+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:25:41 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SOT029 in C2/c CELL 0.71073 21.241 16.179 10.732 90.00 92.64 90.00 ZERR 8.00 0.004 0.003 0.002 0.00 0.03 0.00 LATT 7 SYMM -X, Y, .5-Z SFAC C H O F UNIT 152 144 32 48 V = 3684.22 F(000) = 1744.0 Mu = 0.15 mm-1 Cell Wt = 3394.67 Rho = 1.530 L.S. 4 BOND FMAP 2 PLAN 10 OMIT 1 1 0 OMIT 2 0 0 WGHT 0.100000 FVAR 0.11669 F1 4 0.406878 -0.294343 0.474373 11.00000 0.05758 0.07951 = 0.07361 -0.04143 0.02034 0.00009 F2 4 0.446705 -0.173326 0.460480 11.00000 0.10518 0.06798 = 0.09029 0.02265 0.07004 0.03152 F3 4 0.476877 -0.252390 0.606770 11.00000 0.04503 0.07344 = 0.08651 -0.01433 0.00175 0.02608 F4 4 0.425549 0.029098 0.735410 11.00000 0.03647 0.03771 = 0.05825 0.01103 0.00326 -0.00965 F5 4 0.444930 -0.051603 0.890832 11.00000 0.03402 0.03997 = 0.05681 0.00299 -0.01119 -0.00093 F6 4 0.366219 0.032421 0.891641 11.00000 0.04146 0.03001 = 0.05924 -0.01040 0.00528 -0.00470 O1 3 0.255252 -0.267813 0.799035 11.00000 0.04958 0.02220 = 0.03346 -0.00071 0.00945 -0.00831 O2 3 0.396995 -0.122449 0.672656 11.00000 0.03215 0.02965 = 0.03949 0.00025 0.00939 0.00100 O3 3 0.308439 -0.039577 0.683728 11.00000 0.02887 0.02931 = 0.03476 0.01017 0.00407 0.00032 AFIX 83 H3 2 0.324942 -0.010823 0.631433 11.00000 -1.50000 AFIX 0 O4 3 0.324624 -0.097604 1.043467 11.00000 0.03860 0.02536 = 0.03160 -0.00358 -0.00311 0.00837 C1 1 0.282676 -0.197740 0.742268 11.00000 0.03301 0.02230 = 0.03012 0.00309 0.00423 -0.00175 AFIX 13 H1 2 0.249633 -0.163416 0.701932 11.00000 -1.20000 AFIX 0 C2 1 0.243036 -0.325956 0.699542 11.00000 0.06182 0.02768 = 0.04121 -0.00772 0.00628 -0.00862 AFIX 23 H2A 2 0.203986 -0.312431 0.653638 11.00000 -1.20000 H2B 2 0.239788 -0.381571 0.732389 11.00000 -1.20000 AFIX 0 C3 1 0.298967 -0.319346 0.614705 11.00000 0.05010 0.03114 = 0.03646 -0.00517 0.00604 0.00051 AFIX 23 H3A 2 0.330383 -0.361416 0.634564 11.00000 -1.20000 H3B 2 0.285417 -0.323881 0.527419 11.00000 -1.20000 AFIX 0 C4 1 0.323771 -0.234004 0.645306 11.00000 0.03781 0.02627 = 0.03026 -0.00064 0.00314 0.00566 C5 1 0.376286 -0.195839 0.619559 11.00000 0.03498 0.03187 = 0.03000 0.00163 0.00480 0.00609 C6 1 0.426313 -0.228105 0.539255 11.00000 0.04814 0.03856 = 0.04764 -0.00098 0.01233 0.00838 C7 1 0.354857 -0.081776 0.753707 11.00000 0.02729 0.02615 = 0.03276 0.00184 0.00373 0.00399 C8 1 0.398576 -0.018323 0.819596 11.00000 0.02950 0.02866 = 0.04361 0.00286 0.00199 0.00052 C9 1 0.321939 -0.146192 0.836783 11.00000 0.02909 0.02094 = 0.02954 0.00015 0.00389 0.00130 C10 1 0.369968 -0.199056 0.913371 11.00000 0.03734 0.02434 = 0.03365 0.00042 0.00125 0.00856 AFIX 23 H10A 2 0.411753 -0.193160 0.881608 11.00000 -1.20000 H10B 2 0.358136 -0.256947 0.909992 11.00000 -1.20000 AFIX 0 C11 1 0.368631 -0.166267 1.047689 