+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:19:59 on 07-Jan-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01src993 in P-1 CELL 0.71073 9.9881 10.8183 10.9540 96.541 91.269 99.439 ZERR 2.00 0.0013 0.0014 0.0018 0.008 0.007 0.007 LATT 1 SFAC C H O SI UNIT 32 72 12 8 V = 1158.99 F(000) = 472.0 Mu = 0.28 mm-1 Cell Wt = 873.62 Rho = 1.252 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.1 0.1 0.1 FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.0533 0.0000 FVAR 0.17396 C1 1 0.088644 0.796884 0.739712 11.00000 0.02670 0.03149 = 0.03887 0.00864 0.00141 0.00156 AFIX 23 H1A 2 0.187851 0.809632 0.728585 11.00000 -1.20000 H1B 2 0.043895 0.760505 0.659097 11.00000 -1.20000 AFIX 0 C2 1 0.048609 0.926073 0.772653 11.00000 0.04506 0.04549 = 0.03875 0.01935 0.01261 0.01400 AFIX 13 H2 2 -0.047686 0.911398 0.798123 11.00000 -1.20000 AFIX 0 C3 1 0.051647 0.996611 0.661642 11.00000 0.07396 0.03967 = 0.05957 0.01445 0.01503 0.01445 AFIX 137 H3A 2 0.144616 1.012073 0.633286 11.00000 -1.50000 H3B 2 0.020757 1.077392 0.683537 11.00000 -1.50000 H3C 2 -0.008455 0.946276 0.595856 11.00000 -1.50000 AFIX 0 C4 1 0.132175 1.004424 0.879329 11.00000 0.07895 0.04166 = 0.05780 0.00231 -0.01805 0.00475 AFIX 137 H4A 2 0.227461 1.021795 0.857425 11.00000 -1.50000 H4B 2 0.124876 0.958090 0.951392 11.00000 -1.50000 H4C 2 0.098428 1.084243 0.898410 11.00000 -1.50000 AFIX 0 C5 1 0.242440 0.356842 0.686345 11.00000 0.03234 0.03912 = 0.02905 0.00736 0.00280 0.00801 AFIX 23 H5A 2 0.330665 0.414786 0.693819 11.00000 -1.20000 H5B 2 0.260965 0.273085 0.703062 11.00000 -1.20000 AFIX 0 C6 1 0.189436 0.344095 0.550358 11.00000 0.04755 0.04580 = 0.03359 0.00426 0.01207 0.00675 AFIX 13 H6 2 0.092624 0.300948 0.545971 11.00000 -1.20000 AFIX 0 C7 1 0.268277 0.263389 0.467518 11.00000 0.06549 0.05775 = 0.03719 0.00061 0.01248 0.01303 AFIX 137 H7A 2 0.232762 0.256996 0.382508 11.00000 -1.50000 H7B 2 0.258776 0.178895 0.493829 11.00000 -1.50000 H7C 2 0.364436 0.301926 0.472482 11.00000 -1.50000 AFIX 0 C8 1 0.192798 0.470684 0.505543 11.00000 0.10287 0.05964 = 0.04182 0.01704 0.01362 0.02695 AFIX 137 H8A 2 0.286955 0.514519 0.507408 11.00000 -1.50000 H8B 2 0.139244 0.520986 0.558873 11.00000 -1.50000 H8C 2 0.154389 0.459135 0.421111 11.00000 -1.50000 AFIX 0 C9 1 0.397385 0.411662 1.147774 11.00000 0.03423 0.04550 = 0.03852 0.01113 0.00701 0.00972 AFIX 23 H9A 2 0.471198 0.464432 1.109073 11.00000 -1.20000 H9B 2 0.404146 0.441529 1.236898 11.00000 -1.20000 AFIX 0 C10 1 0.425078 0.276947 1.131903 11.00000 0.03055 0.03247 = 0.05684 0.01373 0.00507 0.01202 AFIX 13 H10 2 0.344894 0.221153 1.160558 11.00000 -1.20000 AFIX 0 C11 1 0.548657 0.265590 1.209418 11.00000 0.04473 0.06690 = 0.08329 0.02023 0.00476 0.02551 AFIX 137 H11A 2 0.561931 0.177307 1.201455 11.00000 -1.50000 H11B 2 0.535208 0.294142 1.295747 11.00000 -1.50000 H11C 2 0.628922 0.317961 1.181285 11.00000 -1.50000 AFIX 0 C12 1 0.445213 0.230865 0.998490 11.00000 0.06380 0.05537 = 0.07299 0.00147 0.01067 0.01897 AFIX 137 H12A 2 0.364510 0.236779 0.948385 11.00000 -1.50000 H12B 2 0.459340 0.142855 0.991760 11.00000 -1.50000 H12C 2 0.524787 0.283212 0.969200 11.00000 -1.50000 AFIX 0 C13 1 0.262122 0.850709 