+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:22:26 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 10.8380 27.4492 19.9239 90.000 92.810 90.000 ZERR 4.00 0.0006 0.0014 0.0014 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O SI UNIT 160 360 60 40 V = 5920.12 F(000) = 2360.0 Mu = 0.28 mm-1 Cell Wt = 4368.08 Rho = 1.225 MERG 2 OMIT 0 6 2 OMIT -1 0 4 SHEL 7 0.84 DFIX 1.5 0.02 C18 C19 C18 C20 C18 C17 DANG 2.5 0.02 C17 C19 C17 C20 C19 C20 FMAP 2 PLAN 10 SIZE 0.04 0.10 0.30 ACTA BOND $H WGHT 0.10960 L.S. 16 TEMP -153.00 FVAR 0.05485 SI1 4 0.277510 0.441140 0.824835 11.00000 0.03727 0.03069 = 0.03292 -0.00110 0.00269 0.00109 SI4 4 0.381431 0.345821 0.626536 11.00000 0.03364 0.03249 = 0.02548 -0.00141 -0.00085 -0.00214 SI5 4 0.323839 0.452952 0.671323 11.00000 0.03936 0.03049 = 0.03184 0.00368 -0.00202 0.00064 SI8 4 0.644687 0.290031 0.785651 11.00000 0.03580 0.04344 = 0.02958 0.00029 0.00043 0.00514 SI2 4 0.294654 0.331572 0.872509 11.00000 0.03758 0.02810 = 0.03518 -0.00189 0.00238 -0.00131 SI6 4 0.559290 0.455165 0.859486 11.00000 0.03914 0.02857 = 0.02997 -0.00141 0.00299 -0.00488 SI9 4 0.661759 0.361837 0.666251 11.00000 0.03202 0.03847 = 0.03191 0.00126 0.00158 -0.00198 SI3 4 0.362300 0.273515 0.746378 11.00000 0.03782 0.03031 = 0.02973 -0.00104 0.00206 -0.00496 SI7 4 0.575664 0.346987 0.910930 11.00000 0.03786 0.02891 = 0.03028 0.00186 0.00065 0.00096 SI10 4 0.604286 0.469359 0.705929 11.00000 0.04181 0.03557 = 0.03457 -0.00360 0.00449 -0.00624 O9 3 0.530276 0.346251 0.630078 11.00000 0.03423 0.03434 = 0.02235 0.00202 0.00193 -0.00453 O8 3 0.510559 0.269276 0.761996 11.00000 0.04871 0.02735 = 0.03872 0.00497 0.00927 0.00518 O6 3 0.410504 0.459724 0.854206 11.00000 0.03879 0.02335 = 0.04976 -0.00423 -0.00097 -0.00035 O10 3 0.461995 0.474369 0.679686 11.00000 0.04436 0.04031 = 0.05137 0.00527 0.00009 0.00513 O7 3 0.430606 0.334962 0.909267 11.00000 0.03233 0.03482 = 0.03405 -0.00418 -0.00213 -0.00331 O2 3 0.296510 0.291495 0.812871 11.00000 0.04678 0.03197 = 0.03126 -0.00437 0.00772 -0.00655 O15 3 0.611605 0.465043 0.787138 11.00000 0.06146 0.04206 = 0.03004 -0.00397 0.01274 -0.01044 O4 3 0.329860 0.400563 0.634670 11.00000 0.04141 0.03151 = 0.04092 -0.00271 -0.00518 0.00463 O11 3 0.597754 0.401203 0.882829 11.00000 0.03948 0.04006 = 0.04442 0.00346 -0.00312 0.00107 O12 3 0.641344 0.309410 0.862256 11.00000 0.03875 0.03712 = 0.03584 0.00354 0.00235 0.00705 O14 3 0.662597 0.421071 0.675752 11.00000 0.04007 0.04654 = 0.04400 -0.00082 0.00401 -0.00255 O5 3 0.268836 0.447528 0.744935 11.00000 0.04752 0.04392 = 0.04029 0.01134 0.00305 0.00118 O13 3 0.676186 0.336078 0.738636 11.00000 0.03858 0.06761 = 0.03631 0.01569 -0.00170 -0.01177 O1 3 0.261140 0.383554 0.839623 11.00000 0.04485 0.03805 = 0.05285 0.00157 -0.00713 -0.00469 O3 3 0.334885 0.313024 0.688402 11.00000 0.03253 0.03839 = 0.03953 0.00861 0.00015 -0.00467 C9 1 0.305535 0.213126 0.719817 11.00000 0.04399 0.04072 = 0.04360 -0.00287 0.01199 0.00115 AFIX 23 H9A 2 0.343494 0.205253 0.676942 11.00000 -1.20000 H9B 2 0.338120 0.189280 0.753491 11.00000 -1.20000 AFIX 0 C13 1 0.323999 0.319675 0.545444 11.00000 0.02734 0.03469 = 0.04381 -0.00565 -0.00155 -0.00159 AFIX 23 H13A 2 0.373122 0.290103 0.536914 11.00000 -1.20000 H13B 2 0.237576 0.309096 0.550335 11.00000 -1.20000 AFIX 0 C37 1 0.690240 0.523287 0.676602 11.00000 0.05060 0.03986 = 0.03223 0.00784 -0.00420 -0.01486 AFIX 23 H37A 2 0.654298 0.532876 0.631904 11.00000 -1.20000 H37B 2 0.676555 0.550618 0.707795 11.00000 -1.20000 AFIX 0 C5 1 0.181716 0.312813 0.933840 11.00000 0.04806 0.02908 = 0.03516 0.00427 0.00187 -0.00162 AFIX 23 H5A 2 0.215239 0.283474 0.957170 11.00000 -1.20000 H5B 2 0.178699 0.338950 0.967961 11.00000 -1.20000 AFIX 0 C25 1 0.640083 0.342875 0.998153 11.00000 0.05133 0.05430 = 0.02666 -0.00482 -0.00230 0.00672 AFIX 23 H25A 2 0.731085 0.340467 0.996923 11.00000 -1.20000 H25B 2 0.621149 0.373635 1.021467 11.00000 -1.20000 AFIX 0 C14 1 0.326762 0.351682 0.484278 11.00000 0.05207 0.04532 = 0.03468 0.00943 -0.00120 -0.00701 AFIX 13 H14 2 0.269363 0.379599 0.490949 11.00000 -1.20000 AFIX 0 C15 1 0.279541 0.324023 0.420646 11.00000 0.08953 0.05464 = 0.03582 0.00123 -0.00453 0.00120 AFIX 137 H15A 2 0.284305 0.345342 0.381402 11.00000 -1.50000 H15B 2 0.193601 0.314090 0.425559 11.00000 -1.50000 H15C 2 0.330732 0.295076 0.414572 11.00000 -1.50000 AFIX 0 C36 1 1.001409 0.358363 0.571125 11.00000 0.04264 0.06099 = 0.09042 0.00151 0.03048 0.00456 AFIX 137 H36A 2 1.079498 0.375871 0.579334 11.00000 -1.50000 H36B 2 0.967540 0.365785 0.525767 11.00000 -1.50000 H36C 2 1.016077 0.323236 0.575226 11.00000 -1.50000 AFIX 0 C26 1 0.594322 0.300409 1.040186 11.00000 0.06301 0.05038 = 0.04603 0.00266 -0.00487 -0.00153 AFIX 13 H26 2 0.502649 0.303703 1.041954 11.00000 -1.20000 AFIX 0 C35 1 0.963366 0.369233 0.693947 11.00000 0.05429 0.09604 = 0.07337 -0.01722 -0.01518 -0.01672 AFIX 137 H35A 2 0.972782 0.334637 0.705215 11.00000 -1.50000 H35B 2 0.907689 0.384609 0.724952 11.00000 -1.50000 H35C 2 1.044243 0.385227 0.697828 11.00000 -1.50000 AFIX 0 C17 1 0.220470 0.494412 0.624362 11.00000 0.08913 0.04554 = 0.03607 -0.00394 -0.00723 0.02048 AFIX 23 H17A 2 0.136142 0.480688 0.625619 11.00000 -1.20000 H17B 2 0.220184 0.525481 0.649589 11.00000 -1.20000 AFIX 0 C33 1 0.788235 0.344586 0.612065 11.00000 0.04549 0.02359 = 0.05448 0.00337 0.00349 -0.00317 AFIX 23 H33A 2 0.807511 0.309717 0.619752 11.00000 -1.20000 H33B 2 0.758164 0.348108 0.564589 11.00000 -1.20000 AFIX 0 C34 1 0.909805 0.374227 0.622531 11.00000 0.04617 0.04885 = 0.05981 -0.00764 0.01355 -0.00474 AFIX 13 H34 2 0.889927 0.409373 0.614394 11.00000 -1.20000 AFIX 0 C21 1 0.626805 0.499665 0.921167 11.00000 0.06291 0.04182 = 0.03115 -0.01297 0.00746 -0.00477 AFIX 23 H21A 2 0.590479 0.492975 0.964858 11.00000 -1.20000 H21B 2 0.716265 0.492578 0.926908 11.00000 -1.20000 AFIX 0 C30 1 0.759042 0.200615 0.830793 11.00000 0.07731 0.05006 = 0.04531 -0.00448 -0.00178 0.01619 AFIX 13 H30 2 0.749336 0.214247 0.876780 11.00000 -1.20000 AFIX 0 C27 1 0.647947 0.302229 1.111909 11.00000 0.10647 0.10614 = 0.04120 0.01362 -0.01167 0.00597 AFIX 137 H27A 2 0.617294 0.274450 1.137118 11.00000 -1.50000 H27B 2 0.622905 0.332633 1.133144 11.00000 -1.50000 H27C 2 0.738285 0.300780 1.111804 11.00000 -1.50000 AFIX 0 C3 1 0.086987 0.551436 0.923917 11.00000 0.07040 0.08227 = 0.10348 -0.04237 0.00982 0.01832 AFIX 137 H3A 2 0.007025 0.549240 0.898919 11.00000 -1.50000 H3B 2 0.107131 0.585727 0.932679 11.00000 -1.50000 H3C 2 0.082697 0.534019 0.966676 11.00000 -1.50000 AFIX 0 C6 1 0.051475 0.301675 0.910651 11.00000 0.03943 0.05116 = 0.05835 -0.00510 0.00641 -0.00304 AFIX 13 H6 2 0.054262 0.279055 0.871410 11.00000 -1.20000 AFIX 0 C38 1 0.827170 0.516797 0.671208 11.00000 0.03554 0.06617 = 0.05282 0.00745 0.00386 -0.00237 AFIX 13 H38 2 0.840203 0.489418 0.639210 11.00000 -1.20000 AFIX 0 C31 1 0.876730 0.170588 0.833026 11.00000 0.07680 0.06703 = 0.13149 -0.01758 -0.01527 0.04690 AFIX 137 H31A 2 0.868061 0.142906 0.863499 11.00000 -1.50000 H31B 2 0.946373 0.190901 0.849183 11.00000 -1.50000 H31C 2 0.891761 0.158564 0.787839 11.00000 -1.50000 AFIX 0 C10 1 0.172144 0.204407 0.710054 11.00000 0.04963 0.06270 = 0.18036 -0.04188 -0.00243 -0.00029 AFIX 13 H10 2 0.141016 0.205815 