11.00000 0.04042 0.02765 = 0.03787 -0.00007 -0.00274 0.01190 AFIX 23 H11A 2 0.354682 -0.209058 1.103401 11.00000 -1.20000 H11B 2 0.410228 -0.147869 1.076707 11.00000 -1.20000 AFIX 0 C12 1 0.280637 -0.114582 0.941208 11.00000 0.03164 0.02202 = 0.02920 0.00099 0.00123 0.00169 AFIX 13 H12 2 0.254896 -0.161415 0.966495 11.00000 -1.20000 AFIX 0 C13 1 0.235545 -0.041370 0.918633 11.00000 0.03344 0.02313 = 0.03504 0.00218 0.00326 0.00407 AFIX 23 H13A 2 0.254500 0.007779 0.956067 11.00000 -1.20000 H13B 2 0.230207 -0.031748 0.829561 11.00000 -1.20000 AFIX 0 C14 1 0.171522 -0.054305 0.971059 11.00000 0.03244 0.02297 = 0.03685 0.00305 0.00012 0.00480 C15 1 0.126192 -0.101499 0.905937 11.00000 0.04489 0.02955 = 0.04408 -0.00070 0.00014 0.00004 AFIX 43 H15 2 0.135735 -0.125587 0.830421 11.00000 -1.20000 AFIX 0 C16 1 0.067181 -0.112996 0.952133 11.00000 0.03779 0.03677 = 0.06712 0.00411 -0.00471 -0.00859 AFIX 43 H16 2 0.037422 -0.144721 0.907465 11.00000 -1.20000 AFIX 0 C17 1 0.052134 -0.078086 1.063105 11.00000 0.03415 0.04291 = 0.08553 0.00460 0.01782 -0.00021 AFIX 43 H17 2 0.012253 -0.085613 1.093579 11.00000 -1.20000 AFIX 0 C18 1 0.096112 -0.032250 1.128412 11.00000 0.05242 0.06522 = 0.06868 -0.02052 0.02584 -0.01085 AFIX 43 H18 2 0.086390 -0.009083 1.204468 11.00000 -1.20000 AFIX 0 C19 1 0.155426 -0.019841 1.082220 11.00000 0.03825 0.05516 = 0.04780 -0.01490 0.00579 -0.00930 AFIX 43 H19 2 0.184733 0.012338 1.127303 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 99SOT029 in C2/c C 0.770 H 0.320 O 0.660 F 0.640 F1 - C6 F2 - C6 F3 - C6 F4 - C8 F5 - C8 F6 - C8 O1 - C1 C2 O2 - C5 C7 O3 - C7 O4 - C12 C11 C1 - O1 C4 C9 C2 - O1 C3 C3 - C4 C2 C4 - C5 C1 C3 C5 - C4 O2 C6 C6 - F2 F3 F1 C5 C7 - O3 O2 C8 C9 C8 - F5 F4 F6 C7 C9 - C1 C10 C12 C7 C10 - C11 C9 C11 - O4 C10 C12 - O4 C13 C9 C13 - C14 C12 C14 - C19 C15 C13 C15 - C16 C14 C16 - C17 C15 C17 - C18 C16 C18 - C17 C19 C19 - C14 C18 14570 Reflections read, of which 241 rejected -27 =< h =< 27, -16 =< k =< 20, -13 =< l =< 10, Max. 2-theta = 55.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 0 6 9.38 0.30 3 5.03 -8 16 6 4.47 1.03 2 5.49 5 11 9 1.79 0.96 4 10.01 3 Inconsistent equivalents 4175 Unique reflections, of which 0 suppressed R(int) = 0.0656 R(sigma) = 0.0871 Friedel opposites merged Maximum memory for data reduction = 2302 / 48829 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3014 / 325736 wR2 = 0.1578 before cycle 1 for 4175 data and 262 / 262 parameters GooF = S = 0.858; Restrained GooF = 0.858 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11746 0.00031 2.435 OSF Mean shift/esd = 0.150 Maximum = 2.435 for OSF Max. shift = 0.001 A for C18 Max. dU = 0.000 for F2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3014 / 325736 wR2 = 0.1579 before cycle 2 for 4175 data and 262 / 262 parameters