+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0043 started at 09:34:22 on 17-Mar-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0043 in P-1 CELL 0.71073 10.0905 12.7583 14.4492 100.026 98.124 108.201 ZERR 2.00 0.0002 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H P CL PT UNIT 80 68 4 4 2 V = 1701.60 F(000) = 832.0 Mu = 4.40 mm-1 Cell Wt = 1685.20 Rho = 1.645 MERG 2 OMIT -3.00 55.00 shel 7 0.77 FMAP 2 PLAN 5 SIZE 0.02 0.05 0.08 ACTA BOND $H WGHT 0.03620 18.56290 L.S. 18 TEMP -153.00 FVAR 0.43530 CL1 4 0.581479 0.461053 0.673900 11.00000 0.03349 0.03589 = 0.02960 -0.00136 0.00284 0.01797 CL2 4 0.751852 0.657399 0.867377 11.00000 0.02412 0.03257 = 0.03351 0.00034 -0.00139 0.00967 PT1 5 0.523047 0.600972 0.768750 11.00000 0.02351 0.02464 = 0.02452 0.00056 0.00058 0.00945 MOLE 1 C1 1 0.276331 0.630129 0.603482 11.00000 0.02793 0.02541 = 0.02434 -0.00347 -0.00314 0.00910 C2 1 0.394255 0.678380 0.562235 11.00000 0.02525 0.03968 = 0.03045 0.00174 -0.00285 0.01532 AFIX 43 H2 2 0.478228 0.660244 0.576162 11.00000 -1.20000 AFIX 0 C3 1 0.389450 0.749465 0.503662 11.00000 0.04059 0.03129 = 0.03598 0.00361 0.00679 0.01182 AFIX 43 H3 2 0.470205 0.780778 0.477517 11.00000 -1.20000 AFIX 0 C4 1 0.266671 0.777920 0.480717 11.00000 0.04171 0.03373 = 0.02789 0.00290 0.00188 0.01574 C5 1 0.152233 0.731364 0.520870 11.00000 0.03212 0.03917 = 0.03750 0.00201 -0.00420 0.01807 AFIX 43 H5 2 0.068646 0.750008 0.506934 11.00000 -1.20000 AFIX 0 C6 1 0.155759 0.657525 0.581490 11.00000 0.02822 0.02753 = 0.03994 -0.00125 0.00258 0.01065 AFIX 43 H6 2 0.074909 0.626208 0.607545 11.00000 -1.20000 AFIX 0 C7 1 0.259129 0.856396 0.418331 11.00000 0.05290 0.04863 = 0.05127 0.01450 0.00101 0.02289 AFIX 43 H7 2 0.168061 0.861277 0.397593 11.00000 -1.20000 AFIX 0 C8 1 0.366939 0.920642 0.388466 11.00000 0.06470 0.06319 = 0.06679 0.03184 0.01583 0.01769 AFIX 93 H8A 2 0.460057 0.918673 0.407323 11.00000 -1.20000 H8B 2 0.351458 0.968876 0.348104 11.00000 -1.20000 AFIX 0 C9 1 0.256086 0.398072 0.588762 11.00000 0.03416 0.02879 = 0.02974 -0.00751 0.00151 0.01584 C10 1 0.248647 0.391233 0.491438 11.00000 0.02937 0.03896 = 0.03187 -0.00234 0.00325 0.01346 AFIX 43 H10 2 0.265805 0.458035 0.467559 11.00000 -1.20000 AFIX 0 C11 1 0.216104 0.286743 0.428605 11.00000 0.03155 0.04319 = 0.03730 -0.00730 0.00294 0.01226 AFIX 43 H11 2 0.208032 0.281991 0.361576 11.00000 -1.20000 AFIX 0 C12 1 0.195609 0.190560 0.462865 11.00000 0.04578 0.03579 = 0.04024 -0.01670 -0.00043 0.01340 AFIX 43 H12 2 0.175464 0.119722 0.419523 11.00000 -1.20000 AFIX 0 C13 1 0.203944 0.195625 0.559573 11.00000 0.05070 0.03070 = 0.05459 -0.00141 0.00395 0.01423 AFIX 43 H13 2 0.188617 0.128396 0.582679 11.00000 -1.20000 AFIX 0 C14 1 0.234923 0.299611 0.623532 11.00000 0.04841 0.03960 = 0.02998 -0.00024 -0.00743 0.01939 AFIX 43 H14 2 0.241631 0.303600 0.690384 11.00000 -1.20000 AFIX 0 C15 1 0.165640 0.494835 0.747262 11.00000 0.02655 0.02310 = 0.03371 -0.00297 0.00153 0.00804 C16 1 0.020269 0.463958 0.708799 11.00000 0.03009 0.03211 = 0.03906 0.00116 -0.00722 0.00780 AFIX 43 H16 2 -0.010828 0.465918 0.644126 11.00000 -1.20000 AFIX 0 C17 1 -0.079253 0.430269 0.765194 11.00000 0.02301 0.04487 = 0.06131 0.00927 0.00771 0.01220 AFIX 43 H17 2 -0.178080 0.409994 0.739035 11.00000 -1.20000 AFIX 0 C18 1 -0.034652 0.426219 0.859280 11.00000 0.03819 0.04146 = 0.05192 0.01213 0.01999 0.01331 AFIX 43 H18 2 -0.102968 0.405156 0.897825 11.00000 -1.20000 AFIX 0 C19 1 0.107956 0.452492 0.897352 11.00000 0.03885 0.03044 = 0.03822 0.00022 0.00785 0.00493 AFIX 43 H19 2 0.138227 0.447655 0.961291 11.00000 -1.20000 AFIX 0 C20 1 0.206875 0.486145 0.840997 11.00000 0.02605 0.02487 = 0.03482 -0.00159 -0.00312 0.00625 AFIX 43 H20 2 0.305213 0.503702 0.867012 11.00000 -1.20000 AFIX 0 P1 3 0.301370 0.532870 0.676889 11.00000 0.02345 0.02673 = 0.02450 -0.00059 -0.00097 0.00983 MOLE 2 C21 1 0.658395 0.875776 0.871858 11.00000 0.02635 0.01840 = 0.03510 0.00059 -0.00091 0.00796 C22 1 0.711283 0.893131 0.788271 11.00000 0.03486 0.02731 = 0.03098 -0.00179 0.00062 0.00848 AFIX 43 H22 2 0.662516 0.842112 