0.756440 11.00000 -1.20000 AFIX 0 C29 1 0.764488 0.242844 0.782858 11.00000 0.04344 0.05685 = 0.03926 -0.00975 0.00196 0.00219 AFIX 23 H29A 2 0.762280 0.229477 0.736665 11.00000 -1.20000 H29B 2 0.845657 0.258929 0.790775 11.00000 -1.20000 AFIX 0 C4 1 0.203953 0.559040 0.820251 11.00000 0.07982 0.03133 = 0.09258 0.00083 -0.00864 -0.00848 AFIX 137 H4A 2 0.131811 0.555497 0.789014 11.00000 -1.50000 H4B 2 0.277835 0.547430 0.798721 11.00000 -1.50000 H4C 2 0.214561 0.593425 0.832452 11.00000 -1.50000 AFIX 0 C28 1 0.619937 0.251856 1.009728 11.00000 0.06319 0.07044 = 0.06712 0.02149 0.00480 -0.00032 AFIX 137 H28A 2 0.708387 0.249048 1.002339 11.00000 -1.50000 H28B 2 0.572818 0.248749 0.966690 11.00000 -1.50000 H28C 2 0.595387 0.225964 1.040202 11.00000 -1.50000 AFIX 0 C16 1 0.451363 0.372373 0.472326 11.00000 0.08134 0.07610 = 0.03649 0.01026 0.01548 0.00018 AFIX 137 H16A 2 0.476970 0.393957 0.509637 11.00000 -1.50000 H16B 2 0.447570 0.390920 0.430246 11.00000 -1.50000 H16C 2 0.511236 0.345809 0.469261 11.00000 -1.50000 AFIX 0 C7 1 -0.019902 0.276725 0.963900 11.00000 0.05412 0.08630 = 0.07205 0.00271 0.02679 -0.02098 AFIX 137 H7A 2 0.023223 0.246862 0.978381 11.00000 -1.50000 H7B 2 -0.102801 0.268520 0.945472 11.00000 -1.50000 H7C 2 -0.026521 0.298576 1.002455 11.00000 -1.50000 AFIX 0 C32 1 0.649882 0.167857 0.814602 11.00000 0.10613 0.05901 = 0.07553 0.03810 0.02757 0.02800 AFIX 137 H32A 2 0.573351 0.185263 0.823302 11.00000 -1.50000 H32B 2 0.656185 0.138636 0.842824 11.00000 -1.50000 H32C 2 0.649183 0.158386 0.767160 11.00000 -1.50000 AFIX 0 C2 1 0.184707 0.529060 0.883484 11.00000 0.04274 0.05139 = 0.08201 -0.01557 -0.00347 0.01251 AFIX 13 H2 2 0.263769 0.529999 0.911522 11.00000 -1.20000 AFIX 0 C8 1 -0.015815 0.347764 0.886840 11.00000 0.03776 0.08347 = 0.11106 0.01184 0.00222 -0.01077 AFIX 137 H8A 2 -0.020996 0.370457 0.924571 11.00000 -1.50000 H8B 2 -0.099293 0.339349 0.869518 11.00000 -1.50000 H8C 2 0.029582 0.363118 0.851124 11.00000 -1.50000 AFIX 0 C40 1 0.889007 0.562644 0.643241 11.00000 0.04197 0.08767 = 0.10527 0.05521 0.01629 -0.01926 AFIX 137 H40A 2 0.853637 0.569591 0.598043 11.00000 -1.50000 H40B 2 0.978041 0.557042 0.641163 11.00000 -1.50000 H40C 2 0.874625 0.590424 0.672750 11.00000 -1.50000 AFIX 0 C1 1 0.156783 0.475775 0.867252 11.00000 0.05157 0.04279 = 0.03430 0.00029 0.00754 0.01199 AFIX 23 H1A 2 0.079805 0.474470 0.838430 11.00000 -1.20000 H1B 2 0.140310 0.458861 0.909777 11.00000 -1.20000 AFIX 0 C12 1 0.102519 0.232919 0.676564 11.00000 0.13423 0.07789 = 0.36221 -0.00942 -0.15940 -0.01663 AFIX 137 H12A 2 0.129407 0.266580 0.684722 11.00000 -1.50000 H12B 2 0.017436 0.229012 0.690217 11.00000 -1.50000 H12C 2 0.106392 0.225409 0.628627 11.00000 -1.50000 AFIX 0 C39 1 0.892150 0.503121 0.739393 11.00000 0.06048 0.06646 = 0.08062 0.01556 -0.01129 0.00300 AFIX 137 H39A 2 0.881426 0.529547 0.771664 11.00000 -1.50000 H39B 2 0.980431 0.498024 0.733412 11.00000 -1.50000 H39C 2 0.855796 0.473121 0.756337 11.00000 -1.50000 AFIX 0 C11 1 0.143147 0.151947 0.686378 11.00000 0.06694 0.09455 = 0.31918 -0.11366 0.00561 -0.01711 AFIX 137 H11A 2 0.056953 0.144175 0.694645 11.00000 -1.50000 H11B 2 0.197802 0.129114 0.711245 11.00000 -1.50000 H11C 2 0.156268 0.149229 0.638204 11.00000 -1.50000 AFIX 0 C19 1 0.344643 0.502861 0.521107 11.00000 0.10407 0.35592 = 0.15647 0.14130 -0.01592 -0.13800 AFIX 137 H19A 2 0.357706 0.533451 0.497106 11.00000 -1.50000 H19B 2 0.336263 0.476045 0.488732 11.00000 -1.50000 H19C 2 0.415364 0.496641 0.552481 11.00000 -1.50000 AFIX 0 C24 1 0.678303 0.581878 0.962776 11.00000 0.21480 0.06452 = 0.07486 -0.02881 -0.06005 -0.02740 AFIX 137 H24A 2 0.690092 0.614766 0.945053 11.00000 -1.50000 H24B 2 0.758802 0.567706 0.976116 11.00000 -1.50000 H24C 2 0.627136 0.583518 1.001926 11.00000 -1.50000 AFIX 0 C18 1 0.240669 0.506234 0.555582 11.00000 0.42394 0.36358 = 0.08800 0.09312 0.07844 0.36521 AFIX 13 H18 2 0.199189 0.476724 0.535546 11.00000 -1.20000 AFIX 0 C23 1 0.562305 0.574800 0.855008 11.00000 0.15926 0.05939 = 0.09675 0.00020 -0.00908 -0.00311 AFIX 137 H23A 2 0.589754 0.560406 0.813270 11.00000 -1.50000 H23B 2 0.587727 0.609041 0.857498 11.00000 -1.50000 H23C 2 0.472110 0.572719 0.855723 11.00000 -1.50000 AFIX 0 C22 1 0.614154 0.550122 0.908537 11.00000 0.44362 0.03971 = 0.12482 0.00437 -0.18288 -0.05994 AFIX 13 H22 2 0.534863 0.551175 0.932134 11.00000 -1.20000 AFIX 0 C20 1 0.146869 0.543484 0.526305 11.00000 0.93196 0.71392 = 0.04807 0.09699 0.07757 0.75939 AFIX 33 H20A 2 0.169907 0.553087 0.481228 11.00000 -1.50000 H20B 2 0.146579 0.572272 0.555389 11.00000 -1.50000 H20C 2 0.064297 0.528850 0.523625 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 O 0.660 SI 1.170 Si1 - O5 O6 O1 C1 Si4 - O9 O4 O3 C13 Si5 - O10 O4 O5 C17 Si8 - O8 O12 O13 C29 Si2 - O1 O7 O2 C5 Si6 - O15 O11 O6 C21 Si9 - O13 O9 O14 C33 Si3 - O3 O2 O8 C9 Si7 - O7 O12 O11 C25 Si10 - O14 O10 O15 C37 O9 - Si4 Si9 O8 - Si8 Si3 O6 - Si1 Si6 O10 - Si5 Si10 O7 - Si7 Si2 O2 - Si3 Si2 O15 - Si6 Si10 O4 - Si4 Si5 O11 - Si6 Si7 O12 - Si7 Si8 O14 - Si10 Si9 O5 - Si1 Si5 O13 - Si9 Si8 O1 - Si2 Si1 O3 - Si3 Si4 C9 - C10 Si3 C13 - C14 Si4 C37 - C38 Si10 C5 - C6 Si2 C25 - C26 Si7 C14 - C16 C13 C15 C15 - C14 C36 - C34 C26 - C28 C27 C25 C35 - C34 C17 - C18 Si5 C33 - C34 Si9 C34 - C35 C36 C33 C21 - C22 Si6 C30 - C29 C32 C31 C27 - C26 C3 - C2 C6 - C5 C7 C8 C38 - C37 C40 C39 C31 - C30 C10 - C12 C9 C11 C29 - C30 Si8 C4 - C2 C28 - C26 C16 - C14 C7 - C6 C32 - C30 C2 - C3 C1 C4 C8 - C6 C40 - C38 C1 - C2 Si1 C12 - C10 C39 - C38 C11 - C10 C19 - C18 C24 - C22 C18 - C19 C17 C20 C23 - C22 C22 - C23 C21 C24 C20 - C18 h k l Fo^2 Sigma Why rejected -8 0 5 4.37 1.09 observed but should be systematically absent 6 0 9 4.34 1.08 observed but should be systematically absent 31314 Reflections read, of which 2048 rejected -12 =< h =< 11, -26 =< k =< 32, -23 =< l =< 23, Max. 2-theta = 50.05 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -8 7 9 11.35 0.73 3 3.99 1 Inconsistent equivalents 8987 Unique reflections, of which 0 suppressed R(int) = 0.1397 R(sigma) = 0.2504 Friedel opposites merged Maximum memory for data reduction = 7048 / 91057 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 = 8967 / 825830 wR2 = 0.2352 before cycle 1 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.3513 1.5000 -0.1487 0.0200 DFIX C18 C19 1.4355 1.5000 -0.0645 0.0200 DFIX C18 C17 2.4229 2.5000 -0.0771 0.0200 DANG C19 C20 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.096 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05485 0.00015 0.027 OSF Mean shift/su = 0.016 Maximum = 0.536 for y C20 Max. shift = 0.028 A for H19C Max. dU =-0.005 for C20 Least-squares cycle 2 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 2 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 1.3513 1.5000 -0.1487 0.0200 DFIX C18 C19 1.4359 1.5000 -0.0641 0.0200 DFIX C18 C17 2.4213 2.5000 -0.0787 0.0200 DANG C19 C20 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.096 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.010 OSF Mean shift/su = 0.009 Maximum = 0.311 for y C20 Max. shift = 0.016 A for C20 Max. dU =-0.002 for C20 Least-squares cycle 3 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 3 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 1.3504 