+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src1074a started at 12:47:18 on 30-Sep-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1074a in P2(1)2(1)2(1) CELL 0.71073 10.5375 15.9336 31.3723 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0012 0.0024 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O SI UNIT 224 288 40 8 V = 5267.42 F(000) = 2064.0 Mu = 0.12 mm-1 Cell Wt = 3845.26 Rho = 1.212 MERG 4 OMIT -3.00 41.60 SHEL 7 1.00 FMAP 2 PLAN 20 SIZE 0.03 0.04 0.30 ACTA BOND $H WGHT 0.03270 14.41760 L.S. 10 TEMP -153.00 FVAR 0.06696 MOLE 1 C1 1 0.184528 0.419869 0.056093 11.00000 0.03297 0.05179 = 0.02549 0.01202 0.00163 -0.00126 C2 1 0.168265 0.339740 0.030653 11.00000 0.02943 0.02835 = 0.02305 0.00254 -0.00715 0.00304 AFIX 13 H2 2 0.211295 0.292074 0.045521 11.00000 -1.20000 AFIX 0 C3 1 0.222267 0.349941 -0.014559 11.00000 0.02314 0.04058 = 0.03735 0.00803 -0.00344 0.01282 AFIX 23 H3A 2 0.210655 0.408993 -0.023565 11.00000 -1.20000 H3B 2 0.314635 0.338728 -0.013643 11.00000 -1.20000 AFIX 0 C4 1 0.164188 0.294499 -0.047167 11.00000 0.02818 0.02604 = 0.02663 -0.00570 -0.00024 0.00332 AFIX 13 H4 2 0.199726 0.307009 -0.076032 11.00000 -1.20000 AFIX 0 C5 1 0.081412 0.158742 -0.049199 11.00000 0.02846 0.04834 = 0.01318 0.00081 0.00058 -0.00545 C6 1 0.068032 0.084239 -0.019985 11.00000 0.03362 0.06498 = 0.03786 0.01086 -0.00578 0.00450 AFIX 137 H6A 2 0.141159 0.046926 -0.023639 11.00000 -1.50000 H6B 2 -0.010037 0.053761 -0.026955 11.00000 -1.50000 H6C 2 0.064269 0.103560 0.009645 11.00000 -1.50000 AFIX 0 C7 1 0.092422 0.135722 -0.095331 11.00000 0.02167 0.04264 = 0.03904 0.00883 -0.00499 -0.00927 AFIX 137 H7A 2 0.103349 0.186751 -0.112380 11.00000 -1.50000 H7B 2 0.015214 0.106472 -0.104419 11.00000 -1.50000 H7C 2 0.165906 0.098879 -0.099385 11.00000 -1.50000 AFIX 0 C8 1 0.018254 0.299102 -0.047889 11.00000 0.02540 0.02561 = 0.03548 0.01040 -0.00257 -0.00535 AFIX 13 H8 2 -0.011342 0.321844 -0.075886 11.00000 -1.20000 AFIX 0 C9 1 -0.036092 0.351066 -0.011707 11.00000 0.01025 0.03114 = 0.04763 -0.00737 0.00770 -0.01335 AFIX 23 H9A 2 -0.018486 0.411191 -0.017033 11.00000 -1.20000 H9B 2 -0.129303 0.343520 -0.010742 11.00000 -1.20000 AFIX 0 C10 1 0.020274 0.325971 0.030682 11.00000 0.01537 0.04189 = 0.01487 -0.00879 -0.00523 -0.00956 AFIX 13 H10 2 0.000552 0.265750 0.036737 11.00000 -1.20000 AFIX 0 C11 1 -0.025795 0.380084 0.066826 11.00000 0.02773 0.04343 = 0.02566 0.00309 -0.00698 -0.00438 AFIX 13 H11 2 -0.106444 0.408109 0.057902 11.00000 -1.20000 AFIX 0 C12 1 -0.047962 0.336393 0.108639 11.00000 0.02786 0.04092 = 0.03004 0.00104 -0.00011 -0.00579 AFIX 23 H12A 2 -0.062894 0.378525 0.131284 11.00000 -1.20000 H12B 2 -0.124232 0.300348 0.106544 11.00000 -1.20000 AFIX 0 C13 1 -0.068284 0.157636 0.164716 11.00000 0.02848 0.02016 = 0.01590 -0.00260 0.00576 -0.00520 C14 1 -0.115817 0.122458 0.127735 11.00000 0.03251 0.04657 = 0.03076 0.00314 -0.00239 -0.00196 AFIX 43 H14 2 -0.077887 0.137172 0.101300 11.00000 -1.20000 AFIX 0 C15 1 -0.219281 0.065099 0.127693 11.00000 0.06821 0.02728 = 0.03109 0.00121 -0.02745 0.01555 AFIX 43 H15 2 -0.248847 0.040710 0.101907 11.00000 -1.20000 AFIX 0 C16 1 -0.275007 0.046082 0.165947 11.00000 0.02254 0.04099 = 0.03433 0.00956 -0.00356 0.00411 AFIX 43 H16 2 -0.346724 0.009953 0.166094 11.00000 -1.20000 AFIX 0 C17 1 -0.231433 0.077122 0.204142 11.00000 0.03262 0.03759 = 0.03869 0.00051 0.01212 -0.00236 AFIX 43 H17 2 -0.269088 0.060955 0.230402 11.00000 -1.20000 AFIX 0 C18 1 -0.128191 0.134168 0.202867 11.00000 0.03477 0.02497 = 0.03358 -0.00880 -0.00916 0.00284 AFIX 43 H18 2 -0.098365 0.157442 0.228884 11.00000 -1.20000 AFIX 0 C19 1 0.057207 0.302545 0.211227 11.00000 0.01982 0.01092 = 0.03813 0.00489 0.01091 -0.00333 C20 1 -0.059898 0.338909 0.220234 11.00000 0.03034 0.03624 = 0.01647 -0.00642 -0.00064 -0.01090 AFIX 43 H20 2 -0.129828 0.325901 0.202300 11.00000 -1.20000 AFIX 0 C21 1 -0.078887 0.392181 0.253503 11.00000 0.01476 0.04995 = 0.03248 -0.00156 -0.00380 -0.01365 AFIX 43 H21 2 -0.160502 0.415628 0.258369 11.00000 -1.20000 AFIX 0 C22 1 0.022107 0.412293 0.280497 11.00000 0.05106 0.01748 = 0.04045 -0.00438 0.01451 0.00772 AFIX 43 H22 2 0.010404 0.449827 0.303694 11.00000 -1.20000 AFIX 0 C23 1 0.140671 0.376111 0.272702 11.00000 0.04414 0.03591 = 0.03270 -0.01084 -0.00765 -0.01284 AFIX 43 H23 2 0.209642 0.388239 0.291204 11.00000 -1.20000 AFIX 0 C24 1 0.158734 0.323607 0.238883 11.00000 0.03357 0.03353 = 0.01368 -0.00013 -0.00800 -0.00507 AFIX 43 H24 2 0.240641 0.300803 0.233788 11.00000 -1.20000 AFIX 0 C25 1 0.224177 0.171884 0.157391 11.00000 0.03173 0.07417 = 0.00847 0.01096 0.00437 0.01757 C26 1 0.247866 0.118198 0.197591 11.00000 0.03132 0.05164 = 0.06101 -0.00334 -0.00310 0.00280 AFIX 137 H26A 2 0.327514 0.087099 0.194332 11.00000 -1.50000 H26B 2 0.177644 0.078557 0.201353 11.00000 -1.50000 H26C 2 0.253472 0.154866 0.222599 11.00000 -1.50000 AFIX 0 C27 1 0.334905 0.232491 0.150745 11.00000 0.02127 0.06018 = 0.07095 0.00546 0.00631 0.01137 AFIX 137 H27A 2 0.340297 0.270972 0.175046 11.00000 -1.50000 H27B 2 0.321248 0.264720 0.124537 11.00000 -1.50000 H27C 2 0.414145 0.200630 0.148390 11.00000 -1.50000 AFIX 0 C28 1 0.214082 0.112921 0.119376 11.00000 0.04102 0.03629 = 0.03998 -0.01990 0.01139 0.00957 AFIX 137 H28A 2 0.194566 0.145409 0.093675 11.00000 -1.50000 H28B 2 0.146345 0.071998 0.124491 11.00000 -1.50000 H28C 2 0.294834 0.083389 0.115485 11.00000 -1.50000 AFIX 0 O1 3 0.071220 0.444963 0.073884 11.00000 0.03211 0.03481 = 0.03577 0.00096 0.01570 -0.00418 O2 3 0.277927 0.461780 0.061393 11.00000 0.03337 0.05902 = 0.04973 -0.00717 0.00724 -0.00887 O3 3 0.188829 0.207203 -0.035429 11.00000 0.01729 0.02991 = 0.04339 0.00001 -0.00058 -0.00346 O4 3 -0.023553 0.213245 -0.042971 11.00000 0.02220 0.02815 = 0.03735 0.00114 -0.00102 -0.00132 O5 3 0.059311 0.286522 0.119284 11.00000 0.01387 0.04298 = 0.02996 0.00213 -0.00029 0.00294 SI1 4 0.068312 0.230668 0.163922 11.00000 0.02371 0.03100 = 0.02493 0.00018 0.00054 -0.00349 MOLE 2 C51 1 0.487968 0.423666 0.443499 11.00000 0.03496 0.03017 = 0.03608 0.00023 0.00633 -0.00277 C52 1 0.506035 0.344642 0.471724 11.00000 0.02334 0.02988 = 0.03281 -0.00968 0.00378 0.00390 AFIX 13 H52 2 0.468163 0.294493 0.457389 11.00000 -1.20000 AFIX 0 C53 1 0.443199 0.358598 0.514899 11.00000 0.02072 0.03200 = 0.04263 -0.00523 0.00428 -0.00393 AFIX 23 H53A 2 0.451665 0.418440 0.522900 11.00000 -1.20000 H53B 2 0.351552 0.345753 0.512523 11.00000 -1.20000 AFIX 0 C54 1 0.500663 0.304695 0.549748 11.00000 0.02337 0.03459 = 0.03231 0.00912 -0.00189 -0.00099 AFIX 13 H54 2 0.462871 0.319598 0.577990 11.00000 -1.20000 AFIX 0 C55 1 0.586930 0.169766 