0.728159 11.00000 -1.20000 AFIX 0 C23 1 0.832073 0.982666 0.792858 11.00000 0.03106 0.03014 = 0.03599 0.00442 0.00706 0.00942 AFIX 43 H23 2 0.863421 0.995234 0.735455 11.00000 -1.20000 AFIX 0 C24 1 0.909781 1.055779 0.881007 11.00000 0.02487 0.02423 = 0.04222 0.00150 0.00464 0.00549 C25 1 0.857488 1.038269 0.963433 11.00000 0.03580 0.02688 = 0.02312 -0.00792 -0.00505 0.01080 AFIX 43 H25 2 0.908635 1.087361 1.023921 11.00000 -1.20000 AFIX 0 C26 1 0.731689 0.950150 0.958689 11.00000 0.02419 0.02952 = 0.03177 0.00041 0.00243 0.00947 AFIX 43 H26 2 0.696145 0.941147 1.015366 11.00000 -1.20000 AFIX 0 C27 1 1.045318 1.147655 0.888646 11.00000 0.03963 0.02616 = 0.04536 -0.00202 0.00134 -0.00126 AFIX 43 H27 2 1.087085 1.197640 0.950127 11.00000 -1.20000 AFIX 0 C28 1 1.114067 1.167809 0.820366 11.00000 0.05835 0.04498 = 0.05250 0.01023 0.00952 -0.00609 AFIX 93 H28A 2 1.077111 1.120463 0.757456 11.00000 -1.20000 H28B 2 1.201246 1.229878 0.833393 11.00000 -1.20000 AFIX 0 C29 1 0.351969 0.803305 0.816286 11.00000 0.02679 0.02532 = 0.02752 -0.00594 -0.00443 0.01201 C30 1 0.376322 0.889607 0.767224 11.00000 0.03161 0.02674 = 0.03942 0.00097 -0.00437 0.00867 AFIX 43 H30 2 0.468648 0.923254 0.755359 11.00000 -1.20000 AFIX 0 C31 1 0.267513 0.926795 0.735621 11.00000 0.05133 0.03614 = 0.05187 0.00652 -0.00129 0.01958 AFIX 43 H31 2 0.285375 0.985333 0.701503 11.00000 -1.20000 AFIX 0 C32 1 0.133278 0.880207 0.752857 11.00000 0.03429 0.03492 = 0.05379 -0.00698 -0.00976 0.01762 AFIX 43 H32 2 0.059610 0.907702 0.732045 11.00000 -1.20000 AFIX 0 C33 1 0.106175 0.793676 0.800333 11.00000 0.03387 0.03561 = 0.03856 -0.00831 0.00182 0.01516 AFIX 43 H33 2 0.012935 0.759467 0.810536 11.00000 -1.20000 AFIX 0 C34 1 0.216415 0.756258 0.833522 11.00000 0.03100 0.02871 = 0.03530 -0.00377 0.00344 0.01225 AFIX 43 H34 2 0.198426 0.698194 0.868134 11.00000 -1.20000 AFIX 0 C35 1 0.476314 0.745805 0.981642 11.00000 0.03022 0.02613 = 0.02028 -0.00312 -0.00257 0.00983 C36 1 0.426845 0.821490 1.034958 11.00000 0.04425 0.03175 = 0.03125 -0.00310 0.00556 0.01375 AFIX 43 H36 2 0.406126 0.879248 1.008652 11.00000 -1.20000 AFIX 0 C37 1 0.407702 0.812402 1.127221 11.00000 0.03660 0.03762 = 0.03256 -0.00493 0.00407 0.01221 AFIX 43 H37 2 0.372207 0.863402 1.163212 11.00000 -1.20000 AFIX 0 C38 1 0.439321 0.731191 1.166396 11.00000 0.03876 0.05768 = 0.03229 0.00648 0.00837 0.01730 AFIX 43 H38 2 0.426714 0.726582 1.229673 11.00000 -1.20000 AFIX 0 C39 1 0.489977 0.654893 1.114391 11.00000 0.03721 0.03131 = 0.03631 0.00536 0.00374 0.00920 AFIX 43 H39 2 0.510997 0.597856 1.141666 11.00000 -1.20000 AFIX 0 C40 1 0.509640 0.662926 1.021714 11.00000 0.02425 0.03081 = 0.03066 0.00293 0.00053 0.00762 AFIX 43 H40 2 0.545637 0.612042 0.986062 11.00000 -1.20000 AFIX 0 P2 3 0.496742 0.753909 0.859482 11.00000 0.02528 0.02467 = 0.02499 0.00052 0.00056 0.01060 HKLF 4 Covalent radii and connectivity table for 2010src0043 in P-1 C 0.770 H 0.320 P 1.100 CL 0.990 PT 1.370 Cl1 - Pt1 Cl2 - Pt1 Pt1 - P1 P2 Cl1 Cl2 C1 - C6 C2 P1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C7 C5 - C4 C6 C6 - C1 C5 C7 - C8 C4 C8 - C7 C9 - C10 C14 P1 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C13 C9 C15 - C20 C16 P1 C16 - C17 C15 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C19 C15 P1 - C15 C1 C9 Pt1 C21 - C26 C22 P2 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C27 C25 - C26 C24 C26 - C21 C25 C27 - C28 C24 C28 - C27 C29 - C30 C34 P2 C30 - C31 C29 C31 - C32 C30 C32 - C33 C31 C33 - C32 C34 C34 - C29 C33 C35 - C36 C40 P2 C36 - C35 C37 C37 - C38 C36 C38 - C37 C39 C39 - C38 C40 C40 - C35 C39 P2 - C35 C21 C29 Pt1 29021 Reflections read, of which 53 rejected -12 =< h =< 13, -16 =< k =< 16, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -8 7 1 79.35 4.88 5 25.33 1 Inconsistent equivalents 7716 Unique reflections, of which 0 suppressed R(int) = 0.0731 R(sigma) = 0.0634 Friedel opposites merged Maximum memory for data reduction = 3798 / 77627 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 = 4948 / 522382 wR2 = 0.1378 before cycle 1 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.039 