+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:00:19 on 17-Sep-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL L s92 in P-1 CELL 0.71073 10.7863 18.4652 19.0801 68.711 81.679 82.351 ZERR 1.00 0.0009 0.0015 0.0019 0.004 0.005 0.007 LATT 1 SFAC C H O SI CL UNIT 104 96 28 8 40 V = 3490.21 F(000) = 1736.0 Mu = 0.91 mm-1 Cell Wt = 3436.53 Rho = 1.635 MERG 2 OMIT 8 3 4 FMAP 2 PLAN 10 BOND $H ACTA SIZE 0.14 0.12 0.03 WGHT 0.03200 L.S. 8 TEMP -153.00 FVAR 0.05407 SI1 4 0.781922 0.440051 0.505176 11.00000 0.04360 0.03649 = 0.02677 -0.01444 0.00279 -0.00606 SI2 4 0.816737 0.554740 0.586297 11.00000 0.03977 0.03641 = 0.02536 -0.01418 0.00534 -0.00450 SI3 4 1.068012 0.456907 0.641328 11.00000 0.03874 0.03725 = 0.02342 -0.01131 0.00536 -0.00624 SI4 4 1.032782 0.342446 0.560360 11.00000 0.04385 0.03188 = 0.02257 -0.00910 0.00606 -0.00702 CL9 5 0.630962 0.151948 0.458946 11.00000 0.07613 0.08256 = 0.06359 -0.02427 0.00672 -0.01153 CL10 5 0.738968 0.005258 0.418297 11.00000 0.06907 0.11353 = 0.07572 -0.05590 0.00475 -0.00870 CL11 5 0.714323 -0.161726 0.539169 11.00000 0.07367 0.08924 = 0.09976 -0.06186 -0.01310 0.00618 CL12 5 0.569730 -0.180219 0.698400 11.00000 0.09652 0.06499 = 0.07409 -0.03039 -0.02147 -0.00217 CL13 5 0.455457 -0.030715 0.734935 11.00000 0.09585 0.07118 = 0.05747 -0.02629 -0.00235 -0.00660 CL22 5 0.437710 0.326454 0.965659 11.00000 0.05012 0.06494 = 0.05033 -0.02576 -0.00785 -0.00672 CL23 5 0.550481 0.187081 1.097868 11.00000 0.06615 0.04956 = 0.05482 -0.01615 0.00481 -0.01331 CL24 5 0.769414 0.211520 1.175919 11.00000 0.07054 0.05561 = 0.04126 -0.00841 -0.00830 0.00249 CL25 5 0.871311 0.375747 1.121891 11.00000 0.05832 0.06311 = 0.04458 -0.02238 -0.00856 -0.00632 CL26 5 0.754970 0.513177 0.990680 11.00000 0.05837 0.04813 = 0.04414 -0.01508 0.00158 -0.01084 CL35 5 0.619821 0.226781 0.841637 11.00000 0.08525 0.06643 = 0.04888 -0.01694 -0.01432 -0.00041 CL36 5 0.532033 0.066224 0.851294 11.00000 0.08321 0.09660 = 0.04523 -0.02733 -0.00596 -0.02701 CL37 5 0.635881 -0.088694 0.970286 11.00000 0.09478 0.07060 = 0.05919 -0.03602 0.01597 -0.02886 CL38 5 0.823885 -0.082316 1.076291 11.00000 0.09331 0.05635 = 0.06288 -0.01602 -0.00750 -0.00208 CL39 5 0.899624 0.077127 1.069024 11.00000 0.07302 0.07744 = 0.05379 -0.02092 -0.01655 -0.00770 CL48 5 1.033057 -0.116140 0.550721 11.00000 0.08399 0.07514 = 0.04824 -0.02612 0.00192 -0.02106 CL49 5 1.052367 -0.300333 0.609940 11.00000 0.10275 0.07271 = 0.07799 -0.05435 -0.00950 -0.00164 CL50 5 0.922293 -0.390458 0.769487 11.00000 0.08266 0.04311 = 0.07730 -0.01838 -0.03114 -0.00370 CL51 5 0.781196 -0.299332 0.870070 11.00000 0.07641 0.06316 = 0.06180 -0.00701 0.00769 -0.02034 CL52 5 0.777126 -0.118087 0.811895 11.00000 0.07878 0.06145 = 0.07247 -0.03175 0.02433 -0.01439 O1 3 0.757553 0.500135 0.552135 11.00000 0.03892 0.03870 = 0.03133 -0.01768 0.01843 -0.01407 O2 3 0.932200 0.504510 0.634312 11.00000 0.04345 0.04081 = 0.02747 -0.01903 0.00882 -0.00679 O3 3 1.065882 0.379841 0.620126 11.00000 0.04489 0.03163 = 0.01680 -0.00405 -0.00337 -0.00314 O4 3 0.890043 0.372337 0.540154 11.00000 0.04035 0.03160 = 0.03134 -0.00997 0.00420 -0.01098 O5 3 0.828336 0.488359 0.418329 11.00000 0.04650 0.03367 = 0.02789 -0.01540 0.00707 -0.00257 O6 3 0.873327 0.627078 0.516948 11.00000 0.05222 0.02667 = 0.01675 -0.00511 0.00454 -0.00206 O7 3 0.672350 0.130721 0.647046 11.00000 0.05872 0.07321 = 0.09499 -0.04095 -0.00727 -0.00317 O8 3 0.492387 0.115890 0.611620 11.00000 0.05942 0.06290 = 0.07013 -0.03382 -0.01545 -0.00412 O9 3 0.705825 0.460025 0.845426 11.00000 0.05085 0.08247 = 0.03252 -0.02163 0.00044 0.00722 O10 3 0.548571 0.474804 0.931475 11.00000 0.05040 0.05813 = 0.02738 -0.02358 0.00385 -0.00626 O11 3 0.954458 0.202583 0.874896 11.00000 0.06518 0.04089 = 0.03668 -0.01930 0.01490 -0.00768 O12 3 0.786072 0.212204 0.955751 11.00000 0.06368 0.04230 = 0.03814 -0.02090 0.00432 -0.00807 O13 3 1.069482 -0.062210 0.725862 11.00000 0.07533 0.04616 = 0.07228 -0.02193 -0.01677 -0.00707 O14 3 0.902712 -0.047573 0.659997 11.00000 0.07468 0.03020 = 0.04884 -0.00708 -0.01255 -0.00688 C1 1 0.636729 0.396176 0.513259 11.00000 0.05641 0.04434 = 0.03468 -0.01304 0.00731 -0.00394 AFIX 23 H1A 2 0.564890 0.435052 0.515206 11.00000 -1.20000 H1B 2 0.635021 0.383661 0.467179 11.00000 -1.20000 AFIX 0 C2 1 0.618188 0.320222 0.584122 11.00000 0.03590 0.05935 = 0.04514 -0.01589 -0.00542 -0.00504 AFIX 23 H2A 2 0.674747 0.277014 0.574961 11.00000 -1.20000 H2B 2 0.644760 0.328235 0.628125 11.00000 -1.20000 AFIX 0 C3 1 0.484125 0.295116 0.604744 11.00000 0.04723 0.04066 = 0.04926 -0.01107 0.01194 0.00120 C4 1 0.404915 0.347764 0.642914 11.00000 0.06952 0.06769 = 0.04731 -0.01648 -0.00213 -0.00797 AFIX 137 H4A 2 0.402455 0.401897 0.607808 11.00000 -1.50000 H4B 2 0.442079 0.343791 0.688239 11.00000 -1.50000 H4C 2 0.319230 0.331491 0.657261 11.00000 -1.50000 AFIX 0 C5 1 0.427643 0.296355 0.535856 11.00000 0.08301 0.07962 = 0.06271 -0.02581 -0.02495 -0.02791 AFIX 137 H5A 2 0.415125 0.350332 0.501192 11.00000 -1.50000 H5B 2 0.346551 0.273714 0.551811 11.00000 -1.50000 H5C 2 0.484799 0.265820 0.510102 11.00000 -1.50000 AFIX 0 C6 1 0.486317 0.214653 0.666091 11.00000 0.04495 0.05287 = 0.08534 -0.03959 -0.00401 0.01794 AFIX 23 H6A 2 0.522209 0.216960 0.710067 11.00000 -1.20000 H6B 2 0.398794 0.200454 0.682921 11.00000 -1.20000 AFIX 0 C7 1 0.560590 0.152265 0.641385 11.00000 0.05613 0.06482 = 0.06189 0.00162 -0.00454 -0.01955 C8 1 0.555150 0.050406 0.596117 11.00000 0.06797 0.07014 = 0.05260 -0.04515 -0.00644 -0.00360 C9 1 0.616916 0.056304 0.526634 11.00000 0.07034 0.06538 = 0.05172 -0.02417 -0.00464 -0.02970 C10 1 0.667936 -0.009289 0.508076 11.00000 0.06544 0.08225 = 0.04798 -0.05042 -0.00013 -0.00036 C11 1 0.651046 -0.083132 0.562815 11.00000 0.08417 0.04177 = 0.04627 -0.01406 -0.01167 0.00558 C12 1 0.592720 -0.088687 0.632678 11.00000 0.07742 0.01980 = 0.05076 0.00289 -0.01511 -0.00231 C13 1 0.537561 -0.023091 0.648667 11.00000 0.05194 0.03641 = 0.05881 0.00523 -0.00436 -0.00002 C14 1 0.694168 0.590818 0.646027 11.00000 0.04650 0.04346 = 0.03266 -0.01897 -0.00299 0.00340 AFIX 23 H14A 2 0.734591 0.602572 0.683609 11.00000 -1.20000 H14B 2 0.651850 0.640231 0.613937 11.00000 -1.20000 AFIX 0 C15 1 0.593143 0.532854 0.688648 11.00000 0.02747 0.05664 = 0.03306 -0.02478 0.00948 0.00106 AFIX 23 H15A 2 0.549958 0.523413 0.650773 11.00000 -1.20000 H15B 2 0.636364 0.482492 0.718211 11.00000 -1.20000 AFIX 0 C16 1 0.493231 0.559454 0.742438 11.00000 0.04926 0.04759 = 0.03726 -0.02241 0.01313 -0.02091 C17 1 0.399242 0.496772 0.776457 11.00000 0.04632 0.08100 = 0.04133 -0.02902 0.01695 -0.01910 AFIX 137 H17A 2 0.444345 0.446296 0.801930 11.00000 -1.50000 H17B 2 0.356616 0.493083 0.736023 11.00000 -1.50000 H17C 2 0.336873 0.510994 0.813096 11.00000 -1.50000 AFIX 0 C18 1 0.417105 0.638567 0.699669 11.00000 0.05544 0.06863 = 0.03923 -0.01852 -0.00648 0.00467 AFIX 137 H18A 2 0.348151 0.650343 0.734478 11.00000 -1.50000 H18B 2 0.382641 0.633833 0.656889 11.00000 -1.50000 H18C 2 0.473181 0.680726 0.681044 11.00000 -1.50000 AFIX 0 C19 1 0.547747 0.571678 0.806430 11.00000 0.05172 0.04265 = 0.02809 -0.01108 0.00299 0.01473 AFIX 23 H19A 2 0.610191 0.610816 0.784218 11.00000 -1.20000 H19B 2 0.479290 0.593171 0.835784 11.00000 -1.20000 AFIX 0 C20 1 0.608998 0.499536 0.858655 11.00000 0.04315 0.06873 = 0.04265 -0.03328 0.00627 -0.01749 C21 1 0.603460 0.410869 0.986444 11.00000 0.04034 0.04305 = 0.01748 -0.00304 -0.00618 0.01468 C22 1 0.557627 0.339814 1.011487 11.00000 0.03416 0.05565 = 0.03499 -0.02150 0.00043 0.00426 C23 1 0.604913 0.277747 1.068043 11.00000 0.04260 0.04588 = 0.03671 -0.02846 0.00163 -0.00850 C24 1 0.700544 0.288117 1.104323 11.00000 0.07191 0.05072 = 0.01540 -0.00845 0.00688 0.00155 C25 1 0.749482 0.360297 1.080420 11.00000 0.03590 0.06030 = 0.03660 -0.03144 -0.00673 0.00696 C26 1 0.698959 0.422282 1.021037 11.00000 0.02917 0.03459 = 0.02493 -0.00693 -0.01163 0.01472 C27 1 1.107673 0.428072 0.738692 11.00000 0.03950 0.01642 = 0.04292 -0.01813 0.00252 -0.00141 AFIX 23 H27A 2 1.190749 0.397582 0.742950 11.00000 -1.20000 H27B 2 1.114776 0.475633 0.749812 11.00000 -1.20000 AFIX 0 C28 1 1.011894 0.379987 0.797029 11.00000 0.04407 0.03371 = 0.03332 -0.00912 0.00847 -0.01430 AFIX 23 H28A 2 1.001569 0.334638 0.783061 11.00000 -1.20000 H28B 2 0.930208 0.412020 0.793322 11.00000 -1.20000 AFIX 0 C29 1 1.039088 0.349057 0.880430 11.00000 0.04006 0.03744 = 0.01741 -0.01059 0.00187 -0.00002 C30 1 1.164178 0.296440 0.890234 11.00000 0.08207 0.03528 = 0.03353 -0.00541 -0.00778 -0.01993 AFIX 137 H30A 2 1.233913 0.327619 0.861981 11.00000 -1.50000 H30B 2 1.160694 0.254338 0.870961 11.00000 -1.50000 H30C 2 1.177196 0.274019 0.943973 11.00000 -1.50000 AFIX 0 C31 1 1.050348 0.415874 0.906529 11.00000 0.07338 0.06222 = 0.02823 -0.02072 0.00274 -0.02322 AFIX 137 H31A 2 0.974355 0.452089 0.897317 11.00000 -1.50000 H31B 2 1.123865 0.443378 0.878453 11.00000 -1.50000 H31C 2 1.060120 0.395439 0.960725 11.00000 -1.50000 AFIX 0 C32 1 0.930520 0.304491 0.928920 11.00000 0.05179 0.04934 = 0.01854 -0.00929 -0.00011 -0.00635 AFIX 23 H32A 2 0.948955 0.286161 0.982251 11.00000 -1.20000 H32B 2 0.854659 0.341870 0.924329 11.00000 -1.20000 AFIX 0 C33 1 0.898324 0.236992 0.913889 11.00000 0.03890 0.05047 = 0.03223 -0.00927 0.00201 -0.01739 C34 1 0.754541 0.139985 0.958376 11.00000 0.05432 0.05930 = 0.03246 -0.02516 -0.00808 -0.01820 C35 1 0.673504 0.141266 0.907012 11.00000 0.08463 0.04251 = 0.04939 -0.02387 0.03397 -0.02115 C36 1 0.631908 0.070046 0.911430 11.00000 0.04755 0.07569 = 0.02751 -0.01304 -0.00056 0.00144 C37 1 0.679520 0.001704 0.963428 11.00000 0.05296 0.04734 = 0.03700 -0.03049 0.01589 -0.02371 C38 1 0.763215 0.002114 1.011601 11.00000 0.06949 0.02603 = 0.03848 0.00167 0.00625 0.01055 C39 1 0.799911 0.073230 1.008912 11.00000 0.05637 0.05137 = 0.03429 -0.02153 0.01011 0.00173 C40 1 1.053956 0.236351 0.598899 11.00000 0.04565 0.04948 = 0.04850 -0.03644 -0.00679 -0.00718 AFIX 23 H40A 2 1.036077 0.216101 0.560287 11.00000 -1.20000 H40B 2 1.143407 0.220576 0.607644 11.00000 -1.20000 AFIX 0 C41 1 0.972574 0.196841 0.672805 11.00000 0.04306 0.04618 = 0.03685 -0.02036 0.00219 -0.00267 AFIX 23 H41A 2 0.883457 0.206503 0.662303 11.00000 -1.20000 H41B 2 0.981383 0.222265 0.709223 11.00000 -1.20000 AFIX 0 C42 1 1.003293 0.107102 0.711330 11.00000 0.05666 0.04753 = 0.03563 -0.02442 0.01001 -0.00676 C43 1 0.908279 0.079723 0.782768 11.00000 0.06817 0.04783 = 0.03040 -0.01651 0.01459 -0.00870 AFIX 137 H43A 2 0.922971 0.023149 0.807872 11.00000 -1.50000 H43B 2 0.822409 0.092707 0.768139 11.00000 -1.50000 H43C 2 0.919314 0.105983 0.817513 11.00000 -1.50000 AFIX 0 C44 1 1.135630 0.090471 0.729824 11.00000 0.05280 0.04584 = 0.03968 -0.01265 -0.00336 -0.00073 AFIX 137 H44A 2 1.154340 0.127743 0.751768 11.00000 -1.50000 H44B 2 1.192332 0.095381 0.683610 11.00000 -1.50000 H44C 2 1.147520 0.037316 0.766294 11.00000 -1.50000 AFIX 0 C45 1 0.975777 0.068619 0.654973 11.00000 0.05538 0.04771 = 0.02444 -0.01760 0.00313 -0.01105 AFIX 23 H45A 2 0.888018 0.084652 0.642467 11.00000 -1.20000 H45B 2 1.032184 0.087818 0.607536 11.00000 -1.20000 AFIX 0 C46 1 0.994320 -0.018497 0.686847 11.00000 0.06634 0.05921 = 0.04189 -0.03458 0.00588 -0.01959 C47 1 0.909647 -0.128934 0.686861 11.00000 0.04668 0.05199 = 0.04528 -0.02679 0.00030 0.00054 C48 1 0.967897 -0.169166 0.638840 11.00000 0.04610 0.04966 = 0.03303 -0.00594 0.00538 -0.02864 C49 1 0.973289 -0.250454 0.667127 11.00000 0.07978 0.02736 = 0.04661 -0.01696 -0.00011 -0.02221 C50 1 0.916971 -0.289840 0.738409 11.00000 0.05493 0.02392 = 0.04717 0.00981 -0.03277 -0.00999 C51 1 0.856364 -0.251137 0.785041 11.00000 0.05300 0.04803 = 0.04420 -0.01951 -0.01549 0.00250 C52 1 0.852617 -0.170909 0.757670 11.00000 0.04384 0.04296 = 0.03901 -0.01837 0.01563 -0.00774 HKLF 4 Covalent radii and connectivity table for L s92 in P-1 C 0.770 H 0.320 O 0.660 SI 1.170 CL 0.990 Si1 - O5 O4 O1 C1 Si2 - O6 O1 O2 C14 Si3 - O2 O3 O5_$1 C27 Si4 - O4 O6_$1 O3 C40 Cl9 - C9 Cl10 - C10 Cl11 - C11 Cl12 - C12 Cl13 - C13 Cl22 - C22 Cl23 - C23 Cl24 - C24 Cl25 - C25 Cl26 - C26 Cl35 - C35 Cl36 - C36 Cl37 - C37 Cl38 - C38 Cl39 - C39 Cl48 - C48 Cl49 - C49 Cl50 - C50 Cl51 - C51 Cl52 - C52 O1 - Si2 Si1 O2 - Si3 Si2 O3 - Si3 Si4 O4 - Si1 Si4 O5 - Si1 Si3_$1 O6 - Si2 Si4_$1 O7 - C7 O8 - C7 C8 O9 - C20 O10 - C20 C21 O11 - C33 O12 - C33 C34 O13 - C46 O14 - C47 C46 C1 - C2 Si1 C2 - C3 C1 C3 - C5 C6 C4 C2 C4 - C3 C5 - C3 C6 - C7 C3 C7 - O7 O8 C6 C8 - C9 C13 O8 C9 - C8 C10 Cl9 C10 - C11 C9 Cl10 C11 - C12 C10 Cl11 C12 - C11 C13 Cl12 C13 - C8 C12 Cl13 C14 - C15 Si2 C15 - C16 C14 C16 - C19 C15 C17 C18 C17 - C16 C18 - C16 C19 - C20 C16 C20 - O9 O10 C19 C21 - C22 C26 O10 C22 - C21 C23 Cl22 C23 - C22 C24 Cl23 C24 - C23 C25 Cl24 C25 - C24 C26 Cl25 C26 - C21 C25 Cl26 C27 - C28 Si3 C28 - C27 C29 C29 - C31 C32 C28 C30 C30 - C29 C31 - C29 C32 - C33 C29 C33 - O11 O12 C32 C34 - C39 C35 O12 C35 - C34 C36 Cl35 C36 - C37 C35 Cl36 C37 - C36 C38 Cl37 C38 - C37 C39 Cl38 C39 - C34 C38 Cl39 C40 - C41 Si4 C41 - C40 C42 C42 - C44 C43 C41 C45 C43 - C42 C44 - C42 C45 - C46 C42 C46 - O13 O14 C45 C47 - C52 O14 C48 C48 - C49 C47 Cl48 C49 - C50 C48 Cl49 C50 - C51 C49 Cl50 C51 - C52 C50 Cl51 C52 - C51 C47 Cl52 Operators for generating equivalent atoms: $1 -x+2, -y+1, -z+1 32443 Reflections read, of which 1 rejected -13 =< h =< 13, -23 =< k =< 23, -24 =< l =< 24, Max. 2-theta = 55.11 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 2 4 60.29 1.90 3 15.72 4 3 5 31.20 1.12 3 10.08 6 5 6 22.01 1.08 4 6.06 3 Inconsistent equivalents 12068 Unique reflections, of which 0 suppressed R(int) = 0.2458 R(sigma) = 0.5300 Friedel opposites merged Maximum memory for data reduction = 6576 / 126639 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 = 8760 / 1198463 wR2 = 0.1681 before cycle 1 for 12068 data and 819 / 819 parameters GooF = S = 0.857; Restrained GooF = 0.857 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05421 0.00009 1.591 OSF Mean shift/esd = 0.028 Maximum = 1.591 for OSF Max. shift = 0.002 A for H5C Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 2 