+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:40:40 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT097 in C2/c CELL 0.71073 14.6339 7.7463 35.8752 90 91.066 90 ZERR 8 0.0003 0.0001 0.0007 0 0.003 0 LATT 7 SYMM -X, Y, 1/2-Z SFAC N H O SI C UNIT 8 248 24 8 160 V = 4066.06 F(000) = 1568.0 Mu = 0.13 mm-1 Cell Wt = 2892.38 Rho = 1.181 SHEL 7 0.84 SIZE 0.15 0.06 0.07 TEMP -153 FMAP 2 PLAN 20 L.S. 4 WGHT 0.130000 EXTI 0.000000 FVAR 0.09152 MOLE 1 N1 1 0.572742 -0.742691 0.794054 11.00000 0.01587 0.03881 = 0.04208 -0.00189 0.00140 0.00226 O1 3 0.577553 -0.888598 0.781422 11.00000 0.04388 0.03376 = 0.05046 0.00114 0.00058 -0.00605 O2 3 0.544689 -0.710832 0.825239 11.00000 0.03359 0.04824 = 0.04774 0.00347 0.01144 -0.00071 O3 3 0.748312 -0.227242 0.677296 11.00000 0.02261 0.03293 = 0.04271 0.00828 0.00589 0.00411 SI1 4 0.689957 0.214112 0.583877 11.00000 0.03809 0.04498 = 0.02947 0.00314 0.00513 0.00585 C1 5 0.618589 -0.295511 0.761920 11.00000 0.03199 0.02494 = 0.03621 -0.00168 -0.00405 0.00800 AFIX 43 H1 2 0.613769 -0.180639 0.770947 11.00000 -1.20000 AFIX 0 C2 5 0.592600 -0.431896 0.784034 11.00000 0.02515 0.03070 = 0.03474 -0.00350 0.00284 0.00255 AFIX 43 H2 2 0.568939 -0.412138 0.808142 11.00000 -1.20000 AFIX 0 C3 5 0.601527 -0.596115 0.770606 11.00000 0.02665 0.01832 = 0.03366 0.00313 0.00078 -0.00146 C4 5 0.635220 -0.630751 0.735954 11.00000 0.02128 0.02823 = 0.03984 0.00236 -0.00535 0.00475 AFIX 43 H4 2 0.641257 -0.746357 0.727512 11.00000 -1.20000 AFIX 0 C5 5 0.660011 -0.494988 0.713750 11.00000 0.02921 0.03338 = 0.03071 -0.00213 -0.00088 0.00373 AFIX 43 H5 2 0.682879 -0.516661 0.689585 11.00000 -1.20000 AFIX 0 C6 5 0.651936 -0.325713 0.726335 11.00000 0.01285 0.03416 = 0.03715 0.00034 -0.00356 -0.00119 C7 5 0.676460 -0.174989 0.701371 11.00000 0.02017 0.03193 = 0.03885 -0.00209 0.00405 0.00031 AFIX 13 H7 2 0.698003 -0.076088 0.717147 11.00000 -1.20000 AFIX 0 C8 5 0.600882 -0.113394 0.674925 11.00000 0.01852 0.04244 = 0.04018 -0.00385 0.00542 0.00742 AFIX 23 H8A 2 0.564980 -0.211411 0.664693 11.00000 -1.20000 H8B 2 0.559261 -0.031772 0.687368 11.00000 -1.20000 AFIX 0 C9 5 0.655144 -0.024537 0.644851 11.00000 0.01935 0.03086 = 0.03266 -0.00439 0.00468 -0.00019 C10 5 0.748688 -0.104838 0.646989 11.00000 0.02703 0.03206 = 0.04617 0.01208 0.00397 0.00262 AFIX 23 H10A 2 0.762441 -0.163987 0.623283 11.00000 -1.20000 H10B 2 0.795690 -0.015081 0.651641 11.00000 -1.20000 AFIX 0 C11 5 0.627164 0.097320 0.621508 11.00000 0.02748 0.04564 = 0.03726 -0.00191 -0.00019 0.00732 AFIX 43 H11 2 0.565270 0.131384 0.624189 11.00000 -1.20000 AFIX 0 C12 5 0.617701 0.407081 0.571107 11.00000 0.07493 0.06128 = 0.03381 0.00994 -0.00632 0.02491 AFIX 13 H12 2 0.661028 0.479532 0.556603 11.00000 -1.20000 AFIX 0 C13 5 0.596564 0.523433 0.604279 11.00000 0.06320 0.04769 = 0.04675 0.00715 0.00520 0.01293 AFIX 33 H13A 2 0.652262 