OSF Mean shift/esd = 0.003 Maximum = -0.045 for U23 Pt1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 2 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.016 for U23 Pt1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 3 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C31 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 4 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 5 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C13 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 6 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C33 Max. dU = 0.000 for C25 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 7 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C8 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 8 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C21 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 9 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C28 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 10 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C32 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 11 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C7 Least-squares cycle 12 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 12 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C8 Least-squares cycle 13 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 13 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C7 Least-squares cycle 14 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 14 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C8 Least-squares cycle 15 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 15 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C28 Least-squares cycle 16 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 16 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C37 Least-squares cycle 17 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 17 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C7 Least-squares cycle 18 Maximum vector length = 511 Memory required = 4948 / 522382 wR2 = 0.1378 before cycle 18 for 7716 data and 406 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43533 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C32 Largest correlation matrix elements 0.563 U11 Pt1 / OSF 0.512 U12 Pt1 / U22 Pt1 0.502 U12 C5 / U22 C5 0.555 U33 Pt1 / OSF 0.510 U12 Cl1 / U22 Cl1 0.549 U22 Pt1 / OSF 0.505 U12 C32 / U22 C32 Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4782 0.6602 0.5762 43 0.950 0.000 C2 C3 C1 H3 0.4702 0.7808 0.4775 43 0.950 0.000 C3 C2 C4 H5 0.0686 0.7500 0.5069 43 0.950 0.000 C5 C4 C6 H6 0.0749 0.6262 0.6075 43 0.950 0.000 C6 C1 C5 H7 0.1681 0.8613 0.3976 43 0.950 0.000 C7 C8 C4 H8A 0.4601 0.9187 0.4073 93 0.950 0.000 C8 C7 C4 H8B 0.3515 0.9689 0.3481 93 0.950 0.000 C8 C7 C4 H10 0.2658 0.4580 0.4676 43 0.950 0.000 C10 C9 C11 H11 0.2080 0.2820 0.3616 43 0.950 0.000 C11 C12 C10 H12 0.1755 0.1197 0.4195 43 0.950 0.000 C12 C11 C13 H13 0.1886 0.1284 0.5827 43 0.950 0.000 C13 C12 C14 H14 0.2416 0.3036 0.6904 43 0.950 0.000 C14 C13 C9 H16 -0.0108 0.4659 0.6441 43 0.950 0.000 C16 C17 C15 H17 -0.1781 0.4100 0.7390 43 0.950 0.000 C17 C18 C16 H18 -0.1030 0.4052 0.8978 43 0.950 0.000 C18 C19 C17 H19 0.1382 0.4477 0.9613 43 0.950 0.000 C19 C18 C20 H20 0.3052 0.5037 0.8670 43 0.950 0.000 C20 C19 C15 H22 0.6625 0.8421 0.7282 43 0.950 0.000 C22 C23 C21 H23 0.8634 0.9952 0.7355 43 0.950 0.000 C23 C22 C24 H25 0.9086 1.0874 1.0239 43 0.950 0.000 C25 C26 C24 H26 0.6961 0.9411 1.0154 43 0.950 0.000 C26 C21 C25 H27 1.0871 1.1976 0.9501 43 0.950 0.000 C27 C28 C24 H28A 1.0771 1.1205 0.7575 93 0.950 0.000 C28 C27 C24 H28B 1.2012 1.2299 0.8334 93 0.950 0.000 C28 C27 C24 H30 0.4686 0.9232 0.7554 43 0.950 0.000 C30 C31 C29 H31 0.2854 0.9853 0.7015 43 0.950 0.000 C31 C32 C30 H32 0.0596 0.9077 0.7321 43 0.950 0.000 C32 C33 C31 H33 0.0129 0.7595 0.8105 43 0.950 0.000 C33 C32 C34 H34 0.1984 0.6982 0.8681 43 0.950 0.000 C34 C29 C33 H36 0.4061 0.8792 1.0087 43 0.950 0.000 C36 C35 C37 H37 0.3722 0.8634 1.1632 43 0.950 0.000 C37 