+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:39:54 on 23-Sep-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 10.6038 11.3298 19.4441 86.132 81.457 68.060 ZERR 2.00 0.0012 0.0014 0.0033 0.005 0.005 0.012 LATT 1 SFAC C H O SI UNIT 64 96 16 16 V = 2142.59 F(000) = 832.0 Mu = 0.29 mm-1 Cell Wt = 1570.85 Rho = 1.217 MERG 2 OMIT 8 6 6 DFIX 1.45 0.05 SI5 H5S SI6 H6S SI7 H7S SI8 H8S DANG 2.52 0.05 H5S O5 H6S O6 H7S O7 H8S O8 DANG 2.75 0.05 H5S C25 H5S C26 H6S C27 H6S C28 DANG 2.75 0.05 H7S C29 H7S C30 H8S C31 H8S C32 FMAP 2 PLAN 10 ACTA SIZE 0.18 0.24 0.38 BOND $H WGHT 0.07880 L.S. 9 TEMP -153.00 FVAR 0.19347 SI1 4 -0.178022 0.087311 0.751608 11.00000 0.03411 0.03162 = 0.03671 -0.00406 -0.00086 -0.01068 SI2 4 0.135945 0.004026 0.682408 11.00000 0.03354 0.02985 = 0.03568 -0.00139 -0.00375 -0.01077 SI3 4 0.170975 -0.281927 0.698021 11.00000 0.03155 0.02935 = 0.03499 -0.00323 -0.00384 -0.00946 SI4 4 -0.133100 -0.199942 0.781993 11.00000 0.03483 0.03384 = 0.03459 -0.00257 0.00041 -0.01407 SI5 4 -0.275155 0.197581 0.897831 11.00000 0.10435 0.06088 = 0.04512 -0.01586 0.00767 -0.03233 SI6 4 0.198225 0.134913 0.799324 11.00000 0.06751 0.04733 = 0.05676 -0.00349 -0.01905 -0.02348 SI7 4 0.323239 -0.378942 0.826104 11.00000 0.06723 0.05031 = 0.04054 0.00535 -0.01801 -0.02654 SI8 4 -0.179140 -0.312171 0.929732 11.00000 0.06585 0.07009 = 0.04396 0.01294 -0.00670 -0.03602 O1 3 -0.027434 0.058922 0.710291 11.00000 0.02026 0.03404 = 0.04530 0.00447 -0.00399 -0.00269 O2 3 0.189558 -0.148774 0.676917 11.00000 0.03723 0.01650 = 0.04128 -0.00176 -0.00163 -0.00842 O3 3 0.019939 -0.255362 0.739793 11.00000 0.02842 0.02478 = 0.04969 -0.00928 0.00121 -0.00740 O4 3 -0.191050 -0.046287 0.778683 11.00000 0.03924 0.01906 = 0.04680 -0.01008 0.00028 -0.00817 O5 3 -0.200900 0.175206 0.817267 11.00000 0.03510 0.03334 = 0.04767 -0.00452 -0.00580 -0.01014 O6 3 0.219848 0.037154 0.735905 11.00000 0.04293 0.02744 = 0.03678 -0.00419 -0.00841 -0.00701 O7 3 0.283933 -0.364478 0.747438 11.00000 0.02753 0.03546 = 0.03925 -0.00276 -0.00995 -0.00322 O8 3 -0.122888 -0.243473 0.862008 11.00000 0.04702 0.04804 = 0.03822 0.00003 -0.00545 -0.01993 C1 1 -0.308680 0.168359 0.694264 11.00000 0.02276 0.02229 = 0.03874 -0.00567 0.00175 -0.00420 C2 1 -0.413160 0.283207 0.710940 11.00000 0.03296 0.03662 = 0.04964 -0.00419 -0.00366 -0.00908 AFIX 43 H2 2 -0.415448 0.324477 0.752303 11.00000 -1.20000 AFIX 0 C3 1 -0.515234 0.340167 0.668794 11.00000 0.03012 0.02467 = 0.07611 -0.00800 -0.00194 0.00532 AFIX 43 H3 2 -0.586293 0.419401 0.681327 11.00000 -1.20000 AFIX 0 C4 1 -0.512754 0.280625 0.608294 11.00000 0.04118 0.05062 = 0.06895 0.00261 -0.01506 -0.01411 AFIX 43 H4 2 -0.582804 0.318832 0.579526 11.00000 -1.20000 AFIX 0 C5 1 -0.409952 0.167265 0.589943 11.00000 0.04071 0.04316 = 0.05292 -0.00752 -0.01603 -0.00914 AFIX 43 H5 2 -0.408165 0.126696 0.548420 11.00000 -1.20000 AFIX 0 C6 1 -0.308793 0.112010 0.631982 11.00000 0.02947 0.03276 = 0.04768 -0.00626 0.00647 -0.00949 AFIX 43 H6 2 -0.237111 0.033648 0.618514 11.00000 -1.20000 AFIX 0 C7 1 0.161714 0.076208 0.595864 11.00000 0.03248 0.02094 = 0.03972 -0.00470 -0.00842 -0.00506 C8 1 0.057614 0.121624 0.553934 11.00000 0.03364 0.05296 = 0.04426 0.00267 -0.00532 -0.01382 AFIX 43 H8 2 -0.028805 0.115543 0.570177 11.00000 -1.20000 AFIX 0 C9 1 0.076873 0.175389 0.489202 11.00000 0.04515 0.04579 = 0.04824 0.00114 -0.01838 -0.00873 AFIX 43 H9 2 0.003614 0.206360 0.461884 11.00000 -1.20000 AFIX 0 C10 1 0.201216 0.184415 0.464020 11.00000 0.05745 0.03776 = 0.02998 -0.00925 -0.00112 -0.01864 AFIX 43 H10 2 0.214090 0.221070 0.419397 11.00000 -1.20000 AFIX 0 C11 1 0.306447 0.140179 0.503729 11.00000 0.04152 0.04353 = 0.04063 -0.00328 0.00284 -0.02094 AFIX 43 H11 2 0.393045 0.145036 0.486478 11.00000 -1.20000 AFIX 0 C12 1 0.286012 0.088020 0.569530 11.00000 0.03598 0.03666 = 0.04084 -0.00747 -0.00609 -0.00960 AFIX 43 H12 2 0.358851 0.059779 0.597140 11.00000 -1.20000 AFIX 0 C13 1 0.191460 -0.369033 0.618605 11.00000 0.02628 0.02776 = 0.03375 0.00207 -0.00915 -0.00161 C14 1 0.124756 -0.453470 0.615881 11.00000 0.04056 0.03458 = 0.03124 -0.00358 0.00116 -0.01156 AFIX 43 H14 2 0.071297 -0.467552 0.657028 11.00000 -1.20000 AFIX 0 C15 1 0.132044 -0.517598 0.556870 11.00000 0.04411 0.03684 = 0.04176 -0.00649 -0.00441 -0.01242 AFIX 43 H15 2 0.081541 -0.571426 0.556927 11.00000 -1.20000 AFIX 0 C16 1 0.214885 -0.502027 0.497095 11.00000 0.04739 0.03857 = 0.03762 -0.01217 -0.00650 -0.00294 AFIX 43 H16 2 0.224896 -0.548368 0.456400 11.00000 -1.20000 AFIX 0 C17 1 0.282705 -0.418474 0.497303 11.00000 0.05438 0.04610 = 0.04319 -0.00270 0.00677 -0.02071 AFIX 43 H17 2 0.335748 -0.403717 0.456172 11.00000 -1.20000 AFIX 0 C18 1 0.272226 -0.357528 0.557553 11.00000 0.03965 0.05637 = 0.03424 -0.00195 -0.00730 -0.02655 AFIX 43 H18 2 0.323324 -0.304228 0.557497 11.00000 -1.20000 AFIX 0 C19 1 -0.243511 -0.261378 0.743180 11.00000 0.02397 