+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:17:56 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT013 in Cc CELL 0.71073 25.5294 18.9718 9.7130 90 103.111 90 ZERR 8 0.0005 0.0005 0.0002 0 0.002 0 LATT -7 SYMM X, -Y, 1/2+Z SFAC C H N O UNIT 208 248 24 16 V = 4581.75 F(000) = 1792.0 Mu = 0.08 mm-1 Cell Wt = 3340.30 Rho = 1.211 FMAP 2 PLAN 5 TEMP -153 L.S. 4 FVAR 0.20215 C1 1 0.122869 1.510137 0.101941 11.00000 0.03444 0.05101 = 0.13147 0.00520 0.01582 0.00137 AFIX 33 H1A 2 0.106953 1.525965 0.179424 11.00000 -1.50000 H1B 2 0.094489 1.492148 0.024461 11.00000 -1.50000 H1C 2 0.141049 1.549826 0.068006 11.00000 -1.50000 AFIX 0 C2 1 0.163267 1.452087 0.154427 11.00000 0.04846 0.02554 = 0.08020 0.00690 0.02630 0.00168 AFIX 23 H2A 2 0.191072 1.470086 0.234932 11.00000 -1.20000 H2B 2 0.144704 1.412349 0.189250 11.00000 -1.20000 AFIX 0 C3 1 0.189909 1.425776 0.042818 11.00000 0.05672 0.03166 = 0.06016 0.00598 0.01657 -0.00999 AFIX 23 H3A 2 0.207645 1.466003 0.006979 11.00000 -1.20000 H3B 2 0.161887 1.407535 -0.036927 11.00000 -1.20000 AFIX 0 C4 1 0.230877 1.369017 0.089933 11.00000 0.04266 0.02329 = 0.07836 0.00507 0.03230 -0.01037 AFIX 23 H4A 2 0.248637 1.358000 0.011872 11.00000 -1.20000 H4B 2 0.258762 1.386566 0.170734 11.00000 -1.20000 AFIX 0 C5 1 0.218336 1.239401 0.093187 11.00000 0.02538 0.02073 = 0.02735 0.00141 0.01173 0.00166 C6 1 0.186202 1.182496 0.132736 11.00000 0.02956 0.01945 = 0.01697 -0.00164 0.00635 0.00348 C7 1 0.164126 1.069658 0.151761 11.00000 0.02726 0.02579 = 0.01765 -0.00587 0.00613 0.00291 C8 1 0.168793 0.991674 0.136751 11.00000 0.01876 0.01758 = 0.02786 0.00056 0.00601 0.00309 C9 1 0.157797 0.877352 0.243828 11.00000 0.06544 0.01802 = 0.03239 0.00523 0.02590 0.00465 AFIX 23 H9A 2 0.185524 0.857655 0.322572 11.00000 -1.20000 H9B 2 0.165227 0.859699 0.154248 11.00000 -1.20000 AFIX 0 C10 1 0.102668 0.851074 0.256583 11.00000 0.05633 0.02294 = 0.04513 0.00645 -0.00879 -0.00627 AFIX 23 H10A 2 0.076030 0.885422 0.205512 11.00000 -1.20000 H10B 2 0.101845 0.854679 0.357752 11.00000 -1.20000 AFIX 0 C11 1 0.081090 0.777125 0.207010 11.00000 0.10325 0.08957 = 0.08188 0.00250 0.02588 0.00599 AFIX 23 H11A 2 0.048746 0.766428 0.243378 11.00000 -1.20000 H11B 2 0.071019 0.775328 0.102457 11.00000 -1.20000 AFIX 0 C12 1 0.119573 0.730135 0.256032 11.00000 0.09218 0.10679 = 0.09525 -0.00622 0.02465 -0.00343 AFIX 33 H12A 2 0.106621 0.682814 0.225124 11.00000 -1.50000 H12B 2 0.129010 0.731921 0.359558 11.00000 -1.50000 H12C 2 0.151401 0.741099 0.219480 11.00000 -1.50000 AFIX 0 C13 1 0.138713 1.181198 0.179061 11.00000 0.02686 0.01670 = 0.01662 0.00273 0.00406 -0.00052 C14 1 0.124966 1.109320 0.192734 11.00000 0.02405 0.02400 = 0.02331 0.00094 0.00383 -0.00151 C15 1 0.103468 1.242976 0.195600 11.00000 0.02361 0.01846 = 0.03006 -0.00070 0.00819 -0.00303 C16 1 0.106096 1.276376 0.324249 11.00000 0.03455 0.02479 = 0.03340 -0.00385 0.01131 0.00177 AFIX 43 H16 2 0.131841 1.261396 0.405681 11.00000 -1.20000 AFIX 0 C17 1 0.071621 1.331153 0.334809 11.00000 0.04093 0.03204 = 0.04500 -0.01361 0.01728 0.00161 AFIX 43 H17 2 0.073408 1.352961 0.423801 11.00000 -1.20000 AFIX 0 C18 1 0.034633 1.354480 0.217390 11.00000 0.04404 0.02210 = 0.05369 -0.00173 0.01848 0.01526 AFIX 43 H18 2 0.011314 1.392589 0.224993 11.00000 -1.20000 AFIX 0 C19 1 0.031723 1.321968 0.088346 11.00000 0.03765 0.03266 = 0.04788 0.00704 0.00584 0.01186 AFIX 43 H19 2 0.006310 1.337798 0.007027 11.00000 -1.20000 AFIX 0 C20 1 0.065676 1.266526 0.077381 11.00000 0.03551 0.02559 = 0.03775 0.00239 0.01028 0.00646 AFIX 43 H20 2 0.063254 1.244261 -0.011451 11.00000 -1.20000 AFIX 0 C21 1 0.073501 1.084543 0.226162 11.00000 0.02433 0.02147 = 0.02488 0.00468 0.00858 -0.00057 C22 1 0.041420 1.036036 0.140438 11.00000 0.02509 0.02386 = 0.03596 -0.00242 0.00811 0.00184 AFIX 43 H22 2 0.052768 1.016266 0.062168 11.00000 -1.20000 AFIX 0 C23 1 -0.007121 1.016198 0.168215 11.00000 0.03437 0.03365 = 0.04155 -0.00170 0.01064 -0.00340 AFIX 43 H23 2 -0.029542 0.983679 0.107545 11.00000 -1.20000 AFIX 0 C24 1 -0.023273 1.043348 0.283672 11.00000 0.01825 0.03834 = 0.05058 0.01301 0.01640 0.00994 AFIX 43 H24 2 -0.056604 1.029093 0.302673 11.00000 -1.20000 AFIX 0 C25 1 0.008867 1.091270 0.371970 11.00000 0.03970 0.03100 = 0.03149 0.00224 0.01166 0.00486 AFIX 43 H25 2 -0.002521 1.110875 0.450327 11.00000 -1.20000 AFIX 0 C26 1 0.058072 1.110292 0.344280 11.00000 0.03002 0.02478 = 0.03268 0.00366 0.00830 0.00444 AFIX 43 H26 2 0.081287 1.141217 0.406968 11.00000 -1.20000 AFIX 0 C27 1 0.332944 0.438071 0.885202 11.00000 0.05852 0.11958 = 0.06545 -0.02519 0.01573 -0.02037 AFIX 33 H27A 2 0.368693 0.459791 0.904167 11.00000 -1.50000 H27B 2 0.334116 0.395419 0.942739 11.00000 -1.50000 H27C 2 0.307054 0.471425 0.909052 11.00000 -1.50000 AFIX 0 C28 1 0.315835 0.418805 0.729570 11.00000 0.05519 0.05910 = 0.05579 -0.01218 0.01936 -0.00818 AFIX 23 H28A 2 0.342693 0.386259 0.705326 11.00000 -1.20000 H28B 2 0.315077 0.461972 0.671884 11.00000 -1.20000 AFIX 0 C29 1 0.260381 0.383849 0.692852 11.00000 0.04250 0.03867 = 0.04360 -0.00693 0.01344 0.00911 AFIX 23 H29A 2 0.234173 0.415486 0.722712 11.00000 -1.20000 H29B 2 0.261918 0.339650 0.747808 11.00000 -1.20000 AFIX 0 C30 1 0.239864 0.366666 0.535534 11.00000 0.04719 0.02196 = 0.04995 -0.00304 0.01385 -0.00033 AFIX 23 H30A 2 0.201063 0.355258 0.517599 11.00000 -1.20000 H30B 2 0.243856 0.408991 0.479179 11.00000 -1.20000 AFIX 0 C31 1 0.251178 0.240674 0.499870 11.00000 0.02536 0.02212 = 0.02549 0.00295 0.00313 0.00346 C32 1 0.283832 0.184610 0.454148 11.00000 0.02487 0.01962 = 0.02588 -0.00021 0.00541 0.00195 C33 1 0.304330 0.071413 0.427139 11.00000 0.01897 0.01861 = 0.01941 -0.00362 0.00485 0.00093 C34 1 0.298375 -0.005353 0.438420 11.00000 0.02112 0.02174 = 0.01909 0.00004 0.00606 0.00060 C35 1 0.305403 -0.120259 0.328018 11.00000 0.03892 0.01815 = 0.02771 -0.00132 0.01094 -0.00088 AFIX 23 H35A 2 0.282512 -0.138837 0.239282 11.00000 -1.20000 H35B 2 0.290826 -0.137905 0.407691 11.00000 -1.20000 AFIX 0 C36 1 0.362361 -0.147286 0.343580 11.00000 0.03172 0.02958 = 0.03290 -0.00550 0.01089 0.00100 AFIX 23 H36A 2 0.376016 -0.133149 0.260045 11.00000 -1.20000 H36B 2 0.385988 -0.126035 0.428433 11.00000 -1.20000 AFIX 0 C37 1 0.363867 -0.226572 0.357119 11.00000 0.03712 0.00975 = 0.03648 -0.00254 0.01324 0.00736 AFIX 23 H37A 2 0.346723 -0.247469 0.264455 11.00000 -1.20000 H37B 2 0.342406 -0.240769 0.425575 11.00000 -1.20000 AFIX 0 C38 1 0.421279 -0.256995 0.406022 11.00000 0.03645 0.03322 = 0.04125 0.00225 0.00881 0.01826 AFIX 33 H38A 2 0.419387 -0.308499 0.410903 11.00000 -1.50000 H38B 2 0.438040 -0.238225 0.499651 11.00000 -1.50000 H38C 2 0.442796 -0.243540 0.338504 11.00000 -1.50000 AFIX 0 C39 1 0.331277 0.183995 0.408124 11.00000 0.02825 0.02290 = 0.02210 0.00379 0.00708 -0.00403 C40 1 0.344407 0.112407 0.390807 11.00000 0.02382 0.02453 = 0.01852 0.00035 0.00461 -0.00004 C41 1 0.366158 0.245095 0.396494 11.00000 0.02805 0.01854 = 0.03287 -0.00204 0.01186 -0.00253 C42 1 0.359200 0.285808 0.274283 11.00000 0.03773 0.03255 = 0.03231 0.00964 0.00002 -0.00539 AFIX 43 H42 2 0.331058 0.274886 0.194883 11.00000 -1.20000 AFIX 0 C43 1 0.393274 0.342399 0.267948 11.00000 0.05387 0.03726 = 0.04515 0.01340 0.00776 -0.01160 AFIX 43 H43 2 0.388120 0.369953 0.184280 11.00000 -1.20000 AFIX 0 C44 1 0.434654 0.358903 0.382628 11.00000 0.04076 0.03007 = 0.06080 0.00045 0.00674 -0.00639 AFIX 43 H44 2 0.458167 0.397030 0.376709 11.00000 -1.20000 AFIX 0 C45 1 0.441560 0.320605 0.503265 11.00000 0.04114 0.03486 = 0.04198 -0.00397 0.00509 -0.00970 AFIX 43 H45 2 0.469295 0.332628 0.582841 11.00000 -1.20000 AFIX 0 C46 1 0.407939 0.263678 0.510216 11.00000 0.03963 0.03180 = 0.02758 -0.00095 0.00660 -0.00799 AFIX 43 H46 2 0.413567 0.236700 0.594700 11.00000 -1.20000 AFIX 0 C47 1 0.394005 0.086927 0.355118 11.00000 0.01891 0.01955 = 0.02852 -0.00295 0.00593 -0.00731 C48 1 0.425322 0.033975 0.433727 11.00000 0.03190 0.02865 = 0.03225 0.00067 0.01235 -0.00083 AFIX 43 H48 2 0.413702 0.013162 0.510636 11.00000 -1.20000 AFIX 0 C49 1 0.473011 0.010932 0.402440 11.00000 0.01811 0.03212 = 0.04855 -0.00214 0.00589 0.00360 AFIX 43 H49 2 0.493020 -0.026239 0.455251 11.00000 -1.20000 AFIX 0 C50 1 0.491045 0.042829 0.293245 11.00000 0.03442 0.03483 = 0.04439 -0.00971 0.01513 0.00117 AFIX 43 H50 2 0.524038 0.028452 0.272362 11.00000 -1.20000 AFIX 0 C51 1 0.461223 0.094899 0.216024 11.00000 0.03190 0.04229 = 0.03807 -0.00590 0.02338 -0.00774 AFIX 43 H51 2 0.473664 0.116303 0.140955 11.00000 -1.20000 AFIX 0 C52 1 0.413447 0.117094 0.244612 11.00000 0.03290 0.02649 = 0.02928 -0.00070 0.01667 0.00016 AFIX 43 H52 2 0.393389 0.153311 0.188771 11.00000 -1.20000 AFIX 0 N1 3 0.207382 1.304756 0.131950 11.00000 0.03998 0.01989 = 0.05579 0.00095 0.02964 -0.00428 AFIX 43 H1 2 0.184386 1.309064 0.186594 11.00000 -1.20000 AFIX 0 N2 3 0.200179 1.114174 0.115694 11.00000 0.02483 0.02370 = 0.02532 -0.00385 0.00944 -0.00021 AFIX 43 H2 2 0.228651 1.100931 0.085480 11.00000 -1.20000 AFIX 0 N3 3 0.162051 0.954368 0.246588 11.00000 0.03487 0.02189 = 0.02575 0.00071 0.01322 0.00245 AFIX 43 H3 2 0.160041 0.976772 0.324553 11.00000 -1.20000 AFIX 0 N4 3 0.268166 0.307763 0.487673 11.00000 0.04202 0.01924 = 0.04651 -0.00044 0.01767 0.00272 AFIX 43 H4 2 0.296132 0.315764 0.451063 11.00000 -1.20000 AFIX 0 N5 3 0.267820 0.115655 0.466266 11.00000 0.02297 0.01571 = 0.02579 -0.00017 0.01157 0.00028 AFIX 43 H5 2 0.238925 0.102378 0.494476 11.00000 -1.20000 AFIX 0 N6 3 0.303203 -0.043054 0.325760 11.00000 0.03495 0.01841 = 0.02281 0.00089 0.00987 -0.00191 AFIX 43 H6 2 0.305127 -0.020784 0.247584 11.00000 -1.20000 AFIX 0 O1 4 0.254310 1.227764 0.029928 11.00000 0.03544 0.03120 = 0.04410 -0.00269 0.02082 -0.00470 O2 4 0.178010 0.966140 0.027194 11.00000 0.03131 0.02367 = 0.02674 -0.00044 0.01388 -0.00046 O3 4 0.213829 0.226435 0.551202 11.00000 0.03263 0.02443 = 0.04271 0.00340 0.01588 0.00551 O4 4 0.291261 -0.032014 0.550630 11.00000 0.03406 0.01908 = 0.02448 0.00201 0.01015 -0.00316 HKLF 4 Covalent radii and connectivity table for 01SOT013 in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C2 - C3 C1 C3 - C2 C4 C4 - N1 C3 C5 - O1 N1 C6 C6 - N2 C13 C5 C7 - N2 C14 C8 C8 - O2 N3 C7 C9 - N3 C10 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 - C6 C14 C15 C14 - C7 C13 C21 C15 - C16 C20 C13 C16 - C17 C15 C17 - C18 C16 C18 - C17 C19 C19 - C20 C18 C20 - C19 C15 