+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0806b started at 13:36:02 on 29-Jun-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0806b in P-1 CELL 0.71073 13.1434 13.5460 15.5201 102.394 104.117 92.925 ZERR 2.00 0.0009 0.0010 0.0010 0.005 0.005 0.005 LATT 1 SFAC C H O P CL RU UNIT 116 110 6 6 8 2 V = 2601.67 F(000) = 1168.0 Mu = 0.64 mm-1 Cell Wt = 2271.60 Rho = 1.450 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 EXTI OMIT 0 2 1 ACTA SIZE 0.48 0.32 0.24 BOND $H WGHT 0.03590 2.96240 L.S. 8 TEMP -153.00 FVAR 0.41533 CL1 5 0.775382 0.408839 0.933840 11.00000 0.02256 0.01885 = 0.01842 0.00518 0.00285 0.00231 RU1 6 0.718055 0.269555 0.797128 11.00000 0.01069 0.01086 = 0.01153 0.00339 0.00265 0.00128 MOLE 1 C1 1 0.793287 0.353971 0.728091 11.00000 0.01145 0.01312 = 0.01212 0.00221 0.00263 0.00124 C2 1 0.902360 0.367596 0.746078 11.00000 0.01265 0.01396 = 0.01184 0.00393 0.00213 0.00345 C3 1 0.956258 0.432831 0.709289 11.00000 0.01170 0.01820 = 0.01239 0.00276 0.00362 0.00184 C4 1 0.892039 0.484112 0.651454 11.00000 0.01377 0.02002 = 0.01358 0.00587 0.00554 0.00094 AFIX 43 H4 2 0.926139 0.530667 0.626845 11.00000 -1.20000 AFIX 0 C5 1 0.781825 0.472301 0.627036 11.00000 0.01409 0.01922 = 0.01254 0.00552 0.00420 0.00266 C6 1 0.735896 0.403499 0.665714 11.00000 0.00955 0.01699 = 0.01298 0.00368 0.00297 0.00137 C7 1 1.077024 0.450361 0.731206 11.00000 0.00990 0.02415 = 0.01706 0.00551 0.00275 0.00121 C8 1 1.122961 0.350546 0.701462 11.00000 0.01391 0.03101 = 0.02860 0.00670 0.00900 0.00566 AFIX 137 H8A 2 1.098587 0.326173 0.634892 11.00000 -1.50000 H8B 2 1.099406 0.299440 0.730598 11.00000 -1.50000 H8C 2 1.200213 0.362314 0.719909 11.00000 -1.50000 AFIX 0 C9 1 1.123056 0.494243 0.834301 11.00000 0.01393 0.02773 = 0.01996 0.00720 -0.00030 -0.00239 AFIX 137 H9A 2 1.200080 0.506386 0.847878 11.00000 -1.50000 H9B 2 1.104014 0.445822 0.867985 11.00000 -1.50000 H9C 2 1.094424 0.558500 0.852776 11.00000 -1.50000 AFIX 0 C10 1 1.112081 0.525842 0.681057 11.00000 0.01373 0.03467 = 0.02425 0.01162 0.00399 -0.00189 AFIX 137 H10A 2 1.081668 0.500632 0.615111 11.00000 -1.50000 H10B 2 1.189259 0.533429 0.694291 11.00000 -1.50000 H10C 2 1.087812 0.591905 0.701587 11.00000 -1.50000 AFIX 0 C11 1 0.717613 0.532366 0.562931 11.00000 0.01558 0.02853 = 0.02252 0.01659 0.00604 0.00509 C12 1 0.646609 0.597209 0.611854 11.00000 0.02157 0.03444 = 0.03831 0.02486 0.01353 0.01399 AFIX 137 H12A 2 0.607898 0.636991 0.571424 11.00000 -1.50000 H12B 2 0.690266 0.643326 0.667770 11.00000 -1.50000 H12C 2 0.596388 0.552658 0.627566 11.00000 -1.50000 AFIX 0 C13 1 0.650702 0.458504 0.475864 11.00000 0.02831 0.05046 = 0.02005 0.01855 -0.00201 -0.00174 AFIX 137 H13A 2 0.608376 0.496867 0.436084 11.00000 -1.50000 H13B 2 0.603813 0.411170 0.492172 11.00000 -1.50000 H13C 2 0.697148 0.420261 0.443684 11.00000 -1.50000 AFIX 0 C14 1 0.788885 0.605614 0.534764 11.00000 0.02029 0.03786 = 0.03429 0.02583 0.00915 0.00664 AFIX 137 H14A 2 0.836495 0.567266 0.504090 11.00000 -1.50000 H14B 2 0.830473 0.655400 0.589229 11.00000 -1.50000 H14C 2 0.745305 0.641062 0.492944 11.00000 -1.50000 AFIX 0 C15 1 0.979956 0.243877 0.950517 11.00000 0.01487 0.01942 = 0.01699 0.00680 0.00106 0.00338 C16 1 1.022642 0.340545 1.004129 11.00000 0.01541 0.02110 = 0.01918 0.00617 0.00420 0.00222 AFIX 43 H16 2 1.007657 0.398791 0.980377 11.00000 -1.20000 AFIX 0 C17 1 1.086987 0.352025 1.092124 11.00000 0.01833 0.02893 = 0.02278 0.00297 0.00175 -0.00186 AFIX 43 H17 2 1.115734 0.417942 1.128339 11.00000 -1.20000 AFIX 0 C18 1 1.108995 0.267375 1.126733 11.00000 0.03014 0.04153 = 0.02210 0.00900 -0.00611 0.00547 AFIX 43 H18 2 1.152383 0.275363 1.187027 11.00000 -1.20000 AFIX 0 C19 1 1.068213 0.171027 1.074094 11.00000 0.04989 0.03253 = 0.02910 0.01627 -0.00828 0.00626 AFIX 43 H19 2 1.084285 0.113066 1.098002 11.00000 -1.20000 AFIX 0 C20 1 1.003654 0.159108 0.986128 11.00000 0.03834 0.02226 = 0.02429 0.00924 -0.00356 0.00272 AFIX 43 H20 2 0.975583 0.092925 0.950151 11.00000 -1.20000 AFIX 0 C21 1 0.922480 0.107941 0.778501 11.00000 0.01940 0.01939 = 0.01578 0.00517 0.00279 0.00660 C22 1 1.021090 0.098692 0.761252 11.00000 0.02317 0.02650 = 0.03915 0.01118 0.01115 0.00949 AFIX 43 H22 2 1.072028 0.156543 0.778757 11.00000 -1.20000 AFIX 0 C23 1 1.045120 0.005457 0.718674 11.00000 0.03897 0.03829 = 0.04852 0.01535 0.02468 0.02359 AFIX 43 H23 2 1.112176 -0.000356 0.706343 11.00000 -1.20000 AFIX 0 C24 1 0.971580 -0.079409 0.694002 11.00000 0.05379 0.02599 = 0.03322 0.00426 0.01615 0.02017 AFIX 43 H24 2 0.988270 -0.143317 0.664792 11.00000 -1.20000 AFIX 0 C25 1 0.874432 -0.071209 0.711762 11.00000 0.03926 0.01800 = 0.02724 0.00343 0.00148 0.00658 AFIX 43 H25 2 0.824282 -0.129569 0.695227 11.00000 -1.20000 AFIX 0 C26 1 0.849537 0.022417 0.753899 11.00000 0.02289 0.01940 = 0.01957 0.00479 0.00336 0.00603 AFIX 43 H26 2 0.782282 0.027846 0.765894 11.00000 -1.20000 AFIX 0 C27 1 0.538266 0.466013 0.771448 11.00000 0.01620 0.01399 = 0.01372 0.00737 0.00515 0.00317 C28 1 0.622087 0.540074 0.821262 11.00000 0.01680 0.01741 = 0.01701 0.00725 0.00087 0.00143 AFIX 43 H28 2 0.692655 0.523618 0.829076 11.00000 -1.20000 AFIX 0 C29 1 0.602863 0.637057 0.859187 11.00000 0.02752 0.01749 = 0.01652 0.00480 0.00149 -0.00110 AFIX 43 H29 2 0.660193 0.686913 0.893030 11.00000 -1.20000 AFIX 0 C30 1 0.500536 0.661649 0.848003 11.00000 0.03291 0.01728 = 0.02760 0.00421 0.01238 0.00700 AFIX 43 H30 2 0.487415 0.728069 0.874811 11.00000 -1.20000 AFIX 0 C31 1 0.417135 0.589368 0.797672 11.00000 0.02044 0.02403 = 0.03759 0.00793 0.01199 0.00887 AFIX 43 H31 2 0.346832 0.606598 0.789865 11.00000 -1.20000 AFIX 0 C32 1 0.435284 0.491640 0.758372 11.00000 0.01667 0.01976 = 0.02462 0.00567 0.00549 0.00222 AFIX 43 H32 2 0.377774 0.442762 0.722866 11.00000 -1.20000 AFIX 0 C33 1 0.460671 0.267016 0.646722 11.00000 0.01163 0.01504 = 0.01459 0.00377 0.00029 0.00161 C34 1 0.460187 0.217042 0.557825 11.00000 0.01825 0.02188 = 0.01910 0.00321 0.00582 0.00097 AFIX 43 H34 2 0.517677 0.231359 0.533725 11.00000 -1.20000 AFIX 0 C35 1 0.375688 0.146404 0.504607 11.00000 