1.196522 11.00000 0.03693 0.04463 = 0.03428 0.01653 0.00366 0.00707 AFIX 23 H13A 2 0.319924 0.886385 1.132530 11.00000 -1.20000 H13B 2 0.206138 0.914312 1.227063 11.00000 -1.20000 AFIX 0 C14 1 0.356540 0.829595 1.305471 11.00000 0.06330 0.04119 = 0.04239 -0.00406 0.00298 -0.01295 AFIX 13 H14 2 0.397027 0.752579 1.279562 11.00000 -1.20000 AFIX 0 C15 1 0.471408 0.939371 1.332534 11.00000 0.07133 0.09108 = 0.05507 0.00646 -0.00778 -0.00088 AFIX 137 H15A 2 0.435007 1.014861 1.364633 11.00000 -1.50000 H15B 2 0.518490 0.954709 1.256776 11.00000 -1.50000 H15C 2 0.535402 0.919910 1.393787 11.00000 -1.50000 AFIX 0 C16 1 0.275510 0.805572 1.416644 11.00000 0.06414 0.08888 = 0.04118 0.02259 -0.00968 -0.00988 AFIX 137 H16A 2 0.337048 0.800553 1.486171 11.00000 -1.50000 H16B 2 0.212060 0.725815 1.399173 11.00000 -1.50000 H16C 2 0.224510 0.874662 1.437184 11.00000 -1.50000 AFIX 0 O1 3 -0.113170 0.650094 0.859213 11.00000 0.03313 0.03532 = 0.03928 0.01267 0.00665 0.00747 O2 3 0.118750 0.725985 0.982445 11.00000 0.04452 0.03592 = 0.02868 0.01333 0.00142 0.00607 O3 3 0.221177 0.587318 1.130756 11.00000 0.03296 0.02927 = 0.03985 0.00571 0.00049 0.00799 O4 3 0.220690 0.419326 0.937559 11.00000 0.03709 0.04626 = 0.02590 0.01023 0.00210 0.01238 O5 3 -0.004578 0.315607 0.809007 11.00000 0.04090 0.03867 = 0.03458 0.00377 0.00646 0.01290 O6 3 0.103222 0.551072 0.794239 11.00000 0.03639 0.02799 = 0.03523 0.00664 0.01182 0.00866 SI1 4 0.049418 0.679262 0.847339 11.00000 0.03360 0.03396 = 0.02755 0.01123 0.00399 0.00809 SI2 4 0.137270 0.412317 0.808205 11.00000 0.03149 0.03497 = 0.02727 0.00974 0.00262 0.00836 SI3 4 0.234849 0.442382 1.086243 11.00000 0.03290 0.03533 = 0.03060 0.01111 0.00520 0.00894 SI4 4 0.148642 0.709586 1.124949 11.00000 0.03330 0.03571 = 0.03121 0.00862 0.00346 0.01138 HKLF 4 Covalent radii and connectivity table for 01src993 in P-1 C 0.770 H 0.320 O 0.660 SI 1.170 C1 - C2 Si1 C2 - C3 C4 C1 C3 - C2 C4 - C2 C5 - C6 Si2 C6 - C8 C7 C5 C7 - C6 C8 - C6 C9 - C10 Si3 C10 - C11 C12 C9 C11 - C10 C12 - C10 C13 - C14 Si4 C14 - C16 C15 C13 C15 - C14 C16 - C14 O1 - Si1 Si3_$1 O2 - Si1 Si4 O3 - Si4 Si3 O4 - Si2 Si3 O5 - Si2 Si4_$1 O6 - Si2 Si1 Si1 - O2 O1 O6 C1 Si2 - O6 O4 O5 C5 Si3 - O1_$1 O3 O4 C9 Si4 - O3 O2 O5_$1 C13 Operators for generating equivalent atoms: $1 -x, -y+1, -z+2 12313 Reflections read, of which 1371 rejected -11 =< h =< 11, -12 =< k =< 12, -12 =< l =< 13, 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) 0 2 1 10.13 1.05 4 9.79 1 -3 6 4.92 0.77 2 4.31 4 -3 6 17.03 0.95 3 6.30 0 -5 8 34.59 1.07 2 36.10 0 -5 9 13.32 1.04 2 13.36 1 -4 9 11.83 0.94 3 5.73 6 Inconsistent equivalents 3921 Unique reflections, of which 0 suppressed R(int) = 0.2177 R(sigma) = 0.2690 Friedel opposites merged Maximum memory for data reduction = 2801 / 39108 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 = 3572 / 301473 wR2 = 0.2024 before cycle 1 for 3921 data and 243 / 243 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0533 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17397 0.00059 0.023 OSF Mean shift/esd = 0.007 Maximum = -0.037 for y C15 Max. shift = 0.001 A for H15B Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3572 / 