0.553416 11.00000 0.03707 0.02834 = 0.01199 0.00603 -0.00967 -0.00109 C56 1 0.598367 0.094861 0.526035 11.00000 0.04681 0.01365 = 0.04652 0.00195 0.00960 -0.00894 AFIX 137 H56A 2 0.525809 0.057645 0.530992 11.00000 -1.50000 H56B 2 0.677158 0.065088 0.532872 11.00000 -1.50000 H56C 2 0.599730 0.112097 0.496052 11.00000 -1.50000 AFIX 0 C57 1 0.577126 0.150381 0.600748 11.00000 0.02024 0.02991 = 0.04225 0.00769 0.00733 -0.00318 AFIX 137 H57A 2 0.560743 0.202357 0.616516 11.00000 -1.50000 H57B 2 0.656902 0.125482 0.610642 11.00000 -1.50000 H57C 2 0.507414 0.110806 0.605598 11.00000 -1.50000 AFIX 0 C58 1 0.648545 0.309570 0.552010 11.00000 0.01896 0.03101 = 0.03535 -0.00408 0.00057 0.00529 AFIX 13 H58 2 0.675993 0.331509 0.580416 11.00000 -1.20000 AFIX 0 C59 1 0.704910 0.363321 0.516154 11.00000 0.02534 0.01359 = 0.03960 0.00788 -0.00683 -0.00416 AFIX 23 H59A 2 0.683513 0.423041 0.521072 11.00000 -1.20000 H59B 2 0.798499 0.357881 0.516268 11.00000 -1.20000 AFIX 0 C60 1 0.653741 0.336027 0.473475 11.00000 0.02324 0.03587 = 0.01624 -0.00215 -0.00506 0.00873 AFIX 13 H60 2 0.676426 0.275737 0.468963 11.00000 -1.20000 AFIX 0 C61 1 0.700146 0.386019 0.435570 11.00000 0.01676 0.03296 = 0.01786 -0.00269 0.00195 -0.00032 AFIX 13 H61 2 0.777952 0.417646 0.444231 11.00000 -1.20000 AFIX 0 C62 1 0.728173 0.339704 0.396315 11.00000 0.02834 0.03903 = 0.03182 -0.00129 -0.00059 -0.00640 AFIX 23 H62A 2 0.743255 0.379600 0.372660 11.00000 -1.20000 H62B 2 0.805798 0.305563 0.400231 11.00000 -1.20000 AFIX 0 C63 1 0.764472 0.162108 0.336358 11.00000 0.02006 0.03695 = 0.02108 0.00052 -0.00450 0.00055 C64 1 0.774331 0.076136 0.342047 11.00000 0.03358 0.03335 = 0.03790 0.01124 0.00502 0.01339 AFIX 43 H64 2 0.702630 0.045035 0.351398 11.00000 -1.20000 AFIX 0 C65 1 0.887404 0.035328 0.334243 11.00000 0.06675 0.01705 = 0.07032 0.01122 0.01294 0.01764 AFIX 43 H65 2 0.892247 -0.023640 0.338412 11.00000 -1.20000 AFIX 0 C66 1 0.995347 0.078818 0.320307 11.00000 0.05193 0.04393 = 0.03860 -0.00672 -0.00402 0.01326 AFIX 43 H66 2 1.072355 0.050158 0.314303 11.00000 -1.20000 AFIX 0 C67 1 0.985759 0.165760 0.315552 11.00000 0.02162 0.06959 = 0.03529 -0.00586 -0.00063 0.00725 AFIX 43 H67 2 1.057875 0.197395 0.307062 11.00000 -1.20000 AFIX 0 C68 1 0.872450 0.205658 0.323108 11.00000 0.02618 0.03744 = 0.02810 0.00298 -0.00176 0.00376 AFIX 43 H68 2 0.867392 0.264687 0.319200 11.00000 -1.20000 AFIX 0 C69 1 0.596601 0.292444 0.295343 11.00000 0.01187 0.03796 = 0.02675 -0.00637 0.00105 -0.00206 C70 1 0.619768 0.258247 0.254998 11.00000 0.02089 0.03800 = 0.02508 0.00457 -0.00309 0.00138 AFIX 43 H70 2 0.650417 0.202306 0.253062 11.00000 -1.20000 AFIX 0 C71 1 0.599763 0.302694 0.218127 11.00000 0.02400 0.03485 = 0.03723 -0.00449 -0.00368 -0.00163 AFIX 43 H71 2 0.617081 0.277677 0.191262 11.00000 -1.20000 AFIX 0 C72 1 0.554219 0.384184 0.220219 11.00000 0.02694 0.05035 = 0.03089 0.02057 -0.00954 -0.00714 AFIX 43 H72 2 0.538090 0.414721 0.194781 11.00000 -1.20000 AFIX 0 C73 1 0.531975 0.421488 0.260152 11.00000 0.03763 0.03978 = 0.04564 0.01745 -0.01381 0.00094 AFIX 43 H73 2 0.501733 0.477555 0.261865 11.00000 -1.20000 AFIX 0 C74 1 0.554324 0.376209 0.296694 11.00000 0.03219 0.02454 = 0.02636 -0.00912 0.00460 -0.00076 AFIX 43 H74 2 0.540873 0.402152 0.323582 11.00000 -1.20000 AFIX 0 C75 1 0.463807 0.162948 0.352635 11.00000 0.01205 0.04250 = 0.02474 -0.00035 -0.00377 -0.00784 C76 1 0.444847 0.101628 0.315344 11.00000 0.04477 0.03585 = 0.04834 0.00033 -0.00316 -0.01323 AFIX 137 H76A 2 0.364079 0.071944 0.318885 11.00000 -1.50000 H76B 2 0.514573 0.060936 0.314922 11.00000 -1.50000 H76C 2 0.443801 0.132913 0.288452 11.00000 -1.50000 AFIX 0 C77 1 0.350948 0.223696 0.352379 11.00000 0.02489 0.04841 = 0.02840 0.00871 -0.00136 0.00404 AFIX 137 H77A 2 0.346135 0.251810 0.324643 11.00000 -1.50000 H77B 2 0.362239 0.265717 0.374872 11.00000 -1.50000 H77C 2 0.272341 0.192385 0.357458 11.00000 -1.50000 AFIX 0 C78 1 0.465642 0.114396 0.394584 11.00000 0.02377 0.03823 = 0.03936 -0.00465 0.00502 0.00306 AFIX 137 H78A 2 0.470429 0.153953 0.418449 11.00000 -1.50000 H78B 2 0.539671 0.077186 0.395188 11.00000 -1.50000 H78C 2 0.388004 0.080882 0.397040 11.00000 -1.50000 AFIX 0 O51 3 0.599251 0.446803 0.425958 11.00000 0.02694 0.02671 = 0.03974 0.00726 0.00811 0.00312 O52 3 0.392865 0.461402 0.437672 11.00000 0.02853 0.03888 = 0.06512 0.01907 -0.00078 0.01411 O53 3 0.477121 0.217857 0.540158 11.00000 0.02273 0.03324 = 0.02835 -0.00141 -0.00510 0.00062 O54 3 0.691146 0.226005 0.546470 11.00000 0.01962 0.03086 = 0.03998 -0.00196 -0.00036 -0.00273 O55 3 0.622396 0.285819 0.386061 11.00000 0.01894 0.05410 = 0.02604 -0.00209 0.00431 -0.00685 SI51 4 0.614156 0.226022 0.344199 11.00000 0.02097 0.03256 = 0.01741 0.00192 -0.00032 -0.00311 HKLF 4 Covalent radii and connectivity table for 2009src1074a in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 SI 1.170 C1 - O2 O1 C2 C2 - C1 C3 C10 C3 - C4 C2 C4 - O3 C3 C8 C5 - O4 O3 C7 C6 C6 - C5 C7 - C5 C8 - O4 C9 C4 C9 - C10 C8 C10 - C11 C9 C2 C11 - O1 C12 C10 C12 - O5 C11 C13 - C14 C18 Si1 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - C13 C17 C19 - C20 C24 Si1 C20 - C21 C19 C21 - C20 C22 C22 - C21 C23 C23 - C24 C22 C24 - C23 C19 C25 - C28 C27 C26 Si1 C26 - C25 C27 - C25 C28 - C25 O1 - C1 C11 O2 - C1 O3 - C5 C4 O4 - C5 C8 O5 - C12 Si1 Si1 - O5 C13 C19 C25 C51 - O52 O51 C52 C52 - C53 C51 C60 C53 - C54 C52 C54 - O53 C53 C58 C55 - O54 O53 C56 C57 C56 - C55 C57 - C55 C58 - O54 C59 C54 C59 - C60 C58 C60 - C59 C61 C52 C61 - C62 O51 C60 C62 - O55 C61 C63 - C64 C68 Si51 C64 - C65 C63 C65 - C64 C66 C66 - C67 C65 C67 - C68 C66 C68 - C67 C63 C69 - C70 C74 Si51 C70 - C71 C69 C71 - C70 C72 C72 - C71 C73 C73 - C74 C72 C74 - C73 C69 C75 - C78 C77 C76 Si51 C76 - C75 C77 - C75 C78 - C75 O51 - C51 C61 O52 - C51 O53 - C54 C55 O54 - C58 C55 O55 - C62 Si51 Si51 - O55 C69 C75 C63 64350 Reflections read, of which 22746 rejected -10 =< h =< 10, -15 =< k =< 15, -31 =< l =< 31, Max. 2-theta = 41.60 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 3 4 3 1.61 0.16 26 1.41 1 Inconsistent equivalents 3108 Unique reflections, of which 0 suppressed R(int) = 0.1565 R(sigma) = 0.0740 Friedel opposites merged Maximum memory for data reduction = 6475 / 30343 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 = 8346 / 855323 wR2 = 0.1544 before cycle 1 for 3108 data and 623 / 623 parameters GooF = S = 1.196; Restrained GooF = 1.196 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06692 0.00020 -0.183 OSF Mean shift/su = 0.022 Maximum = -0.183 for OSF Max. shift = 0.003 A for H78B Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 2 for 3108 data and 623 / 623 parameters