+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:09:10 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SOT036 in P2(1)/c CELL 0.71073 9.2288 20.3616 7.6375 90.000 91.003 90.000 ZERR 4.00 0.0018 0.0041 0.0015 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O F UNIT 64 68 8 12 V = 1434.97 F(000) = 624.0 Mu = 0.12 mm-1 Cell Wt = 1193.18 Rho = 1.381 L.S. 4 BOND FMAP 2 PLAN 10 OMIT -3 55 OMIT -2 9 1 OMIT -1 7 3 SIZE 0.25 0.2 0.05 WGHT 0.100000 FVAR 0.53018 F1 4 0.659841 0.279174 0.511855 11.00000 0.06821 0.03135 = 0.04690 -0.00683 -0.00119 -0.00670 F2 4 0.558000 0.351851 0.347213 11.00000 0.03677 0.06148 = 0.04199 -0.01076 -0.00990 -0.00052 F3 4 0.778479 0.325596 0.307666 11.00000 0.04149 0.06678 = 0.03564 -0.01562 0.00143 0.00274 O1 3 0.434959 0.491672 0.774708 11.00000 0.03969 0.03424 = 0.03391 0.00061 0.00288 0.01013 O2 3 0.771317 0.445583 0.459042 11.00000 0.03482 0.03718 = 0.03851 0.01253 -0.00004 0.00056 AFIX 83 H2 2 0.704416 0.457543 0.394559 11.00000 -1.50000 AFIX 0 C1 1 0.597413 0.407486 0.674954 11.00000 0.03120 0.03152 = 0.02722 0.00241 -0.00259 -0.00055 C2 1 0.526478 0.355243 0.784039 11.00000 0.03691 0.03409 = 0.04145 0.00556 0.00434 -0.00219 AFIX 23 H2A 2 0.599683 0.325979 0.832715 11.00000 -1.20000 H2B 2 0.460545 0.329515 0.711369 11.00000 -1.20000 AFIX 0 C3 1 0.443891 0.387570 0.930815 11.00000 0.04126 0.03973 = 0.03510 0.00306 0.00587 -0.00236 AFIX 23 H3A 2 0.384153 0.355131 0.988221 11.00000 -1.20000 H3B 2 0.511787 0.405232 1.017012 11.00000 -1.20000 AFIX 0 C4 1 0.350150 0.441671 0.859819 11.00000 0.03668 0.04768 = 0.03893 0.00072 0.00633 0.00438 AFIX 23 H4A 2 0.280418 0.423569 0.776470 11.00000 -1.20000 H4B 2 0.296860 0.461357 0.954769 11.00000 -1.20000 AFIX 0 C5 1 0.552159 0.469263 0.684211 11.00000 0.03326 0.02960 = 0.03049 0.00166 0.00086 0.00207 AFIX 43 H5 2 0.605117 0.500406 0.623365 11.00000 -1.20000 AFIX 0 C6 1 0.726112 0.391351 0.560049 11.00000 0.03204 0.02727 = 0.03027 0.00368 0.00016 -0.00115 C7 1 0.681481 0.337017 0.430983 11.00000 0.03323 0.04356 = 0.03055 -0.00362 0.00008 0.00419 C8 1 0.859141 0.369837 0.674611 11.00000 0.03184 0.02842 = 0.03453 0.00227 -0.00131 0.00110 AFIX 13 H8 2 0.828185 0.331759 0.742952 11.00000 -1.20000 AFIX 0 C9 1 0.899120 0.422923 0.804356 11.00000 0.03839 0.03864 = 0.03798 -0.00501 -0.00714 0.00092 AFIX 43 H9 2 0.918104 0.464776 0.761735 11.00000 -1.20000 AFIX 0 C10 1 0.908560 0.413388 0.973200 11.00000 0.05986 0.05643 = 0.04111 -0.00383 -0.00731 -0.00060 AFIX 93 H10A 2 0.890150 0.372023 1.019403 