301473 wR2 = 0.2024 before cycle 2 for 3921 data and 243 / 243 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0533 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17398 0.00059 0.008 OSF Mean shift/esd = 0.002 Maximum = -0.012 for y C15 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3572 / 301473 wR2 = 0.2024 before cycle 3 for 3921 data and 243 / 243 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0533 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17398 0.00059 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H15A Max. dU = 0.000 for C15 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3572 / 301473 wR2 = 0.2024 before cycle 4 for 3921 data and 243 / 243 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0533 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17398 0.00059 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U33 O6 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C15 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 H1A 0.1878 0.8096 0.7286 23 0.990 0.000 C1 C2 Si1 H1B 0.0439 0.7605 0.6591 23 0.990 0.000 C1 C2 Si1 H2 -0.0477 0.9114 0.7981 13 1.000 0.000 C2 C3 C4 C1 H3A 0.1446 1.0121 0.6333 137 0.980 0.000 C3 C2 H3A H3B 0.0208 1.0774 0.6835 137 0.980 0.000 C3 C2 H3A H3C -0.0084 0.9463 0.5958 137 0.980 0.000 C3 C2 H3A H4A 0.2275 1.0218 0.8574 137 0.980 0.000 C4 C2 H4A H4B 0.1249 0.9581 0.9514 137 0.980 0.000 C4 C2 H4A H4C 0.0985 1.0842 0.8984 137 0.980 0.000 C4 C2 H4A H5A 0.3307 0.4148 0.6938 23 0.990 0.000 C5 C6 Si2 H5B 0.2610 0.2731 0.7030 23 0.990 0.000 C5 C6 Si2 H6 0.0926 0.3010 0.5460 13 1.000 0.000 C6 C8 C7 C5 H7A 0.2328 0.2570 0.3825 137 0.980 0.000 C7 C6 H7A H7B 0.2588 0.1789 0.4938 137 0.980 0.000 C7 C6 H7A H7C 0.3644 0.3019 0.4725 137 0.980 0.000 C7 C6 H7A H8A 0.2870 0.5145 0.5075 137 0.980 0.000 C8 C6 H8A H8B 0.1392 0.5210 0.5588 137 0.980 0.000 C8 C6 H8A H8C 0.1544 0.4591 0.4211 137 0.980 0.000 C8 C6 H8A H9A 0.4712 0.4644 1.1091 23 0.990 0.000 C9 C10 Si3 H9B 0.4042 0.4415 1.2369 23 0.990 0.000 C9 C10 Si3 H10 0.3449 0.2212 1.1606 13 1.000 0.000 C10 C11 C12 C9 H11A 0.5619 0.1773 1.2015 137 0.980 0.000 C11 C10 H11A H11B 0.5352 0.2942 1.2957 137 0.980 0.000 C11 C10 H11A H11C 0.6289 0.3180 1.1813 137 0.980 0.000 C11 C10 H11A H12A 0.3645 0.2368 0.9484 137 0.980 0.000 C12 C10 H12A H12B 0.4593 0.1429 0.9918 137 0.980 0.000 C12 C10 H12A H12C 0.5248 0.2832 0.9692 137 0.980 0.000 C12 C10 H12A H13A 0.3199 0.8864 1.1325 23 0.990 0.000 C13 C14 Si4 H13B 0.2061 0.9143 1.2271 23 0.990 0.000 C13 C14 Si4 H14 0.3970 0.7526 1.2796 13 1.000 0.000 C14 C16 C15 C13 H15A 0.4350 1.0148 1.3646 137 0.980 0.000 C15 C14 H15A H15B 0.5185 0.9546 1.2568 137 0.980 0.000 C15 C14 H15A H15C 0.5354 0.9199 1.3938 137 0.980 0.000 C15 C14 H15A H16A 0.3371 0.8005 1.4862 137 0.980 0.000 C16 C14 H16A H16B 0.2121 0.7258 1.3992 137 0.980 0.000 C16 C14 H16A H16C 0.2245 0.8746 1.4372 137 0.980 0.000 C16 C14 H16A 01src993 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08864 0.79688 0.73970 1.00000 0.02668 0.03158 0.03889 0.00866 0.00137 0.00160 0.03241 0.01301 0.00069 0.00056 0.00059 0.00000 0.00458 0.00448 0.00448 0.00358 0.00357 0.00361 0.00186 H1A 0.18785 0.80962 0.72857 1.00000 0.03889 0.00000 