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 0.273 OSF Mean shift/esd = 0.010 Maximum = 0.273 for OSF Max. shift = 0.001 A for H4A Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 3 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 0.012 OSF Mean shift/esd = 0.001 Maximum = 0.012 for OSF Max. shift = 0.000 A for H4B Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 4 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 0.004 OSF Mean shift/esd = 0.000 Maximum = -0.005 for x C7 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 5 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for x C7 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 6 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H4A Max. dU = 0.000 for C7 Least-squares cycle 7 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 7 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cl24 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 511 Memory required = 8760 / 1198463 wR2 = 0.1680 before cycle 8 for 12068 data and 819 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05423 0.00009 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cl39 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C7 Largest correlation matrix elements -0.618 U23 Cl11 / U33 Cl11 -0.594 z C10 / y C10 -0.575 U23 Cl10 / U33 Cl10 -0.615 U23 Cl49 / U33 Cl49 -0.593 U23 C23 / U22 C23 -0.571 z C39 / y C39 -0.610 U23 C46 / U22 C46 -0.592 U23 C37 / U22 C37 -0.569 U23 Cl10 / U22 Cl10 -0.608 z C22 / y C22 -0.590 U23 C10 / U33 C10 -0.568 U23 C6 / U22 C6 -0.606 U23 Cl49 / U22 Cl49 -0.587 z C25 / y C25 -0.567 U23 O7 / U33 O7 -0.600 U23 C10 / U22 C10 -0.582 U23 C40 / U33 C40 -0.566 U23 C25 / U33 C25 -0.595 z C37 / y C37 -0.578 U23 Cl11 / U22 Cl11 -0.563 z C23 / y C23 -0.594 U23 C6 / U33 C6 -0.576 z C46 / y C46 -0.563 U23 C23 / U33 C23 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5649 0.4351 0.5152 23 0.990 0.000 C1 C2 Si1 H1B 0.6350 0.3837 0.4672 23 0.990 0.000 C1 C2 Si1 H2A 0.6748 0.2770 0.5750 23 0.990 0.000 C2 C3 C1 H2B 0.6448 0.3282 0.6282 23 0.990 0.000 C2 C3 C1 H4A 0.4028 0.4019 0.6079 137 0.980 0.000 C4 C3 H4A H4B 0.4421 0.3436 0.6883 137 0.980 0.000 C4 C3 H4A H4C 0.3193 0.3316 0.6571 137 0.980 0.000 C4 C3 H4A H5A 0.4152 0.3503 0.5012 137 0.980 0.000 C5 C3 H5A H5B 0.3465 0.2738 0.5518 137 0.980 0.000 C5 C3 H5A H5C 0.4847 0.2657 0.5102 137 0.980 0.000 C5 C3 H5A H6A 0.5223 0.2170 0.7100 23 0.990 0.000 C6 C7 C3 H6B 0.3988 0.2005 0.6830 23 0.990 0.000 C6 C7 C3 H14A 0.7347 0.6025 0.6836 23 0.990 0.000 C14 C15 Si2 H14B 0.6519 0.6402 0.6139 23 0.990 0.000 C14 C15 Si2 H15A 0.5499 0.5234 0.6508 23 0.990 0.000 C15 C16 C14 H15B 0.6363 0.4825 0.7182 23 0.990 0.000 C15 C16 C14 H17A 0.4443 0.4463 0.8019 137 0.980 0.000 C17 C16 H17A H17B 0.3566 0.4931 0.7360 137 0.980 0.000 C17 C16 H17A H17C 0.3369 0.5110 0.8131 137 0.980 0.000 C17 C16 H17A H18A 0.3482 0.6503 0.7345 137 0.980 0.000 C18 C16 H18A H18B 0.3826 0.6338 0.6569 137 0.980 0.000 C18 C16 H18A H18C 0.4732 0.6807 0.6810 137 0.980 0.000 C18 C16 H18A H19A 0.6102 0.6108 0.7842 23 0.990 0.000 C19 C20 C16 H19B 0.4793 0.5932 0.8357 23 0.990 0.000 C19 C20 C16 H27A 1.1907 0.3976 0.7430 23 0.990 0.000 C27 C28 Si3 H27B 1.1147 0.4756 0.7498 23 0.990 0.000 C27 C28 Si3 H28A 1.0016 0.3346 0.7831 23 0.990 0.000 C28 C27 C29 H28B 0.9302 0.4120 0.7933 23 0.990 0.000 C28 C27 C29 H30A 1.2340 0.3276 0.8619 137 0.980 0.000 C30 C29 H30A H30B 1.1608 0.2543 0.8710 137 0.980 0.000 C30 C29 H30A H30C 1.1773 0.2740 0.9440 137 0.980 0.000 C30 C29 H30A H31A 0.9744 0.4521 0.8973 137 0.980 0.000 C31 C29 H31A H31B 1.1239 0.4433 0.8785 137 0.980 0.000 C31 C29 H31A H31C 1.0600 0.3954 0.9608 137 0.980 0.000 C31 C29 H31A H32A 0.9491 0.2861 0.9823 23 0.990 0.000 C32 C33 C29 H32B 0.8547 0.3418 0.9244 23 0.990 0.000 C32 C33 C29 H40A 1.0360 0.2161 0.5603 23 0.990 0.000 C40 C41 Si4 H40B 1.1434 0.2206 0.6076 23 0.990 0.000 C40 C41 Si4 H41A 0.8835 0.2065 0.6623 23 0.990 0.000 C41 C40 C42 H41B 0.9815 0.2222 0.7092 23 0.990 0.000 C41 C40 C42 H43A 0.9230 0.0231 0.8078 137 0.980 0.000 C43 C42 H43A H43B 0.8224 0.0927 0.7681 137 0.980 0.000 C43 C42 H43A H43C 0.9194 0.1060 0.8175 137 0.980 0.000 C43 C42 H43A H44A 1.1542 0.1277 0.7519 137 0.980 0.000 C44 C42 H44A H44B 1.1923 0.0955 0.6836 137 0.980 0.000 C44 C42 H44A H44C 1.1474 0.0373 0.7663 137 0.980 0.000 C44 C42 H44A H45A 0.8880 0.0847 0.6425 23 0.990 0.000 C45 C46 C42 H45B 1.0321 0.0878 0.6076 23 0.990 0.000 C45 C46 C42 L s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.78192 0.44005 0.50518 1.00000 0.04386 0.03668 0.02698 -0.01453 0.00278 -0.00608 0.03533 0.00415 0.00029 0.00018 0.00015 0.00000 0.00218 0.00229 0.00185 0.00170 0.00166 0.00178 0.00086 Si2 0.81674 0.55474 0.58629 1.00000 0.04003 0.03663 0.02560 -0.01427 0.00530 -0.00448 0.03395 0.00416 0.00028 0.00018 0.00015 0.00000 0.00212 0.00227 0.00178 0.00173 0.00165 0.00172 0.00084 Si3 1.06801 0.45691 0.64133 1.00000 0.03898 0.03744 0.02360 -0.01136 0.00535 -0.00627 0.03378 0.00424 0.00028 0.00018 0.00015 0.00000 0.00214 0.00228 0.00175 0.00166 0.00163 0.00173 0.00083 Si4 1.03279 0.34245 0.56036 1.00000 0.04413 0.03206 0.02279 -0.00915 0.00604 -0.00707 0.03377 0.00424 0.00029 0.00018 0.00015 0.00000 0.00220 0.00220 0.00179 0.00157 0.00167 0.00167 0.00083 Cl9 0.63098 0.15194 0.45894 1.00000 0.07654 0.08287 0.06393 -0.02433 0.00669 -0.01163 0.07587 0.00488 0.00032 0.00021 0.00018 0.00000 0.00255 0.00300 0.00220 0.00214 0.00192 0.00206 0.00107 Cl10 0.73898 0.00526 0.41829 1.00000 0.06932 0.11396 0.07600 -0.05608 0.00477 -0.00875 0.08125 0.00459 0.00030 0.00022 0.00018 0.00000 0.00251 0.00341 0.00243 0.00238 0.00201 0.00220 0.00116 Cl11 0.71433 -0.16173 0.53918 1.00000 0.07401 0.08971 0.10014 -0.06207 -0.01319 0.00612 0.08071 0.00461 0.00031 0.00021 0.00019 0.00000 0.00255 0.00307 0.00272 0.00249 0.00215 0.00214 0.00114 Cl12 0.56973 -0.18022 0.69840 1.00000 0.09678 0.06532 0.07446 -0.03046 -0.02151 -0.00227 0.07632 0.00463 0.00033 0.00021 0.00018 0.00000 0.00280 0.00270 0.00236 0.00210 0.00207 0.00204 0.00106 Cl13 0.45546 -0.03071 0.73493 1.00000 0.09612 0.07149 0.05776 -0.02642 -0.00245 -0.00660 0.07472 0.00467 0.00033 0.00020 0.00017 0.00000 0.00283 0.00275 0.00219 0.00199 0.00206 0.00213 0.00107 Cl22 0.43771 0.32645 0.96566 1.00000 0.05039 0.06520 0.05053 -0.02579 -0.00793 -0.00675 0.05338 0.00395 0.00027 0.00018 0.00015 0.00000 0.00201 0.00241 0.00186 0.00174 0.00161 0.00166 0.00086 Cl23 0.55050 0.18708 1.09787 1.00000 0.06646 0.04981 0.05508 -0.01622 0.00480 -0.01339 0.05810 0.00424 0.00028 0.00018 0.00016 0.00000 0.00222 0.00235 0.00194 0.00172 0.00171 0.00176 0.00089 Cl24 0.76941 0.21152 1.17592 1.00000 0.07084 0.05588 0.04151 -0.00852 -0.00834 0.00248 0.05900 0.00436 0.00029 0.00018 0.00015 0.00000 0.00232 0.00235 0.00182 0.00169 0.00167 0.00177 0.00092 Cl25 0.87130 0.37574 1.12190 1.00000 0.05852 0.06344 0.04480 -0.02251 -0.00859 -0.00635 0.05415 0.00391 0.00027 0.00018 0.00015 0.00000 0.00218 0.00243 0.00180 0.00172 0.00163 0.00172 0.00088 Cl26 0.75498 0.51317 0.99069 1.00000 0.05864 0.04837 0.04442 -0.01513 0.00159 -0.01087 