11.00000 -1.20000 H10B 2 0.933696 0.447962 1.047279 11.00000 -1.20000 AFIX 0 C11 1 0.989185 0.347966 0.570522 11.00000 0.02934 0.03323 = 0.03253 -0.00342 -0.00328 -0.00005 C12 1 1.026834 0.282123 0.570585 11.00000 0.03613 0.03914 = 0.04229 0.00256 -0.00084 0.00728 AFIX 43 H12 2 0.971940 0.252289 0.633475 11.00000 -1.20000 AFIX 0 C13 1 1.145450 0.260084 0.477989 11.00000 0.04187 0.05435 = 0.06411 -0.00523 -0.00143 0.01552 AFIX 43 H13 2 1.167959 0.215569 0.476664 11.00000 -1.20000 AFIX 0 C14 1 1.229468 0.303788 0.388509 11.00000 0.02736 0.07156 = 0.05340 -0.01259 0.00166 0.00291 AFIX 43 H14 2 1.309899 0.289096 0.328160 11.00000 -1.20000 AFIX 0 C15 1 1.194550 0.369217 0.388269 11.00000 0.03390 0.06521 = 0.05031 -0.00914 0.00687 -0.01522 AFIX 43 H15 2 1.250929 0.398852 0.326650 11.00000 -1.20000 AFIX 0 C16 1 1.075360 0.391457 0.479624 11.00000 0.03773 0.04062 = 0.04751 -0.00316 0.00153 -0.00522 AFIX 43 H16 2 1.053186 0.436012 0.479762 11.00000 -1.20000 HKLF 4 1 0 0 1 0 -1 0 1 0 0 Covalent radii and connectivity table for 00SOT036 in P2(1)/c C 0.770 H 0.320 O 0.660 F 0.640 F1 - C7 F2 - C7 F3 - C7 O1 - C5 C4 O2 - C6 C1 - C5 C2 C6 C2 - C1 C3 C3 - C4 C2 C4 - O1 C3 C5 - C1 O1 C6 - O2 C1 C7 C8 C7 - F3 F2 F1 C6 C8 - C9 C11 C6 C9 - C10 C8 C10 - C9 C11 - C16 C12 C8 C12 - C11 C13 C13 - C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C11 C15 h k l Fo^2 Sigma Why rejected -3 0 3 4.13 0.87 observed but should be systematically absent -1 0 1 1.52 0.33 observed but should be systematically absent -1 0 1 1.41 0.32 observed but should be systematically absent -2 0 1 9.31 1.69 observed but should be systematically absent -2 0 1 4.88 0.74 observed but should be systematically absent -2 0 1 3.27 0.53 observed but should be systematically absent -6 0 1 4.70 1.07 observed but should be systematically absent 0 3 0 1.72 0.22 observed but should be systematically absent 1 0 1 1.96 0.33 observed but should be systematically absent 1 0 1 1.97 0.33 observed but should be systematically absent 1 0 1 1.77 0.44 observed but should be systematically absent 1 0 1 1.87 0.44 observed but should be systematically absent 2 0 3 2.71 0.54 observed but should be systematically absent 2 0 3 3.56 0.89 observed but should be systematically absent 14575 Reflections read, of which 982 rejected -11 =< h =< 11, -26 =< k =< 26, -9 =< l =< 9, Max. 2-theta = 55.00 14 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 1 0 14.42 0.52 5 2.94 -1 1 1 32.57 0.77 4 6.50 2 1 1 12.43 0.44 4 2.88 0 3 1 3073.74 