C21 - C22 C26 C14 C22 - C21 C23 C23 - C22 C24 C24 - C23 C25 C25 - C24 C26 C26 - C21 C25 C27 - C28 C28 - C27 C29 C29 - C28 C30 C30 - N4 C29 C31 - O3 N4 C32 C32 - C39 N5 C31 C33 - N5 C40 C34 C34 - O4 N6 C33 C35 - N6 C36 C36 - C37 C35 C37 - C36 C38 C38 - C37 C39 - C32 C40 C41 C40 - C33 C39 C47 C41 - C42 C46 C39 C42 - C43 C41 C43 - C44 C42 C44 - C45 C43 C45 - C44 C46 C46 - C45 C41 C47 - C48 C52 C40 C48 - C49 C47 C49 - C50 C48 C50 - C51 C49 C51 - C50 C52 C52 - C51 C47 N1 - C5 C4 N2 - C7 C6 N3 - C8 C9 N4 - C31 C30 N5 - C33 C32 N6 - C34 C35 O1 - C5 O2 - C8 O3 - C31 O4 - C34 Floating origin restraints generated h k l Fo^2 Sigma Why rejected -2 0 -1 1.02 0.23 observed but should be systematically absent -2 0 -1 2.82 0.40 observed but should be systematically absent 24093 Reflections read, of which 311 rejected -33 =< h =< 32, -24 =< k =< 24, -11 =< l =< 12, Max. 2-theta = 54.96 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 6 -9 15.50 0.99 3 6.35 13 7 -9 44.92 1.76 3 13.35 12 8 -9 133.12 6.43 3 43.40 -1 9 -9 29.87 1.15 3 19.36 16 0 -8 77.50 4.73 2 27.07 16 2 -8 33.95 0.74 2 70.61 17 3 -8 80.82 4.92 2 33.27 14 4 -8 41.05 0.70 3 26.47 13 5 -8 16.65 0.61 3 6.72 15 5 -8 93.24 1.69 2 168.82 -2 6 -8 28.84 1.01 3 11.37 10 6 -8 9.75 0.51 3 3.51 14 6 -8 13.96 0.94 2 10.63 2 8 -8 26.15 0.66 5 5.74 12 8 -8 2.61 0.75 2 4.53 13 1 -7 14.71 0.68 3 4.71 14 2 -7 8.88 0.69 2 8.35 10 4 -7 11.91 0.73 2 6.20 0 6 -7 50.96 0.84 4 12.35 10 6 -7 5.75 0.42 2 6.91 3 7 -7 11.88 0.55 4 3.79 7 7 -7 3.40 0.61 2 4.74 6 10 -7 63.23 3.87 2 19.59 -1 3 -6 10.89 0.45 3 3.59 9 3 -6 9.50 0.32 3 3.86 11 3 -6 102.40 3.38 2 65.78 2 4 -6 36.81 0.44 3 27.43 4 4 -6 14.46 0.49 2 10.35 7 5 -6 16.08 0.94 2 5.57 4 6 -6 18.58 0.40 4 5.50 9 1 -5 95.96 0.51 3 100.75 3 3 -5 58.42 0.44 3 38.07 5 3 -5 46.93 0.44 2 141.00 7 1 -4 5.21 0.37 2 12.98 2 2 -4 8.93 0.24 5 1.34 4 2 -4 2.24 0.14 3 0.84 6 2 -4 13.61 0.41 3 6.79 5 1 -3 132.58 5.48 2 54.32 6 6 -3 296.70 10.26 2 61.35 1 1 -2 558.75 23.03 2 180.73 3 1 -2 411.35 15.02 2 180.62 -9 3 -2 107.18 4.04 2 23.02 -7 1 -1 107.74 3.98 2 20.61 8 4 -1 264.55 8.18 2 71.36 5 3 0 1258.67 29.31 3 187.10 3 5 0 1008.30 25.63 3 138.73 3 5 1 227.28 7.47 2 38.50 -8 8 1 239.30 6.21 3 38.10 5 9 1 500.65 13.83 3 75.13 -10 2 2 177.61 5.80 2 48.90 ** etc. ** 53 Inconsistent equivalents 9719 Unique reflections, of which 0 suppressed R(int) = 0.0855 R(sigma) = 0.0949 Friedel opposites not merged Maximum memory for data reduction = 4543 / 116057 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 = 6218 / 751931 wR2 = 0.1871 before cycle 1 for 9719 data and 559 / 559 parameters GooF = S = 1.106; Restrained GooF = 1.106 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/esd from 18.23 to 15.00 N value esd shift/esd parameter 1 0.20153 0.00044 -1.402 OSF 95 0.16668 0.00564 11.250 U11 C11 97 0.04884 0.00411 -8.044 U33 C11 98 0.01487 0.00334 3.707 U23 C11 99 0.04392 0.00389 4.640 U13 C11 100 0.03216 0.00442 5.924 U12 C11 105 0.14666 0.00543 7.343 U22 C12 106 0.07769 0.00473 -3.715 U33 C12 107 -0.02336 0.00384 -4.465 U23 C12 109 -0.02034 0.00438 -3.864 U12 C12 331 0.04304 0.00182 3.599 U33 C37 340 0.04721 0.00185 3.223 U33 C38 343 0.02984 0.00166 6.980 U12 C38 Mean shift/esd = 0.617 Maximum = 11.250 for U11 C11 Max. shift = 0.016 A for H12B Max. dU = 0.005 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6218 / 751931 wR2 = 0.1753 before cycle 2 for 9719 data and 559 / 559 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20192 0.00042 0.944 OSF 95 0.22941 0.00716 8.759 U11 C11 97 0.03834 0.00291 -3.602 U33 C11 98 0.02427 0.00260 3.614 U23 C11 99 0.06211 0.00365 4.979 U13 C11 100 0.06147 0.00448 6.537 U12 C11 104 0.06234 0.00424 -3.472 U11 C12 105 0.19608 0.00656 7.539 U22 C12 107 -0.03909 0.00388 -4.054 U23 C12 109 -0.03651 0.00433 -3.733 U12 C12 331 0.05020 0.00190 3.760 U33 C37 340 0.05326 0.00186 3.259 U33 C38 343 0.03664 0.00158 4.306 U12 C38 Mean shift/esd = 0.456 Maximum = 8.759 for U11 C11 Max. shift = 0.021 A for C12 Max. dU = 0.017 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6218 / 751931 wR2 = 0.1722 before cycle 3 for 9719 data and 559 / 559 parameters GooF = S = 1.011; Restrained GooF = 1.010 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20209 0.00041 0.407 OSF 92 0.07878 0.00039 -3.464 x C11 93 0.77577 0.00031 -4.291 y C11 96 0.10420 0.00424 4.396 U22 C11 100 0.07705 0.00508 3.068 U12 C11 102 0.73292 0.00049 4.125 y C12 Mean shift/esd = 0.212 Maximum = 4.396 for U22 C11 Max. shift = 0.042 A for C11 Max. dU = 0.007 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6218 / 751931 wR2 = 0.1712 before cycle 4 for 9719 data and 559 / 559 parameters GooF = S = 1.003; Restrained GooF = 1.003 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20230 0.00041 0.531 OSF 92 0.07711 0.00040 -4.141 x C11 93 0.77472 0.00033 -3.174 y C11 94 0.20495 0.00057 -2.412 z C11 96 0.12958 0.00495 5.126 U22 C11 98 0.03481 0.00282 2.062 U23 C11 100 0.09725 0.00561 3.603 U12 C11 101 0.11788 0.00023 -1.697 x C12 102 0.73454 0.00052 3.098 y C12 103 0.25336 0.00059 -1.856 z C12 105 0.23811 0.00909 1.967 U22 C12 107 -0.05389 0.00452 -1.786 U23 C12 109 -0.05160 0.00474 -1.813 U12 C12 326 0.36480 0.00015 1.111 