C38 C36 H38 0.4267 0.7266 1.2297 43 0.950 0.000 C38 C37 C39 H39 0.5110 0.5979 1.1417 43 0.950 0.000 C39 C38 C40 H40 0.5456 0.6120 0.9861 43 0.950 0.000 C40 C35 C39 2010src0043 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl1 0.58148 0.46105 0.67390 1.00000 0.03349 0.03588 0.02960 -0.00136 0.00284 0.01796 0.03311 0.00445 0.00021 0.00017 0.00014 0.00000 0.00100 0.00105 0.00096 0.00080 0.00077 0.00085 0.00043 Cl2 0.75185 0.65740 0.86738 1.00000 0.02412 0.03256 0.03351 0.00033 -0.00141 0.00966 0.03184 0.00419 0.00020 0.00017 0.00014 0.00000 0.00089 0.00100 0.00100 0.00080 0.00074 0.00077 0.00042 Pt1 0.52305 0.60097 0.76875 1.00000 0.02351 0.02464 0.02452 0.00055 0.00058 0.00944 0.02509 0.00064 0.00003 0.00003 0.00002 0.00000 0.00016 0.00016 0.00016 0.00011 0.00010 0.00011 0.00010 C1 0.27633 0.63013 0.60348 1.00000 0.02792 0.02541 0.02434 -0.00349 -0.00316 0.00910 0.02804 0.01650 0.00082 0.00065 0.00054 0.00000 0.00387 0.00381 0.00372 0.00303 0.00297 0.00314 0.00162 C2 0.39426 0.67838 0.56224 1.00000 0.02526 0.03968 0.03045 0.00175 -0.00285 0.01532 0.03255 0.01810 0.00085 0.00073 0.00058 0.00000 0.00390 0.00465 0.00414 0.00356 0.00316 0.00351 0.00180 H2 0.47823 0.66024 0.57617 1.00000 0.03906 0.00000 0.00000 C3 0.38945 0.74947 0.50366 1.00000 0.04058 0.03127 0.03598 0.00358 0.00676 0.01181 0.03677 0.01961 0.00098 0.00073 0.00063 0.00000 0.00480 0.00440 0.00458 0.00364 0.00370 0.00376 0.00191 H3 0.47020 0.78078 0.47751 1.00000 0.04413 0.00000 0.00000 C4 0.26668 0.77792 0.48072 1.00000 0.04170 0.03370 0.02789 0.00288 0.00186 0.01572 0.03491 0.01923 0.00095 0.00073 0.00059 0.00000 0.00476 0.00445 0.00412 0.00346 0.00349 0.00379 0.00185 C5 0.15223 0.73137 0.52087 1.00000 0.03211 0.03915 0.03750 0.00200 -0.00422 0.01807 0.03697 0.01916 0.00092 0.00076 0.00062 0.00000 0.00442 0.00480 0.00464 0.00380 0.00354 0.00380 0.00196 H5 0.06865 0.75001 0.50694 1.00000 0.04436 0.00000 0.00000 C6 0.15576 0.65753 0.58149 1.00000 0.02821 0.02751 0.03993 -0.00127 0.00258 0.01063 0.03331 0.01810 0.00088 0.00069 0.00062 0.00000 0.00406 0.00406 0.00462 0.00349 0.00340 0.00331 0.00180 H6 0.07491 0.62621 0.60755 1.00000 0.03997 0.00000 0.00000 C7 0.25913 0.85640 0.41833 1.00000 0.05292 0.04861 0.05129 0.01450 0.00097 0.02286 0.05032 0.02421 0.00118 0.00089 0.00076 0.00000 0.00605 0.00589 0.00594 0.00482 0.00472 0.00494 0.00246 H7 0.16806 0.86128 0.39760 1.00000 0.06038 0.00000 0.00000 C8 0.36693 0.92064 0.38847 1.00000 0.06469 0.06319 0.06678 0.03182 0.01578 0.01770 0.06356 0.02867 0.00135 0.00104 0.00089 0.00000 0.00742 0.00742 0.00760 0.00626 0.00596 0.00605 0.00307 H8A 0.46005 0.91867 0.40732 1.00000 0.07627 0.00000 0.00000 H8B 0.35145 0.96888 0.34811 1.00000 0.07627 0.00000 0.00000 C9 0.25609 0.39807 0.58876 1.00000 0.03415 0.02878 0.02974 -0.00750 0.00150 0.01585 0.03210 0.01782 0.00088 0.00069 0.00058 0.00000 0.00429 0.00409 0.00407 0.00330 0.00330 0.00346 0.00179 C10 0.24864 0.39123 0.49144 1.00000 0.02935 0.03892 0.03187 -0.00234 0.00325 0.01344 0.03469 0.01856 0.00087 0.00077 0.00060 0.00000 0.00414 0.00467 0.00428 0.00360 0.00332 0.00360 0.00185 H10 0.26578 0.45803 0.46756 1.00000 0.04163 0.00000 0.00000 C11 0.21611 0.28674 0.42860 1.00000 0.03152 0.04318 0.03731 -0.00733 0.00291 0.01223 0.04013 0.01941 0.00091 0.00080 0.00067 0.00000 0.00447 0.00519 0.00474 0.00398 0.00361 0.00391 0.00209 H11 0.20804 0.28199 0.36157 1.00000 0.04816 0.00000 0.00000 C12 0.19562 0.19056 0.46287 1.00000 0.04579 0.03577 0.04025 -0.01671 -0.00043 0.01340 0.04509 0.01994 0.00102 0.00080 0.00068 0.00000 0.00537 0.00498 0.00511 0.00406 0.00408 0.00418 0.00234 H12 0.17547 0.11972 0.41953 1.00000 0.05411 0.00000 0.00000 C13 0.20395 0.19562 0.55957 1.00000 0.05073 0.03068 0.05459 -0.00142 0.00394 0.01423 0.04752 0.02170 0.00109 0.00081 0.00075 0.00000 0.00577 0.00473 0.00610 0.00430 0.00464 0.00426 0.00238 H13 0.18863 0.12839 0.58267 1.00000 0.05702 0.00000 0.00000 C14 0.23493 0.29961 0.62353 1.00000 0.04839 0.03960 0.02999 -0.00025 -0.00743 0.01938 0.04105 0.01994 0.00102 0.00078 0.00064 0.00000 0.00532 0.00498 0.00440 0.00376 0.00378 0.00422 