71.22 3 619.32 -2 7 1 9.91 0.34 4 2.92 1 7 1 11.76 0.39 6 2.01 -1 13 1 7.20 0.40 5 2.18 3 2 2 27.01 0.56 5 9.68 -1 3 2 2.72 0.20 3 1.18 3 4 2 14.15 0.63 3 4.53 1 6 2 31.54 0.56 7 5.29 0 8 2 5.98 0.36 5 1.81 0 9 2 10.06 0.44 5 2.34 3 3 3 14.56 0.43 7 2.95 0 4 3 43.23 1.78 2 13.95 -4 5 3 16.21 1.25 2 8.44 -3 5 3 4.98 0.46 2 2.55 1 5 3 44.25 1.04 6 5.61 1 6 3 49.46 0.91 7 4.76 -2 7 3 10.12 0.43 3 3.58 -1 3 4 12.59 0.52 3 4.22 4 3 4 15.05 0.59 6 3.17 -1 4 5 85.36 1.05 6 9.28 -4 2 6 57.83 2.63 2 17.37 24 Inconsistent equivalents 3244 Unique reflections, of which 0 suppressed R(int) = 0.0734 R(sigma) = 0.0550 Friedel opposites merged Maximum memory for data reduction = 1861 / 31806 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 = 2399 / 235700 wR2 = 0.1778 before cycle 1 for 3244 data and 190 / 190 parameters GooF = S = 1.139; Restrained GooF = 1.139 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 0.52983 0.00192 -0.181 OSF Mean shift/esd = 0.153 Maximum = 0.536 for y C5 Max. shift = 0.001 A for C15 Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2399 / 235700 wR2 = 0.1775 before cycle 2 for 3244 data and 190 / 190 parameters GooF = S = 1.136; Restrained GooF = 1.136 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 0.52974 0.00192 -0.051 OSF Mean shift/esd = 0.055 Maximum = -0.211 for y C15 Max. shift = 0.001 A for C15 Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2399 / 235700 wR2 = 0.1774 before cycle 3 for 3244 data and 190 / 190 parameters GooF = S = 1.136; Restrained GooF = 1.136 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 0.52974 0.00192 0.000 OSF Mean shift/esd = 0.004 Maximum = 0.021 for U23 F2 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2399 / 235700 wR2 = 0.1774 before cycle 4 for 3244 data and 190 / 190 parameters GooF = S = 1.136; Restrained GooF = 1.136 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 0.52973 0.00192 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U33 C3 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7044 0.4575 0.3946 83 0.820 0.000 O2 C6 H2 H2A 0.5996 0.3260 0.8328 23 0.970 0.000 C2 C1 C3 H2B 0.4605 0.3296 0.7114 23 0.970 0.000 C2 C1 C3 H3A 0.3841 0.3551 0.9881 23 0.970 0.000 C3 C4 C2 H3B 0.5118 0.4052 1.0170 23 0.970 0.000 C3 C4 C2 H4A 0.2806 0.4236 0.7763 23 0.970 0.000 C4 O1 C3 H4B 0.2969 0.4614 0.9546 23 0.970 0.000 C4 O1 C3 H5 0.6051 0.5005 0.6235 43 0.930 0.000 C5 C1 O1 H8 0.8282 0.3317 0.7429 13 0.980 0.000 C8 C9 C11 C6 H9 0.9181 0.4648 0.7617 43 0.930 0.000 C9 C10 C8 