1.5000 -0.1496 0.0200 DFIX C18 C19 1.4364 1.5000 -0.0636 0.0200 DFIX C18 C17 2.4206 2.5000 -0.0794 0.0200 DANG C19 C20 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.096 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.004 Maximum = 0.136 for x C18 Max. shift = 0.009 A for H19A Max. dU =-0.001 for C20 Least-squares cycle 4 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 4 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 1.3500 1.5000 -0.1500 0.0200 DFIX C18 C19 1.4365 1.5000 -0.0635 0.0200 DFIX C18 C17 2.4207 2.5000 -0.0793 0.0200 DANG C19 C20 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.096 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.003 Maximum = 0.093 for x C18 Max. shift = 0.003 A for C18 Max. dU = 0.000 for C20 Least-squares cycle 5 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 5 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 1.3496 1.5000 -0.1504 0.0200 DFIX C18 C19 1.4366 1.5000 -0.0634 0.0200 DFIX C18 C17 2.4209 2.5000 -0.0791 0.0200 DANG C19 C20 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.002 Maximum = 0.061 for x C18 Max. shift = 0.002 A for H19A Max. dU = 0.000 for C20 Least-squares cycle 6 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 6 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 1.3493 1.5000 -0.1507 0.0200 DFIX C18 C19 1.4367 1.5000 -0.0633 0.0200 DFIX C18 C17 2.4210 2.5000 -0.0790 0.0200 DANG C19 C20 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = 0.037 for x C18 Max. shift = 0.002 A for H19A Max. dU = 0.000 for C20 Least-squares cycle 7 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 7 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 1.3492 1.5000 -0.1508 0.0200 DFIX C18 C19 1.4367 1.5000 -0.0633 0.0200 DFIX C18 C17 2.4211 2.5000 -0.0789 0.0200 DANG C19 C20 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.001 Maximum = 0.023 for x C18 Max. shift = 0.001 A for C18 Max. dU = 0.000 for C20 Least-squares cycle 8 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 8 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 1.3491 1.5000 -0.1509 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4211 2.5000 -0.0789 0.0200 DANG C19 C20 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.015 for x C18 Max. shift = 0.001 A for H19A Max. dU = 0.000 for C20 Least-squares cycle 9 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 9 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4211 2.5000 -0.0789 0.0200 DANG C19 C20 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = 0.009 for x C18 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C20 Least-squares cycle 10 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 10 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = 0.006 for x C18 Max. shift = 0.000 A for H23A Max. dU = 0.000 for C20 Least-squares cycle 11 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 11 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = 0.004 for x C18 Max. shift = 0.000 A for H23A Max. dU = 0.000 for C20 Least-squares cycle 12 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 12 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.002 for x C18 Max. shift = 0.000 A for H23A Max. dU = 0.000 for C19 Least-squares cycle 13 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 13 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.953; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.001 OSF Mean shift/su = 0.000 Maximum = -0.002 for tors H23A Max. shift = 0.000 A for H23C Max. dU = 0.000 for C20 Least-squares cycle 14 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 14 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for tors H23A Max. shift = 0.000 A for H23A Max. dU = 0.000 for C20 Least-squares cycle 15 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 15 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H23A Max. shift = 0.000 A for H23A Max. dU = 0.000 for C19 Least-squares cycle 16 Maximum vector length = 511 Memory required = 8967 / 825830 wR2 = 0.2351 before cycle 16 for 8987 data and 605 / 605 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.05486 0.00015 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H23A Max. shift = 0.000 A for H23A Max. dU = 0.000 for C20 Largest correlation matrix elements 0.904 U12 C20 / U22 C20 0.792 U13 C18 / U23 C18 -0.548 U13 C12 / U11 C12 0.894 U12 C20 / U11 C20 0.658 U22 C20 / U11 C20 0.542 U22 C18 / U11 C18 0.868 y C20 / x C20 -0.655 U13 C22 / U11 C22 0.525 U23 C19 / U22 C19 0.853 U12 C18 / U22 C18 -0.616 U12 C19 / U11 C19 0.518 U23 C19 / U33 C19 0.853 U12 C18 / U11 C18 -0.614 U13 C12 / U33 C12 -0.507 U13 C19 / U23 C19 0.823 U13 C20 / U23 C20 -0.610 U12 C19 / U22 C19 0.798 y C18 / x C18 -0.596 U13 C22 / U33 C22 Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H9A 0.3435 0.2053 0.6769 23 0.990 0.000 C9 C10 Si3 H9B 0.3381 0.1893 0.7535 23 0.990 0.000 C9 C10 Si3 H13A 0.3731 0.2901 0.5369 23 0.990 0.000 C13 C14 Si4 H13B 0.2376 0.3091 0.5503 23 0.990 0.000 C13 C14 Si4 H37A 0.6542 0.5329 0.6319 23 0.990 0.000 C37 C38 Si10 H37B 0.6765 0.5506 0.7078 23 0.990 0.000 C37 C38 Si10 H5A 0.2152 0.2835 0.9572 23 0.990 0.000 C5 C6 Si2 H5B 0.1787 0.3390 0.9680 23 0.990 0.000 C5 C6 Si2 H25A 0.7311 0.3405 0.9969 23 0.990 0.000 C25 C26 Si7 H25B 0.6211 0.3736 1.0215 23 0.990 0.000 C25 C26 Si7 H14 0.2694 0.3796 0.4910 13 1.000 0.000 C14 C16 C13 C15 H15A 0.2842 0.3453 0.3814 137 0.980 0.000 C15 C14 H15A H15B 0.1936 0.3140 0.4256 137 0.980 0.000 C15 C14 H15A H15C 0.3307 0.2951 0.4146 137 0.980 0.000 C15 C14 H15A H36A 1.0796 0.3759 0.5794 137 0.980 0.000 C36 C34 H36A H36B 0.9676 0.3659 0.5258 137 0.980 0.000 C36 C34 H36A H36C 1.0160 0.3232 0.5752 137 0.980 0.000 C36 C34 H36A H26 0.5026 0.3037 1.0420 13 1.000 0.000 C26 C28 C27 C25 H35A 0.9729 0.3346 0.7052 137 0.980 0.000 C35 C34 H35A H35B 0.9076 0.3845 0.7250 137 0.980 0.000 C35 C34 H35A H35C 1.0442 0.3852 0.6979 137 0.980 0.000 C35 C34 H35A H17A 0.1364 0.4804 0.6248 23 0.990 0.000 C17 C18 Si5 H17B 0.2190 0.5253 0.6499 23 0.990 0.000 C17 C18 Si5 H33A 0.8075 0.3097 0.6197 23 0.990 0.000 C33 C34 Si9 H33B 0.7581 0.3481 0.5646 23 0.990 0.000 C33 C34 Si9 H34 0.8900 0.4094 0.6144 13 1.000 0.000 C34 C35 C36 C33 H21A 0.5905 0.4930 0.9649 23 0.990 0.000 C21 C22 Si6 H21B 0.7163 0.4926 0.9269 23 0.990 0.000 C21 C22 Si6 H30 0.7493 0.2143 0.8768 13 1.000 0.000 C30 C29 C32 C31 H27A 0.6174 0.2744 1.1371 137 0.980 0.000 C27 C26 H27A H27B 0.6228 0.3326 1.1332 137 0.980 0.000 C27 C26 H27A H27C 0.7383 0.3009 1.1118 137 0.980 0.000 C27 C26 H27A H3A 0.0070 0.5493 0.8989 137 0.980 0.000 C3 C2 H3A H3B 0.1072 0.5857 0.9328 137 0.980 0.000 C3 C2 H3A H3C 0.0826 0.5340 0.9667 137 0.980 0.000 C3 C2 H3A H6 0.0543 0.2791 0.8714 13 1.000 0.000 C6 C5 C7 C8 H38 0.8402 0.4894 0.6392 13 1.000 0.000 C38 C37 C40 C39 H31A 0.8682 0.1429 0.8636 137 0.980 0.000 C31 C30 H31A H31B 0.9465 0.1909 0.8491 137 0.980 0.000 C31 C30 H31A H31C 0.8918 0.1586 0.7879 137 0.980 0.000 C31 C30 H31A H10 0.1411 0.2058 0.7564 13 1.000 0.000 C10 C12 C9 C11 H29A 0.7622 0.2295 0.7367 23 0.990 0.000 C29 C30 Si8 H29B 0.8457 0.2589 0.7907 23 0.990 0.000 C29 C30 Si8 H4A 0.1318 0.5555 0.7890 137 0.980 0.000 C4 C2 H4A H4B 0.2779 0.5474 0.7987 137 0.980 0.000 C4 C2 H4A H4C 0.2147 0.5934 0.8325 137 0.980 0.000 C4 C2 H4A H28A 