+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1017 started at 10:52:55 on 07-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1017 in P-1 CELL 0.71073 10.6069 10.7107 10.7782 83.058 64.192 88.751 ZERR 3.00 0.0012 0.0013 0.0015 0.007 0.006 0.009 LATT 1 SFAC C H N O SI UNIT 30 66 6 6 6 V = 1093.62 F(000) = 420.0 Mu = 0.23 mm-1 Cell Wt = 775.43 Rho = 1.177 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.02 0.08 0.14 ACTA BOND $H WGHT 0.00000 8.66980 L.S. 4 TEMP -153.00 FVAR 0.75884 MOLE 1 SI1 5 0.162266 0.327869 0.337738 11.00000 0.02636 0.03039 = 0.02612 -0.00494 -0.01383 0.00143 SI2 5 0.159239 0.770166 0.944365 11.00000 0.03107 0.02799 = 0.02269 -0.00650 -0.00907 0.00026 SI3 5 0.458780 0.828670 0.318622 11.00000 0.03002 0.02740 = 0.02323 -0.00340 -0.01273 -0.00228 O5 4 0.352797 0.621502 0.546595 11.00000 0.03581 0.04302 = 0.02105 -0.00355 -0.01635 -0.00638 O22 4 -0.133617 0.702366 1.111784 11.00000 0.03067 0.02745 = 0.03786 -0.00791 -0.00717 0.00564 O2 4 0.324279 0.510881 0.100080 11.00000 0.04388 0.03829 = 0.02086 -0.00277 -0.01996 -0.00685 N21 3 0.070814 0.621429 0.973700 11.00000 0.03404 0.01595 = 0.02186 -0.00159 -0.01366 -0.00365 N1 3 0.293218 0.440674 0.319295 11.00000 0.03434 0.02665 = 0.02040 -0.00242 -0.01487 -0.00627 C2 1 0.356071 0.516559 0.196211 11.00000 0.02323 0.01854 = 0.02090 -0.00222 -0.00396 0.00007 N4 3 0.428655 0.666144 0.313925 11.00000 0.03329 0.02966 = 0.01615 -0.00133 -0.00921 -0.00381 C6 1 0.347880 0.451970 0.422124 11.00000 0.03054 0.03248 = 0.02608 -0.00559 -0.01662 0.00092 AFIX 23 H6A 2 0.435911 0.405808 0.395925 11.00000 -1.20000 H6B 2 0.279326 0.411715 0.514101 11.00000 -1.20000 AFIX 0 C5 1 0.376209 0.587020 0.433790 11.00000 0.02477 0.03003 = 0.03289 -0.00815 -0.01975 0.00419 C22 1 -0.067554 0.611835 1.058702 11.00000 0.02610 0.03447 = 0.02126 -0.00408 -0.00892 -0.00111 C26 1 0.148425 0.511181 0.913922 11.00000 0.03324 0.03304 = 0.02011 -0.00496 -0.01574 -0.00194 AFIX 23 H26A 2 0.220777 0.495795 0.948258 11.00000 -1.20000 H26B 2 0.198236 0.533851 0.812029 11.00000 -1.20000 AFIX 0 C3 1 0.469339 0.608576 0.182618 11.00000 0.02666 0.02844 = 0.02800 -0.01667 -0.00709 0.00474 AFIX 23 H3A 2 0.557974 0.564160 0.160632 11.00000 -1.20000 H3B 2 0.485399 0.675788 0.105187 11.00000 -1.20000 AFIX 0 C12 1 0.587124 0.848436 0.388592 11.00000 0.03373 0.02561 = 0.02657 -0.00257 -0.00950 -0.00364 AFIX 137 H12A 2 0.546451 0.814240 0.487032 11.00000 -1.50000 H12B 2 0.611059 0.938097 0.378716 11.00000 -1.50000 H12C 2 0.671956 0.803459 0.337151 11.00000 -1.50000 AFIX 0 C28 1 0.345574 0.745066 0.825876 11.00000 0.04608 0.03009 = 0.03135 -0.00323 -0.01923 -0.01309 AFIX 137 H28A 2 0.384082 0.682016 0.872526 11.00000 -1.50000 H28B 2 0.399840 0.824530 0.801513 11.00000 -1.50000 H28C 2 0.350805 0.715449 0.741268 11.00000 -1.50000 AFIX 0 C8 1 0.106244 0.237283 0.513365 11.00000 0.03026 0.02733 = 0.04283 0.00145 -0.01695 -0.00061 AFIX 137 H8A 2 0.188227 0.200636 0.521421 11.00000 -1.50000 H8B 2 0.038998 0.169869 0.526424 11.00000 -1.50000 H8C 2 0.062076 0.293752 0.584521 11.00000 -1.50000 AFIX 0 