x C37 330 0.00758 0.00139 -1.019 U22 C37 339 0.03622 0.00193 1.429 U22 C38 Mean shift/esd = 0.202 Maximum = 5.126 for U22 C11 Max. shift = 0.046 A for C11 Max. dU = 0.009 for C11 Largest correlation matrix elements 0.626 U12 C33 / U12 C7 0.589 U12 C31 / U12 C5 0.580 U12 C32 / U12 C6 -0.618 U11 C40 / U11 C14 -0.589 U11 O3 / U11 O1 -0.580 U11 C32 / U11 C6 -0.612 U11 C50 / U11 C24 -0.587 U13 C47 / U13 C21 0.578 U12 C34 / U12 C8 -0.610 U13 N5 / U13 N2 0.586 U12 C40 / U12 C14 -0.578 U11 C33 / U11 C7 0.604 U12 C39 / U12 C13 0.586 U12 C41 / U12 C15 -0.575 U13 O3 / U13 O1 -0.603 U13 C40 / U13 C14 -0.581 U11 C41 / U11 C15 -0.573 U13 C32 / U13 C6 0.595 U13 C11 / U11 C11 -0.581 U11 N5 / U11 N2 -0.573 U11 C51 / U11 C25 -0.592 U11 C34 / U11 C8 0.580 U12 N5 / U12 N2 0.572 U12 C47 / U12 C21 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.1069 1.5258 0.1800 33 0.980 0.001 C1 C2 H1A H1B 0.0944 1.4921 0.0249 33 0.980 0.001 C1 C2 H1A H1C 0.1409 1.5498 0.0684 33 0.980 0.001 C1 C2 H1A H2A 0.1911 1.4702 0.2344 23 0.990 0.001 C2 C3 C1 H2B 0.1447 1.4125 0.1897 23 0.990 0.001 C2 C3 C1 H3A 0.2072 1.4657 0.0057 23 0.990 0.001 C3 C2 C4 H3B 0.1616 1.4071 -0.0370 23 0.990 0.001 C3 C2 C4 H4A 0.2492 1.3572 0.0131 23 0.990 0.000 C4 N1 C3 H4B 0.2589 1.3859 0.1719 23 0.990 0.001 C4 N1 C3 H9A 0.1856 0.8576 0.3215 23 0.990 0.000 C9 N3 C10 H9B 0.1650 0.8601 0.1532 23 0.990 0.001 C9 N3 C10 H10A 0.0763 0.8865 0.2074 23 0.990 0.012 C10 C9 C11 H10B 0.1024 0.8547 0.3582 23 0.990 0.007 C10 C9 C11 H11A 0.0463 0.7632 0.2472 23 0.990 0.025 C11 C12 C10 H11B 0.0656 0.7719 0.1007 23 0.990 0.014 C11 C12 C10 H12A 0.1083 0.6855 0.2270 33 0.980 0.042 C12 C11 H12A H12B 0.1281 0.7385 0.3566 33 0.980 0.021 C12 C11 H12A H12C 0.1481 0.7490 0.2132 33 0.980 0.035 C12 C11 H12A H16 0.1324 1.2621 0.4055 43 0.950 0.000 C16 C17 C15 H17 0.0731 1.3529 0.4240 43 0.950 0.000 C17 C18 C16 H18 0.0113 1.3928 0.2250 43 0.950 0.001 C18 C17 C19 H19 0.0065 1.3375 0.0068 43 0.950 0.000 C19 C20 C18 H20 0.0629 1.2442 -0.0105 43 0.950 0.001 C20 C19 C15 H22 0.0524 1.0171 0.0607 43 0.950 0.000 C22 C21 C23 H23 -0.0296 0.9830 0.1083 43 0.950 0.001 C23 C22 C24 H24 -0.0566 1.0294 0.3031 43 0.950 0.001 C24 C23 C25 H25 -0.0024 1.1109 0.4503 43 0.950 0.001 C25 C24 C26 H26 0.0811 1.1418 0.4065 43 0.950 0.001 C26 C21 C25 H27A 0.3685 0.4598 0.9046 33 0.980 0.000 C27 C28 H27A H27B 0.3339 0.3953 0.9424 33 0.980 0.000 C27 C28 H27A H27C 0.3068 0.4713 0.9091 33 0.980 0.000 C27 C28 H27A H28A 0.3427 0.3867 0.7050 23 0.990 0.000 C28 C27 C29 H28B 0.3150 0.4624 0.6720 23 0.990 0.001 C28 C27 C29 H29A 0.2341 0.4155 0.7225 23 0.990 0.000 C29 C28 C30 H29B 0.2620 0.3397 0.7472 23 0.990 0.000 C29 C28 C30 H30A 0.2011 0.3558 0.5182 23 0.990 0.000 C30 N4 C29 H30B 0.2441 0.4093 0.4799 23 0.990 0.000 C30 N4 C29 H35A 0.2827 -0.1389 0.2392 23 0.990 0.002 C35 N6 C36 H35B 0.2909 -0.1380 0.4076 23 0.990 0.002 C35 N6 C36 H36A 0.3759 -0.1327 0.2601 23 0.990 0.002 C36 C37 C35 H36B 0.3859 -0.1255 0.4284 23 0.990 0.003 C36 C37 C35 H37A 0.3477 -0.2475 0.2649 23 0.990 0.001 C37 C36 C38 H37B 0.3433 -0.2410 0.4258 23 0.990 0.000 C37 C36 C38 H38A 0.4191 -0.3089 0.4108 33 0.980 0.002 C38 C37 H38A H38B 0.4382 -0.2389 0.5000 33 0.980 0.001 C38 C37 H38A H38C 0.4431 -0.2442 0.3390 33 0.980 0.001 C38 C37 H38A H42 0.3314 0.2744 0.1945 43 0.950 0.000 C42 C43 C41 H43 0.3880 0.3699 0.1841 43 0.950 0.001 C43 C44 C42 H44 0.4581 0.3974 0.3766 43 0.950 0.002 C44 C45 C43 H45 0.4694 0.3326 0.5830 43 0.950 0.002 C45 C44 C46 H46 0.4132 0.2366 0.5953 43 0.950 0.002 C46 C45 C41 H48 0.4134 0.0126 0.5103 43 0.950 0.002 C48 C49 C47 H49 0.4928 -0.0259 0.4551 43 0.950 0.001 C49 C50 C48 H50 0.5245 0.0280 0.2741 43 0.950 0.002 C50 C51 C49 H51 0.4736 0.1162 0.1399 43 0.950 0.002 C51 C50 C52 H52 0.3933 0.1534 0.1890 43 0.950 0.002 C52 C51 C47 H1 0.1839 1.3095 0.1856 43 0.880 0.000 N1 C5 C4 H2 0.2288 1.1009 0.0856 43 0.880 0.000 N2 C7 C6 H3 0.1596 0.9764 0.3248 43 0.880 0.001 N3 C8 C9 H4 0.2960 0.3157 0.4505 43 0.880 0.000 N4 C31 C30 H5 0.2387 0.1027 0.4934 43 0.880 0.000 N5 C33 C32 H6 0.3049 -0.0207 0.2476 43 0.880 0.001 N6 C34 C35 01SOT013 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.12277 1.51006 0.10233 1.00000 0.03528 0.04965 0.13254 0.00627 0.01762 0.00022 0.07271 0.00988 0.00018 0.00023 0.00063 0.00000 0.00230 0.00258 0.00407 0.00254 0.00250 0.00198 0.00135 H1A 0.10692 1.52579 0.18001 1.00000 0.10907 0.00000 0.00000 H1B 0.09435 1.49208 0.02495 1.00000 0.10907 0.00000 0.00000 H1C 0.14086 1.54983 0.06836 1.00000 0.10907 0.00000 0.00000 C2 0.16319 1.45216 0.15433 1.00000 0.04599 0.02697 0.07643 0.00340 0.02593 -0.00041 0.04788 0.00771 0.00016 0.00018 0.00043 0.00000 0.00227 0.00178 0.00254 0.00161 0.00189 0.00160 0.00091 H2A 0.19113 1.47025 0.23444 1.00000 0.05745 0.00000 0.00000 H2B 0.14474 1.41247 0.18968 1.00000 0.05745 0.00000 0.00000 C3 0.18964 1.42561 0.04229 1.00000 0.05423 0.03135 0.05582 0.00771 0.01523 -0.00759 0.04670 0.00742 0.00016 0.00018 0.00039 0.00000 0.00242 0.00184 0.00224 0.00151 0.00175 0.00168 0.00089 H3A 0.20723 1.46574 0.00571 1.00000 0.05604 0.00000 0.00000 H3B 0.16155 1.40706 -0.03696 1.00000 0.05604 0.00000 0.00000 C4 0.23122 1.36838 0.09074 1.00000 0.04772 0.01967 0.07795 0.00500 0.03344 -0.00729 0.04539 0.00850 0.00017 0.00018 0.00048 0.00000 0.00241 0.00179 0.00275 0.00163 0.00202 0.00165 0.00101 H4A 0.24917 1.35716 0.01313 1.00000 0.05447 0.00000 0.00000 H4B 0.25895 1.38593 0.17190 1.00000 0.05447 0.00000 0.00000 C5 0.21840 1.23940 0.09344 1.00000 0.02651 0.02027 0.02611 -0.00319 0.00957 -0.00087 0.02372 0.00604 0.00013 0.00017 0.00032 0.00000 0.00193 0.00176 0.00157 0.00125 0.00137 0.00145 0.00071 C6 0.18616 1.18221 0.13243 1.00000 0.02706 0.02176 0.01777 0.00058 0.00639 0.00310 0.02199 0.00584 0.00013 0.00017 0.00029 0.00000 0.00196 0.00171 0.00154 0.00118 0.00131 0.00141 0.00071 C7 0.16408 1.06948 0.15129 1.00000 0.02226 0.02365 0.02061 -0.00447 0.00441 0.00304 0.02225 0.00588 0.00014 0.00016 0.00030 0.00000 0.00183 0.00171 0.00153 0.00126 0.00127 0.00150 0.00070 C8 0.16890 0.99184 0.13695 1.00000 0.01995 0.01936 0.02623 0.00246 0.00608 0.00277 0.02171 0.00609 0.00014 0.00016 0.00032 0.00000 0.00179 0.00161 0.00165 0.00118 0.00130 0.00138 0.00069 C9 0.15779 0.87744 0.24324 1.00000 0.06633 0.02019 0.03438 0.00481 0.02748 0.00798 0.03774 0.00789 0.00017 0.00018 0.00039 0.00000 0.00285 0.00174 0.00186 0.00131 0.00180 0.00174 0.00094 H9A 0.18564 0.85756 0.32146 1.00000 0.04529 0.00000 0.00000 H9B 0.16499 0.86006 0.15321 1.00000 0.04529 0.00000 0.00000 C10 0.10256 0.85126 0.25663 1.00000 0.05603 0.02231 0.04665 0.00655 -0.00958 -0.00665 0.04505 0.00710 0.00017 0.00020 0.00040 0.00000 0.00282 0.00201 0.00207 0.00151 0.00176 0.00185 0.00102 H10A 0.07630 0.88654 0.20744 1.00000 0.05406 0.00000 0.00000 H10B 0.10239 0.85473 0.35823 1.00000 0.05406 0.00000 0.00000 C11 0.07711 0.77472 0.20495 1.00000 0.23051 0.12958 0.03953 0.03481 0.05987 0.09725 0.12854 0.01695 0.00040 0.00033 0.00057 0.00000 0.00947 0.00495 0.00276 0.00282 0.00412 0.00561 0.00317 H11A 0.04632 0.76319 0.24718 1.00000 0.15425 0.00000 0.00000 H11B 0.06560 0.77193 0.10067 1.00000 0.15425 0.00000 0.00000 C12 0.11788 0.73454 0.25336 1.00000 0.05996 0.23811 0.06587 -0.05389 0.02869 -0.05160 0.11901 0.01105 0.00023 0.00052 0.00059 0.00000 0.00365 0.00909 0.00360 0.00452 0.00292 0.00474 0.00285 H12A 0.10835 0.68554 0.22704 1.00000 0.17852 0.00000 0.00000 H12B 0.12814 0.73854 0.35658 1.00000 0.17852 0.00000 0.00000 H12C 0.14814 0.74900 0.21324 1.00000 0.17852 0.00000 0.00000 C13 0.13857 1.18116 0.17967 1.00000 0.02584 0.02065 0.02053 0.00036 0.00625 -0.00231 0.02218 0.00576 0.00013 0.00016 0.00030 0.00000 0.00192 0.00162 0.00153 0.00118 0.00128 0.00145 0.00069 C14 0.12497 1.10938 0.19292 1.00000 0.02147 0.02290 0.02364 0.00069 0.00488 -0.00033 0.02270 0.00581 0.00013 0.00016 0.00031 0.00000 0.00190 0.00172 0.00164 0.00123 0.00132 0.00143 0.00072 C15 0.10368 1.24303 0.19561 1.00000 0.02161 0.01756 0.03224 0.00193 0.00733 0.00015 0.02361 0.00607 0.00013 0.00017 0.00033 0.00000 0.00192 0.00165 0.00173 0.00127 0.00134 0.00139 0.00071 C16 0.10640 1.27667 0.32421 1.00000 0.03062 0.02691 0.03343 -0.00558 0.00947 0.00265 0.02997 0.00682 0.00015 0.00017 0.00037 0.00000 0.00203 0.00170 0.00170 0.00130 0.00141 0.00150 0.00075 H16 0.13239 1.26206 0.40548 1.00000 0.03596 0.00000 0.00000 C17 0.07156 1.33130 0.33489 1.00000 0.03988 0.03263 0.04549 -0.01392 0.01406 0.00297 0.03863 0.00702 0.00015 0.00019 0.00040 0.00000 0.00229 0.00193 0.00203 0.00155 0.00163 0.00165 0.00088 H17 0.07315 1.35286 0.42401 1.00000 0.04636 0.00000 0.00000 C18 0.03465 1.35464 0.21763 1.00000 0.04099 0.02195 0.05692 -0.00335 0.01814 0.01340 0.03883 0.00747 0.00016 0.00019 0.00041 0.00000 0.00250 0.00185 0.00227 0.00163 0.00188 0.00171 0.00093 H18 0.01134 1.39280 0.22502 1.00000 0.04660 0.00000 0.00000 C19 0.03186 1.32180 0.08842 1.00000 0.03361 0.03049 0.05090 0.00770 0.00590 0.01218 0.03892 0.00752 0.00016 0.00019 0.00041 0.00000 0.00224 0.00209 0.00222 0.00159 0.00169 0.00170 0.00090 H19 0.00653 1.33752 0.00683 1.00000 0.04670 0.00000 0.00000 C20 0.06560 1.26667 0.07826 1.00000 0.03710 0.02753 0.03292 0.00331 0.00948 0.00636 0.03227 0.00691 0.00015 0.00018 0.00035 0.00000 0.00222 0.00178 0.00182 0.00136 0.00158 0.00162 0.00081 H20 0.06294 1.24420 -0.01047 1.00000 0.03872 0.00000 0.00000 C21 0.07395 1.08405 0.22632 1.00000 0.02105 0.02218 0.02588 0.00582 0.00787 0.00137 0.02263 0.00602 0.00013 0.00016 0.00031 0.00000 0.00185 0.00170 0.00164 0.00127 0.00137 0.00140 0.00071 C22 0.04142 1.03626 0.14007 1.00000 0.02616 0.02542 0.03224 -0.00007 0.00702 0.00272 0.02788 0.00630 0.00014 0.00017 0.00034 0.00000 0.00198 0.00186 0.00171 0.00133 0.00143 0.00154 0.00075 H22 0.05240 1.01713 0.06070 1.00000 0.03345 0.00000 0.00000 C23 -0.00725 1.01589 0.16832 1.00000 0.03360 0.03278 0.04350 -0.00300 0.00802 -0.00483 0.03674 0.00726 0.00016 0.00020 0.00039 0.00000 0.00231 0.00200 0.00202 0.00148 0.00165 0.00163 0.00087 H23 -0.02956 0.98303 0.10826 1.00000 0.04409 0.00000 0.00000 C24 -0.02324 1.04344 0.28393 1.00000 0.02279 0.03996 0.05254 0.01482 0.02100 0.00919 0.03644 0.00770 0.00015 0.00020 0.00039 0.00000 0.00215 0.00227 0.00223 0.00169 0.00172 0.00169 0.00090 H24 -0.05659 1.02940 0.30314 1.00000 0.04373 0.00000 0.00000 C25 0.00897 1.09131 0.37186 1.00000 0.03904 0.02927 0.03707 0.00232 0.01488 0.00689 0.03413 0.00718 0.00015 0.00019 0.00037 0.00000 0.00243 0.00200 