0.00212 H14 0.24164 0.30360 0.69038 1.00000 0.04926 0.00000 0.00000 C15 0.16564 0.49483 0.74726 1.00000 0.02654 0.02310 0.03371 -0.00298 0.00153 0.00804 0.02966 0.01707 0.00083 0.00065 0.00058 0.00000 0.00387 0.00374 0.00420 0.00320 0.00318 0.00311 0.00168 C16 0.02026 0.46395 0.70880 1.00000 0.03009 0.03210 0.03906 0.00116 -0.00721 0.00781 0.03691 0.01839 0.00089 0.00073 0.00065 0.00000 0.00430 0.00441 0.00474 0.00368 0.00352 0.00354 0.00195 H16 -0.01084 0.46590 0.64412 1.00000 0.04429 0.00000 0.00000 C17 -0.07925 0.43027 0.76519 1.00000 0.02300 0.04485 0.06131 0.00925 0.00769 0.01218 0.04346 0.02172 0.00092 0.00082 0.00075 0.00000 0.00415 0.00531 0.00623 0.00462 0.00397 0.00382 0.00222 H17 -0.17808 0.41001 0.73903 1.00000 0.05215 0.00000 0.00000 C18 -0.03466 0.42622 0.85928 1.00000 0.03819 0.04147 0.05192 0.01213 0.01997 0.01331 0.04269 0.02233 0.00100 0.00080 0.00073 0.00000 0.00493 0.00516 0.00571 0.00439 0.00427 0.00410 0.00216 H18 -0.10297 0.40515 0.89782 1.00000 0.05123 0.00000 0.00000 C19 0.10795 0.45249 0.89735 1.00000 0.03883 0.03046 0.03821 0.00023 0.00783 0.00492 0.03858 0.01959 0.00095 0.00073 0.00067 0.00000 0.00480 0.00440 0.00474 0.00369 0.00375 0.00370 0.00198 H19 0.13823 0.44766 0.96129 1.00000 0.04629 0.00000 0.00000 C20 0.20687 0.48615 0.84100 1.00000 0.02605 0.02488 0.03482 -0.00161 -0.00312 0.00624 0.03131 0.01723 0.00085 0.00066 0.00059 0.00000 0.00391 0.00388 0.00430 0.00330 0.00322 0.00316 0.00174 H20 0.30521 0.50371 0.86701 1.00000 0.03758 0.00000 0.00000 P1 0.30137 0.53287 0.67689 1.00000 0.02345 0.02673 0.02450 -0.00061 -0.00099 0.00982 0.02610 0.00430 0.00021 0.00017 0.00014 0.00000 0.00094 0.00099 0.00095 0.00079 0.00074 0.00079 0.00041 C21 0.65839 0.87577 0.87186 1.00000 0.02636 0.01839 0.03508 0.00057 -0.00092 0.00795 0.02807 0.01675 0.00081 0.00062 0.00058 0.00000 0.00382 0.00350 0.00421 0.00310 0.00314 0.00299 0.00163 C22 0.71127 0.89313 0.78827 1.00000 0.03485 0.02730 0.03097 -0.00180 0.00062 0.00847 0.03337 0.01835 0.00090 0.00069 0.00060 0.00000 0.00437 0.00410 0.00422 0.00335 0.00337 0.00344 0.00180 H22 0.66250 0.84211 0.72816 1.00000 0.04005 0.00000 0.00000 C23 0.83208 0.98267 0.79286 1.00000 0.03106 0.03014 0.03598 0.00440 0.00704 0.00940 0.03310 0.01862 0.00087 0.00070 0.00063 0.00000 0.00420 0.00421 0.00444 0.00349 0.00341 0.00342 0.00177 H23 0.86343 0.99523 0.73545 1.00000 0.03972 0.00000 0.00000 C24 0.90978 1.05578 0.88101 1.00000 0.02489 0.02421 0.04219 0.00148 0.00462 0.00549 0.03222 0.01795 0.00084 0.00067 0.00063 0.00000 0.00388 0.00390 0.00469 0.00344 0.00336 0.00315 0.00177 C25 0.85748 1.03827 0.96343 1.00000 0.03579 0.02688 0.02312 -0.00793 -0.00504 0.01079 0.03158 0.01728 0.00088 0.00068 0.00056 0.00000 0.00433 0.00401 0.00381 0.00312 0.00318 0.00340 0.00178 H25 0.90863 1.08736 1.02391 1.00000 0.03789 0.00000 0.00000 C26 0.73169 0.95015 0.95869 1.00000 0.02420 0.02953 0.03176 0.00040 0.00242 0.00947 0.02969 0.01725 0.00081 0.00067 0.00059 0.00000 0.00378 0.00407 0.00411 0.00330 0.00310 0.00321 0.00167 H26 0.69615 0.94115 1.01537 1.00000 0.03563 0.00000 0.00000 C27 1.04532 1.14765 0.88865 1.00000 0.03964 0.02615 0.04534 -0.00202 0.00131 -0.00126 0.04225 0.01961 0.00098 0.00074 0.00071 0.00000 0.00497 0.00433 0.00529 0.00385 0.00406 0.00371 0.00216 H27 1.08709 1.19764 0.95013 1.00000 0.05070 0.00000 0.00000 C28 1.11406 1.16781 0.82036 1.00000 0.05834 0.04498 0.05247 0.01017 0.00951 -0.00612 0.05812 0.02487 0.00122 0.00093 0.00082 0.00000 0.00665 0.00592 0.00637 0.00498 0.00519 0.00499 0.00288 H28A 1.07711 1.12046 0.75746 1.00000 0.06974 0.00000 0.00000 H28B 1.20124 1.22987 0.83339 1.00000 0.06974 0.00000 0.00000 C29 0.35197 0.80330 0.81629 1.00000 0.02677 0.02532 0.02753 -0.00594 -0.00443 0.01200 0.02845 0.01646 0.00081 0.00065 0.00055 0.00000 0.00384 0.00382 0.00385 0.00309 0.00302 0.00315 0.00166 C30 0.37632 0.88960 0.76722 1.00000 0.03161 0.02674 0.03941 0.00096 -0.00436 0.00866 0.03505 0.01823 0.00092 0.00070 0.00062 0.00000 0.00427 0.00410 0.00467 0.00354 0.00351 0.00340 0.00187 H30 0.46864 0.92325 0.75535 1.00000 0.04206 0.00000 0.00000 C31 0.26751 