0.02774 = 0.03418 -0.00225 -0.00099 -0.00082 C20 1 -0.206265 -0.393227 0.736448 11.00000 0.02953 0.04310 = 0.04809 -0.00680 0.00529 -0.00341 AFIX 43 H20 2 -0.125962 -0.450106 0.753943 11.00000 -1.20000 AFIX 0 C21 1 -0.285577 -0.441603 0.704451 11.00000 0.05427 0.04261 = 0.06695 -0.01031 -0.00341 -0.02647 AFIX 43 H21 2 -0.258425 -0.530894 0.699572 11.00000 -1.20000 AFIX 0 C22 1 -0.403928 -0.359617 0.679767 11.00000 0.04235 0.08402 = 0.05047 -0.01551 0.00085 -0.03426 AFIX 43 H22 2 -0.457012 -0.392855 0.657331 11.00000 -1.20000 AFIX 0 C23 1 -0.444895 -0.231074 0.687481 11.00000 0.02786 0.05661 = 0.06200 0.00072 -0.00289 -0.01073 AFIX 43 H23 2 -0.527359 -0.175318 0.671449 11.00000 -1.20000 AFIX 0 C24 1 -0.365207 -0.181962 0.718984 11.00000 0.04091 0.05184 = 0.04638 -0.00644 0.00336 -0.02516 AFIX 43 H24 2 -0.394409 -0.092522 0.724080 11.00000 -1.20000 AFIX 0 C25 1 -0.185391 0.067424 0.952541 11.00000 0.26007 0.05396 = 0.05280 0.00452 -0.00742 -0.00404 AFIX 137 H25A 2 -0.163339 -0.013326 0.929301 11.00000 -1.50000 H25B 2 -0.243629 0.069016 0.996875 11.00000 -1.50000 H25C 2 -0.100429 0.075855 0.961177 11.00000 -1.50000 AFIX 0 C26 1 -0.292944 0.351433 0.925127 11.00000 0.13905 0.05143 = 0.06058 -0.01198 -0.02677 -0.01969 AFIX 137 H26A 2 -0.202008 0.356352 0.922428 11.00000 -1.50000 H26B 2 -0.338586 0.365245 0.973177 11.00000 -1.50000 H26C 2 -0.347975 0.416919 0.894718 11.00000 -1.50000 AFIX 0 C27 1 0.106724 0.300211 0.772148 11.00000 0.09298 0.01631 = 0.10837 0.00282 -0.05427 -0.00126 AFIX 137 H27A 2 0.164127 0.324715 0.734071 11.00000 -1.50000 H27B 2 0.086665 0.356826 0.811577 11.00000 -1.50000 H27C 2 0.020669 0.307086 0.756329 11.00000 -1.50000 AFIX 0 C28 1 0.364953 0.109543 0.824084 11.00000 0.06353 0.05208 = 0.09663 -0.02206 -0.01506 -0.02561 AFIX 137 H28A 2 0.404957 0.022673 0.842351 11.00000 -1.50000 H28B 2 0.354457 0.170473 0.859973 11.00000 -1.50000 H28C 2 0.425464 0.121786 0.783296 11.00000 -1.50000 AFIX 0 C29 1 0.252960 -0.223708 0.867766 11.00000 0.19904 0.06399 = 0.05443 -0.01201 -0.03048 -0.04098 AFIX 137 H29A 2 0.284367 -0.163380 0.838654 11.00000 -1.50000 H29B 2 0.284290 -0.231750 0.913410 11.00000 -1.50000 H29C 2 0.152527 -0.192731 0.873581 11.00000 -1.50000 AFIX 0 C30 1 0.260504 -0.493827 0.875340 11.00000 0.09266 0.06341 = 0.05535 0.00588 -0.00149 -0.03977 AFIX 137 H30A 2 0.161502 -0.467048 0.874567 11.00000 -1.50000 H30B 2 0.278928 -0.498104 0.923549 11.00000 -1.50000 H30C 2 0.307455 -0.577905 0.854296 11.00000 -1.50000 AFIX 0 C31 1 -0.097394 -0.294117 1.003480 11.00000 0.10860 0.07260 = 0.03205 0.00325 -0.00843 -0.03795 AFIX 137 H31A 2 0.002556 -0.331326 0.991723 11.00000 -1.50000 H31B 2 -0.125730 -0.337878 1.044548 11.00000 -1.50000 H31C 2 -0.125502 -0.203538 1.013416 11.00000 -1.50000 AFIX 0 C32 1 -0.367186 -0.244143 0.944293 11.00000 0.06637 0.23064 = 0.09031 0.04499 0.00572 -0.04883 AFIX 137 H32A 2 -0.398203 -0.152196 0.951073 11.00000 -1.50000 H32B 2 -0.400499 -0.283670 0.985763 11.00000 -1.50000 H32C 2 -0.403338 -0.260213 0.903824 11.00000 -1.50000 AFIX 0 H5S 2 -0.419538 0.192118 0.898251 11.00000 -1.20000 H6S 2 0.111637 0.096749 0.859677 11.00000 -1.20000 H7S 2 0.473435 -0.424837 0.826955 11.00000 -1.20000 H8S 2 -0.120861 -0.452175 0.911988 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 O 0.660 SI 1.170 Si1 - O1 O5 O4 C1 Si2 - O6 O2 O1 C7 Si3 - O2 O3 O7 C13 Si4 - O8 O4 O3 C19 Si5 - O5 C26 C25 Si6 - O6 C28 C27 Si7 - O7 C29 C30 Si8 - O8 C32 C31 O1 - Si1 Si2 O2 - Si3 Si2 O3 - Si3 Si4 O4 - Si4 Si1 O5 - Si1 Si5 O6 - Si2 Si6 O7 - Si3 Si7 O8 - Si4 Si8 C1 - C2 C6 Si1 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 Si2 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C7 C11 C13 - C18 C14 Si3 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C18 C16 C18 - C17 C13 C19 - C24 C20 Si4 C20 - C21 C19 C21 - C22 C20 C22 - C23 C21 C23 - C22 C24 C24 - C23 C19 C25 - Si5 C26 - Si5 C27 - Si6 C28 - Si6 C29 - Si7 C30 - Si7 C31 - Si8 C32 - Si8 12781 Reflections read, of which 1 rejected -13 =< h =< 13, -14 =< k =< 14, -25 =< l =< 25, Max. 2-theta = 55.17 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 -3 1 32.17 0.89 3 10.06 -3 -2 1 89.90 1.51 5 14.28 -4 -3 2 75.38 0.90 4 15.72 3 4 2 57.51 1.75 2 27.76 -5 -8 3 25.76 0.88 3 9.70 -5 -8 4 10.49 0.88 3 5.02 8 5 4 14.69 0.92 3 6.65 -6 -7 6 50.39 1.88 2 32.53 8 Inconsistent equivalents 5962 Unique reflections, of which 0 suppressed R(int) = 0.0864 R(sigma) = 0.1774 Friedel opposites merged Maximum memory for data reduction = 4527 / 67003 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 = 5841 / 589698 wR2 = 0.1901 before cycle 1 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19352 0.00049 0.093 OSF Mean shift/esd = 0.012 Maximum = 0.093 for OSF Max. shift = 0.002 A for H26C Max. dU = 0.000 for C27 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 2 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19353 0.00049 0.034 