H10A 0.8901 0.3721 1.0195 93 0.930 0.000 C10 C9 C8 H10B 0.9336 0.4481 1.0473 93 0.930 0.000 C10 C9 C8 H12 0.9720 0.2523 0.6336 43 0.930 0.000 C12 C11 C13 H13 1.1680 0.2155 0.4767 43 0.930 0.000 C13 C14 C12 H14 1.3099 0.2892 0.3282 43 0.930 0.000 C14 C15 C13 H15 1.2510 0.3987 0.3266 43 0.930 0.000 C15 C14 C16 H16 1.0531 0.4360 0.4797 43 0.930 0.000 C16 C11 C15 00SOT036 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.65974 0.27918 0.51197 1.00000 0.06811 0.03133 0.04693 -0.00681 -0.00128 -0.00677 0.04882 0.00211 0.00015 0.00005 0.00017 0.00000 0.00095 0.00062 0.00075 0.00053 0.00063 0.00057 0.00038 F2 0.55803 0.35186 0.34722 1.00000 0.03664 0.06115 0.04192 -0.01053 -0.00975 -0.00084 0.04669 0.00198 0.00014 0.00006 0.00016 0.00000 0.00070 0.00081 0.00072 0.00059 0.00054 0.00056 0.00037 F3 0.77844 0.32558 0.30770 1.00000 0.04128 0.06670 0.03565 -0.01536 0.00134 0.00251 0.04787 0.00214 0.00014 0.00007 0.00016 0.00000 0.00072 0.00086 0.00067 0.00058 0.00054 0.00061 0.00037 O1 0.43497 0.49164 0.77463 1.00000 0.03952 0.03468 0.03397 0.00055 0.00255 0.01030 0.03604 0.00242 0.00015 0.00006 0.00018 0.00000 0.00082 0.00072 0.00074 0.00057 0.00060 0.00057 0.00036 O2 0.77129 0.44558 0.45906 1.00000 0.03490 0.03667 0.03854 0.01263 0.00000 0.00062 0.03671 0.00243 0.00015 0.00006 0.00018 0.00000 0.00077 0.00071 0.00078 0.00059 0.00059 0.00057 0.00037 H2 0.70437 0.45753 0.39460 1.00000 0.05506 0.00000 0.00000 C1 0.59743 0.40742 0.67499 1.00000 0.03081 0.03148 0.02731 0.00242 -0.00271 -0.00037 0.02990 0.00315 0.00021 0.00009 0.00024 0.00000 0.00099 0.00094 0.00095 0.00073 0.00074 0.00075 0.00043 C2 0.52641 0.35528 0.78407 1.00000 0.03684 0.03405 0.04151 0.00523 0.00427 -0.00184 0.03743 0.00377 0.00024 0.00009 0.00028 0.00000 0.00114 0.00099 0.00112 0.00085 0.00089 0.00082 0.00048 H2A 0.59956 0.32599 0.83275 1.00000 0.04491 0.00000 0.00000 H2B 0.46045 0.32957 0.71140 1.00000 0.04491 0.00000 0.00000 C3 0.44388 0.38757 0.93080 1.00000 0.04115 0.04011 0.03523 0.00305 0.00579 -0.00230 0.03877 0.00373 0.00023 0.00010 0.00027 0.00000 0.00118 0.00109 0.00109 0.00086 0.00086 0.00087 0.00049 H3A 0.38408 0.35513 0.98814 1.00000 0.04653 0.00000 0.00000 H3B 0.51175 0.40521 1.01705 1.00000 0.04653 0.00000 0.00000 C4 0.35026 0.44168 0.85966 1.00000 0.03682 0.04701 0.03900 0.00076 0.00646 0.00434 0.04087 0.00393 0.00024 0.00011 0.00029 0.00000 0.00114 0.00116 0.00115 0.00093 0.00088 0.00091 0.00050 H4A 0.28056 0.42357 0.77628 1.00000 0.04905 0.00000 0.00000 H4B 0.29691 0.46137 0.95455 1.00000 