C27 1 0.147463 0.815400 1.110161 11.00000 0.03763 0.04128 = 0.03193 -0.00394 -0.01276 -0.00833 AFIX 137 H27A 2 0.049311 0.828001 1.172527 11.00000 -1.50000 H27B 2 0.202409 0.893654 1.091290 11.00000 -1.50000 H27C 2 0.184462 0.748390 1.154067 11.00000 -1.50000 AFIX 0 C11 1 0.286861 0.895148 0.420863 11.00000 0.04783 0.02922 = 0.05141 -0.01281 -0.02660 0.00335 AFIX 137 H11A 2 0.224698 0.885516 0.376681 11.00000 -1.50000 H11B 2 0.299892 0.984662 0.424709 11.00000 -1.50000 H11C 2 0.245021 0.850445 0.515301 11.00000 -1.50000 AFIX 0 C29 1 0.084402 0.892231 0.858572 11.00000 0.05508 0.03352 = 0.03259 0.00142 -0.02529 -0.00164 AFIX 137 H29A 2 0.101433 0.870362 0.767001 11.00000 -1.50000 H29B 2 0.129245 0.974430 0.847823 11.00000 -1.50000 H29C 2 -0.016697 0.895877 0.915927 11.00000 -1.50000 AFIX 0 C7 1 0.238915 0.219573 0.201981 11.00000 0.03705 0.03841 = 0.02937 -0.01020 -0.01278 -0.00439 AFIX 137 H7A 2 0.247106 0.262232 0.112944 11.00000 -1.50000 H7B 2 0.177950 0.144004 0.228768 11.00000 -1.50000 H7C 2 0.331950 0.195597 0.192921 11.00000 -1.50000 AFIX 0 C10 1 0.533463 0.902837 0.135628 11.00000 0.07764 0.04011 = 0.02928 0.00002 -0.02637 -0.01331 AFIX 137 H10A 2 0.623303 0.865537 0.082223 11.00000 -1.50000 H10B 2 0.548046 0.993465 0.132189 11.00000 -1.50000 H10C 2 0.468517 0.888714 0.095739 11.00000 -1.50000 AFIX 0 C9 1 0.012125 0.414652 0.328541 11.00000 0.02864 0.04165 = 0.03989 -0.01484 -0.00779 -0.00130 AFIX 137 H9A 2 -0.034530 0.458291 0.410985 11.00000 -1.50000 H9B 2 -0.054601 0.355092 0.324783 11.00000 -1.50000 H9C 2 0.046409 0.476292 0.245008 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src1017 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 Si1 - N1 C9 C8 C7 Si2 - N21 C27 C28 C29 Si3 - N4 C12 C11 C10 O5 - C5 O22 - C22 O2 - C2 N21 - C22 C26 Si2 N1 - C2 C6 Si1 C2 - O2 N1 C3 N4 - C5 C3 Si3 C6 - N1 C5 C5 - O5 N4 C6 C22 - O22 N21 C26_$1 C26 - N21 C22_$1 C3 - N4 C2 C12 - Si3 C28 - Si2 C8 - Si1 C27 - Si2 C11 - Si3 C29 - Si2 C7 - Si1 C10 - Si3 C9 - Si1 Operators for generating equivalent atoms: $1 -x, -y+1, -z+2 15729 Reflections read, of which 57 rejected -13 =< h =< 13, -13 =< k =< 13, -13 =< l =< 13, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 6 3 0 8.69 3.39 4 17.96 5 8 0 0.78 2.12 6 11.66 6 8 0 -20.00 16.50 2 90.73 5 10 0 7.63 14.24 2 86.72 6 5 1 26.77 2.89 7 14.48 5 6 1 19.82 3.72 2 33.81 -11 0 2 16.38 12.15 2 64.36 -2 9 2 33.55 20.87 2 105.30 -7 10 2 69.97 28.18 2 150.89 -2 -7 3 27.61 6.57 3 33.91 -1 -6 3 30.06 13.72 2 69.49 11 -3 3 45.33 16.09 2 96.25 6 10 5 70.18 18.11 2 101.15 -4 -5 6 8.99 2.28 3 18.03 14 Inconsistent equivalents 4889 Unique reflections, of which 0 suppressed R(int) = 0.1521 R(sigma) = 0.1966 Friedel opposites merged Maximum memory for data reduction = 2799 / 48752 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 = 3511 / 281092 wR2 = 0.2719 before cycle 1 for 4889 data and 226 / 226 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 8.