OSF Mean shift/esd = 0.005 Maximum = -0.039 for tors H26A Max. shift = 0.002 A for H26C Max. dU = 0.000 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 3 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.006 OSF Mean shift/esd = 0.001 Maximum = -0.030 for tors H26A Max. shift = 0.002 A for H26C Max. dU = 0.000 for C32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 4 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.022 for tors H26A Max. shift = 0.001 A for H26C Max. dU = 0.000 for C32 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 5 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.017 for tors H26A Max. shift = 0.001 A for H26C Max. dU = 0.000 for C29 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 6 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.013 for tors H26A Max. shift = 0.001 A for H26C Max. dU = 0.000 for C29 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 7 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.009 for tors H26A Max. shift = 0.000 A for H26C Max. dU = 0.000 for C29 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 8 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.007 for tors H26A Max. shift = 0.000 A for H26C Max. dU = 0.000 for C32 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5841 / 589698 wR2 = 0.1901 before cycle 9 for 5962 data and 453 / 453 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19354 0.00049 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.005 for tors H26A Max. shift = 0.000 A for H26C Max. dU = 0.000 for C32 Largest correlation matrix elements -0.693 U12 C21 / U22 C21 -0.659 U12 Si8 / U22 Si8 -0.637 U12 C7 / U22 C7 -0.680 U12 Si6 / U22 Si6 -0.658 U12 C18 / U22 C18 -0.636 U12 C6 / U11 C6 -0.678 U12 Si4 / U22 Si4 -0.657 U12 C22 / U22 C22 -0.636 U12 C24 / U11 C24 -0.674 U12 C22 / U11 C22 -0.651 U12 C2 / U22 C2 -0.636 U12 C8 / U11 C8 -0.670 U12 C11 / U11 C11 -0.648 U12 C1 / U22 C1 -0.635 U12 C2 / U11 C2 -0.668 U12 C24 / U22 C24 -0.645 y C2 / x C2 -0.635 U12 C6 / U22 C6 -0.666 U12 Si2 / U22 Si2 -0.643 U12 C18 / U11 C18 -0.634 U12 C21 / U11 C21 -0.660 U12 Si7 / U22 Si7 -0.643 U12 Si8 / U11 Si8 -0.634 U12 C10 / U22 C10 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.4154 0.3245 0.7523 43 0.950 0.000 C2 C1 C3 H3 -0.5863 0.4194 0.6813 43 0.950 0.000 C3 C4 C2 H4 -0.5828 0.3189 0.5795 43 0.950 0.000 C4 C5 C3 H5 -0.4081 0.1267 0.5484 43 0.950 0.000 C5 C4 C6 H6 -0.2371 0.0337 0.6185 43 0.950 0.000 C6 C5 C1 H8 -0.0288 0.1155 0.5702 43 0.950 0.000 C8 C9 C7 H9 0.0036 0.2064 0.4619 43 0.950 0.000 C9 C10 C8 H10 0.2141 0.2211 0.4194 43 0.950 0.000 C10 C11 C9 H11 0.3930 0.1450 0.4865 43 0.950 0.000 C11 C10 C12 H12 0.3589 0.0597 0.5971 43 0.950 0.000 C12 C7 C11 H14 0.0713 -0.4676 0.6570 43 0.950 0.000 C14 C15 C13 H15 0.0816 -0.5714 0.5569 43 0.950 0.000 C15 C14 C16 H16 0.2248 -0.5483 0.4564 43 0.950 0.000 C16 C17 C15 H17 0.3358 -0.4037 0.4562 43 0.950 0.000 C17 C18 C16 H18 0.3233 -0.3042 0.5575 43 0.950 0.000 C18 C17 C13 H20 -0.1260 -0.4501 0.7539 43 0.950 0.000 C20 C21 C19 H21 -0.2584 -0.5309 0.6996 43 0.950 0.000 C21 C22 C20 H22 -0.4570 -0.3929 0.6573 43 0.950 0.000 C22 C23 C21 H23 -0.5273 -0.1753 0.6714 43 0.950 0.000 C23 C22 C24 H24 -0.3944 -0.0925 0.7241 43 0.950 0.000 C24 C23 C19 H25A -0.1633 -0.0133 0.9293 137 0.980 0.000 C25 Si5 H25A H25B -0.2437 0.0689 0.9969 137 0.980 0.000 C25 Si5 H25A H25C -0.1005 0.0759 0.9612 137 0.980 0.000 C25 Si5 H25A H26A -0.2019 0.3561 0.9229 137 0.980 0.000 C26 Si5 H26A H26B -0.3394 0.3656 0.9730 137 0.980 0.000 C26 Si5 H26A H26C -0.3472 0.4169 0.8944 137 0.980 0.000 C26 Si5 H26A H27A 0.1642 0.3248 0.7341 137 0.980 0.000 C27 Si6 H27A H27B 0.0866 0.3568 0.8116 137 0.980 0.000 C27 Si6 H27A H27C 0.0207 0.3071 0.7563 137 0.980 0.000 C27 Si6 H27A H28A 0.4050 0.0226 0.8423 137 0.980 0.000 C28 Si6 H28A H28B 0.3544 0.1703 0.8600 137 0.980 0.000 C28 Si6 H28A H28C 0.4254 0.1219 0.7833 137 0.980 0.000 C28 Si6 H28A H29A 0.2841 -0.1633 0.8386 137 0.980 0.000 C29 Si7 H29A H29B 0.2845 -0.2317 0.9133 137 0.980 0.000 C29 Si7 H29A H29C 0.1525 -0.1929 0.8737 137 0.980 0.000 C29 Si7 H29A H30A 0.1615 -0.4671 0.8745 137 0.980 0.000 C30 Si7 H30A H30B 0.2789 -0.4980 0.9236 137 0.980 0.000 C30 Si7 H30A H30C 0.3075 -0.5779 0.8543 137 0.980 0.000 C30 Si7 H30A H31A 0.0025 -0.3314 0.9917 137 0.980 0.000 C31 Si8 H31A H31B -0.1258 -0.3378 1.0446 137 0.980 0.000 C31 Si8 H31A H31C -0.1255 -0.2035 1.0134 137 0.980 0.000 C31 Si8 H31A H32A -0.3982 -0.1522 0.9512 137 0.980 0.000 C32 Si8 H32A H32B -0.4005 -0.2837 0.9857 137 0.980 0.000 C32 Si8 H32A H32C -0.4034 -0.2600 0.9038 137 0.980 0.000 C32 Si8 H32A s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 -0.17802 0.08731 0.75161 1.00000 0.03417 0.03165 0.03671 -0.00406 -0.00087 -0.01067 0.03485 0.00263 0.00020 0.00020 0.00009 0.00000 0.00147 0.00170 0.00106 0.00096 0.00092 0.00135 0.00060 Si2 0.13594 0.00403 0.68241 1.00000 0.03362 0.02989 