0.7083 0.2490 1.0023 137 0.980 0.000 C28 C26 H28A H28B 0.5727 0.2487 0.9667 137 0.980 0.000 C28 C26 H28A H28C 0.5954 0.2259 1.0403 137 0.980 0.000 C28 C26 H28A H16A 0.4770 0.3939 0.5097 137 0.980 0.000 C16 C14 H16A H16B 0.4475 0.3909 0.4303 137 0.980 0.000 C16 C14 H16A H16C 0.5112 0.3458 0.4693 137 0.980 0.000 C16 C14 H16A H7A 0.0235 0.2469 0.9785 137 0.980 0.000 C7 C6 H7A H7B -0.1026 0.2683 0.9454 137 0.980 0.000 C7 C6 H7A H7C -0.0269 0.2986 1.0024 137 0.980 0.000 C7 C6 H7A H32A 0.5734 0.1852 0.8234 137 0.980 0.000 C32 C30 H32A H32B 0.6563 0.1386 0.8428 137 0.980 0.000 C32 C30 H32A H32C 0.6491 0.1584 0.7671 137 0.980 0.000 C32 C30 H32A H2 0.2638 0.5300 0.9115 13 1.000 0.000 C2 C3 C1 C4 H8A -0.0209 0.3705 0.9246 137 0.980 0.000 C8 C6 H8A H8B -0.0994 0.3393 0.8696 137 0.980 0.000 C8 C6 H8A H8C 0.0294 0.3631 0.8511 137 0.980 0.000 C8 C6 H8A H40A 0.8537 0.5696 0.5980 137 0.980 0.000 C40 C38 H40A H40B 0.9781 0.5570 0.6412 137 0.980 0.000 C40 C38 H40A H40C 0.8747 0.5904 0.6727 137 0.980 0.000 C40 C38 H40A H1A 0.0798 0.4745 0.8384 23 0.990 0.000 C1 C2 Si1 H1B 0.1403 0.4589 0.9098 23 0.990 0.000 C1 C2 Si1 H12A 0.1293 0.2666 0.6848 137 0.980 0.000 C12 C10 H12A H12B 0.0174 0.2290 0.6902 137 0.980 0.000 C12 C10 H12A H12C 0.1064 0.2254 0.6286 137 0.980 0.000 C12 C10 H12A H39A 0.8814 0.5296 0.7717 137 0.980 0.000 C39 C38 H39A H39B 0.9804 0.4980 0.7335 137 0.980 0.000 C39 C38 H39A H39C 0.8557 0.4732 0.7564 137 0.980 0.000 C39 C38 H39A H11A 0.0570 0.1442 0.6945 137 0.980 0.000 C11 C10 H11A H11B 0.1978 0.1291 0.7111 137 0.980 0.000 C11 C10 H11A H11C 0.1563 0.1493 0.6381 137 0.980 0.000 C11 C10 H11A H19A 0.3597 0.5328 0.4967 137 0.980 0.000 C19 C18 H19A H19B 0.3345 0.4756 0.4886 137 0.980 0.000 C19 C18 H19A H19C 0.4160 0.4955 0.5519 137 0.980 0.000 C19 C18 H19A H24A 0.6907 0.6147 0.9450 137 0.980 0.000 C24 C22 H24A H24B 0.7584 0.5675 0.9764 137 0.980 0.000 C24 C22 H24A H24C 0.6267 0.5837 1.0018 137 0.980 0.000 C24 C22 H24A H18 0.1987 0.4779 0.5354 13 1.000 0.000 C18 C19 C17 C20 H23A 0.5901 0.5605 0.8133 137 0.980 0.000 C23 C22 H23A H23B 0.5873 0.6091 0.8576 137 0.980 0.000 C23 C22 H23A H23C 0.4721 0.5725 0.8556 137 0.980 0.000 C23 C22 H23A H22 0.5348 0.5512 0.9321 13 1.000 0.000 C22 C23 C21 C24 H20A 0.1737 0.5544 0.4818 33 0.980 0.000 C20 C18 H20A H20B 0.1518 0.5736 0.5561 33 0.980 0.000 C20 C18 H20A H20C 0.0670 0.5310 0.5243 33 0.980 0.000 C20 C18 H20A s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.27751 0.44114 0.82483 1.00000 0.03733 0.03068 0.03293 -0.00109 0.00267 0.00107 0.03361 0.00418 0.00021 0.00009 0.00012 0.00000 0.00155 0.00157 0.00163 0.00119 0.00116 0.00108 0.00065 Si4 0.38143 0.34582 0.62654 1.00000 0.03364 0.03250 0.02553 -0.00141 -0.00086 -0.00215 0.03063 0.00399 0.00021 0.00008 0.00012 0.00000 0.00144 0.00153 0.00146 0.00116 0.00107 0.00108 0.00062 Si5 0.32384 0.45295 0.67133 1.00000 0.03932 0.03051 0.03188 0.00368 -0.00203 0.00063 0.03403 0.00417 0.00022 0.00009 0.00012 0.00000 0.00153 0.00155 0.00157 0.00121 0.00114 0.00112 0.00065 Si8 0.64469 0.29003 0.78565 1.00000 0.03581 0.04343 0.02958 0.00028 0.00042 0.00513 0.03632 0.00430 0.00021 0.00009 0.00012 0.00000 0.00152 0.00168 0.00160 0.00126 0.00114 0.00115 0.00067 Si2 0.29466 0.33157 0.87251 1.00000 0.03762 0.02808 0.03522 -0.00190 0.00238 -0.00132 0.03362 0.00416 0.00022 0.00008 0.00012 0.00000 0.00150 0.00151 0.00157 0.00120 0.00114 0.00109 0.00064 Si6 0.55929 0.45517 0.85949 1.00000 0.03917 0.02857 0.02998 -0.00143 0.00301 -0.00489 0.03253 0.00411 0.00022 0.00008 0.00012 0.00000 0.00153 0.00153 0.00153 0.00116 0.00111 0.00109 0.00063 Si9 0.66176 0.36184 0.66625 1.00000 0.03203 0.03845 0.03190 0.00125 0.00157 -0.00198 0.03413 0.00416 0.00021 0.00009 0.00012 0.00000 0.00148 0.00171 0.00160 0.00122 0.00113 0.00109 0.00066 Si3 0.36231 0.27352 0.74638 1.00000 0.03781 0.03033 0.02973 -0.00106 0.00207 -0.00496 0.03261 0.00403 0.00021 0.00008 0.00012 0.00000 0.00151 0.00152 0.00153 0.00118 0.00112 0.00110 0.00064 Si7 0.57566 0.34699 0.91093 1.00000 0.03786 0.02895 0.03026 0.00187 0.00064 0.00099 0.03239 0.00418 0.00021 0.00008 0.00012 0.00000 0.00149 0.00152 0.00152 0.00119 0.00112 0.00110 0.00063 Si10 0.60428 0.46936 0.70593 1.00000 0.04181 0.03556 0.03456 -0.00362 0.00450 -0.00624 0.03722 0.00424 0.00022 0.00009 0.00012 0.00000 0.00159 0.00162 0.00162 0.00123 0.00117 0.00117 0.00067 O9 0.53029 0.34625 0.63008 1.00000 0.03425 0.03439 0.02232 0.00194 0.00197 -0.00454 0.03030 0.00861 0.00045 0.00018 0.00024 0.00000 0.00339 0.00342 0.00333 0.00260 0.00250 0.00253 0.00136 O8 0.51052 0.26928 0.76198 1.00000 0.04875 0.02721 0.03868 0.00491 0.00925 0.00515 0.03798 0.00962 0.00049 0.00019 0.00027 0.00000 0.00388 0.00347 0.00377 0.00276 0.00284 0.00266 0.00149 O6 0.41049 0.45973 0.85420 1.00000 0.03867 0.02338 0.04981 -0.00429 -0.00097 -0.00038 0.03739 0.00905 0.00047 0.00018 0.00028 0.00000 0.00360 0.00334 0.00400 0.00282 0.00278 0.00257 0.00147 O10 0.46201 0.47437 0.67968 1.00000 0.04443 0.04034 0.05125 0.00520 0.00011 0.00514 0.04542 0.01000 0.00050 0.00020 0.00029 0.00000 0.00388 0.00383 0.00419 0.00316 0.00300 0.00290 0.00160 O7 0.43060 0.33496 0.90926 1.00000 0.03234 0.03487 0.03411 -0.00415 -0.00215 -0.00331 0.03390 0.00868 0.00045 0.00019 0.00026 0.00000 0.00338 0.00352 0.00357 0.00271 0.00260 0.00255 0.00142 O2 0.29653 0.29150 0.81287 1.00000 0.04680 0.03198 0.03125 -0.00439 0.00773 -0.00659 0.03649 0.00900 0.00048 0.00018 0.00026 0.00000 0.00362 0.00355 0.00361 0.00280 0.00271 0.00267 0.00146 O15 0.61162 0.46505 0.78714 1.00000 0.06157 0.04198 0.03015 -0.00396 0.01280 -0.01046 0.04422 0.00964 0.00053 0.00020 0.00027 0.00000 0.00406 0.00391 0.00378 0.00296 0.00291 0.00300 0.00158 O4 0.32985 0.40056 0.63469 1.00000 0.04147 0.03149 0.04102 -0.00282 -0.00517 0.00461 0.03823 0.00911 0.00048 0.00019 0.00027 0.00000 0.00350 0.00362 0.00391 0.00290 0.00272 0.00267 0.00148 O11 0.59775 0.40120 0.88284 1.00000 0.03952 0.04008 0.04440 0.00344 -0.00322 0.00115 0.04150 0.00951 0.00048 0.00020 0.00028 0.00000 0.00354 0.00395 0.00397 0.00308 0.00278 0.00276 0.00153 O12 0.64133 0.30941 0.86226 1.00000 0.03876 0.03718 0.03583 0.00356 0.00240 0.00708 0.03724 0.00943 0.00047 0.00019 0.00027 0.00000 0.00345 0.00362 0.00378 0.00288 0.00265 0.00269 0.00146 O14 0.66259 0.42108 0.67575 1.00000 0.04006 0.04669 0.04386 -0.00082 0.00400 -0.00252 0.04347 0.00976 0.00049 0.00021 0.00029 0.00000 0.00366 0.00415 0.00405 0.00315 0.00282 0.00286 0.00157 O5 0.26884 0.44752 0.74493 1.00000 0.04750 0.04409 0.04029 0.01136 0.00307 0.00118 0.04393 0.01018 0.00051 0.00020 0.00029 0.00000 0.00384 0.00392 0.00412 0.00302 0.00291 0.00285 0.00158 O13 0.67616 0.33608 0.73862 1.00000 0.03850 0.06760 0.03622 0.01561 -0.00172 -0.01179 0.04756 0.00994 0.00049 0.00022 0.00028 0.00000 0.00365 0.00455 0.00394 0.00332 0.00284 0.00305 0.00168 O1 0.26113 0.38355 0.83963 1.00000 0.04486 0.03806 0.05275 0.00163 -0.00716 -0.00476 0.04554 0.00954 0.00050 0.00020 0.00030 0.00000 0.00379 0.00407 0.00438 0.00314 0.00302 0.00284 0.00164 O3 0.33489 0.31303 0.68840 1.00000 0.03250 0.03841 0.03955 0.00857 0.00022 -0.00471 0.03687 0.00915 0.00046 0.00019 0.00027 0.00000 0.00337 0.00362 0.00374 0.00298 0.00262 0.00261 0.00146 C9 0.30554 0.21313 0.71981 1.00000 0.04392 0.04056 0.04362 -0.00287 0.01205 0.00119 0.04238 