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.75884 0.00265 0.001 OSF Mean shift/su = 0.000 Maximum = 0.003 for U12 Si1 Max. shift = 0.000 A for H10B Max. dU = 0.000 for C27 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3511 / 281092 wR2 = 0.2719 before cycle 2 for 4889 data and 226 / 226 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 8.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.75884 0.00265 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.002 for U12 Si1 Max. shift = 0.000 A for H29B Max. dU = 0.000 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3511 / 281092 wR2 = 0.2719 before cycle 3 for 4889 data and 226 / 226 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 8.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.75884 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U12 Si2 Max. shift = 0.000 A for H10B Max. dU = 0.000 for C28 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3511 / 281092 wR2 = 0.2719 before cycle 4 for 4889 data and 226 / 226 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 8.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.75884 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U33 Si1 Max. shift = 0.000 A for H27B Max. dU = 0.000 for C11 Largest correlation matrix elements -0.604 U13 C5 / U11 C5 -0.578 U13 C6 / U33 C6 -0.565 U13 O2 / U33 O2 -0.597 U13 C5 / U33 C5 -0.577 U13 C10 / U11 C10 -0.564 U13 C28 / U11 C28 -0.594 U13 C29 / U11 C29 -0.574 U13 C11 / U33 C11 -0.564 U13 C10 / U33 C10 -0.591 U13 O2 / U11 O2 -0.572 U13 N21 / U11 N21 -0.560 U12 C5 / U23 C5 -0.587 U13 C26 / U11 C26 -0.572 U13 Si1 / U11 Si1 -0.559 U13 C8 / U33 C8 -0.586 U13 C6 / U11 C6 -0.571 U13 C26 / U33 C26 -0.558 U13 N1 / U33 N1 -0.583 U13 C29 / U33 C29 -0.571 U13 O5 / U11 O5 -0.557 U13 Si1 / U33 Si1 -0.579 U13 C11 / U11 C11 -0.568 U13 N1 / U11 N1 -0.554 U13 Si3 / U11 Si3 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6A 0.4359 0.4058 0.3959 23 0.990 0.000 C6 N1 C5 H6B 0.2793 0.4117 0.5141 23 0.990 0.000 C6 N1 C5 H26A 0.2208 0.4958 0.9483 23 0.990 0.000 C26 N21 C22_$1 H26B 0.1982 0.5339 0.8120 23 0.990 0.000 C26 N21 C22_$1 H3A 0.5580 0.5642 0.1606 23 0.990 0.000 C3 N4 C2 H3B 0.4854 0.6758 0.1052 23 0.990 0.000 C3 N4 C2 H12A 0.5465 0.8142 0.4870 137 0.980 0.000 C12 Si3 H12A H12B 0.6111 0.9381 0.3787 137 0.980 0.000 C12 Si3 H12A H12C 0.6720 0.8035 0.3372 137 0.980 0.000 C12 Si3 H12A H28A 0.3841 0.6820 0.8725 137 0.980 0.000 C28 Si2 H28A H28B 0.3998 0.8245 0.8015 137 0.980 0.000 C28 Si2 H28A H28C 0.3508 0.7154 0.7413 137 0.980 0.000 C28 Si2 H28A H8A 0.1882 0.2006 0.5214 137 0.980 0.000 C8 Si1 H8A H8B 0.0390 0.1699 0.5264 137 0.980 0.000 C8 Si1 H8A H8C 0.0621 0.2938 0.5845 137 0.980 0.000 C8 Si1 H8A H27A 0.0493 0.8280 1.1725 137 0.980 0.000 C27 Si2 H27A H27B 0.2024 0.8937 1.0913 137 0.980 0.000 C27 Si2 H27A H27C 0.1845 0.7484 1.1541 137 0.980 0.000 C27 Si2 H27A H11A 0.2247 0.8855 0.3767 137 0.980 0.000 C11 Si3 H11A H11B 0.2999 0.9847 0.4247 137 0.980 0.000 C11 Si3 H11A H11C 0.2450 0.8504 0.5153 137 0.980 0.000 C11 Si3 H11A H29A 0.1014 0.8704 0.7670 137 0.980 0.000 C29 Si2 H29A H29B 0.1292 0.9744 0.8478 137 0.980 0.000 C29 Si2 H29A H29C -0.0167 0.8959 0.9159 137 0.980 0.000 C29 Si2 