0.03571 -0.00138 -0.00375 -0.01080 0.03339 0.00263 0.00020 0.00021 0.00008 0.00000 0.00153 0.00179 0.00104 0.00094 0.00091 0.00138 0.00061 Si3 0.17098 -0.28193 0.69802 1.00000 0.03157 0.02937 0.03501 -0.00323 -0.00384 -0.00945 0.03244 0.00253 0.00020 0.00020 0.00008 0.00000 0.00147 0.00167 0.00105 0.00092 0.00090 0.00132 0.00059 Si4 -0.13310 -0.19994 0.78199 1.00000 0.03485 0.03388 0.03460 -0.00257 0.00042 -0.01406 0.03448 0.00264 0.00020 0.00022 0.00009 0.00000 0.00149 0.00184 0.00104 0.00094 0.00092 0.00139 0.00062 Si5 -0.27514 0.19758 0.89783 1.00000 0.10444 0.06096 0.04523 -0.01585 0.00762 -0.03238 0.07083 0.00339 0.00028 0.00025 0.00011 0.00000 0.00231 0.00224 0.00134 0.00129 0.00134 0.00189 0.00086 Si6 0.19824 0.13491 0.79932 1.00000 0.06768 0.04737 0.05690 -0.00349 -0.01912 -0.02353 0.05532 0.00286 0.00024 0.00023 0.00010 0.00000 0.00192 0.00212 0.00135 0.00120 0.00120 0.00172 0.00076 Si7 0.32324 -0.37894 0.82610 1.00000 0.06739 0.05031 0.04058 0.00533 -0.01801 -0.02654 0.05045 0.00283 0.00023 0.00022 0.00009 0.00000 0.00182 0.00192 0.00119 0.00109 0.00111 0.00160 0.00071 Si8 -0.17915 -0.31217 0.92973 1.00000 0.06588 0.07005 0.04402 0.01291 -0.00670 -0.03596 0.05753 0.00315 0.00024 0.00023 0.00010 0.00000 0.00193 0.00212 0.00121 0.00119 0.00113 0.00171 0.00077 O1 -0.02744 0.05892 0.71029 1.00000 0.02020 0.03410 0.04526 0.00447 -0.00399 -0.00273 0.03560 0.00560 0.00039 0.00038 0.00018 0.00000 0.00302 0.00346 0.00253 0.00222 0.00211 0.00276 0.00121 O2 0.18958 -0.14879 0.67692 1.00000 0.03730 0.01640 0.04131 -0.00176 -0.00164 -0.00839 0.03243 0.00542 0.00039 0.00040 0.00018 0.00000 0.00316 0.00345 0.00244 0.00211 0.00208 0.00270 0.00119 O3 0.01994 -0.25536 0.73980 1.00000 0.02839 0.02481 0.04965 -0.00925 0.00120 -0.00739 0.03525 0.00539 0.00040 0.00039 0.00019 0.00000 0.00303 0.00329 0.00257 0.00221 0.00222 0.00270 0.00121 O4 -0.19106 -0.04627 0.77868 1.00000 0.03919 0.01899 0.04680 -0.01006 0.00023 -0.00811 0.03593 0.00548 0.00040 0.00040 0.00019 0.00000 0.00329 0.00371 0.00258 0.00221 0.00220 0.00290 0.00124 O5 -0.20090 0.17520 0.81728 1.00000 0.03514 0.03327 0.04763 -0.00451 -0.00577 -0.01010 0.03919 0.00552 0.00039 0.00039 0.00019 0.00000 0.00317 0.00362 0.00270 0.00232 0.00221 0.00285 0.00128 O6 0.21985 0.03714 0.73590 1.00000 0.04296 0.02739 0.03674 -0.00426 -0.00843 -0.00691 0.03694 0.00550 0.00042 0.00039 0.00018 0.00000 0.00330 0.00346 0.00244 0.00216 0.00211 0.00279 0.00124 O7 0.28394 -0.36448 0.74744 1.00000 0.02748 0.03550 0.03930 -0.00278 -0.00993 -0.00323 0.03583 0.00539 0.00041 0.00040 0.00019 0.00000 0.00304 0.00349 0.00247 0.00221 0.00212 0.00276 0.00123 O8 -0.12288 -0.24347 0.86201 1.00000 0.04697 0.04799 0.03825 0.00000 -0.00548 -0.01986 0.04376 0.00564 0.00042 0.00040 0.00019 0.00000 0.00336 0.00380 0.00249 0.00238 0.00225 0.00305 0.00135 C1 -0.30865 0.16834 0.69426 1.00000 0.02270 0.02223 0.03879 -0.00574 0.00179 -0.00424 0.02947 0.00903 0.00074 0.00074 0.00030 0.00000 0.00506 0.00579 0.00400 0.00355 0.00340 0.00471 0.00188 C2 -0.41316 0.28320 0.71094 1.00000 0.03295 0.03657 0.04962 -0.00429 -0.00357 -0.00903 0.04085 0.01011 0.00081 0.00078 0.00035 0.00000 0.00601 0.00678 0.00449 0.00418 0.00400 0.00552 0.00215 H2 -0.41544 0.32446 0.75230 1.00000 0.04902 0.00000 0.00000 C3 -0.51523 0.34016 0.66880 1.00000 0.03017 0.02465 0.07599 -0.00810 -0.00196 0.00539 0.04832 0.01091 0.00075 0.00072 0.00038 0.00000 0.00593 0.00636 0.00570 0.00451 0.00437 0.00526 0.00224 H3 -0.58628 0.41940 0.68134 1.00000 0.05798 0.00000 0.00000 C4 -0.51278 0.28066 0.60830 1.00000 0.04100 0.05055 0.06913 0.00256 -0.01502 -0.01404 0.05371 0.01139 0.00088 0.00088 0.00039 0.00000 0.00634 0.00759 0.00570 0.00498 0.00450 0.00589 0.00236 H4 -0.58284 0.31887 0.57954 1.00000 0.06446 0.00000 0.00000 C5 -0.40993 0.16727 0.58994 1.00000 0.04101 0.04325 0.05289 -0.00745 -0.01616 -0.00928 0.04613 0.01031 0.00084 0.00083 0.00037 0.00000 0.00640 0.00702 0.00471 0.00452 0.00435 0.00570 0.00225 H5 -0.40814 0.12671 0.54842 1.00000 0.05535 0.00000 0.00000 C6 -0.30878 0.11202 0.63198 1.00000 0.02949 0.03267 0.04768 -0.00628 0.00644 -0.00936 0.03820 0.00950 0.00071 0.00069 0.00032 0.00000 0.00539 0.00587 0.00433 0.00381 0.00359 0.00477 0.00201 H6 -0.23710 0.03366 0.61851 1.00000 0.04584 0.00000 0.00000 C7 0.16170 0.07621 0.59587 1.00000 0.03230 0.02085 0.03984 -0.00475 -0.00847 -0.00500 0.03178 0.00857 0.00070 0.00060 0.00029 0.00000 0.00524 0.00544 0.00382 0.00325 0.00341 0.00461 0.00190 C8 0.05761 0.12160 0.55394 1.00000 0.03358 0.05293 0.04435 0.00266 -0.00528 -0.01378 0.04440 0.00958 0.00072 0.00067 0.00032 0.00000 0.00547 0.00636 0.00430 0.00393 0.00361 0.00497 0.00211 H8 -0.02880 0.11550 0.57018 1.00000 0.05328 0.00000 0.00000 C9 0.07686 0.17539 0.48919 1.00000 0.04517 0.04592 0.04822 0.00113 -0.01827 -0.00882 0.04753 0.00970 0.00076 0.00066 0.00033 0.00000 0.00581 0.00633 0.00450 0.00397 0.00388 0.00515 0.00211 H9 0.00360 