0.05093 0.00393 0.00027 0.00017 0.00014 0.00000 0.00208 0.00228 0.00180 0.00164 0.00159 0.00166 0.00084 Cl35 0.61984 0.22678 0.84164 1.00000 0.08567 0.06672 0.04906 -0.01704 -0.01434 -0.00039 0.06791 0.00451 0.00031 0.00019 0.00016 0.00000 0.00260 0.00271 0.00196 0.00188 0.00185 0.00199 0.00100 Cl36 0.53204 0.06621 0.85130 1.00000 0.08350 0.09694 0.04548 -0.02745 -0.00597 -0.02708 0.07283 0.00433 0.00031 0.00021 0.00016 0.00000 0.00262 0.00302 0.00197 0.00197 0.00185 0.00214 0.00107 Cl37 0.63587 -0.08869 0.97030 1.00000 0.09512 0.07087 0.05948 -0.03616 0.01591 -0.02886 0.07185 0.00441 0.00032 0.00020 0.00016 0.00000 0.00271 0.00268 0.00213 0.00199 0.00196 0.00208 0.00104 Cl38 0.82390 -0.08231 1.07629 1.00000 0.09358 0.05661 0.06311 -0.01615 -0.00744 -0.00215 0.07297 0.00468 0.00032 0.00019 0.00017 0.00000 0.00278 0.00257 0.00216 0.00193 0.00200 0.00202 0.00104 Cl39 0.89964 0.07713 1.06901 1.00000 0.07324 0.07779 0.05402 -0.02101 -0.01661 -0.00771 0.06778 0.00438 0.00030 0.00020 0.00016 0.00000 0.00250 0.00271 0.00203 0.00189 0.00185 0.00197 0.00101 Cl48 1.03306 -0.11614 0.55073 1.00000 0.08429 0.07547 0.04847 -0.02621 0.00190 -0.02112 0.06771 0.00436 0.00032 0.00019 0.00016 0.00000 0.00251 0.00268 0.00201 0.00190 0.00184 0.00200 0.00099 Cl49 1.05236 -0.30033 0.60995 1.00000 0.10307 0.07299 0.07834 -0.05454 -0.00956 -0.00165 0.07750 0.00453 0.00034 0.00020 0.00018 0.00000 0.00286 0.00275 0.00239 0.00221 0.00213 0.00216 0.00110 Cl50 0.92231 -0.39046 0.76948 1.00000 0.08291 0.04338 0.07758 -0.01848 -0.03126 -0.00370 0.06648 0.00422 0.00031 0.00018 0.00017 0.00000 0.00254 0.00238 0.00227 0.00188 0.00199 0.00183 0.00098 Cl51 0.78119 -0.29932 0.87008 1.00000 0.07658 0.06348 0.06211 -0.00708 0.00768 -0.02034 0.07179 0.00471 0.00031 0.00019 0.00017 0.00000 0.00249 0.00259 0.00225 0.00194 0.00195 0.00195 0.00102 Cl52 0.77714 -0.11808 0.81190 1.00000 0.07909 0.06178 0.07268 -0.03187 0.02432 -0.01439 0.07146 0.00471 0.00031 0.00019 0.00018 0.00000 0.00252 0.00254 0.00224 0.00201 0.00196 0.00193 0.00103 O1 0.75755 0.50013 0.55213 1.00000 0.03901 0.03899 0.03140 -0.01772 0.01845 -0.01417 0.03625 0.00858 0.00056 0.00037 0.00031 0.00000 0.00460 0.00500 0.00396 0.00377 0.00352 0.00367 0.00186 O2 0.93222 0.50451 0.63430 1.00000 0.04361 0.04128 0.02768 -0.01918 0.00879 -0.00680 0.03655 0.00858 0.00059 0.00037 0.00031 0.00000 0.00483 0.00499 0.00396 0.00372 0.00369 0.00387 0.00185 O3 1.06587 0.37983 0.62012 1.00000 0.04516 0.03187 0.01700 -0.00412 -0.00347 -0.00314 0.03259 0.00862 0.00057 0.00036 0.00030 0.00000 0.00467 0.00473 0.00361 0.00339 0.00331 0.00351 0.00177 O4 0.89002 0.37235 0.54015 1.00000 0.04052 0.03191 0.03140 -0.01000 0.00415 -0.01090 0.03500 0.00864 0.00059 0.00037 0.00032 0.00000 0.00480 0.00486 0.00393 0.00353 0.00362 0.00380 0.00179 O5 0.82834 0.48838 0.41833 1.00000 0.04681 0.03396 0.02802 -0.01557 0.00704 -0.00256 0.03619 0.00862 0.00058 0.00037 0.00032 0.00000 0.00473 0.00485 0.00415 0.00373 0.00372 0.00374 0.00184 O6 0.87334 0.62708 0.51694 1.00000 0.05241 0.02707 0.01682 -0.00520 0.00467 -0.00211 0.03381 0.00854 0.00058 0.00035 0.00030 0.00000 0.00483 0.00469 0.00378 0.00350 0.00356 0.00365 0.00182 O7 0.67222 0.13075 0.64705 1.00000 0.05932 0.07316 0.09482 -0.04074 -0.00708 -0.00344 0.07292 0.01260 0.00089 0.00049 0.00047 0.00000 0.00639 0.00725 0.00689 0.00561 0.00586 0.00549 0.00268 O8 0.49231 0.11588 0.61162 1.00000 0.05982 0.06332 0.07058 -0.03414 -0.01557 -0.00422 0.06076 0.01289 0.00074 0.00051 0.00042 0.00000 0.00608 0.00687 0.00588 0.00528 0.00488 0.00520 0.00234 O9 0.70577 0.46001 0.84542 1.00000 0.05106 0.08292 0.03287 -0.02185 0.00031 0.00714 0.05693 0.01079 0.00076 0.00049 0.00037 0.00000 0.00567 0.00701 0.00471 0.00464 0.00435 0.00501 0.00237 O10 0.54862 0.47479 0.93149 1.00000 0.05062 0.05848 0.02763 -0.02371 0.00395 -0.00635 0.04385 0.00909 0.00064 0.00043 0.00040 0.00000 0.00525 0.00612 0.00464 0.00453 0.00436 0.00441 0.00202 O11 0.95445 0.20261 0.87491 1.00000 0.06558 0.04093 0.03693 -0.01932 0.01492 -0.00793 0.04804 0.01029 0.00070 0.00043 0.00039 0.00000 0.00587 0.00563 0.00476 0.00426 0.00425 0.00430 0.00221 O12 0.78612 0.21218 0.95573 1.00000 0.06378 0.04271 0.03837 -0.02106 0.00450 -0.00811 0.04706 0.01118 0.00075 0.00046 0.00037 0.00000 0.00607 0.00588 0.00476 0.00429 0.00443 0.00461 0.00204 O13 1.06945 -0.06219 0.72584 1.00000 0.07569 0.04646 0.07272 -0.02224 -0.01675 -0.00736 0.06343 0.01188 0.00083 0.00049 0.00046 0.00000 0.00692 0.00661 0.00625 0.00520 0.00527 0.00501 0.00257 O14 0.90274 -0.04757 0.65999 1.00000 0.07472 0.03059 0.04912 -0.00718 -0.01258 -0.00690 0.05252 0.01161 0.00072 0.00048 0.00038 0.00000 0.00623 0.00597 0.00500 0.00453 0.00446 0.00466 0.00215 C1 0.63674 0.39618 0.51327 1.00000 0.05685 0.04450 0.03485 -0.01305 0.00744 -0.00385 0.04699 0.01462 0.00097 0.00063 0.00054 0.00000 0.00831 0.00868 0.00695 0.00670 0.00611 0.00647 0.00319 H1A 0.56491 0.43506 0.51524 1.00000 0.05639 0.00000 0.00000 H1B 0.63501 0.38369 0.46718 1.00000 0.05639 0.00000 0.00000 C2 0.61822 0.32019 0.58413 1.00000 0.03629 0.05967 0.04532 -0.01600 -0.00549 -0.00496 0.04756 0.01478 0.00095 0.00065 0.00057 0.00000 0.00791 0.00949 0.00749 0.00709 0.00640 0.00652 0.00319 H2A 0.67477 0.27699 0.57496 1.00000 0.05708 0.00000 0.00000 H2B 0.64478 0.32819 0.62815 1.00000 0.05708 0.00000 0.00000 C3 0.48412 0.29512 0.60471 1.00000 0.04737 0.04086 0.04956 -0.01123 0.01196 0.00137 0.04953 0.01752 0.00106 0.00071 0.00063 0.00000 0.00878 0.00948 0.00816 0.00754 0.00709 0.00687 0.00328 C4 0.40502 0.34775 0.64290 1.00000 0.06943 0.06805 0.04797 -0.01651 -0.00234 -0.00809 0.06309 0.01588 0.00107 0.00070 0.00059 0.00000 0.00940 0.01022 0.00770 0.00749 0.00710 0.00775 0.00372 H4A 0.40277 0.40191 0.60786 1.00000 0.09464 0.00000 0.00000 H4B 0.44210 0.34364 0.68830 1.00000 0.09464 0.00000 0.00000 H4C 0.31926 0.33159 0.65714 1.00000 0.09464 0.00000 0.00000 C5 0.42765 0.29634 0.53588 1.00000 0.08351 0.07990 0.06298 -0.02583 -0.02509 -0.02798 0.07138 0.01467 0.00112 0.00071 0.00060 0.00000 0.01025 0.01088 0.00864 0.00783 0.00779 0.00799 0.00399 H5A 0.41523 0.35030 0.50117 1.00000 0.10707 0.00000 0.00000 H5B 0.34650 0.27376 0.55184 1.00000 0.10707 0.00000 0.00000 H5C 0.48474 0.26574 0.51017 1.00000 0.10707 0.00000 0.00000 C6 0.48632 0.21468 0.66610 1.00000 0.04506 0.05308 0.08630 -0.03990 -0.00428 0.01838 0.05960 0.01709 0.00105 0.00075 0.00067 0.00000 0.00826 0.01010 0.01024 0.00935 0.00733 0.00725 0.00370 H6A 0.52235 0.21700 0.71003 1.00000 0.07152 0.00000 0.00000 H6B 0.39880 0.20051 0.68300 1.00000 0.07152 0.00000 0.00000 C7 0.56039 0.15232 0.64138 1.00000 0.05526 0.06569 0.06294 0.00171 -0.00489 -0.01914 0.06692 0.02303 0.00147 0.00085 0.00072 0.00000 0.01081 0.01196 0.00930 0.00830 0.00930 0.00959 0.00410 C8 0.55512 0.05037 0.59616 1.00000 0.06822 0.07097 0.05255 -0.04552 -0.00630 -0.00353 0.05745 0.01636 0.00118 0.00094 0.00079 0.00000 0.00991 0.01278 0.00985 0.00984 0.00803 0.00888 0.00372 C9 0.61697 0.05627 0.52668 1.00000 0.07066 0.06571 0.05217 -0.02430 -0.00493 -0.02983 0.05967 0.01629 0.00120 