H29A H7A 0.2471 0.2622 0.1129 137 0.980 0.000 C7 Si1 H7A H7B 0.1780 0.1440 0.2288 137 0.980 0.000 C7 Si1 H7A H7C 0.3320 0.1956 0.1929 137 0.980 0.000 C7 Si1 H7A H10A 0.6233 0.8655 0.0822 137 0.980 0.000 C10 Si3 H10A H10B 0.5480 0.9935 0.1322 137 0.980 0.000 C10 Si3 H10A H10C 0.4685 0.8887 0.0957 137 0.980 0.000 C10 Si3 H10A H9A -0.0345 0.4583 0.4110 137 0.980 0.000 C9 Si1 H9A H9B -0.0546 0.3551 0.3248 137 0.980 0.000 C9 Si1 H9A H9C 0.0464 0.4763 0.2450 137 0.980 0.000 C9 Si1 H9A 2008src1017 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.16227 0.32787 0.33774 1.00000 0.02636 0.03039 0.02612 -0.00494 -0.01383 0.00143 0.02664 0.00316 0.00023 0.00022 0.00022 0.00000 0.00117 0.00132 0.00115 0.00095 0.00096 0.00098 0.00053 Si2 0.15924 0.77017 0.94437 1.00000 0.03107 0.02799 0.02269 -0.00650 -0.00907 0.00026 0.02789 0.00324 0.00023 0.00022 0.00022 0.00000 0.00123 0.00131 0.00110 0.00093 0.00096 0.00101 0.00054 Si3 0.45878 0.82867 0.31862 1.00000 0.03002 0.02740 0.02323 -0.00340 -0.01273 -0.00228 0.02640 0.00313 0.00023 0.00021 0.00022 0.00000 0.00120 0.00128 0.00111 0.00092 0.00095 0.00098 0.00053 O5 0.35280 0.62150 0.54660 1.00000 0.03581 0.04302 0.02105 -0.00355 -0.01635 -0.00638 0.03178 0.00741 0.00056 0.00052 0.00051 0.00000 0.00314 0.00365 0.00278 0.00249 0.00243 0.00274 0.00134 O22 -0.13362 0.70237 1.11178 1.00000 0.03067 0.02745 0.03786 -0.00791 -0.00717 0.00564 0.03452 0.00827 0.00056 0.00052 0.00056 0.00000 0.00312 0.00331 0.00329 0.00264 0.00265 0.00264 0.00137 O2 0.32428 0.51088 0.10008 1.00000 0.04388 0.03829 0.02086 -0.00277 -0.01996 -0.00685 0.03218 0.00732 0.00057 0.00052 0.00051 0.00000 0.00339 0.00349 0.00278 0.00241 0.00258 0.00275 0.00134 N21 0.07081 0.62143 0.97370 1.00000 0.03404 0.01595 0.02186 -0.00159 -0.01366 -0.00365 0.02342 0.00844 0.00065 0.00055 0.00060 0.00000 0.00371 0.00339 0.00321 0.00258 0.00290 0.00282 0.00140 N1 0.29322 0.44067 0.31930 1.00000 0.03434 0.02665 0.02040 -0.00242 -0.01487 -0.00627 0.02600 0.00857 0.00066 0.00059 0.00060 0.00000 0.00369 0.00372 0.00320 0.00274 0.00290 0.00301 0.00147 C2 0.35607 0.51656 0.19621 1.00000 0.02323 0.01854 0.02090 -0.00222 -0.00396 0.00007 0.02294 0.01087 0.00075 0.00068 0.00072 0.00000 0.00395 0.00413 0.00384 0.00309 0.00321 0.00321 0.00164 N4 0.42865 0.66614 0.31393 1.00000 0.03329 0.02966 0.01615 -0.00133 -0.00921 -0.00381 0.02699 0.00907 0.00066 0.00060 0.00060 0.00000 0.00372 0.00388 0.00310 0.00271 0.00279 0.00304 0.00149 C6 0.34788 0.45197 0.42212 1.00000 0.03054 0.03248 0.02608 -0.00559 -0.01662 0.00092 0.02798 0.01062 0.00083 0.00074 0.00078 0.00000 0.00430 0.00475 0.00411 0.00345 0.00354 0.00363 0.00178 H6A 0.43591 0.40581 0.39593 1.00000 0.03357 0.00000 0.00000 H6B 0.27933 0.41172 0.51410 1.00000 0.03357 0.00000 0.00000 C5 0.37621 0.58702 0.43379 1.00000 0.02477 0.03003 0.03289 -0.00815 -0.01975 0.00419 0.02630 0.01067 0.00077 0.00073 0.00080 0.00000 0.00406 0.00468 0.00441 0.00358 0.00357 0.00349 0.00175 C22 -0.06755 0.61183 1.05870 1.00000 0.02610 0.03447 0.02126 -0.00408 -0.00892 -0.00111 0.02769 0.01132 0.00080 0.00079 0.00075 