0.540701 0.619409 11.00000 -1.50000 H13B 2 0.549725 0.468902 0.619501 11.00000 -1.50000 H13C 2 0.574159 0.635269 0.595188 11.00000 -1.50000 AFIX 0 C14 5 0.546201 0.390503 0.547130 11.00000 0.32922 0.18614 = 0.12173 -0.08905 -0.13983 0.18146 AFIX 33 H14A 2 0.563623 0.316636 0.526254 11.00000 -1.50000 H14B 2 0.528373 0.504562 0.537678 11.00000 -1.50000 H14C 2 0.494633 0.338260 0.560030 11.00000 -1.50000 AFIX 0 C15 5 0.809598 0.276025 0.599246 11.00000 0.04469 0.04417 = 0.03754 0.00336 0.00610 0.00134 AFIX 13 H15 2 0.845702 0.166487 0.600382 11.00000 -1.20000 AFIX 0 C16 5 0.819601 0.360606 0.637984 11.00000 0.04501 0.04444 = 0.04152 0.00487 0.00280 -0.00232 AFIX 33 H16A 2 0.791320 0.286478 0.656664 11.00000 -1.50000 H16B 2 0.789272 0.473404 0.637671 11.00000 -1.50000 H16C 2 0.884574 0.375727 0.644255 11.00000 -1.50000 AFIX 0 C17 5 0.856660 0.392931 0.570453 11.00000 0.03582 0.11010 = 0.05258 0.01960 0.00820 -0.01731 AFIX 33 H17A 2 0.851560 0.339992 0.545691 11.00000 -1.50000 H17B 2 0.921325 0.406640 0.577417 11.00000 -1.50000 H17C 2 0.826941 0.506303 0.569989 11.00000 -1.50000 AFIX 0 C18 5 0.698925 0.071047 0.540937 11.00000 0.05560 0.04831 = 0.03050 0.00011 0.00496 -0.00278 AFIX 13 H18 2 0.706027 0.150037 0.519134 11.00000 -1.20000 AFIX 0 C19 5 0.781335 -0.048893 0.541304 11.00000 0.16967 0.16173 = 0.08448 -0.07268 -0.03304 0.11473 AFIX 33 H19A 2 0.837122 0.018579 0.545766 11.00000 -1.50000 H19B 2 0.785015 -0.107853 0.517210 11.00000 -1.50000 H19C 2 0.774924 -0.134620 0.561174 11.00000 -1.50000 AFIX 0 C20 5 0.612828 -0.033241 0.533493 11.00000 0.10388 0.07587 = 0.05643 -0.01864 0.03195 -0.03386 AFIX 33 H20A 2 0.559817 0.044080 0.532852 11.00000 -1.50000 H20B 2 0.605542 -0.118738 0.553352 11.00000 -1.50000 H20C 2 0.617474 -0.092472 0.509465 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 01SOT097 in C2/c N 0.700 H 0.320 O 0.660 SI 1.170 C 0.770 N1 - O1 O2 C3 O1 - N1 O2 - N1 O3 - C7 C10 Si1 - C11 C12 C15 C18 C1 - C2 C6 C2 - C3 C1 C3 - C2 C4 N1 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 C7 - O3 C6 C8 C8 - C9 C7 C9 - C11 C10 C8 C10 - O3 C9 C11 - C9 Si1 C12 - C14 C13 Si1 C13 - C12 C14 - C12 C15 - C16 C17 Si1 C16 - C15 C17 - C15 C18 - C20 C19 Si1 C19 - C18 C20 - C18 7533 Reflections read, of which 621 rejected -17 =< h =< 17, -8 =< k =< 8, -42 =< l =< 42, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 4.30 0.16 4 1.87 -1 1 1 6.71 0.13 6 3.26 1 1 1 22.86 0.18 5 48.88 -1 1 2 16.92 0.17 7 21.60 -1 1 3 74.58 2.73 5 17.83 0 2 4 9.86 0.20 5 2.64 -1 3 4 37.83 0.31 7 6.74 0 2 5 11.72 0.20 3 6.47 1 3 7 25.05 1.13 3 9.41 1 3 8 14.56 0.40 5 3.40 0 4 11 36.26 0.43 4 18.16 2 4 11 6.73 0.52 2 9.09 0 4 12 6.63 0.60 2 7.09 13 Inconsistent equivalents 3107 Unique reflections, of which 0 suppressed R(int) = 0.1029 R(sigma) = 0.1814 Friedel opposites merged Maximum memory for data reduction = 2243 / 38140 