0.02710 0.02609 = 0.01995 -0.00275 0.00234 -0.00227 AFIX 43 H35 2 0.376008 0.112530 0.444372 11.00000 -1.20000 AFIX 0 C36 1 0.291230 0.125065 0.538621 11.00000 0.02246 0.02307 = 0.02688 0.00104 0.00041 -0.00762 AFIX 43 H36 2 0.234054 0.076335 0.502130 11.00000 -1.20000 AFIX 0 C37 1 0.290478 0.175058 0.626043 11.00000 0.01404 0.02404 = 0.02786 0.00669 0.00420 -0.00253 AFIX 43 H37 2 0.231937 0.161457 0.649119 11.00000 -1.20000 AFIX 0 C38 1 0.374875 0.245145 0.680441 11.00000 0.01336 0.01796 = 0.01754 0.00406 0.00318 0.00091 AFIX 43 H38 2 0.374177 0.278281 0.740773 11.00000 -1.20000 AFIX 0 O1 3 0.960229 0.313201 0.804705 11.00000 0.01092 0.01720 = 0.01848 0.00842 0.00160 0.00327 O2 3 0.625891 0.383150 0.642031 11.00000 0.00819 0.02300 = 0.01457 0.00849 0.00224 0.00089 P1 4 0.891990 0.229744 0.837140 11.00000 0.01285 0.01334 = 0.01432 0.00477 0.00221 0.00260 P2 4 0.578463 0.346198 0.719982 11.00000 0.00939 0.01367 = 0.01316 0.00449 0.00287 0.00120 MOLE 2 C41 1 0.678261 0.174080 0.999110 11.00000 0.02250 0.01657 = 0.02203 0.01037 0.01061 0.00744 C42 1 0.778139 0.220144 1.048311 11.00000 0.02459 0.02792 = 0.02348 0.01308 0.00608 0.00288 AFIX 43 H42 2 0.819733 0.255752 1.020159 11.00000 -1.20000 AFIX 0 C43 1 0.818201 0.214645 1.139042 11.00000 0.03413 0.03793 = 0.02502 0.01330 0.00108 -0.00053 AFIX 43 H43 2 0.887618 0.244597 1.171732 11.00000 -1.20000 AFIX 0 C44 1 0.756763 0.165596 1.181204 11.00000 0.04307 0.03214 = 0.02208 0.01449 0.00955 0.01053 AFIX 43 H44 2 0.783466 0.162793 1.243192 11.00000 -1.20000 AFIX 0 C45 1 0.656391 0.120625 1.133015 11.00000 0.03785 0.02607 = 0.02940 0.01648 0.01907 0.01192 AFIX 43 H45 2 0.613962 0.087279 1.162058 11.00000 -1.20000 AFIX 0 C46 1 0.617642 0.124110 1.042556 11.00000 0.02485 0.02275 = 0.02925 0.01172 0.01288 0.00631 AFIX 43 H46 2 0.549017 0.092145 1.009626 11.00000 -1.20000 AFIX 0 C47 1 0.587538 0.048233 0.820417 11.00000 0.02261 0.01411 = 0.02968 0.00565 0.01459 -0.00006 C48 1 0.639225 -0.028460 0.853648 11.00000 0.03421 0.01728 = 0.04255 0.01128 0.02166 0.00566 AFIX 43 H48 2 0.687291 -0.013624 0.912588 11.00000 -1.20000 AFIX 0 C49 1 0.619469 -0.127875 0.799055 11.00000 0.05467 0.01680 = 0.06509 0.01399 0.03863 0.01029 AFIX 43 H49 2 0.655278 -0.180332 0.821019 11.00000 -1.20000 AFIX 0 C50 1 0.549573 -0.150279 0.714882 11.00000 0.06129 0.01652 = 0.05703 -0.00482 0.03832 -0.00707 AFIX 43 H50 2 0.536040 -0.218227 0.679144 11.00000 -1.20000 AFIX 0 C51 1 0.498580 -0.074660 0.681580 11.00000 0.04417 0.02709 = 0.03743 -0.00631 0.02010 -0.01293 AFIX 43 H51 2 0.450262 -0.090427 0.622736 11.00000 -1.20000 AFIX 0 C52 1 0.517660 0.024818 0.733928 11.00000 0.02810 0.02016 = 0.03120 0.00123 0.01211 -0.00358 AFIX 43 H52 2 0.482811 0.076934 0.710486 11.00000 -1.20000 AFIX 0 C53 1 0.497299 0.227913 0.891246 11.00000 0.01707 0.02178 = 0.01798 0.00885 0.00631 0.00553 C54 1 0.405946 0.163629 0.878925 11.00000 0.02112 0.02609 = 0.02903 0.01157 0.00847 0.00274 AFIX 43 H54 2 0.406799 0.092047 0.862038 11.00000 -1.20000 AFIX 0 C55 1 0.313977 0.203314 0.891114 11.00000 0.01731 0.04418 = 0.03046 0.01665 0.00732 0.00352 AFIX 43 H55 2 0.252273 0.158923 0.882907 11.00000 -1.20000 AFIX 0 C56 1 0.311860 0.307708 0.915269 11.00000 0.02236 0.05138 = 0.02443 0.01677 0.01079 0.01808 AFIX 43 H56 2 0.248401 0.334833 0.922500 11.00000 -1.20000 AFIX 0 C57 1 0.402135 0.372288 0.928824 11.00000 0.03212 0.03028 = 0.01859 0.00961 0.00976 0.01595 AFIX 43 H57 2 0.400767 0.443792 0.945824 11.00000 -1.20000 AFIX 0 C58 1 0.495070 0.332800 0.917622 11.00000 0.02350 0.02255 = 0.01542 0.00834 0.00692 0.00745 AFIX 43 H58 2 0.557215 0.377441 0.927977 11.00000 -1.20000 AFIX 0 P41 4 0.623270 0.181866 0.880409 11.00000 0.01527 0.01263 = 0.01843 0.00628 0.00608 0.00231 MOLE 3 C61 1 0.684679 0.164974 0.689413 11.00000 0.00880 0.01765 = 0.03921 0.01845 0.00717 0.00491 O61 3 0.668065 0.108823 0.626123 11.00000 0.02424 0.03249 = 0.02450 0.00921 0.00484 0.00736 MOLE 4 C71 1 0.863782 0.229507 0.510408 11.00000 0.04029 0.04528 = 0.02307 0.00363 0.00728 -0.00498 AFIX 13 H71 2 0.854050 0.274557 0.567293 11.00000 -1.20000 AFIX 0 CL71 5 0.932226 0.128913 0.539178 11.00000 0.08014 0.04622 = 0.06289 0.02704 -0.00575 -0.00628 CL72 5 0.933971 0.301396 0.457420 11.00000 0.05880 0.03570 = 0.03636 0.00836 0.02368 0.00146 CL73 5 0.740384 0.182079 0.436374 11.00000 0.04297 0.11059 = 0.06027 0.01675 0.00069 -0.02105 HKLF 4 Covalent radii and connectivity table for 2005src0806b in P-1 C 0.770 H 0.320 O 0.660 P 1.100 CL 0.990 RU 1.330 Cl1 - Ru1 Ru1 - C61 C1 P1 P2 P41 Cl1 C1 - C2 C6 Ru1 C2 - C1 O1 C3 C3 - C4 C2 C7 C4 - C5 C3 C5 - C4 C6 C11 C6 - C1 C5 O2 C7 - C10 C3 C8 C9 C8 - C7 C9 - C7 C10 - C7 C11 - C14 C13 C12 C5 C12 - C11 C13 - C11 C14 - C11 C15 - C20 C16 P1 C16 - C17 C15 C17 - C18 C16 C18 - C17 C19 C19 - C18 C20 C20 - C19 C15 C21 - C26 C22 P1 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - C21 C25 C27 - C32 C28 P2 C28 - C29 C27 C29 - C30 C28 C30 - C29 C31 C31 - C30 C32 C32 - C27 C31 C33 - C38 C34 P2 C34 - C35 C33 C35 - C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - C37 C33 O1 - C2 P1 O2 - C6 P2 P1 - O1 C15 C21 Ru1 P2 - O2 C27 C33 Ru1 C41 - C42 C46 P41 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 C45 - C44 C46 C46 - C45 C41 C47 - C52 C48 P41 C48 - C47 C49 C49 - C50 C48 C50 - C49 C51 C51 - C50 C52 C52 - C47 C51 C53 - C54 C58 P41 C54 - C55 C53 C55 - C54 C56 C56 - C57 C55 C57 - C56 C58 C58 - C57 C53 P41 - C47 C53 C41 Ru1 C61 - O61 Ru1 O61 - C61 C71 - Cl73 Cl71 Cl72 Cl71 - C71 Cl72 - C71 Cl73 - C71 56593 Reflections read, of which 100 rejected -16 =< h =< 17, -17 =< k =< 17, -20 =< l =< 20, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 3 0 -0.35 0.06 4 0.63 5 11 3 37.53 1.57 4 9.30 -8 5 4 26.97 0.64 3 4.45 -4 0 12 30.01 0.88 3 5.18 4 Inconsistent equivalents 11904 Unique reflections, of which 0 suppressed R(int) = 0.0320 R(sigma) = 0.0287 Friedel opposites merged Maximum memory for data reduction = 5821 / 119556 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 = 7605 / 867270 wR2 = 0.0827 before cycle 1 for 11904 data and 629 / 629 