0.20636 0.46188 1.00000 0.05704 0.00000 0.00000 C10 0.20119 0.18443 0.46402 1.00000 0.05720 0.03764 0.03011 -0.00929 -0.00114 -0.01843 0.04145 0.00910 0.00077 0.00063 0.00031 0.00000 0.00626 0.00606 0.00378 0.00346 0.00381 0.00532 0.00214 H10 0.21406 0.22110 0.41940 1.00000 0.04974 0.00000 0.00000 C11 0.30644 0.14018 0.50373 1.00000 0.04134 0.04362 0.04072 -0.00329 0.00295 -0.02086 0.04116 0.00931 0.00073 0.00063 0.00031 0.00000 0.00571 0.00604 0.00414 0.00370 0.00361 0.00499 0.00207 H11 0.39304 0.14504 0.48648 1.00000 0.04939 0.00000 0.00000 C12 0.28602 0.08800 0.56952 1.00000 0.03598 0.03659 0.04086 -0.00750 -0.00608 -0.00957 0.03848 0.00878 0.00069 0.00062 0.00030 0.00000 0.00511 0.00583 0.00404 0.00356 0.00343 0.00471 0.00194 H12 0.35887 0.05974 0.59713 1.00000 0.04617 0.00000 0.00000 C13 0.19143 -0.36902 0.61861 1.00000 0.02629 0.02774 0.03372 0.00213 -0.00906 -0.00162 0.03126 0.00882 0.00063 0.00062 0.00028 0.00000 0.00460 0.00550 0.00370 0.00319 0.00310 0.00428 0.00180 C14 0.12475 -0.45347 0.61588 1.00000 0.04052 0.03456 0.03115 -0.00356 0.00120 -0.01155 0.03658 0.00905 0.00065 0.00063 0.00030 0.00000 0.00510 0.00574 0.00365 0.00336 0.00324 0.00460 0.00192 H14 0.07129 -0.46756 0.65702 1.00000 0.04389 0.00000 0.00000 C15 0.13205 -0.51759 0.55686 1.00000 0.04411 0.03694 0.04165 -0.00649 -0.00437 -0.01245 0.04148 0.00940 0.00067 0.00064 0.00032 0.00000 0.00528 0.00581 0.00420 0.00364 0.00361 0.00466 0.00200 H15 0.08156 -0.57143 0.55692 1.00000 0.04977 0.00000 0.00000 C16 0.21486 -0.50201 0.49709 1.00000 0.04746 0.03840 0.03762 -0.01215 -0.00653 -0.00290 0.04427 0.01006 0.00068 0.00066 0.00032 0.00000 0.00554 0.00619 0.00404 0.00363 0.00366 0.00497 0.00206 H16 0.22485 -0.54834 0.45640 1.00000 0.05313 0.00000 0.00000 C17 0.28271 -0.41846 0.49730 1.00000 0.05452 0.04609 0.04319 -0.00272 0.00682 -0.02073 0.04864 0.01041 0.00070 0.00070 0.00033 0.00000 0.00581 0.00635 0.00431 0.00388 0.00376 0.00526 0.00218 H17 0.33577 -0.40372 0.45617 1.00000 0.05837 0.00000 0.00000 C18 0.27223 -0.35752 0.55755 1.00000 0.03978 0.05636 0.03428 -0.00198 -0.00734 -0.02669 0.04052 0.00904 0.00065 0.00065 0.00030 0.00000 0.00510 0.00614 0.00389 0.00370 0.00338 0.00481 0.00205 H18 0.32333 -0.30423 0.55750 1.00000 0.04862 0.00000 0.00000 C19 -0.24351 -0.26138 0.74318 1.00000 0.02385 0.02787 0.03419 -0.00217 -0.00095 -0.00076 0.03143 0.00958 0.00073 0.00078 0.00029 0.00000 0.00529 0.00627 0.00369 0.00344 0.00320 0.00511 0.00195 C20 -0.20626 -0.39324 0.73645 1.00000 0.02970 0.04295 0.04798 -0.00680 0.00532 -0.00331 0.04399 0.01080 0.00072 0.00080 0.00031 0.00000 0.00526 0.00709 0.00434 0.00399 0.00350 0.00539 0.00212 H20 -0.12596 -0.45013 0.75394 1.00000 0.05279 0.00000 0.00000 C21 -0.28560 -0.44159 0.70445 1.00000 0.05425 0.04287 0.06707 -0.01033 -0.00348 -0.02659 0.05222 0.01049 0.00086 0.00081 0.00035 0.00000 0.00669 0.00719 0.00509 0.00441 0.00461 0.00622 0.00245 H21 -0.25845 -0.53088 0.69957 1.00000 0.06266 0.00000 0.00000 C22 -0.40394 -0.35962 0.67977 1.00000 0.04220 0.08413 0.05051 -0.01558 0.00095 -0.03423 0.05580 0.01148 0.00088 0.00100 0.00035 0.00000 0.00680 0.00916 0.00466 0.00510 0.00420 0.00711 0.00278 H22 -0.45704 -0.39286 0.65735 1.00000 0.06696 0.00000 0.00000 C23 -0.44488 -0.23109 0.68748 1.00000 0.02785 0.05656 0.06201 0.00074 -0.00290 -0.01072 0.05063 0.01160 0.00076 0.00089 0.00034 0.00000 0.00567 0.00787 0.00494 0.00468 0.00388 0.00602 0.00235 H23 -0.52733 -0.17533 0.67144 1.00000 0.06076 0.00000 0.00000 C24 -0.36521 -0.18196 0.71898 1.00000 0.04082 0.05176 0.04656 -0.00643 0.00333 -0.02504 0.04476 0.00965 0.00077 0.00077 0.00031 0.00000 0.00592 0.00682 0.00416 0.00391 0.00381 0.00569 0.00222 H24 -0.39442 -0.09252 0.72408 1.00000 0.05371 0.00000 0.00000 C25 -0.18542 0.06741 0.95254 1.00000 0.26041 0.05376 0.05276 0.00448 -0.00751 -0.00376 0.13984 0.01512 0.00115 0.00079 0.00041 0.00000 0.01397 0.00795 0.00558 0.00523 0.00721 0.00826 0.00474 H25A -0.16328 -0.01333 0.92928 1.00000 0.20975 0.00000 0.00000 H25B -0.24371 0.06895 0.99685 1.00000 0.20975 0.00000 0.00000 H25C -0.10050 0.07588 0.96123 1.00000 0.20975 0.00000 0.00000 C26 -0.29291 0.35146 0.92511 1.00000 0.13916 0.05140 0.06077 -0.01184 -0.02700 -0.01959 0.08628 0.01064 0.00089 0.00070 0.00038 0.00000 0.00878 0.00710 0.00524 0.00465 0.00546 0.00634 0.00298 H26A -0.20192 0.35608 0.92285 1.00000 0.12942 0.00000 0.00000 H26B -0.33938 0.36564 0.97300 1.00000 0.12942 0.00000 0.00000 H26C -0.34716 0.41689 0.89441 1.00000 0.12942 0.00000 0.00000 C27 0.10674 0.30024 0.77213 1.00000 0.09334 0.01619 0.10872 0.00294 -0.05461 -0.00137 0.07394 0.01023 0.00078 0.00062 0.00040 0.00000 0.00739 0.00656 0.00653 0.00473 0.00563 0.00557 0.00273 H27A 0.16418 0.32476 0.73408 1.00000 0.11092 0.00000 0.00000 H27B 0.08662 0.35684 0.81157 1.00000 0.11092 0.00000 0.00000 H27C 0.02072 0.30711 0.75628 1.00000 0.11092 0.00000 0.00000 C28 0.36496 0.10952 0.82408 1.00000 0.06333 