+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:56:54 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC394 in C2/c CELL 0.71073 23.8267 12.9976 22.1794 90 108.155 90 ZERR 4 0.0004 0.0003 0.0005 0 0.0012 0 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O SI F N UNIT 256 304 48 32 4 4 V = 6526.79 F(000) = 2736.0 Mu = 0.23 mm-1 Cell Wt = 5179.91 Rho = 1.318 SHEL 7 0.84 TEMP -153 SIZE 0.3 0.2 0.1 FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.053200 8.161302 FVAR 0.15121 MOLE 1 C1 1 0.119677 0.689260 0.401978 11.00000 0.01831 0.01692 = 0.01240 -0.00229 0.00560 0.00133 C2 1 0.099164 0.605249 0.428105 11.00000 0.01833 0.02292 = 0.01931 0.00046 0.00839 0.00017 AFIX 43 H2 2 0.057800 0.595406 0.418557 11.00000 -1.20000 AFIX 0 C3 1 0.137627 0.535460 0.467771 11.00000 0.02852 0.02409 = 0.02443 0.00684 0.01272 0.00098 AFIX 43 H3 2 0.122467 0.478655 0.484764 11.00000 -1.20000 AFIX 0 C4 1 0.198178 0.548933 0.482487 11.00000 0.02796 0.02508 = 0.01842 0.00433 0.00367 0.00816 AFIX 43 H4 2 0.224642 0.501008 0.509123 11.00000 -1.20000 AFIX 0 C5 1 0.219707 0.632530 0.458129 11.00000 0.01711 0.03235 = 0.02700 0.00128 0.00289 0.00019 AFIX 43 H5 2 0.261120 0.642704 0.468534 11.00000 -1.20000 AFIX 0 C6 1 0.181053 0.701594 0.418556 11.00000 0.02172 0.02234 = 0.02310 0.00384 0.00509 -0.00241 AFIX 43 H6 2 0.196554 0.758757 0.402248 11.00000 -1.20000 AFIX 0 C7 1 0.114139 0.691096 0.170490 11.00000 0.01809 0.01918 = 0.01151 0.00355 0.00606 0.00203 C8 1 0.094140 0.601602 0.136057 11.00000 0.02079 0.02380 = 0.01675 -0.00016 0.00682 0.00169 AFIX 43 H8 2 0.053031 0.586962 0.122557 11.00000 -1.20000 AFIX 0 C9 1 0.132271 0.533032 0.120790 11.00000 0.03673 0.02294 = 0.02441 -0.00313 0.01137 0.00504 AFIX 43 H9 2 0.117428 0.472090 0.097666 11.00000 -1.20000 AFIX 0 C10 1 0.192153 0.554375 0.139612 11.00000 0.03310 0.04067 = 0.02805 0.00102 0.01654 0.01817 AFIX 43 H10 2 0.218762 0.507546 0.129978 11.00000 -1.20000 AFIX 0 C11 1 0.213079 0.643716 0.172358 11.00000 0.01822 0.05639 = 0.03740 -0.00901 0.01182 0.00327 AFIX 43 H11 2 0.254042 0.659263 0.184299 11.00000 -1.20000 AFIX 0 C12 1 0.174702 0.710872 0.187923 11.00000 0.02069 0.03464 = 0.02990 -0.01038 0.01058 -0.00387 AFIX 43 H12 2 0.189871 0.771737 0.210962 11.00000 -1.20000 AFIX 0 C13 1 0.108461 1.094621 0.163318 11.00000 0.01483 0.01521 = 0.02098 0.00186 0.00896 0.00376 C14 1 0.100168 1.085647 0.098142 11.00000 0.02663 0.02398 = 0.02502 -0.00433 0.01304 -0.00415 AFIX 43 H14 2 0.075857 1.031858 0.074998 11.00000 -1.20000 AFIX 0 C15 1 0.126288 1.152689 0.066512 11.00000 0.03662 0.03160 = 0.02512 0.00163 0.02098 0.00020 AFIX 43 H15 2 0.119626 1.144821 0.022245 11.00000 -1.20000 AFIX 0 C16 1 0.162088 1.231150 0.099281 11.00000 0.03051 0.02486 = 0.03981 0.00630 0.02348 -0.00193 AFIX 43 H16 2 0.179868 1.277796 0.077701 11.00000 -1.20000 AFIX 0 C17 1 0.171766 1.241073 0.163790 11.00000 0.02919 0.02759 = 0.03675 -0.00189 0.01274 -0.01049 AFIX 43 H17 2 0.196732 1.294187 0.186855 11.00000 -1.20000 AFIX 0 C18 1 0.145023 1.173463 0.194897 11.00000 0.02233 0.02858 = 0.02091 -0.00079 0.00866 -0.00228 AFIX 43 H18 2 0.152014 1.181521 0.239206 11.00000 -1.20000 AFIX 0 C19 1 -0.114773 1.093436 0.094893 11.00000 0.01497 0.01729 = 0.01769 -0.00131 0.00390 -0.00290 C20 1 -0.110234 1.081447 0.033786 11.00000 0.03223 0.02452 = 0.02055 0.00005 0.00644 0.00497 AFIX 43 H20 2 -0.087510 1.026018 0.025854 11.00000 -1.20000 AFIX 0 C21 1 -0.137745 1.147649 -0.015340 11.00000 0.03936 0.03799 = 0.01554 0.00154 0.00440 -0.00047 AFIX 43 H21 2 -0.134474 1.136685 -0.056462 11.00000 -1.20000 AFIX 0 C22 1 -0.170071 1.229967 -0.004291 11.00000 0.03518 0.03186 = 0.02748 0.01295 -0.00073 0.00441 AFIX 43 H22 2 -0.188245 1.276885 -0.037476 11.00000 -1.20000 AFIX 0 C23 1 -0.175743 1.243478 0.055566 11.00000 0.02951 0.02873 = 0.03485 0.00591 0.00744 0.01172 AFIX 43 H23 2 -0.198159 1.299496 0.063340 11.00000 -1.20000 AFIX 0 C24 1 -0.148782 1.175435 0.104085 11.00000 0.02118 0.02463 = 0.02286 0.00298 0.00693 0.00318 AFIX 43 H24 2 -0.153643 1.185022 0.144629 11.00000 -1.20000 AFIX 0 O1 3 0.086643 0.891735 0.363292 11.00000 0.01877 0.01572 = 0.01752 -0.00020 0.00540 0.00038 O2 3 0.082780 0.745817 0.275586 11.00000 0.01938 0.01821 = 0.01526 0.00208 0.00678 0.00318 O3 3 -0.002272 0.743397 0.161726 11.00000 0.01472 0.01880 = 0.01759 -0.00291 