0.00199 0.00149 0.00173 0.00170 0.00088 H25 -0.00239 1.11089 0.45027 1.00000 0.04096 0.00000 0.00000 C26 0.05814 1.11048 0.34435 1.00000 0.02942 0.02489 0.02957 0.00369 0.00887 0.00299 0.02761 0.00653 0.00014 0.00017 0.00034 0.00000 0.00201 0.00174 0.00174 0.00129 0.00142 0.00150 0.00075 H26 0.08113 1.14184 0.40653 1.00000 0.03314 0.00000 0.00000 C27 0.33274 0.43804 0.88521 1.00000 0.05745 0.11941 0.05941 -0.02824 0.01820 -0.02375 0.07797 0.00842 0.00020 0.00031 0.00047 0.00000 0.00288 0.00431 0.00265 0.00263 0.00215 0.00283 0.00147 H27A 0.36849 0.45979 0.90460 1.00000 0.11696 0.00000 0.00000 H27B 0.33387 0.39527 0.94237 1.00000 0.11696 0.00000 0.00000 H27C 0.30680 0.47130 0.90913 1.00000 0.11696 0.00000 0.00000 C28 0.31579 0.41908 0.72936 1.00000 0.05240 0.05900 0.05076 -0.00726 0.01678 -0.00769 0.05324 0.00702 0.00017 0.00022 0.00039 0.00000 0.00250 0.00245 0.00215 0.00175 0.00179 0.00196 0.00097 H28A 0.34271 0.38669 0.70496 1.00000 0.06389 0.00000 0.00000 H28B 0.31497 0.46238 0.67200 1.00000 0.06389 0.00000 0.00000 C29 0.26039 0.38398 0.69247 1.00000 0.04327 0.03852 0.04200 -0.00820 0.01442 0.00707 0.04051 0.00634 0.00014 0.00019 0.00034 0.00000 0.00207 0.00192 0.00185 0.00136 0.00149 0.00156 0.00080 H29A 0.23414 0.41549 0.72251 1.00000 0.04861 0.00000 0.00000 H29B 0.26200 0.33972 0.74725 1.00000 0.04861 0.00000 0.00000 C30 0.23996 0.36703 0.53616 1.00000 0.04262 0.02428 0.05006 -0.00373 0.01193 0.00523 0.03876 0.00720 0.00016 0.00019 0.00039 0.00000 0.00225 0.00180 0.00207 0.00141 0.00165 0.00159 0.00089 H30A 0.20112 0.35584 0.51821 1.00000 0.04651 0.00000 0.00000 H30B 0.24408 0.40935 0.47991 1.00000 0.04651 0.00000 0.00000 C31 0.25157 0.24076 0.50062 1.00000 0.02458 0.02250 0.02798 -0.00156 0.00157 0.00237 0.02572 0.00630 0.00014 0.00017 0.00033 0.00000 0.00190 0.00185 0.00164 0.00129 0.00138 0.00149 0.00074 C32 0.28378 0.18473 0.45452 1.00000 0.02512 0.01788 0.02742 0.00150 0.00526 0.00101 0.02359 0.00602 0.00014 0.00016 0.00031 0.00000 0.00192 0.00166 0.00167 0.00125 0.00136 0.00139 0.00071 C33 0.30422 0.07152 0.42665 1.00000 0.02246 0.01965 0.02137 -0.00145 0.00716 0.00396 0.02081 0.00584 0.00014 0.00015 0.00030 0.00000 0.00179 0.00160 0.00147 0.00123 0.00127 0.00144 0.00066 C34 0.29857 -0.00541 0.43881 1.00000 0.01951 0.02120 0.02187 0.00034 0.00431 0.00128 0.02092 0.00580 0.00013 0.00016 0.00031 0.00000 0.00181 0.00162 0.00151 0.00119 0.00126 0.00139 0.00068 C35 0.30553 -0.12029 0.32803 1.00000 0.03332 0.02004 0.02860 -0.00236 0.01112 0.00086 0.02667 0.00624 0.00014 0.00017 0.00033 0.00000 0.00195 0.00166 0.00168 0.00117 0.00138 0.00142 0.00074 H35A 0.28270 -0.13888 0.23922 1.00000 0.03200 0.00000 0.00000 H35B 0.29094 -0.13804 0.40762 1.00000 0.03200 0.00000 0.00000 C36 0.36237 -0.14705 0.34367 1.00000 0.03174 0.02900 0.03521 -0.00271 0.01071 0.00136 0.03148 0.00665 0.00014 0.00018 0.00036 0.00000 0.00202 0.00183 0.00184 0.00137 0.00144 0.00154 0.00078 H36A 0.37595 -0.13273 0.26012 1.00000 0.03778 0.00000 0.00000 H36B 0.38588 -0.12551 0.42838 1.00000 0.03778 0.00000 0.00000 C37 0.36480 -0.22662 0.35764 1.00000 0.04815 0.00758 0.04924 -0.00345 0.01727 0.00641 0.03400 0.00680 0.00015 0.00015 0.00037 0.00000 0.00228 0.00139 0.00203 0.00127 0.00165 0.00141 0.00082 H37A 0.34774 -0.24753 0.26492 1.00000 0.04080 0.00000 0.00000 H37B 0.34325 -0.24103 0.42575 1.00000 0.04080 0.00000 0.00000 C38 0.42137 -0.25745 0.40622 1.00000 0.04231 0.03622 0.05732 0.00790 0.00980 0.03864 0.04552 0.00777 0.00015 0.00018 0.00039 0.00000 0.00209 0.00193 0.00202 0.00152 0.00159 0.00165 0.00091 H38A 0.41909 -0.30893 0.41080 1.00000 0.06828 0.00000 0.00000 H38B 0.43818 -0.23892 0.50002 1.00000 0.06828 0.00000 0.00000 H38C 0.44307 -0.24424 0.33897 1.00000 0.06828 0.00000 0.00000 C39 0.33118 0.18413 0.40799 1.00000 0.02735 0.01949 0.02358 0.00033 0.00634 -0.00391 0.02338 0.00595 0.00014 0.00016 0.00031 0.00000 0.00191 0.00170 0.00157 0.00124 0.00129 0.00147 0.00070 C40 0.34454 0.11222 0.39099 1.00000 0.02433 0.02496 0.02080 0.00100 0.00649 -0.00022 0.02315 0.00590 0.00013 0.00017 0.00030 0.00000 0.00196 0.00176 0.00158 0.00125 0.00134 0.00150 0.00072 C41 0.36625 0.24513 0.39654 1.00000 0.02726 0.02001 0.02871 0.00006 0.01133 0.00076 0.02453 0.00617 0.00014 0.00017 0.00032 0.00000 0.00202 0.00167 0.00168 0.00125 0.00141 0.00148 0.00073 C42 0.35936 0.28563 0.27410 1.00000 0.03806 0.03379 0.03430 0.00829 -0.00082 -0.00485 0.03682 0.00726 0.00016 0.00019 0.00037 0.00000 0.00238 0.00206 0.00187 0.00138 0.00156 0.00164 0.00091 H42 0.33137 0.27443 0.19452 1.00000 0.04419 0.00000 0.00000 C43 0.39323 0.34237 0.26776 1.00000 0.05141 0.03729 0.04639 0.01379 0.00853 -0.01028 0.04544 0.00760 0.00017 0.00020 0.00042 0.00000 0.00269 0.00218 0.00215 0.00161 0.00181 0.00186 0.00102 H43 0.38796 0.36993 0.18407 1.00000 0.05452 0.00000 0.00000 C44 0.43469 0.35915 0.38253 1.00000 0.04316 0.03217 0.05866 -0.00083 0.00705 -0.01059 0.04538 0.00752 0.00017 0.00021 0.00041 0.00000 0.00264 0.00214 0.00252 0.00177 0.00192 0.00189 0.00101 H44 0.45813 0.39735 0.37660 1.00000 0.05446 0.00000 0.00000 C45 0.44160 0.32061 0.50353 1.00000 0.04148 0.03966 0.03794 -0.00303 0.00223 -0.00972 0.04077 0.00713 0.00017 0.00020 0.00040 0.00000 