0.00078 0.00072 0.00000 0.00971 0.01141 0.00932 0.00857 0.00778 0.00808 0.00366 C10 0.66799 -0.00933 0.50809 1.00000 0.06561 0.08284 0.04836 -0.05088 -0.00034 -0.00037 0.05895 0.01718 0.00112 0.00099 0.00069 0.00000 0.00924 0.01259 0.00903 0.00978 0.00710 0.00854 0.00378 C11 0.65098 -0.08315 0.56284 1.00000 0.08441 0.04192 0.04624 -0.01397 -0.01181 0.00558 0.05849 0.01701 0.00123 0.00080 0.00081 0.00000 0.01060 0.01039 0.00898 0.00845 0.00810 0.00796 0.00375 C12 0.59266 -0.08868 0.63268 1.00000 0.07744 0.02005 0.05099 0.00309 -0.01529 -0.00235 0.05315 0.01704 0.00120 0.00070 0.00072 0.00000 0.00998 0.00889 0.00921 0.00747 0.00770 0.00729 0.00346 C13 0.53752 -0.02308 0.64870 1.00000 0.05200 0.03638 0.05898 0.00565 -0.00448 0.00004 0.05593 0.01829 0.00107 0.00088 0.00068 0.00000 0.00887 0.00994 0.00938 0.00838 0.00721 0.00747 0.00364 C14 0.69421 0.59079 0.64602 1.00000 0.04681 0.04366 0.03285 -0.01891 -0.00309 0.00325 0.04037 0.01403 0.00091 0.00061 0.00052 0.00000 0.00768 0.00832 0.00654 0.00611 0.00608 0.00639 0.00301 H14A 0.73465 0.60253 0.68360 1.00000 0.04844 0.00000 0.00000 H14B 0.65191 0.64021 0.61394 1.00000 0.04844 0.00000 0.00000 C15 0.59310 0.53287 0.68867 1.00000 0.02826 0.05680 0.03316 -0.02479 0.00934 0.00104 0.03865 0.01420 0.00090 0.00064 0.00054 0.00000 0.00670 0.00883 0.00641 0.00641 0.00576 0.00613 0.00296 H15A 0.54988 0.52345 0.65080 1.00000 0.04639 0.00000 0.00000 H15B 0.63628 0.48249 0.71823 1.00000 0.04639 0.00000 0.00000 C16 0.49323 0.55945 0.74246 1.00000 0.04934 0.04786 0.03734 -0.02246 0.01323 -0.02073 0.04300 0.01497 0.00105 0.00067 0.00059 0.00000 0.00803 0.00905 0.00698 0.00674 0.00670 0.00697 0.00309 C17 0.39925 0.49678 0.77644 1.00000 0.04640 0.08135 0.04162 -0.02904 0.01709 -0.01923 0.05532 0.01483 0.00096 0.00069 0.00056 0.00000 0.00795 0.01064 0.00724 0.00721 0.00628 0.00734 0.00352 H17A 0.44435 0.44629 0.80189 1.00000 0.08297 0.00000 0.00000 H17B 0.35663 0.49312 0.73599 1.00000 0.08297 0.00000 0.00000 H17C 0.33687 0.51098 0.81309 1.00000 0.08297 0.00000 0.00000 C18 0.41710 0.63855 0.69966 1.00000 0.05584 0.06876 0.03949 -0.01840 -0.00639 0.00465 0.05569 0.01566 0.00101 0.00067 0.00055 0.00000 0.00845 0.01030 0.00720 0.00712 0.00654 0.00731 0.00352 H18A 0.34816 0.65035 0.73447 1.00000 0.08353 0.00000 0.00000 H18B 0.38261 0.63378 0.65691 1.00000 0.08353 0.00000 0.00000 H18C 0.47317 0.68071 0.68100 1.00000 0.08353 0.00000 0.00000 C19 0.54775 0.57168 0.80641 1.00000 0.05189 0.04294 0.02828 -0.01123 0.00293 0.01500 0.04400 0.01539 0.00099 0.00063 0.00052 0.00000 0.00805 0.00872 0.00658 0.00644 0.00621 0.00662 0.00318 H19A 0.61022 0.61080 0.78418 1.00000 0.05280 0.00000 0.00000 H19B 0.47931 0.59320 0.83575 1.00000 0.05280 0.00000 0.00000 C20 0.60893 0.49958 0.85864 1.00000 0.04302 0.06913 0.04312 -0.03351 0.00644 -0.01740 0.04780 0.01502 0.00121 0.00077 0.00067 0.00000 0.00877 0.01120 0.00897 0.00838 0.00777 0.00796 0.00342 C21 0.60349 0.41088 0.98643 1.00000 0.04031 0.04306 0.01768 -0.00283 -0.00619 0.01457 0.03732 0.01833 0.00106 0.00076 0.00056 0.00000 0.00827 0.00967 0.00657 0.00685 0.00623 0.00715 0.00304 C22 0.55765 0.33986 1.01146 1.00000 0.03410 0.05599 0.03508 -0.02148 0.00052 0.00440 0.04141 0.01631 0.00098 0.00086 0.00065 0.00000 0.00779 0.01039 0.00750 0.00762 0.00645 0.00736 0.00312 C23 0.60495 0.27776 1.06805 1.00000 0.04278 0.04616 0.03689 -0.02858 0.00178 -0.00850 0.03818 0.01556 0.00104 0.00068 0.00062 0.00000 0.00795 0.00938 0.00711 0.00710 0.00643 0.00659 0.00297 C24 0.70054 0.28811 1.10434 1.00000 0.07217 0.05134 0.01535 -0.00875 0.00687 0.00163 0.04900 0.01972 0.00119 0.00074 0.00053 0.00000 0.00980 0.01015 0.00646 0.00666 0.00662 0.00785 0.00339 C25 0.74955 0.36031 1.08045 1.00000 0.03635 0.06013 0.03664 -0.03131 -0.00656 0.00692 0.04113 0.01561 0.00098 0.00079 0.00060 0.00000 0.00756 0.01000 0.00726 0.00738 0.00625 0.00706 0.00307 C26 0.69895 0.42228 1.02105 1.00000 0.02918 0.03481 0.02521 -0.00711 -0.01164 0.01487 0.03147 0.01539 0.00094 0.00059 0.00053 0.00000 0.00716 0.00814 0.00618 0.00597 0.00573 0.00580 0.00277 C27 1.10765 0.42807 0.73871 1.00000 0.03968 0.01646 0.04329 -0.01817 0.00264 -0.00158 0.03180 0.01297 0.00090 0.00056 0.00049 0.00000 0.00696 0.00675 0.00669 0.00566 0.00590 0.00549 0.00271 H27A 1.19074 0.39760 0.74297 1.00000 0.03815 0.00000 0.00000 H27B 1.11473 0.47564 0.74983 1.00000 0.03815 0.00000 0.00000 C28 1.01192 0.37999 0.79703 1.00000 0.04415 0.03388 0.03354 -0.00917 0.00844 -0.01420 0.03821 0.01370 0.00095 0.00059 0.00050 0.00000 0.00738 0.00784 0.00691 0.00599 0.00609 0.00608 0.00289 H28A 1.00162 0.33464 0.78306 1.00000 0.04585 0.00000 0.00000 H28B 0.93022 0.41201 0.79331 1.00000 0.04585 0.00000 0.00000 C29 1.03905 0.34906 0.88042 1.00000 0.04017 0.03763 0.01758 -0.01072 0.00182 0.00009 0.03235 0.01474 0.00099 0.00062 0.00051 0.00000 0.00765 0.00802 0.00617 0.00581 0.00577 0.00635 0.00279 C30 1.16427 0.29642 0.89023 1.00000 0.08273 0.03543 0.03373 -0.00547 -0.00790 -0.02008 0.05087 0.01434 0.00103 0.00060 0.00053 0.00000 0.00998 0.00827 0.00673 0.00594 0.00665 0.00726 0.00335 H30A 1.23398 0.32761 0.86193 1.00000 0.07630 0.00000 0.00000 H30B 1.16078 0.25429 0.87100 1.00000 0.07630 0.00000 0.00000 H30C 1.17733 0.27405 0.94396 1.00000 0.07630 0.00000 0.00000 C31 1.05032 0.41587 0.90654 1.00000 0.07349 0.06246 0.02859 -0.02094 0.00274 -0.02328 0.05261 0.01420 0.00104 0.00064 0.00052 0.00000 0.00919 0.00961 0.00657 0.00665 0.00629 0.00713 0.00342 H31A 0.97439 0.45213 0.89726 1.00000 0.07892 0.00000 0.00000 H31B 1.12392 0.44332 0.87853 1.00000 0.07892 0.00000 0.00000 H31C 1.05996 0.39543 0.96076 1.00000 0.07892 0.00000 0.00000 C32 0.93057 0.30445 0.92895 1.00000 0.05178 0.04931 0.01896 -0.00957 -0.00002 -0.00640 0.04088 0.01506 0.00100 0.00065 0.00051 0.00000 0.00816 0.00884 0.00622 0.00617 0.00608 0.00677 0.00304 H32A 0.94911 0.28608 0.98226 1.00000 0.04906 0.00000 0.00000 H32B 0.85470 0.34182 0.92444 1.00000 0.04906 0.00000 0.00000 C33 0.89828 0.23701 0.91392 1.00000 0.03896 0.05082 0.03222 -0.00948 0.00239 -0.01724 0.04145 0.01691 0.00116 0.00073 0.00065 0.00000 0.00865 0.00996 0.00773 0.00707 0.00679 0.00721 0.00319 C34 0.75454 0.13994 0.95836 1.00000 0.05475 0.05942 0.03263 -0.02539 -0.00758 -0.01863 0.04469 0.01684 0.00109 0.00084 0.00063 0.00000 0.00886 0.01121 0.00741 0.00773 0.00671 0.00774 0.00329 C35 0.67347 0.14129 0.90699 1.00000 0.08461 0.04306 0.04937 -0.02412 0.03355 -0.02113 0.05956 0.02123 0.00126 0.00075 0.00065 0.00000 0.01076 0.00994 0.00870 0.00776 0.00805 0.00814 0.00381 C36 0.63187 0.07006 0.91143 1.00000 0.04771 0.07608 0.02774 -0.01321 -0.00056 0.00156 0.05295 0.01832 0.00106 0.00092 0.00060 0.00000 0.00858 0.01165 0.00721 0.00783 0.00638 0.00806 0.00357 C37 0.67950 0.00171 0.96344 1.00000 0.05279 0.04790 0.03702 -0.03067 0.01580 -0.02383 0.04174 0.01597 0.00112 0.00072 0.00066 0.00000 0.00856 0.00967 0.00730 0.00728 0.00682 0.00709 0.00315 C38 0.76315 0.00208 1.01157 1.00000 0.06949 0.02607 0.03875 0.00159 0.00654 0.01021 0.05110 0.02220 0.00117 0.00073 0.00061 0.00000 0.00974 0.00899 0.00754 0.00660 