0.00000 0.00423 0.00496 0.00391 0.00346 0.00340 0.00373 0.00178 C26 0.14843 0.51118 0.91392 1.00000 0.03324 0.03304 0.02011 -0.00496 -0.01574 -0.00194 0.02711 0.01050 0.00081 0.00073 0.00075 0.00000 0.00436 0.00479 0.00379 0.00337 0.00343 0.00374 0.00178 H26A 0.22078 0.49579 0.94826 1.00000 0.03253 0.00000 0.00000 H26B 0.19824 0.53385 0.81203 1.00000 0.03253 0.00000 0.00000 C3 0.46934 0.60858 0.18262 1.00000 0.02666 0.02844 0.02800 -0.01667 -0.00709 0.00474 0.02830 0.01062 0.00079 0.00075 0.00078 0.00000 0.00418 0.00461 0.00418 0.00349 0.00343 0.00351 0.00180 H3A 0.55797 0.56416 0.16063 1.00000 0.03397 0.00000 0.00000 H3B 0.48540 0.67579 0.10519 1.00000 0.03397 0.00000 0.00000 C12 0.58712 0.84844 0.38859 1.00000 0.03373 0.02561 0.02657 -0.00257 -0.00950 -0.00364 0.02994 0.01105 0.00082 0.00075 0.00078 0.00000 0.00454 0.00456 0.00414 0.00342 0.00360 0.00369 0.00184 H12A 0.54645 0.81424 0.48703 1.00000 0.04491 0.00000 0.00000 H12B 0.61106 0.93810 0.37872 1.00000 0.04491 0.00000 0.00000 H12C 0.67196 0.80346 0.33715 1.00000 0.04491 0.00000 0.00000 C28 0.34557 0.74507 0.82588 1.00000 0.04608 0.03009 0.03135 -0.00323 -0.01923 -0.01309 0.03481 0.01129 0.00086 0.00079 0.00081 0.00000 0.00521 0.00485 0.00449 0.00366 0.00406 0.00409 0.00203 H28A 0.38408 0.68202 0.87253 1.00000 0.05222 0.00000 0.00000 H28B 0.39984 0.82453 0.80151 1.00000 0.05222 0.00000 0.00000 H28C 0.35081 0.71545 0.74127 1.00000 0.05222 0.00000 0.00000 C8 0.10624 0.23728 0.51337 1.00000 0.03026 0.02733 0.04283 0.00145 -0.01695 -0.00061 0.03361 0.01219 0.00084 0.00077 0.00084 0.00000 0.00446 0.00481 0.00502 0.00384 0.00400 0.00377 0.00196 H8A 0.18823 0.20064 0.52142 1.00000 0.05041 0.00000 0.00000 H8B 0.03900 0.16987 0.52642 1.00000 0.05041 0.00000 0.00000 H8C 0.06208 0.29375 0.58452 1.00000 0.05041 0.00000 0.00000 C27 0.14746 0.81540 1.11016 1.00000 0.03763 0.04128 0.03193 -0.00394 -0.01276 -0.00833 0.03770 0.01193 0.00091 0.00085 0.00083 0.00000 0.00487 0.00543 0.00459 0.00393 0.00393 0.00418 0.00208 H27A 0.04931 0.82800 1.17253 1.00000 0.05656 0.00000 0.00000 H27B 0.20241 0.89365 1.09129 1.00000 0.05656 0.00000 0.00000 H27C 0.18446 0.74839 1.15407 1.00000 0.05656 0.00000 0.00000 C11 0.28686 0.89515 0.42086 1.00000 0.04782 0.02922 0.05141 -0.01281 -0.02660 0.00335 0.04035 0.01234 0.00091 0.00081 0.00093 0.00000 0.00553 0.00510 0.00560 0.00423 0.00471 0.00428 0.00219 H11A 0.22470 0.88552 0.37668 1.00000 0.06052 0.00000 0.00000 H11B 0.29989 0.98466 0.42471 1.00000 0.06052 0.00000 0.00000 H11C 0.24502 0.85044 0.51530 1.00000 0.06052 0.00000 0.00000 C29 0.08440 0.89223 0.85857 1.00000 0.05508 0.03352 0.03259 0.00142 -0.02529 -0.00164 0.03861 0.01261 0.00097 0.00079 0.00086 0.00000 0.00569 0.00519 0.00467 0.00385 0.00434 0.00437 0.00213 H29A 0.10143 0.87036 0.76700 1.00000 0.05792 0.00000 0.00000 H29B 0.12924 0.97443 0.84782 1.00000 0.05792 0.00000 0.00000 H29C -0.01670 0.89588 0.91593 1.00000 0.05792 0.00000 0.00000 C7 0.23891 0.21957 0.20198 1.00000 0.03705 0.03841 0.02937 -0.01020 -0.01278 -0.00439 0.03492 0.01157 0.00087 0.00080 0.00081 0.00000 0.00481 0.00531 