0.00240 0.00228 0.00200 0.00162 0.00163 0.00187 0.00092 H45 0.46940 0.33256 0.58302 1.00000 0.04893 0.00000 0.00000 C46 0.40779 0.26348 0.51079 1.00000 0.03743 0.03225 0.02889 0.00074 0.00538 -0.00769 0.03320 0.00650 0.00015 0.00019 0.00035 0.00000 0.00221 0.00201 0.00172 0.00140 0.00153 0.00171 0.00083 H46 0.41323 0.23658 0.59534 1.00000 0.03984 0.00000 0.00000 C47 0.39412 0.08727 0.35475 1.00000 0.02292 0.01951 0.03043 -0.00262 0.00767 -0.00571 0.02403 0.00599 0.00014 0.00017 0.00033 0.00000 0.00185 0.00168 0.00174 0.00128 0.00140 0.00144 0.00072 C48 0.42516 0.03370 0.43394 1.00000 0.02727 0.02952 0.03414 0.00262 0.01065 0.00198 0.02972 0.00662 0.00015 0.00018 0.00035 0.00000 0.00204 0.00190 0.00178 0.00139 0.00150 0.00159 0.00077 H48 0.41337 0.01257 0.51029 1.00000 0.03566 0.00000 0.00000 C49 0.47281 0.01124 0.40208 1.00000 0.02216 0.03510 0.04473 -0.00046 0.00662 0.00434 0.03415 0.00690 0.00015 0.00020 0.00039 0.00000 0.00193 0.00205 0.00203 0.00150 0.00153 0.00159 0.00083 H49 0.49278 -0.02592 0.45507 1.00000 0.04098 0.00000 0.00000 C50 0.49135 0.04249 0.29403 1.00000 0.02959 0.03386 0.04374 -0.00822 0.01304 0.00229 0.03498 0.00698 0.00016 0.00019 0.00038 0.00000 0.00218 0.00217 0.00202 0.00162 0.00163 0.00173 0.00085 H50 0.52448 0.02800 0.27408 1.00000 0.04197 0.00000 0.00000 C51 0.46127 0.09501 0.21529 1.00000 0.03180 0.04630 0.03595 -0.00542 0.02258 -0.00530 0.03564 0.00700 0.00015 0.00020 0.00038 0.00000 0.00221 0.00234 0.00206 0.00159 0.00168 0.00179 0.00090 H51 0.47360 0.11624 0.13987 1.00000 0.04277 0.00000 0.00000 C52 0.41345 0.11714 0.24472 1.00000 0.03512 0.02850 0.02984 -0.00030 0.01555 -0.00017 0.02985 0.00666 0.00015 0.00018 0.00034 0.00000 0.00211 0.00180 0.00177 0.00130 0.00147 0.00156 0.00078 H52 0.39334 0.15336 0.18901 1.00000 0.03582 0.00000 0.00000 N1 0.20726 1.30501 0.13199 1.00000 0.03918 0.02164 0.05406 0.00071 0.02797 -0.00456 0.03552 0.00601 0.00013 0.00015 0.00032 0.00000 0.00181 0.00152 0.00183 0.00119 0.00144 0.00124 0.00074 H1 0.18394 1.30955 0.18564 1.00000 0.04263 0.00000 0.00000 N2 0.20029 1.11411 0.11548 1.00000 0.02514 0.02219 0.02489 -0.00394 0.00838 -0.00208 0.02364 0.00472 0.00011 0.00014 0.00025 0.00000 0.00164 0.00149 0.00143 0.00103 0.00120 0.00124 0.00062 H2 0.22884 1.10095 0.08555 1.00000 0.02837 0.00000 0.00000 N3 0.16189 0.95414 0.24683 1.00000 0.03188 0.02125 0.02667 0.00153 0.01207 0.00208 0.02574 0.00507 0.00011 0.00013 0.00026 0.00000 0.00172 0.00142 0.00135 0.00106 0.00114 0.00119 0.00063 H3 0.15964 0.97636 0.32481 1.00000 0.03088 0.00000 0.00000 N4 0.26820 0.30769 0.48783 1.00000 0.04194 0.02029 0.04500 0.00089 0.01663 0.00286 0.03467 0.00582 0.00013 0.00015 0.00032 0.00000 0.00184 0.00150 0.00162 0.00112 0.00134 0.00126 0.00071 H4 0.29598 0.31570 0.45050 1.00000 0.04160 0.00000 0.00000 N5 0.26773 0.11593 0.46568 1.00000 0.02217 0.01764 0.02836 -0.00114 0.01108 -0.00107 0.02187 0.00478 0.00011 0.00013 0.00026 0.00000 0.00158 0.00138 0.00143 0.00100 0.00117 0.00116 0.00059 H5 0.23873 0.10266 0.49340 1.00000 0.02625 0.00000 0.00000 N6 0.30321 -0.04305 0.32590 1.00000 0.03572 0.01866 0.02239 0.00189 0.00973 -0.00199 0.02509 0.00499 0.00012 0.00013 0.00025 0.00000 0.00172 0.00140 0.00128 0.00098 0.00112 0.00120 0.00062 H6 0.30493 -0.02074 0.24762 1.00000 0.03011 0.00000 0.00000 O1 0.25432 1.22765 0.02991 1.00000 0.03266 0.03323 0.04453 -0.00300 0.02286 -0.00510 0.03456 0.00466 0.00010 0.00013 0.00024 0.00000 0.00157 0.00139 0.00155 0.00104 0.00124 0.00116 0.00062 O2 0.17792 0.96604 0.02679 1.00000 0.03219 0.02584 0.02460 -0.00031 0.01371 0.00078 0.02638 0.00407 0.00009 0.00011 0.00020 0.00000 0.00144 0.00124 0.00115 0.00093 0.00096 0.00108 0.00052 O3 0.21354 0.22641 0.55115 1.00000 0.03263 0.02536 0.04368 0.00287 0.01564 0.00498 0.03278 0.00457 0.00010 0.00013 0.00023 0.00000 0.00159 0.00129 0.00150 0.00099 0.00124 0.00112 0.00060 O4 0.29121 -0.03191 0.55043 1.00000 0.03474 0.01867 0.02508 0.00277 0.01071 -0.00270 0.02554 0.00397 0.00009 0.00011 0.00019 0.00000 0.00145 0.00114 0.00116 0.00088 0.00097 0.00102 0.00052 Final Structure Factor Calculation for 01SOT013 in Cc Total number of l.s. parameters = 559 Maximum vector length = 511 Memory required = 5661 / 25046 wR2 = 0.1705 before cycle 5 for 9719 data and 2 / 559 parameters GooF = S = 0.999; Restrained GooF = 0.999 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0610 for 6788 Fo > 4sig(Fo) and 0.0986 for all 9719 data wR2 = 0.1705, GooF = S = 0.999, Restrained GooF = 0.999 for all data Flack x parameter = 0.2017 with esd 1.2552 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 62.00 for non-hydrogen and 62.00 for hydrogen atoms Principal mean square atomic displacements U 0.1347 0.0492 0.0343 C1 0.0786 0.0385 0.0265 C2 0.0581 0.0565 0.0255 C3 0.0838 0.0380 0.0144 C4 0.0299 0.0227 0.0185 C5 0.0285 0.0204 0.0171 C6 0.0289 0.0214 0.0164 C7 0.0271 0.0212 0.0169 C8 0.0715 0.0231 0.0187 C9 0.0812 0.0336 0.0203 C10 0.2903 0.0716 0.0238 C11 may be split into 0.0850 0.7811 0.2062 and 0.0692 0.7683 0.2037 0.2623 0.0512 0.0435 C12 may be split into 0.1151 0.7459 0.2480 and 0.1207 0.7231 0.2587 0.0267 0.0209 0.0189 C13 0.0242 0.0225 0.0214 C14 0.0325 0.0210 0.0173 C15 0.0367 0.0319 