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 = 2956 / 282343 wR2 = 0.2539 before cycle 1 for 3107 data and 227 / 227 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1300 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09153 0.00049 0.022 OSF 2 0.00000 0.00047 -0.359 EXTI Mean shift/esd = 0.004 Maximum = -0.359 for EXTI Max. shift = 0.001 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2956 / 282343 wR2 = 0.2539 before cycle 2 for 3107 data and 227 / 227 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1300 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09152 0.00049 -0.014 OSF 2 0.00000 0.00047 -0.478 EXTI Mean shift/esd = 0.005 Maximum = -0.478 for EXTI Max. shift = 0.001 A for C14 Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2956 / 282343 wR2 = 0.2539 before cycle 3 for 3107 data and 227 / 227 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1300 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09153 0.00049 0.003 OSF 2 0.00000 0.00047 -0.478 EXTI Mean shift/esd = 0.004 Maximum = -0.478 for EXTI Max. shift = 0.000 A for C14 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2956 / 282343 wR2 = 0.2539 before cycle 4 for 3107 data and 227 / 227 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1300 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09153 0.00049 0.002 OSF 2 0.00000 0.00047 -0.477 EXTI Mean shift/esd = 0.004 Maximum = -0.477 for EXTI Max. shift = 0.000 A for C14 Max. dU = 0.000 for C14 Largest correlation matrix elements 0.617 U12 C14 / U22 C14 0.564 U13 C14 / U23 C14 0.608 U12 C14 / U11 C14 -0.522 U13 C14 / U11 C14 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.6138 -0.1806 0.7709 43 0.950 0.000 C1 C2 C6 H2 0.5689 -0.4121 0.8081 43 0.950 0.000 C2 C3 C1 H4 0.6413 -0.7464 0.7275 43 0.950 0.000 C4 C5 C3 H5 0.6829 -0.5167 0.6896 43 0.950 0.000 C5 C4 C6 H7 0.6980 -0.0761 0.7171 13 1.000 0.000 C7 O3 C6 C8 H8A 0.5650 -0.2114 0.6647 23 0.990 0.000 C8 C9 C7 H8B 0.5593 -0.0318 0.6874 23 0.990 0.000 C8 C9 C7 H10A 0.7624 -0.1640 0.6233 23 0.990 0.000 C10 O3 C9 H10B 0.7957 -0.0151 0.6516 23 0.990 0.000 C10 O3 C9 H11 0.5653 0.1314 0.6242 43 0.950 0.000 C11 C9 Si1 H12 0.6611 0.4795 0.5566 13 1.000 0.000 C12 C14 C13 Si1 H13A 0.6523 0.5407 0.6194 33 0.980 0.000 C13 C12 H13A H13B 0.5497 0.4689 0.6195 33 0.980 0.000 C13 C12 H13A H13C 0.5742 0.6353 0.5952 33 0.980 0.000 C13 C12 H13A H14A 0.5638 0.3168 0.5262 33 0.980 0.000 C14 C12 H14A H14B 0.5286 0.5047 0.5377 33 0.980 0.000 C14 C12 H14A H14C 0.4947 0.3385 0.5600 33 0.980 0.000 C14 C12 H14A H15 0.8457 0.1665 0.6004 13 1.000 0.000 C15 C16 C17 Si1 H16A 0.7913 0.2865 0.6567 33 0.980 0.000 C16 C15 H16A H16B 0.7893 0.4734 0.6377 33 0.980 0.000 C16 C15 H16A H16C 0.8846 0.3757 0.6443 33 0.980 0.000 C16 C15 H16A H17A 0.8516 0.3400 0.5457 33 0.980 0.000 C17 C15 H17A H17B 0.9213 0.4066 0.5774 33 0.980 0.000 C17 C15 H17A H17C 