0.92679 0.73562 1.00000 0.05129 0.03609 0.05190 0.00651 -0.00131 0.01954 0.04711 0.02218 0.00109 0.00083 0.00074 0.00000 0.00584 0.00501 0.00584 0.00436 0.00455 0.00445 0.00235 H31 0.28537 0.98533 0.70150 1.00000 0.05653 0.00000 0.00000 C32 0.13328 0.88021 0.75286 1.00000 0.03432 0.03493 0.05378 -0.00698 -0.00977 0.01764 0.04388 0.01964 0.00097 0.00078 0.00071 0.00000 0.00474 0.00484 0.00573 0.00425 0.00406 0.00395 0.00232 H32 0.05961 0.90770 0.73205 1.00000 0.05266 0.00000 0.00000 C33 0.10618 0.79368 0.80034 1.00000 0.03386 0.03558 0.03857 -0.00833 0.00181 0.01514 0.03806 0.01914 0.00095 0.00075 0.00064 0.00000 0.00452 0.00470 0.00471 0.00381 0.00363 0.00376 0.00203 H33 0.01294 0.75946 0.81054 1.00000 0.04567 0.00000 0.00000 C34 0.21641 0.75626 0.83352 1.00000 0.03101 0.02871 0.03529 -0.00378 0.00344 0.01226 0.03303 0.01798 0.00086 0.00071 0.00061 0.00000 0.00419 0.00411 0.00438 0.00341 0.00336 0.00340 0.00180 H34 0.19843 0.69820 0.86814 1.00000 0.03963 0.00000 0.00000 C35 0.47632 0.74581 0.98164 1.00000 0.03023 0.02610 0.02029 -0.00313 -0.00258 0.00980 0.02746 0.01648 0.00083 0.00065 0.00052 0.00000 0.00394 0.00382 0.00352 0.00296 0.00293 0.00318 0.00160 C36 0.42684 0.82149 1.03496 1.00000 0.04422 0.03177 0.03123 -0.00309 0.00554 0.01374 0.03720 0.01921 0.00097 0.00074 0.00061 0.00000 0.00497 0.00443 0.00436 0.00354 0.00366 0.00384 0.00195 H36 0.40612 0.87925 1.00865 1.00000 0.04463 0.00000 0.00000 C37 0.40770 0.81241 1.12722 1.00000 0.03663 0.03761 0.03255 -0.00494 0.00407 0.01221 0.03779 0.01907 0.00094 0.00077 0.00062 0.00000 0.00460 0.00475 0.00443 0.00370 0.00357 0.00383 0.00198 H37 0.37221 0.86341 1.16321 1.00000 0.04535 0.00000 0.00000 C38 0.43932 0.73119 1.16639 1.00000 0.03876 0.05764 0.03228 0.00647 0.00834 0.01727 0.04317 0.02148 0.00098 0.00087 0.00066 0.00000 0.00493 0.00609 0.00458 0.00427 0.00378 0.00451 0.00218 H38 0.42671 0.72658 1.22967 1.00000 0.05180 0.00000 0.00000 C39 0.48998 0.65490 1.11439 1.00000 0.03720 0.03130 0.03631 0.00535 0.00373 0.00919 0.03633 0.01917 0.00093 0.00074 0.00063 0.00000 0.00461 0.00439 0.00457 0.00362 0.00361 0.00365 0.00188 H39 0.51100 0.59786 1.14167 1.00000 0.04359 0.00000 0.00000 C40 0.50964 0.66293 1.02172 1.00000 0.02424 0.03080 0.03065 0.00291 0.00052 0.00759 0.03013 0.01729 0.00081 0.00069 0.00057 0.00000 0.00376 0.00418 0.00406 0.00333 0.00309 0.00326 0.00168 H40 0.54564 0.61205 0.98607 1.00000 0.03616 0.00000 0.00000 P2 0.49674 0.75391 0.85948 1.00000 0.02528 0.02466 0.02500 0.00051 0.00055 0.01059 0.02568 0.00436 0.00021 0.00017 0.00014 0.00000 0.00096 0.00096 0.00095 0.00077 0.00075 0.00078 0.00041 Final Structure Factor Calculation for 2010src0043 in P-1 Total number of l.s. parameters = 406 Maximum vector length = 511 Memory required = 4542 / 24017 wR2 = 0.1378 before cycle 19 for 7716 data and 0 / 406 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 18.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0585 for 6475 Fo > 4sig(Fo) and 0.0789 for all 7716 data wR2 = 0.1378, GooF = S = 1.118, Restrained GooF = 1.118 for all data Occupancy sum of asymmetric unit = 45.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0478 0.0287 0.0228 Cl1 0.0440 0.0302 0.0213 Cl2 0.0330 0.0223 0.0200 Pt1 0.0404 0.0270 0.0167 C1 0.0475 0.0315 0.0187 C2 0.0413 0.0397 0.0293 C3 0.0461 0.0322 0.0264 C4 0.0549 0.0336 0.0224 C5 0.0483 0.0275 0.0241 C6 0.0647 0.0514 0.0348 C7 0.0820 0.0659 0.0427 C8 0.0504 0.0303 0.0156 C9 0.0498 0.0281 0.0261 C10 0.0622 0.0317 0.0265 C11 0.0721 0.0463 0.0169 C12 0.0652 0.0497 0.0277 C13 0.0637 0.0357 0.0237 C14 0.0428 0.0269 0.0193 C15 0.0539 0.0352 0.0216 C16 0.0631 0.0453 0.0219 C17 0.0566 0.0418 0.0297 C18 0.0503 0.0388 0.0266 C19 0.0453 0.0293 0.0193 C20 0.0361 0.0233 0.0188 P1 0.0423 0.0243 0.0176 C21 0.0424 0.0359 0.0218 C22 0.0386 0.0314 0.0292 C23 0.0461 0.0286 0.0220 C24 0.0488 0.0324 0.0135 C25 0.0397 0.0259 0.0234 C26 0.0541 0.0526 0.0201 C27 0.0892 0.0527 0.0324 C28 0.0469 0.0220 0.0165 C29 0.0517 0.0299 0.0236 C30 0.0676 0.0418 0.0319 C31 0.0785 0.0279 0.0252 C32 0.0601 0.0319 0.0221 C33 0.0476 0.0301 0.0214 C34 0.0388 0.0282 0.0154 C35 0.0465 0.0430 0.0221 C36 0.0524 0.0370 0.0240 C37 0.0599 0.0380 0.0316 C38 0.0420 0.0368 0.0302 C39 0.0367 0.0316 0.0221 C40 0.0343 0.0222 0.0206 P2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.036 0.066 0.095 0.122 0.149 0.176 0.209 0.257 0.342 1.000 Number in group 783. 