GooF = S = 0.860; Restrained GooF = 0.860 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11766 0.00032 0.640 OSF Mean shift/esd = 0.053 Maximum = 0.640 for OSF Max. shift = 0.000 A for C18 Max. dU = 0.000 for F2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3014 / 325736 wR2 = 0.1579 before cycle 3 for 4175 data and 262 / 262 parameters GooF = S = 0.860; Restrained GooF = 0.860 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11767 0.00032 0.022 OSF Mean shift/esd = 0.003 Maximum = 0.022 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for F2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3014 / 325736 wR2 = 0.1579 before cycle 4 for 4175 data and 262 / 262 parameters GooF = S = 0.860; Restrained GooF = 0.860 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11767 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for x C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C17 Largest correlation matrix elements 0.510 U13 F2 / U33 F2 0.505 U13 F2 / U11 F2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.3249 -0.0108 0.6314 83 0.820 0.000 O3 C7 H3 H1 0.2496 -0.1634 0.7019 13 0.980 0.000 C1 O1 C4 C9 H2A 0.2040 -0.3124 0.6537 23 0.970 0.000 C2 O1 C3 H2B 0.2398 -0.3816 0.7324 23 0.970 0.000 C2 O1 C3 H3A 0.3304 -0.3614 0.6345 23 0.970 0.000 C3 C4 C2 H3B 0.2854 -0.3238 0.5274 23 0.970 0.000 C3 C4 C2 H10A 0.3581 -0.2569 0.9100 23 0.970 0.000 C10 C11 C9 H10B 0.4117 -0.1932 0.8816 23 0.970 0.000 C10 C11 C9 H11A 0.3546 -0.2090 1.1034 23 0.970 0.000 C11 O4 C10 H11B 0.4102 -0.1479 1.0767 23 0.970 0.000 C11 O4 C10 H12 0.2549 -0.1614 0.9665 13 0.980 0.000 C12 O4 C13 C9 H13A 0.2545 0.0078 0.9560 23 0.970 0.000 C13 C14 C12 H13B 0.2302 -0.0318 0.8295 23 0.970 0.000 C13 C14 C12 H15 0.1358 -0.1256 0.8305 43 0.930 0.000 C15 C16 C14 H16 0.0375 -0.1448 0.9075 43 0.930 0.000 C16 C17 C15 H17 0.0123 -0.0856 1.0936 43 0.930 0.000 C17 C18 C16 H18 0.0865 -0.0091 1.2045 43 0.930 0.000 C18 C17 C19 H19 0.1848 0.0123 1.1273 43 0.930 0.000 C19 C14 C18 99SOT029 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.40685 -0.29433 0.47436 1.00000 0.05827 0.08008 0.07417 -0.04151 0.02048 0.00005 0.07031 0.00300 0.00008 0.00011 0.00017 0.00000 0.00118 0.00121 0.00131 0.00100 0.00098 0.00093 0.00057 F2 0.44669 -0.17332 0.46047 1.00000 0.10601 0.06858 0.09094 0.02268 0.07031 0.03158 0.08649 0.00431 0.00010 0.00011 0.00019 0.00000 0.00167 0.00125 0.00151 0.00106 0.00133 0.00108 0.00073 F3 0.47687 -0.25238 0.60676 1.00000 0.04576 0.07410 0.08707 -0.01432 0.00184 0.02623 0.06901 0.00326 0.00008 0.00011 0.00019 0.00000 0.00112 0.00116 0.00142 0.00099 0.00102 0.00090 0.00055 F4 0.42554 0.02909 0.73542 1.00000 0.03703 0.03822 0.05891 0.01104 0.00333 -0.00971 0.04468 0.00253 0.00007 0.00008 0.00014 0.00000 0.00091 0.00081 0.00103 0.00067 0.00076 0.00062 0.00041 F5 0.44492 -0.05160 0.89083 1.00000 0.03463 0.04046 0.05740 0.00299 -0.01112 -0.00095 0.04457 0.00241 0.00007 0.00008 0.00014 0.00000 0.00090 0.00083 0.00102 0.00068 0.00076 0.00064 0.00041 F6 0.36621 0.03242 0.89163 1.00000 0.04193 0.03050 0.05991 -0.01044 0.00535 -0.00469 0.04402 0.00241 0.00007 0.00008 0.00014 0.00000 0.00095 0.00075 0.00100 0.00064 0.00077 0.00060 0.00041 O1 0.25526 -0.26781 0.79903 1.00000 0.05015 0.02264 0.03401 -0.00073 0.00945 -0.00828 0.03537 0.00279 0.00008 0.00009 0.00015 0.00000 0.00114 0.00083 0.00099 0.00064 0.00083 0.00070 0.00043 O2 0.39698 -0.12244 0.67265 1.00000 0.03265 0.03011 0.04010 0.00029 0.00943 0.00103 0.03405 0.00281 0.00008 0.00009 0.00015 0.00000 0.00102 0.00088 0.00105 0.00070 0.00081 0.00068 0.00043 O3 0.30843 -0.03957 0.68373 1.00000 0.02940 0.02982 0.03530 0.01022 0.00416 0.00033 0.03143 0.00273 0.00007 0.00009 0.00015 0.00000 0.00097 0.00085 0.00095 0.00067 0.00076 0.00066 0.00041 H3 0.32493 -0.01082 0.63144 1.00000 0.04714 0.00000 0.00000 O4 0.32462 -0.09760 1.04347 1.00000 0.03919 0.02585 0.03211 -0.00358 -0.00310 0.00839 0.03253 0.00276 0.00008 0.00009 0.00014 0.00000 0.00106 0.00081 0.00097 0.00064 0.00080 0.00068 0.00042 C1 0.28267 -0.19775 0.74227 1.00000 0.03344 0.02284 0.03069 0.00315 0.00425 -0.00171 0.02890 0.00401 0.00011 0.00013 0.00021 0.00000 0.00140 0.00112 0.00133 0.00089 0.00107 0.00093 0.00054 H1 0.24962 -0.16344 0.70193 1.00000 0.03469 0.00000 0.00000 C2 0.24304 -0.32595 0.69956 1.00000 0.06220 0.02810 0.04188 -0.00765 0.00622 -0.00846 0.04394 0.00448 0.00014 0.00015 0.00024 0.00000 0.00198 0.00133 0.00159 0.00108 0.00139 0.00119 0.00070 H2A 0.20398 -0.31244 0.65368 1.00000 0.05273 0.00000 0.00000 H2B 0.23980 -0.38157 0.73241 1.00000 0.05273 0.00000 0.00000 C3 0.29894 -0.31933 0.61471 1.00000 0.05069 0.03166 0.03687 -0.00514 0.00604 0.00059 0.03962 0.00439 0.00012 0.00015 0.00024 0.00000 0.00177 0.00133 0.00148 0.00106 0.00128 0.00113 0.00064 H3A 0.33035 -0.36141 0.63453 1.00000 0.04754 0.00000 0.00000 H3B 0.28537 -0.32385 0.52743 1.00000 0.04754 0.00000 0.00000 C4 0.32375 -0.23402 0.64532 1.00000 0.03839 0.02675 0.03068 -0.00059 0.00315 0.00571 0.03189 0.00425 0.00012 0.00013 0.00022 0.00000 0.00157 0.00123 0.00137 0.00093 0.00114 0.00102 0.00058 C5 0.37627 -0.19583 0.61954 1.00000 0.03546 0.03227 0.03046 0.00164 0.00479 0.00606 0.03263 0.00439 0.00012 0.00014 0.00022 0.00000 0.00151 0.00126 0.00137 0.00099 0.00113 0.00106 0.00057 C6 0.42627 -0.22809 0.53927 1.00000 0.04883 0.03896 0.04814 -0.00090 0.01232 0.00852 0.04500 0.00523 0.00014 0.00015 0.00027 0.00000 0.00184 0.00150 0.00176 0.00124 0.00144 0.00127 0.00070 C7 0.35484 -0.08177 0.75372 1.00000 0.02775 0.02661 0.03326 0.00185 0.00371 0.00404 0.02914 0.00414 0.00011 0.00013 0.00022 0.00000 0.00138 0.00120 0.00139 0.00092 0.00110 0.00093 0.00055 