GooF = S = 1.196; Restrained GooF = 1.196 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 -0.072 OSF Mean shift/su = 0.012 Maximum = -0.072 for OSF Max. shift = 0.001 A for H76A Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 3 for 3108 data and 623 / 623 parameters GooF = S = 1.196; Restrained GooF = 1.196 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 -0.009 OSF Mean shift/su = 0.004 Maximum = -0.022 for U33 C77 Max. shift = 0.001 A for H26C Max. dU = 0.000 for C26 Least-squares cycle 4 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 4 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 -0.001 OSF Mean shift/su = 0.002 Maximum = 0.012 for U33 O53 Max. shift = 0.000 A for H78A Max. dU = 0.000 for C27 Least-squares cycle 5 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 5 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.001 Maximum = -0.006 for U33 C23 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 Least-squares cycle 6 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 6 for 3108 data and 623 / 623 parameters GooF = S = 1.196; Restrained GooF = 1.196 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.001 Maximum = 0.004 for U33 O53 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 Least-squares cycle 7 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 7 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U33 O53 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 Least-squares cycle 8 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 8 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for U33 O4 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 Least-squares cycle 9 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 9 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U33 O53 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 Least-squares cycle 10 Maximum vector length = 511 Memory required = 8346 / 855323 wR2 = 0.1543 before cycle 10 for 3108 data and 623 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.06691 0.00020 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U33 O4 Max. shift = 0.000 A for H77C Max. dU = 0.000 for C27 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2114 0.2921 0.0455 13 1.000 0.000 C2 C1 C3 C10 H3A 0.2106 0.4089 -0.0236 23 0.990 0.000 C3 C4 C2 H3B 0.3146 0.3387 -0.0137 23 0.990 0.000 C3 C4 C2 H4 0.1997 0.3070 -0.0760 13 1.000 0.000 C4 O3 C3 C8 H6A 0.1411 0.0469 -0.0236 137 0.980 0.000 C6 C5 H6A H6B -0.0101 0.0537 -0.0270 137 0.980 0.000 C6 C5 H6A H6C 0.0641 0.1036 0.0096 137 0.980 0.000 C6 C5 H6A H7A 0.1033 0.1867 -0.1124 137 0.980 0.000 C7 C5 H7A H7B 0.0153 0.1064 -0.1044 137 0.980 0.000 C7 C5 H7A H7C 0.1660 0.0989 -0.0994 137 0.980 0.000 C7 C5 H7A H8 -0.0113 0.3218 -0.0759 13 1.000 0.000 C8 O4 C9 C4 H9A -0.0184 0.4112 -0.0170 23 0.990 0.000 C9 C10 C8 H9B -0.1293 0.3435 -0.0108 23 0.990 0.000 C9 C10 C8 H10 0.0006 0.2657 0.0368 13 1.000 0.000 C10 C11 C9 C2 H11 -0.1064 0.4081 0.0579 13 1.000 0.000 C11 O1 C12 C10 H12A -0.0629 0.3785 0.1313 23 0.990 0.000 C12 O5 C11 H12B -0.1242 0.3003 0.1066 23 0.990 0.000 C12 O5 C11 H14 -0.0779 0.1371 0.1013 43 0.950 0.000 C14 C13 C15 H15 -0.2489 0.0407 0.1019 43 0.950 0.000 C15 C16 C14 H16 -0.3468 0.0100 0.1661 43 0.950 0.000 C16 C15 C17 H17 -0.2690 0.0610 0.2304 43 0.950 0.000 C17 C16 C18 H18 -0.0984 0.1574 0.2289 43 0.950 0.000 C18 C13 C17 H20 -0.1298 0.3259 0.2023 43 0.950 0.000 C20 C21 C19 H21 -0.1605 0.4155 0.2584 43 0.950 0.000 C21 C20 C22 H22 0.0105 0.4500 0.3037 43 0.950 0.000 C22 C21 C23 H23 0.2096 0.3882 0.2912 43 0.950 0.000 C23 C24 C22 H24 0.2406 0.3009 0.2338 43 0.950 0.000 C24 C23 C19 H26A 0.3275 0.0871 0.1943 137 0.980 0.000 C26 C25 H26A H26B 0.1776 0.0785 0.2013 137 0.980 0.000 C26 C25 H26A H26C 0.2534 0.1548 0.2226 137 0.980 0.000 C26 C25 H26A H27A 0.3403 0.2710 0.1750 137 0.980 0.000 C27 C25 H27A H27B 0.3214 0.2646 0.1245 137 0.980 0.000 C27 C25 H27A H27C 0.4141 0.2005 0.1484 137 0.980 0.000 C27 C25 H27A H28A 0.1946 0.1454 0.0937 137 0.980 0.000 C28 C25 H28A H28B 0.1463 0.0720 0.1245 137 0.980 0.000 C28 C25 H28A H28C 0.2948 0.0834 0.1155 137 0.980 0.000 C28 C25 H28A H52 0.4683 0.2945 0.4574 13 1.000 0.000 C52 C53 C51 C60 H53A 0.4518 0.4185 0.5229 23 0.990 0.000 C53 C54 C52 H53B 0.3516 0.3459 0.5125 23 0.990 0.000 C53 C54 C52 H54 0.4628 0.3196 0.5780 13 1.000 0.000 C54 O53 C53 C58 H56A 0.5258 0.0577 0.5310 137 0.980 0.000 C56 C55 H56A H56B 0.6772 0.0650 0.5330 137 0.980 0.000 C56 C55 H56A H56C 0.6001 0.1120 0.4961 137 0.980 0.000 C56 C55 H56A H57A 0.5605 0.2023 0.6165 137 0.980 0.000 C57 C55 H57A H57B 0.6569 0.1256 0.6107 137 0.980 0.000 C57 C55 H57A H57C 0.5075 0.1107 0.6056 137 0.980 0.000 C57 C55 H57A H58 0.6760 0.3315 0.5804 13 1.000 0.000 C58 O54 C59 C54 H59A 0.6835 0.4231 0.5210 23 0.990 0.000 C59 C60 C58 H59B 0.7985 0.3579 0.5162 23 0.990 0.000 C59 C60 C58 H60 0.6765 0.2758 0.4690 13 1.000 0.000 C60 C59 C61 C52 H61 0.7779 0.4177 0.4442 13 1.000 0.000 C61 C62 O51 C60 H62A 0.7433 0.3797 0.3727 23 0.990 0.000 C62 O55 C61 H62B 0.8058 0.3057 0.4003 23 0.990 0.000 C62 O55 C61 H64 0.7027 0.0451 0.3514 43 0.950 0.000 C64 C65 C63 H65 0.8923 -0.0237 0.3384 43 0.950 0.000 C65 C64 C66 H66 1.0724 0.0502 0.3143 43 0.950 0.000 C66 C67 C65 H67 1.0579 0.1975 0.3071 43 0.950 0.000 C67 C68 C66 H68 0.8674 0.2647 0.3191 43 0.950 0.000 C68 C67 C63 H70 0.6504 0.2023 0.2531 43 0.950 0.000 C70 C71 C69 H71 0.6172 0.2777 0.1912 43 0.950 0.000 C71 C70 C72 H72 0.5379 0.4147 0.1948 43 0.950 0.000 C72 C71 C73 H73 0.5018 0.4776 0.2619 43 0.950 0.000 C73 C74 C72 H74 0.5410 0.4021 0.3236 43 0.950 0.000 C74 C73 C69 H76A 0.3642 0.0718 0.3189 137 0.980 0.000 C76 C75 H76A H76B 0.5147 0.0610 0.3149 137 0.980 0.000 C76 C75 H76A H76C 0.4437 0.1329 0.2885 137 0.980 0.000 C76 C75 H76A H77A 0.3462 0.2518 0.3246 137 0.980 0.000 C77 C75 H77A H77B 0.3621 0.2657 0.3749 137 0.980 0.000 C77 C75 H77A H77C 0.2723 0.1924 0.3574 137 0.980 0.000 C77 C75 H77A H78A 0.4702 0.1539 0.4185 137 0.980 0.000 C78 C75 H78A H78B 0.5398 0.0773 0.3952 137 0.980 0.000 C78 C75 H78A H78C 0.3881 0.0807 0.3970 137 0.980 0.000 C78 C75 H78A 2009src1074a in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.18456 0.41993 0.05611 1.00000 0.03287 0.05268 0.02486 0.01241 0.00198 -0.00142 0.03680 0.02296 0.00119 0.00080 0.00037 0.00000 0.00802 0.00903 0.00797 0.00689 0.00669 0.00730 0.00327 C2 0.16831 0.33970 0.03064 1.00000 0.02920 0.02854 0.02235 0.00303 -0.00696 0.00298 0.02670 0.01803 0.00095 0.00070 0.00034 0.00000 0.00665 0.00669 0.00733 0.00618 0.00569 0.00539 0.00284 H2 0.21141 0.29206 0.04550 1.00000 0.03203 0.00000 0.00000 C3 0.22221 0.34990 -0.01456 1.00000 0.02265 0.04096 0.03694 0.00824 -0.00357 