0.04905 0.00000 0.00000 C5 0.55214 0.46933 0.68425 1.00000 0.03342 0.02962 0.03023 0.00173 0.00073 0.00229 0.03109 0.00325 0.00021 0.00009 0.00024 0.00000 0.00104 0.00093 0.00097 0.00075 0.00076 0.00075 0.00043 H5 0.60512 0.50049 0.62349 1.00000 0.03731 0.00000 0.00000 C6 0.72612 0.39138 0.56014 1.00000 0.03184 0.02765 0.03044 0.00379 0.00002 -0.00110 0.02998 0.00316 0.00020 0.00009 0.00025 0.00000 0.00101 0.00090 0.00097 0.00073 0.00074 0.00072 0.00043 C7 0.68154 0.33701 0.43093 1.00000 0.03319 0.04278 0.03052 -0.00359 0.00018 0.00423 0.03550 0.00346 0.00022 0.00010 0.00026 0.00000 0.00108 0.00111 0.00103 0.00082 0.00081 0.00084 0.00048 C8 0.85912 0.36978 0.67461 1.00000 0.03170 0.02837 0.03458 0.00225 -0.00127 0.00142 0.03157 0.00329 0.00021 0.00009 0.00025 0.00000 0.00104 0.00090 0.00102 0.00078 0.00079 0.00074 0.00044 H8 0.82819 0.33169 0.74294 1.00000 0.03789 0.00000 0.00000 C9 0.89912 0.42299 0.80439 1.00000 0.03825 0.03858 0.03807 -0.00516 -0.00710 0.00130 0.03839 0.00339 0.00023 0.00010 0.00028 0.00000 0.00114 0.00107 0.00116 0.00089 0.00086 0.00087 0.00049 H9 0.91810 0.46483 0.76169 1.00000 0.04607 0.00000 0.00000 C10 0.90853 0.41348 0.97322 1.00000 0.05986 0.05605 0.04128 -0.00402 -0.00729 0.00004 0.05249 0.00423 0.00028 0.00013 0.00032 0.00000 0.00159 0.00139 0.00131 0.00105 0.00111 0.00116 0.00062 H10A 0.89011 0.37212 1.01946 1.00000 0.06299 0.00000 0.00000 H10B 0.93364 0.44807 1.04727 1.00000 0.06299 0.00000 0.00000 C11 0.98920 0.34802 0.57051 1.00000 0.02934 0.03335 0.03273 -0.00356 -0.00344 0.00041 0.03185 0.00313 0.00021 0.00009 0.00025 0.00000 0.00104 0.00096 0.00104 0.00077 0.00079 0.00075 0.00045 C12 1.02685 0.28210 0.57066 1.00000 0.03596 0.03844 0.04273 0.00283 -0.00092 0.00735 0.03906 0.00389 0.00023 0.00010 0.00029 0.00000 0.00114 0.00105 0.00119 0.00087 0.00088 0.00085 0.00049 H12 0.97196 0.25228 0.63360 1.00000 0.04688 0.00000 0.00000 C13 1.14543 0.26004 0.47806 1.00000 0.04184 0.05453 0.06377 -0.00518 -0.00194 0.01539 0.05341 0.00457 0.00026 0.00013 0.00036 0.00000 0.00136 0.00135 0.00158 0.00120 0.00113 0.00109 0.00063 H13 1.16797 0.21553 0.47667 1.00000 0.06410 0.00000 0.00000 C14 1.22945 0.30387 0.38856 1.00000 0.02717 0.07143 0.05344 -0.01249 0.00185 0.00255 0.05067 0.00402 0.00024 0.00013 0.00034 0.00000 0.00117 0.00163 0.00140 0.00121 0.00099 0.00106 0.00061 H14 1.30993 0.28922 0.32824 1.00000 0.06080 0.00000 0.00000 C15 1.19460 0.36912 0.38826 1.00000 0.03369 0.06555 0.05044 -0.00917 0.00681 -0.01498 0.04982 0.00391 0.00025 