C8 0.39855 -0.01832 0.81959 1.00000 0.02993 0.02910 0.04409 0.00292 0.00199 0.00064 0.03437 0.00434 0.00012 0.00014 0.00024 0.00000 0.00147 0.00129 0.00156 0.00104 0.00123 0.00104 0.00059 C9 0.32192 -0.14617 0.83679 1.00000 0.02949 0.02150 0.02997 0.00014 0.00388 0.00133 0.02691 0.00388 0.00011 0.00013 0.00021 0.00000 0.00138 0.00112 0.00133 0.00086 0.00107 0.00091 0.00053 C10 0.36992 -0.19906 0.91337 1.00000 0.03781 0.02485 0.03422 0.00048 0.00140 0.00861 0.03230 0.00426 0.00012 0.00014 0.00022 0.00000 0.00154 0.00117 0.00141 0.00094 0.00114 0.00097 0.00058 H10A 0.35806 -0.25694 0.91000 1.00000 0.03876 0.00000 0.00000 H10B 0.41171 -0.19319 0.88161 1.00000 0.03876 0.00000 0.00000 C11 0.36860 -0.16626 1.04768 1.00000 0.04100 0.02808 0.03844 -0.00004 -0.00277 0.01190 0.03598 0.00444 0.00012 0.00013 0.00023 0.00000 0.00162 0.00126 0.00149 0.00099 0.00122 0.00104 0.00062 H11A 0.35465 -0.20904 1.10340 1.00000 0.04318 0.00000 0.00000 H11B 0.41020 -0.14787 1.07669 1.00000 0.04318 0.00000 0.00000 C12 0.28062 -0.11457 0.94121 1.00000 0.03213 0.02249 0.02968 0.00100 0.00114 0.00161 0.02811 0.00400 0.00011 0.00012 0.00021 0.00000 0.00142 0.00114 0.00133 0.00087 0.00110 0.00093 0.00054 H12 0.25487 -0.16140 0.96649 1.00000 0.03373 0.00000 0.00000 C13 0.23558 -0.04138 0.91862 1.00000 0.03392 0.02360 0.03558 0.00218 0.00332 0.00405 0.03098 0.00425 0.00011 0.00013 0.00023 0.00000 0.00150 0.00114 0.00141 0.00093 0.00112 0.00094 0.00057 H13A 0.25454 0.00777 0.95604 1.00000 0.03718 0.00000 0.00000 H13B 0.23024 -0.03177 0.82954 1.00000 0.03718 0.00000 0.00000 C14 0.17155 -0.05429 0.97105 1.00000 0.03294 0.02340 0.03733 0.00308 0.00013 0.00485 0.03127 0.00416 0.00011 0.00013 0.00023 0.00000 0.00147 0.00115 0.00145 0.00096 0.00116 0.00097 0.00057 C15 0.12625 -0.10151 0.90596 1.00000 0.04515 0.03009 0.04468 -0.00069 0.00019 0.00008 0.04003 0.00462 0.00013 0.00014 0.00025 0.00000 0.00174 0.00132 0.00164 0.00107 0.00136 0.00110 0.00065 H15 0.13581 -0.12561 0.83047 1.00000 0.04804 0.00000 0.00000 C16 0.06724 -0.11302 0.95214 1.00000 0.03858 0.03725 0.06751 0.00415 -0.00464 -0.00861 0.04800 0.00501 0.00013 0.00015 0.00029 0.00000 0.00173 0.00149 0.00209 0.00131 0.00152 0.00119 0.00074 H16 0.03750 -0.14476 0.90746 1.00000 0.05760 0.00000 0.00000 C17 0.05216 -0.07810 1.06315 1.00000 0.03473 0.04349 0.08616 0.00468 0.01791 -0.00010 0.05433 0.00570 0.00014 0.00017 0.00032 0.00000 0.00172 0.00166 0.00247 0.00151 0.00168 0.00123 0.00083 H17 0.01228 -0.08562 1.09363 1.00000 0.06519 0.00000 0.00000 C18 0.09618 -0.03225 1.12844 1.00000 0.05318 0.06577 0.06914 -0.02072 0.02595 -0.01111 0.06198 0.00564 0.00015 0.00019 0.00032 0.00000 0.00213 0.00203 0.00222 0.00161 0.00179 0.00156 0.00091 H18 0.08648 -0.00907 1.20450 1.00000 0.07438 0.00000 0.00000 C19 0.15548 -0.01985 1.08222 1.00000 0.03871 