0.00438 0.00379 0.00382 0.00407 0.00201 H7A 0.24711 0.26223 0.11294 1.00000 0.05238 0.00000 0.00000 H7B 0.17795 0.14400 0.22877 1.00000 0.05238 0.00000 0.00000 H7C 0.33195 0.19560 0.19292 1.00000 0.05238 0.00000 0.00000 C10 0.53346 0.90284 0.13563 1.00000 0.07764 0.04011 0.02928 0.00002 -0.02637 -0.01331 0.04805 0.01322 0.00110 0.00088 0.00085 0.00000 0.00720 0.00582 0.00480 0.00410 0.00494 0.00521 0.00255 H10A 0.62330 0.86554 0.08222 1.00000 0.07207 0.00000 0.00000 H10B 0.54805 0.99347 0.13219 1.00000 0.07207 0.00000 0.00000 H10C 0.46852 0.88871 0.09574 1.00000 0.07207 0.00000 0.00000 C9 0.01212 0.41465 0.32854 1.00000 0.02864 0.04165 0.03989 -0.01484 -0.00779 -0.00130 0.03838 0.01235 0.00084 0.00084 0.00090 0.00000 0.00451 0.00557 0.00495 0.00418 0.00390 0.00405 0.00212 H9A -0.03453 0.45829 0.41099 1.00000 0.05756 0.00000 0.00000 H9B -0.05460 0.35509 0.32478 1.00000 0.05756 0.00000 0.00000 H9C 0.04641 0.47629 0.24501 1.00000 0.05756 0.00000 0.00000 Final Structure Factor Calculation for 2008src1017 in P-1 Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 3285 / 24017 wR2 = 0.2719 before cycle 5 for 4889 data and 0 / 226 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 8.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1451 for 2657 Fo > 4sig(Fo) and 0.2538 for all 4889 data wR2 = 0.2719, GooF = S = 1.176, Restrained GooF = 1.176 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0307 0.0275 0.0217 Si1 0.0348 0.0283 0.0206 Si2 0.0324 0.0257 0.0211 Si3 0.0482 0.0315 0.0156 O5 0.0489 0.0327 0.0219 O22 0.0501 0.0330 0.0135 O2 0.0353 0.0202 0.0147 N21 0.0390 0.0234 0.0156 N1 0.0322 0.0187 0.0179 C2 0.0378 0.0273 0.0159 N4 0.0329 0.0316 0.0194 C6 0.0370 0.0269 0.0149 C5 0.0353 0.0267 0.0211 C22 0.0363 0.0307 0.0143 C26 0.0424 0.0297 0.0129 C3 0.0393 0.0270 0.0235 C12 0.0553 0.0308 0.0183 C28 0.0459 0.0289 0.0260 C8 0.0509 0.0323 0.0299 C27 0.0545 0.0417 0.0249 C11 0.0559 0.0355 0.0244 C29 0.0479 0.0332 0.0236 C7 0.0844 0.0352 0.0246 C10 0.0567 0.0315 0.0270 C9 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.033 0.044 0.059 0.074 0.093 0.120 0.173 1.000 Number in group 510. 494. 479. 472. 506. 484. 490. 479. 488. 487. GooF 1.285 1.283 1.257 1.184 1.158 1.214 1.255 1.113 1.034 0.913 K 42.100 6.754 3.003 1.783 1.358 1.190 1.104 1.025 0.989 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.67 inf Number in group 502. 485. 482. 493. 488. 489. 483. 490. 485. 492. GooF 1.317 1.339 1.341 1.230 1.280 1.128 1.085 1.077 0.935 0.927 K 1.654 1.577 1.449 1.264 1.193 1.094 1.026 0.998 0.976 1.023 R1 0.512 0.439 0.442 0.346 0.338 0.233 0.197 0.136 0.090 0.058 Recommended weighting scheme: WGHT 0.0000 8.6697 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)/su Fc/Fc(max) Resolution(A) -4 -6 1 445.34 888.49 4.66 0.227 1.32 -4 9 6 568.82 81.32 4.36 0.069 0.86 11 -6 4 500.66 83.82 3.95 0.070 0.84 9 -8 3 324.81 10.50 3.77 0.025 0.87 -6 -2 8 1.63 126.71 3.73 0.086 0.78 -2 2 11 275.92 15.50 3.66 0.030 0.81 3 10 10 194.90 25.00 3.45 0.038 0.80 1 2 9 363.80 110.24 3.35 0.080 1.12 -5 -6 6 285.48 7.30 3.35 0.021 