0.00013 0.00032 0.00000 0.00118 0.00150 0.00131 0.00115 0.00096 0.00107 0.00059 H15 1.25099 0.39874 0.32663 1.00000 0.05979 0.00000 0.00000 C16 1.07524 0.39143 0.47966 1.00000 0.03773 0.03991 0.04774 -0.00324 0.00186 -0.00515 0.04178 0.00366 0.00023 0.00011 0.00030 0.00000 0.00117 0.00109 0.00127 0.00094 0.00094 0.00089 0.00052 H16 1.05305 0.43598 0.47969 1.00000 0.05013 0.00000 0.00000 Final Structure Factor Calculation for 00SOT036 in P2(1)/c Total number of l.s. parameters = 190 Maximum vector length = 511 Memory required = 2209 / 22995 wR2 = 0.1774 before cycle 5 for 3244 data and 0 / 190 parameters GooF = S = 1.136; Restrained GooF = 1.136 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 = 0.0571 for 2259 Fo > 4sig(Fo) and 0.0860 for all 3244 data wR2 = 0.1774, GooF = S = 1.136, Restrained GooF = 1.136 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0694 0.0495 0.0276 F1 0.0663 0.0467 0.0271 F2 0.0732 0.0413 0.0291 F3 0.0479 0.0338 0.0264 O1 0.0503 0.0350 0.0249 O2 0.0340 0.0309 0.0249 C1 0.0449 0.0377 0.0297 C2 0.0441 0.0416 0.0306 C3 0.0494 0.0419 0.0313 C4 0.0347 0.0309 0.0277 C5 0.0337 0.0313 0.0249 C6 0.0452 0.0319 0.0293 C7 0.0358 0.0320 0.0269 C8 0.0483 0.0373 0.0296 C9 0.0634 0.0565 0.0376 C10 0.0379 0.0314 0.0263 C11 0.0452 0.0428 0.0291 C12 0.0704 0.0583 0.0315 C13 0.0779 0.0473 0.0268 C14 0.0759 0.0462 0.0274 C15 0.0496 0.0422 0.0335 C16 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.012 0.018 0.025 0.034 0.044 0.059 0.082 0.123 1.000 Number in group 367. 285. 348. 306. 342. 316. 314. 327. 315. 324. GooF 0.964 1.095 1.099 1.277 1.303 1.252 1.190 1.193 1.029 0.899 K 3.318 1.111 1.014 1.026 1.017 1.034 1.014 1.021 1.006 0.992 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 325. 325. 326. 322. 329. 319. 329. 324. 321. 324. GooF 0.861 1.001 0.902 1.088 1.058 1.067 1.160 1.069 1.443 1.531 K 1.060 1.061 1.050 1.010 1.016 1.027 1.034 1.034 1.033 0.973 R1 0.245 0.220 0.159 0.150 0.104 0.068 0.059 0.051 0.053 0.049 Recommended weighting scheme: WGHT 0.0880 0.4027 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) 3 8 2 40.05 20.57 4.80 0.029 1.74 2 5 3 18.96 5.60 4.64 0.015 1.94 -3 7 3 36.37 19.99 4.43 0.028 1.64 -4 0 2 175.67 108.71 4.29 0.066 1.99 1 14 1 4.38 11.14 4.26 0.021 1.41 -4 3 1 72.30 30.79 4.23 0.035 2.11 3 7 3 24.00 9.91 4.10 0.020 1.62 7 0 0 37.40 16.83 3.98 0.026 1.32 -8 1 3 1.19 11.45 3.94 0.021 1.06 0 4 2 10.28 18.80 3.85 0.028 3.05 5 5 2 23.85 13.81 3.76 0.024 1.53 1 4 2 22.38 9.02 3.72 0.019 2.89 -2 11 2 237.48 