0.05559 0.04851 -0.01487 0.00587 -0.00932 0.04748 0.00482 0.00013 0.00017 0.00027 0.00000 0.00173 0.00167 0.00178 0.00130 0.00140 0.00128 0.00072 H19 0.18480 0.01232 1.12730 1.00000 0.05698 0.00000 0.00000 Final Structure Factor Calculation for 99SOT029 in C2/c Total number of l.s. parameters = 262 Maximum vector length = 511 Memory required = 2752 / 22995 wR2 = 0.1579 before cycle 5 for 4175 data and 0 / 262 parameters GooF = S = 0.860; Restrained GooF = 0.860 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0499 for 2262 Fo > 4sig(Fo) and 0.1220 for all 4175 data wR2 = 0.1579, GooF = S = 0.860, Restrained GooF = 0.860 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.1204 0.0620 0.0284 F1 0.1752 0.0558 0.0285 F2 0.1024 0.0756 0.0290 F3 0.0642 0.0446 0.0253 F4 0.0645 0.0400 0.0291 F5 0.0639 0.0417 0.0265 F6 0.0547 0.0312 0.0201 O1 0.0447 0.0303 0.0272 O2 0.0434 0.0293 0.0216 O3 0.0460 0.0300 0.0216 O4 0.0350 0.0306 0.0211 C1 0.0653 0.0428 0.0238 C2 0.0516 0.0391 0.0281 C3 0.0408 0.0307 0.0241 C4 0.0411 0.0295 0.0272 C5 0.0597 0.0441 0.0312 C6 0.0352 0.0291 0.0231 C7 0.0446 0.0301 0.0284 C8 0.0322 0.0272 0.0213 C9 0.0421 0.0342 0.0205 C10 0.0498 0.0374 0.0208 C11 0.0324 0.0298 0.0221 C12 0.0377 0.0331 0.0221 C13 0.0381 0.0350 0.0208 C14 0.0469 0.0431 0.0301 C15 0.0707 0.0440 0.0292 C16 0.0901 0.0432 0.0297 C17 0.1000 0.0509 0.0350 C18 0.0699 0.0387 0.0338 C19 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.013 0.020 0.028 0.037 0.048 0.064 0.087 0.136 1.000 Number in group 420. 438. 395. 432. 434. 401. 419. 407. 414. 415. GooF 0.794 0.764 0.806 0.919 0.995 0.990 0.988 0.832 0.784 0.658 K 6.834 1.387 1.103 1.020 0.949 1.030 1.013 0.997 1.015 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 429. 426. 410. 413. 416. 410. 421. 417. 414. 419. GooF 0.823 0.762 0.873 0.805 0.874 0.885 0.844 0.822 0.929 0.969 K 1.099 1.069 1.102 1.042 1.006 0.992 1.018 1.019 1.038 0.987 R1 0.415 0.353 0.304 0.222 0.180 0.104 0.062 0.056 0.048 0.034 Recommended weighting scheme: WGHT 0.0621 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) 0 6 0 122.06 261.08 3.80 0.045 2.70 -13 13 4 362.25 181.88 3.72 0.037 0.94 0 10 0 169.01 372.54 3.57 0.054 1.62 -11 5 8 204.97 96.73 3.39 0.027 1.06 2 8 4 92.29 170.34 3.37 0.036 1.59 -4 2 4 179.85 120.56 3.32 0.030 2.33 5 11 10 -19.07 149.77 3.29 0.034 0.84 -5 5 8 158.53 287.89 3.25 0.047 1.20 -10 4 3 294.22 195.93 3.25 0.039 1.69 6 0 10 -8.23 171.13 3.24 0.036 1.01 5 7 2 422.23 308.69 3.23 0.049 1.88 -10 10 6 -17.60 74.66 3.19 0.024 1.06 2 10 0 146.76 222.31 3.14 0.041 1.60 -5 13 5 432.60 288.73 3.12 0.047 1.05 9 3 4 1203.64 903.94 3.12 0.083 1.65 -3 1 1 203.38 274.78 3.04 0.046 5.65 -14 12 2 101.81 0.00 3.03 0.000 1.00 6 6 1 875.63 1152.96 3.00 0.094 2.09 18 4 8 789.25 349.49 3.00 0.052 0.85 -18 0 10 3370.12 2038.17 2.99 