0.00700 0.00697 0.00333 C39 0.79998 0.07319 1.00894 1.00000 0.05677 0.05172 0.03411 -0.02136 0.01031 0.00186 0.04799 0.01751 0.00106 0.00087 0.00064 0.00000 0.00905 0.01044 0.00765 0.00775 0.00669 0.00780 0.00334 C40 1.05393 0.23634 0.59891 1.00000 0.04554 0.05000 0.04891 -0.03677 -0.00703 -0.00703 0.04218 0.01328 0.00097 0.00060 0.00056 0.00000 0.00742 0.00875 0.00752 0.00677 0.00648 0.00628 0.00309 H40A 1.03602 0.21609 0.56030 1.00000 0.05062 0.00000 0.00000 H40B 1.14338 0.22056 0.60763 1.00000 0.05062 0.00000 0.00000 C41 0.97262 0.19681 0.67281 1.00000 0.04317 0.04632 0.03681 -0.02028 0.00219 -0.00268 0.04129 0.01450 0.00096 0.00065 0.00054 0.00000 0.00752 0.00910 0.00716 0.00663 0.00628 0.00631 0.00301 H41A 0.88350 0.20648 0.66233 1.00000 0.04955 0.00000 0.00000 H41B 0.98146 0.22222 0.70923 1.00000 0.04955 0.00000 0.00000 C42 1.00328 0.10713 0.71132 1.00000 0.05670 0.04778 0.03582 -0.02461 0.00975 -0.00660 0.04531 0.01570 0.00111 0.00069 0.00058 0.00000 0.00903 0.00955 0.00728 0.00680 0.00689 0.00692 0.00317 C43 0.90832 0.07972 0.78274 1.00000 0.06813 0.04824 0.03057 -0.01684 0.01473 -0.00866 0.04988 0.01482 0.00099 0.00062 0.00052 0.00000 0.00887 0.00881 0.00677 0.00629 0.00669 0.00679 0.00335 H43A 0.92304 0.02314 0.80782 1.00000 0.07482 0.00000 0.00000 H43B 0.82244 0.09270 0.76813 1.00000 0.07482 0.00000 0.00000 H43C 0.91936 0.10596 0.81751 1.00000 0.07482 0.00000 0.00000 C44 1.13555 0.09049 0.72985 1.00000 0.05301 0.04590 0.03991 -0.01278 -0.00333 -0.00075 0.04742 0.01516 0.00100 0.00063 0.00054 0.00000 0.00882 0.00865 0.00694 0.00623 0.00642 0.00648 0.00317 H44A 1.15421 0.12771 0.75187 1.00000 0.07112 0.00000 0.00000 H44B 1.19229 0.09547 0.68363 1.00000 0.07112 0.00000 0.00000 H44C 1.14744 0.03731 0.76626 1.00000 0.07112 0.00000 0.00000 C45 0.97575 0.06863 0.65500 1.00000 0.05561 0.04790 0.02451 -0.01752 0.00332 -0.01094 0.04148 0.01432 0.00102 0.00070 0.00053 0.00000 0.00813 0.00941 0.00629 0.00644 0.00569 0.00653 0.00303 H45A 0.88800 0.08468 0.64250 1.00000 0.04978 0.00000 0.00000 H45B 1.03215 0.08783 0.60756 1.00000 0.04978 0.00000 0.00000 C46 0.99425 -0.01846 0.68681 1.00000 0.06663 0.05955 0.04199 -0.03448 0.00528 -0.01929 0.05118 0.01826 0.00130 0.00087 0.00067 0.00000 0.01099 0.01243 0.00834 0.00847 0.00743 0.00874 0.00364 C47 0.90966 -0.12897 0.68689 1.00000 0.04701 0.05198 0.04556 -0.02676 0.00001 0.00058 0.04645 0.01638 0.00105 0.00082 0.00071 0.00000 0.00828 0.01089 0.00874 0.00870 0.00699 0.00737 0.00325 C48 0.96791 -0.16916 0.63884 1.00000 0.04602 0.05017 0.03322 -0.00623 0.00573 -0.02890 0.04414 0.01534 0.00099 0.00077 0.00057 0.00000 0.00796 0.00999 0.00741 0.00743 0.00627 0.00696 0.00318 C49 0.97333 -0.25048 0.66713 1.00000 0.08008 0.02750 0.04664 -0.01674 -0.00018 -0.02254 0.04931 0.01468 0.00109 0.00075 0.00068 0.00000 0.00993 0.00900 0.00866 0.00739 0.00731 0.00725 0.00334 C50 0.91707 -0.28985 0.73839 1.00000 0.05488 0.02421 0.04730 0.00988 -0.03284 -0.00997 0.04490 0.01484 0.00113 0.00063 0.00073 0.00000 0.00849 0.00849 0.00839 0.00732 0.00719 0.00668 0.00325 C51 0.85637 -0.25114 0.78504 1.00000 0.05310 0.04811 0.04428 -0.01923 -0.01578 0.00255 0.04719 0.01699 0.00108 0.00083 0.00062 0.00000 0.00848 0.01050 0.00843 0.00814 0.00693 0.00733 0.00331 C52 0.85260 -0.17092 0.75770 1.00000 0.04402 0.04312 0.03904 -0.01832 0.01544 -0.00780 0.04266 0.01568 0.00099 0.00079 0.00067 0.00000 0.00779 0.00990 0.00803 0.00746 0.00649 0.00682 0.00308 Final Structure Factor Calculation for L s92 in P-1 Total number of l.s. parameters = 819 Maximum vector length = 511 Memory required = 7941 / 24017 wR2 = 0.1680 before cycle 9 for 12068 data and 0 / 819 parameters GooF = S = 0.859; Restrained GooF = 0.859 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0320 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0794 for 3235 Fo > 4sig(Fo) and 0.3570 for all 12068 data wR2 = 0.1680, GooF = S = 0.859, Restrained GooF = 0.859 for all data Occupancy sum of asymmetric unit = 90.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0470 0.0356 0.0234 Si1 0.0452 0.0363 0.0204 Si2 0.0439 0.0372 0.0203 Si3 0.0489 0.0324 0.0200 Si4 0.0873 0.0842 0.0562 Cl9 0.1191 0.0747 0.0499 Cl10 0.1188 0.0736 0.0497 Cl11 0.1017 0.0699 0.0573 Cl12 0.0981 0.0716 0.0545 Cl13 0.0657 0.0523 0.0421 Cl22 0.0746 0.0555 0.0442 Cl23 0.0777 0.0605 0.0388 Cl24 0.0636 0.0588 0.0401 Cl25 0.0627 0.0486 0.0415 Cl26 0.0882 0.0688 0.0468 Cl35 0.1095 0.0681 0.0408 Cl36 0.1154 0.0567 0.0435 Cl37 0.0957 0.0681 0.0551 Cl38 0.0813 0.0745 0.0475 Cl39 0.0943 0.0640 0.0449 Cl48 0.1053 0.0951 0.0322 Cl49 0.1021 0.0547 0.0427 Cl50 0.0891 0.0836 0.0427 Cl51 0.1121 0.0578 0.0445 Cl52 0.0612 0.0328 0.0147 O1 0.0525 0.0391 0.0181 O2 0.0454 0.0356 0.0167 O3 0.0466 0.0333 0.0250 O4 0.0538 0.0348 0.0200 O5 0.0571 0.0286 0.0157 O6 0.0968 0.0631 0.0588 O7 0.0780 0.0601 0.0442 O8 0.0920 0.0499 0.0289 O9 0.0595 0.0522 0.0198 O10 0.0787 0.0403 0.0250 O11 0.0683 0.0435 0.0294 O12 0.0830 0.0641 0.0432 O13 0.0760 0.0517 0.0299 O14 0.0658 0.0448 0.0303 C1 0.0616 0.0454 0.0357 C2 0.0765 0.0400 0.0320 C3 0.0711 0.0705 0.0476 C4 0.1078 0.0715 0.0348 C5 0.0886 0.0689 0.0213 C6 0.1021 0.0587 0.0399 C7 0.0814 0.0682 0.0227 C8 0.0903 0.0531 0.0355 C9 0.0916 0.0677 0.0176 C10 0.0884 0.0474 0.0397 C11 0.0795 0.0625 0.0174 C12 0.0878 0.0519 0.0281 C13 0.0535 0.0406 0.0270 C14 0.0581 0.0438 0.0140 C15 0.0702 0.0326 0.0262 C16 0.0863 0.0558 0.0239 C17 0.0773 0.0512 0.0386 C18 0.0766 0.0322 0.0232 C19 0.0769 0.0370 0.0295 C20 0.0677 0.0291 0.0152 C21 0.0598 0.0392 0.0252 C22 0.0558 0.0397 0.0191 C23 0.0829 0.0504 0.0137 C24 0.0673 0.0342 0.0219 C25 0.0525 0.0296 0.0123 C26 0.0495 0.0359 0.0100 C27 0.0542 0.0378 0.0226 C28 0.0457 0.0356 0.0157 C29 0.0864 0.0380 0.0282 C30 0.0851 0.0482 0.0245 C31 0.0528 0.0513 0.0186 C32 0.0596 0.0387 0.0260 C33 0.0698 0.0466 0.0177 C34 0.1159 0.0368 0.0259 C35 0.0844 0.0473 0.0271 C36 0.0784 0.0296 0.0172 C37 0.0925 0.0403 0.0205 C38 0.0704 0.0517 0.0219 C39 0.0639 0.0463 0.0164 C40 0.0482 0.0466 0.0290 C41 0.0660 0.0476 0.0223 C42 0.0794 0.0478 0.0225 C43 0.0570 0.0456 0.0397 C44 0.0601 0.0439 0.0205 C45 0.0813 0.0500 0.0223 C46 0.0567 0.0513 0.0313 C47 0.0718 0.0423 0.0184 C48 0.0849 0.0461 0.0169 C49 0.0905 0.0297 0.0145 C50 0.0615 0.0448 0.0352 C51 0.0638 0.0415 0.0226 C52 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.022 0.032 0.042 0.055 0.072 0.099 0.151 1.000 Number in group 1208. 1219. 1194. 1308. 1143. 1225. 1168. 1208. 1183. 1212. GooF 0.749 0.762 0.766 0.767 0.788 0.857 0.869 0.943 1.002 1.038 K 29.484 4.620 2.547 1.551 1.364 1.169 0.952 0.985 0.971 1.015 Resolution(A) 0.77 0.84 0.89 0.93 0.99 1.05 1.14 1.25 1.42 1.76 inf Number in group 1226. 1225. 1188. 1212. 1192. 1218. 1182. 1220. 1194. 