0.00632 0.00040 O4 3 0.081919 0.892445 0.188620 11.00000 0.01956 0.01629 = 0.01889 0.00013 0.00944 -0.00034 O5 3 0.086845 1.039689 0.276576 11.00000 0.01727 0.01930 = 0.01592 -0.00137 0.00562 -0.00383 O6 3 -0.002305 1.039075 0.165772 11.00000 0.01532 0.01791 = 0.01881 0.00374 0.00597 -0.00002 SI1 4 0.069277 0.773969 0.340932 11.00000 0.01453 0.01415 = 0.01356 0.00038 0.00565 0.00020 SI2 4 0.065383 0.774776 0.200781 11.00000 0.01410 0.01448 = 0.01354 0.00001 0.00599 0.00026 SI3 4 0.066191 1.010019 0.201487 11.00000 0.01401 0.01467 = 0.01420 0.00060 0.00622 -0.00080 SI4 4 -0.069948 1.009478 0.159895 11.00000 0.01461 0.01462 = 0.01334 0.00031 0.00510 0.00062 MOLE 2 C25 1 -0.001498 0.318574 0.194771 11.00000 0.01988 0.01631 = 0.01932 -0.00257 0.00706 -0.00006 AFIX 23 H25A 2 0.034173 0.274555 0.207714 11.00000 -1.20000 H25B 2 -0.036242 0.272784 0.186941 11.00000 -1.20000 AFIX 0 C26 1 -0.004236 0.370587 0.133376 11.00000 0.07138 0.02167 = 0.02295 -0.00016 0.02268 0.00223 AFIX 23 H26A 2 -0.040941 0.411741 0.118472 11.00000 -1.20000 H26B 2 0.029670 0.418186 0.140681 11.00000 -1.20000 AFIX 0 C27 1 -0.002938 0.295074 0.083621 11.00000 0.04457 0.02455 = 0.02148 -0.00088 0.01558 0.00007 AFIX 23 H27A 2 -0.036885 0.247790 0.077128 11.00000 -1.20000 H27B 2 0.033505 0.253488 0.099643 11.00000 -1.20000 AFIX 0 C28 1 -0.005009 0.339186 0.020271 11.00000 0.05064 0.03725 = 0.02295 0.00114 0.01660 0.00382 AFIX 33 H28A 2 -0.003382 0.283181 -0.008722 11.00000 -1.50000 H28B 2 0.028783 0.385186 0.025599 11.00000 -1.50000 H28C 2 -0.041776 0.377932 0.002657 11.00000 -1.50000 AFIX 0 C29 1 0.053759 0.460259 0.266722 11.00000 0.01944 0.01535 = 0.02145 -0.00189 0.00777 -0.00259 AFIX 23 H29A 2 0.049568 0.507407 0.230525 11.00000 -1.20000 H29B 2 0.053141 0.502928 0.303484 11.00000 -1.20000 AFIX 0 C30 1 0.113597 0.408863 0.282546 11.00000 0.02118 0.02281 = 0.05087 -0.00007 0.00865 0.00036 AFIX 23 H30A 2 0.117867 0.358668 0.317264 11.00000 -1.20000 H30B 2 0.116473 0.370868 0.244935 11.00000 -1.20000 AFIX 0 C31 1 0.162656 0.486782 0.302520 11.00000 0.02036 0.02553 = 0.02524 0.00012 0.00683 -0.00104 AFIX 23 H31A 2 0.159230 0.524253 0.340076 11.00000 -1.20000 H31B 2 0.157289 0.537460 0.267854 11.00000 -1.20000 AFIX 0 C32 1 0.224319 0.442145 0.318589 11.00000 0.02305 0.04060 = 0.05360 -0.00190 0.01001 0.00173 AFIX 33 H32A 2 0.253433 0.497761 0.330953 11.00000 -1.50000 H32B 2 0.228703 0.406406 0.281409 11.00000 -1.50000 H32C 2 0.230702 0.393400 0.353800 11.00000 -1.50000 AFIX 0 N1 6 0.000000 0.389531 0.250000 10.50000 0.01896 0.01369 = 0.01741 0.00000 0.00694 0.00000 MOLE 3 F1 5 0.000000 0.892155 0.250000 10.50000 0.02162 0.01997 = 0.01828 0.00000 0.00812 0.00000 HKLF 4 Covalent radii and connectivity table for 01SRC394 in C2/c C 0.770 H 0.320 O 0.660 SI 1.170 F 0.640 N 0.700 C1 - C2 C6 Si1 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 Si2 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 Si3 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - C13 C17 C19 - C24 C20 Si4 C20 - C21 C19 C21 - C20 C22 C22 - C21 C23 C23 - C24 C22 C24 - C23 C19 O1 - Si1 Si4_$1 O2 - Si1 Si2 O3 - Si2 Si1_$1 O4 - Si3 Si2 O5 - Si3 Si4_$1 O6 - Si3 Si4 Si1 - O2 O1 O3_$1 C1 Si2 - O4 O2 O3 C7 Si3 - O4 O6 O5 C13 Si4 - O6 O1_$1 O5_$1 C19 C25 - C26 N1 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 - C30 N1 C30 - C31 C29 C31 - C30 C32 C32 - C31 N1 - C25 C25_$1 C29 C29_$1 F1 - no bonds found Operators for generating equivalent atoms: $1 -x, y, -z+1/2 20504 Reflections read, of which 3539 rejected -28 =< h =< 28, -15 =< k =< 15, -25 =< l =< 26, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 3 2 5.02 0.34 4 2.43 3 1 3 40.45 0.22 4 10.41 2 2 3 47.51 0.24 2 764.87 4 2 4 307.65 7.81 3 57.90 5 3 4 44.84 0.64 4 8.87 6 2 5 142.07 0.35 3 287.33 -6 0 6 14.93 0.62 4 3.18 9 3 6 10.78 0.60 3 4.12 5 5 6 25.27 0.44 3 10.77 7 1 7 205.73 5.69 3 29.03 10 2 8 37.39 0.66 3 14.27 4 8 9 70.12 2.99 2 40.37 9 1 10 63.89 0.65 3 33.54 9 1 11 121.51 3.80 3 19.84 -1 3 11 21.10 0.41 6 2.84 -1 5 11 69.64 0.57 2 96.36 13 3 12 0.80 0.35 2 1.81 -1 3 13 184.20 4.76 3 43.74 -2 4 14 78.13 0.72 2 167.26 -2 4 15 38.97 0.89 3 14.33 -3 5 16 120.37 0.83 3 78.76 -3 5 17 16.32 0.82 3 6.06 22 Inconsistent equivalents 5719 Unique reflections, of which 0 suppressed R(int) = 0.0555 R(sigma) = 0.0502 Friedel opposites merged Maximum memory for data reduction = 3831 / 68765 Special position constraints for N1 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for F1 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 4976 / 499230 wR2 = 0.1134 before cycle 1 for 5719 data and 389 / 389 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0532 * P )^2 + 8.