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41612 0.00041 1.924 OSF 2 0.00111 0.00026 4.288 EXTI Mean shift/esd = 0.174 Maximum = 4.288 for EXTI Max. shift = 0.004 A for H14C Max. dU = 0.000 for Cl73 Least-squares cycle 2 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 2 for 11904 data and 629 / 629 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41639 0.00042 0.642 OSF 2 0.00160 0.00028 1.758 EXTI Mean shift/esd = 0.060 Maximum = 1.758 for EXTI Max. shift = 0.001 A for H14C Max. dU = 0.000 for Cl73 Least-squares cycle 3 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 3 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 0.060 OSF 2 0.00162 0.00029 0.071 EXTI Mean shift/esd = 0.004 Maximum = 0.071 for EXTI Max. shift = 0.000 A for H9B Max. dU = 0.000 for Cl73 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 4 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 0.001 OSF 2 0.00162 0.00029 0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for U22 C61 Max. shift = 0.000 A for H13A Max. dU = 0.000 for C58 Least-squares cycle 5 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 5 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 -0.001 OSF 2 0.00162 0.00029 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U22 Ru1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C23 Least-squares cycle 6 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 6 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 0.000 OSF 2 0.00162 0.00029 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for x Ru1 Max. shift = 0.000 A for H10A Max. dU = 0.000 for C23 Least-squares cycle 7 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 7 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 -0.001 OSF 2 0.00162 0.00029 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for x Ru1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C36 Least-squares cycle 8 Maximum vector length = 511 Memory required = 7605 / 867270 wR2 = 0.0822 before cycle 8 for 11904 data and 629 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41641 0.00042 0.000 OSF 2 0.00162 0.00029 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for x Ru1 Max. shift = 0.000 A for C71 Max. dU = 0.000 for C13 Largest correlation matrix elements 0.595 EXTI / OSF 0.571 U13 C49 / U33 C49 0.558 U13 C50 / U11 C50 0.572 U11 Ru1 / OSF 0.570 U33 Ru1 / OSF 0.552 U13 C49 / U11 C49 0.571 U22 Ru1 / OSF 0.568 U13 C50 / U33 C50 0.512 U23 C61 / U33 C61 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.9260 0.5306 0.6267 43 0.950 0.000 C4 C5 C3 H8A 1.0984 0.3261 0.6349 137 0.980 0.000 C8 C7 H8A H8B 1.0994 0.2995 0.7307 137 0.980 0.000 C8 C7 H8A H8C 1.2001 0.3623 0.7198 137 0.980 0.000 C8 C7 H8A H9A 1.2001 0.5063 0.8479 137 0.980 0.000 C9 C7 H9A H9B 1.1040 0.4458 0.8680 137 0.980 0.000 C9 C7 H9A H9C 1.0944 0.5585 0.8528 137 0.980 0.000 C9 C7 H9A H10A 1.0815 0.5007 0.6151 137 0.980 0.000 C10 C7 H10A H10B 1.1892 0.5332 0.6941 137 0.980 0.000 C10 C7 H10A H10C 1.0880 0.5919 0.7016 137 0.980 0.000 C10 C7 H10A H12A 0.6079 0.6370 0.5714 137 0.980 0.000 C12 C11 H12A H12B 0.6903 0.6432 0.6678 137 0.980 0.000 C12 C11 H12A H12C 0.5964 0.5526 0.6275 137 0.980 0.000 C12 C11 H12A H13A 0.6083 0.4969 0.4362 137 0.980 0.000 C13 C11 H13A H13B 0.6038 0.4111 0.4922 137 0.980 0.000 C13 C11 H13A H13C 0.6971 0.4203 0.4436 137 0.980 0.000 C13 C11 H13A H14A 0.8362 0.5672 0.5039 137 0.980 0.000 C14 C11 H14A H14B 0.8307 0.6552 0.5893 137 0.980 0.000 C14 C11 H14A H14C 0.7452 0.6413 0.4932 137 0.980 0.000 C14 C11 H14A H16 1.0076 0.3987 0.9804 43 0.950 0.000 C16 C17 C15 H17 1.1158 0.4179 1.1282 43 0.950 0.000 C17 C18 C16 H18 1.1523 0.2753 1.1870 43 0.950 0.000 C18 C17 C19 H19 1.0842 0.1132 1.0979 43 0.950 0.000 C19 C18 C20 H20 0.9755 0.0930 0.9503 43 0.950 0.000 C20 C19 C15 H22 1.0721 0.1565 0.7787 43 0.950 0.000 C22 C23 C21 H23 1.1121 -0.0005 0.7063 43 0.950 0.000 C23 C22 C24 H24 0.9883 -0.1432 0.6648 43 0.950 0.000 C24 C25 C23 H25 0.8243 -0.1296 0.6952 43 0.950 0.000 C25 C24 C26 H26 0.7824 0.0279 0.7659 43 0.950 0.000 C26 C21 C25 H28 0.6925 0.5236 0.8292 43 0.950 0.000 C28 C29 C27 H29 0.6601 0.6869 0.8929 43 0.950 0.000 C29 C30 C28 H30 0.4874 0.7280 0.8749 43 0.950 0.000 C30 C29 C31 H31 0.3469 0.6066 0.7897 43 0.950 0.000 C31 C30 C32 H32 0.3778 0.4428 0.7229 43 0.950 0.000 C32 C27 C31 H34 0.5176 0.2313 0.5338 43 0.950 0.000 C34 C35 C33 H35 0.3761 0.1126 0.4444 43 0.950 0.000 C35 C36 C34 H36 0.2341 0.0764 0.5021 43 0.950 0.000 C36 C37 C35 H37 0.2320 0.1615 0.6492 43 0.950 0.000 C37 C36 C38 H38 0.3741 0.2783 0.7407 43 0.950 0.000 C38 C37 C33 H42 0.8198 0.2557 1.0202 43 0.950 0.000 C42 C41 C43 H43 0.8874 0.2445 1.1717 43 0.950 0.000 C43 C44 C42 H44 0.7835 0.1627 1.2431 43 0.950 0.000 C44 C43 C45 H45 0.6140 0.0873 1.1620 43 0.950 0.000 C45 C44 C46 H46 0.5491 0.0921 1.0096 43 0.950 0.000 C46 C45 C41 H48 0.6874 -0.0136 0.9124 43 0.950 0.000 C48 C47 C49 H49 0.6552 -0.1802 0.8211 43 0.950 0.000 C49 C50 C48 H50 0.5360 -0.2183 0.6792 43 0.950 0.000 C50 C49 C51 H51 0.4503 -0.0904 0.6228 43 0.950 0.000 C51 C50 C52 H52 0.4828 0.0769 0.7106 43 0.950 0.000 C52 C47 C51 H54 0.4068 0.0920 0.8621 43 0.950 0.000 C54 C55 C53 H55 0.2524 0.1590 0.8829 43 0.950 0.000 C55 C54 C56 H56 0.2484 0.3348 0.9225 43 0.950 0.000 C56 C57 C55 H57 0.4007 0.4436 0.9457 43 0.950 0.000 C57 C56 C58 H58 0.5571 0.3775 0.9280 43 0.950 0.000 C58 C57 C53 H71 0.8540 0.2744 0.5673 13 1.000 0.000 C71 Cl73 Cl71 Cl72 2005src0806b in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl1 0.77536 0.40885 0.93385 1.00000 0.02265 0.01912 0.01872 0.00537 0.00292 0.00239 0.02046 0.00106 0.00004 0.00004 0.00003 0.00000 0.00025 0.00024 0.00024 0.00019 0.00019 0.00019 0.00011 Ru1 0.71805 0.26955 0.79713 1.00000 0.01076 0.01089 0.01155 0.00340 0.00269 0.00127 0.01099 0.00031 0.00001 0.00001 0.00001 0.00000 0.00008 0.00008 0.00008 0.00006 0.00006 0.00005 0.00005 C1 0.79328 0.35400 0.72806 1.00000 0.01147 0.01279 0.01193 0.00181 0.00255 0.00138 0.01232 0.00392 0.00014 0.00014 0.00013 0.00000 0.00086 0.00087 0.00087 0.00069 0.00069 0.00068 0.00036 C2 0.90235 0.36764 0.74608 1.00000 