0.8269 0.5063 0.5700 33 0.980 0.000 C17 C15 H17A H18 0.7060 0.1500 0.5191 13 1.000 0.000 C18 C20 C19 Si1 H19A 0.8371 0.0186 0.5458 33 0.980 0.000 C19 C18 H19A H19B 0.7850 -0.1078 0.5172 33 0.980 0.000 C19 C18 H19A H19C 0.7749 -0.1346 0.5612 33 0.980 0.000 C19 C18 H19A H20A 0.5598 0.0441 0.5329 33 0.980 0.000 C20 C18 H20A H20B 0.6056 -0.1187 0.5534 33 0.980 0.000 C20 C18 H20A H20C 0.6175 -0.0925 0.5095 33 0.980 0.000 C20 C18 H20A 01SOT097 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.57275 -0.74268 0.79405 1.00000 0.01588 0.03877 0.04209 -0.00190 0.00140 0.00226 0.03223 0.00884 0.00033 0.00067 0.00015 0.00000 0.00322 0.00341 0.00345 0.00269 0.00253 0.00262 0.00131 O1 0.57755 -0.88859 0.78142 1.00000 0.04387 0.03378 0.05045 0.00116 0.00059 -0.00605 0.04270 0.00704 0.00028 0.00052 0.00011 0.00000 0.00322 0.00261 0.00290 0.00216 0.00229 0.00229 0.00123 O2 0.54469 -0.71083 0.82524 1.00000 0.03362 0.04821 0.04775 0.00348 0.01144 -0.00072 0.04306 0.00724 0.00029 0.00049 0.00012 0.00000 0.00298 0.00270 0.00296 0.00225 0.00233 0.00223 0.00119 O3 0.74832 -0.22725 0.67730 1.00000 0.02265 0.03293 0.04271 0.00829 0.00590 0.00412 0.03270 0.00644 0.00026 0.00044 0.00010 0.00000 0.00262 0.00226 0.00254 0.00192 0.00198 0.00200 0.00107 Si1 0.68996 0.21411 0.58388 1.00000 0.03810 0.04499 0.02947 0.00313 0.00513 0.00585 0.03746 0.00312 0.00013 0.00022 0.00005 0.00000 0.00133 0.00116 0.00105 0.00082 0.00085 0.00094 0.00063 C1 0.61859 -0.29551 0.76192 1.00000 0.03199 0.02496 0.03619 -0.00167 -0.00405 0.00800 0.03110 0.00968 0.00039 0.00070 0.00015 0.00000 0.00430 0.00334 0.00383 0.00291 0.00310 0.00301 0.00156 H1 0.61377 -0.18064 0.77095 1.00000 0.03732 0.00000 0.00000 C2 0.59260 -0.43190 0.78403 1.00000 0.02512 0.03072 0.03476 -0.00350 0.00284 0.00253 0.03017 0.00947 0.00038 0.00069 0.00016 0.00000 0.00412 0.00365 0.00364 0.00282 0.00293 0.00303 0.00155 H2 0.56894 -0.41214 0.80814 1.00000 0.03621 0.00000 0.00000 C3 0.60153 -0.59612 0.77061 1.00000 0.02666 0.01833 0.03364 0.00310 0.00079 -0.00146 0.02621 0.00946 0.00039 0.00066 0.00016 0.00000 0.00405 0.00319 0.00357 0.00265 0.00293 0.00282 0.00145 C4 0.63522 -0.63076 0.73596 1.00000 0.02127 0.02825 0.03986 0.00238 -0.00535 0.00474 0.02987 0.00962 0.00038 0.00072 0.00016 0.00000 0.00398 0.00345 0.00390 0.00297 0.00301 0.00299 0.00153 H4 0.64126 -0.74636 0.72751 1.00000 0.03584 0.00000 0.00000 C5 0.66001 -0.49498 0.71375 1.00000 0.02921 0.03340 0.03073 -0.00213 -0.00089 0.00371 0.03113 0.00956 0.00040 0.00072 0.00016 0.00000 0.00431 0.00369 0.00356 0.00294 0.00302 0.00301 0.00157 H5 0.68288 -0.51665 0.68958 1.00000 0.03736 0.00000 0.00000 C6 0.65193 -0.32571 0.72634 1.00000 0.01287 0.03412 0.03716 0.00033 -0.00356 -0.00119 0.02810 0.00945 0.00038 0.00071 0.00016 0.00000 0.00380 0.00375 0.00381 0.00282 0.00287 0.00292 0.00152 C7 0.67646 -0.17499 0.70137 1.00000 0.02019 0.03194 