0.00000 H1B 0.04388 0.76051 0.65909 1.00000 0.03889 0.00000 0.00000 C2 0.04862 0.92607 0.77267 1.00000 0.04510 0.04550 0.03878 0.01938 0.01264 0.01408 0.04110 0.01494 0.00078 0.00066 0.00062 0.00000 0.00534 0.00511 0.00482 0.00416 0.00412 0.00430 0.00207 H2 -0.04767 0.91140 0.79814 1.00000 0.04932 0.00000 0.00000 C3 0.05166 0.99660 0.66163 1.00000 0.07403 0.03967 0.05955 0.01445 0.01505 0.01444 0.05634 0.01591 0.00085 0.00067 0.00068 0.00000 0.00670 0.00494 0.00560 0.00427 0.00489 0.00475 0.00242 H3A 0.14462 1.01205 0.63327 1.00000 0.08452 0.00000 0.00000 H3B 0.02077 1.07738 0.68351 1.00000 0.08452 0.00000 0.00000 H3C -0.00845 0.94625 0.59585 1.00000 0.08452 0.00000 0.00000 C4 0.13219 1.00441 0.87931 1.00000 0.07891 0.04167 0.05777 0.00230 -0.01805 0.00478 0.06065 0.01483 0.00087 0.00071 0.00071 0.00000 0.00699 0.00516 0.00581 0.00455 0.00521 0.00496 0.00254 H4A 0.22747 1.02177 0.85740 1.00000 0.09098 0.00000 0.00000 H4B 0.12489 0.95809 0.95138 1.00000 0.09098 0.00000 0.00000 H4C 0.09846 1.08424 0.89839 1.00000 0.09098 0.00000 0.00000 C5 0.24243 0.35684 0.68634 1.00000 0.03234 0.03912 0.02902 0.00732 0.00279 0.00805 0.03298 0.01335 0.00070 0.00064 0.00055 0.00000 0.00467 0.00441 0.00425 0.00353 0.00349 0.00374 0.00183 H5A 0.33066 0.41479 0.69381 1.00000 0.03958 0.00000 0.00000 H5B 0.26095 0.27308 0.70305 1.00000 0.03958 0.00000 0.00000 C6 0.18942 0.34411 0.55037 1.00000 0.04765 0.04579 0.03360 0.00425 0.01211 0.00686 0.04234 0.01490 0.00080 0.00068 0.00062 0.00000 0.00546 0.00496 0.00454 0.00394 0.00402 0.00433 0.00205 H6 0.09261 0.30096 0.54598 1.00000 0.05080 0.00000 0.00000 C7 0.26828 0.26340 0.46751 1.00000 0.06550 0.05781 0.03726 0.00066 0.01255 0.01301 0.05346 0.01551 0.00084 0.00072 0.00064 0.00000 0.00632 0.00553 0.00502 0.00423 0.00450 0.00494 0.00232 H7A 0.23276 0.25701 0.38250 1.00000 0.08018 0.00000 0.00000 H7B 0.25878 0.17890 0.49382 1.00000 0.08018 0.00000 0.00000 H7C 0.36444 0.30194 0.47248 1.00000 0.08018 0.00000 0.00000 C8 0.19280 0.47069 0.50555 1.00000 0.10293 0.05964 0.04173 0.01699 0.01358 0.02700 0.06557 0.01717 0.00096 0.00071 0.00067 0.00000 0.00790 0.00584 0.00531 0.00451 0.00506 0.00561 0.00268 H8A 0.28695 0.51454 0.50746 1.00000 0.09836 0.00000 0.00000 H8B 0.13921 0.52098 0.55885 1.00000 0.09836 0.00000 0.00000 H8C 0.15444 0.45914 0.42110 1.00000 0.09836 0.00000 0.00000 C9 0.39738 0.41166 1.14776 1.00000 0.03424 0.04550 0.03852 0.01113 0.00695 0.00974 0.03851 0.01350 0.00069 0.00062 0.00061 0.00000 0.00493 0.00493 0.00459 0.00377 0.00377 0.00402 0.00198 H9A 0.47119 0.46443 1.10905 1.00000 0.04622 0.00000 0.00000 H9B 0.40415 0.44154 1.23688 1.00000 0.04622 0.00000 0.00000 C10 0.42508 0.27695 1.13190 1.00000 0.03049 0.03245 0.05688 0.01370 0.00509 0.01199 0.03848 0.01426 0.00072 0.00064 0.00069 0.00000 0.00491 0.00459 0.00534 0.00399 0.00400 0.00382 0.00196 H10 0.34489 0.22116 1.16055 1.00000 0.04617 0.00000 0.00000 C11 0.54865 0.26561 1.20942 1.00000 0.04470 0.06691 0.08338 0.02026 0.00478 0.02553 0.06225 0.01633 0.00080 0.00077 0.00075 0.00000 0.00568 0.00596 0.00660 0.00509 0.00501 0.00489 0.00254 H11A 0.56192 0.17733 1.20147 1.00000 0.09338 0.00000 0.00000 H11B 0.53520 0.29417 1.29575 1.00000 0.09338 