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15121 0.00024 -0.017 OSF Mean shift/esd = 0.002 Maximum = -0.017 for OSF Max. shift = 0.000 A for C28 Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4976 / 499230 wR2 = 0.1134 before cycle 2 for 5719 data and 389 / 389 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0532 * P )^2 + 8.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15121 0.00024 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.005 for U12 Si1 Max. shift = 0.000 A for C28 Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4976 / 499230 wR2 = 0.1134 before cycle 3 for 5719 data and 389 / 389 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0532 * P )^2 + 8.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15121 0.00024 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Si3 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4976 / 499230 wR2 = 0.1134 before cycle 4 for 5719 data and 389 / 389 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0532 * P )^2 + 8.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15121 0.00024 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Si3 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C32 Largest correlation matrix elements 0.528 U13 C15 / U33 C15 0.510 U13 C16 / U33 C16 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0578 0.5954 0.4186 43 0.950 0.000 C2 C3 C1 H3 0.1225 0.4787 0.4848 43 0.950 0.000 C3 C4 C2 H4 0.2246 0.5010 0.5091 43 0.950 0.000 C4 C5 C3 H5 0.2611 0.6427 0.4685 43 0.950 0.000 C5 C4 C6 H6 0.1966 0.7588 0.4022 43 0.950 0.000 C6 C5 C1 H8 0.0530 0.5870 0.1226 43 0.950 0.000 C8 C9 C7 H9 0.1174 0.4721 0.0977 43 0.950 0.000 C9 C10 C8 H10 0.2188 0.5075 0.1300 43 0.950 0.000 C10 C11 C9 H11 0.2540 0.6593 0.1843 43 0.950 0.000 C11 C10 C12 H12 0.1899 0.7717 0.2110 43 0.950 0.000 C12 C11 C7 H14 0.0759 1.0319 0.0750 43 0.950 0.000 C14 C15 C13 H15 0.1196 1.1448 0.0222 43 0.950 0.000 C15 C16 C14 H16 0.1799 1.2778 0.0777 43 0.950 0.000 C16 C15 C17 H17 0.1967 1.2942 0.1869 43 0.950 0.000 C17 C16 C18 H18 0.1520 1.1815 0.2392 43 0.950 0.000 C18 C13 C17 H20 -0.0875 1.0260 0.0259 43 0.950 0.000 C20 C21 C19 H21 -0.1345 1.1367 -0.0565 43 0.950 0.000 C21 C20 C22 H22 -0.1882 1.2769 -0.0375 43 0.950 0.000 C22 C21 C23 H23 -0.1982 1.2995 0.0633 43 0.950 0.000 C23 C24 C22 H24 -0.1536 1.1850 0.1446 43 0.950 0.000 C24 C23 C19 H25A 0.0342 0.2746 0.2077 23 0.990 0.000 C25 C26 N1 H25B -0.0362 0.2728 0.1869 23 0.990 0.000 C25 C26 N1 H26A -0.0409 0.4117 0.1185 23 0.990 0.000 C26 C27 C25 H26B 0.0297 0.4182 0.1407 23 0.990 0.000 C26 C27 C25 H27A -0.0369 0.2478 0.0771 23 0.990 0.000 C27 C26 C28 H27B 0.0335 0.2535 0.0996 23 0.990 0.000 C27 C26 C28 H28A -0.0034 0.2832 -0.0087 33 0.980 0.000 C28 C27 H28A H28B 0.0288 0.3852 0.0256 33 0.980 0.000 C28 C27 H28A H28C -0.0418 0.3779 0.0027 33 0.980 0.000 C28 C27 H28A H29A 0.0496 0.5074 0.2305 23 0.990 0.000 C29 C30 N1 H29B 0.0531 0.5029 0.3035 23 0.990 0.000 C29 C30 N1 H30A 0.1179 0.3587 0.3173 23 0.990 0.000 C30 C31 C29 H30B 0.1165 0.3709 0.2449 23 0.990 0.000 C30 C31 C29 H31A 0.1592 0.5243 0.3401 23 0.990 0.000 C31 C30 C32 H31B 0.1573 0.5375 0.2679 23 0.990 0.000 C31 C30 C32 H32A 0.2534 0.4978 0.3310 33 0.980 0.000 C32 C31 H32A H32B 0.2287 0.4064 0.2814 33 0.980 0.000 C32 C31 H32A H32C 0.2307 0.3934 0.3538 33 0.980 0.000 C32 C31 H32A 01SRC394 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.11968 0.68926 0.40198 1.00000 0.01831 0.01692 0.01240 -0.00229 0.00560 0.00133 0.01569 0.00405 0.00009 0.00016 0.00009 0.00000 0.00114 0.00108 0.00105 0.00089 0.00088 0.00089 0.00046 C2 0.09916 0.60525 0.42811 1.00000 0.01833 0.02292 0.01931 0.00046 0.00839 0.00017 0.01961 0.00439 0.00010 0.00017 0.00010 0.00000 0.00118 0.00121 0.00118 0.00095 0.00095 0.00093 0.00049 H2 0.05780 0.59541 0.41856 1.00000 0.02353 0.00000 0.00000 C3 0.13763 0.53546 0.46777 1.00000 0.02852 0.02409 0.02443 0.00684 0.01272 0.00098 0.02465 0.00473 0.00010 0.00018 0.00011 0.00000 0.00135 0.00126 0.00128 0.00103 