0.03886 -0.00209 0.00405 0.00029 0.03029 0.01016 0.00040 0.00070 0.00016 0.00000 0.00395 0.00348 0.00378 0.00278 0.00308 0.00303 0.00155 H7 0.69800 -0.07609 0.71715 1.00000 0.03634 0.00000 0.00000 C8 0.60088 -0.11339 0.67493 1.00000 0.01852 0.04247 0.04020 -0.00384 0.00542 0.00743 0.03367 0.01001 0.00039 0.00072 0.00015 0.00000 0.00389 0.00366 0.00381 0.00301 0.00299 0.00320 0.00158 H8A 0.56498 -0.21140 0.66469 1.00000 0.04040 0.00000 0.00000 H8B 0.55926 -0.03177 0.68737 1.00000 0.04040 0.00000 0.00000 C9 0.65514 -0.02453 0.64485 1.00000 0.01933 0.03087 0.03267 -0.00440 0.00468 -0.00020 0.02757 0.00917 0.00040 0.00069 0.00015 0.00000 0.00407 0.00336 0.00357 0.00285 0.00290 0.00307 0.00150 C10 0.74869 -0.10484 0.64699 1.00000 0.02707 0.03206 0.04617 0.01207 0.00398 0.00263 0.03506 0.01071 0.00041 0.00069 0.00016 0.00000 0.00436 0.00354 0.00404 0.00300 0.00310 0.00327 0.00163 H10A 0.76244 -0.16399 0.62328 1.00000 0.04207 0.00000 0.00000 H10B 0.79569 -0.01508 0.65164 1.00000 0.04207 0.00000 0.00000 C11 0.62716 0.09732 0.62151 1.00000 0.02748 0.04563 0.03726 -0.00190 -0.00020 0.00733 0.03680 0.00974 0.00043 0.00075 0.00015 0.00000 0.00420 0.00392 0.00390 0.00317 0.00309 0.00336 0.00164 H11 0.56527 0.13137 0.62419 1.00000 0.04416 0.00000 0.00000 C12 0.61769 0.40706 0.57111 1.00000 0.07503 0.06128 0.03374 0.00996 -0.00630 0.02495 0.05678 0.01294 0.00053 0.00085 0.00018 0.00000 0.00598 0.00469 0.00409 0.00352 0.00398 0.00436 0.00211 H12 0.66106 0.47952 0.55663 1.00000 0.06813 0.00000 0.00000 C13 0.59656 0.52344 0.60428 1.00000 0.06312 0.04774 0.04675 0.00715 0.00518 0.01289 0.05249 0.01154 0.00048 0.00079 0.00017 0.00000 0.00566 0.00415 0.00438 0.00340 0.00385 0.00378 0.00202 H13A 0.65226 0.54071 0.61941 1.00000 0.07873 0.00000 0.00000 H13B 0.54972 0.46892 0.61950 1.00000 0.07873 0.00000 0.00000 H13C 0.57416 0.63527 0.59518 1.00000 0.07873 0.00000 0.00000 C14 0.54633 0.39063 0.54711 1.00000 0.33245 0.18703 0.12175 -0.08972 -0.14105 0.18353 0.21554 0.02107 0.00103 0.00151 0.00030 0.00000 0.02037 0.01210 0.00943 0.00870 0.01174 0.01348 0.00875 H14A 0.56379 0.31676 0.52624 1.00000 0.32332 0.00000 0.00000 H14B 0.52858 0.50473 0.53766 1.00000 0.32332 0.00000 0.00000 H14C 0.49469 0.33846 0.55998 1.00000 0.32332 0.00000 0.00000 C15 0.80960 0.27601 0.59925 1.00000 0.04471 0.04418 0.03753 0.00334 0.00610 0.00135 0.04207 0.01044 0.00045 0.00079 0.00016 0.00000 0.00482 0.00385 0.00410 0.00311 0.00333 0.00352 0.00177 H15 0.84571 0.16648 0.60038 1.00000 0.05049 0.00000 0.00000 C16 0.81960 0.36061 0.63799 1.00000 0.04503 0.04445 0.04153 0.00486 0.00277 -0.00233 0.04365 0.01050 0.00045 0.00074 0.00016 0.00000 0.00479 0.00395 0.00409 0.00319 0.00346 0.00354 0.00180 H16A 0.79132 0.28648 0.65667 1.00000 0.06547 0.00000 0.00000 H16B 0.78927 0.47341 0.63767 1.00000 0.06547 0.00000 0.00000 H16C 0.88458 0.37574 0.64426 1.00000 0.06547 0.00000 