0.05172 0.09697 -0.02215 -0.01499 -0.02534 0.06796 0.00909 0.00070 0.00069 0.00038 0.00000 0.00615 0.00664 0.00606 0.00477 0.00489 0.00553 0.00251 H28A 0.40503 0.02260 0.84227 1.00000 0.10194 0.00000 0.00000 H28B 0.35444 0.17035 0.86004 1.00000 0.10194 0.00000 0.00000 H28C 0.42543 0.12192 0.78332 1.00000 0.10194 0.00000 0.00000 C29 0.25295 -0.22372 0.86777 1.00000 0.19924 0.06373 0.05450 -0.01200 -0.03055 -0.04069 0.10605 0.01128 0.00099 0.00075 0.00037 0.00000 0.01082 0.00766 0.00524 0.00491 0.00616 0.00740 0.00353 H29A 0.28409 -0.16331 0.83859 1.00000 0.15908 0.00000 0.00000 H29B 0.28454 -0.23171 0.91335 1.00000 0.15908 0.00000 0.00000 H29C 0.15252 -0.19289 0.87374 1.00000 0.15908 0.00000 0.00000 C30 0.26051 -0.49382 0.87534 1.00000 0.09256 0.06349 0.05550 0.00579 -0.00132 -0.03981 0.06854 0.01024 0.00077 0.00067 0.00034 0.00000 0.00686 0.00660 0.00470 0.00436 0.00446 0.00572 0.00251 H30A 0.16152 -0.46708 0.87454 1.00000 0.10281 0.00000 0.00000 H30B 0.27887 -0.49804 0.92356 1.00000 0.10281 0.00000 0.00000 H30C 0.30751 -0.57791 0.85432 1.00000 0.10281 0.00000 0.00000 C31 -0.09742 -0.29412 1.00348 1.00000 0.10857 0.07255 0.03222 0.00329 -0.00843 -0.03798 0.07007 0.00963 0.00077 0.00070 0.00030 0.00000 0.00720 0.00701 0.00402 0.00405 0.00429 0.00606 0.00260 H31A 0.00253 -0.33140 0.99174 1.00000 0.10510 0.00000 0.00000 H31B -0.12583 -0.33782 1.04455 1.00000 0.10510 0.00000 0.00000 H31C -0.12547 -0.20354 1.01339 1.00000 0.10510 0.00000 0.00000 C32 -0.36720 -0.24412 0.94430 1.00000 0.06616 0.23107 0.09036 0.04534 0.00572 -0.04885 0.13501 0.01551 0.00083 0.00102 0.00045 0.00000 0.00743 0.01335 0.00691 0.00782 0.00560 0.00801 0.00445 H32A -0.39820 -0.15220 0.95117 1.00000 0.20252 0.00000 0.00000 H32B -0.40052 -0.28375 0.98573 1.00000 0.20252 0.00000 0.00000 H32C -0.40336 -0.26005 0.90380 1.00000 0.20252 0.00000 0.00000 H5S -0.41960 0.19223 0.89820 1.00000 0.16201 0.06472 0.00351 0.00489 0.00275 0.00000 0.00000 H6S 0.11160 0.09682 0.85973 1.00000 0.16201 0.07656 0.00465 0.00484 0.00208 0.00000 0.00000 H7S 0.47341 -0.42475 0.82699 1.00000 0.16201 0.07038 0.00311 0.00468 0.00278 0.00000 0.00000 H8S -0.12085 -0.45223 0.91204 1.00000 0.16201 0.06601 0.00511 0.00296 0.00271 0.00000 0.00000 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 453 Maximum vector length = 511 Memory required = 5388 / 22995 wR2 = 0.1901 before cycle 10 for 5962 data and 0 / 453 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 12. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.050 0.050 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.073 0.051 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.000; Restrained GooF = 1.001 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0788 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0751 for 2567 Fo > 4sig(Fo) and 0.1995 for all 5962 data wR2 = 0.1901, GooF = S = 1.000, Restrained GooF = 1.001 for all data Occupancy sum of asymmetric unit = 48.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0401 0.0352 0.0292 Si1 0.0362 0.0343 0.0297 Si2 0.0362 0.0330 0.0280 Si3 0.0407 0.0326 0.0302 Si4 0.1124 0.0643 0.0358 Si5 0.0738 0.0528 0.0394 Si6 0.0702 0.0460 0.0351 Si7 0.0783 0.0586 0.0357 Si8 0.0507 0.0373 0.0188 O1 0.0445 0.0367 0.0160 O2 0.0533 0.0310 0.0214 O3 0.0513 0.0407 0.0158 O4 0.0488 0.0370 0.0318 O5 0.0499 0.0350 0.0259 O6 0.0482 0.0362 0.0231 O7 0.0493 0.0438 0.0382 O8 0.0417 0.0289 0.0178 C1 0.0506 0.0406 0.0313 C2 0.0775 0.0521 0.0154 C3 0.0703 0.0531 0.0378 C4 0.0650 0.0396 0.0337 C5 0.0551 0.0349 0.0246 C6 0.0440 0.0316 0.0198 C7 0.0565 0.0433 0.0334 C8 0.0623 0.0484 0.0319 C9 0.0588 0.0418 0.0237 C10 0.0520 0.0400 0.0314 C11 0.0482 0.0360 0.0313 C12 0.0404 0.0347 0.0188 C13 0.0455 0.0361 0.0280 C14 0.0470 0.0447 0.0328 C15 0.0659 0.0410 0.0259 C16 0.0656 0.0449 0.0355 C17 0.0580 0.0364 0.0272 C18 0.0407 0.0346 0.0189 C19 0.0566 0.0519 0.0235 C20 0.0722 0.0540 0.0304 C21 0.0901 0.0448 0.0325 C22 0.0659 0.0581 0.0278 C23 0.0601 0.0432 0.0310 C24 0.3141 0.0577 0.0476 C25 may be split into -0.1688 0.0777 0.9546 and -0.2020 0.0571 0.9505 0.1537 0.0640 0.0411 C26 0.1451 0.0614 0.0153 C27 0.1059 0.0635 0.0345 C28 0.2084 0.0711 0.0386 C29 may be split into 0.2682 -0.2193 0.8674 and 0.2377 -0.2281 0.8681 0.0960 0.0648 0.0448 C30 0.1093 0.0691 0.0318 C31 0.2639 0.0932 0.0480 C32 may be split into -0.3774 -0.2260 0.9482 and -0.3570 -0.2623 0.9404 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.024 0.033 0.043 0.055 0.072 0.098 0.156 1.000 Number in group 638. 559. 651. 584. 567. 583. 594. 605. 581. 600. GooF 0.786 0.810 0.885 0.972 0.954 1.015 1.162 1.189 1.174 0.974 K 7.788 0.840 1.178 1.118 1.023 1.032 1.029 1.039 1.013 1.028 Resolution(A) 0.77 0.81 0.85 0.90 0.96 1.03 1.13 1.27 1.49 1.92 inf Number in group 609. 590. 608. 582. 590. 596. 599. 595. 594. 