0.01286 0.01390 0.01179 0.00363 0.00222 0.00365 0.01285 0.00399 0.00015 0.00014 0.00013 0.00000 0.00088 0.00089 0.00088 0.00071 0.00070 0.00070 0.00036 C3 0.95622 0.43278 0.70928 1.00000 0.01192 0.01810 0.01199 0.00248 0.00342 0.00180 0.01411 0.00405 0.00015 0.00015 0.00013 0.00000 0.00088 0.00095 0.00089 0.00073 0.00071 0.00072 0.00037 C4 0.89195 0.48405 0.65139 1.00000 0.01379 0.01966 0.01385 0.00570 0.00570 0.00097 0.01515 0.00417 0.00015 0.00015 0.00013 0.00000 0.00090 0.00097 0.00091 0.00076 0.00073 0.00074 0.00038 H4 0.92604 0.53056 0.62674 1.00000 0.01818 0.00000 0.00000 C5 0.78184 0.47228 0.62703 1.00000 0.01403 0.01902 0.01255 0.00545 0.00408 0.00281 0.01478 0.00416 0.00015 0.00015 0.00013 0.00000 0.00091 0.00097 0.00090 0.00075 0.00073 0.00073 0.00038 C6 0.73596 0.40353 0.66572 1.00000 0.00916 0.01716 0.01288 0.00356 0.00298 0.00127 0.01305 0.00398 0.00014 0.00014 0.00013 0.00000 0.00084 0.00093 0.00089 0.00072 0.00069 0.00069 0.00036 C7 1.07698 0.45040 0.73120 1.00000 0.01000 0.02389 0.01735 0.00582 0.00289 0.00120 0.01707 0.00427 0.00015 0.00016 0.00014 0.00000 0.00087 0.00104 0.00097 0.00080 0.00074 0.00075 0.00040 C8 1.12289 0.35055 0.70144 1.00000 0.01353 0.03108 0.02840 0.00675 0.00877 0.00552 0.02367 0.00486 0.00016 0.00017 0.00016 0.00000 0.00096 0.00119 0.00117 0.00094 0.00086 0.00085 0.00046 H8A 1.09841 0.32612 0.63488 1.00000 0.03550 0.00000 0.00000 H8B 1.09942 0.29948 0.73065 1.00000 0.03550 0.00000 0.00000 H8C 1.20014 0.36232 0.71979 1.00000 0.03550 0.00000 0.00000 C9 1.12303 0.49421 0.83431 1.00000 0.01354 0.02751 0.02022 0.00710 -0.00034 -0.00234 0.02120 0.00437 0.00016 0.00017 0.00014 0.00000 0.00094 0.00112 0.00105 0.00086 0.00079 0.00080 0.00043 H9A 1.20005 0.50633 0.84789 1.00000 0.03181 0.00000 0.00000 H9B 1.10397 0.44576 0.86796 1.00000 0.03181 0.00000 0.00000 H9C 1.09442 0.55847 0.85283 1.00000 0.03181 0.00000 0.00000 C10 1.11206 0.52581 0.68100 1.00000 0.01369 0.03431 0.02439 0.01165 0.00424 -0.00192 0.02368 0.00477 0.00016 0.00018 0.00015 0.00000 0.00096 0.00124 0.00112 0.00095 0.00084 0.00086 0.00046 H10A 1.08147 0.50066 0.61507 1.00000 0.03552 0.00000 0.00000 H10B 1.18923 0.53322 0.69409 1.00000 0.03552 0.00000 0.00000 H10C 1.08799 0.59194 0.70163 1.00000 0.03552 0.00000 0.00000 C11 0.71763 0.53235 0.56297 1.00000 0.01535 0.02845 0.02222 0.01626 0.00580 0.00490 0.02014 0.00473 0.00016 0.00017 0.00015 0.00000 0.00096 0.00113 0.00106 0.00089 0.00081 0.00082 0.00043 C12 0.64662 0.59716 0.61187 1.00000 0.02196 0.03437 0.03807 0.02487 0.01352 0.01423 0.02749 0.00567 0.00018 0.00019 0.00017 0.00000 0.00110 0.00127 0.00134 0.00108 0.00098 0.00095 0.00051 H12A 0.60795 0.63697 0.57145 1.00000 0.04123 0.00000 0.00000 H12B 0.69025 0.64325 0.66781 1.00000 0.04123 0.00000 0.00000 H12C 0.59636 0.55260 0.62753 1.00000 0.04123 0.00000 0.00000 C13 0.65067 0.45853 0.47588 1.00000 0.02823 0.05038 0.02033 0.01895 -0.00194 -0.00186 0.03302 0.00524 0.00019 0.00021 0.00016 0.00000 0.00123 0.00157 0.00115 0.00109 0.00095 0.00109 0.00056 H13A 0.60829 0.49693 0.43617 1.00000 0.04953 0.00000 0.00000 H13B 0.60384 0.41114 0.49219 1.00000 0.04953 0.00000 0.00000 H13C 0.69710 0.42035 0.44363 1.00000 0.04953 0.00000 0.00000 C14 0.78884 0.60561 0.53482 1.00000 0.02045 0.03795 0.03413 0.02563 0.00905 0.00683 0.02768 0.00549 0.00018 0.00019 0.00017 0.00000 0.00108 0.00132 0.00129 0.00108 0.00095 0.00095 0.00051 H14A 0.83623 0.56725 0.50388 1.00000 0.04152 0.00000 0.00000 H14B 0.83066 0.65519 0.58932 1.00000 0.04152 0.00000 0.00000 H14C 0.74522 0.64128 0.49324 1.00000 0.04152 0.00000 0.00000 C15 0.97999 0.24389 0.95051 1.00000 0.01488 0.01959 0.01686 0.00675 0.00147 0.00314 0.01715 0.00429 0.00015 0.00015 0.00014 0.00000 0.00092 0.00099 0.00097 0.00078 0.00076 0.00076 0.00040 C16 1.02265 0.34044 1.00413 1.00000 0.01548 0.02112 0.01914 0.00626 0.00433 0.00217 0.01837 0.00436 0.00016 0.00016 0.00014 0.00000 0.00094 0.00102 0.00101 0.00081 0.00078 0.00077 0.00041 H16 1.00763 0.39869 0.98040 1.00000 0.02204 0.00000 0.00000 C17 1.08697 0.35195 1.09203 1.00000 0.01788 0.02884 0.02273 0.00259 0.00171 -0.00209 0.02450 0.00470 0.00017 0.00018 0.00015 0.00000 0.00102 0.00117 0.00111 0.00090 0.00085 0.00086 0.00046 H17 1.11576 0.41788 1.12819 1.00000 0.02940 0.00000 0.00000 C18 1.10897 0.26733 1.12671 1.00000 0.03039 0.04136 0.02176 0.00878 -0.00589 0.00537 0.03317 0.00529 0.00020 0.00020 0.00017 0.00000 0.00127 0.00144 0.00117 0.00104 0.00097 0.00107 0.00056 H18 1.15234 0.27529 1.18701 1.00000 0.03981 0.00000 0.00000 C19 1.06814 0.17115 1.07404 1.00000 0.04976 0.03232 0.02907 0.01623 -0.00801 0.00660 0.03884 0.00563 0.00023 0.00020 0.00018 0.00000 0.00163 0.00136 0.00132 0.00109 0.00117 0.00118 0.00064 H19 1.08417 0.11316 1.09792 1.00000 0.04661 0.00000 0.00000 C20 1.00365 0.15922 0.98619 1.00000 0.03816 0.02201 0.02427 0.00885 -0.00356 0.00277 0.02973 0.00511 0.00020 0.00018 0.00016 0.00000 0.00135 0.00114 0.00117 0.00092 0.00100 0.00097 0.00053 H20 0.97555 0.09302 0.95026 1.00000 0.03567 0.00000 0.00000 C21 0.92250 0.10794 0.77851 1.00000 0.01948 0.01941 0.01552 0.00539 0.00268 0.00662 0.01811 0.00442 0.00016 0.00016 0.00014 0.00000 0.00099 0.00100 0.00095 0.00078 0.00078 0.00078 0.00040 C22 1.02112 0.09866 0.76124 1.00000 0.02330 0.02632 0.03875 0.01134 0.01064 0.00925 0.02818 0.00542 0.00018 0.00018 0.00017 0.00000 0.00113 0.00118 0.00136 0.00102 0.00100 0.00092 0.00050 H22 1.07209 0.15648 0.77872 1.00000 0.03382 0.00000 0.00000 C23 1.04504 0.00539 0.71867 1.00000 0.03838 0.03852 0.04877 0.01561 0.02473 0.02357 0.03796 0.00651 0.00022 0.00021 0.00020 0.00000 0.00144 0.00147 0.00162 0.00124 0.00126 0.00119 0.00062 H23 1.11209 -0.00048 0.70635 1.00000 0.04555 0.00000 0.00000 C24 0.97156 -0.07930 0.69402 1.00000 0.05368 0.02563 0.03284 0.00420 0.01600 0.01994 0.03639 0.00601 0.00023 0.00019 0.00018 0.00000 0.00167 0.00125 0.00135 0.00103 0.00121 0.00117 0.00060 H24 0.98825 -0.14320 0.66478 1.00000 0.04367 0.00000 0.00000 C25 0.87442 -0.07120 0.71176 1.00000 0.03871 0.01794 0.02715 0.00358 0.00160 0.00654 0.02933 0.00515 0.00020 0.00017 0.00016 0.00000 