0.00000 C17 0.85666 0.39293 0.57045 1.00000 0.03584 0.11009 0.05260 0.01961 0.00821 -0.01729 0.06609 0.01237 0.00047 0.00095 0.00018 0.00000 0.00499 0.00612 0.00473 0.00443 0.00374 0.00457 0.00228 H17A 0.85156 0.33999 0.54569 1.00000 0.09913 0.00000 0.00000 H17B 0.92133 0.40664 0.57742 1.00000 0.09913 0.00000 0.00000 H17C 0.82694 0.50629 0.56999 1.00000 0.09913 0.00000 0.00000 C18 0.69892 0.07105 0.54094 1.00000 0.05561 0.04833 0.03050 0.00012 0.00493 -0.00278 0.04476 0.01104 0.00047 0.00081 0.00016 0.00000 0.00529 0.00410 0.00386 0.00309 0.00350 0.00402 0.00185 H18 0.70602 0.15004 0.51913 1.00000 0.05371 0.00000 0.00000 C19 0.78134 -0.04888 0.54130 1.00000 0.16976 0.16185 0.08450 -0.07269 -0.03305 0.11488 0.13914 0.01697 0.00072 0.00129 0.00023 0.00000 0.01115 0.00955 0.00711 0.00664 0.00695 0.00891 0.00490 H19A 0.83713 0.01860 0.54576 1.00000 0.20871 0.00000 0.00000 H19B 0.78502 -0.10783 0.51720 1.00000 0.20871 0.00000 0.00000 H19C 0.77494 -0.13462 0.56117 1.00000 0.20871 0.00000 0.00000 C20 0.61284 -0.03324 0.53349 1.00000 0.10386 0.07589 0.05647 -0.01864 0.03197 -0.03386 0.07836 0.01276 0.00058 0.00097 0.00019 0.00000 0.00765 0.00547 0.00512 0.00412 0.00482 0.00544 0.00270 H20A 0.55983 0.04407 0.53285 1.00000 0.11754 0.00000 0.00000 H20B 0.60556 -0.11874 0.55335 1.00000 0.11754 0.00000 0.00000 H20C 0.61749 -0.09247 0.50947 1.00000 0.11754 0.00000 0.00000 Final Structure Factor Calculation for 01SOT097 in C2/c Total number of l.s. parameters = 227 Maximum vector length = 511 Memory required = 2729 / 24017 wR2 = 0.2539 before cycle 5 for 3107 data and 0 / 227 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1300 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0824 for 1445 Fo > 4sig(Fo) and 0.2006 for all 3107 data wR2 = 0.2539, GooF = S = 0.968, Restrained GooF = 0.968 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0430 0.0381 0.0156 N1 0.0507 0.0466 0.0309 O1 0.0545 0.0473 0.0274 O2 0.0490 0.0283 0.0208 O3 0.0495 0.0354 0.0274 Si1 0.0417 0.0319 0.0197 C1 0.0368 0.0307 0.0230 C2 0.0343 0.0269 0.0175 C3 0.0418 0.0306 0.0172 C4 0.0367 0.0296 0.0270 C5 0.0380 0.0341 0.0122 C6 0.0399 0.0315 0.0194 C7 0.0459 0.0402 0.0150 C8 0.0369 0.0279 0.0179 C9 0.0537 0.0266 0.0249 C10 0.0486 0.0369 0.0249 C11 0.0940 0.0510 0.0252 C12 0.0723 0.0470 0.0381 C13 0.5321 0.0646 0.0500 C14 may be split into 0.5640 0.4132 0.5433 and 0.5287 0.3680 0.5509 0.0491 0.0431 0.0340 C15 0.0483 0.0459 0.0368 C16 0.1188 0.0534 0.0260 C17 0.0570 0.0475 0.0297 C18 0.3085 0.0818 0.0271 C19 may be split into 0.7918 -0.0279 0.5391 and 0.7708 -0.0698 0.5435 0.1408 0.0534 0.0408 C20 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.032 0.042 0.054 0.068 0.090 0.129 1.000 Number in group 337. 295. 301. 315. 305. 314. 307. 313. 309. 