0.01278 0.03352 0.01956 0.00097 0.00072 0.00036 0.00000 0.00659 0.00765 0.00835 0.00674 0.00614 0.00577 0.00316 H3A 0.21055 0.40895 -0.02356 1.00000 0.04022 0.00000 0.00000 H3B 0.31458 0.33871 -0.01365 1.00000 0.04022 0.00000 0.00000 C4 0.16419 0.29448 -0.04716 1.00000 0.02798 0.02569 0.02655 -0.00563 -0.00039 0.00339 0.02674 0.01767 0.00093 0.00063 0.00036 0.00000 0.00647 0.00697 0.00727 0.00584 0.00564 0.00542 0.00286 H4 0.19972 0.30701 -0.07602 1.00000 0.03209 0.00000 0.00000 C5 0.08134 0.15870 -0.04921 1.00000 0.02854 0.04855 0.01328 0.00098 0.00040 -0.00598 0.03012 0.01851 0.00103 0.00072 0.00033 0.00000 0.00710 0.00750 0.00691 0.00613 0.00589 0.00694 0.00292 C6 0.06794 0.08423 -0.01999 1.00000 0.03374 0.06476 0.03842 0.01033 -0.00585 0.00427 0.04564 0.02067 0.00111 0.00073 0.00037 0.00000 0.00711 0.00881 0.00842 0.00715 0.00671 0.00679 0.00340 H6A 0.14108 0.04692 -0.02363 1.00000 0.06846 0.00000 0.00000 H6B -0.01012 0.05374 -0.02697 1.00000 0.06846 0.00000 0.00000 H6C 0.06414 0.10356 0.00963 1.00000 0.06846 0.00000 0.00000 C7 0.09246 0.13570 -0.09532 1.00000 0.02127 0.04264 0.03846 0.00879 -0.00482 -0.00932 0.03412 0.01799 0.00099 0.00068 0.00033 0.00000 0.00651 0.00739 0.00835 0.00599 0.00606 0.00571 0.00310 H7A 0.10327 0.18674 -0.11237 1.00000 0.05118 0.00000 0.00000 H7B 0.01534 0.10636 -0.10442 1.00000 0.05118 0.00000 0.00000 H7C 0.16605 0.09894 -0.09936 1.00000 0.05118 0.00000 0.00000 C8 0.01830 0.29909 -0.04788 1.00000 0.02532 0.02560 0.03543 0.01042 -0.00272 -0.00528 0.02878 0.01826 0.00093 0.00063 0.00037 0.00000 0.00645 0.00686 0.00782 0.00585 0.00585 0.00546 0.00296 H8 -0.01128 0.32183 -0.07588 1.00000 0.03454 0.00000 0.00000 C9 -0.03607 0.35105 -0.01172 1.00000 0.01064 0.03080 0.04833 -0.00737 0.00807 -0.01358 0.02992 0.01761 0.00092 0.00066 0.00035 0.00000 0.00584 0.00688 0.00856 0.00634 0.00601 0.00524 0.00305 H9A -0.01842 0.41117 -0.01704 1.00000 0.03591 0.00000 0.00000 H9B -0.12929 0.34352 -0.01078 1.00000 0.03591 0.00000 0.00000 C10 0.02029 0.32588 0.03072 1.00000 0.01523 0.04150 0.01442 -0.00891 -0.00509 -0.00946 0.02372 0.01660 0.00087 0.00071 0.00032 0.00000 0.00582 0.00685 0.00678 0.00570 0.00527 0.00521 0.00278 H10 0.00057 0.26567 0.03678 1.00000 0.02846 0.00000 0.00000 C11 -0.02577 0.38007 0.06683 1.00000 0.02730 0.04411 0.02587 0.00312 -0.00730 -0.00426 0.03243 0.01851 0.00104 0.00070 0.00034 0.00000 0.00679 0.00761 0.00772 0.00650 0.00592 0.00616 0.00308 H11 -0.10642 0.40807 0.05790 1.00000 0.03891 0.00000 0.00000 C12 -0.04793 0.33638 0.10865 1.00000 0.02752 0.04112 0.02925 0.00072 0.00009 -0.00618 0.03263 0.01911 0.00102 0.00070 0.00034 0.00000 0.00697 0.00716 0.00755 0.00607 0.00590 0.00640 0.00299 H12A -0.06285 0.37851 0.13129 1.00000 0.03916 0.00000 0.00000 H12B -0.12419 0.30032 0.10656 1.00000 0.03916 0.00000 0.00000 C13 -0.06823 0.15763 0.16474 1.00000 0.02823 0.01979 0.01650 -0.00255 0.00572 -0.00510 0.02150 0.01766 0.00096 0.00059 0.00034 0.00000 0.00611 0.00574 0.00663 0.00559 0.00612 0.00535 0.00252 C14 -0.11584 0.12243 0.12774 1.00000 0.03209 0.04640 0.03079 0.00299 -0.00253 -0.00241 0.03643 0.02021 0.00106 0.00071 0.00038 0.00000 0.00721 0.00786 0.00824 0.00660 0.00631 0.00698 0.00315 H14 -0.07792 0.13712 0.10130 1.00000 0.04371 0.00000 0.00000 C15 -0.21934 0.06509 0.12771 1.00000 0.06772 0.02742 0.03096 0.00081 -0.02741 0.01525 0.04203 0.02067 0.00123 0.00069 0.00040 0.00000 0.00962 0.00746 0.00902 0.00634 0.00785 0.00728 0.00356 H15 -0.24893 0.04071 0.10192 1.00000 0.05044 0.00000 0.00000 C16 -0.27508 0.04607 0.16597 1.00000 0.02236 0.04121 0.03430 0.00931 -0.00365 0.00378 0.03262 0.02123 0.00099 0.00070 0.00041 0.00000 0.00638 0.00733 0.00852 0.00710 0.00658 0.00552 0.00293 H16 -0.34681 0.00996 0.16613 1.00000 0.03915 0.00000 0.00000 C17 -0.23140 0.07713 0.20415 1.00000 0.03254 0.03734 0.03862 0.00065 0.01221 -0.00244 0.03616 0.02145 0.00105 0.00068 0.00042 0.00000 0.00736 0.00774 0.00908 0.00664 0.00663 0.00646 0.00316 H17 -0.26901 0.06097 0.23042 1.00000 0.04340 0.00000 0.00000 C18 -0.12823 0.13412 0.20286 1.00000 0.03486 0.02489 0.03337 -0.00882 -0.00922 0.00288 0.03104 0.01893 0.00103 0.00064 0.00038 0.00000 0.00721 0.00664 0.00835 0.00573 0.00645 0.00618 0.00301 H18 -0.09843 0.15739 0.22889 1.00000 0.03725 0.00000 0.00000 C19 0.05722 0.30258 0.21124 1.00000 0.01989 0.01057 0.03795 0.00468 0.01106 -0.00347 0.02280 0.01811 0.00096 0.00057 0.00034 0.00000 0.00624 0.00569 0.00772 0.00506 0.00594 0.00519 0.00277 C20 -0.05985 0.33892 0.22023 1.00000 0.02995 0.03629 0.01633 -0.00649 -0.00060 -0.01119 0.02752 0.01844 0.00106 0.00066 0.00032 0.00000 0.00728 0.00686 0.00689 0.00578 0.00578 0.00624 0.00283 H20 -0.12975 0.32594 0.20228 1.00000 0.03303 0.00000 0.00000 C21 -0.07886 0.39215 0.25351 1.00000 0.01481 0.04969 0.03244 -0.00148 -0.00313 -0.01396 0.03231 0.01832 0.00100 0.00069 0.00035 0.00000 0.00626 0.00769 0.00766 0.00658 0.00626 0.00587 0.00295 H21 -0.16052 0.41551 0.25840 1.00000 0.03878 0.00000 0.00000 C22 0.02214 0.41236 0.28050 1.00000 0.05082 0.01745 0.04093 -0.00410 0.01418 0.00764 0.03640 0.02088 0.00114 0.00065 0.00038 0.00000 0.00877 0.00645 0.00860 0.00571 0.00713 0.00636 0.00331 H22 0.01048 0.44996 0.30368 1.00000 0.04368 0.00000 0.00000 C23 0.14059 0.37614 0.27269 1.00000 0.04499 0.03630 0.03176 -0.01106 -0.00754 -0.01318 0.03769 0.01947 0.00116 0.00070 0.00037 0.00000 0.00825 0.00755 0.00834 0.00679 0.00667 0.00685 0.00330 H23 0.20956 0.38823 0.29120 1.00000 0.04522 0.00000 0.00000 C24 0.15869 0.32366 0.23889 1.00000 0.03378 0.03395 0.01254 0.00000 -0.00799 -0.00543 0.02676 0.01773 0.00101 0.00067 0.00032 0.00000 0.00697 0.00710 0.00699 0.00590 0.00578 0.00566 0.00289 H24 0.24062 0.30088 0.23380 1.00000 0.03211 0.00000 0.00000 C25 0.22407 0.17188 0.15738 1.00000 0.03223 0.07441 0.00847 0.01125 0.00428 0.01759 0.03837 0.02171 0.00104 0.00081 0.00036 0.00000 0.00717 0.00932 0.00695 0.00691 0.00574 0.00680 0.00335 C26 0.24782 0.11818 0.19756 1.00000 0.03149 0.05210 0.05974 -0.00349 -0.00287 0.00288 0.04778 0.02139 0.00111 0.00076 0.00041 0.00000 0.00709 0.00866 0.01014 0.00776 0.00688 0.00664 0.00367 H26A 0.32747 0.08709 0.19428 1.00000 0.07167 0.00000 0.00000 H26B 0.17761 0.07852 0.20132 1.00000 0.07167 0.00000 0.00000 H26C 0.25344 0.15482 0.22257 1.00000 0.07167 0.00000 0.00000 C27 0.33492 0.23241 0.15073 1.00000 0.02126 0.06023 0.07109 0.00487 0.00570 0.01165 0.05086 0.02109 0.00092 0.00078 0.00042 0.00000 0.00662 0.00875 0.01019 0.00806 0.00666 0.00642 0.00372 H27A 0.34028 0.27097 0.17500 1.00000 0.07629 0.00000 0.00000 H27B 0.32138 0.26457 0.12449 1.00000 0.07629 0.00000 0.00000 H27C 0.41412 0.20050 0.14843 1.00000 0.07629 0.00000 0.00000 C28 0.21404 