0.00135 0.00108 0.00120 0.00091 0.00102 0.00095 0.00052 H25 0.82428 -0.12956 0.69524 1.00000 0.03520 0.00000 0.00000 C26 0.84964 0.02244 0.75388 1.00000 0.02268 0.01972 0.01959 0.00536 0.00343 0.00619 0.02078 0.00456 0.00017 0.00016 0.00014 0.00000 0.00105 0.00103 0.00103 0.00082 0.00083 0.00082 0.00043 H26 0.78238 0.02789 0.76585 1.00000 0.02493 0.00000 0.00000 C27 0.53834 0.46604 0.77145 1.00000 0.01613 0.01445 0.01348 0.00747 0.00524 0.00311 0.01374 0.00416 0.00015 0.00014 0.00013 0.00000 0.00092 0.00090 0.00090 0.00072 0.00073 0.00072 0.00037 C28 0.62195 0.54007 0.82126 1.00000 0.01674 0.01761 0.01686 0.00742 0.00108 0.00172 0.01714 0.00425 0.00016 0.00015 0.00014 0.00000 0.00095 0.00096 0.00096 0.00078 0.00076 0.00075 0.00040 H28 0.69253 0.52363 0.82917 1.00000 0.02057 0.00000 0.00000 C29 0.60273 0.63704 0.85912 1.00000 0.02749 0.01785 0.01622 0.00504 0.00158 -0.00126 0.02123 0.00452 0.00018 0.00016 0.00014 0.00000 0.00111 0.00101 0.00099 0.00080 0.00084 0.00083 0.00043 H29 0.66006 0.68692 0.89290 1.00000 0.02548 0.00000 0.00000 C30 0.50054 0.66160 0.84798 1.00000 0.03288 0.01706 0.02732 0.00425 0.01242 0.00676 0.02494 0.00498 0.00019 0.00017 0.00016 0.00000 0.00122 0.00103 0.00117 0.00087 0.00097 0.00089 0.00047 H30 0.48739 0.72798 0.87486 1.00000 0.02993 0.00000 0.00000 C31 0.41720 0.58933 0.79758 1.00000 0.02024 0.02413 0.03760 0.00841 0.01200 0.00884 0.02611 0.00512 0.00018 0.00017 0.00017 0.00000 0.00107 0.00113 0.00132 0.00097 0.00096 0.00087 0.00048 H31 0.34690 0.60658 0.78967 1.00000 0.03134 0.00000 0.00000 C32 0.43531 0.49167 0.75839 1.00000 0.01649 0.01968 0.02418 0.00586 0.00536 0.00193 0.02000 0.00461 0.00016 0.00016 0.00015 0.00000 0.00097 0.00102 0.00108 0.00083 0.00082 0.00078 0.00042 H32 0.37779 0.44277 0.72295 1.00000 0.02399 0.00000 0.00000 C33 0.46065 0.26702 0.64672 1.00000 0.01191 0.01458 0.01464 0.00398 0.00025 0.00154 0.01419 0.00401 0.00015 0.00014 0.00013 0.00000 0.00087 0.00091 0.00092 0.00073 0.00072 0.00070 0.00037 C34 0.46014 0.21703 0.55789 1.00000 0.01796 0.02200 0.01913 0.00335 0.00579 0.00099 0.01980 0.00442 0.00016 0.00016 0.00014 0.00000 0.00098 0.00104 0.00102 0.00082 0.00081 0.00080 0.00042 H34 0.51764 0.23133 0.53380 1.00000 0.02376 0.00000 0.00000 C35 0.37572 0.14645 0.50468 1.00000 0.02717 0.02597 0.01917 -0.00286 0.00254 -0.00222 0.02619 0.00466 0.00018 0.00017 0.00015 0.00000 0.00116 0.00115 0.00107 0.00088 0.00089 0.00091 0.00048 H35 0.37606 0.11260 0.44444 1.00000 0.03143 0.00000 0.00000 C36 0.29126 0.12510 0.53864 1.00000 0.02229 0.02307 0.02655 0.00078 0.00002 -0.00787 0.02627 0.00463 0.00018 0.00017 0.00016 0.00000 0.00109 0.00112 0.00117 0.00091 0.00090 0.00087 0.00048 H36 0.23410 0.07636 0.50214 1.00000 0.03153 0.00000 0.00000 C37 0.29053 0.17513 0.62608 1.00000 0.01393 0.02420 0.02795 0.00724 0.00446 -0.00221 0.02219 0.00454 0.00016 0.00016 0.00015 0.00000 0.00095 0.00109 0.00115 0.00090 0.00084 0.00081 0.00044 H37 0.23199 0.16155 0.64917 1.00000 0.02662 0.00000 0.00000 C38 0.37486 0.24514 0.68040 1.00000 0.01355 0.01797 0.01737 0.00431 0.00311 0.00106 0.01646 0.00423 0.00015 0.00015 0.00014 0.00000 0.00091 0.00096 0.00097 0.00077 0.00075 0.00074 0.00039 H38 0.37415 0.27829 0.74072 1.00000 0.01975 0.00000 0.00000 O1 0.96022 0.31320 0.80472 1.00000 0.01079 0.01713 0.01838 0.00855 0.00152 0.00312 0.01510 0.00288 0.00010 0.00010 0.00009 0.00000 0.00062 0.00068 0.00070 0.00055 0.00053 0.00052 0.00028 O2 0.62587 0.38315 0.64204 1.00000 0.00814 0.02301 0.01454 0.00849 0.00227 0.00086 0.01474 0.00286 0.00010 0.00011 0.00009 0.00000 0.00061 0.00072 0.00067 0.00056 0.00051 0.00052 0.00028 P1 0.89199 0.22975 0.83714 1.00000 0.01292 0.01334 0.01445 0.00480 0.00228 0.00254 0.01352 0.00105 0.00004 0.00004 0.00003 0.00000 0.00023 0.00023 0.00024 0.00018 0.00019 0.00018 0.00010 P2 0.57847 0.34619 0.71998 1.00000 0.00940 0.01371 0.01316 0.00450 0.00290 0.00115 0.01189 0.00102 0.00004 0.00004 0.00003 0.00000 0.00022 0.00023 0.00023 0.00018 0.00018 0.00017 0.00010 C41 0.67827 0.17410 0.99907 1.00000 0.02271 0.01619 0.02194 0.01012 0.01059 0.00766 0.01834 0.00463 0.00016 0.00015 0.00014 0.00000 0.00103 0.00096 0.00104 0.00080 0.00084 0.00079 0.00041 C42 0.77811 0.22008 1.04833 1.00000 0.02476 0.02809 0.02360 0.01310 0.00650 0.00296 0.02435 0.00492 0.00018 0.00017 0.00015 0.00000 0.00111 0.00117 0.00112 0.00092 0.00090 0.00090 0.00046 H42 0.81978 0.25567 1.02023 1.00000 0.02922 0.00000 0.00000 C43 0.81803 0.21454 1.13899 1.00000 0.03379 0.03741 0.02544 0.01325 0.00069 -0.00033 0.03271 0.00546 0.00021 0.00020 0.00017 0.00000 0.00132 0.00139 0.00122 0.00104 0.00102 0.00107 0.00055 H43 0.88743 0.24452 1.17171 1.00000 0.03925 0.00000 0.00000 C44 0.75673 0.16555 1.18114 1.00000 0.04292 0.03242 0.02176 0.01472 0.00949 0.01076 0.03063 0.00558 0.00021 0.00019 0.00016 0.00000 0.00144 0.00128 0.00115 0.00098 0.00103 0.00108 0.00053 H44 0.78345 0.16272 1.24311 1.00000 0.03676 0.00000 0.00000 C45 0.65646 0.12065 1.13297 1.00000 0.03775 0.02597 0.02955 0.01636 0.01925 0.01207 0.02737 0.00549 0.00020 0.00018 0.00016 0.00000 0.00132 0.00116 0.00122 0.00097 0.00104 0.00099 0.00050 H45 0.61402 0.08732 1.16202 1.00000 0.03284 0.00000 0.00000 C46 0.61771 0.12410 1.04256 1.00000 0.02471 0.02250 0.02904 0.01135 0.01271 0.00635 0.02343 0.00511 0.00018 0.00017 0.00016 0.00000 0.00111 0.00108 0.00118 0.00091 0.00093 0.00086 0.00045 H46 0.54910 0.09209 1.00964 1.00000 0.02812 0.00000 0.00000 C47 0.58753 0.04821 0.82040 1.00000 0.02261 0.01413 0.02920 0.00573 0.01473 -0.00021 0.02054 0.00467 0.00017 0.00015 0.00015 0.00000 0.00104 0.00095 0.00116 0.00083 0.00089 0.00079 0.00043 C48 0.63920 -0.02848 0.85353 1.00000 0.03379 0.01775 0.04244 0.01156 0.02187 0.00574 0.02839 0.00564 0.00020 0.00017 0.00018 0.00000 0.00127 0.00107 0.00141 0.00098 0.00110 0.00092 0.00051 H48 0.68737 -0.01363 0.91242 1.00000 0.03407 0.00000 0.00000 C49 0.61939 -0.12780 0.79908 1.00000 0.05453 0.01678 0.06467 0.01432 0.03862 0.01005 0.04023 0.00672 0.00024 0.00018 0.00022 0.00000 0.00174 0.00115 0.00197 0.00120 0.00156 0.00112 0.00068 H49 0.65516 -0.18024 