0.00106 0.00105 0.00053 H3 0.12247 0.47866 0.48476 1.00000 0.02959 0.00000 0.00000 C4 0.19818 0.54893 0.48249 1.00000 0.02797 0.02508 0.01842 0.00433 0.00367 0.00816 0.02464 0.00462 0.00010 0.00018 0.00011 0.00000 0.00131 0.00129 0.00120 0.00100 0.00100 0.00104 0.00053 H4 0.22464 0.50101 0.50912 1.00000 0.02957 0.00000 0.00000 C5 0.21971 0.63253 0.45813 1.00000 0.01711 0.03235 0.02700 0.00128 0.00289 0.00019 0.02640 0.00467 0.00010 0.00019 0.00011 0.00000 0.00122 0.00137 0.00132 0.00110 0.00101 0.00103 0.00055 H5 0.26112 0.64270 0.46853 1.00000 0.03169 0.00000 0.00000 C6 0.18105 0.70159 0.41856 1.00000 0.02172 0.02234 0.02310 0.00384 0.00509 -0.00241 0.02282 0.00441 0.00010 0.00018 0.00011 0.00000 0.00124 0.00122 0.00123 0.00100 0.00100 0.00098 0.00052 H6 0.19655 0.75876 0.40225 1.00000 0.02738 0.00000 0.00000 C7 0.11414 0.69110 0.17049 1.00000 0.01809 0.01918 0.01151 0.00355 0.00606 0.00203 0.01593 0.00416 0.00009 0.00016 0.00009 0.00000 0.00113 0.00113 0.00104 0.00090 0.00088 0.00090 0.00046 C8 0.09414 0.60160 0.13606 1.00000 0.02079 0.02380 0.01675 -0.00016 0.00682 0.00169 0.02022 0.00440 0.00010 0.00017 0.00010 0.00000 0.00121 0.00123 0.00115 0.00096 0.00096 0.00095 0.00050 H8 0.05303 0.58696 0.12256 1.00000 0.02427 0.00000 0.00000 C9 0.13227 0.53303 0.12079 1.00000 0.03673 0.02294 0.02441 -0.00313 0.01137 0.00504 0.02760 0.00495 0.00011 0.00019 0.00011 0.00000 0.00150 0.00127 0.00131 0.00104 0.00113 0.00110 0.00057 H9 0.11743 0.47209 0.09767 1.00000 0.03312 0.00000 0.00000 C10 0.19215 0.55437 0.13961 1.00000 0.03310 0.04067 0.02805 0.00102 0.01653 0.01817 0.03233 0.00530 0.00011 0.00021 0.00012 0.00000 0.00147 0.00159 0.00137 0.00121 0.00117 0.00123 0.00062 H10 0.21876 0.50755 0.12998 1.00000 0.03879 0.00000 0.00000 C11 0.21308 0.64372 0.17236 1.00000 0.01822 0.05639 0.03740 -0.00901 0.01182 0.00327 0.03661 0.00534 0.00011 0.00023 0.00013 0.00000 0.00131 0.00179 0.00152 0.00139 0.00115 0.00123 0.00065 H11 0.25404 0.65926 0.18430 1.00000 0.04393 0.00000 0.00000 C12 0.17470 0.71087 0.18792 1.00000 0.02069 0.03464 0.02989 -0.01038 0.01058 -0.00387 0.02779 0.00475 0.00010 0.00019 0.00012 0.00000 0.00126 0.00142 0.00136 0.00112 0.00107 0.00105 0.00057 H12 0.18987 0.77174 0.21096 1.00000 0.03334 0.00000 0.00000 C13 0.10846 1.09462 0.16332 1.00000 0.01483 0.01521 0.02098 0.00186 0.00896 0.00376 0.01622 0.00425 0.00009 0.00016 0.00010 0.00000 0.00109 0.00110 0.00116 0.00090 0.00092 0.00086 0.00047 C14 0.10017 1.08565 0.09814 1.00000 0.02663 0.02398 0.02502 -0.00433 0.01304 -0.00415 0.02406 0.00471 0.00010 0.00018 0.00011 0.00000 0.00130 0.00127 0.00129 0.00102 0.00105 0.00100 0.00053 H14 0.07586 1.03186 0.07500 1.00000 0.02888 0.00000 0.00000 C15 0.12629 1.15269 0.06651 1.00000 0.03662 0.03160 0.02512 0.00163 0.02098 0.00020 0.02850 0.00505 0.00011 0.00019 0.00011 0.00000 0.00149 0.00139 0.00129 0.00112 0.00116 0.00116 0.00057 H15 0.11963 1.14482 0.02225 1.00000 0.03420 0.00000 0.00000 C16 0.16209 1.23115 0.09928 1.00000 0.03051 0.02486 0.03981 0.00630 0.02348 -0.00193 0.02884 0.00503 0.00011 0.00018 0.00012 0.00000 0.00142 0.00132 0.00154 0.00113 0.00123 0.00108 0.00059 H16 0.17987 1.27780 0.07770 1.00000 0.03461 0.00000 0.00000 C17 0.17177 1.24107 0.16379 1.00000 0.02919 0.02759 0.03675 -0.00189 0.01274 -0.01049 0.03061 0.00499 0.00011 0.00019 0.00012 0.00000 0.00139 0.00135 0.00151 0.00116 0.00119 0.00111 0.00059 H17 0.19673 1.29419 0.18686 1.00000 0.03673 0.00000 0.00000 C18 0.14502 1.17346 0.19490 1.00000 0.02233 0.02858 0.02091 -0.00079 0.00866 -0.00228 0.02350 0.00451 0.00010 0.00018 0.00011 0.00000 0.00125 0.00131 0.00119 0.00103 0.00099 0.00102 0.00052 H18 0.15201 1.18152 0.23921 1.00000 0.02820 0.00000 0.00000 C19 -0.11477 1.09344 0.09489 1.00000 0.01497 0.01729 0.01769 -0.00131 0.00390 -0.00290 0.01692 0.00409 0.00009 0.00016 0.00010 0.00000 0.00110 0.00112 0.00112 0.00090 0.00089 0.00087 0.00047 C20 -0.11023 1.08145 0.03379 1.00000 0.03223 0.02452 0.02055 0.00005 0.00644 0.00497 0.02618 0.00468 0.00011 0.00019 0.00011 0.00000 0.00139 0.00127 0.00125 0.00102 0.00106 0.00105 0.00055 H20 -0.08751 1.02602 0.02585 1.00000 0.03141 0.00000 0.00000 C21 -0.13774 1.14765 -0.01534 1.00000 0.03936 0.03799 0.01554 0.00154 0.00440 -0.00047 0.03192 0.00495 0.00012 0.00020 0.00011 0.00000 0.00155 0.00149 0.00122 0.00112 0.00111 0.00124 