1211. GooF 0.726 0.748 0.804 0.788 0.864 0.910 0.897 0.936 0.903 0.983 K 1.740 1.527 1.414 1.178 1.095 0.973 1.001 0.974 1.013 1.008 R1 0.764 0.693 0.636 0.582 0.472 0.383 0.249 0.180 0.121 0.061 Recommended weighting scheme: WGHT 0.0319 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) -3 9 17 1584.99 240.57 5.14 0.047 1.00 0 1 5 8921.67 10550.65 4.92 0.309 3.73 0 -11 6 555.80 1969.68 4.65 0.134 1.21 0 2 5 5197.05 6152.02 4.43 0.236 3.77 -7 -3 16 3121.26 59.47 4.14 0.023 0.82 4 -1 8 2126.66 2841.65 4.04 0.160 1.72 9 11 1 2317.76 749.71 3.98 0.082 1.00 7 -6 14 1768.71 397.23 3.94 0.060 0.87 3 0 2 1768.03 3235.60 3.93 0.171 3.41 -6 13 12 3121.26 263.87 3.86 0.049 0.93 -7 6 4 -176.66 531.18 3.72 0.069 1.27 8 11 4 955.06 106.41 3.68 0.031 1.11 3 8 16 0.00 670.41 3.66 0.078 1.16 5 -4 3 17837.65 15199.06 3.65 0.371 1.73 -4 15 7 4882.49 3491.46 3.62 0.178 1.05 2 -1 3 6181.39 5396.09 3.53 0.221 3.79 6 6 17 -281.26 532.36 3.49 0.069 1.01 4 12 9 1326.61 1960.63 3.41 0.133 1.34 -3 2 11 779.46 148.86 3.41 0.037 1.46 0 3 6 6060.56 6843.04 3.40 0.249 3.10 -2 11 2 668.96 47.94 3.36 0.021 1.52 3 2 5 7541.35 8484.64 3.36 0.277 2.80 4 -6 18 2645.25 196.31 3.35 0.042 0.82 3 2 2 4344.17 5095.82 3.34 0.215 3.44 -2 9 7 0.00 612.90 3.34 0.075 1.68 1 4 6 4602.56 5309.44 3.33 0.219 2.98 -2 16 4 445.41 1549.22 3.33 0.118 1.08 9 9 1 -279.55 491.76 3.32 0.067 1.06 2 3 2 2376.50 1653.37 3.32 0.122 4.27 0 4 7 10697.47 12210.06 3.24 0.333 2.61 10 -1 1 534.47 0.21 3.23 0.001 1.06 3 7 18 793.43 8.68 3.22 0.009 1.05 -11 -1 1 882.32 47.75 3.22 0.021 0.96 1 1 6 4969.59 5609.80 3.22 0.225 3.07 -6 10 12 -445.41 740.03 3.21 0.082 1.01 -8 -8 2 -110.39 843.59 3.20 0.087 1.12 2 -6 1 3526.83 2880.39 3.20 0.162 2.33 -2 -2 4 1589.67 2202.03 3.19 0.141 2.84 4 5 16 635.72 71.72 3.18 0.025 1.14 4 8 17 881.71 300.31 3.18 0.052 1.08 9 -11 2 2658.85 319.62 3.18 0.054 0.89 2 -10 2 1896.99 2966.13 3.17 0.164 1.49 -4 -9 4 13463.45 9611.34 3.16 0.295 1.37 2 2 3 4931.51 3953.89 3.15 0.189 4.33 -2 0 19 1966.73 31.67 3.14 0.017 0.90 10 3 1 738.32 14.10 3.13 0.011 1.07 -3 -6 2 6184.19 4275.08 3.12 0.197 2.08 7 8 6 1801.42 2622.44 3.12 0.154 1.34 2 15 12 223.13 1152.51 3.08 0.102 1.13 6 -7 1 -89.08 419.55 3.08 0.062 1.36 Bond lengths and angles Si1 - Distance Angles O5 1.6119 (0.0064) O4 1.6121 (0.0069) 108.98 (0.34) O1 1.6366 (0.0063) 108.40 (0.35) 109.76 (0.34) C1 1.8191 (0.0105) 111.58 (0.39) 109.25 (0.44) 108.84 (0.41) Si1 - O5 O4 O1 Si2 - Distance Angles O6 1.6149 (0.0065) O1 1.6181 (0.0064) 108.68 (0.31) O2 1.6300 (0.0069) 107.97 (0.34) 109.11 (0.36) C14 1.8356 (0.0092) 110.12 (0.42) 109.77 (0.41) 111.13 (0.38) Si2 - O6 O1 O2 Si3 - Distance Angles O2 1.6013 (0.0067) O3 1.6184 (0.0065) 109.43 (0.35) O5_$1 1.6320 (0.0068) 109.12 (0.36) 108.54 (0.32) C27 1.8357 (0.0090) 109.33 (0.38) 109.60 (0.38) 110.81 (0.41) Si3 - O2 O3 O5_$1 Si4 - Distance Angles O4 1.6173 (0.0068) O6_$1 1.6229 (0.0064) 108.28 (0.32) O3 1.6307 (0.0063) 109.16 (0.34) 108.92 (0.34) C40 1.8208 (0.0105) 110.95 (0.41) 108.65 (0.41) 110.83 (0.38) Si4 - O4 O6_$1 O3 Cl9 - Distance Angles C9 1.7806 (0.0126) Cl9 - Cl10 - Distance Angles C10 1.7131 (0.0118) Cl10 - Cl11 - Distance Angles C11 1.7026 (0.0124) Cl11 - Cl12 - Distance Angles C12 1.7243 (0.0116) Cl12 - Cl13 - Distance Angles C13 1.7186 (0.0124) Cl13 - Cl22 - Distance Angles C22 1.7516 (0.0109) Cl22 - Cl23 - Distance Angles C23 1.7163 (0.0113) Cl23 - Cl24 - Distance Angles C24 1.7403 (0.0110) Cl24 - Cl25 - Distance Angles C25 1.7306 (0.0105) Cl25 - Cl26 - Distance Angles C26 1.7264 (0.0107) Cl26 - Cl35 - Distance Angles C35 1.7081 (0.0129) Cl35 - Cl36 - Distance Angles C36 1.7083 (0.0112) Cl36 - Cl37 - Distance Angles C37 1.7487 (0.0109) Cl37 - Cl38 - Distance Angles C38 1.7168 (0.0112) Cl38 - Cl39 - Distance Angles C39 1.7066 (0.0116) Cl39 - Cl48 - Distance Angles C48 1.7103 (0.0105) Cl48 - Cl49 - Distance Angles C49 1.7366 (0.0111) Cl49 - Cl50 - Distance Angles C50 1.7285 (0.0109) Cl50 - Cl51 - Distance Angles C51 1.6867 (0.0120) Cl51 - Cl52 - Distance Angles C52 1.7207 (0.0107) Cl52 - O1 - Distance Angles Si2 1.6181 (0.0064) Si1 1.6366 (0.0063) 147.86 (0.42) O1 - Si2 O2 - Distance Angles Si3 1.6013 (0.0067) Si2 1.6300 (0.0068) 152.57 (0.39) O2 - Si3 O3 - Distance Angles Si3 1.6184 (0.0065) Si4 1.6307 (0.0062) 147.96 (0.41) O3 - Si3 O4 - Distance Angles Si1 1.6121 (0.0069) Si4 1.6173 (0.0068) 152.18 (0.45) O4 - Si1 O5 - Distance Angles Si1 1.6119 (0.0064) Si3_$1 1.6320 (0.0067) 147.57 (0.42) O5 - Si1 O6 - Distance Angles Si2 1.6149 (0.0064) Si4_$1 1.6229 (0.0063) 148.61 (0.42) O6 - Si2 O7 - Distance Angles C7 1.2264 (0.0136) O7 - O8 - Distance Angles C7 1.3580 (0.0141) C8 1.4116 (0.0133) 115.95 (1.01) O8 - C7 O9 - Distance Angles C20 1.2421 (0.0121) O9 - O10 - Distance Angles C20 1.3857 (0.0116) C21 1.3917 (0.0114) 118.80 (0.86) O10 - C20 O11 - Distance Angles C33 1.1978 (0.0117) O11 - O12 - Distance Angles C33 1.3832 (0.0121) C34 1.4019 (0.0127) 116.21 (0.86) O12 - C33 O13 - Distance Angles C46 1.1951 (0.0132) O13 - O14 - Distance Angles C47 1.3961 (0.0127) C46 1.4184 (0.0128) 112.69 (0.89) O14 - C47 C1 - Distance Angles C2 1.5671 (0.0132) Si1 1.8191 (0.0105) 114.56 (0.70) H1A 0.9900 108.62 108.62 H1B 0.9900 108.62 108.62 107.58 C1 - C2 Si1 H1A C2 - Distance Angles C3 1.5305 (0.0133) C1 1.5671 (0.0132) 115.44 (0.88) H2A 0.9900 108.42 108.42 H2B 0.9900 108.42 108.42 107.47 C2 - C3 C1 H2A C3 - Distance Angles C5 1.5175 (0.0131) C6 1.5212 (0.0141) 111.75 (1.00) C4 1.5221 (0.0133) 111.76 (0.96) 104.00 (0.92) C2 1.5305 (0.0133) 111.53 (0.92) 108.67 (0.94) 108.80 (0.96) C3 - C5 C6 C4 C4 - Distance Angles C3 1.5221 (0.0134) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C3 H4A H4B C5 - Distance Angles C3 1.5175 (0.0131) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C3 H5A H5B C6 - Distance Angles C7 1.4923 (0.0164) C3 1.5212 (0.0141) 113.74 (1.01) H6A 0.9900 108.81 108.81 H6B 0.9900 108.81 108.81 107.68 C6 - C7 C3 H6A C7 - Distance Angles O7 1.2264 (0.0136) O8 1.3580 (0.0141) 118.83 (1.41) C6 1.4923 (0.0164) 126.84 (1.36) 114.30 (1.23) C7 - O7 O8 C8 - Distance Angles C9 1.3684 (0.0147) C13 1.3808 (0.0155) 118.48 (1.26) O8 1.4116 (0.0133) 122.07 (1.39) 118.70 (1.20) C8 - C9 C13 C9 - Distance Angles C8 1.3684 (0.0147) C10 1.4050 (0.0156) 122.56 (1.25) Cl9 1.7806 (0.0126) 117.12 (1.19) 120.32 (1.13) C9 - C8 C10 C10 - Distance Angles C11 1.4000 (0.0155) C9 1.4050 (0.0156) 117.82 (1.06) Cl10 1.7131 (0.0118) 123.73 (1.12) 118.33 (1.24) C10 - C11 C9 C11 - Distance Angles C12 1.3630 (0.0144) C10 1.4000 (0.0155) 119.33 (1.10) Cl11 1.7026 (0.0123) 123.58 (1.16) 116.97 (1.10) C11 - C12 C10 C12 - Distance Angles C11 1.3630 (0.0145) C13 1.3924 (0.0148) 121.67 (1.10) Cl12 1.7243 (0.0116) 118.41 (1.11) 119.39 (1.11) C12 - C11 C13 C13 - Distance Angles C8 1.3808 (0.0156) C12 1.3924 (0.0148) 119.65 (1.16) Cl13 1.7186 (0.0124) 118.62 (1.10) 121.61 (1.11) C13 - C8 C12 C14 - Distance Angles C15 1.5547 (0.0129) Si2 1.8356 (0.0092) 114.14 (0.67) H14A 0.9900 108.72 108.72 H14B 0.9900 108.72 108.72 107.63 C14 - C15 Si2 H14A C15 - Distance Angles C16 1.5361 (0.0124) C14 1.5547 (0.0129) 115.41 (0.83) H15A 0.9900 108.42 108.42 H15B 0.9900 108.42 108.42 107.47 C15 - C16 C14 H15A C16 - Distance Angles C19 1.5259 (0.0126) C15 1.5361 (0.0124) 113.49 (0.89) C17 1.5377 (0.0134) 109.18 (0.86) 107.79 (0.84) C18 1.5758 (0.0142) 106.79 (0.84) 111.94 (0.85) 107.48 (0.94) C16 - C19 C15 