0.85 -4 8 4 315.97 47.66 3.33 0.052 1.02 11 -4 2 161.53 5.44 3.31 0.018 0.88 -8 -7 2 411.21 110.88 3.30 0.080 0.84 1 -3 12 479.92 170.33 3.28 0.099 0.79 11 -5 3 219.96 8.27 3.25 0.022 0.87 -4 6 7 -23.33 126.28 3.23 0.085 0.92 7 2 8 174.22 403.18 3.21 0.153 1.19 9 -1 2 130.27 3.26 3.19 0.014 1.14 6 7 7 179.44 21.95 3.19 0.036 1.07 0 6 6 125.39 15.58 3.13 0.030 1.27 4 1 13 219.18 8.70 3.10 0.022 0.82 7 -11 3 367.55 65.30 3.08 0.061 0.81 5 -2 13 -102.01 156.58 3.03 0.095 0.80 4 9 10 310.49 107.75 3.02 0.079 0.85 -8 2 2 139.96 0.96 2.99 0.007 1.05 -2 5 8 348.43 98.32 2.94 0.075 1.00 8 -4 4 218.25 1.12 2.94 0.008 1.17 0 -13 2 412.77 77.73 2.94 0.067 0.79 0 -3 9 -60.49 97.10 2.93 0.075 0.99 -5 7 1 -39.76 79.61 2.91 0.068 1.17 7 -11 4 157.86 0.62 2.90 0.006 0.80 10 -2 1 147.05 5.04 2.89 0.017 0.98 -7 -4 6 803.78 285.06 2.86 0.128 0.80 -3 13 2 282.96 0.39 2.86 0.005 0.79 -10 6 1 183.08 10.25 2.85 0.024 0.83 12 4 5 269.80 0.25 2.83 0.004 0.84 -1 8 10 259.40 30.97 2.81 0.042 0.80 12 -5 2 471.83 238.10 2.80 0.117 0.79 -6 9 3 -36.05 72.22 2.79 0.065 0.88 1 -6 8 281.79 514.52 2.79 0.172 0.97 5 -1 13 247.05 2.29 2.79 0.012 0.81 12 -3 10 108.76 5.61 2.79 0.018 0.78 3 13 4 937.74 0.00 2.76 0.001 0.80 3 8 5 87.35 0.87 2.75 0.007 1.18 10 7 6 149.67 27.68 2.75 0.040 0.88 1 -11 5 181.54 2.31 2.74 0.012 0.84 3 -8 9 160.64 10.26 2.74 0.024 0.83 10 -6 7 143.16 0.23 2.72 0.004 0.86 5 6 11 203.88 2.22 2.72 0.011 0.90 8 -7 7 353.28 27.73 2.71 0.040 0.91 4 5 13 290.78 9.29 2.71 0.023 0.79 Bond lengths and angles Si1 - Distance Angles N1 1.7898 (0.0063) C9 1.8603 (0.0086) 108.24 (0.35) C8 1.8653 (0.0081) 106.05 (0.33) 109.95 (0.38) C7 1.8657 (0.0080) 109.89 (0.34) 112.75 (0.38) 109.73 (0.39) Si1 - N1 C9 C8 Si2 - Distance Angles N21 1.7896 (0.0062) C27 1.8590 (0.0081) 110.55 (0.34) C28 1.8632 (0.0086) 105.00 (0.34) 109.63 (0.37) C29 1.8698 (0.0081) 109.80 (0.35) 111.44 (0.41) 110.23 (0.40) Si2 - N21 C27 C28 Si3 - Distance Angles N4 1.7873 (0.0067) C12 1.8471 (0.0077) 111.12 (0.34) C11 1.8520 (0.0089) 107.54 (0.35) 113.07 (0.38) C10 1.8539 (0.0084) 105.84 (0.35) 108.75 (0.41) 110.27 (0.45) Si3 - N4 C12 C11 O5 - Distance Angles C5 1.2321 (0.0083) O5 - O22 - Distance Angles C22 1.2304 (0.0091) O22 - O2 - Distance Angles C2 1.2294 (0.0082) O2 - N21 - Distance Angles C22 1.3480 (0.0094) C26 1.4720 (0.0095) 121.07 (0.61) Si2 1.7896 (0.0062) 117.84 (0.54) 120.99 (0.48) N21 - C22 C26 N1 - Distance Angles C2 1.3630 (0.0089) C6 1.4745 (0.0085) 116.51 (0.60) Si1 1.7898 (0.0063) 117.88 (0.48) 125.41 (0.48) N1 - C2 C6 C2 - Distance Angles O2 1.2294 (0.0082) N1 1.3630 (0.0089) 122.30 (0.66) C3 1.5165 (0.0100) 121.17 (0.64) 116.53 (0.63) C2 - O2 N1 N4 - Distance Angles C5 1.3516 (0.0094) C3 1.4956 (0.0088) 116.83 (0.63) Si3 1.7873 (0.0067) 119.25 (0.50) 123.72 (0.49) N4 - C5 C3 C6 - Distance Angles N1 1.4745 (0.0085) C5 1.5147 (0.0106) 113.20 (0.61) H6A 0.9900 108.94 108.94 H6B 0.9900 108.94 108.94 107.75 C6 - N1 C5 H6A C5 - Distance Angles O5 1.2321 (0.0083) N4 1.3516 (0.0094) 122.51 (0.71) C6 1.5147 (0.0106) 121.34 (0.70) 116.15 (0.64) C5 - O5 N4 C22 - Distance