0.125 0.81 -13 1 6 228.02 105.94 2.98 0.029 1.23 10 4 9 529.25 318.44 2.94 0.049 0.99 12 4 1 801.71 1067.81 2.89 0.091 1.59 2 12 1 248.70 430.71 2.88 0.058 1.33 3 3 2 2482.50 3205.46 2.84 0.157 3.30 -6 8 3 308.81 226.19 2.81 0.042 1.59 -2 8 1 84.01 53.51 2.81 0.020 1.96 5 13 6 415.30 587.24 2.80 0.067 0.99 -3 7 9 199.50 334.74 2.79 0.051 1.05 -15 13 5 332.92 532.84 2.77 0.064 0.87 -7 3 4 263.70 186.54 2.77 0.038 1.92 -17 7 5 -26.23 67.54 2.77 0.023 0.99 0 18 6 758.39 338.86 2.76 0.051 0.80 -18 8 2 639.83 401.30 2.76 0.056 1.01 6 0 12 582.15 139.44 2.75 0.033 0.86 7 5 0 63.97 31.10 2.75 0.015 2.21 1 7 0 376.67 495.10 2.74 0.062 2.30 -12 18 3 -90.28 234.43 2.71 0.042 0.79 -5 7 3 528.85 407.10 2.71 0.056 1.78 1 9 4 61.55 17.61 2.71 0.012 1.49 -4 8 7 84.62 149.41 2.70 0.034 1.20 1 9 3 564.82 725.31 2.70 0.075 1.60 8 2 2 255.13 178.42 2.70 0.037 2.24 0 6 5 995.44 784.60 2.70 0.078 1.68 4 2 4 159.54 228.71 2.69 0.042 2.26 -7 7 2 310.20 231.31 2.68 0.042 1.75 -12 4 1 133.22 220.11 2.68 0.041 1.61 0 2 4 892.05 1133.55 2.65 0.093 2.54 -9 13 3 -8.25 51.80 2.64 0.020 1.06 -12 12 9 490.28 290.09 2.63 0.047 0.81 Bond lengths and angles F1 - Distance Angles C6 1.3332 (0.0031) F1 - F2 - Distance Angles C6 1.3123 (0.0031) F2 - F3 - Distance Angles C6 1.3275 (0.0033) F3 - F4 - Distance Angles C8 1.3345 (0.0027) F4 - F5 - Distance Angles C8 1.3323 (0.0027) F5 - F6 - Distance Angles C8 1.3388 (0.0027) F6 - O1 - Distance Angles C1 1.4238 (0.0026) C2 1.4375 (0.0028) 105.47 (0.17) O1 - C1 O2 - Distance Angles C5 1.3804 (0.0028) C7 1.4363 (0.0027) 116.64 (0.18) O2 - C5 O3 - Distance Angles C7 1.3908 (0.0027) O3 - O4 - Distance Angles C12 1.4348 (0.0028) C11 1.4508 (0.0026) 105.85 (0.16) O4 - C12 C1 - Distance Angles O1 1.4238 (0.0026) C4 1.5073 (0.0032) 104.27 (0.17) C9 1.5306 (0.0031) 111.81 (0.18) 110.77 (0.19) C1 - O1 C4 C2 - Distance Angles O1 1.4375 (0.0028) C3 1.5330 (0.0037) 106.08 (0.20) C2 - O1 C3 - Distance Angles C4 1.5083 (0.0033) C2 1.5330 (0.0037) 101.95 (0.19) C3 - C4 C4 - Distance Angles C5 1.3157 (0.0034) C1 1.5073 (0.0032) 119.06 (0.21) C3 1.5083 (0.0033) 132.46 (0.22) 107.40 (0.20) C4 - C5 C1 C5 - Distance Angles C4 1.3157 (0.0034) O2 1.3804 (0.0028) 125.05 (0.21) C6 1.4924 (0.0036) 126.17 (0.23) 108.50 (0.21) C5 - C4 O2 C6 - Distance Angles F2 1.3123 (0.0031) F3 1.3275 (0.0033) 105.56 (0.25) F1 1.3332 (0.0031) 108.03 (0.24) 105.68 (0.21) C5 1.4924 (0.0036) 113.65 (0.21) 111.61 (0.23) 111.80 (0.24) C6 - F2 F3 F1 C7 - Distance Angles O3 1.3908 (0.0027) O2 1.4363 (0.0027) 110.11 (0.18) C8 1.5346 (0.0033) 108.61 (0.18) 101.82 (0.18) C9 1.5577 (0.0030) 108.16 (0.18) 110.43 (0.17) 117.50 (0.19) C7 - O3 O2 C8 C8 - Distance Angles F5 1.3323 (0.0027) F4 1.3345 (0.0027) 106.94 (0.19) F6 1.3388 (0.0027) 107.57 (0.20) 106.63 (0.18) C7 1.5346 (0.0033) 114.18 (0.19) 110.02 (0.20) 