0.00000 0.00000 H11C 0.62891 0.31798 1.18128 1.00000 0.09338 0.00000 0.00000 C12 0.44521 0.23088 0.99849 1.00000 0.06381 0.05537 0.07303 0.00141 0.01066 0.01897 0.06342 0.01623 0.00087 0.00075 0.00074 0.00000 0.00675 0.00575 0.00671 0.00488 0.00514 0.00512 0.00257 H12A 0.36453 0.23683 0.94838 1.00000 0.09514 0.00000 0.00000 H12B 0.45931 0.14286 0.99175 1.00000 0.09514 0.00000 0.00000 H12C 0.52481 0.28321 0.96921 1.00000 0.09514 0.00000 0.00000 C13 0.26211 0.85070 1.19652 1.00000 0.03691 0.04463 0.03427 0.01649 0.00364 0.00713 0.03762 0.01326 0.00072 0.00065 0.00061 0.00000 0.00492 0.00470 0.00445 0.00369 0.00373 0.00393 0.00194 H13A 0.31991 0.88638 1.13253 1.00000 0.04514 0.00000 0.00000 H13B 0.20613 0.91430 1.22707 1.00000 0.04514 0.00000 0.00000 C14 0.35655 0.82959 1.30547 1.00000 0.06324 0.04109 0.04244 -0.00406 0.00292 -0.01311 0.05209 0.01490 0.00085 0.00073 0.00067 0.00000 0.00639 0.00512 0.00527 0.00418 0.00474 0.00484 0.00231 H14 0.39702 0.75257 1.27956 1.00000 0.06251 0.00000 0.00000 C15 0.47142 0.93933 1.33252 1.00000 0.07152 0.09123 0.05500 0.00652 -0.00780 -0.00075 0.07454 0.01649 0.00091 0.00086 0.00075 0.00000 0.00748 0.00740 0.00588 0.00533 0.00528 0.00635 0.00287 H15A 0.43503 1.01483 1.36460 1.00000 0.11181 0.00000 0.00000 H15B 0.51851 0.95464 1.25676 1.00000 0.11181 0.00000 0.00000 H15C 0.53540 0.91986 1.39379 1.00000 0.11181 0.00000 0.00000 C16 0.27552 0.80556 1.41665 1.00000 0.06419 0.08884 0.04113 0.02260 -0.00965 -0.00989 0.06631 0.01592 0.00085 0.00082 0.00067 0.00000 0.00672 0.00678 0.00529 0.00491 0.00478 0.00543 0.00267 H16A 0.33706 0.80054 1.48617 1.00000 0.09947 0.00000 0.00000 H16B 0.21208 0.72579 1.39917 1.00000 0.09947 0.00000 0.00000 H16C 0.22451 0.87464 1.43719 1.00000 0.09947 0.00000 0.00000 O1 -0.11317 0.65009 0.85921 1.00000 0.03311 0.03535 0.03928 0.01271 0.00663 0.00747 0.03499 0.00859 0.00045 0.00039 0.00038 0.00000 0.00321 0.00285 0.00296 0.00234 0.00241 0.00245 0.00125 O2 0.11875 0.72599 0.98245 1.00000 0.04460 0.03591 0.02859 0.01331 0.00142 0.00607 0.03571 0.00850 0.00046 0.00038 0.00038 0.00000 0.00326 0.00293 0.00277 0.00225 0.00238 0.00252 0.00125 O3 0.22119 0.58731 1.13076 1.00000 0.03296 0.02923 0.03987 0.00566 0.00047 0.00796 0.03361 0.00837 0.00044 0.00037 0.00038 0.00000 0.00305 0.00282 0.00287 0.00228 0.00231 0.00235 0.00121 O4 0.22069 0.41932 0.93756 1.00000 0.03708 0.04622 0.02588 0.01022 0.00210 0.01239 0.03530 0.00853 0.00045 0.00040 0.00037 0.00000 0.00320 0.00300 0.00272 0.00233 0.00227 0.00253 0.00125 O5 -0.00458 0.31560 0.80900 1.00000 0.04086 0.03867 0.03456 0.00379 0.00647 0.01289 0.03730 0.00886 0.00047 0.00040 0.00038 0.00000 0.00342 0.00296 0.00290 0.00233 0.00247 0.00262 0.00128 O6 0.10322 0.55107 0.79423 1.00000 0.03637 0.02797 0.03519 0.00660 0.01179 0.00865 0.03243 0.00838 0.00044 0.00037 0.00038 0.00000 0.00312 0.00278 0.00279 0.00224 0.00232 0.00239 0.00121 Si1 0.04942 0.67926 0.84734 1.00000 0.03360 0.03398 0.02757 0.01123 0.00400 0.00808 0.03081 0.00405 0.00021 0.00018 0.00018 0.00000 0.00137 0.00128 0.00118 0.00099 0.00098 0.00106 0.00058 Si2 0.13727 0.41232 0.80820 1.00000 0.03152 0.03499 0.02727 0.00974 0.00262 0.00838 0.03045 0.00392 0.00020 0.00018 