0.01505 0.00078 0.00030 0.00046 0.00000 0.00599 0.00592 0.00621 0.00465 0.00440 0.00433 0.00237 H9A 0.34351 0.20527 0.67693 1.00000 0.05085 0.00000 0.00000 H9B 0.33813 0.18928 0.75348 1.00000 0.05085 0.00000 0.00000 C13 0.32400 0.31966 0.54544 1.00000 0.02736 0.03461 0.04377 -0.00568 -0.00153 -0.00150 0.03535 0.01357 0.00073 0.00030 0.00041 0.00000 0.00491 0.00552 0.00599 0.00463 0.00400 0.00383 0.00221 H13A 0.37314 0.29010 0.53691 1.00000 0.04243 0.00000 0.00000 H13B 0.23758 0.30908 0.55032 1.00000 0.04243 0.00000 0.00000 C37 0.69019 0.52330 0.67662 1.00000 0.05047 0.03993 0.03226 0.00772 -0.00404 -0.01488 0.04108 0.01474 0.00078 0.00031 0.00044 0.00000 0.00622 0.00595 0.00563 0.00452 0.00429 0.00450 0.00236 H37A 0.65424 0.53289 0.63192 1.00000 0.04930 0.00000 0.00000 H37B 0.67650 0.55062 0.70782 1.00000 0.04930 0.00000 0.00000 C5 0.18172 0.31282 0.93384 1.00000 0.04814 0.02912 0.03517 0.00433 0.00192 -0.00155 0.03748 0.01469 0.00075 0.00031 0.00041 0.00000 0.00596 0.00535 0.00568 0.00427 0.00431 0.00412 0.00224 H5A 0.21525 0.28348 0.95717 1.00000 0.04498 0.00000 0.00000 H5B 0.17868 0.33896 0.96795 1.00000 0.04498 0.00000 0.00000 C25 0.64005 0.34289 0.99815 1.00000 0.05132 0.05426 0.02683 -0.00489 -0.00233 0.00681 0.04428 0.01542 0.00083 0.00034 0.00041 0.00000 0.00605 0.00657 0.00559 0.00480 0.00444 0.00482 0.00244 H25A 0.73106 0.34049 0.99692 1.00000 0.05313 0.00000 0.00000 H25B 0.62109 0.37365 1.02145 1.00000 0.05313 0.00000 0.00000 C14 0.32677 0.35169 0.48428 1.00000 0.05215 0.04539 0.03473 0.00964 -0.00126 -0.00693 0.04420 0.01557 0.00085 0.00034 0.00044 0.00000 0.00629 0.00612 0.00617 0.00505 0.00471 0.00466 0.00245 H14 0.26936 0.37960 0.49095 1.00000 0.05304 0.00000 0.00000 C15 0.27952 0.32399 0.42066 1.00000 0.08975 0.05457 0.03572 0.00131 -0.00463 0.00114 0.06027 0.01688 0.00099 0.00036 0.00047 0.00000 0.00804 0.00705 0.00645 0.00542 0.00549 0.00568 0.00291 H15A 0.28422 0.34530 0.38140 1.00000 0.09040 0.00000 0.00000 H15B 0.19360 0.31404 0.42560 1.00000 0.09040 0.00000 0.00000 H15C 0.33075 0.29505 0.41459 1.00000 0.09040 0.00000 0.00000 C36 1.00143 0.35838 0.57112 1.00000 0.04257 0.06096 0.09069 0.00155 0.03048 0.00451 0.06385 0.01924 0.00087 0.00036 0.00055 0.00000 0.00627 0.00730 0.00887 0.00624 0.00577 0.00489 0.00311 H36A 1.07956 0.37586 0.57936 1.00000 0.09577 0.00000 0.00000 H36B 0.96758 0.36585 0.52577 1.00000 0.09577 0.00000 0.00000 H36C 1.01602 0.32325 0.57516 1.00000 0.09577 0.00000 0.00000 C26 0.59432 0.30042 1.04020 1.00000 0.06278 0.05090 0.04600 0.00283 -0.00479 -0.00161 0.05347 0.01703 0.00093 0.00037 0.00048 0.00000 0.00688 0.00715 0.00700 0.00568 0.00516 0.00528 0.00268 H26 0.50265 0.30371 1.04197 1.00000 0.06416 0.00000 0.00000 C35 0.96337 0.36922 0.69395 1.00000 0.05410 0.09634 0.07314 -0.01747 -0.01510 -0.01669 0.07513 0.01758 0.00096 0.00043 0.00057 0.00000 0.00703 0.00943 0.00904 0.00706 0.00604 0.00611 0.00347 H35A 0.97288 0.33462 0.70518 1.00000 0.11269 0.00000 0.00000 H35B 0.90763 0.38455 0.72496 1.00000 0.11269 0.00000 0.00000 H35C 1.04421 0.38524 0.69786 1.00000 0.11269 0.00000 0.00000 C17 0.22053 0.49443 0.62430 1.00000 0.08990 0.04545 0.03585 -0.00391 -0.00737 0.02062 0.05741 0.01793 0.00095 0.00034 0.00044 0.00000 0.00803 0.00654 0.00663 0.00507 0.00533 0.00547 0.00287 H17A 0.13642 0.48041 0.62476 1.00000 0.06889 0.00000 0.00000 H17B 0.21899 0.52531 0.64993 1.00000 0.06889 0.00000 0.00000 C33 0.78822 0.34457 0.61205 1.00000 0.04556 0.02343 0.05460 0.00341 0.00353 -0.00318 0.04116 0.01497 0.00075 0.00030 0.00047 0.00000 0.00579 0.00521 0.00655 0.00457 0.00462 0.00414 0.00236 H33A 0.80748 0.30970 0.61973 1.00000 0.04939 0.00000 0.00000 H33B 0.75815 0.34810 0.56457 1.00000 0.04939 0.00000 0.00000 C34 0.90986 0.37423 0.62254 1.00000 0.04611 0.04887 0.05977 -0.00771 0.01355 -0.00459 0.05122 0.01650 0.00082 0.00035 0.00050 0.00000 0.00628 0.00650 0.00752 0.00538 0.00531 0.00480 0.00268 H34 0.88997 0.40938 0.61443 1.00000 0.06147 0.00000 0.00000 C21 0.62681 0.49965 0.92117 1.00000 0.06293 0.04212 0.03100 -0.01297 0.00747 -0.00465 0.04518 0.01471 0.00086 0.00032 0.00043 0.00000 0.00658 0.00656 0.00589 0.00467 0.00464 0.00468 0.00250 H21A 0.59050 0.49296 0.96486 1.00000 0.05422 0.00000 0.00000 H21B 0.71627 0.49257 0.92690 1.00000 0.05422 0.00000 0.00000 C30 0.75905 0.20063 0.83081 1.00000 0.07731 0.04988 0.04555 -0.00442 -0.00171 0.01604 0.05773 0.01877 0.00098 0.00037 0.00051 0.00000 0.00808 0.00721 0.00704 0.00573 0.00546 0.00603 0.00286 H30 0.74933 0.21427 0.87679 1.00000 0.06928 0.00000 0.00000 C27 0.64792 0.30225 1.11192 1.00000 0.10627 0.10656 0.04124 0.01373 -0.01151 0.00583 0.08518 0.02049 0.00114 0.00046 0.00052 0.00000 0.00956 0.01022 0.00763 0.00689 0.00636 0.00759 0.00374 H27A 0.61736 0.27444 1.13712 1.00000 0.12777 0.00000 0.00000 H27B 0.62277 0.33263 1.13317 1.00000 0.12777 0.00000 0.00000 H27C 0.73827 0.30085 1.11182 1.00000 0.12777 0.00000 0.00000 C3 0.08698 0.55143 0.92394 1.00000 0.07043 0.08259 0.10366 -0.04274 0.00969 0.01827 0.08538 0.02041 0.00102 0.00043 0.00064 0.00000 0.00819 0.00892 0.01029 0.00765 0.00697 0.00644 0.00388 H3A 0.00703 0.54928 0.89892 1.00000 0.12807 0.00000 0.00000 H3B 0.10719 0.58570 0.93277 1.00000 0.12807 0.00000 0.00000 H3C 0.08263 0.53397 0.96666 1.00000 0.12807 0.00000 0.00000 C6 0.05149 0.30167 0.91065 1.00000 0.03930 0.05135 0.05843 -0.00511 0.00636 -0.00313 0.04956 0.01641 0.00080 0.00035 0.00050 0.00000 0.00613 0.00678 0.00697 0.00547 0.00498 0.00490 0.00259 H6 0.05429 0.27905 0.87140 1.00000 0.05948 0.00000 0.00000 C38 0.82717 0.51680 0.67122 1.00000 0.03567 0.06632 0.05318 0.00752 0.00386 -0.00236 0.05167 0.01695 0.00079 0.00036 0.00049 0.00000 0.00609 0.00729 0.00708 0.00556 0.00487 0.00490 0.00267 H38 0.84019 0.48941 0.63924 1.00000 0.06200 0.00000 0.00000 C31 0.87681 0.17061 0.83303 1.00000 0.07680 0.06704 0.13180 -0.01743 -0.01523 0.04688 0.09255 0.02181 0.00103 0.00042 0.00068 0.00000 0.00844 0.00838 0.01176 0.00774 0.00757 0.00664 0.00423 H31A 0.86821 0.14295 0.86355 1.00000 0.13882 0.00000 0.00000 H31B 0.94645 0.19094 0.84913 1.00000 0.13882 0.00000 0.00000 H31C 0.89179 0.15856 0.78786 1.00000 0.13882 0.00000 0.00000 C10 0.17220 0.20440 0.71003 1.00000 0.04969 0.06280 0.17963 -0.04160 -0.00232 -0.00023 0.09763 0.02160 0.00110 0.00045 0.00088 0.00000 0.00823 0.00936 0.01540 0.00953 0.00819 0.00643 0.00478 H10 0.14107 0.20577 0.75642 1.00000 0.11716 0.00000 0.00000 C29 0.76448 0.24284 0.78285 1.00000 0.04340 0.05681 0.03932 -0.00990 0.00203 0.00217 0.04651 0.01595 0.00079 0.00034 0.00046 0.00000 0.00585 0.00684 0.00627 0.00532 0.00449 0.00469 0.00253 H29A 0.76225 0.22946 0.73666 1.00000 0.05581 0.00000 0.00000 H29B 0.84566 0.25893 0.79075 1.00000 0.05581 0.00000 0.00000 C4 0.20400 0.55902 0.82026 1.00000 0.08006 0.03122 0.09258 0.00073 -0.00873 -0.00856 0.06838 0.01816 0.00101 0.00035 0.00059 0.00000 0.00818 0.00632 0.00966 0.00627 0.00658 0.00526 0.00327 H4A 0.13185 0.55550 0.78903 1.00000 0.10257 0.00000 0.00000 H4B 0.27786 0.54739 0.79873 1.00000 0.10257 0.00000 0.00000 H4C 0.21466 0.59340 0.83246 1.00000 0.10257 0.00000 0.00000 C28 0.61990 0.25182 1.00974 1.00000 0.06320 0.07010 0.06741 0.02102 0.00470 -0.00024 0.06685 0.01946 0.00095 0.00040 0.00053 0.00000 0.00718 0.00844 0.00809 0.00663 0.00572 0.00580 0.00315 H28A 