0.11291 0.11937 1.00000 0.04159 0.03649 0.03892 -0.02060 0.01125 0.00934 0.03900 0.01895 0.00109 0.00069 0.00036 0.00000 0.00773 0.00761 0.00867 0.00669 0.00655 0.00650 0.00338 H28A 0.19460 0.14540 0.09366 1.00000 0.05850 0.00000 0.00000 H28B 0.14627 0.07201 0.12447 1.00000 0.05850 0.00000 0.00000 H28C 0.29478 0.08336 0.11551 1.00000 0.05850 0.00000 0.00000 O1 0.07120 0.44496 0.07389 1.00000 0.03240 0.03445 0.03561 0.00126 0.01558 -0.00428 0.03415 0.01246 0.00068 0.00043 0.00023 0.00000 0.00469 0.00450 0.00504 0.00385 0.00423 0.00418 0.00194 O2 0.27795 0.46181 0.06139 1.00000 0.03310 0.05928 0.05008 -0.00707 0.00716 -0.00906 0.04749 0.01459 0.00077 0.00052 0.00026 0.00000 0.00509 0.00587 0.00625 0.00475 0.00450 0.00487 0.00234 O3 0.18882 0.20722 -0.03545 1.00000 0.01720 0.02982 0.04287 0.00011 -0.00032 -0.00340 0.02997 0.01162 0.00060 0.00043 0.00023 0.00000 0.00391 0.00476 0.00534 0.00399 0.00369 0.00364 0.00196 O4 -0.02354 0.21324 -0.04296 1.00000 0.02211 0.02795 0.03683 0.00099 -0.00110 -0.00114 0.02897 0.01140 0.00060 0.00042 0.00022 0.00000 0.00411 0.00457 0.00512 0.00392 0.00357 0.00376 0.00192 O5 0.05936 0.28654 0.11927 1.00000 0.01371 0.04297 0.02979 0.00197 -0.00044 0.00298 0.02882 0.01144 0.00059 0.00043 0.00021 0.00000 0.00373 0.00465 0.00465 0.00384 0.00339 0.00396 0.00184 Si1 0.06831 0.23065 0.16393 1.00000 0.02366 0.03083 0.02475 0.00024 0.00057 -0.00349 0.02641 0.00510 0.00027 0.00018 0.00010 0.00000 0.00163 0.00178 0.00188 0.00158 0.00153 0.00153 0.00078 C51 0.48799 0.42361 0.44349 1.00000 0.03492 0.02934 0.03660 0.00056 0.00653 -0.00261 0.03362 0.02008 0.00120 0.00070 0.00037 0.00000 0.00830 0.00757 0.00840 0.00619 0.00690 0.00675 0.00312 C52 0.50610 0.34467 0.47174 1.00000 0.02330 0.02998 0.03318 -0.00999 0.00345 0.00407 0.02882 0.01852 0.00093 0.00068 0.00035 0.00000 0.00640 0.00675 0.00766 0.00611 0.00597 0.00549 0.00293 H52 0.46826 0.29449 0.45742 1.00000 0.03458 0.00000 0.00000 C53 0.44324 0.35866 0.51490 1.00000 0.02095 0.03172 0.04282 -0.00541 0.00449 -0.00381 0.03183 0.01852 0.00099 0.00066 0.00035 0.00000 0.00615 0.00685 0.00806 0.00606 0.00624 0.00550 0.00298 H53A 0.45177 0.41850 0.52290 1.00000 0.03819 0.00000 0.00000 H53B 0.35158 0.34586 0.51251 1.00000 0.03819 0.00000 0.00000 C54 0.50064 0.30470 0.54976 1.00000 0.02369 0.03477 0.03162 0.00917 -0.00173 -0.00097 0.03003 0.01892 0.00096 0.00066 0.00037 0.00000 0.00629 0.00752 0.00774 0.00595 0.00579 0.00546 0.00298 H54 0.46285 0.31960 0.57800 1.00000 0.03603 0.00000 0.00000 C55 0.58701 0.16978 0.55341 1.00000 0.03710 0.02808 0.01153 0.00622 -0.00939 -0.00077 0.02557 0.01794 0.00104 0.00065 0.00031 0.00000 0.00737 0.00655 0.00658 0.00538 0.00573 0.00637 0.00281 C56 0.59849 0.09482 0.52605 1.00000 0.04676 0.01344 0.04628 0.00191 0.00973 -0.00921 0.03549 0.01833 0.00107 0.00058 0.00036 0.00000 0.00761 0.00591 0.00808 0.00580 0.00679 0.00562 0.00311 H56A 0.52581 0.05768 0.53096 1.00000 0.05323 0.00000 0.00000 H56B 0.67716 0.06498 0.53297 1.00000 0.05323 0.00000 0.00000 H56C 0.60011 0.11202 0.49607 1.00000 0.05323 0.00000 0.00000 C57 0.57711 0.15039 0.60073 1.00000 0.02026 0.02934 0.04293 0.00778 0.00708 -0.00309 0.03084 0.01853 0.00099 0.00065 0.00033 0.00000 0.00618 0.00684 0.00813 0.00577 0.00599 0.00560 0.00295 H57A 0.56047 0.20234 0.61649 1.00000 0.04627 0.00000 0.00000 H57B 0.65694 0.12562 0.61066 1.00000 0.04627 0.00000 0.00000 H57C 0.50752 0.11070 0.60555 1.00000 0.04627 0.00000 0.00000 C58 0.64857 0.30960 0.55202 1.00000 0.01897 0.03015 0.03555 -0.00443 0.00053 0.00582 0.02822 0.01925 0.00092 0.00067 0.00037 0.00000 0.00617 0.00736 0.00806 0.00581 0.00570 0.00539 0.00300 H58 0.67604 0.33155 0.58042 1.00000 0.03387 0.00000 0.00000 C59 0.70489 0.36335 0.51613 1.00000 0.02477 0.01383 0.03934 0.00851 -0.00688 -0.00418 0.02598 0.01768 0.00097 0.00061 0.00034 0.00000 0.00617 0.00628 0.00823 0.00570 0.00604 0.00507 0.00291 H59A 0.68349 0.42307 0.52105 1.00000 0.03118 0.00000 0.00000 H59B 0.79848 0.35792 0.51624 1.00000 0.03118 0.00000 0.00000 C60 0.65376 0.33610 0.47347 1.00000 0.02358 0.03591 0.01609 -0.00186 -0.00543 0.00885 0.02520 0.01808 0.00090 0.00072 0.00032 0.00000 0.00627 0.00679 0.00695 0.00601 0.00557 0.00543 0.00278 H60 0.67646 0.27581 0.46895 1.00000 0.03023 0.00000 0.00000 C61 0.70011 0.38606 0.43558 1.00000 0.01716 0.03255 0.01747 -0.00259 0.00217 -0.00057 0.02240 0.01790 0.00094 0.00065 0.00032 0.00000 0.00601 0.00694 0.00714 0.00581 0.00533 0.00557 0.00276 H61 0.77789 0.41771 0.44424 1.00000 0.02687 0.00000 0.00000 C62 0.72820 0.33978 0.39634 1.00000 0.02856 0.03866 0.03214 -0.00138 -0.00035 -0.00673 0.03312 0.01829 0.00101 0.00072 0.00035 0.00000 0.00689 0.00742 0.00804 0.00645 0.00606 0.00628 0.00309 H62A 0.74328 0.37969 0.37269 1.00000 0.03974 0.00000 0.00000 H62B 0.80584 0.30566 0.40026 1.00000 0.03974 0.00000 0.00000 C63 0.76454 0.16214 0.33637 1.00000 0.01946 0.03741 0.02036 0.00034 -0.00463 0.00070 0.02574 0.01821 0.00092 0.00071 0.00035 0.00000 0.00647 0.00786 0.00699 0.00625 0.00552 0.00581 0.00278 C64 0.77437 0.07614 0.34208 1.00000 0.03329 0.03341 0.03722 0.01134 0.00547 0.01356 0.03464 0.01993 0.00102 0.00069 0.00036 0.00000 0.00736 0.00813 0.00836 0.00641 0.00635 0.00610 0.00310 H64 0.70267 0.04506 0.35145 1.00000 0.04157 0.00000 0.00000 C65 0.88745 0.03530 0.33426 1.00000 0.06691 0.01703 0.07007 0.01086 0.01293 0.01795 0.05134 0.02293 0.00124 0.00070 0.00042 0.00000 0.00955 0.00645 0.01031 0.00668 0.00858 0.00732 0.00370 H65 0.89230 -0.02366 0.33843 1.00000 0.06160 0.00000 0.00000 C66 0.99540 0.07881 0.32030 1.00000 0.05164 0.04381 0.03854 -0.00682 -0.00347 0.01314 0.04466 0.02112 0.00123 0.00079 0.00038 0.00000 0.00884 0.00913 0.00866 0.00671 0.00718 0.00759 0.00347 H66 1.07240 0.05015 0.31428 1.00000 0.05359 0.00000 0.00000 C67 0.98578 0.16582 0.31556 1.00000 0.02156 0.06938 0.03568 -0.00559 -0.00076 0.00697 0.04221 0.02064 0.00106 0.00086 0.00036 0.00000 0.00721 0.01026 0.00822 0.00722 0.00597 0.00691 0.00341 H67 1.05790 0.19748 0.30710 1.00000 0.05065 0.00000 0.00000 C68 0.87252 0.20566 0.32309 1.00000 0.02591 0.03750 0.02778 0.00340 -0.00163 0.00359 0.03040 0.01778 0.00095 0.00070 0.00033 0.00000 0.00673 0.00694 0.00735 0.00578 0.00558 0.00622 0.00290 H68 0.86743 0.26468 0.31914 1.00000 0.03647 0.00000 0.00000 C69 0.59655 0.29246 0.29534 1.00000 0.01211 0.03761 0.02714 -0.00655 0.00127 -0.00159 0.02562 0.01708 0.00089 0.00064 0.00034 0.00000 0.00570 0.00750 0.00755 0.00598 0.00534 0.00578 0.00274 C70 0.61979 0.25822 0.25501 1.00000 0.02061 0.03812 0.02517 0.00490 -0.00316 0.00136 0.02796 0.01735 0.00088 0.00070 0.00033 0.00000 0.00617 0.00691 0.00732 0.00637 0.00565 0.00544 0.00279 H70 0.65044 0.20228 