144.89 3.69 0.076 1.57 -5 2 2 136.48 91.55 3.64 0.061 1.65 6 4 2 32.05 54.29 3.61 0.047 1.37 5 15 1 10.18 0.80 3.56 0.006 1.08 4 1 0 5.27 1.27 3.52 0.007 2.29 5 0 0 635.17 432.56 3.47 0.132 1.85 -2 8 6 9.14 0.12 3.45 0.002 1.11 3 12 1 41.07 25.11 3.43 0.032 1.46 -2 6 4 33.77 13.83 3.40 0.024 1.57 1 4 0 134.59 84.38 3.36 0.058 4.46 -4 1 1 831.95 571.23 3.34 0.152 2.21 -1 8 3 80.35 55.30 3.33 0.047 1.77 3 11 2 12.64 6.60 3.30 0.016 1.46 -2 8 3 177.50 264.28 3.27 0.103 1.68 3 9 3 4.80 0.31 3.24 0.004 1.47 -7 4 3 73.33 47.27 3.22 0.044 1.15 -1 5 2 127.71 88.95 3.18 0.060 2.68 -3 14 5 20.98 39.51 3.17 0.040 1.00 3 19 3 4.54 11.72 3.15 0.022 0.94 3 5 1 54.90 34.32 3.10 0.037 2.33 -3 6 4 202.70 143.72 3.07 0.076 1.47 1 3 4 5.06 0.57 3.02 0.005 1.80 4 6 2 6.78 2.52 2.99 0.010 1.70 3 0 8 14.18 3.17 2.98 0.011 0.91 3 0 4 114.11 80.80 2.98 0.057 1.61 0 15 7 83.54 45.88 2.93 0.043 0.85 0 14 5 157.39 113.07 2.93 0.067 1.05 0 3 5 15.36 25.36 2.92 0.032 1.49 -7 8 5 -0.92 10.23 2.92 0.020 0.94 6 0 4 36.25 55.80 2.91 0.047 1.19 -2 7 1 35.31 1.78 2.90 0.008 2.35 3 12 6 37.96 21.41 2.88 0.029 0.96 5 20 1 20.08 34.74 2.86 0.037 0.88 6 6 5 4.10 11.35 2.85 0.021 1.02 -3 8 1 38.32 66.15 2.82 0.052 1.90 -4 0 4 8.26 2.99 2.81 0.011 1.48 1 19 1 14.66 8.27 2.79 0.018 1.05 -4 1 3 75.33 47.15 2.79 0.044 1.72 Bond lengths and angles F1 - Distance Angles C7 1.3470 (0.0024) F1 - F2 - Distance Angles C7 1.3319 (0.0024) F2 - F3 - Distance Angles C7 1.3301 (0.0025) F3 - O1 - Distance Angles C5 1.3705 (0.0024) C4 1.4442 (0.0026) 115.54 (0.15) O1 - C5 O2 - Distance Angles C6 1.4137 (0.0022) O2 - C1 - Distance Angles C5 1.3302 (0.0026) C2 1.5066 (0.0027) 119.88 (0.18) C6 1.5242 (0.0028) 118.84 (0.17) 121.21 (0.16) C1 - C5 C2 C2 - Distance Angles C1 1.5066 (0.0027) C3 1.5159 (0.0030) 109.41 (0.16) C2 - C1 C3 - Distance Angles C4 1.4964 (0.0030) C2 1.5159 (0.0030) 110.20 (0.17) C3 - C4 C4 - Distance Angles O1 1.4442 (0.0026) C3 1.4964 (0.0030) 111.61 (0.17) C4 - O1 C5 - Distance Angles C1 1.3302 (0.0026) O1 1.3705 (0.0024) 126.32 (0.18) C5 - C1 C6 - Distance Angles O2 1.4137 (0.0022) C1 1.5242 (0.0028) 112.78 (0.15) C7 1.5345 (0.0027) 106.88 (0.15) 108.78 (0.16) C8 1.5578 (0.0026) 106.85 (0.15) 110.59 (0.15) 110.91 (0.15) C6 - O2 C1 C7 C7 - Distance Angles F3 1.3301 (0.0025) F2 1.3319 (0.0024) 106.28 (0.16) F1 1.3470 (0.0024) 106.26 (0.16) 106.59 (0.17) C6 1.5345 (0.0027) 113.91 (0.17) 111.25 (0.16) 112.07 (0.16) C7 - F3 F2 F1 C8 - Distance Angles C9 1.5098 (0.0027) C11 1.5176 (0.0028) 111.52 (0.16) C6 