111.14 (0.19) C8 - F5 F4 F6 C9 - Distance Angles C1 1.5306 (0.0031) C10 1.5395 (0.0031) 112.21 (0.18) C12 1.5419 (0.0031) 110.59 (0.19) 100.44 (0.17) C7 1.5577 (0.0030) 103.33 (0.17) 111.94 (0.19) 118.66 (0.17) C9 - C1 C10 C12 C10 - Distance Angles C11 1.5374 (0.0033) C9 1.5395 (0.0031) 105.57 (0.18) C10 - C11 C11 - Distance Angles O4 1.4508 (0.0026) C10 1.5374 (0.0033) 105.94 (0.18) C11 - O4 C12 - Distance Angles O4 1.4348 (0.0028) C13 1.5346 (0.0030) 110.64 (0.17) C9 1.5419 (0.0031) 104.30 (0.18) 120.83 (0.19) C12 - O4 C13 C13 - Distance Angles C14 1.5101 (0.0034) C12 1.5346 (0.0030) 113.58 (0.18) C13 - C14 C14 - Distance Angles C19 1.3741 (0.0035) C15 1.3912 (0.0035) 117.71 (0.24) C13 1.5101 (0.0034) 122.10 (0.23) 120.18 (0.22) C14 - C19 C15 C15 - Distance Angles C16 1.3815 (0.0037) C14 1.3912 (0.0035) 120.79 (0.25) C15 - C16 C16 - Distance Angles C17 1.3699 (0.0042) C15 1.3815 (0.0037) 120.58 (0.27) C16 - C17 C17 - Distance Angles C18 1.3620 (0.0043) C16 1.3699 (0.0042) 119.31 (0.28) C17 - C18 C18 - Distance Angles C17 1.3620 (0.0043) C19 1.3894 (0.0040) 120.48 (0.29) C18 - C17 C19 - Distance Angles C14 1.3741 (0.0035) C18 1.3894 (0.0040) 121.12 (0.26) C19 - C14 FMAP and GRID set by program FMAP 2 2 20 GRID -1.471 -2 -1 1.471 2 1 R1 = 0.1219 for 4175 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.3358 0.1145 0.3032 [ 0.70 A from C9 ] Deepest hole -0.33 at 0.4821 0.1557 0.0198 [ 1.00 A from F2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3073 / 32248 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3358 -0.1145 0.8032 1.00000 0.05 0.27 0.70 C9 0.86 C7 1.84 O3 1.86 C1 Q2 1 0.4822 -0.2106 0.5351 1.00000 0.05 0.24 1.03 F3 1.22 C6 1.23 F2 2.17 F1 Q3 1 0.4050 -0.2348 0.4367 1.00000 0.05 0.23 1.04 F1 1.18 C6 1.35 F2 2.18 C5 Q4 1 0.4198 -0.1946 0.3900 1.00000 0.05 0.21 0.99 F2 1.69 C6 1.88 F1 2.65 H2A Q5 1 0.3004 -0.1264 0.8738 1.00000 0.05 0.20 0.70 C9 0.87 C12 1.53 H12 1.85 C1 Q6 1 0.3990 -0.1919 0.4310 1.00000 0.05 0.18 1.09 F2 1.40 C6 1.73 F1 2.10 C5 Q7 1 0.3075 -0.2205 0.6820 1.00000 0.05 0.18 0.58 C4 0.93 C1 1.56 H1 1.68 C5 Q8 1 0.3689 -0.2209 0.6550 1.00000 0.05 0.17 0.58 C5 0.98 C4 1.71 O2 1.78 C6 Q9 1 0.0579 -0.0725 0.9850 1.00000 0.05 0.17 0.77 C16 0.86 C17 1.49 H16 1.56 H17 Q10 1 0.4787 0.0445 0.6558 1.00000 0.05 0.17 1.47 F4 2.31 F4 2.32 F5 2.35 H11B Shortest distances between peaks (including symmetry equivalents) 4 6 0.64 3 6 0.71 3 4 0.89 1 5 1.11 7 8 1.35 2 3 1.95 2 4 2.01 2 6 2.07 10 10 2.18 1 7 2.22 1 8 2.47 3 8 2.51 6 8 2.56 5 7 2.57 2 8 2.78 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 2.08: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.63: Structure factors and derivatives 2.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:25:48 Total CPU time: 7.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++