0.70832 0.24901 1.00229 1.00000 0.10028 0.00000 0.00000 H28B 0.57268 0.24869 0.96674 1.00000 0.10028 0.00000 0.00000 H28C 0.59543 0.22594 1.04026 1.00000 0.10028 0.00000 0.00000 C16 0.45133 0.37237 0.47235 1.00000 0.08122 0.07618 0.03647 0.01040 0.01544 0.00023 0.06421 0.01888 0.00096 0.00039 0.00049 0.00000 0.00822 0.00796 0.00671 0.00558 0.00547 0.00610 0.00306 H16A 0.47695 0.39394 0.50968 1.00000 0.09632 0.00000 0.00000 H16B 0.44754 0.39094 0.43029 1.00000 0.09632 0.00000 0.00000 H16C 0.51120 0.34581 0.46926 1.00000 0.09632 0.00000 0.00000 C7 -0.01986 0.27670 0.96390 1.00000 0.05407 0.08646 0.07201 0.00249 0.02676 -0.02122 0.07007 0.01887 0.00092 0.00040 0.00054 0.00000 0.00690 0.00858 0.00819 0.00663 0.00574 0.00584 0.00328 H7A 0.02352 0.24693 0.97854 1.00000 0.10511 0.00000 0.00000 H7B -0.10261 0.26833 0.94540 1.00000 0.10511 0.00000 0.00000 H7C -0.02688 0.29861 1.00236 1.00000 0.10511 0.00000 0.00000 C32 0.64989 0.16786 0.81459 1.00000 0.10634 0.05912 0.07535 0.03817 0.02800 0.02810 0.07950 0.02377 0.00113 0.00040 0.00059 0.00000 0.00999 0.00800 0.00875 0.00666 0.00722 0.00728 0.00373 H32A 0.57335 0.18524 0.82335 1.00000 0.11925 0.00000 0.00000 H32B 0.65626 0.13862 0.84276 1.00000 0.11925 0.00000 0.00000 H32C 0.64914 0.15843 0.76713 1.00000 0.11925 0.00000 0.00000 C2 0.18472 0.52906 0.88347 1.00000 0.04267 0.05130 0.08173 -0.01537 -0.00347 0.01246 0.05878 0.01763 0.00087 0.00036 0.00057 0.00000 0.00614 0.00737 0.00845 0.00651 0.00541 0.00500 0.00292 H2 0.26378 0.52999 0.91151 1.00000 0.07054 0.00000 0.00000 C8 -0.01585 0.34775 0.88685 1.00000 0.03794 0.08341 0.11043 0.01210 0.00221 -0.01089 0.07731 0.01975 0.00090 0.00041 0.00063 0.00000 0.00633 0.00903 0.01026 0.00756 0.00607 0.00597 0.00356 H8A -0.02092 0.37046 0.92456 1.00000 0.11596 0.00000 0.00000 H8B -0.09938 0.33933 0.86960 1.00000 0.11596 0.00000 0.00000 H8C 0.02944 0.36308 0.85107 1.00000 0.11596 0.00000 0.00000 C40 0.88906 0.56264 0.64322 1.00000 0.04191 0.08763 0.10558 0.05543 0.01605 -0.01945 0.07797 0.02096 0.00089 0.00040 0.00060 0.00000 0.00652 0.00893 0.01005 0.00738 0.00606 0.00568 0.00385 H40A 0.85371 0.56958 0.59802 1.00000 0.11695 0.00000 0.00000 H40B 0.97809 0.55703 0.64116 1.00000 0.11695 0.00000 0.00000 H40C 0.87468 0.59043 0.67271 1.00000 0.11695 0.00000 0.00000 C1 0.15676 0.47577 0.86725 1.00000 0.05156 0.04293 0.03435 0.00043 0.00753 0.01203 0.04277 0.01603 0.00080 0.00031 0.00044 0.00000 0.00601 0.00650 0.00585 0.00465 0.00439 0.00463 0.00240 H1A 0.07979 0.47447 0.83843 1.00000 0.05132 0.00000 0.00000 H1B 0.14029 0.45886 0.90978 1.00000 0.05132 0.00000 0.00000 C12 0.10250 0.23292 0.67657 1.00000 0.13447 0.07792 0.36017 -0.00846 -0.15879 -0.01716 0.19645 0.02496 0.00171 0.00059 0.00124 0.00000 0.01489 0.01214 0.03129 0.01471 0.01838 0.01064 0.01164 H12A 0.12931 0.26658 0.68478 1.00000 0.29468 0.00000 0.00000 H12B 0.01742 0.22897 0.69021 1.00000 0.29468 0.00000 0.00000 H12C 0.10641 0.22544 0.62862 1.00000 0.29468 0.00000 0.00000 C39 0.89212 0.50314 0.73943 1.00000 0.06054 0.06664 0.08060 0.01560 -0.01153 0.00296 0.06975 0.01859 0.00094 0.00039 0.00055 0.00000 0.00718 0.00804 0.00885 0.00645 0.00616 0.00568 0.00328 H39A 0.88145 0.52958 0.77167 1.00000 0.10463 0.00000 0.00000 H39B 0.98039 0.49801 0.73345 1.00000 0.10463 0.00000 0.00000 H39C 0.85570 0.47316 0.75640 1.00000 0.10463 0.00000 0.00000 C11 0.14316 0.15196 0.68627 1.00000 0.06696 0.09424 0.32029 -0.11377 0.00518 -0.01706 0.16064 0.02337 0.00120 0.00052 0.00105 0.00000 0.00941 0.01160 0.02549 0.01407 0.01164 0.00779 0.00850 H11A 0.05697 0.14418 0.69453 1.00000 0.24095 0.00000 0.00000 H11B 0.19782 0.12910 0.71109 1.00000 0.24095 0.00000 0.00000 H11C 0.15626 0.14928 0.63809 1.00000 0.24095 0.00000 0.00000 C19 0.34517 0.50235 0.52085 1.00000 0.10483 0.35756 0.15567 0.14070 -0.01426 -0.13780 0.20670 0.03182 0.00121 0.00076 0.00081 0.00000 0.01349 0.03128 0.01779 0.01961 0.01154 0.01735 0.01238 H19A 0.35974 0.53275 0.49670 1.00000 0.31004 0.00000 0.00000 H19B 0.33451 0.47556 0.48857 1.00000 0.31004 0.00000 0.00000 H19C 0.41600 0.49549 0.55188 1.00000 0.31004 0.00000 0.00000 C24 0.67821 0.58188 0.96278 1.00000 0.21530 0.06471 0.07488 -0.02882 -0.06035 -0.02793 0.12051 0.01895 0.00153 0.00045 0.00064 0.00000 0.01640 0.00888 0.01008 0.00750 0.00984 0.00959 0.00569 H24A 0.69069 0.61470 0.94496 1.00000 0.18076 0.00000 0.00000 H24B 0.75837 0.56754 0.97641 1.00000 0.18076 0.00000 0.00000 H24C 0.62666 0.58374 1.00176 1.00000 0.18076 0.00000 0.00000 C18 0.24230 0.50682 0.55582 1.00000 0.42307 0.36508 0.08657 0.09064 0.07451 0.36646 0.28954 0.05735 0.00230 0.00094 0.00079 0.00000 0.03884 0.03433 0.01385 0.01726 0.01809 0.03399 0.02041 H18 0.19874 0.47791 0.53537 1.00000 0.34745 0.00000 0.00000 C23 0.56228 0.57480 0.85502 1.00000 0.15914 0.05926 0.09658 0.00038 -0.00931 -0.00298 0.10550 0.02379 0.00141 0.00045 0.00072 0.00000 0.01324 0.00884 0.01157 0.00821 0.00933 0.00863 0.00455 H23A 0.59014 0.56053 0.81330 1.00000 0.15825 0.00000 0.00000 H23B 0.58726 0.60909 0.85764 1.00000 0.15825 0.00000 0.00000 H23C 0.47210 0.57254 0.85559 1.00000 0.15825 0.00000 0.00000 C22 0.61411 0.55017 0.90852 1.00000 0.44458 0.03937 0.12508 0.00448 -0.18331 -0.06005 0.20947 0.02255 0.00239 0.00050 0.00089 0.00000 0.03441 0.00956 0.01473 0.00924 0.01932 0.01360 0.01289 H22 0.53481 0.55121 0.93211 1.00000 0.25137 0.00000 0.00000 C20 0.15038 0.54492 0.52689 1.00000 0.91472 0.70230 0.05074 0.09932 0.07980 0.74351 0.55408 0.07747 0.00332 0.00132 0.00082 0.00000 0.08735 0.07078 0.01355 0.02252 0.02380 0.07438 0.04683 H20A 0.17369 0.55444 0.48183 1.00000 0.83112 0.00000 0.00000 H20B 0.15179 0.57364 0.55615 1.00000 0.83112 0.00000 0.00000 H20C 0.06703 0.53099 0.52426 1.00000 0.83112 0.00000 0.00000 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 605 Maximum vector length = 511 Memory required = 8362 / 22995 wR2 = 0.2351 before cycle 17 for 8987 data and 0 / 605 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 1.3490 1.5000 -0.1510 0.0200 DFIX C18 C19 1.4368 1.5000 -0.0632 0.0200 DFIX C18 C17 2.4212 2.5000 -0.0788 0.0200 DANG C19 C20 Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.097 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.954; Restrained GooF = 0.958 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1096 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0904 for 3791 Fo > 4sig(Fo) and 0.2406 for all 8987 data wR2 = 0.2351, GooF = S = 0.954, Restrained GooF = 0.958 for all data Occupancy sum of asymmetric unit = 65.00 for non-hydrogen and 90.00 for hydrogen atoms Principal mean square atomic displacements U 0.0376 0.0333 0.0300 Si1 0.0355 0.0319 0.0246 Si4 0.0412 0.0340 0.0269 Si5 0.0460 0.0336 0.0293 Si8 0.0380 0.0353 0.0275 Si2 0.0413 0.0298 0.0265 Si6 0.0392 0.0319 0.0312 Si9 0.0403 0.0299 0.0277 Si3 0.0381 0.0316 0.0275 Si7 0.0468 0.0340 0.0308 Si10 0.0390 0.0301 0.0218 O9 0.0538 0.0350 0.0252 O8 0.0514 0.0381 0.0227 O6 0.0534 0.0477 0.0351 O10 0.0387 0.0366 0.0265 O7 0.0514 0.0309 0.0272 O2 0.0688 0.0375 0.0264 O15 0.0504 0.0346 0.0297 O4 0.0487 0.0410 0.0348 O11 0.0458 0.0359 0.0300 O12 0.0480 0.0438 0.0386 O14 0.0539 0.0472 0.0307 O5 0.0783 0.0350 0.0294 O13 0.0604 0.0412 0.0350 O1 0.0490 0.0333 0.0283 O3 0.0533 0.0415 0.0323 C9 0.0469 0.0331 0.0261 C13 0.0643 0.0325 0.0265 C37 