0.00060 H21 -0.13447 1.13669 -0.05646 1.00000 0.03831 0.00000 0.00000 C22 -0.17007 1.22997 -0.00429 1.00000 0.03518 0.03186 0.02748 0.01295 -0.00073 0.00441 0.03392 0.00509 0.00011 0.00020 0.00012 0.00000 0.00152 0.00145 0.00140 0.00116 0.00117 0.00117 0.00063 H22 -0.18825 1.27688 -0.03748 1.00000 0.04070 0.00000 0.00000 C23 -0.17574 1.24348 0.05557 1.00000 0.02951 0.02873 0.03485 0.00591 0.00744 0.01172 0.03163 0.00508 0.00011 0.00020 0.00012 0.00000 0.00141 0.00138 0.00151 0.00118 0.00118 0.00112 0.00060 H23 -0.19816 1.29950 0.06334 1.00000 0.03795 0.00000 0.00000 C24 -0.14878 1.17543 0.10408 1.00000 0.02118 0.02463 0.02286 0.00298 0.00693 0.00318 0.02287 0.00450 0.00010 0.00018 0.00011 0.00000 0.00124 0.00125 0.00122 0.00101 0.00099 0.00098 0.00052 H24 -0.15364 1.18502 0.14463 1.00000 0.02745 0.00000 0.00000 O1 0.08664 0.89174 0.36329 1.00000 0.01877 0.01572 0.01752 -0.00020 0.00540 0.00038 0.01740 0.00280 0.00006 0.00011 0.00007 0.00000 0.00080 0.00079 0.00079 0.00062 0.00064 0.00061 0.00034 O2 0.08278 0.74582 0.27559 1.00000 0.01938 0.01821 0.01526 0.00208 0.00678 0.00318 0.01730 0.00284 0.00006 0.00011 0.00007 0.00000 0.00079 0.00078 0.00079 0.00062 0.00064 0.00064 0.00034 O3 -0.00227 0.74340 0.16173 1.00000 0.01472 0.01880 0.01759 -0.00291 0.00632 0.00040 0.01674 0.00275 0.00006 0.00011 0.00007 0.00000 0.00077 0.00077 0.00077 0.00064 0.00063 0.00061 0.00033 O4 0.08192 0.89245 0.18862 1.00000 0.01956 0.01629 0.01889 0.00013 0.00944 -0.00034 0.01745 0.00283 0.00006 0.00011 0.00007 0.00000 0.00081 0.00079 0.00080 0.00062 0.00065 0.00061 0.00034 O5 0.08684 1.03969 0.27658 1.00000 0.01727 0.01930 0.01592 -0.00137 0.00562 -0.00383 0.01739 0.00273 0.00006 0.00011 0.00007 0.00000 0.00077 0.00080 0.00079 0.00063 0.00062 0.00064 0.00034 O6 -0.00230 1.03908 0.16577 1.00000 0.01532 0.01791 0.01881 0.00374 0.00597 -0.00002 0.01720 0.00277 0.00006 0.00011 0.00007 0.00000 0.00079 0.00078 0.00078 0.00063 0.00063 0.00061 0.00033 Si1 0.06928 0.77397 0.34093 1.00000 0.01453 0.01415 0.01356 0.00038 0.00565 0.00020 0.01379 0.00112 0.00002 0.00004 0.00003 0.00000 0.00031 0.00031 0.00031 0.00023 0.00025 0.00023 0.00015 Si2 0.06538 0.77478 0.20078 1.00000 0.01410 0.01448 0.01354 0.00001 0.00599 0.00026 0.01365 0.00111 0.00003 0.00004 0.00003 0.00000 0.00031 0.00031 0.00031 0.00023 0.00025 0.00023 0.00015 Si3 0.06619 1.01002 0.20149 1.00000 0.01401 0.01467 0.01420 0.00060 0.00622 -0.00080 0.01387 0.00113 0.00003 0.00004 0.00003 0.00000 0.00031 0.00031 0.00032 0.00023 0.00025 0.00023 0.00015 Si4 -0.06995 1.00948 0.15989 1.00000 0.01462 0.01462 0.01334 0.00031 0.00510 0.00062 0.01402 0.00113 0.00003 0.00004 0.00003 0.00000 0.00032 0.00031 0.00031 0.00023 0.00025 0.00022 0.00015 C25 -0.00150 0.31857 0.19477 1.00000 0.01988 0.01631 0.01932 -0.00257 0.00706 -0.00006 0.01828 0.00423 0.00010 0.00017 0.00010 0.00000 0.00117 0.00111 0.00115 0.00093 0.00093 0.00090 0.00048 H25A 0.03417 0.27456 0.20771 1.00000 0.02194 0.00000 0.00000 H25B -0.03624 0.27278 0.18694 1.00000 0.02194 0.00000 0.00000 C26 -0.00424 0.37059 0.13338 1.00000 0.07138 0.02167 0.02295 -0.00016 0.02268 0.00223 0.03683 0.00564 0.00014 0.00019 0.00011 0.00000 0.00206 0.00133 0.00138 0.00107 0.00137 0.00129 0.00068 H26A -0.04094 0.41174 0.11847 1.00000 0.04419 0.00000 0.00000 H26B 0.02967 0.41819 0.14068 1.00000 0.04419 0.00000 0.00000 C27 -0.00294 0.29507 0.08362 1.00000 0.04457 0.02455 0.02148 -0.00088 0.01558 0.00007 0.02898 0.00498 0.00012 0.00019 0.00011 0.00000 0.00160 0.00132 0.00128 0.00104 0.00117 0.00113 0.00058 H27A -0.03688 0.24779 0.07713 1.00000 0.03478 0.00000 0.00000 H27B 0.03350 0.25349 0.09964 1.00000 0.03478 0.00000 0.00000 C28 -0.00501 0.33919 0.02027 1.00000 0.05064 0.03725 0.02295 0.00114 0.01660 0.00382 0.03577 0.00546 0.00013 0.00021 0.00011 0.00000 0.00176 0.00159 0.00133 0.00117 0.00124 0.00130 0.00065 H28A -0.00338 0.28318 -0.00872 1.00000 0.05365 0.00000 0.00000 H28B 0.02878 0.38519 0.02560 1.00000 0.05365 0.00000 0.00000 H28C -0.04178 0.37793 0.00266 1.00000 0.05365 0.00000 0.00000 C29 0.05376 0.46026 0.26672 1.00000 0.01944 0.01535 0.02145 -0.00189 0.00777 -0.00259 0.01842 0.00418 0.00009 0.00016 0.00010 0.00000 0.00117 0.00111 0.00119 0.00092 0.00094 0.00091 0.00048 H29A 0.04957 0.50741 0.23052 1.00000 0.02211 0.00000 0.00000 H29B 0.05314 0.50293 0.30348 1.00000 