0.0213 C16 0.0544 0.0409 0.0206 C17 0.0583 0.0456 0.0125 C18 0.0538 0.0439 0.0190 C19 0.0407 0.0320 0.0242 C20 0.0304 0.0202 0.0173 C21 0.0323 0.0285 0.0229 C22 0.0443 0.0376 0.0283 C23 0.0649 0.0301 0.0143 C24 0.0456 0.0317 0.0251 C25 0.0334 0.0267 0.0227 C26 0.1348 0.0520 0.0471 C27 0.0671 0.0477 0.0449 C28 0.0498 0.0465 0.0251 C29 0.0506 0.0439 0.0218 C30 0.0331 0.0231 0.0209 C31 0.0280 0.0252 0.0176 C32 0.0253 0.0222 0.0149 C33 0.0221 0.0219 0.0188 C34 0.0349 0.0262 0.0188 C35 0.0369 0.0317 0.0259 C36 0.0539 0.0424 0.0057 C37 0.0780 0.0580 0.0005 C38 0.0290 0.0235 0.0176 C39 0.0252 0.0246 0.0197 C40 0.0321 0.0217 0.0198 C41 0.0535 0.0313 0.0256 C42 0.0655 0.0472 0.0235 C43 0.0617 0.0487 0.0257 C44 0.0527 0.0414 0.0282 C45 0.0441 0.0288 0.0267 C46 0.0315 0.0253 0.0152 C47 0.0363 0.0283 0.0245 C48 0.0455 0.0363 0.0207 C49 0.0484 0.0336 0.0229 C50 0.0531 0.0394 0.0144 C51 0.0396 0.0285 0.0215 C52 0.0624 0.0268 0.0174 N1 0.0293 0.0223 0.0193 N2 0.0347 0.0217 0.0208 N3 0.0493 0.0348 0.0199 N4 0.0306 0.0178 0.0172 N5 0.0361 0.0224 0.0168 N6 0.0525 0.0326 0.0186 O1 0.0353 0.0259 0.0180 O2 0.0466 0.0293 0.0224 O3 0.0356 0.0249 0.0160 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.023 0.030 0.038 0.047 0.059 0.074 0.098 0.140 1.000 Number in group 1080. 898. 968. 967. 946. 1041. 915. 958. 966. 980. GooF 0.858 0.949 0.958 1.050 1.094 1.089 1.032 1.034 0.942 0.967 K 1.415 0.965 1.043 0.975 1.011 1.005 1.002 1.000 1.017 0.992 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.06 1.17 1.34 1.68 inf Number in group 973. 1007. 933. 973. 996. 948. 990. 959. 969. 971. GooF 0.871 0.911 0.957 0.984 0.986 1.012 0.942 0.991 1.057 1.237 K 1.060 1.047 1.013 0.989 1.000 1.005 1.025 1.041 1.046 0.965 R1 0.260 0.212 0.181 0.148 0.104 0.080 0.056 0.053 0.054 0.053 Recommended weighting scheme: WGHT 0.0943 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) 2 10 -9 5.13 217.09 9.39 0.044 0.93 7 1 -4 127.35 2102.22 5.84 0.138 2.20 7 3 -4 628.27 365.04 5.45 0.058 2.09 2 2 4 74.78 19.25 5.11 0.013 2.17 5 7 -8 7.82 89.12 4.92 0.028 1.11 0 0 2 2207.08 3667.89 4.48 0.182 4.73 4 0 0 301.09 515.55 4.41 0.068 6.22 -6 0 2 1293.31 2128.68 4.28 0.139 3.54 -5 13 -2 186.87 356.51 4.17 0.057 1.32 -4 0 0 321.13 517.68 4.11 0.069 6.22 -1 3 1 680.18 1163.37 3.94 0.103 5.28 1 3 -1 695.32 1163.32 3.89 0.103 5.28 -25 3 -3 18.92 127.94 3.87 0.034 0.88 14 0 0 830.43 526.28 3.84 0.069 1.78 6 0 -2 1387.89 2128.92 3.82 0.139 3.54 6 0 2 25264.69 39078.46 3.76 0.595 2.82 -2 18 0 356.29 163.16 3.76 0.038 1.05 30 0 -4 169.85 906.72 3.71 0.091 0.84 -7 1 -2 366.72 249.74 3.68 0.048 2.55 0 16 0 300.41 503.45 3.61 0.068 1.19 -7 3 4 543.53 364.60 3.55 0.057 2.09 8 6 -5 1243.91 875.27 3.52 0.089 1.57 -11 5 0 695.30 1038.54 3.50 0.097 1.94 -11 1 8 570.16 903.33 3.48 0.091 1.16 18 12 -7 210.17 440.91 3.48 0.063 0.90 -2 2 -4 58.47 19.02 3.45 0.013 2.17 0 6 5 432.98 296.95 3.42 0.052 1.62 -5 5 2 1507.16 2157.09 3.39 0.140 2.72 8 0 0 3376.72 5077.94 3.38 0.215 3.11 -15 1 0 1319.16 1975.05 3.38 0.134 1.65 -4 18 4 111.56 323.81 3.36 0.054 0.96 14 2 -8 57.58 99.58 3.34 0.030 1.10 -25 15 5 126.72 397.46 3.34 0.060 0.77 14 0 6 173.52 484.38 3.34 0.066 1.07 9 5 1 573.16 829.73 3.33 0.087 2.09 8 20 -4 40.84 159.75 3.33 0.038 0.87 27 7 -3 39.52 215.13 3.32 0.044 0.89 22 14 4 203.82 677.06 3.30 0.078 0.77 6 12 -5 322.47 206.14 3.28 0.043 1.21 1 19 -3 283.85 129.20 3.28 0.034 0.95 20 18 -1 -78.20 172.16 3.27 0.040 0.81 -5 19 -2 82.82 230.36 3.23 0.046 0.95 17 1 8 -61.28 132.50 3.23 0.035 0.83 -6 12 5 316.55 206.00 3.22 0.043 1.21 19 11 2 -27.37 111.05 3.22 0.032 0.98 -10 14 -1 103.37 209.66 3.21 0.044 1.17 -14 0 -6 295.22 484.24 3.20 0.066 1.07 -10 12 -6 303.89 156.66 3.15 0.038 0.96 -5 1 -1 566.54 792.82 3.14 0.085 3.95 2 2 1 1952.38 2862.12 3.12 0.161 5.54 FMAP and GRID set by program FMAP 2 2 45 GRID -1.190 -2 -1 1.190 2 1 R1 = 0.0877 for 5193 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.0543 0.2718 0.6902 [ 0.92 A from H11A ] Deepest hole -0.49 at 0.1270 0.3132 0.7818 [ 0.63 A from H12A ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5415 / 65589 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0543 0.7282 0.1902 1.00000 0.05 0.44 0.92 H11A 1.05 C11 1.28 H11B 1.57 H12A Q2 1 0.1268 0.7173 0.2521 1.00000 0.05 0.29 0.40 C12 0.77 H12A 0.95 H12C 1.09 H12B Q3 1 0.2028 1.3789 -0.1318 1.00000 0.05 0.28 1.64 H3B 1.67 H4A 1.91 H29A 2.00 C3 Q4 1 0.3084 0.5469 0.9210 1.00000 0.05 0.28 1.44 H27C 2.04 H30B 2.21 C27 2.28 H27A Q5 1 0.1131 0.7721 0.2393 1.00000 0.05 0.24 0.73 C12 0.91 C11 1.08 H12C 1.29 H12B Shortest distances between peaks (including symmetry equivalents) 2 5 1.09 1 5 1.69 1 2 1.82 2 3 2.72 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: 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. 3.45: 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 9.25: Structure factors and derivatives 20.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 2.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.25: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.31: Fourier summations 0.19: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:18:33 Total CPU time: 35.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++