765. 777. 773. 774. 773. 764. 770. 762. 775. GooF 1.187 1.218 1.218 1.135 1.161 1.061 1.016 0.893 0.994 1.238 K 2.311 1.175 1.001 0.999 1.010 1.011 1.008 1.007 1.009 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 787. 764. 789. 763. 765. 770. 774. 759. 771. 774. GooF 1.251 1.269 1.179 1.167 1.056 1.011 0.907 0.863 0.976 1.378 K 1.040 1.047 1.045 1.043 1.017 1.004 1.000 0.991 1.000 1.022 R1 0.195 0.152 0.127 0.109 0.082 0.062 0.050 0.043 0.038 0.043 Recommended weighting scheme: WGHT 0.0361 18.5512 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 0 7196.61 5056.89 4.31 0.315 4.36 -4 11 10 350.04 6.68 3.94 0.011 0.82 6 -3 2 726.38 1393.48 3.90 0.165 1.57 9 -6 5 2541.91 3787.49 3.78 0.272 0.98 0 1 4 3018.87 2003.87 3.77 0.198 3.14 10 -1 6 545.72 17.89 3.75 0.019 0.83 2 4 2 23198.49 18747.90 3.70 0.606 1.94 2 1 3 18608.58 14887.13 3.66 0.540 2.68 2 -16 4 841.80 1870.68 3.59 0.191 0.79 -1 -12 10 878.00 1862.53 3.58 0.191 0.89 -2 2 3 29241.32 35585.15 3.51 0.835 3.27 2 5 3 12632.01 10122.32 3.42 0.445 1.59 3 3 0 11616.55 9167.77 3.41 0.424 2.12 0 -9 9 849.50 350.16 3.35 0.083 1.14 -7 4 13 48.92 409.16 3.35 0.089 0.90 5 -9 12 220.32 715.81 3.33 0.118 0.91 8 -14 4 255.42 860.02 3.31 0.130 0.83 2 1 2 8752.75 6900.84 3.25 0.368 3.10 5 1 0 168.83 11.18 3.24 0.015 1.76 -2 0 1 1312.48 792.13 3.23 0.125 4.75 -2 -10 15 1585.72 851.25 3.23 0.129 0.81 -5 1 0 9677.69 13950.74 3.22 0.523 1.96 3 2 4 6610.57 5162.96 3.21 0.318 1.79 1 3 4 18171.66 14922.89 3.20 0.540 2.11 10 4 2 33.24 385.59 3.20 0.087 0.79 -2 -14 8 821.41 298.12 3.20 0.076 0.79 -3 1 0 501.20 1067.80 3.18 0.145 3.32 2 5 2 24004.51 19944.06 3.17 0.625 1.69 2 3 2 6385.74 4997.68 3.16 0.313 2.25 1 2 5 18907.69 15560.90 3.15 0.552 2.10 3 1 3 31917.57 26823.26 3.15 0.725 2.17 -2 15 0 409.79 1029.83 3.14 0.142 0.82 -4 -9 15 2408.71 1440.97 3.14 0.168 0.80 2 7 4 226.80 34.37 3.13 0.026 1.22 1 3 1 2376.83 1644.49 3.13 0.179 2.99 -1 -13 6 350.08 1.97 3.11 0.006 0.89 -8 -7 12 1728.47 675.90 3.10 0.115 0.78 -1 -3 18 1916.04 1208.17 3.10 0.154 0.80 -1 -5 18 720.81 252.08 3.04 0.070 0.79 3 -11 2 1887.71 2935.71 3.03 0.240 1.16 1 5 3 6819.55 5393.56 3.02 0.325 1.76 5 6 6 1627.93 890.12 3.01 0.132 0.95 2 -7 17 607.70 215.50 3.01 0.065 0.80 -5 2 14 158.37 569.79 3.00 0.106 0.95 -3 -2 1 37145.25 31377.54 3.00 0.784 2.51 -2 -9 16 846.39 200.48 3.00 0.063 0.80 2 -10 13 2770.60 1843.90 3.00 0.190 0.90 2 2 4 3493.47 2602.05 2.97 0.226 2.08 1 6 1 10028.39 8132.94 2.97 0.399 1.73 0 2 2 18916.95 15721.71 2.95 0.555 4.06 Bond lengths and angles Cl1 - Distance Angles Pt1 2.3338 (0.0019) Cl1 - Cl2 - Distance Angles Pt1 2.3567 (0.0018) Cl2 - Pt1 - Distance Angles P1 2.2506 (0.0019) P2 2.2644 (0.0019) 96.05 (0.07) Cl1 2.3338 (0.0019) 89.76 (0.07) 171.85 (0.08) Cl2 2.3567 (0.0018) 175.32 (0.08) 86.88 (0.07) 87.70 (0.07) Pt1 - P1 P2 Cl1 C1 - Distance Angles C6 1.3778 (0.0109) C2 1.4215 (0.0119) 117.95 (0.77) P1 1.8185 (0.0084) 127.26 (0.67) 114.75 (0.58) C1 - C6 C2 C2 - Distance Angles C3 1.3507 (0.0124) C1 1.4215 (0.0118) 121.40 (0.76) H2 0.9500 119.30 119.30 C2 - C3 C1 C3 - Distance Angles C2 1.3507 (0.0124) C4 1.4082 (0.0122) 121.07 (0.85) H3 0.9500 119.46 119.46 C3 - C2 C4 C4 - Distance Angles C5 1.3798 (0.0129) C3 1.4082 (0.0122) 117.60 (0.81) C7 1.4708 (0.0133) 120.10 (0.83) 122.28 (0.87) C4 - C5 C3 C5 - Distance Angles C4 1.3798 (0.0129) C6 1.3983 (0.0126) 121.89 (0.78) H5 0.9500 119.06 119.06 C5 - C4 C6 C6 - Distance Angles C1 1.3778 (0.0109) C5 1.3983 (0.0126) 120.09 (0.81) H6 0.9500 119.95 119.95 C6 - C1 C5 C7 - Distance Angles C8 1.3192 (0.0156) C4 1.4708 (0.0133) 126.13 (1.03) H7 0.9500 116.94 116.94 C7 - C8 C4 C8 - Distance Angles C7 1.3192 (0.0155) H8A 0.9500 120.00 H8B 0.9500 120.00 120.00 C8 - C7 H8A C9 - Distance Angles C10 1.3835 (0.0118) C14 1.3994 (0.0129) 