0.25309 1.00000 0.03356 0.00000 0.00000 C71 0.59982 0.30267 0.21809 1.00000 0.02368 0.03442 0.03733 -0.00413 -0.00402 -0.00131 0.03181 0.01841 0.00097 0.00069 0.00038 0.00000 0.00649 0.00753 0.00847 0.00606 0.00585 0.00614 0.00295 H71 0.61723 0.27767 0.19123 1.00000 0.03817 0.00000 0.00000 C72 0.55416 0.38418 0.22020 1.00000 0.02626 0.05107 0.03110 0.02110 -0.01020 -0.00769 0.03614 0.02039 0.00101 0.00076 0.00039 0.00000 0.00684 0.00897 0.00840 0.00674 0.00633 0.00670 0.00320 H72 0.53790 0.41471 0.19476 1.00000 0.04337 0.00000 0.00000 C73 0.53199 0.42150 0.26017 1.00000 0.03781 0.03966 0.04590 0.01780 -0.01400 0.00131 0.04112 0.02045 0.00103 0.00075 0.00041 0.00000 0.00773 0.00752 0.00951 0.00757 0.00687 0.00624 0.00336 H73 0.50179 0.47757 0.26190 1.00000 0.04935 0.00000 0.00000 C74 0.55437 0.37619 0.29669 1.00000 0.03210 0.02410 0.02661 -0.00926 0.00446 -0.00080 0.02760 0.01767 0.00098 0.00063 0.00035 0.00000 0.00676 0.00673 0.00738 0.00590 0.00604 0.00566 0.00278 H74 0.54098 0.40213 0.32358 1.00000 0.03313 0.00000 0.00000 C75 0.46375 0.16299 0.35266 1.00000 0.01210 0.04246 0.02497 -0.00047 -0.00355 -0.00823 0.02651 0.01753 0.00089 0.00070 0.00034 0.00000 0.00588 0.00699 0.00715 0.00635 0.00520 0.00553 0.00281 C76 0.44488 0.10158 0.31536 1.00000 0.04562 0.03597 0.04744 0.00078 -0.00287 -0.01316 0.04301 0.01844 0.00115 0.00068 0.00036 0.00000 0.00776 0.00749 0.00874 0.00648 0.00686 0.00633 0.00341 H76A 0.36422 0.07179 0.31893 1.00000 0.06452 0.00000 0.00000 H76B 0.51474 0.06099 0.31492 1.00000 0.06452 0.00000 0.00000 H76C 0.44365 0.13286 0.28846 1.00000 0.06452 0.00000 0.00000 C77 0.35091 0.22370 0.35237 1.00000 0.02559 0.04846 0.02696 0.00896 -0.00092 0.00442 0.03367 0.01889 0.00088 0.00071 0.00034 0.00000 0.00623 0.00753 0.00719 0.00629 0.00547 0.00608 0.00297 H77A 0.34616 0.25181 0.32463 1.00000 0.05051 0.00000 0.00000 H77B 0.36214 0.26573 0.37486 1.00000 0.05051 0.00000 0.00000 H77C 0.27230 0.19239 0.35743 1.00000 0.05051 0.00000 0.00000 C78 0.46566 0.11439 0.39460 1.00000 0.02367 0.03815 0.03894 -0.00490 0.00513 0.00305 0.03359 0.01874 0.00099 0.00067 0.00034 0.00000 0.00657 0.00717 0.00803 0.00623 0.00596 0.00583 0.00307 H78A 0.47020 0.15394 0.41848 1.00000 0.05038 0.00000 0.00000 H78B 0.53984 0.07732 0.39522 1.00000 0.05038 0.00000 0.00000 H78C 0.38815 0.08074 0.39702 1.00000 0.05038 0.00000 0.00000 O51 0.59923 0.44679 0.42597 1.00000 0.02678 0.02658 0.03948 0.00757 0.00825 0.00317 0.03095 0.01216 0.00064 0.00041 0.00023 0.00000 0.00455 0.00425 0.00514 0.00376 0.00407 0.00385 0.00190 O52 0.39291 0.46140 0.43768 1.00000 0.02859 0.03863 0.06499 0.01934 -0.00085 0.01403 0.04407 0.01386 0.00074 0.00047 0.00026 0.00000 0.00477 0.00500 0.00652 0.00445 0.00447 0.00448 0.00229 O53 0.47709 0.21785 0.54017 1.00000 0.02306 0.03294 0.02853 -0.00190 -0.00516 0.00060 0.02817 0.01141 0.00059 0.00044 0.00021 0.00000 0.00417 0.00478 0.00485 0.00392 0.00348 0.00368 0.00189 O54 0.69115 0.22603 0.54646 1.00000 0.01947 0.03139 0.03962 -0.00191 -0.00018 -0.00297 0.03016 0.01170 0.00060 0.00046 0.00023 0.00000 0.00392 0.00478 0.00504 0.00414 0.00360 0.00394 0.00191 O55 0.62243 0.28584 0.38605 1.00000 0.01927 0.05371 0.02594 -0.00201 0.00447 -0.00659 0.03297 0.01185 0.00061 0.00046 0.00021 0.00000 0.00389 0.00498 0.00466 0.00402 0.00344 0.00419 0.00194 Si51 0.61413 0.22603 0.34420 1.00000 0.02080 0.03254 0.01702 0.00191 -0.00029 -0.00310 0.02345 0.00495 0.00026 0.00019 0.00009 0.00000 0.00160 0.00180 0.00180 0.00155 0.00138 0.00151 0.00078 Final Structure Factor Calculation for 2009src1074a in P2(1)2(1)2(1) Total number of l.s. parameters = 623 Maximum vector length = 511 Memory required = 7725 / 25046 wR2 = 0.1543 before cycle 11 for 3108 data and 2 / 623 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0327 * P )^2 + 14.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0791 for 2689 Fo > 4sig(Fo) and 0.0948 for all 3108 data wR2 = 0.1543, GooF = S = 1.195, Restrained GooF = 1.195 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 68.00 for non-hydrogen and 72.00 for hydrogen atoms Principal mean square atomic displacements U 0.0574 0.0333 0.0197 C1 0.0337 0.0298 0.0166 C2 0.0503 0.0364 0.0139 C3 0.0332 0.0272 0.0198 C4 0.0502 0.0269 0.0132 C5 0.0685 0.0412 0.0273 C6 0.0530 0.0318 0.0177 C7 0.0435 0.0252 0.0176 C8 0.0547 0.0316 0.0034 C9 0.0461 0.0199 0.0051 C10 0.0463 0.0317 0.0192 C11 0.0435 0.0293 0.0251 C12 0.0330 0.0174 0.0141 C13 0.0475 0.0330 0.0288 C14 0.0853 0.0291 0.0117 C15 0.0477 0.0309 0.0192 C16 0.0482 0.0376 0.0226 C17 0.0465 0.0278 0.0188 C18 0.0434 0.0180 0.0069 C19 0.0456 0.0238 0.0133 C20 0.0546 0.0330 0.0094 C21 0.0612 0.0343 0.0136 C22 0.0545 0.0429 0.0157 C23 0.0405 0.0300 0.0097 C24 0.0827 0.0259 0.0065 C25 0.0616 0.0509 0.0309 C26 0.0748 0.0601 0.0177 C27 0.0586 0.0481 0.0103 C28 0.0499 0.0352 0.0174 O1 0.0670 0.0464 0.0291 O2 0.0429 0.0307 0.0163 O3 0.0370 0.0280 0.0218 O4 0.0435 0.0295 0.0134 O5 0.0322 0.0249 0.0221 Si1 0.0425 0.0315 0.0269 C51 0.0417 0.0278 0.0170 C52 0.0463 0.0298 0.0194 C53 0.0427 0.0244 0.0230 C54 0.0408 0.0290 0.0069 C55 0.0569 0.0390 0.0105 C56 0.0475 0.0290 0.0160 C57 0.0384 0.0301 0.0162 C58 0.0449 0.0221 0.0109 C59 0.0412 0.0215 0.0129 C60 0.0330 0.0191 0.0150 C61 0.0421 0.0321 0.0251 C62 0.0374 0.0246 0.0152 C63 0.0551 0.0303 0.0186 C64 0.0873 0.0562 0.0105 C65 0.0634 0.0388 0.0318 C66 0.0713 0.0348 0.0206 C67 0.0392 0.0286 0.0233 C68 0.0409 0.0240 0.0120 C69 0.0398 0.0258 0.0183 C70 0.0407 0.0327 0.0221 C71 0.0679 0.0253 0.0152 C72 0.0648 0.0398 0.0187 C73 0.0376 0.0296 0.0157 C74 0.0446 0.0258 0.0092 C75 0.0558 0.0465 0.0267 C76 0.0523 0.0268 0.0219 C77 0.0436 0.0362 0.0210 C78 0.0469 0.0235 0.0225 O51 0.0760 0.0408 0.0154 O52 0.0343 0.0302 0.0199 O53 0.0400 0.0317 0.0188 O54 0.0552 0.0274 0.0163 O55 0.0335 0.0200 0.0168 Si51 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.024 0.032 0.040 0.047 0.056 0.067 0.083 0.112 1.000 Number in group 322. 303. 331. 321. 287. 326. 294. 301. 312. 311. GooF 1.730 1.357 1.262 1.076 1.105 1.038 0.981 0.969 0.950 1.233 K 5.319 1.795 1.370 1.146 1.093 1.022 1.003 1.012 0.986 0.979 Resolution(A) 1.00 1.04 1.08 1.13 1.20 1.27 1.38 1.52 1.74 2.21 inf Number in group 314. 308. 315. 317. 301. 313. 309. 307. 312. 