599. GooF 0.820 0.868 0.838 0.884 0.905 1.030 1.085 1.040 1.100 1.323 K 1.134 1.193 1.078 1.176 1.084 1.051 1.006 0.994 1.010 1.031 R1 0.539 0.494 0.412 0.332 0.245 0.223 0.153 0.091 0.068 0.048 Recommended weighting scheme: WGHT 0.0783 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 8 5 3 113.20 8.75 5.35 0.014 1.29 -3 0 4 213.23 338.50 4.60 0.086 2.54 2 0 6 198.59 359.04 4.54 0.089 2.86 -1 -2 8 622.98 358.37 4.50 0.089 2.14 -6 -2 8 13.86 151.29 3.87 0.058 1.32 -8 -2 4 685.77 363.22 3.86 0.089 1.21 11 7 11 406.50 143.97 3.78 0.056 0.87 1 2 8 86.61 26.80 3.75 0.024 2.28 11 5 13 510.21 220.89 3.72 0.070 0.86 -2 3 13 -140.16 362.93 3.70 0.089 1.23 1 0 9 74.04 16.98 3.64 0.019 2.15 5 -1 3 411.72 280.25 3.62 0.078 1.79 5 1 2 211.53 32.11 3.61 0.027 2.07 5 9 5 111.06 309.41 3.51 0.082 1.20 -8 -7 6 24.40 89.61 3.41 0.044 1.06 6 6 0 360.42 171.09 3.36 0.061 1.50 -2 3 1 683.21 513.04 3.35 0.106 2.41 3 4 4 359.48 487.24 3.31 0.103 2.37 0 1 5 116.59 61.73 3.28 0.037 3.63 -2 -3 2 187.07 132.99 3.28 0.054 3.20 -5 -4 10 -13.80 46.74 3.28 0.032 1.28 5 2 1 840.90 1104.44 3.27 0.156 2.12 -7 -7 11 477.36 251.69 3.27 0.074 0.97 2 7 0 147.85 85.43 3.27 0.043 1.61 2 -1 8 69.41 7.43 3.26 0.013 2.15 -2 -4 3 -5.53 33.61 3.26 0.027 2.47 4 -2 1 79.20 34.50 3.22 0.028 1.96 -1 -5 12 -28.01 59.29 3.22 0.036 1.27 1 4 3 115.26 67.40 3.22 0.038 2.62 -5 -1 9 295.49 432.26 3.21 0.097 1.39 -7 -7 6 5412.40 3991.42 3.19 0.296 1.14 -6 0 1 197.43 75.60 3.16 0.041 1.60 -1 -6 1 69.50 26.48 3.14 0.024 1.83 -4 -3 5 837.39 1095.77 3.13 0.155 1.96 -3 3 12 1349.30 2009.80 3.12 0.210 1.22 -6 -1 11 946.16 573.97 3.11 0.112 1.14 -5 -7 9 58.32 152.56 3.11 0.058 1.16 4 7 0 56.33 119.79 3.10 0.051 1.56 -3 -3 4 -12.20 24.29 3.09 0.023 2.40 -5 -3 9 139.53 223.34 3.09 0.070 1.38 10 12 3 709.09 216.38 3.08 0.069 0.82 -4 -2 5 197.03 107.46 3.07 0.049 2.02 0 0 7 241.88 176.57 3.03 0.062 2.75 -6 -2 13 25.87 138.07 3.03 0.055 1.05 -6 0 13 472.01 911.60 3.02 0.141 1.03 -6 1 9 314.66 137.86 3.02 0.055 1.17 -8 0 2 449.28 241.55 3.02 0.073 1.19 6 9 3 501.91 318.45 3.00 0.084 1.18 0 -2 8 1469.30 1138.56 3.00 0.158 2.17 5 3 2 590.07 778.95 2.98 0.131 2.07 Bond lengths and angles Si1 - Distance Angles O1 1.6026 (0.0040) O5 1.6062 (0.0041) 109.52 (0.23) O4 1.6168 (0.0043) 108.72 (0.24) 109.24 (0.22) C1 1.8372 (0.0070) 110.31 (0.25) 109.61 (0.29) 109.42 (0.25) Si1 - O1 O5 O4 Si2 - Distance Angles O6 1.6097 (0.0040) O2 1.6136 (0.0042) 107.96 (0.23) O1 1.6259 (0.0041) 110.56 (0.22) 109.17 (0.22) C7 1.8492 (0.0060) 110.77 (0.26) 110.39 (0.25) 107.99 (0.27) Si2 - O6 O2 O1 Si3 - Distance Angles O2 1.6117 (0.0042) O3 1.6130 (0.0040) 109.78 (0.23) O7 1.6176 (0.0041) 109.82 (0.21) 108.80 (0.21) C13 1.8306 (0.0061) 108.80 (0.25) 109.30 (0.26) 110.33 (0.26) Si3 - O2 O3 O7 Si4 - Distance Angles O8 1.6070 (0.0040) O4 1.6156 (0.0044) 107.95 (0.22) O3 1.6165 (0.0042) 107.76 (0.24) 109.51 (0.22) C19 1.8350 (0.0066) 111.92 (0.25) 110.76 (0.31) 108.88 (0.27) Si4 - O8 O4 O3 Si5 - Distance Angles O5 1.6357 (0.0043) C26 1.7906 (0.0072) 109.51 (0.32) C25 1.8034 (0.0082) 110.37 (0.35) 114.62 (0.40) H5S 1.5544 (0.0293) 106.24 (1.98) 109.50 (1.94) 106.24 (1.93) Si5 - O5 C26 C25 Si6 - Distance Angles O6 1.6464 (0.0041) C28 1.8151 (0.0066) 108.45 (0.29) C27 1.8412 (0.0068) 110.07 (0.29) 112.97 (0.35) H6S 1.5222 (0.0293) 105.78 (1.98) 109.33 (1.94) 109.98 (1.95) Si6 - O6 C28 C27 Si7 - Distance Angles O7 1.6261 (0.0040) C29 1.8271 (0.0075) 109.94 (0.32) C30 1.8283 (0.0062) 109.69 (0.27) 111.71 (0.37) H7S 1.4815 (0.0294) 112.09 (2.08) 105.68 (2.01) 107.69 (2.03) Si7 - O7 C29 C30 Si8 - Distance Angles O8 1.6343 (0.0040) C32 1.8341 (0.0083) 109.68 (0.33) C31 1.8412 (0.0064) 107.40 (0.28) 114.06 (0.41) H8S 1.5153 (0.0293) 104.40 (2.03) 113.62 (2.00) 107.08 (1.96) Si8 - O8 C32 C31 O1 - Distance Angles Si1 1.6026 (0.0040) Si2 1.6259 (0.0041) 166.42 (0.28) O1 - Si1 O2 - Distance Angles Si3 1.6117 (0.0042) Si2 1.6136 (0.0042) 150.50 (0.27) O2 - Si3 O3 - Distance Angles Si3 1.6130 (0.0040) Si4 1.6165 (0.0042) 168.62 (0.30) O3 - Si3 O4 - Distance Angles Si4 1.6156 (0.0044) Si1 1.6168 (0.0043) 151.92 (0.28) O4 - Si4 O5 - Distance Angles Si1 1.6062 (0.0041) Si5 1.6357 (0.0043) 141.25 (0.28) O5 - Si1 O6 - Distance Angles Si2 1.6097 (0.0040) Si6 1.6464 (0.0041) 141.24 (0.30) O6 - Si2 O7 - Distance Angles Si3 1.6176 (0.0041) Si7 1.6261 (0.0040) 143.99 (0.29) O7 - Si3 O8 - Distance Angles Si4 1.6070 (0.0040) Si8 1.6343 (0.0040) 147.07 (0.28) O8 - Si4 C1 - Distance Angles C2 1.3781 (0.0081) C6 1.4068 (0.0082) 116.96 (0.68) Si1 1.8372 (0.0070) 122.32 (0.52) 120.67 (0.63) C1 - C2 C6 C2 - Distance Angles C1 1.3781 (0.0081) C3 1.3891 (0.0082) 121.67 (0.68) H2 0.9500 119.16 119.16 C2 - C1 C3 C3 - Distance Angles C4 1.3870 (0.0092) C2 1.3891 (0.0082) 119.60 (0.76) H3 0.9500 120.20 120.20 C3 - C4 C2 C4 - Distance Angles C5 1.3662 (0.0088) C3 1.3870 (0.0092) 120.21 (0.78) H4 0.9500 119.90 119.90 C4 - C5 C3 C5 - Distance Angles C4 1.3662 (0.0088) C6 1.3784 (0.0081) 119.66 (0.72) H5 0.9500 120.17 120.17 C5 - C4 C6 