0.02211 0.00000 0.00000 C30 0.11360 0.40886 0.28255 1.00000 0.02118 0.02281 0.05087 -0.00007 0.00865 0.00036 0.03221 0.00503 0.00011 0.00018 0.00014 0.00000 0.00132 0.00132 0.00169 0.00119 0.00119 0.00102 0.00061 H30A 0.11787 0.35867 0.31726 1.00000 0.03865 0.00000 0.00000 H30B 0.11647 0.37087 0.24493 1.00000 0.03865 0.00000 0.00000 C31 0.16266 0.48678 0.30252 1.00000 0.02036 0.02553 0.02524 0.00012 0.00683 -0.00104 0.02377 0.00448 0.00010 0.00018 0.00011 0.00000 0.00127 0.00128 0.00129 0.00102 0.00105 0.00097 0.00053 H31A 0.15923 0.52425 0.34008 1.00000 0.02852 0.00000 0.00000 H31B 0.15729 0.53746 0.26785 1.00000 0.02852 0.00000 0.00000 C32 0.22432 0.44215 0.31859 1.00000 0.02305 0.04060 0.05360 -0.00190 0.01001 0.00173 0.03953 0.00547 0.00011 0.00022 0.00014 0.00000 0.00138 0.00164 0.00182 0.00140 0.00126 0.00121 0.00068 H32A 0.25343 0.49776 0.33095 1.00000 0.05930 0.00000 0.00000 H32B 0.22870 0.40641 0.28141 1.00000 0.05930 0.00000 0.00000 H32C 0.23070 0.39340 0.35380 1.00000 0.05930 0.00000 0.00000 N1 0.00000 0.38953 0.25000 0.50000 0.01896 0.01369 0.01741 0.00000 0.00694 0.00000 0.01640 0.00236 0.00000 0.00018 0.00000 0.00000 0.00138 0.00129 0.00134 0.00000 0.00110 0.00000 0.00056 F1 0.00000 0.89216 0.25000 0.50000 0.02162 0.01997 0.01828 0.00000 0.00812 0.00000 0.01952 0.00163 0.00000 0.00013 0.00000 0.00000 0.00097 0.00094 0.00092 0.00000 0.00076 0.00000 0.00039 Final Structure Factor Calculation for 01SRC394 in C2/c Total number of l.s. parameters = 389 Maximum vector length = 511 Memory required = 4587 / 25039 wR2 = 0.1134 before cycle 5 for 5719 data and 0 / 389 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0532 * P )^2 + 8.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0397 for 4545 Fo > 4sig(Fo) and 0.0560 for all 5719 data wR2 = 0.1134, GooF = S = 1.032, Restrained GooF = 1.032 for all data Occupancy sum of asymmetric unit = 43.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0195 0.0170 0.0105 C1 0.0230 0.0207 0.0151 C2 0.0327 0.0261 0.0152 C3 0.0354 0.0241 0.0144 C4 0.0329 0.0297 0.0166 C5 0.0294 0.0208 0.0182 C6 0.0214 0.0168 0.0095 C7 0.0246 0.0201 0.0160 C8 0.0386 0.0269 0.0174 C9 0.0554 0.0293 0.0122 C10 0.0608 0.0341 0.0149 C11 0.0430 0.0218 0.0186 C12 0.0227 0.0158 0.0101 C13 0.0328 0.0210 0.0184 C14 0.0410 0.0316 0.0129 C15 0.0463 0.0277 0.0126 C16 0.0397 0.0350 0.0171 C17 0.0294 0.0225 0.0186 C18 0.0193 0.0186 0.0129 C19 0.0359 0.0221 0.0205 C20 0.0425 0.0379 0.0154 C21 0.0496 0.0379 0.0143 C22 0.0409 0.0371 0.0169 C23 0.0274 0.0221 0.0191 C24 0.0190 0.0175 0.0156 O1 0.0223 0.0156 0.0140 O2 0.0212 0.0162 0.0128 O3 0.0219 0.0164 0.0141 O4 0.0223 0.0156 0.0143 O5 0.0222 0.0157 0.0137 O6 0.0152 0.0141 0.0121 Si1 0.0152 0.0144 0.0113 Si2 0.0155 0.0150 0.0111 Si3 0.0153 0.0141 0.0127 Si4 0.0210 0.0193 0.0145 C25 0.0715 0.0218 0.0172 C26 0.0447 0.0247 0.0176 C27 0.0517 0.0362 0.0194 C28 0.0227 0.0185 0.0141 C29 0.0528 0.0229 0.0210 C30 0.0260 0.0252 0.0201 C31 0.0556 0.0404 0.0226 C32 0.0194 0.0161 0.0137 N1 0.0220 0.0200 0.0165 F1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.041 0.056 0.075 0.100 0.129 0.172 0.251 1.000 Number in group 617. 549. 576. 550. 574. 583. 571. 562. 560. 577. GooF 0.921 1.021 1.006 1.050 1.105 1.138 1.112 1.003 0.976 0.970 K 1.759 1.058 0.980 0.966 0.978 0.979 0.990 1.005 1.023 1.006 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.81 inf Number in group 580. 573. 584. 563. 566. 571. 576. 564. 566. 576. GooF 0.883 0.886 0.887 0.835 0.859 0.865 0.924 0.970 1.283 1.632 K 1.035 1.025 1.028 1.025 1.011 1.002 1.006 0.997 1.034 0.989 R1 0.093 0.089 0.083 0.066 0.060 0.046 0.037 0.036 0.045 0.045 Recommended weighting scheme: WGHT 0.0509 8.7240 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 5 0 1326.55 2759.02 7.58 0.125 2.58 8 0 0 2038.50 3794.34 6.40 0.146 2.83 6 4 0 1204.03 618.34 5.98 0.059 2.46 -8 0 10 2850.35 1681.71 5.84 0.097 2.02 8 0 4 2000.64 1244.57 4.91 0.084 2.22 2 0 10 2939.06 1988.33 4.78 0.106 1.96 -8 0 12 314.97 37.49 4.67 0.015 1.76 -1 3 9 343.79 94.27 4.56 0.023 2.10 -9 3 7 110.87 348.86 4.54 0.044 2.04 -7 3 9 340.96 126.23 4.47 0.027 2.00 -9 3 1 3829.31 2724.12 4.36 0.124 2.23 4 6 0 1844.93 1226.75 4.35 0.083 2.02 2 0 8 385.59 736.47 4.27 0.064 2.41 -17 1 1 504.17 920.49 4.17 0.072 1.35 -19 1 12 368.50 40.26 4.14 0.015 1.17 -5 1 9 119.34 18.35 