312. GooF 1.190 1.186 1.204 1.257 1.099 1.120 1.006 1.220 1.324 1.307 K 1.092 1.103 1.062 1.041 1.027 1.019 1.013 1.033 1.033 0.973 R1 0.189 0.166 0.147 0.131 0.106 0.082 0.078 0.074 0.056 0.041 Recommended weighting scheme: WGHT 0.0321 14.9842 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) 0 8 1 1306.43 11.96 6.93 0.007 1.99 3 6 0 627.55 133.24 4.91 0.024 2.12 5 7 2 644.71 224.76 4.38 0.031 1.54 0 6 1 689.47 113.29 4.13 0.022 2.65 1 6 0 1431.65 831.10 3.98 0.059 2.58 4 10 0 382.10 48.92 3.95 0.014 1.36 1 8 0 1164.25 632.42 3.87 0.052 1.96 3 7 1 863.52 437.89 3.80 0.043 1.91 2 0 3 191.98 17.89 3.76 0.009 4.71 2 9 1 648.08 233.84 3.73 0.031 1.68 4 5 2 1098.19 555.90 3.69 0.048 2.01 5 7 0 5255.13 4006.06 3.39 0.130 1.55 5 6 0 2313.03 1545.95 3.35 0.081 1.65 1 7 1 948.66 575.44 3.19 0.049 2.22 3 1 26 787.83 241.50 3.18 0.032 1.14 1 9 0 4823.22 3716.33 3.17 0.125 1.75 4 2 26 580.89 113.65 3.08 0.022 1.09 0 14 3 1807.86 515.19 3.07 0.047 1.13 1 8 2 781.19 451.86 3.06 0.044 1.94 0 5 23 591.76 20.00 3.05 0.009 1.25 0 1 13 264.92 25.20 3.05 0.010 2.39 6 5 0 250.05 51.09 3.03 0.015 1.54 5 5 1 4798.80 3812.41 3.01 0.127 1.76 0 3 3 140.41 6.25 3.01 0.005 4.74 5 6 2 645.61 306.80 2.95 0.036 1.64 3 5 4 203.81 44.84 2.92 0.014 2.26 3 5 0 1733.81 1213.57 2.91 0.072 2.36 4 8 18 245.85 5.85 2.90 0.005 1.17 5 13 9 1226.57 682.26 2.85 0.054 1.01 3 0 20 452.85 0.03 2.83 0.000 1.43 3 9 21 306.58 19.55 2.79 0.009 1.09 8 4 16 343.33 4.78 2.78 0.004 1.05 2 8 0 305.31 100.83 2.76 0.021 1.86 4 2 24 435.89 74.52 2.75 0.018 1.16 0 7 19 410.72 35.23 2.68 0.012 1.34 0 3 27 605.87 15.69 2.68 0.008 1.14 6 0 2 10967.62 9287.20 2.61 0.198 1.75 2 1 25 422.30 53.73 2.60 0.015 1.22 3 9 15 240.29 38.70 2.60 0.013 1.26 1 8 26 595.81 238.84 2.58 0.032 1.03 3 1 25 524.99 111.51 2.57 0.022 1.18 8 6 4 122.06 0.83 2.55 0.002 1.17 0 13 9 324.70 69.78 2.55 0.017 1.16 0 12 1 2389.95 1779.48 2.54 0.087 1.33 2 9 24 291.78 4.57 2.53 0.004 1.03 4 7 24 344.24 45.62 2.52 0.014 1.04 3 9 0 206.33 40.29 2.51 0.013 1.58 4 1 2 19514.72 17237.15 2.51 0.270 2.56 0 3 1 93.57 2.30 2.50 0.003 5.24 2 0 2 230.96 93.90 2.49 0.020 4.99 Bond lengths and angles C1 - Distance Angles O2 1.2005 (0.0131) O1 1.3773 (0.0130) 119.62 (1.12) C2 1.5172 (0.0162) 129.30 (1.09) 111.06 (1.01) C1 - O2 O1 C2 - Distance Angles C1 1.5172 (0.0162) C3 1.5360 (0.0144) 110.82 (0.93) C10 1.5752 (0.0137) 103.22 (0.92) 112.48 (0.86) H2 1.0000 110.05 110.05 110.05 C2 - C1 C3 C10 C3 - Distance Angles C4 1.4831 (0.0140) C2 1.5360 (0.0144) 114.91 (0.93) H3A 0.9900 108.54 108.54 H3B 0.9900 108.54 108.54 107.53 C3 - C4 C2 H3A C4 - Distance Angles O3 1.4613 (0.0123) C3 1.4831 (0.0140) 108.66 (0.86) C8 1.5392 (0.0140) 103.09 (0.81) 113.17 (0.93) H4 1.0000 110.56 110.56 110.56 C4 - O3 C3 C8 C5 - Distance Angles O4 1.4195 (0.0125) O3 1.4376 (0.0122) 104.04 (0.77) C7 1.4970 (0.0137) 110.13 (0.88) 111.11 (0.87) C6 1.5059 (0.0146) 108.99 (0.87) 108.36 (0.87) 113.74 (0.97) C5 - O4 O3 C7 C6 - Distance Angles C5 1.5059 (0.0146) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C5 H6A H6B C7 - Distance Angles C5 1.4970 (0.0137) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C5 H7A H7B C8 - Distance Angles O4 1.4455 (0.0118) C9 1.5166 (0.0139) 108.76 (0.84) C4 1.5392 (0.0140) 104.94 (0.82) 113.10 (0.92) H8 1.0000 109.97 109.97 109.97 C8 - O4 C9 C4 C9 - Distance Angles C10 1.5120 (0.0139) C8 1.5166 (0.0139) 111.43 (0.88) H9A 0.9900 109.34 109.34 H9B 0.9900 109.34 109.34 107.98 C9 - C10 C8 H9A C10 - Distance Angles C11 1.5049 (0.0138) C9 1.5120 (0.0139) 112.59 (0.89) C2 1.5752 (0.0137) 103.91 (0.83) 110.52 (0.88) H10 1.0000 109.89 109.89 109.89 C10 - C11 C9 C2 C11 - Distance Angles O1 1.4704 (0.0122) C12 1.5034 (0.0141) 107.58 (0.84) C10 1.5049 (0.0138) 107.02 (0.81) 116.19 (0.95) H11 1.0000 108.61 108.61 108.61 C11 - O1 C12 C10 C12 - Distance Angles O5 1.4212 (0.0118) C11 1.5034 (0.0141) 109.86 (0.86) H12A 0.9900 109.69 109.69 H12B 0.9900 109.69 109.69 108.18 C12 - O5 C11 H12A C13 - Distance Angles C14 1.3834 (0.0141) C18 1.4038 (0.0144) 116.32 (0.95) Si1 1.8505 (0.0101) 121.69 (0.83) 121.98 (0.82) C13 - C14 C18 C14 - Distance Angles C13 1.3834 (0.0141) C15 1.4227 (0.0151) 122.61 (1.10) H14 0.9500 118.70 118.70 C14 - C13 C15 C15 - Distance Angles C16 1.3703 (0.0148) C14 1.4227 (0.0151) 118.03 (1.10) H15 0.9500 120.98 120.98 C15 - C16 C14 C16 - Distance Angles C15 1.3703 (0.0148) C17 1.3752 (0.0150) 122.68 (1.07) H16 0.9500 118.66 118.66 C16 - C15 C17 C17 - Distance Angles C16 1.3752 (0.0150) C18 1.4171 (0.0143) 117.55 (1.11) H17 0.9500 121.22 121.22 C17 - C16 C18 C18 - Distance Angles C13 1.4038 (0.0144) C17 1.4171 (0.0143) 122.74 (1.08) H18 0.9500 118.63 118.63 C18 - C13 C17 C19 - Distance Angles C20 1.3916 (0.0140) C24 1.4172 (0.0137) 116.50 (0.93) Si1 1.8789 (0.0107) 117.97 (0.82) 125.53 (0.77) C19 - C20 C24 C20 - Distance Angles C21 1.3601 (0.0136) C19 1.3916 (0.0141) 123.07 (1.04) H20 0.9500 118.47 118.47 C20 - C21 C19 C21 - Distance Angles C20 1.3601 (0.0136) C22 1.3977 (0.0145) 119.78 (1.07) H21 0.9500 120.11 120.11 C21 - C20 C22 C22 - Distance Angles C21 1.3977 (0.0144) C23 1.3968 (0.0152) 118.62 (1.04) H22 0.9500 120.69 120.69 C22 - C21 C23 C23 - Distance Angles C24 1.3640 (0.0142) C22 1.3968 (0.0152) 120.98 (1.10) H23 0.9500 119.51 119.51 C23 - C24 C22 C24 - Distance Angles C23 1.3640 (0.0142) C19 1.4172 (0.0137) 121.04 (1.03) H24 0.9500 119.48 119.48 C24 - C23 C19 C25 - Distance Angles C28 1.5218 (0.0151) C27 1.5291 (0.0154) 109.60 (0.96) C26 1.5439 (0.0156) 107.98 (1.01) 109.71 (0.96) Si1 1.9008 (0.0110) 109.20 (0.78) 111.32 (0.81) 108.96 (0.76) C25 - C28 C27 C26 C26 - Distance Angles C25 1.5439 (0.0156) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5291 (0.0154) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C25 H27A H27B C28 - Distance Angles C25 1.5218 (0.0151) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C25 H28A H28B O1 - Distance Angles C1 1.3773 (0.0131) C11 1.4704 (0.0122) 109.76 (0.85) O1 - C1 O2 - Distance Angles C1 1.2005 (0.0131) O2 - O3 - Distance Angles C5 1.4376 (0.0122) C4 1.4613 (0.0123) 107.23 (0.76) O3 - C5 O4 - Distance Angles C5 1.4195 (0.0126) C8 1.4455 (0.0118) 109.10 (0.74) O4 - C5 O5 - Distance Angles C12 1.4212 (0.0118) Si1 1.6627 (0.0072) 122.82 (0.61) O5 - C12 Si1 - Distance Angles O5 1.6627 (0.0072) C13 1.8505 (0.0101) 107.71 (0.43) C19 1.8789 (0.0107) 109.60 (0.39) 108.92 (0.46) C25 1.9008 (0.0110) 102.82 (0.43) 111.29 (0.49) 116.07 (0.51) Si1 - O5 C13 C19 C51 - Distance Angles O52 1.1831 (0.0126) O51 1.3463 (0.0126) 122.33 (1.02) C52 1.5505 (0.0154) 127.24 (1.02) 110.41 (0.98) C51 - O52 O51 C52 - Distance Angles C53 1.5238 (0.0142) C51 1.5505 (0.0155) 109.62 (0.87) C60 1.5629 (0.0134) 114.50 (0.90) 102.31 (0.92) H52 1.0000 110.05 110.05 110.05 C52 - C53 C51 C60 C53 - Distance Angles C54 1.5170 (0.0141) C52 1.5238 (0.0142) 112.60 (0.88) H53A 0.9900 109.07 109.07 H53B 0.9900 109.07 109.07 107.83 C53 - C54 C52 H53A C54 - Distance Angles O53 1.4376 (0.0124) C53 1.5170 (0.0141) 109.01 (0.88) C58 1.5623 (0.0140) 103.30 (0.85) 113.71 (0.93) H54 1.0000 110.20 110.20 