C6 - Distance Angles C5 1.3784 (0.0081) C1 1.4068 (0.0082) 121.89 (0.73) H6 0.9500 119.05 119.05 C6 - C5 C1 C7 - Distance Angles C8 1.3906 (0.0076) C12 1.3928 (0.0076) 116.73 (0.58) Si2 1.8492 (0.0060) 121.55 (0.49) 121.71 (0.50) C7 - C8 C12 C8 - Distance Angles C9 1.3825 (0.0083) C7 1.3906 (0.0077) 121.59 (0.65) H8 0.9500 119.21 119.21 C8 - C9 C7 C9 - Distance Angles C10 1.3749 (0.0081) C8 1.3825 (0.0083) 120.53 (0.66) H9 0.9500 119.74 119.74 C9 - C10 C8 C10 - Distance Angles C11 1.3708 (0.0079) C9 1.3749 (0.0081) 119.56 (0.61) H10 0.9500 120.22 120.22 C10 - C11 C9 C11 - Distance Angles C10 1.3708 (0.0079) C12 1.3944 (0.0078) 119.79 (0.64) H11 0.9500 120.10 120.10 C11 - C10 C12 C12 - Distance Angles C7 1.3928 (0.0076) C11 1.3944 (0.0078) 121.78 (0.64) H12 0.9500 119.11 119.11 C12 - C7 C11 C13 - Distance Angles C18 1.3859 (0.0075) C14 1.3935 (0.0076) 114.93 (0.56) Si3 1.8306 (0.0061) 123.92 (0.50) 121.15 (0.44) C13 - C18 C14 C14 - Distance Angles C15 1.3764 (0.0075) C13 1.3935 (0.0076) 123.62 (0.56) H14 0.9500 118.19 118.19 C14 - C15 C13 C15 - Distance Angles C14 1.3764 (0.0075) C16 1.3921 (0.0082) 118.71 (0.64) H15 0.9500 120.65 120.65 C15 - C14 C16 C16 - Distance Angles C17 1.3871 (0.0077) C15 1.3921 (0.0082) 119.62 (0.62) H16 0.9500 120.19 120.19 C16 - C17 C15 C17 - Distance Angles C18 1.3692 (0.0080) C16 1.3871 (0.0077) 119.14 (0.59) H17 0.9500 120.43 120.43 C17 - C18 C16 C18 - Distance Angles C17 1.3692 (0.0080) C13 1.3859 (0.0075) 123.84 (0.62) H18 0.9500 118.08 118.08 C18 - C17 C13 C19 - Distance Angles C24 1.3972 (0.0083) C20 1.4053 (0.0081) 117.36 (0.65) Si4 1.8350 (0.0066) 122.68 (0.60) 119.96 (0.58) C19 - C24 C20 C20 - Distance Angles C21 1.3931 (0.0087) C19 1.4053 (0.0081) 120.84 (0.74) H20 0.9500 119.58 119.58 C20 - C21 C19 C21 - Distance Angles C22 1.3840 (0.0089) C20 1.3931 (0.0087) 120.04 (0.81) H21 0.9500 119.98 119.98 C21 - C22 C20 C22 - Distance Angles C23 1.3672 (0.0089) C21 1.3840 (0.0089) 120.38 (0.78) H22 0.9500 119.81 119.81 C22 - C23 C21 C23 - Distance Angles C22 1.3672 (0.0089) C24 1.3964 (0.0086) 119.85 (0.80) H23 0.9500 120.08 120.08 C23 - C22 C24 C24 - Distance Angles C23 1.3964 (0.0086) C19 1.3972 (0.0083) 121.48 (0.77) H24 0.9500 119.26 119.26 C24 - C23 C19 C25 - Distance Angles Si5 1.8034 (0.0082) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - Si5 H25A H25B C26 - Distance Angles Si5 1.7906 (0.0072) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - Si5 H26A H26B C27 - Distance Angles Si6 1.8412 (0.0068) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - Si6 H27A H27B C28 - Distance Angles Si6 1.8151 (0.0066) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - Si6 H28A H28B C29 - Distance Angles Si7 1.8271 (0.0075) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - Si7 H29A H29B C30 - Distance Angles Si7 1.8283 (0.0062) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - Si7 H30A H30B C31 - Distance Angles Si8 1.8412 (0.0064) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - Si8 H31A H31B C32 - Distance Angles Si8 1.8341 (0.0082) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - Si8 H32A H32B FMAP and GRID set by program FMAP 2 3 50 GRID -1.064 -2 -2 1.064 2 2 R1 = 0.1992 for 5962 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.86 at 0.7167 0.8640 0.2429 [ 1.13 A from SI6 ] Deepest hole -0.41 at 0.8202 0.8951 0.1717 [ 0.68 A from SI6 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4950 / 34115 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2833 0.1360 0.7571 1.00000 0.05 0.86 1.13 SI6 1.61 O6 1.61 H28C 1.62 C28 Q2 1 -0.1596 0.2222 0.8876 1.00000 0.05 0.37 1.34 SI5 1.59 H26A 1.67 O5 1.72 C26 Q3 1 0.1707 0.0147 0.7224 1.00000 0.05 0.31 0.74 O6 0.94 SI2 2.02 O1 2.04 O2 Q4 1 0.1358 -0.6381 0.5646 1.00000 0.05 0.31 0.78 H15 1.35 C15 2.27 C16 2.33 C14 Q5 1 0.1853 0.0600 0.7766 1.00000 0.05 0.30 0.84 O6 1.04 SI6 1.69 H6S 2.17 SI2 Q6 1 -0.1492 0.1716 0.9100 1.00000 0.05 0.27 1.31 SI5 1.42 H25C 1.53 C25 1.95 O5 Q7 1 0.0922 0.3249 0.7113 1.00000 0.05 0.26 0.94 H27A 1.13 H27C 1.22 C27 1.99 H27B Q8 1 -0.0114 -0.2154 0.7524 1.00000 0.05 0.26 0.50 O3 1.28 SI4 1.96 SI3 2.16 O4 Q9 1 -0.2856 0.1535 0.8344 1.00000 0.05 0.26 1.02 O5 1.40 SI5 1.68 H5S 1.85 SI1 Q10 1 -0.7409 0.5000 0.7118 1.00000 0.05 0.25 1.59 H3 1.85 O7 2.29 C13 2.29 H14 Shortest distances between peaks (including symmetry equivalents) 2 6 0.68 3 5 1.26 1 5 1.57 2 9 2.18 6 9 2.28 1 3 2.32 1 7 2.55 4 7 2.85 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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. 0.92: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.50: Structure factors and derivatives 22.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.14: Apply other restraints 2.64: Solve l.s. equations 0.00: Generate HTAB table 0.20: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:40:27 Total CPU time: 33.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++