4.07 0.010 2.37 -1 1 9 113.54 20.40 4.06 0.011 2.37 5 3 6 837.45 495.87 4.05 0.053 2.12 -2 0 8 29.17 166.98 4.05 0.031 2.76 -15 1 9 409.40 147.27 3.98 0.029 1.49 5 5 0 1957.77 2755.98 3.98 0.124 2.25 -5 9 6 4971.51 3704.61 3.97 0.144 1.32 0 6 2 1350.81 877.49 3.93 0.070 2.12 10 0 4 6742.39 5081.52 3.91 0.169 1.88 0 6 5 1638.57 1094.42 3.86 0.078 1.93 -14 2 3 2225.41 1509.86 3.83 0.092 1.64 9 3 2 736.94 409.35 3.76 0.048 2.03 -6 6 5 250.43 501.21 3.64 0.053 1.82 -2 0 10 27332.67 22149.25 3.60 0.353 2.20 -9 3 6 898.54 573.26 3.57 0.057 2.12 10 2 6 4944.56 3829.58 3.56 0.147 1.63 -14 2 1 14934.38 11605.88 3.55 0.255 1.60 -2 6 5 1012.31 628.39 3.53 0.059 1.95 10 0 0 65701.66 50155.64 3.47 0.531 2.26 11 1 3 13719.74 10965.03 3.37 0.248 1.81 -2 6 2 1465.79 1037.21 3.36 0.076 2.11 -5 3 3 78.67 9.66 3.35 0.007 3.12 -10 0 4 3431.76 2543.94 3.32 0.120 2.36 9 5 3 624.83 387.91 3.27 0.047 1.66 10 4 6 497.36 931.74 3.23 0.072 1.49 -16 6 21 211.85 595.66 3.22 0.058 0.89 9 1 2 1201.12 847.52 3.20 0.069 2.26 -3 3 8 1185.09 844.86 3.16 0.069 2.33 -11 3 1 105.07 9.25 3.16 0.007 1.90 8 2 11 53.12 1.53 3.16 0.003 1.37 -4 0 10 29943.06 24448.00 3.13 0.371 2.21 4 4 10 149.59 375.78 3.10 0.046 1.57 12 2 3 5236.83 4153.24 3.09 0.153 1.64 -1 1 10 1035.90 738.63 3.07 0.064 2.13 1 1 21 4896.50 3763.25 3.06 0.145 0.99 Bond lengths and angles C1 - Distance Angles C2 1.3941 (0.0030) C6 1.4016 (0.0031) 116.93 (0.20) Si1 1.8640 (0.0021) 122.32 (0.17) 120.42 (0.16) C1 - C2 C6 C2 - Distance Angles C3 1.3908 (0.0032) C1 1.3941 (0.0030) 121.77 (0.21) C2 - C3 C3 - Distance Angles C4 1.3875 (0.0033) C2 1.3908 (0.0032) 119.89 (0.21) C3 - C4 C4 - Distance Angles C5 1.3814 (0.0034) C3 1.3875 (0.0033) 119.53 (0.21) C4 - C5 C5 - Distance Angles C4 1.3814 (0.0034) C6 1.3859 (0.0032) 120.18 (0.22) C5 - C4 C6 - Distance Angles C5 1.3859 (0.0032) C1 1.4016 (0.0031) 121.68 (0.21) C6 - C5 C7 - Distance Angles C8 1.3916 (0.0030) C12 1.3965 (0.0031) 116.96 (0.20) Si2 1.8628 (0.0022) 122.72 (0.17) 119.96 (0.17) C7 - C8 C12 C8 - Distance Angles C9 1.3879 (0.0032) C7 1.3916 (0.0030) 122.17 (0.22) C8 - C9 C9 - Distance Angles C10 1.3841 (0.0035) C8 1.3879 (0.0032) 119.30 (0.23) C9 - C10 C10 - Distance Angles C11 1.3780 (0.0038) C9 1.3841 (0.0035) 119.84 (0.22) C10 - C11 C11 - Distance Angles C10 1.3780 (0.0038) C12 1.3835 (0.0034) 120.30 (0.24) C11 - C10 C12 - Distance Angles C11 1.3835 (0.0034) C7 1.3965 (0.0031) 121.41 (0.23) C12 - C11 C13 - Distance Angles C18 1.3854 (0.0031) C14 1.4015 (0.0031) 116.57 (0.20) Si3 1.8632 (0.0022) 123.41 (0.17) 119.81 (0.16) C13 - C18 C14 C14 - Distance Angles C15 1.3823 (0.0033) C13 1.4015 (0.0031) 122.00 (0.22) C14 - C15 C15 - Distance Angles C16 1.3819 (0.0035) C14 1.3823 (0.0033) 120.00 (0.22) C15 - C16 C16 - Distance Angles C15 1.3819 (0.0035) C17 1.3825 (0.0035) 119.32 (0.22) C16 - C15 C17 - Distance Angles C16 1.3825 (0.0035) C18 1.3886 (0.0033) 120.05 (0.23) C17 - C16 C18 - Distance Angles C13 1.3854 (0.0031) C17 1.3886 (0.0033) 122.04 (0.22) C18 - C13 C19 - Distance Angles C24 1.3918 (0.0031) C20 1.4015 (0.0032) 116.79 (0.20) Si4 1.8575 (0.0022) 123.81 (0.17) 119.10 (0.17) C19 - C24 C20 C20 - Distance Angles C21 1.3828 (0.0034) C19 1.4015 (0.0032) 122.16 (0.23) C20 - C21 C21 - Distance Angles C20 1.3828 (0.0034) C22 1.3841 (0.0036) 119.66 (0.23) C21 - C20 C22 - Distance Angles C21 1.3841 (0.0036) C23 1.3869 (0.0036) 119.54 (0.23) C22 - C21 C23 - Distance Angles C24 1.3864 (0.0033) C22 1.3869 (0.0036) 120.16 (0.23) C23 - C24 C24 - Distance Angles C23 1.3864 (0.0033) C19 1.3918 (0.0031) 121.66 (0.22) C24 - C23 O1 - Distance Angles Si1 1.6224 (0.0015) Si4_$1 1.6240 (0.0015) 141.11 (0.10) O1 - Si1 O2 - Distance Angles Si1 1.6213 (0.0015) Si2 1.6241 (0.0015) 143.36 (0.10) O2 - Si1 O3 - Distance Angles Si2 1.6264 (0.0015) Si1_$1 1.6284 (0.0015) 139.11 (0.10) O3 - Si2 O4 - Distance Angles Si3 1.6198 (0.0015) Si2 1.6227 (0.0015) 141.11 (0.10) O4 - Si3 O5 - Distance Angles Si3 1.6291 (0.0015) Si4_$1 1.6295 (0.0015) 138.56 (0.10) O5 - Si3 O6 - Distance Angles Si3 1.6211 (0.0015) Si4 1.6222 (0.0015) 143.88 (0.10) O6 - Si3 Si1 - Distance Angles O2 1.6213 (0.0015) O1 1.6224 (0.0015) 112.55 (0.08) O3_$1 1.6284 (0.0015) 112.21 (0.08) 113.27 (0.08) C1 1.8640 (0.0021) 104.69 (0.08) 106.86 (0.09) 106.54 (0.09) Si1 - O2 O1 O3_$1 Si2 - Distance Angles O4 1.6227 (0.0015) O2 1.6241 (0.0015) 112.98 (0.08) O3 1.6264 (0.0015) 113.55 (0.08) 112.40 (0.08) C7 1.8628 (0.0022) 106.22 (0.09) 104.11 (0.08) 106.71 (0.09) Si2 - O4 O2 O3 Si3 - Distance Angles O4 1.6198 (0.0015) O6 1.6211 (0.0015) 112.75 (0.08) O5 1.6291 (0.0015) 113.00 (0.08) 112.45 (0.08) C13 1.8632 (0.0022) 106.81 (0.09) 104.18 (0.09) 106.91 (0.09) Si3 - O4 O6 O5 Si4 - Distance Angles O6 1.6222 (0.0015) O1_$1 1.6240 (0.0015) 112.84 (0.08) O5_$1 1.6295 (0.0015) 112.36 (0.08) 113.50 (0.08) C19 1.8575 (0.0022) 103.86 (0.09) 106.44 (0.09) 107.00 (0.09) Si4 - O6 O1_$1 O5_$1 C25 - Distance Angles C26 1.5034 (0.0031) N1 1.5248 (0.0025) 116.05 (0.18) C25 - C26 C26 - Distance Angles C27 1.4844 (0.0033) C25 1.5034 (0.0031) 111.78 (0.20) C26 - C27 C27 - Distance Angles C26 1.4844 (0.0033) C28 1.5041 (0.0032) 116.12 (0.21) C27 - C26 C28 - Distance Angles C27 1.5041 (0.0032) C28 - C29 - Distance Angles C30 1.5134 (0.0031) N1 1.5255 (0.0025) 116.70 (0.18) C29 - C30 C30 - Distance Angles C31 1.5052 (0.0032) C29 1.5134 (0.0031) 111.12 (0.19) C30 - C31 C31 - Distance Angles C30 1.5052 (0.0032) C32 1.5152 (0.0033) 114.76 (0.21) C31 - C30 C32 - Distance Angles C31 1.5152 (0.0033) C32 - N1 - Distance Angles C25 1.5248 (0.0025) C25_$1 1.5248 (0.0025) 105.57 (0.22) C29 1.5255 (0.0025) 111.56 (0.12) 111.19 (0.12) C29_$1 1.5255 (0.0025) 111.19 (0.12) 111.56 (0.12) 105.89 (0.22) N1 - C25 C25_$1 C29 FMAP and GRID set by program FMAP 2 3 27 GRID -1.042 -1 -2 1.042 1 2 R1 = 0.0559 for 5719 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.4976 0.7221 0.0883 [ 0.85 A from H27A ] Deepest hole -0.39 at 0.4570 0.9125 0.1248 [ 0.16 A from H26A ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4749 / 27465 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0024 0.2221 0.0883 1.00000 0.05 0.50 0.85 H27A 0.91 H27B 0.95 C27 2.13 C28 Q2 1 -0.0025 0.4459 0.1285 1.00000 0.05 0.36 0.81 H26B 0.98 H26A 0.99 C26 2.20 C27 Q3 1 0.0973 0.7231 0.3728 1.00000 0.05 0.34 0.83 C1 1.04 SI1 1.95 C2 1.96 C6 Q4 1 -0.0886 1.0821 0.1325 1.00000 0.05 0.33 0.88 C19 1.13 SI4 1.83 C24 2.03 O6 Q5 1 0.0797 0.8645 0.2014 1.00000 0.05 0.31 0.47 O4 1.21 SI2 1.92 SI3 2.24 O2 Q6 1 -0.0961 1.0616 0.1255 1.00000 0.05 0.31 0.80 C19 1.06 SI4 1.90 C24 1.97 C20 Q7 1 0.0893 0.9190 0.2054 1.00000 0.05 0.30 0.50 O4 1.30 SI3 1.95 SI2 2.24 O5 Q8 1 0.0670 0.7660 0.2482 1.00000 0.05 0.30 0.66 O2 1.05 SI2 2.04 SI1 2.13 O3 Q9 1 0.1604 0.5637 0.3015 1.00000 0.05 0.28 0.80 H31B 1.00 C31 1.00 H31A 2.14 C32 Q10 1 0.0865 1.0161 0.2992 1.00000 0.05 0.26 0.59 O5 1.10 SI4 2.07 SI3 2.15 O1 Q11 1 -0.0044 0.1276 0.0818 1.00000 0.05 0.26 1.73 H27A 1.85 H27B 2.18 O6 2.18 C27 Q12 1 -0.0076 0.4065 0.0170 1.00000 0.05 0.26 0.86 H28C 0.87 H28B 0.88 C28 1.71 H28A Q13 1 0.0666 0.2200 0.1990 1.00000 0.05 0.25 1.11 H25A 1.99 C18 2.01 H18 2.05 C25 Q14 1 -0.0073 0.3277 -0.0276 1.00000 0.05 0.25 0.70 H28A 1.06 C28 1.38 H28C 1.43 H28B Q15 1 0.0695 1.2325 0.0377 1.00000 0.05 0.25 1.67 C15 1.76 H15 1.84 H28A 1.85 H27B Q16 1 -0.0610 0.9824 -0.0122 1.00000 0.05 0.24 1.33 H20 1.34 H14 2.04 C14 2.13 H15 Q17 1 0.0697 0.4439 0.2058 1.00000 0.05 0.24 1.17 H29A 1.50 H26B 1.51 H30B 1.53 C29 Q18 1 0.0848 0.7397 0.1638 1.00000 0.05 0.23 0.92 C7 1.15 SI2 1.93 C8 2.06 O3 Q19 1 -0.0049 0.9736 0.1701 1.00000 0.05 0.23 0.86 O6 1.57 SI4 1.69 SI3 2.04 F1 Q20 1 0.0931 1.1007 0.1379 1.00000 0.05 0.23 0.57 C13 0.97 C14 1.60 H14 1.75 C18 Shortest distances between peaks (including symmetry equivalents) 4 6 0.33 5 7 0.74 1 11 1.24 12 14 1.43 6 10 1.72 4 10 1.73 5 8 1.73 5 18 1.84 2 17 2.01 8 18 2.07 7 19 2.25 13 20 2.28 11 20 2.29 14 15 2.31 10 19 2.32 1 15 2.33 7 8 2.34 4 19 2.37 6 19 2.38 5 19 2.38 7 10 2.45 2 12 2.49 1 13 2.49 7 18 2.50 12 12 2.60 11 15 2.64 4 11 2.65 3 8 2.69 1 20 2.70 15 20 2.72 6 11 2.79 11 19 2.80 7 20 2.81 16 16 2.82 11 16 2.83 15 16 2.84 1 12 2.85 12 15 2.86 16 20 2.86 11 13 2.88 1 14 2.88 11 16 2.89 5 10 2.90 13 17 2.91 9 17 2.96 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 2.89: 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 3.80: Structure factors and derivatives 5.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.88: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.11: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:57:08 Total CPU time: 14.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++