1.5578 (0.0026) 110.31 (0.15) 114.28 (0.16) C8 - C9 C11 C9 - Distance Angles C10 1.3053 (0.0033) C8 1.5098 (0.0027) 123.60 (0.20) C9 - C10 C10 - Distance Angles C9 1.3053 (0.0033) C10 - C11 - Distance Angles C16 1.3829 (0.0030) C12 1.3865 (0.0028) 118.23 (0.20) C8 1.5176 (0.0028) 122.87 (0.18) 118.87 (0.18) C11 - C16 C12 C12 - Distance Angles C11 1.3865 (0.0028) C13 1.3880 (0.0033) 120.84 (0.21) C12 - C11 C13 - Distance Angles C14 1.3724 (0.0037) C12 1.3880 (0.0033) 120.05 (0.23) C13 - C14 C14 - Distance Angles C15 1.3669 (0.0037) C13 1.3724 (0.0037) 119.86 (0.23) C14 - C15 C15 - Distance Angles C14 1.3669 (0.0037) C16 1.3906 (0.0034) 120.33 (0.23) C15 - C14 C16 - Distance Angles C11 1.3829 (0.0030) C15 1.3906 (0.0034) 120.66 (0.21) C16 - C11 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 24 -2 2.500 1 2 R1 = 0.0860 for 3244 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.0270 0.4008 0.8804 [ 1.34 A from C10 ] Deepest hole -0.25 at 0.3256 0.6900 0.6235 [ 0.69 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2393 / 27171 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0270 0.4008 0.8804 1.00000 0.05 0.51 1.34 C10 1.38 C9 1.76 H10A 1.83 H10B Q2 1 0.8472 0.4728 0.6756 1.00000 0.05 0.47 0.93 H9 1.49 C9 1.87 O2 2.10 C8 Q3 1 0.8677 0.3370 0.9566 1.00000 0.05 0.46 0.88 H10A 1.61 C10 1.67 H8 2.12 C9 Q4 1 0.8493 0.4391 1.0493 1.00000 0.05 0.37 0.80 H10B 0.96 C10 1.44 H10A 1.96 C9 Q5 1 0.6302 0.4266 0.7785 1.00000 0.05 0.32 0.93 C1 1.33 C5 1.74 C2 1.93 H5 Q6 1 0.7985 0.3667 0.5967 1.00000 0.05 0.31 0.81 C8 0.88 C6 1.35 H8 1.76 C7 Q7 1 0.6991 0.3685 0.4800 1.00000 0.05 0.29 0.76 C7 0.81 C6 1.67 F2 1.71 O2 Q8 1 0.5574 0.3717 0.8786 1.00000 0.05 0.27 0.84 C2 1.07 H2A 1.17 C3 1.33 H3B Q9 1 0.8716 0.3900 0.8976 1.00000 0.05 0.26 0.82 C10 1.01 H10A 1.01 C9 1.72 H8 Q10 1 1.0069 0.3924 0.4022 1.00000 0.05 0.25 0.86 C16 1.14 H16 1.58 C11 1.80 C15 Shortest distances between peaks (including symmetry equivalents) 3 9 1.17 6 7 1.27 1 9 1.46 5 8 1.52 4 9 1.55 1 3 2.05 3 4 2.20 1 4 2.24 2 6 2.29 2 5 2.36 2 9 2.40 5 6 2.43 6 9 2.43 5 9 2.50 6 10 2.51 5 7 2.66 1 2 2.69 3 6 2.88 4 5 2.88 2 7 2.92 8 9 2.92 2 4 2.94 7 10 2.95 3 8 3.00 Time profile in seconds ----------------------- 0.17: 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. 2.13: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.03: Structure factors and derivatives 1.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:09:14 Total CPU time: 4.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++