311. GooF 0.873 0.879 0.916 0.974 0.974 1.049 1.046 1.010 1.068 0.874 K 13.781 1.794 1.310 1.032 1.068 1.002 1.031 1.029 1.013 1.018 Resolution(A) 0.84 0.88 0.92 0.97 1.03 1.10 1.19 1.32 1.51 1.89 inf Number in group 312. 311. 318. 309. 305. 313. 308. 313. 306. 312. GooF 0.833 0.872 0.926 0.896 0.879 0.936 0.926 1.023 1.190 1.144 K 1.066 1.156 1.176 1.078 1.017 1.029 1.002 1.026 1.033 1.011 R1 0.463 0.421 0.388 0.290 0.210 0.183 0.130 0.112 0.095 0.064 Recommended weighting scheme: WGHT 0.1098 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) -1 1 2 2018.40 16822.57 5.29 0.301 6.41 -6 2 8 670.78 215.36 4.72 0.034 1.89 -6 2 10 1913.32 1015.75 4.34 0.074 1.80 1 1 1 2727.08 26184.84 3.99 0.375 6.71 -6 0 12 616.10 105.27 3.85 0.024 1.91 -4 2 17 451.58 152.44 3.71 0.029 1.66 2 0 4 123.28 14.98 3.71 0.009 5.62 -7 7 6 755.07 44.10 3.29 0.015 0.97 7 3 2 1211.03 742.92 3.23 0.063 1.62 7 7 2 2388.08 1220.80 3.19 0.081 0.98 -2 0 10 1841.95 1183.79 3.14 0.080 3.24 1 1 7 185.02 88.44 3.12 0.022 4.09 -5 1 14 3312.79 2116.86 3.06 0.107 1.89 -2 0 12 2181.71 1411.25 3.02 0.087 2.79 -8 6 16 710.15 94.54 2.96 0.023 0.96 -6 2 5 669.15 400.46 2.95 0.046 1.99 -4 6 17 1068.19 594.35 2.95 0.057 1.06 -6 4 10 750.41 403.04 2.90 0.047 1.40 -4 2 20 280.26 19.96 2.90 0.010 1.50 1 1 14 635.50 420.01 2.85 0.048 2.39 0 2 22 802.31 1267.88 2.84 0.083 1.50 3 7 6 -125.76 273.82 2.82 0.038 1.06 -3 1 16 1579.60 1094.68 2.81 0.077 1.98 -1 1 1 800.17 1941.08 2.79 0.102 6.74 -10 2 13 311.15 767.80 2.77 0.064 1.23 -5 1 15 738.90 421.79 2.74 0.048 1.82 -6 6 10 501.46 116.35 2.73 0.025 1.09 5 5 3 392.45 748.53 2.71 0.063 1.36 10 4 5 733.60 197.53 2.71 0.033 1.15 -4 4 14 -71.62 123.77 2.68 0.026 1.43 8 4 5 292.35 33.45 2.68 0.013 1.30 -6 2 20 2208.18 1443.01 2.67 0.088 1.36 -9 1 4 747.91 183.66 2.67 0.031 1.57 -1 1 42 823.53 0.01 2.66 0.000 0.85 5 3 4 3244.16 2303.68 2.65 0.111 1.89 1 1 12 1440.73 2061.76 2.65 0.105 2.73 -1 3 6 0.15 86.73 2.61 0.022 2.34 -6 2 7 620.49 1023.96 2.61 0.074 1.92 2 4 3 2064.14 1463.43 2.61 0.089 1.85 11 1 6 1325.13 2076.14 2.60 0.106 1.28 -7 1 31 1123.91 381.11 2.58 0.045 1.01 -3 3 13 977.76 665.52 2.58 0.060 1.77 -14 2 15 947.12 66.73 2.57 0.019 0.94 -6 4 18 2917.16 1849.51 2.56 0.100 1.21 8 4 27 1077.14 115.62 2.55 0.025 0.93 5 3 6 149.49 2.01 2.54 0.003 1.84 4 6 0 519.43 143.37 2.53 0.028 1.22 -10 4 6 3106.17 1953.73 2.52 0.103 1.15 0 6 2 138.38 0.65 2.51 0.002 1.29 9 3 3 167.16 438.41 2.51 0.049 1.36 FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 24 -2 3.125 1 2 R1 = 0.2001 for 3107 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.74 at 0.8715 0.0076 0.4638 [ 0.87 A from H12 ] Deepest hole -0.58 at 0.9179 0.0855 0.4601 [ 0.62 A from C14 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3765 / 31783 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6285 0.4924 0.5362 1.00000 0.05 0.74 0.87 H12 1.43 C12 1.47 H14B 1.50 C14 Q2 1 0.7951 -0.0435 0.5288 1.00000 0.05 0.41 0.50 C19 0.66 H19B 0.98 H19A 1.39 H19C Q3 