0.00017 0.00000 0.00137 0.00130 0.00120 0.00097 0.00098 0.00109 0.00058 Si3 0.23485 0.44238 1.08624 1.00000 0.03292 0.03536 0.03060 0.01112 0.00520 0.00897 0.03197 0.00396 0.00021 0.00018 0.00017 0.00000 0.00137 0.00133 0.00125 0.00101 0.00100 0.00107 0.00059 Si4 0.14864 0.70958 1.12495 1.00000 0.03330 0.03573 0.03123 0.00862 0.00346 0.01139 0.03239 0.00393 0.00020 0.00018 0.00017 0.00000 0.00143 0.00134 0.00126 0.00103 0.00104 0.00110 0.00060 Final Structure Factor Calculation for 01src993 in P-1 Total number of l.s. parameters = 243 Maximum vector length = 511 Memory required = 3329 / 22995 wR2 = 0.2024 before cycle 5 for 3921 data and 0 / 243 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0533 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0841 for 1619 Fo > 4sig(Fo) and 0.2189 for all 3921 data wR2 = 0.2024, GooF = S = 0.968, Restrained GooF = 0.968 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0409 0.0313 0.0250 C1 0.0606 0.0378 0.0248 C2 0.0808 0.0531 0.0351 C3 0.0931 0.0488 0.0400 C4 0.0400 0.0313 0.0276 C5 0.0538 0.0456 0.0276 C6 0.0686 0.0597 0.0321 C7 0.1063 0.0554 0.0350 C8 0.0493 0.0360 0.0303 C9 0.0589 0.0340 0.0226 C10 0.0886 0.0660 0.0322 C11 0.0780 0.0673 0.0449 C12 0.0511 0.0368 0.0250 C13 0.0827 0.0449 0.0287 C14 0.1018 0.0718 0.0501 C15 0.1111 0.0542 0.0336 C16 0.0459 0.0318 0.0273 O1 0.0452 0.0412 0.0208 O2 0.0401 0.0340 0.0267 O3 0.0486 0.0341 0.0232 O4 0.0457 0.0368 0.0293 O5 0.0458 0.0266 0.0249 O6 0.0392 0.0317 0.0215 Si1 0.0383 0.0300 0.0230 Si2 0.0413 0.0302 0.0244 Si3 0.0409 0.0299 0.0264 Si4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.038 0.054 0.072 0.095 0.121 0.158 0.231 1.000 Number in group 416. 380. 401. 399. 370. 395. 389. 389. 387. 395. GooF 0.816 0.855 0.872 0.930 0.908 1.020 1.039 1.120 1.087 0.994 K 4.821 1.997 1.280 1.155 1.106 1.028 1.027 1.066 1.036 1.027 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.07 1.15 1.26 1.44 1.80 inf Number in group 400. 394. 383. 398. 389. 395. 385. 393. 390. 394. GooF 0.905 0.829 0.862 0.907 0.882 1.041 1.030 0.924 0.957 1.270 K 1.220 1.203 1.105 1.147 1.059 1.044 1.043 1.006 1.012 1.023 R1 0.485 0.479 0.417 0.350 0.275 0.211 0.159 0.099 0.071 0.064 Recommended weighting scheme: WGHT 0.0531 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 1 802.14 1147.16 5.58 0.298 6.57 2 1 1 145.70 28.22 5.56 0.047 3.82 -2 2 0 930.55 654.98 5.14 0.225 3.95 -4 -1 1 140.17 64.49 4.56 0.071 2.29 5 -1 2 653.08 257.88 4.55 0.141 1.86 4 -3 1 438.54 309.58 4.44 0.155 2.17 4 3 3 304.49 110.05 4.27 0.092 1.61 0 -1 2 243.15 109.63 3.96 0.092 5.09 8 -6 8 908.85 377.40 3.90 0.171 0.87 8 -5 2 198.95 17.10 3.72 0.036 1.13 2 -8 7 2126.94 1437.75 3.67 0.334 1.07 2 -4 2 149.95 100.75 3.35 0.088 2.37 1 2 1 870.31 614.78 3.31 0.218 3.90 0 2 3 464.70 578.58 3.31 0.212 2.84 -2 -2 9 400.87 11.31 3.30 0.030 1.18 -6 -6 2 256.18 31.70 3.29 0.050 1.11 1 5 6 0.00 125.60 3.27 0.099 1.27 4 -7 6 3655.90 2501.81 3.23 0.441 1.16 -6 -2 6 277.20 438.49 3.18 0.184 1.20 -4 8 4 -35.54 117.37 3.15 0.095 1.10 1 -5 11 1117.79 743.57 3.15 0.240 0.94 5 8 3 330.54 39.41 3.14 0.055 0.96 -2 1 11 -18.34 209.77 3.11 0.128 0.97 -2 4 0 -17.92 33.93 3.08 0.051 2.52 8 -4 2 111.95 13.19 