Angles O22 1.2304 (0.0090) N21 1.3480 (0.0094) 121.99 (0.72) C26_$1 1.5145 (0.0107) 117.69 (0.68) 120.25 (0.70) C22 - O22 N21 C26 - Distance Angles N21 1.4720 (0.0095) C22_$1 1.5145 (0.0107) 118.53 (0.63) H26A 0.9900 107.68 107.68 H26B 0.9900 107.68 107.68 107.08 C26 - N21 C22_$1 H26A C3 - Distance Angles N4 1.4956 (0.0088) C2 1.5165 (0.0100) 111.04 (0.59) H3A 0.9900 109.43 109.43 H3B 0.9900 109.43 109.43 108.03 C3 - N4 C2 H3A C12 - Distance Angles Si3 1.8471 (0.0077) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - Si3 H12A H12B C28 - Distance Angles Si2 1.8632 (0.0085) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - Si2 H28A H28B C8 - Distance Angles Si1 1.8653 (0.0081) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - Si1 H8A H8B C27 - Distance Angles Si2 1.8590 (0.0081) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - Si2 H27A H27B C11 - Distance Angles Si3 1.8520 (0.0088) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - Si3 H11A H11B C29 - Distance Angles Si2 1.8698 (0.0081) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - Si2 H29A H29B C7 - Distance Angles Si1 1.8657 (0.0080) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - Si1 H7A H7B C10 - Distance Angles Si3 1.8539 (0.0084) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - Si3 H10A H10B C9 - Distance Angles Si1 1.8603 (0.0086) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - Si1 H9A H9B FMAP and GRID set by program FMAP 2 3 31 GRID -1.786 -2 -2 1.786 2 2 R1 = 0.2530 for 4889 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.56 at 0.0976 0.3863 0.3247 [ 0.94 A from C9 ] Deepest hole -0.49 at 0.5000 0.5000 0.5000 [ 1.92 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3198 / 27198 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0976 0.3863 0.3247 1.00000 0.05 0.56 0.94 C9 0.96 SI1 1.46 H9C 1.55 H9A Q2 1 0.0912 0.8248 0.9239 1.00000 0.05 0.56 0.97 C29 1.00 SI2 1.39 H29C 1.66 H29A Q3 1 0.1980 0.2731 0.2660 1.00000 0.05 0.52 0.90 C7 0.96 SI1 1.52 H7A 1.53 H7B Q4 1 0.4440 0.6280 0.5619 1.00000 0.05 0.50 1.05 O5 1.55 H6A 1.91 C5 2.08 H28C Q5 1 0.1565 0.9633 0.5006 1.00000 0.05 0.49 1.39 H11B 1.50 C11 1.55 H11C 1.55 H11A Q6 1 0.1792 0.9378 1.1085 1.00000 0.05 0.48 0.54 H27B 1.36 C27 1.67 H27A 2.03 H27C Q7 1 0.1205 0.1625 0.1910 1.00000 0.05 0.48 0.88 H7B 1.46 C7 1.59 H7A 2.06 H29C Q8 1 0.5301 0.9001 0.6533 1.00000 0.05 0.47 1.71 H28B 2.00 H11B 2.05 H12A 2.36 H12B Q9 1 0.2355 0.5825 0.6051 1.00000 0.05 0.47 1.18 O5 1.80 C5 1.87 H9B 2.09 H26B Q10 1 -0.1426 0.3014 0.6065 1.00000 0.05 0.47 2.08 H8C 2.16 H11A 2.27 H8B 2.39 H9A Shortest distances between peaks (including symmetry equivalents) 1 3 1.60 3 7 1.89 4 9 2.11 6 7 2.63 1 7 2.90 2 6 2.92 9 10 2.99 2 7 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.70: 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 0.98: Structure factors and derivatives 1.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.14: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1017 finished at 10:52:59 Total CPU time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++