C17 C17 - Distance Angles C16 1.5377 (0.0134) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C16 H17A H17B C18 - Distance Angles C16 1.5758 (0.0142) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C16 H18A H18B C19 - Distance Angles C20 1.4813 (0.0143) C16 1.5259 (0.0126) 113.81 (0.92) H19A 0.9900 108.80 108.80 H19B 0.9900 108.80 108.80 107.67 C19 - C20 C16 H19A C20 - Distance Angles O9 1.2421 (0.0121) O10 1.3857 (0.0116) 117.29 (1.10) C19 1.4813 (0.0143) 128.50 (1.08) 114.21 (1.04) C20 - O9 O10 C21 - Distance Angles C22 1.3571 (0.0145) C26 1.3770 (0.0130) 119.40 (0.98) O10 1.3917 (0.0114) 121.68 (1.11) 118.63 (1.13) C21 - C22 C26 C22 - Distance Angles C21 1.3571 (0.0145) C23 1.3587 (0.0140) 122.80 (1.06) Cl22 1.7516 (0.0108) 118.53 (0.99) 118.59 (1.07) C22 - C21 C23 C23 - Distance Angles C22 1.3587 (0.0140) C24 1.3908 (0.0138) 118.75 (1.07) Cl23 1.7163 (0.0113) 122.93 (0.98) 118.31 (0.99) C23 - C22 C24 C24 - Distance Angles C23 1.3908 (0.0138) C25 1.3932 (0.0144) 120.01 (0.99) Cl24 1.7403 (0.0110) 122.02 (1.06) 117.84 (0.99) C24 - C23 C25 C25 - Distance Angles C24 1.3932 (0.0144) C26 1.4010 (0.0137) 119.08 (0.98) Cl25 1.7306 (0.0105) 121.96 (0.96) 118.97 (1.01) C25 - C24 C26 C26 - Distance Angles C21 1.3770 (0.0130) C25 1.4010 (0.0137) 119.89 (1.04) Cl26 1.7264 (0.0107) 119.47 (0.84) 120.64 (0.89) C26 - C21 C25 C27 - Distance Angles C28 1.5123 (0.0119) Si3 1.8357 (0.0090) 113.31 (0.66) H27A 0.9900 108.91 108.91 H27B 0.9900 108.91 108.91 107.74 C27 - C28 Si3 H27A C28 - Distance Angles C27 1.5123 (0.0119) C29 1.5408 (0.0119) 117.75 (0.85) H28A 0.9900 107.87 107.87 H28B 0.9900 107.87 107.87 107.18 C28 - C27 C29 H28A C29 - Distance Angles C31 1.5129 (0.0126) C32 1.5147 (0.0131) 107.92 (0.80) C28 1.5408 (0.0119) 110.63 (0.85) 109.00 (0.85) C30 1.5477 (0.0130) 108.09 (0.87) 110.91 (0.88) 110.27 (0.78) C29 - C31 C32 C28 C30 - Distance Angles C29 1.5477 (0.0130) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C29 H30A H30B C31 - Distance Angles C29 1.5129 (0.0126) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C29 H31A H31B C32 - Distance Angles C33 1.4690 (0.0142) C29 1.5147 (0.0132) 118.71 (0.91) H32A 0.9900 107.64 107.64 H32B 0.9900 107.64 107.64 107.06 C32 - C33 C29 H32A C33 - Distance Angles O11 1.1978 (0.0117) O12 1.3832 (0.0120) 120.06 (1.08) C32 1.4690 (0.0142) 130.28 (1.13) 109.62 (1.08) C33 - O11 O12 C34 - Distance Angles C39 1.3427 (0.0144) C35 1.3965 (0.0143) 122.39 (1.19) O12 1.4019 (0.0126) 120.68 (1.06) 116.93 (1.16) C34 - C39 C35 C35 - Distance Angles C34 1.3965 (0.0143) C36 1.4154 (0.0154) 118.72 (1.15) Cl35 1.7081 (0.0129) 121.56 (1.06) 119.69 (1.11) C35 - C34 C36 C36 - Distance Angles C37 1.3810 (0.0146) C35 1.4154 (0.0154) 118.35 (1.09) Cl36 1.7083 (0.0112) 119.61 (1.14) 121.94 (1.11) C36 - C37 C35 C37 - Distance Angles C36 1.3810 (0.0146) C38 1.3797 (0.0141) 121.47 (1.05) Cl37 1.7487 (0.0109) 120.92 (1.04) 117.62 (1.07) C37 - C36 C38 C38 - Distance Angles C37 1.3797 (0.0141) C39 1.4036 (0.0151) 119.83 (1.02) Cl38 1.7168 (0.0112) 122.14 (1.12) 118.03 (1.10) C38 - C37 C39 C39 - Distance Angles C34 1.3427 (0.0144) C38 1.4036 (0.0151) 119.12 (1.13) Cl39 1.7066 (0.0115) 119.15 (1.07) 121.73 (1.09) C39 - C34 C38 C40 - Distance Angles C41 1.5346 (0.0125) Si4 1.8208 (0.0105) 116.10 (0.70) H40A 0.9900 108.26 108.26 H40B 0.9900 108.26 108.26 107.38 C40 - C41 Si4 H40A C41 - Distance Angles C40 1.5346 (0.0125) C42 1.5596 (0.0136) 115.96 (0.83) H41A 0.9900 108.29 108.29 H41B 0.9900 108.29 108.29 107.40 C41 - C40 C42 H41A C42 - Distance Angles C44 1.4850 (0.0128) C43 1.5478 (0.0127) 112.14 (0.86) C41 1.5596 (0.0136) 109.85 (0.90) 107.01 (0.85) C45 1.5657 (0.0126) 113.21 (0.88) 107.71 (0.87) 106.59 (0.87) C42 - C44 C43 C41 C43 - Distance Angles C42 1.5478 (0.0127) H43A 0.9800 109.47 H43B 0.9800 109.47 109.47 H43C 0.9800 109.47 109.47 109.47 C43 - C42 H43A H43B C44 - Distance Angles C42 1.4850 (0.0128) H44A 0.9800 109.47 H44B 0.9800 109.47 109.47 H44C 0.9800 109.47 109.47 109.47 C44 - C42 H44A H44B C45 - Distance Angles C46 1.4951 (0.0157) C42 1.5657 (0.0126) 112.35 (0.89) H45A 0.9900 109.13 109.13 H45B 0.9900 109.13 109.13 107.86 C45 - C46 C42 H45A C46 - Distance Angles O13 1.1951 (0.0132) O14 1.4184 (0.0128) 120.55 (1.27) C45 1.4951 (0.0157) 132.06 (1.20) 107.36 (1.13) C46 - O13 O14 C47 - Distance Angles C52 1.3895 (0.0138) O14 1.3961 (0.0127) 121.53 (1.08) C48 1.4104 (0.0135) 119.20 (1.16) 119.10 (1.13) C47 - C52 O14 C48 - Distance Angles C49 1.3952 (0.0140) C47 1.4104 (0.0135) 117.90 (1.04) Cl48 1.7103 (0.0105) 123.59 (1.01) 118.46 (1.02) C48 - C49 C47 C49 - Distance Angles C50 1.3806 (0.0138) C48 1.3952 (0.0140) 120.79 (1.03) Cl49 1.7366 (0.0111) 121.21 (1.03) 118.00 (1.00) C49 - C50 C48 C50 - Distance Angles C51 1.3786 (0.0139) C49 1.3806 (0.0139) 121.85 (1.06) Cl50 1.7285 (0.0109) 119.27 (1.06) 118.89 (1.07) C50 - C51 C49 C51 - Distance Angles C52 1.3774 (0.0141) C50 1.3786 (0.0139) 117.47 (1.08) Cl51 1.6867 (0.0120) 120.91 (1.05) 121.50 (1.10) C51 - C52 C50 C52 - Distance Angles C51 1.3774 (0.0141) C47 1.3895 (0.0139) 122.64 (1.06) Cl52 1.7207 (0.0107) 120.42 (1.02) 116.93 (1.01) C52 - C51 C47 FMAP and GRID set by program FMAP 2 2 91 GRID -1.136 -1 -2 1.136 1 2 R1 = 0.3559 for 12068 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.8951 0.9001 0.4119 [ 0.84 A from H45B ] Deepest hole -0.44 at 0.1245 0.4748 0.4612 [ 1.27 A from SI2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 7269 /100751 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1049 0.0999 0.5881 1.00000 0.05 0.40 0.84 H45B 1.75 C45 2.07 H40A 2.14 H44B Q2 1 0.5293 0.5225 0.9705 1.00000 0.05 0.39 1.33 O10 1.95 O10 2.04 C21 2.04 C21 Q3 1 0.8480 0.0237 0.5472 1.00000 0.05 0.37 2.20 O14 2.37 CL48 2.40 C10 2.54 C9 Q4 1 0.9254 -0.1922 0.5396 1.00000 0.05 0.37 2.02 CL48 2.08 H40A 2.21 C48 2.27 CL11 Q5 1 0.7419 0.0223 0.5710 1.00000 0.05 0.36 1.63 C9 1.82 C10 2.05 C8 2.36 C11 Q6 1 0.7017 0.2737 0.8193 1.00000 0.05 0.35 1.24 CL35 2.44 C35 2.68 O12 2.84 C33 Q7 1 0.4217 0.4404 0.7489 1.00000 0.05 0.35 1.09 H17B 1.12 H17A 1.31 C17 2.13 H17C Q8 1 1.1262 -0.1424 0.5795 1.00000 0.05 0.35 1.18 CL48 1.92 C48 2.62 CL9 2.68 C49 Q9 1 0.5570 0.1927 0.7555 1.00000 0.05 0.35 0.93 H6A 1.86 C6 2.18 CL35 2.31 H6B Q10 1 0.9425 0.6222 0.5304 1.00000 0.05 0.35 0.81 O6 1.61 SI4 1.90 SI2 2.08 O4 Shortest distances between peaks (including symmetry equivalents) 3 5 1.17 2 2 1.27 1 4 2.45 3 8 2.62 4 8 2.76 6 9 2.94 Time profile in seconds ----------------------- 0.13: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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 0.02: Analyse other restraints etc. 2.09: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.02: Generate idealized H-atoms 18.13: Structure factors and derivatives 123.70: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 13.06: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.13: Merge reflections for Fourier and .fcf 0.33: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:02:57 Total CPU time: 158.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++