0.82112 1.00000 0.04828 0.00000 0.00000 C50 0.54954 -0.15029 0.71495 1.00000 0.06139 0.01644 0.05689 -0.00490 0.03861 -0.00735 0.04330 0.00642 0.00025 0.00019 0.00022 0.00000 0.00187 0.00117 0.00188 0.00116 0.00159 0.00116 0.00073 H50 0.53600 -0.21826 0.67925 1.00000 0.05196 0.00000 0.00000 C51 0.49856 -0.07466 0.68162 1.00000 0.04380 0.02732 0.03729 -0.00624 0.02001 -0.01278 0.03722 0.00557 0.00022 0.00019 0.00019 0.00000 0.00151 0.00129 0.00145 0.00108 0.00121 0.00110 0.00062 H51 0.45027 -0.09040 0.62277 1.00000 0.04466 0.00000 0.00000 C52 0.51767 0.02476 0.73398 1.00000 0.02857 0.02003 0.03133 0.00155 0.01272 -0.00317 0.02668 0.00487 0.00018 0.00017 0.00016 0.00000 0.00118 0.00109 0.00125 0.00092 0.00098 0.00089 0.00049 H52 0.48281 0.07687 0.71055 1.00000 0.03201 0.00000 0.00000 C53 0.49729 0.22793 0.89127 1.00000 0.01741 0.02165 0.01759 0.00891 0.00636 0.00555 0.01776 0.00449 0.00016 0.00016 0.00014 0.00000 0.00096 0.00102 0.00098 0.00081 0.00078 0.00079 0.00040 C54 0.40597 0.16363 0.87895 1.00000 0.02127 0.02579 0.02846 0.01149 0.00848 0.00279 0.02401 0.00496 0.00017 0.00018 0.00016 0.00000 0.00106 0.00114 0.00117 0.00093 0.00090 0.00087 0.00046 H54 0.40681 0.09205 0.86207 1.00000 0.02881 0.00000 0.00000 C55 0.31410 0.20338 0.89115 1.00000 0.01711 0.04420 0.03036 0.01682 0.00734 0.00323 0.02909 0.00539 0.00018 0.00020 0.00016 0.00000 0.00105 0.00144 0.00125 0.00108 0.00092 0.00097 0.00051 H55 0.25240 0.15898 0.88294 1.00000 0.03491 0.00000 0.00000 C56 0.31188 0.30764 0.91529 1.00000 0.02256 0.05141 0.02401 0.01684 0.01070 0.01838 0.03006 0.00557 0.00018 0.00020 0.00016 0.00000 0.00114 0.00155 0.00117 0.00108 0.00094 0.00106 0.00054 H56 0.24842 0.33476 0.92254 1.00000 0.03608 0.00000 0.00000 C57 0.40213 0.37212 0.92878 1.00000 0.03232 0.02996 0.01817 0.00954 0.00967 0.01573 0.02521 0.00519 0.00018 0.00018 0.00015 0.00000 0.00122 0.00120 0.00105 0.00090 0.00092 0.00097 0.00048 H57 0.40073 0.44363 0.94574 1.00000 0.03025 0.00000 0.00000 C58 0.49502 0.33279 0.91765 1.00000 0.02325 0.02236 0.01480 0.00812 0.00671 0.00695 0.01908 0.00462 0.00017 0.00016 0.00014 0.00000 0.00105 0.00104 0.00095 0.00080 0.00080 0.00083 0.00041 H58 0.55714 0.37747 0.92803 1.00000 0.02289 0.00000 0.00000 P41 0.62326 0.18185 0.88039 1.00000 0.01537 0.01264 0.01840 0.00631 0.00612 0.00225 0.01472 0.00110 0.00004 0.00004 0.00004 0.00000 0.00024 0.00023 0.00025 0.00019 0.00020 0.00018 0.00011 C61 0.68472 0.16503 0.68945 1.00000 0.00867 0.01749 0.03843 0.01831 0.00720 0.00502 0.01938 0.00496 0.00015 0.00016 0.00017 0.00000 0.00088 0.00100 0.00134 0.00099 0.00086 0.00074 0.00044 O61 0.66812 0.10882 0.62617 1.00000 0.02402 0.03229 0.02464 0.00955 0.00485 0.00719 0.02665 0.00362 0.00012 0.00013 0.00011 0.00000 0.00082 0.00091 0.00087 0.00076 0.00067 0.00068 0.00034 C71 0.86373 0.22938 0.51041 1.00000 0.04073 0.04499 0.02329 0.00334 0.00717 -0.00543 0.03765 0.00556 0.00022 0.00022 0.00017 0.00000 0.00148 0.00156 0.00124 0.00110 0.00109 0.00120 0.00060 H71 0.85400 0.27440 0.56731 1.00000 0.04518 0.00000 0.00000 Cl71 0.93223 0.12886 0.53909 1.00000 0.08043 0.04634 0.06295 0.02717 -0.00557 -0.00618 0.06582 0.00190 0.00008 0.00006 0.00006 0.00000 0.00062 0.00045 0.00053 0.00040 0.00045 0.00041 0.00025 Cl72 0.93389 0.30137 0.45739 1.00000 0.05949 0.03602 0.03649 0.00846 0.02395 0.00164 0.04209 0.00156 0.00006 0.00005 0.00005 0.00000 0.00044 0.00035 0.00035 0.00028 0.00032 0.00030 0.00016 Cl73 0.74044 0.18203 0.43639 1.00000 0.04329 0.11139 0.06069 0.01682 0.00067 -0.02103 0.07570 0.00201 0.00007 0.00009 0.00007 0.00000 0.00046 0.00084 0.00056 0.00054 0.00040 0.00049 0.00030 Final Structure Factor Calculation for 2005src0806b in P-1 Total number of l.s. parameters = 629 Maximum vector length = 511 Memory required = 6976 / 25039 wR2 = 0.0822 before cycle 9 for 11904 data and 0 / 629 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0359 * P )^2 + 2.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0320 for 10460 Fo > 4sig(Fo) and 0.0394 for all 11904 data wR2 = 0.0822, GooF = S = 1.037, Restrained GooF = 1.037 for all data Occupancy sum of asymmetric unit = 69.00 for non-hydrogen and 55.00 for hydrogen atoms Principal mean square atomic displacements U 0.0247 0.0195 0.0171 Cl1 0.0120 0.0108 0.0101 Ru1 0.0140 0.0117 0.0112 C1 0.0158 0.0127 0.0100 C2 0.0186 0.0122 0.0115 C3 0.0200 0.0153 0.0101 C4 0.0192 0.0137 0.0114 C5 0.0172 0.0128 0.0091 C6 0.0241 0.0171 0.0100 C7 0.0314 0.0285 0.0111 C8 0.0306 0.0212 0.0119 C9 0.0374 0.0211 0.0126 C10 0.0342 0.0149 0.0114 C11 0.0506 0.0193 0.0125 C12 0.0567 0.0297 0.0126 C13 0.0501 0.0195 0.0134 C14 0.0209 0.0186 0.0120 C15 0.0218 0.0179 0.0154 C16 0.0319 0.0259 0.0157 C17 0.0448 0.0408 0.0140 C18 0.0670 0.0361 0.0135 C19 0.0490 0.0238 0.0163 C20 0.0244 0.0174 0.0125 C21 0.0392 0.0280 0.0173 C22 0.0604 0.0387 0.0147 C23 0.0595 0.0345 0.0151 C24 0.0457 0.0254 0.0169 C25 0.0265 0.0201 0.0157 C26 0.0180 0.0148 0.0083 C27 0.0225 0.0170 0.0119 C28 0.0314 0.0170 0.0153 C29 0.0346 0.0251 0.0152 C30 0.0379 0.0265 0.0140 C31 0.0243 0.0193 0.0163 C32 0.0179 0.0145 0.0102 C33 0.0234 0.0189 0.0171 C34 0.0342 0.0297 0.0146 C35 0.0348 0.0316 0.0124 C36 0.0293 0.0249 0.0124 C37 0.0184 0.0175 0.0135 C38 0.0220 0.0144 0.0089 O1 0.0244 0.0117 0.0081 O2 0.0158 0.0141 0.0107 P1 0.0147 0.0116 0.0093 P2 0.0283 0.0160 0.0108 C41 0.0322 0.0248 0.0161 C42 0.0457 0.0321 0.0204 C43 0.0455 0.0318 0.0146 C44 0.0460 0.0221 0.0141 C45 0.0333 0.0194 0.0176 C46 0.0335 0.0174 0.0107 C47 0.0483 0.0216 0.0152 C48 0.0785 0.0279 0.0143 C49 0.0875 0.0278 0.0146 C50 0.0660 0.0273 0.0184 C51 0.0387 0.0238 0.0175 C52 0.0244 0.0154 0.0135 C53 0.0314 0.0222 0.0184 C54 0.0468 0.0242 0.0163 C55 0.0561 0.0194 0.0148 C56 0.0424 0.0175 0.0157 C57 0.0269 0.0183 0.0120 C58 0.0192 0.0143 0.0107 P41 0.0418 0.0096 0.0067 C61 0.0336 0.0264 0.0200 O61 0.0548 0.0351 0.0231 C71 0.1110 0.0528 0.0336 Cl71 0.0634 0.0360 0.0268 Cl72 0.1260 0.0669 0.0342 Cl73 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.038 0.056 0.076 0.096 0.118 0.145 0.180 0.234 1.000 Number in group 1228. 1220. 1126. 1226. 