110.20 C54 - O53 C53 C58 C55 - Distance Angles O54 1.4336 (0.0120) O53 1.4495 (0.0119) 103.75 (0.70) C56 1.4757 (0.0137) 110.78 (0.87) 109.05 (0.85) C57 1.5199 (0.0133) 109.16 (0.82) 109.42 (0.85) 114.15 (0.88) C55 - O54 O53 C56 C56 - Distance Angles C55 1.4757 (0.0137) H56A 0.9800 109.47 H56B 0.9800 109.47 109.47 H56C 0.9800 109.47 109.47 109.47 C56 - C55 H56A H56B C57 - Distance Angles C55 1.5199 (0.0133) H57A 0.9800 109.47 H57B 0.9800 109.47 109.47 H57C 0.9800 109.47 109.47 109.47 C57 - C55 H57A H57B C58 - Distance Angles O54 1.4159 (0.0118) C59 1.5340 (0.0140) 108.18 (0.85) C54 1.5623 (0.0140) 105.28 (0.85) 112.37 (0.92) H58 1.0000 110.29 110.29 110.29 C58 - O54 C59 C54 C59 - Distance Angles C60 1.5066 (0.0137) C58 1.5340 (0.0140) 110.66 (0.85) H59A 0.9900 109.52 109.51 H59B 0.9900 109.52 109.51 108.08 C59 - C60 C58 H59A C60 - Distance Angles C59 1.5066 (0.0137) C61 1.5117 (0.0138) 115.55 (0.87) C52 1.5629 (0.0134) 111.21 (0.90) 104.38 (0.87) H60 1.0000 108.49 108.49 108.49 C60 - C59 C61 C52 C61 - Distance Angles C62 1.4652 (0.0137) O51 1.4688 (0.0115) 107.78 (0.84) C60 1.5117 (0.0138) 117.45 (0.90) 105.93 (0.77) H61 1.0000 108.46 108.46 108.46 C61 - C62 O51 C60 C62 - Distance Angles O55 1.4439 (0.0119) C61 1.4652 (0.0137) 109.35 (0.84) H62A 0.9900 109.81 109.81 H62B 0.9900 109.81 109.81 108.25 C62 - O55 C61 H62A C63 - Distance Angles C64 1.3858 (0.0142) C68 1.3961 (0.0138) 117.96 (0.97) Si51 1.8997 (0.0105) 125.13 (0.81) 116.90 (0.80) C63 - C64 C68 C64 - Distance Angles C65 1.3797 (0.0149) C63 1.3858 (0.0142) 120.52 (1.06) H64 0.9500 119.74 119.74 C64 - C65 C63 C65 - Distance Angles C64 1.3797 (0.0149) C66 1.4022 (0.0158) 121.53 (1.01) H65 0.9500 119.23 119.23 C65 - C64 C66 C66 - Distance Angles C67 1.3981 (0.0162) C65 1.4022 (0.0158) 117.69 (1.12) H66 0.9500 121.16 121.16 C66 - C67 C65 C67 - Distance Angles C68 1.3722 (0.0145) C66 1.3981 (0.0162) 120.23 (1.17) H67 0.9500 119.88 119.88 C67 - C68 C66 C68 - Distance Angles C67 1.3722 (0.0145) C63 1.3961 (0.0138) 122.03 (1.04) H68 0.9500 118.98 118.98 C68 - C67 C63 C69 - Distance Angles C70 1.3996 (0.0137) C74 1.4069 (0.0133) 116.87 (1.00) Si51 1.8721 (0.0110) 120.18 (0.80) 122.88 (0.83) C69 - C70 C74 C70 - Distance Angles C71 1.3738 (0.0140) C69 1.3996 (0.0137) 122.31 (1.05) H70 0.9500 118.84 118.84 C70 - C71 C69 C71 - Distance Angles C70 1.3738 (0.0140) C72 1.3866 (0.0144) 119.72 (1.11) H71 0.9500 120.14 120.14 C71 - C70 C72 C72 - Distance Angles C71 1.3866 (0.0144) C73 1.4075 (0.0152) 119.72 (1.07) H72 0.9500 120.14 120.14 C72 - C71 C73 C73 - Distance Angles C74 1.3744 (0.0141) C72 1.4075 (0.0152) 119.49 (1.07) H73 0.9500 120.25 120.25 C73 - C74 C72 C74 - Distance Angles C73 1.3744 (0.0141) C69 1.4069 (0.0133) 121.82 (1.05) H74 0.9500 119.09 119.09 C74 - C73 C69 C75 - Distance Angles C78 1.5267 (0.0138) C77 1.5329 (0.0136) 109.59 (0.84) C76 1.5383 (0.0139) 109.56 (0.88) 107.25 (0.85) Si51 1.8949 (0.0100) 112.24 (0.69) 108.26 (0.70) 109.80 (0.73) C75 - C78 C77 C76 C76 - Distance Angles C75 1.5383 (0.0139) H76A 0.9800 109.47 H76B 0.9800 109.47 109.47 H76C 0.9800 109.47 109.47 109.47 C76 - C75 H76A H76B C77 - Distance Angles C75 1.5329 (0.0136) H77A 0.9800 109.47 H77B 0.9800 109.47 109.47 H77C 0.9800 109.47 109.47 109.47 C77 - C75 H77A H77B C78 - Distance Angles C75 1.5267 (0.0139) H78A 0.9800 109.47 H78B 0.9800 109.47 109.47 H78C 0.9800 109.47 109.47 109.47 C78 - C75 H78A H78B O51 - Distance Angles C51 1.3463 (0.0126) C61 1.4688 (0.0115) 111.44 (0.80) O51 - C51 O52 - Distance Angles C51 1.1831 (0.0126) O52 - O53 - Distance Angles C54 1.4376 (0.0124) C55 1.4495 (0.0119) 108.10 (0.73) O53 - C54 O54 - Distance Angles C58 1.4159 (0.0119) C55 1.4336 (0.0121) 109.06 (0.74) O54 - C58 O55 - Distance Angles C62 1.4439 (0.0119) Si51 1.6246 (0.0075) 124.84 (0.62) O55 - C62 Si51 - Distance Angles O55 1.6246 (0.0075) C69 1.8721 (0.0110) 109.60 (0.43) C75 1.8949 (0.0100) 104.05 (0.43) 109.37 (0.45) C63 1.8997 (0.0106) 111.97 (0.43) 106.23 (0.48) 115.58 (0.46) Si51 - O55 C69 C75 FMAP and GRID set by program FMAP 2 3 28 GRID -1.000 -2 -2 1.000 2 2 R1 = 0.0948 for 3108 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.0481 0.2412 0.2047 [ 1.00 A from C19 ] Deepest hole -0.27 at 0.5799 0.2549 0.0438 [ 1.09 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 6835 / 23631 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0481 0.2412 0.2047 1.00000 0.05 0.34 1.00 C19 1.31 SI1 1.99 C20 2.06 C24 Q2 1 0.1817 0.2041 0.0020 1.00000 0.05 0.26 1.18 O3 1.98 H2 2.04 H6C 2.05 C5 Q3 1 0.6158 0.3012 0.4195 1.00000 0.05 0.25 1.08 O55 1.52 C62 1.69 C61 1.73 H60 Q4 1 0.4887 0.2192 0.5026 1.00000 0.05 0.25 1.18 O53 1.87 H52 2.01 C54 2.06 C55 Q5 1 0.6178 0.2322 0.3059 1.00000 0.05 0.25 1.04 C69 1.20 SI51 1.65 C70 1.76 H70 Q6 1 0.6853 0.2236 0.5012 1.00000 0.05 0.24 1.31 H60 1.42 O54 2.00 H56C 2.02 C60 Q7 1 0.6250 0.0838 0.4790 1.00000 0.05 0.23 0.75 H56C 1.51 C56 1.80 H56B 1.98 H56A Q8 1 0.2614 0.0007 0.1478 1.00000 0.05 0.22 1.70 H28C 1.82 H28B 2.03 H62A 2.06 C28 Q9 1 -0.0206 0.2247 0.0096 1.00000 0.05 0.22 1.10 H10 1.66 O4 1.80 C10 2.01 H3B Q10 1 0.0502 0.2029 0.0539 1.00000 0.05 0.22 1.25 H10 2.11 H6C 2.11 C10 2.17 H28A Q11 1 0.0754 0.1683 0.0938 1.00000 0.05 0.21 1.31 H28A 1.71 H14 1.89 C28 1.96 H28B Q12 1 -0.0554 0.2380 0.0566 1.00000 0.05 0.21 0.96 H10 1.81 C10 1.99 H12B 2.15 H14 Q13 1 0.2948 0.3761 0.4773 1.00000 0.05 0.21 1.35 H53B 1.59 H56B 1.98 C53 2.10 O54 Q14 1 0.2165 0.2547 0.0832 1.00000 0.05 0.20 1.33 H2 1.71 H27B 1.79 H28A 2.07 O5 Q15 1 0.9488 -0.0551 0.3176 1.00000 0.05 0.20 1.02 H65 1.66 C65 2.13 H66 2.19 C66 Q16 1 0.1599 0.3818 0.3087 1.00000 0.05 0.20 0.77 H23 1.15 C23 1.77 C22 1.92 H22 Q17 1 -0.3077 0.0417 0.2583 1.00000 0.05 0.20 1.01 H17 1.96 C17 2.37 H73 2.60 H76B Q18 1 0.6344 0.1437 0.4096 1.00000 0.05 0.20 1.52 H78B 1.76 H78A 1.90 C78 2.38 O55 Q19 1 0.0688 0.1397 -0.1384 1.00000 0.05 0.20 1.17 H7A 1.32 H7B 1.38 C7 1.72 H7C Q20 1 -0.1161 0.2767 0.0917 1.00000 0.05 0.20 0.61 H12B 1.30 C12 2.05 O5 2.05 C11 Shortest distances between peaks (including symmetry equivalents) 10 12 1.25 10 11 1.40 12 20 1.41 9 12 1.53 9 10 1.61 11 14 2.05 4 6 2.07 6 13 2.08 11 12 2.12 2 10 2.14 10 14 2.14 2 9 2.17 7 13 2.34 7 18 2.38 6 7 2.42 10 20 2.42 3 18 2.54 11 20 2.66 4 7 2.69 2 14 2.70 9 20 2.89 3 6 2.94 9 11 2.97 12 14 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.48: 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 5.14: Structure factors and derivatives 13.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 2.94: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1074a finished at 12:47:42 Total CPU time: 23.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++