3.05 0.032 1.17 1 0 5 1833.63 1511.23 3.00 0.342 2.11 0 8 1 203.68 87.83 2.97 0.083 1.30 -3 -3 12 1085.60 561.27 2.97 0.209 0.87 4 -5 3 80.75 132.38 2.96 0.101 1.63 2 2 8 36.57 119.94 2.93 0.096 1.22 0 3 1 5027.12 2495.93 2.89 0.440 3.25 -8 2 0 129.88 222.64 2.85 0.131 1.25 -3 3 0 41.95 0.16 2.84 0.004 2.63 3 -4 6 4026.58 3201.92 2.82 0.498 1.47 -1 -9 3 140.04 2.48 2.81 0.014 1.13 11 -5 3 217.20 2.48 2.76 0.014 0.86 2 -1 1 187.37 138.66 2.75 0.104 4.40 7 7 1 449.64 196.02 2.73 0.123 0.94 6 -6 3 524.78 397.66 2.71 0.176 1.26 5 -3 8 49.67 182.35 2.70 0.119 1.11 -2 3 8 156.35 32.52 2.69 0.050 1.21 -6 4 7 -52.20 78.80 2.67 0.078 1.07 2 -5 11 741.02 375.91 2.67 0.171 0.93 -8 -7 1 385.99 117.55 2.67 0.096 0.89 6 -9 3 233.42 356.52 2.63 0.166 1.02 7 -3 3 8.72 58.60 2.62 0.067 1.30 6 -5 5 259.14 426.64 2.62 0.182 1.21 2 -8 10 729.46 298.76 2.61 0.152 0.89 1 -6 8 205.49 38.02 2.59 0.054 1.15 4 3 7 106.82 219.71 2.59 0.131 1.14 Bond lengths and angles C1 - Distance Angles C2 1.5225 (0.0085) Si1 1.8334 (0.0060) 118.02 (0.46) C1 - C2 C2 - Distance Angles C3 1.5060 (0.0086) C4 1.5096 (0.0093) 111.14 (0.65) C1 1.5225 (0.0085) 110.67 (0.56) 113.59 (0.61) C2 - C3 C4 C3 - Distance Angles C2 1.5060 (0.0086) C3 - C4 - Distance Angles C2 1.5096 (0.0093) C4 - C5 - Distance Angles C6 1.5530 (0.0088) Si2 1.8253 (0.0066) 119.19 (0.47) C5 - C6 C6 - Distance Angles C8 1.5021 (0.0093) C7 1.5110 (0.0088) 110.47 (0.60) C5 1.5530 (0.0088) 111.75 (0.62) 111.24 (0.56) C6 - C8 C7 C7 - Distance Angles C6 1.5110 (0.0088) C7 - C8 - Distance Angles C6 1.5021 (0.0093) C8 - C9 - Distance Angles C10 1.5190 (0.0086) Si3 1.8383 (0.0066) 118.37 (0.50) C9 - C10 C10 - Distance Angles C11 1.5121 (0.0093) C12 1.5180 (0.0094) 109.40 (0.64) C9 1.5190 (0.0086) 110.69 (0.61) 112.00 (0.61) C10 - C11 C12 C11 - Distance Angles C10 1.5121 (0.0092) C11 - C12 - Distance Angles C10 1.5180 (0.0094) C12 - C13 - Distance Angles C14 1.5650 (0.0093) Si4 1.8304 (0.0072) 115.40 (0.47) C13 - C14 C14 - Distance Angles C16 1.5008 (0.0098) C15 1.5072 (0.0103) 112.11 (0.66) C13 1.5650 (0.0093) 110.49 (0.68) 110.70 (0.59) C14 - C16 C15 C15 - Distance Angles C14 1.5072 (0.0102) C15 - C16 - Distance Angles C14 1.5008 (0.0098) C16 - O1 - Distance Angles Si1 1.6138 (0.0047) Si3_$1 1.6138 (0.0046) 143.70 (0.28) O1 - Si1 O2 - Distance Angles Si1 1.6109 (0.0046) Si4 1.6177 (0.0043) 153.35 (0.30) O2 - Si1 O3 - Distance Angles Si4 1.6157 (0.0043) Si3 1.6166 (0.0044) 151.86 (0.31) O3 - Si4 O4 - Distance Angles Si2 1.6156 (0.0044) Si3 1.6189 (0.0045) 152.50 (0.32) O4 - Si2 O5 - Distance Angles Si2 1.6182 (0.0049) Si4_$1 1.6219 (0.0048) 144.22 (0.30) O5 - Si2 O6 - Distance Angles Si2 1.6154 (0.0043) Si1 1.6202 (0.0044) 152.06 (0.29) O6 - Si2 Si1 - Distance Angles O2 1.6109 (0.0046) O1 1.6138 (0.0048) 108.48 (0.24) O6 1.6202 (0.0044) 108.27 (0.24) 109.55 (0.25) C1 1.8334 (0.0060) 112.89 (0.29) 108.46 (0.27) 109.14 (0.27) Si1 - O2 O1 O6 Si2 - Distance Angles O6 1.6154 (0.0043) O4 1.6156 (0.0044) 108.19 (0.24) O5 1.6182 (0.0050) 108.38 (0.24) 109.52 (0.23) C5 1.8253 (0.0066) 112.63 (0.27) 107.63 (0.27) 110.44 (0.29) Si2 - O6 O4 O5 Si3 - Distance Angles O1_$1 1.6138 (0.0046) O3 1.6166 (0.0044) 109.19 (0.24) O4 1.6189 (0.0045) 108.64 (0.26) 108.58 (0.23) C9 1.8383 (0.0067) 108.51 (0.27) 108.77 (0.28) 113.10 (0.29) Si3 - O1_$1 O3 O4 Si4 - Distance Angles O3 1.6157 (0.0043) O2 1.6177 (0.0043) 108.91 (0.24) O5_$1 1.6219 (0.0049) 108.11 (0.23) 108.39 (0.25) C13 1.8304 (0.0073) 109.58 (0.29) 108.70 (0.27) 113.07 (0.30) Si4 - O3 O2 O5_$1 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.2185 for 3921 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.0547 0.9722 0.1688 [ 1.28 A from H2 ] Deepest hole -0.40 at 0.1056 0.7643 0.1236 [ 0.79 A from SI4 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3173 / 20665 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0547 1.0278 0.8312 1.00000 0.05 0.44 1.28 H2 1.67 H4C 1.71 C2 1.86 H13B Q2 1 0.1235 0.8044 0.6370 1.00000 0.05 0.40 0.91 H1B 1.17 H1A 1.19 C1 2.10 C2 Q3 1 0.4823 0.4399 0.9957 1.00000 0.05 0.38 1.25 H9A 1.66 H9A 1.81 H12C 1.92 C9 Q4 1 0.0557 0.7622 0.8026 1.00000 0.05 0.38 0.87 C1 1.06 SI1 1.57 H1B 1.61 H1A Q5 1 0.1603 0.3478 0.8707 1.00000 0.05 0.37 1.08 SI2 1.09 O4 1.73 O5 2.20 C5 Q6 1 0.5697 0.1718 0.9414 1.00000 0.05 0.36 1.25 H12B 1.36 H12C 1.56 H13A 1.60 C12 Q7 1 0.2952 0.5405 1.1335 1.00000 0.05 0.35 0.96 O3 1.19 SI3 1.88 C9 2.05 H9B Q8 1 0.3410 0.4577 1.3559 1.00000 0.05 0.33 1.47 H9B 1.83 H8A 2.01 H8C 2.24 C8 Q9 1 0.2430 0.1560 0.7724 1.00000 0.05 0.32 1.54 H5B 1.80 H4A 2.13 H4C 2.15 H3A Q10 1 0.0534 0.3526 0.9586 1.00000 0.05 0.32 1.71 O5 1.74 O4 1.95 O2 1.99 SI2 Q11 1 0.1423 0.8100 1.4174 1.00000 0.05 0.32 0.99 H16C 1.24 H16B 1.34 C16 2.09 H16A Q12 1 -0.1282 0.6616 0.9485 1.00000 0.05 0.32 0.99 O1 1.43 SI3 1.79 O4 2.11 SI1 Q13 1 -0.0426 0.9510 0.8869 1.00000 0.05 0.31 1.01 H2 1.59 C2 1.75 C4 1.79 H4B Q14 1 0.0725 0.6819 0.9956 1.00000 0.05 0.31 0.64 O2 1.57 SI4 1.63 SI1 2.26 O5 Q15 1 0.4570 0.4976 1.1748 1.00000 0.05 0.31 0.79 H9A 1.03 C9 1.06 H9B 2.35 C10 Q16 1 0.1215 1.0232 0.7986 1.00000 0.05 0.30 0.94 C4 1.18 C2 1.23 H4A 1.26 H4C Q17 1 -0.0585 0.3040 0.6781 1.00000 0.05 0.30 1.50 O5 1.70 H16B 2.12 H6 2.37 SI4 Q18 1 0.1967 0.5328 1.2066 1.00000 0.05 0.30 1.08 O3 1.64 SI3 2.06 O1 2.32 SI4 Q19 1 0.3218 0.4670 1.2206 1.00000 0.05 0.30 0.93 H9B 1.28 C9 1.66 SI3 1.95 H9A Q20 1 0.2584 0.2997 1.0684 1.00000 0.05 0.30 1.59 SI3 1.70 H10 1.80 O1 1.82 C9 Shortest distances between peaks (including symmetry equivalents) 1 13 1.10 7 18 1.28 3 3 1.28 10 12 1.29 7 19 1.36 10 14 1.37 12 20 1.44 15 19 1.45 5 10 1.46 8 19 1.51 18 19 1.55 11 17 1.63 9 16 1.78 1 16 1.81 7 15 1.81 13 16 2.01 3 15 2.02 2 4 2.02 5 12 2.02 12 14 2.03 3 15 2.12 19 20 2.31 8 15 2.37 4 14 2.39 2 11 2.42 8 18 2.45 5 9 2.50 5 20 2.50 4 13 2.50 10 20 2.53 12 18 2.54 7 12 2.58 7 20 2.59 4 12 2.64 17 18 2.64 13 13 2.64 3 7 2.65 3 20 2.68 15 18 2.71 3 7 2.72 12 19 2.73 7 8 2.74 5 14 2.77 2 16 2.79 15 20 2.80 4 16 2.80 5 17 2.95 18 20 2.95 3 19 2.98 Time profile in seconds ----------------------- 0.11: 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 0.00: Analyse other restraints etc. 0.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.16: Structure factors and derivatives 1.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:20:02 Total elapsed time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++