1188. 1161. 1200. 1172. 1182. 1201. GooF 1.008 1.026 1.053 1.138 1.092 1.000 1.001 0.934 1.014 1.088 K 1.411 0.986 0.956 0.973 0.976 0.985 0.993 1.007 1.014 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 1192. 1194. 1213. 1165. 1199. 1181. 1187. 1196. 1177. 1200. GooF 0.925 0.904 0.902 0.866 0.894 0.839 0.879 0.885 1.064 1.819 K 0.973 0.990 1.003 1.004 1.008 1.016 1.022 1.023 1.009 0.991 R1 0.078 0.064 0.057 0.048 0.038 0.032 0.027 0.024 0.026 0.033 Recommended weighting scheme: WGHT 0.0319 3.1460 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) -1 -2 2 1102.42 2635.46 10.95 0.212 5.32 0 1 2 2101.71 4328.87 10.08 0.272 5.84 0 -2 2 2021.62 3799.28 9.28 0.255 5.58 -2 0 1 130.42 405.77 6.70 0.083 6.46 2 0 0 50.62 214.47 6.46 0.060 6.34 -4 -4 16 526.51 942.07 6.34 0.127 0.97 2 0 1 1591.84 3218.77 6.33 0.234 5.33 0 -3 6 79.24 8.32 6.25 0.012 2.38 1 -1 7 1454.58 1000.30 6.03 0.131 2.03 -4 -4 6 152.50 49.84 5.93 0.029 1.98 3 -5 4 276.51 505.25 5.77 0.093 2.04 -5 1 2 237.56 451.91 5.73 0.088 2.58 -6 2 0 245.81 460.08 5.72 0.089 2.08 2 -7 4 1060.68 717.36 5.62 0.111 1.77 3 4 0 532.53 325.46 5.37 0.075 2.47 -6 2 2 82.40 18.88 5.33 0.018 2.10 -2 -5 2 242.91 430.39 5.02 0.086 2.46 -2 0 8 242.58 429.96 4.97 0.086 1.89 -6 3 2 1854.15 2442.79 4.86 0.204 1.99 2 2 5 843.46 1177.71 4.81 0.142 2.12 1 -2 6 8.11 74.33 4.77 0.036 2.34 2 -5 5 891.90 1240.80 4.72 0.145 2.04 0 6 1 121.46 245.04 4.71 0.065 2.10 -1 -6 5 1045.72 769.42 4.50 0.115 1.99 2 -3 6 156.14 72.56 4.46 0.035 2.10 -1 2 5 144.66 263.80 4.31 0.067 2.55 4 1 3 7275.99 8768.56 4.31 0.387 2.27 -4 0 3 1856.05 1453.40 4.28 0.157 3.04 2 -2 7 717.51 989.24 4.27 0.130 1.90 -5 -3 5 320.51 496.05 4.24 0.092 2.05 2 2 3 28.53 0.59 4.21 0.003 2.81 -1 8 2 144.75 66.10 4.20 0.034 1.55 6 1 0 2767.74 2242.16 4.14 0.196 2.05 1 -3 7 119.08 48.42 4.14 0.029 1.99 -4 -4 8 394.55 258.07 4.13 0.066 1.71 -2 -5 1 4513.63 5457.83 4.12 0.305 2.43 -7 1 3 42.47 4.82 4.09 0.009 1.85 0 5 3 -0.12 43.24 4.08 0.027 2.12 -1 7 4 457.99 306.94 4.08 0.072 1.56 -5 -2 6 668.21 913.95 4.05 0.125 2.01 -1 -3 9 489.95 335.97 4.02 0.076 1.69 -7 2 1 349.06 224.50 4.00 0.062 1.83 -4 -4 4 610.72 836.94 3.99 0.119 2.22 -5 -3 7 1200.91 926.57 3.97 0.126 1.81 -3 0 6 1373.42 1731.29 3.85 0.172 2.40 -1 3 6 -0.93 35.42 3.85 0.025 2.00 -3 5 3 977.32 750.69 3.81 0.113 2.07 4 2 3 72.07 149.67 3.79 0.051 2.11 -2 -3 1 2839.80 3424.55 3.76 0.242 3.61 -2 -4 4 4931.18 5845.52 3.75 0.316 2.66 Bond lengths and angles Cl1 - Distance Angles Ru1 2.4468 (0.0006) Cl1 - Ru1 - Distance Angles C61 1.8850 (0.0025) C1 2.0888 (0.0019) 86.96 (0.08) P1 2.3408 (0.0005) 91.68 (0.06) 77.68 (0.05) P2 2.3524 (0.0005) 85.37 (0.06) 77.62 (0.05) 155.24 (0.02) P41 2.4345 (0.0005) 95.65 (0.06) 175.77 (0.05) 105.52 (0.02) 99.24 (0.02) Cl1 2.4468 (0.0006) 175.14 (0.06) 89.02 (0.05) 84.79 (0.02) 96.44 (0.02) 88.53 (0.02) Ru1 - C61 C1 P1 P2 P41 C1 - Distance Angles C2 1.3865 (0.0026) C6 1.3887 (0.0026) 117.22 (0.17) Ru1 2.0888 (0.0019) 121.59 (0.14) 121.10 (0.13) C1 - C2 C6 C2 - Distance Angles C1 1.3865 (0.0026) O1 1.3995 (0.0022) 117.42 (0.16) C3 1.3986 (0.0027) 123.43 (0.17) 119.16 (0.16) C2 - C1 O1 C3 - Distance Angles C4 1.4001 (0.0027) C2 1.3986 (0.0027) 115.19 (0.17) C7 1.5346 (0.0026) 121.21 (0.17) 123.58 (0.17) C3 - C4 C2 C4 - Distance Angles C5 1.3952 (0.0027) C3 1.4001 (0.0027) 125.21 (0.18) H4 0.9500 117.39 117.39 C4 - C5 C3 C5 - Distance Angles C4 1.3952 (0.0027) C6 1.3967 (0.0027) 114.94 (0.17) C11 1.5398 (0.0026) 121.55 (0.17) 123.51 (0.17) C5 - C4 C6 C6 - Distance Angles C1 1.3887 (0.0026) C5 1.3967 (0.0027) 123.78 (0.17) O2 1.4004 (0.0022) 117.10 (0.16) 119.11 (0.16) C6 - C1 C5 C7 - Distance Angles C10 1.5270 (0.0029) C3 1.5346 (0.0026) 111.29 (0.16) C8 1.5355 (0.0029) 107.41 (0.17) 110.65 (0.17) C9 1.5372 (0.0028) 107.95 (0.17) 109.73 (0.16) 109.74 (0.17) C7 - C10 C3 C8 C8 - Distance Angles C7 1.5355 (0.0029) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C7 1.5372 (0.0028) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C7 1.5270 (0.0029) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C7 H10A H10B C11 - Distance Angles C14 1.5304 (0.0029) C13 1.5333 (0.0033) 107.98 (0.19) C12 1.5366 (0.0030) 106.82 (0.18) 110.30 (0.19) C5 1.5398 (0.0026) 111.95 (0.17) 109.74 (0.18) 109.99 (0.17) C11 - C14 C13 C12 C12 - Distance Angles C11 1.5366 (0.0030) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles C11 1.5333 (0.0033) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C11 H13A H13B C14 - Distance Angles C11 1.5304 (0.0029) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C11 H14A H14B C15 - Distance Angles C20 1.3942 (0.0029) C16 1.3956 (0.0029) 118.96 (0.19) P1 1.8194 (0.0020) 120.83 (0.16) 120.19 (0.15) C15 - C20 C16 C16 - Distance Angles C17 1.3902 (0.0030) C15 1.3956 (0.0029) 120.46 (0.20) H16 0.9500 119.77 119.77 C16 - C17 C15 C17 - Distance Angles C18 1.3821 (0.0034) C16 1.3902 (0.0030) 119.89 (0.21) H17 0.9500 120.05 120.05 C17 - C18 C16 C18 - Distance Angles C17 1.3821 (0.0034) C19 1.3825 (0.0037) 120.29 (0.22) H18 0.9500 119.86 119.86 C18 - C17 C19 C19 - Distance Angles C18 1.3825 (0.0037) C20 1.3896 (0.0032) 120.05 (0.22) H19 0.9500 119.97 119.97 C19 - C18 C20 C20 - Distance Angles C19 1.3896 (0.0032) C15 1.3942 (0.0029) 120.35 (0.22) H20 0.9500 119.83 119.83 C20 - C19 C15 C21 - Distance Angles C26 1.3866 (0.0030) C22 1.3927 (0.0030) 119.17 (0.20) P1 1.8201 (0.0021) 120.51 (0.16) 120.26 (0.17) C21 - C26 C22 C22 - Distance Angles C23 1.3838 (0.0034) C21 1.3927 (0.0030) 120.15 (0.23) H22 0.9500 119.93 119.93 C22 - C23 C21 C23 - Distance Angles C22 1.3838 (0.0034) C24 1.3833 (0.0040) 120.17 (0.24) H23 0.9500 119.91 119.91 C23 - C22 C24 C24 - Distance Angles C25 1.3750 (0.0037) C23 1.3833 (0.0040) 120.14 (0.22) H24 0.9500 119.93 119.93 C24 - C25 C23 C25 - Distance Angles C24 1.3750 (0.0037) C26 1.3902 (0.0030) 119.96 (0.23) H25 0.9500 120.02 120.02 C25 - C24 C26 C26 - Distance Angles C21 1.3866 (0.0030) C25 1.3902 (0.0030) 120.40 (0.21) H26 0.9500 119.80 119.80 C26 - C21 C25 C27 - Distance Angles C32 1.3927 (0.0028) C28 1.3968 (0.0028) 119.27 (0.18) P2 1.8134 (0.0019) 126.06 (0.16) 114.39 (0.14) C27 - C32 C28 C28 - Distance Angles C29 1.3819 (0.0029) C27 1.3968 (0.0028) 120.47 (0.19) H28 0.9500 119.76 119.76 C28 - C29 C27 C29 - Distance Angles C30 1.3790 (0.0032) C28 1.3819 (0.0029) 120.17 (0.20) H29 0.9500 119.92 119.92 C29 - C30 C28 C30 - Distance Angles C29 1.3790 (0.0032) C31 1.3834 (0.0033) 119.84 (0.20) H30 0.9500 120.08 120.08 C30 - C29 C31 C31 - Distance Angles C30 1.3834 (0.0033) C32 1.3907 (0.0030) 120.66 (0.20) H31 0.9500 119.67 119.67 C31 - C30 C32 C32 - Distance Angles C27 1.3927 (0.0028) C31 1.3907 (0.0030) 119.55 (0.20) H32 0.9500 120.22 120.22 C32 - C27 C31 C33 - Distance Angles C38 1.3973 (0.0028) C34 1.3977 (0.0028) 118.82 (0.18) P2 1.8135 (0.0019) 121.33 (0.15) 119.42 (0.15) C33 - C38 C34 C34 - Distance Angles C35 1.3904 (0.0030) C33 1.3977 (0.0028) 120.20 (0.20) H34 0.9500 119.90 119.90 C34 - C35 C33 C35 - Distance Angles C36 1.3826 (0.0033) C34 1.3904 (0.0030) 120.59 (0.21) H35 0.9500 119.70 119.70 C35 - C36 C34 C36 - Distance Angles C37 1.3832 (0.0032) C35 1.3826 (0.0033) 119.59 (0.20) H36 0.9500 120.20 120.20 C36 - C37 C35 C37 - Distance Angles C36 1.3832 (0.0032) C38 1.3901 (0.0028) 120.45 (0.20) H37 0.9500 119.77 119.77 C37 - C36 C38 C38 - Distance Angles C37 1.3901 (0.0028) C33 1.3973 (0.0028) 120.34 (0.19) H38 0.9500 119.83 119.83 C38 - C37 C33 O1 - Distance Angles C2 1.3995 (0.0022) P1 1.6419 (0.0014) 116.51 (0.12) O1 - C2 O2 - Distance Angles C6 1.4004 (0.0022) P2 1.6424 (0.0014) 114.47 (0.11) O2 - C6 P1 - Distance Angles O1 1.6419 (0.0014) C15 1.8194 (0.0020) 96.85 (0.08) C21 1.8201 (0.0021) 103.64 (0.09) 100.69 (0.09) Ru1 2.3408 (0.0005) 104.42 (0.05) 128.73 (0.07) 118.09 (0.07) P1 - O1 C15 C21 P2 - Distance Angles O2 1.6424 (0.0014) C27 1.8134 (0.0020) 98.92 (0.08) C33 1.8135 (0.0020) 99.53 (0.08) 107.66 (0.09) Ru1 2.3524 (0.0005) 103.13 (0.05) 122.93 (0.06) 119.29 (0.06) P2 - O2 C27 C33 C41 - Distance Angles C42 1.3846 (0.0031) C46 1.3968 (0.0030) 118.62 (0.20) P41 1.8350 (0.0021) 121.36 (0.16) 119.99 (0.17) C41 - C42 C46 C42 - Distance Angles C41 1.3846 (0.0031) C43 1.3965 (0.0032) 120.52 (0.21) H42 0.9500 119.74 119.74 C42 - C41 C43 C43 - Distance Angles C44 1.3806 (0.0036) C42 1.3965 (0.0032) 120.06 (0.23) H43 0.9500 119.97 119.97 C43 - C44 C42 C44 - Distance Angles C43 1.3806 (0.0036) C45 1.3813 (0.0036) 119.85 (0.22) H44 0.9500 120.08 120.08 C44 - C43 C45 C45 - Distance Angles C44 1.3813 (0.0036) C46 1.3830 (0.0032) 120.15 (0.21) H45 0.9500 119.93 119.93 C45 - C44 C46 C46 - Distance Angles C45 1.3830 (0.0032) C41 1.3968 (0.0030) 120.78 (0.22) H46 0.9500 119.61 119.61 C46 - C45 C41 C47 - Distance Angles C52 1.3891 (0.0033) C48 1.3912 (0.0031) 119.35 (0.21) P41 1.8279 (0.0021) 118.61 (0.16) 121.43 (0.18) C47 - C52 C48 C48 - Distance Angles C47 1.3912 (0.0031) C49 1.4003 (0.0035) 119.25 (0.25) H48 0.9500 120.37 120.37 C48 - C47 C49 C49 - Distance Angles C50 1.3626 (0.0045) C48 1.4003 (0.0035) 120.93 (0.25) H49 0.9500 119.53 119.53 C49 - C50 C48 C50 - Distance Angles C49 1.3626 (0.0045) C51 1.3764 (0.0043) 120.08 (0.23) H50 0.9500 119.96 119.96 C50 - C49 C51 C51 - Distance Angles C50 1.3764 (0.0042) C52 1.3904 (0.0032) 120.08 (0.27) H51 0.9500 119.96 119.96 C51 - C50 C52 C52 - Distance Angles C47 1.3891 (0.0033) C51 1.3904 (0.0032) 120.29 (0.24) H52 0.9500 119.86 119.86 C52 - C47 C51 C53 - Distance Angles C54 1.3948 (0.0030) C58 1.3953 (0.0029) 118.90 (0.19) P41 1.8319 (0.0020) 123.37 (0.16) 117.65 (0.16) C53 - C54 C58 C54 - Distance Angles C55 1.3849 (0.0031) C53 1.3948 (0.0030) 120.49 (0.22) H54 0.9500 119.76 119.76 C54 - C55 C53 C55 - Distance Angles C54 1.3849 (0.0031) C56 1.3850 (0.0037) 120.22 (0.22) H55 0.9500 119.89 119.89 C55 - C54 C56 C56 - Distance Angles C57 1.3815 (0.0036) C55 1.3850 (0.0037) 119.86 (0.21) H56 0.9500 120.07 120.07 C56 - C57 C55 C57 - Distance Angles C56 1.3815 (0.0036) C58 1.3908 (0.0029) 120.27 (0.22) H57 0.9500 119.87 119.87 C57 - C56 C58 C58 - Distance Angles C57 1.3908 (0.0029) C53 1.3953 (0.0029) 120.23 (0.21) H58 0.9500 119.88 119.88 C58 - C57 C53 P41 - Distance Angles C47 1.8279 (0.0021) C53 1.8319 (0.0020) 104.06 (0.10) C41 1.8350 (0.0021) 102.57 (0.10) 98.77 (0.09) Ru1 2.4345 (0.0005) 109.96 (0.07) 115.53 (0.07) 123.60 (0.07) P41 - C47 C53 C41 C61 - Distance Angles O61 1.0721 (0.0027) Ru1 1.8850 (0.0025) 176.28 (0.19) C61 - O61 O61 - Distance Angles C61 1.0721 (0.0027) O61 - C71 - Distance Angles Cl73 1.7397 (0.0028) Cl71 1.7473 (0.0030) 109.73 (0.16) Cl72 1.7611 (0.0028) 109.12 (0.15) 110.90 (0.16) H71 1.0000 109.02 109.02 109.02 C71 - Cl73 Cl71 Cl72 Cl71 - Distance Angles C71 1.7473 (0.0031) Cl71 - Cl72 - Distance Angles C71 1.7611 (0.0028) Cl72 - Cl73 - Distance Angles C71 1.7397 (0.0028) Cl73 - FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0388 for 11904 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.12 at 0.8562 0.2732 0.4310 [ 1.02 A from CL72 ] Deepest hole -0.84 at 0.7389 0.1460 0.4511 [ 0.58 A from CL73 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 6465 / 43727 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8562 0.2732 0.4310 1.00000 0.05 1.12 1.02 CL72 1.46 C71 1.94 CL73 2.12 H71 Q2 1 0.9818 0.1374 0.5209 1.00000 0.05 0.59 0.78 CL71 2.04 C71 2.66 CL72 2.67 H71 Q3 1 0.7631 0.4587 0.9733 1.00000 0.05 0.52 0.86 CL1 2.56 H28 2.63 H9A 2.66 H9B Q4 1 0.7403 0.3559 0.8760 1.00000 0.05 0.49 1.01 CL1 1.46 RU1 2.55 C1 2.59 H28 Q5 1 0.8729 0.1124 0.4997 1.00000 0.05 0.48 0.85 CL71 1.57 C71 2.15 CL73 2.27 H71 Shortest distances between peaks (including symmetry equivalents) 2 5 1.39 3 4 1.77 1 5 2.62 1 2 2.89 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.04: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 9.21: Structure factors and derivatives 54.56: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 3.30: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.21: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.07: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0806b finished at 13:37:14 Total CPU time: 70.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++