.0370 0.0341 0.0250 C10B 0.0583 0.0438 0.0300 C3A 0.0512 0.0356 0.0248 C2B 0.0470 0.0370 0.0285 C2A 0.0535 0.0493 0.0208 C4A 0.0491 0.0449 0.0225 C12B 0.0370 0.0325 0.0229 C10A 0.0520 0.0401 0.0316 C14A 0.0560 0.0460 0.0385 C1A 0.0487 0.0446 0.0236 C4B 0.0536 0.0405 0.0294 C12A 0.0564 0.0433 0.0299 C3B 0.0567 0.0471 0.0332 C5A 0.0733 0.0427 0.0349 C9B 0.0647 0.0508 0.0297 C1B 0.0555 0.0458 0.0317 C13B 0.0728 0.0498 0.0382 C5B 0.0542 0.0493 0.0301 C13A 0.1060 0.0542 0.0398 C8A 0.0486 0.0452 0.0377 C14B 0.0779 0.0559 0.0406 C6A 0.0725 0.0503 0.0404 C9A 0.1373 0.0544 0.0361 C7B 0.0888 0.0620 0.0525 C7A 0.1121 0.0493 0.0396 C8B 0.1149 0.0590 0.0534 C6B 0.0472 0.0417 0.0312 C15A 0.0684 0.0572 0.0392 C16A 0.0542 0.0491 0.0291 C15B 0.1047 0.0535 0.0413 C16B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.029 0.040 0.054 0.070 0.089 0.119 0.181 1.000 Number in group 458. 443. 482. 415. 457. 462. 430. 454. 446. 448. GooF 0.789 0.773 0.840 0.860 0.891 0.946 1.029 1.016 0.889 1.167 K 9.436 2.029 1.176 0.972 0.997 0.977 0.975 0.974 0.993 1.017 Resolution(A) 0.90 0.93 0.97 1.02 1.07 1.14 1.22 1.34 1.54 1.93 inf Number in group 455. 450. 469. 439. 441. 441. 456. 448. 446. 450. GooF 0.822 0.830 0.867 0.872 0.887 0.894 0.936 0.923 1.048 1.142 K 1.140 0.987 1.006 1.000 0.983 0.991 1.003 1.025 1.038 1.004 R1 0.421 0.358 0.322 0.236 0.190 0.141 0.135 0.116 0.067 0.035 Recommended weighting scheme: WGHT 0.0000 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) -2 1 10 179.33 102.41 3.80 0.076 1.69 8 8 2 16.40 100.03 3.80 0.075 0.93 -2 -1 7 3794.66 3288.95 3.69 0.430 2.21 3 1 15 9.11 239.88 3.64 0.116 1.14 0 -2 1 2418.04 2612.19 3.61 0.384 4.65 -3 0 7 2182.05 1952.42 3.47 0.332 1.90 -2 -4 3 129.76 77.92 3.47 0.066 2.21 -2 0 1 19533.88 17749.57 3.46 1.000 3.86 -4 -2 11 119.44 225.87 3.45 0.113 1.29 -5 6 2 -21.37 59.44 3.42 0.058 1.00 -3 -1 5 2345.43 2023.77 3.41 0.338 2.21 1 0 2 1844.85 2089.46 3.39 0.343 5.90 1 -1 1 2644.52 2927.90 3.38 0.406 5.03 -4 2 5 1243.41 1035.42 3.21 0.242 1.56 2 10 10 123.94 0.08 3.18 0.002 0.99 4 6 9 1415.52 1120.80 3.17 0.251 1.32 -1 2 15 -11.10 47.62 3.16 0.052 1.24 -3 1 1 75.40 36.07 3.10 0.045 2.35 4 5 4 105.24 40.49 3.10 0.048 1.65 2 6 4 48.98 105.93 3.08 0.077 1.73 -3 -1 6 4570.04 4129.39 3.01 0.482 2.05 -2 8 13 -31.07 62.85 2.99 0.060 0.95 -2 -1 9 4652.26 4122.50 2.99 0.482 1.83 -2 -2 4 765.10 662.55 2.95 0.193 2.79 -1 4 5 86.21 131.13 2.94 0.086 2.04 2 0 0 2800.22 3051.08 2.91 0.415 3.91 3 4 1 2407.31 2098.07 2.90 0.344 2.20 1 -1 16 60.93 127.29 2.90 0.085 1.12 4 7 9 183.40 82.96 2.90 0.068 1.23 1 -6 8 104.02 48.55 2.88 0.052 1.20 0 6 3 71.74 142.06 2.87 0.089 1.69 -7 -5 11 143.73 10.70 2.86 0.025 0.92 -1 0 10 52.03 99.23 2.85 0.075 1.84 -2 6 6 -11.62 17.49 2.83 0.031 1.35 5 5 12 123.13 50.27 2.82 0.053 1.13 3 -7 2 -29.85 44.46 2.82 0.050 1.09 -2 7 3 2.79 104.13 2.81 0.077 1.24 -6 5 5 -17.13 25.21 2.80 0.038 0.96 -5 6 1 -22.23 32.60 2.79 0.043 1.00 1 -5 4 2020.06 1825.63 2.79 0.321 1.60 5 8 8 296.11 168.96 2.78 0.098 1.11 -5 2 2 633.10 531.97 2.77 0.173 1.38 -3 6 12 131.96 241.77 2.77 0.117 1.05 1 0 7 827.73 731.33 2.76 0.203 2.51 -6 2 1 108.59 54.25 2.73 0.055 1.18 1 2 3 1079.74 1238.63 2.72 0.264 4.21 -4 2 14 82.03 0.39 2.70 0.005 1.09 -3 -2 4 1134.06 1006.56 2.65 0.238 2.28 3 0 10 162.33 24.92 2.65 0.037 1.50 3 11 10 334.99 157.39 2.64 0.094 0.92 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.04 2.872(4) 172.9 O1B-H1B...O2A_$1 0.84 2.10 2.940(4) 175.5 O1A-H1A...O2B_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)