1 0.6656 -0.1478 0.5600 1.00000 0.05 0.30 0.93 H20B 1.50 C20 1.60 H19C 1.90 C18 Q4 1 0.7500 -0.2500 0.5000 0.50000 0.05 0.29 1.36 H19B 2.19 C19 2.32 H20C 2.39 H19C Q5 1 0.6270 0.6678 0.6163 1.00000 0.05 0.29 1.06 H13A 1.10 H13C 1.28 C13 1.92 H13B Q6 1 0.5218 0.6048 0.5978 1.00000 0.05 0.28 0.81 H13C 1.28 C13 1.37 H13B 2.11 H13A Q7 1 0.7116 -0.2813 0.5692 1.00000 0.05 0.27 1.50 H19C 2.04 H12 2.07 H20B 2.26 H10A Q8 1 0.7462 -0.1467 0.5513 1.00000 0.05 0.27 0.55 H19C 0.99 C19 1.39 H19B 1.86 C18 Q9 1 0.5905 -0.2420 0.6623 1.00000 0.05 0.27 0.45 H8A 1.10 C8 1.92 H8B 1.94 C7 Q10 1 0.6779 0.6597 0.6376 1.00000 0.05 0.27 1.19 H13A 1.92 H10A 1.95 O3 1.98 C13 Q11 1 0.6065 -0.0908 0.7823 1.00000 0.05 0.26 0.81 H1 1.62 O1 1.76 C1 2.65 H16C Q12 1 0.6836 0.6341 0.6061 1.00000 0.05 0.26 0.98 H13A 1.54 C13 1.64 H13C 2.03 H10A Q13 1 0.6548 -0.2364 0.5122 1.00000 0.05 0.26 1.24 H20C 1.84 H19B 1.86 C20 1.89 H20B Q14 1 0.6364 -0.1963 0.4804 1.00000 0.05 0.25 1.35 H20C 1.90 H19B 2.32 C20 2.39 H19C Q15 1 0.7959 0.6305 0.5724 1.00000 0.05 0.25 1.07 H17C 1.89 H19C 2.05 C17 2.35 H12 Q16 1 0.5014 -0.0727 0.6901 1.00000 0.05 0.24 0.91 H8B 1.60 C8 1.70 H8A 2.11 O1 Q17 1 0.5044 -0.1741 0.7001 1.00000 0.05 0.24 1.44 H8B 1.59 H8A 1.76 C8 2.03 H1 Q18 1 0.7956 -0.1171 0.5024 1.00000 0.05 0.23 0.56 H19B 1.51 C19 1.96 H19A 2.14 H19C Q19 1 0.8298 0.4002 0.6925 1.00000 0.05 0.23 1.65 H16A 1.66 H1 1.93 H16C 1.98 C16 Q20 1 0.7969 -0.1033 0.5697 1.00000 0.05 0.23 0.50 H19C 1.12 C19 1.41 H19A 1.89 H19B Shortest distances between peaks (including symmetry equivalents) 16 17 0.86 5 12 0.95 8 20 1.04 5 10 1.06 2 18 1.10 10 12 1.15 13 14 1.21 3 8 1.22 4 18 1.23 3 7 1.27 11 19 1.29 7 8 1.33 2 8 1.35 7 15 1.41 13 18 1.45 4 13 1.47 2 20 1.54 7 12 1.54 5 6 1.74 9 10 1.74 4 14 1.84 3 13 1.85 14 18 1.85 7 20 1.86 11 17 1.87 5 9 1.88 11 16 1.88 8 18 1.92 9 17 1.94 3 20 1.98 2 4 2.01 4 8 2.01 8 15 2.01 1 18 2.04 8 13 2.04 12 15 2.06 15 20 2.06 9 16 2.11 5 7 2.15 14 15 2.21 7 13 2.22 2 14 2.28 13 18 2.29 1 13 2.31 2 3 2.36 3 12 2.38 2 13 2.38 6 12 2.39 8 14 2.41 18 20 2.41 1 7 2.43 18 18 2.46 14 18 2.52 16 19 2.52 3 5 2.55 7 10 2.55 4 7 2.57 14 20 2.58 3 15 2.60 2 13 2.60 3 4 2.62 17 19 2.63 9 12 2.63 1 2 2.64 2 7 2.66 7 18 2.69 6 10 2.70 8 18 2.72 8 12 2.77 6 9 2.77 4 20 2.82 4 15 2.83 1 12 2.84 3 18 2.84 1 6 2.86 8 13 2.87 7 14 2.88 3 14 2.90 10 15 2.94 13 13 2.94 12 20 2.95 3 18 2.95 1 15 2.95 1 3 2.96 5 15 2.97 2 15 2.97 15 18 2.98 1 4 2.99 7 18 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 0.02: 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 0.00: Analyse other restraints etc. 1.09: 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 1.36: Structure factors and derivatives 1.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.06: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:40:44 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++