0.0483 0.0374 0.0267 C5 0.0613 0.0458 0.0257 C25 0.0597 0.0439 0.0290 C14 0.0913 0.0547 0.0349 C15 0.1019 0.0611 0.0285 C36 0.0664 0.0510 0.0429 C26 0.1064 0.0836 0.0353 C35 0.1006 0.0374 0.0343 C17 0.0550 0.0459 0.0225 C33 0.0691 0.0451 0.0395 C34 0.0656 0.0477 0.0223 C21 0.0860 0.0462 0.0410 C30 0.1124 0.1075 0.0356 C27 0.1384 0.0800 0.0377 C3 0.0620 0.0488 0.0380 C6 0.0698 0.0501 0.0350 C38 0.1548 0.0981 0.0248 C31 0.1938 0.0512 0.0479 C10 0.0616 0.0433 0.0347 C29 0.1018 0.0736 0.0298 C4 0.0898 0.0633 0.0475 C28 0.0849 0.0774 0.0303 C16 0.0997 0.0807 0.0298 C7 0.1407 0.0700 0.0278 C32 0.0913 0.0518 0.0332 C2 0.1157 0.0809 0.0353 C8 0.1531 0.0643 0.0165 C40 0.0606 0.0369 0.0308 C1 0.4610 0.0874 0.0410 C12 may be split into 0.0910 0.2329 0.6903 and 0.1140 0.2329 0.6629 0.0953 0.0666 0.0473 C39 0.3677 0.0749 0.0392 C11 may be split into 0.1450 0.1482 0.6988 and 0.1413 0.1557 0.6737 0.4820 0.1149 0.0232 C19 may be split into 0.3365 0.5117 0.5271 and 0.3539 0.4930 0.5147 0.2472 0.0939 0.0204 C24 may be split into 0.6945 0.5813 0.9590 and 0.6619 0.5825 0.9665 0.7731 0.0749 0.0207 C18 may be split into 0.2705 0.5171 0.5585 and 0.2141 0.4965 0.5531 0.1637 0.0936 0.0592 C23 0.5551 0.0574 0.0159 C22 may be split into 0.6423 0.5488 0.9006 and 0.5859 0.5516 0.9164 1.5626 0.0756 0.0241 C20 may be split into 0.1929 0.5595 0.5283 and 0.1078 0.5304 0.5255 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.026 0.037 0.048 0.063 0.080 0.106 0.150 1.000 Number in group 950. 928. 827. 931. 856. 934. 882. 899. 874. 906. GooF 0.792 0.832 0.864 0.878 0.961 0.986 1.070 1.094 1.023 0.997 K 8.423 1.676 1.272 1.277 1.090 1.026 1.066 1.043 1.024 1.029 Resolution(A) 0.84 0.88 0.93 0.98 1.04 1.10 1.19 1.31 1.50 1.86 inf Number in group 900. 918. 908. 892. 892. 893. 905. 883. 894. 902. GooF 0.820 0.846 0.910 0.932 0.942 0.953 0.920 0.955 0.990 1.216 K 1.306 1.162 1.175 1.037 1.060 1.013 0.995 0.993 1.003 1.058 R1 0.581 0.541 0.466 0.368 0.284 0.215 0.134 0.106 0.101 0.084 Recommended weighting scheme: WGHT 0.1093 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)/su Fc/Fc(max) Resolution(A) 4 6 1 1296.61 566.71 4.86 0.060 2.30 -2 6 12 851.51 27.45 4.41 0.013 1.52 1 18 11 0.00 1533.27 4.39 0.099 1.16 10 15 2 1428.97 67.34 4.11 0.021 0.92 -2 2 4 2269.05 1322.58 4.04 0.092 3.62 1 4 1 2898.89 1735.62 4.03 0.105 5.53 -6 1 18 1831.08 514.94 3.76 0.057 0.96 3 2 2 2196.70 1434.12 3.75 0.096 3.25 0 20 7 1061.52 2165.56 3.68 0.118 1.24 -6 11 13 1336.04 507.15 3.68 0.057 1.08 1 6 3 1950.51 1147.19 3.66 0.086 3.53 7 3 3 465.58 3.29 3.64 0.005 1.47 1 8 13 1335.93 577.08 3.63 0.061 1.38 7 13 13 1253.68 18.38 3.61 0.011 0.95 0 8 0 36583.70 25216.46 3.61 0.402 3.43 -1 6 13 627.17 37.46 3.55 0.015 1.45 6 6 8 450.07 35.50 3.50 0.015 1.36 -7 20 2 -227.61 512.57 3.48 0.057 1.02 -3 29 9 2518.98 186.67 3.48 0.035 0.85 -1 8 6 515.63 72.29 3.47 0.022 2.35 -2 4 2 1425.65 269.17 3.46 0.042 3.96 -3 13 11 1069.37 312.42 3.46 0.045 1.30 3 11 0 2279.70 1485.43 3.45 0.098 2.05 -5 1 12 464.49 28.48 3.43 0.014 1.35 3 10 1 659.73 181.06 3.43 0.034 2.16 -1 4 3 18077.93 12903.32 3.43 0.288 4.42 4 6 4 1758.19 1127.48 3.42 0.085 2.08 -10 13 3 1432.30 282.49 3.41 0.043 0.96 -2 25 8 5776.23 3436.70 3.36 0.148 0.99 -8 11 4 120.92 595.24 3.31 0.062 1.17 9 1 7 1387.03 795.84 3.29 0.071 1.09 2 2 2 3173.86 4577.05 3.27 0.171 4.41 -2 1 3 2897.53 4254.76 3.25 0.165 4.25 2 2 3 8228.22 5988.56 3.23 0.196 3.93 8 24 5 3602.34 1352.89 3.23 0.093 0.85 9 2 8 1649.42 812.55 3.21 0.072 1.06 -2 6 13 788.29 291.74 3.21 0.043 1.42 -3 7 15 -118.89 958.82 3.20 0.078 1.20 1 4 4 6006.47 4385.87 3.17 0.168 3.73 -4 1 2 3651.78 5262.91 3.15 0.184 2.63 1 2 4 33531.90 24518.86 3.14 0.396 4.22 0 3 2 7324.59 10291.56 3.14 0.257 6.74 3 12 13 1455.56 2739.63 3.14 0.132 1.18 1 4 3 59410.51 43721.60 3.11 0.529 4.31 5 23 5 -507.57 960.16 3.11 0.078 1.01 -5 7 1 1183.03 505.30 3.11 0.057 1.89 0 10 2 2403.25 1650.95 3.11 0.103 2.65 -3 4 14 630.71 109.54 3.10 0.026 1.32 -7 13 10 2176.71 1310.03 3.10 0.092 1.08 -2 17 6 -72.04 391.07 3.07 0.050 1.41 Bond lengths and angles Si1 - Distance Angles O5 1.5998 (0.0061) O6 1.6116 (0.0058) 109.54 (0.31) O1 1.6193 (0.0061) 106.65 (0.32) 110.31 (0.29) C1 1.8545 (0.0083) 112.89 (0.36) 108.11 (0.36) 109.35 (0.36) Si1 - O5 O6 O1 Si4 - Distance Angles O9 1.6115 (0.0054) O4 1.6142 (0.0057) 109.86 (0.29) O3 1.6262 (0.0057) 108.54 (0.28) 108.50 (0.30) C13 1.8480 (0.0083) 109.55 (0.33) 110.25 (0.34) 110.12 (0.34) Si4 - O9 O4 O3 Si5 - Distance Angles O10 1.6097 (0.0061) O4 1.6154 (0.0058) 108.29 (0.30) O5 1.6167 (0.0061) 108.80 (0.32) 110.65 (0.31) C17 1.8235 (0.0089) 111.70 (0.41) 111.16 (0.38) 106.21 (0.38) Si5 - O10 O4 O5 Si8 - Distance Angles O8 1.6107 (0.0060) O12 1.6185 (0.0058) 109.30 (0.29) O13 1.6197 (0.0061) 108.63 (0.30) 107.71 (0.32) C29 1.8367 (0.0089) 111.78 (0.37) 108.00 (0.35) 111.33 (0.38) Si8 - O8 O12 O13 Si2 - Distance Angles O1 1.6043 (0.0061) O7 1.6155 (0.0055) 108.50 (0.29) O2 1.6202 (0.0056) 108.36 (0.31) 109.12 (0.29) C5 1.8448 (0.0083) 111.99 (0.36) 109.63 (0.35) 109.20 (0.35) Si2 - O1 O7 O2 Si6 - Distance Angles O15 1.5979 (0.0059) O11 1.6019 (0.0060) 108.67 (0.32) O6 1.6158 (0.0058) 108.98 (0.32) 109.59 (0.29) C21 1.8570 (0.0087) 109.86 (0.37) 109.11 (0.37) 110.60 (0.36) Si6 - O15 O11 O6 Si9 - Distance Angles O13 1.6066 (0.0060) O9 1.6224 (0.0055) 109.10 (0.29) O14 1.6371 (0.0063) 109.48 (0.33) 108.24 (0.29) C33 1.8479 (0.0088) 111.69 (0.37) 109.46 (0.35) 108.80 (0.34) Si9 - O13 O9 O14 Si3 - Distance Angles O3 1.6017 (0.0057) O2 1.6121 (0.0057) 108.15 (0.30) O8 1.6253 (0.0059) 109.46 (0.28) 109.73 (0.30) C9 1.8369 (0.0087) 110.82 (0.37) 110.96 (0.36) 107.72 (0.35) Si3 - O3 O2 O8 Si7 - Distance Angles O7 1.6052 (0.0055) O12 1.6058 (0.0058) 108.54 (0.30) O11 1.6117 (0.0061) 110.16 (0.29) 107.80 (0.31) C25 1.8440 (0.0086) 109.39 (0.36) 111.80 (0.37) 109.13 (0.37) Si7 - O7 O12 O11 Si10 - Distance Angles O14 1.5982 (0.0062) O10 1.6097 (0.0061) 109.80 (0.32) O15 1.6204 (0.0059) 108.30 (0.32) 109.27 (0.31) C37 1.8583 (0.0083) 109.21 (0.38) 108.46 (0.36) 111.79 (0.36) Si10 - O14 O10 O15 O9 - Distance Angles Si4 1.6115 (0.0054) Si9 1.6224 (0.0055) 151.28 (0.36) O9 - Si4 O8 - Distance Angles Si8 1.6107 (0.0059) Si3 1.6253 (0.0059) 154.20 (0.37) O8 - Si8 O6 - Distance Angles Si1 1.6116 (0.0057) Si6 1.6158 (0.0057) 150.59 (0.37) O6 - Si1 O10 - Distance Angles Si5 1.6097 (0.0060) Si10 1.6097 (0.0060) 150.91 (0.39) O10 - Si5 O7 - Distance Angles Si7 1.6052 (0.0055) Si2 1.6155 (0.0055) 153.10 (0.38) O7 - Si7 O2 - Distance Angles Si3 1.6121 (0.0057) Si2 1.6202 (0.0056) 146.35 (0.36) O2 - Si3 O15 - Distance Angles Si6 1.5979 (0.0059) Si10 1.6204 (0.0059) 155.64 (0.41) O15 - Si6 O4 - Distance Angles Si4 1.6142 (0.0057) Si5 1.6154 (0.0058) 153.63 (0.37) O4 - Si4 O11 - Distance Angles Si6 1.6019 (0.0060) Si7 1.6117 (0.0061) 156.02 (0.39) O11 - Si6 O12 - Distance Angles Si7 1.6058 (0.0058) Si8 1.6185 (0.0058) 144.26 (0.36) O12 - Si7 O14 - Distance Angles Si10 1.5982 (0.0062) Si9 1.6371 (0.0063) 150.13 (0.39) O14 - Si10 O5 - Distance Angles Si1 1.5998 (0.0061) Si5 1.6167 (0.0061) 155.02 (0.40) O5 - Si1 O13 - Distance Angles Si9 1.6066 (0.0060) Si8 1.6197 (0.0061) 148.06 (0.41) O13 - Si9 O1 - Distance Angles Si2 1.6043 (0.0061) Si1 1.6193 (0.0061) 156.61 (0.39) O1 - Si2 O3 - Distance Angles Si3 1.6017 (0.0057) Si4 1.6262 (0.0057) 150.22 (0.36) O3 - Si3 C9 - Distance Angles C10 1.4685 (0.0137) Si3 1.8369 (0.0087) 119.94 (0.68) H9A 0.9900 107.34 107.34 H9B 0.9900 107.34 107.34 106.91 C9 - C10 Si3 H9A C13 - Distance Angles C14 1.5040 (0.0112) Si4 1.8480 (0.0083) 117.52 (0.59) H13A 0.9900 107.92 107.92 H13B 0.9900 107.92 107.92 107.21 C13 - C14 Si4 H13A C37 - Distance Angles C38 1.5043 (0.0116) Si10 1.8583 (0.0082) 116.06 (0.63) H37A 0.9900 108.27 108.27 H37B 0.9900 108.27 108.27 107.39 C37 - C38 Si10 H37A C5 - Distance Angles C6 1.4951 (0.0117) Si2 1.8448 (0.0083) 119.96 (0.63) H5A 0.9900 107.33 107.33 H5B 0.9900 107.33 107.33 106.91 C5 - C6 Si2 H5A C25 - Distance Angles C26 1.5322 (0.0126) Si7 1.8440 (0.0086) 116.36 (0.65) H25A 0.9900 108.20 108.20 H25B 0.9900 108.20 108.20 107.35 C25 - C26 Si7 H25A C14 - Distance Angles C16 1.4943 (0.0123) C13 1.5040 (0.0112) 113.90 (0.75) C15 1.5438 (0.0121) 108.81 (0.79) 111.00 (0.73) H14 1.0000 107.63 107.63 107.63 C14 - C16 C13 C15 C15 - Distance Angles C14 1.5438 (0.0121) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C36 - Distance Angles C34 1.5244 (0.0123) H36A 0.9800 109.47 H36B 0.9800 109.47 109.47 H36C 0.9800 109.47 109.47 109.47 C36 - C34 H36A H36B C26 - Distance Angles C28 1.4969 (0.0134) C27 1.5169 (0.0132) 109.96 (0.87) C25 1.5322 (0.0126) 112.65 (0.84) 111.76 (0.84) H26 1.0000 107.40 107.40 107.40 C26 - C28 C27 C25 C35 - Distance Angles C34 1.5161 (0.0134) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35 - C34 H35A H35B C17 - Distance Angles C18 1.4368 (0.0128) Si5 1.8235 (0.0089) 120.69 (0.73) H17A 0.9900 107.15 107.15 H17B 0.9900 107.15 107.15 106.82 C17 - C18 Si5 H17A C33 - Distance Angles C34 1.5548 (0.0116) Si9 1.8479 (0.0088) 115.81 (0.60) H33A 0.9900 108.33 108.33 H33B 0.9900 108.33 108.33 107.42 C33 - C34 Si9 H33A C34 - Distance Angles C35 1.5161 (0.0134) C36 1.5244 (0.0123) 111.90 (0.85) C33 1.5548 (0.0116) 111.19 (0.79) 109.63 (0.77) H34 1.0000 107.99 107.99 107.99 C34 - C35 C36 C33 C21 - Distance Angles C22 1.4148 (0.0159) Si6 1.8570 (0.0086) 119.66 (0.78) H21A 0.9900 107.41 107.41 H21B 0.9900 107.41 107.41 106.94 C21 - C22 Si6 H21A C30 - Distance Angles C29 1.5048 (0.0126) C32 1.5085 (0.0145) 112.20 (0.81) C31 1.5180 (0.0129) 112.18 (0.94) 109.39 (0.89) H30 1.0000 107.62 107.62 107.62 C30 - C29 C32 C31 C27 - Distance Angles C26 1.5169 (0.0132) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C26 H27A H27B C3 - Distance Angles C2 1.4942 (0.0134) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C2 H3A H3B C6 - Distance Angles C5 1.4951 (0.0117) C7 1.5079 (0.0127) 112.61 (0.82) C8 1.5243 (0.0133) 110.89 (0.78) 109.99 (0.84) H6 1.0000 107.72 107.72 107.72 C6 - C5 C7 C8 C38 - Distance Angles C37 1.5043 (0.0115) C40 1.5431 (0.0125) 112.16 (0.78) C39 1.5457 (0.0127) 111.99 (0.78) 109.17 (0.82) H38 1.0000 107.78 107.78 107.78 C38 - C37 C40 C39 C31 - Distance Angles C30 1.5180 (0.0129) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C30 H31A H31B C10 - Distance Angles C12 1.2564 (0.0170) C9 1.4685 (0.0137) 122.06 (1.47) C11 1.5430 (0.0161) 108.07 (1.38) 112.18 (0.96) H10 1.0000 104.22 104.22 104.22 C10 - C12 C9 C11 C29 - Distance Angles C30 1.5048 (0.0126) Si8 1.8367 (0.0089) 118.30 (0.65) H29A 0.9900 107.74 107.74 H29B 0.9900 107.74 107.74 107.11 C29 - C30 Si8 H29A C4 - Distance Angles C2 1.5270 (0.0140) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C2 H4A H4B C28 - Distance Angles C26 1.4969 (0.0134) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C26 H28A H28B C16 - Distance Angles C14 1.4943 (0.0123) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C14 H16A H16B C7 - Distance Angles C6 1.5079 (0.0127) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C32 - Distance Angles C30 1.5085 (0.0144) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C30 H32A H32B C2 - Distance Angles C3 1.4942 (0.0134) C1 1.5252 (0.0125) 111.69 (0.86) C4 1.5270 (0.0140) 110.67 (0.91) 112.06 (0.83) H2 1.0000 107.38 107.38 107.38 C2 - C3 C1 C4 C8 - Distance Angles C6 1.5243 (0.0133) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C6 H8A H8B C40 - Distance Angles C38 1.5431 (0.0125) H40A 0.9800 109.47 H40B 0.9800 109.47 109.47 H40C 0.9800 109.47 109.47 109.47 C40 - C38 H40A H40B C1 - Distance Angles C2 1.5252 (0.0125) Si1 1.8545 (0.0083) 116.80 (0.63) H1A 0.9900 108.09 108.09 H1B 0.9900 108.09 108.09 107.29 C1 - C2 Si1 H1A C12 - Distance Angles C10 1.2564 (0.0170) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C39 - Distance Angles C38 1.5457 (0.0127) H39A 0.9800 109.47 H39B 0.9800 109.47 109.47 H39C 0.9800 109.47 109.47 109.47 C39 - C38 H39A H39B C11 - Distance Angles C10 1.5430 (0.0161) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C19 - Distance Angles C18 1.3490 (0.0149) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C18 H19A H19B C24 - Distance Angles C22 1.5282 (0.0153) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B C18 - Distance Angles C19 1.3490 (0.0148) C17 1.4368 (0.0128) 130.34 (1.40) C20 1.5370 (0.0134) 113.90 (1.42) 112.55 (1.02) H18 1.0000 95.91 95.91 95.91 C18 - C19 C17 C20 C23 - Distance Angles C22 1.3602 (0.0165) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C22 - Distance Angles C23 1.3602 (0.0165) C21 1.4148 (0.0158) 131.27 (1.14) C24 1.5282 (0.0153) 115.28 (1.20) 113.29 (1.18) H22 1.0000 91.29 91.29 91.29 C22 - C23 C21 C24 C20 - Distance Angles C18 1.5370 (0.0134) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C18 H20A H20B FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 24 -2 2.381 1 2 R1 = 0.2402 for 8987 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.87 at 0.2338 0.5622 0.5348 [ 1.03 A from C20 ] Deepest hole -0.61 at 0.1438 0.5496 0.5311 [ 0.17 A from C20 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 8604 / 66588 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2338 0.5622 0.5348 1.00000 0.05 0.87 1.03 C20 1.05 H20B 1.23 H20A 1.58 C18 Q2 1 0.3062 0.5281 0.5620 1.00000 0.05 0.65 0.91 C18 1.18 C19 1.46 H19A 1.51 H19C Q3 1 0.0864 0.5195 0.5196 1.00000 0.05 0.61 0.39 H20C 0.99 C20 1.57 H20A 1.69 H18 Q4 1 0.7171 0.3320 0.6566 1.00000 0.05 0.55 1.04 SI9 1.25 C33 1.39 H33A 1.72 O13 Q5 1 0.0716 0.2192 0.7405 1.00000 0.05 0.50 0.88 H10 1.17 H12B 1.34 C10 1.39 C12 Q6 1 0.7549 0.2956 1.0876 1.00000 0.05 0.43 0.54 H27C 1.29 C27 1.92 H27A 1.94 C26 Q7 1 0.7348 0.5212 0.9189 1.00000 0.05 0.43 0.83 H21B 1.31 C21 1.54 C22 1.72 H24B Q8 1 0.3013 0.2766 0.7007 1.00000 0.05 0.43 1.10 O3 1.10 SI3 1.78 C9 1.90 H12A Q9 1 0.6418 0.2507 0.7848 1.00000 0.05 0.41 1.08 SI8 1.35 C29 1.56 O8 1.76 H29A Q10 1 0.2208 0.4905 0.5426 1.00000 0.05 0.39 0.44 H18 0.57 C18 1.47 C19 1.63 C17 Shortest distances between peaks (including symmetry equivalents) 1 2 1.32 2 10 1.43 3 10 1.70 1 10 1.98 1 3 1.99 3 3 2.26 2 3 2.50 Time profile in seconds ----------------------- 0.02: 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. 1.19: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 18.56: Structure factors and derivatives 67.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 4.75: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.05: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:24:00 Total CPU time: 92.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++