119.49 (0.75) P1 1.8358 (0.0077) 122.85 (0.68) 117.60 (0.63) C9 - C10 C14 C10 - Distance Angles C9 1.3835 (0.0118) C11 1.3893 (0.0117) 120.05 (0.88) H10 0.9500 119.97 119.97 C10 - C9 C11 C11 - Distance Angles C12 1.3696 (0.0143) C10 1.3893 (0.0117) 120.29 (0.88) H11 0.9500 119.86 119.86 C11 - C12 C10 C12 - Distance Angles C11 1.3696 (0.0143) C13 1.3768 (0.0143) 120.59 (0.83) H12 0.9500 119.71 119.71 C12 - C11 C13 C13 - Distance Angles C12 1.3768 (0.0143) C14 1.3944 (0.0124) 119.88 (0.95) H13 0.9500 120.06 120.06 C13 - C12 C14 C14 - Distance Angles C13 1.3944 (0.0123) C9 1.3994 (0.0129) 119.68 (0.86) H14 0.9500 120.16 120.16 C14 - C13 C9 C15 - Distance Angles C20 1.3934 (0.0116) C16 1.3958 (0.0112) 118.34 (0.79) P1 1.8153 (0.0085) 118.66 (0.60) 122.74 (0.67) C15 - C20 C16 C16 - Distance Angles C17 1.3930 (0.0133) C15 1.3958 (0.0111) 120.04 (0.84) H16 0.9500 119.98 119.98 C16 - C17 C15 C17 - Distance Angles C18 1.3854 (0.0140) C16 1.3930 (0.0133) 120.26 (0.83) H17 0.9500 119.87 119.87 C17 - C18 C16 C18 - Distance Angles C19 1.3771 (0.0132) C17 1.3854 (0.0140) 120.50 (0.86) H18 0.9500 119.75 119.75 C18 - C19 C17 C19 - Distance Angles C18 1.3771 (0.0132) C20 1.3882 (0.0123) 119.08 (0.88) H19 0.9500 120.46 120.46 C19 - C18 C20 C20 - Distance Angles C19 1.3882 (0.0123) C15 1.3934 (0.0116) 121.70 (0.78) H20 0.9500 119.15 119.15 C20 - C19 C15 P1 - Distance Angles C15 1.8153 (0.0086) C1 1.8185 (0.0084) 113.58 (0.37) C9 1.8358 (0.0077) 100.78 (0.38) 103.57 (0.37) Pt1 2.2506 (0.0019) 112.01 (0.27) 110.55 (0.26) 115.87 (0.27) P1 - C15 C1 C9 C21 - Distance Angles C26 1.3807 (0.0107) C22 1.4121 (0.0120) 118.73 (0.74) P2 1.8293 (0.0079) 123.29 (0.65) 117.97 (0.58) C21 - C26 C22 C22 - Distance Angles C23 1.3697 (0.0117) C21 1.4121 (0.0120) 120.76 (0.75) H22 0.9500 119.62 119.62 C22 - C23 C21 C23 - Distance Angles C22 1.3697 (0.0117) C24 1.3980 (0.0116) 120.78 (0.81) H23 0.9500 119.61 119.61 C23 - C22 C24 C24 - Distance Angles C25 1.3939 (0.0121) C23 1.3980 (0.0116) 118.25 (0.75) C27 1.4722 (0.0116) 119.94 (0.77) 121.79 (0.81) C24 - C25 C23 C25 - Distance Angles C26 1.3918 (0.0116) C24 1.3939 (0.0121) 121.18 (0.71) H25 0.9500 119.41 119.41 C25 - C26 C24 C26 - Distance Angles C21 1.3807 (0.0107) C25 1.3918 (0.0116) 120.20 (0.77) H26 0.9500 119.90 119.90 C26 - C21 C25 C27 - Distance Angles C28 1.3004 (0.0143) C24 1.4722 (0.0115) 127.06 (0.90) H27 0.9500 116.47 116.47 C27 - C28 C24 C28 - Distance Angles C27 1.3004 (0.0143) H28A 0.9500 120.00 H28B 0.9500 120.00 120.00 C28 - C27 H28A C29 - Distance Angles C30 1.3883 (0.0122) C34 1.3887 (0.0117) 118.65 (0.74) P2 1.8371 (0.0077) 120.75 (0.63) 120.58 (0.66) C29 - C30 C34 C30 - Distance Angles C31 1.3778 (0.0124) C29 1.3883 (0.0122) 120.46 (0.87) H30 0.9500 119.77 119.77 C30 - C31 C29 C31 - Distance Angles C32 1.3762 (0.0144) C30 1.3778 (0.0124) 120.83 (0.96) H31 0.9500 119.59 119.59 C31 - C32 C30 C32 - Distance Angles C33 1.3756 (0.0141) C31 1.3762 (0.0145) 119.75 (0.85) H32 0.9500 120.13 120.13 C32 - C33 C31 C33 - Distance Angles C32 1.3756 (0.0141) C34 1.3985 (0.0118) 119.75 (0.86) H33 0.9500 120.13 120.13 C33 - C32 C34 C34 - Distance Angles C29 1.3887 (0.0117) C33 1.3985 (0.0118) 120.53 (0.86) H34 0.9500 119.73 119.73 C34 - C29 C33 C35 - Distance Angles C36 1.3878 (0.0110) C40 1.3952 (0.0113) 119.74 (0.76) P2 1.8226 (0.0080) 120.22 (0.64) 120.04 (0.59) C35 - C36 C40 C36 - Distance Angles C35 1.3878 (0.0110) C37 1.3929 (0.0125) 119.71 (0.84) H36 0.9500 120.14 120.14 C36 - C35 C37 C37 - Distance Angles C38 1.3622 (0.0136) C36 1.3929 (0.0125) 120.72 (0.83) H37 0.9500 119.64 119.64 C37 - C38 C36 C38 - Distance Angles C37 1.3622 (0.0137) C39 1.3922 (0.0127) 120.49 (0.87) H38 0.9500 119.76 119.76 C38 - C37 C39 C39 - Distance Angles C38 1.3922 (0.0128) C40 1.3976 (0.0119) 119.43 (0.84) H39 0.9500 120.28 120.28 C39 - C38 C40 C40 - Distance Angles C35 1.3952 (0.0113) C39 1.3976 (0.0119) 119.89 (0.76) H40 0.9500 120.06 120.06 C40 - C35 C39 P2 - Distance Angles C35 1.8226 (0.0080) C21 1.8293 (0.0081) 105.74 (0.37) C29 1.8371 (0.0077) 102.61 (0.37) 103.70 (0.36) Pt1 2.2644 (0.0019) 116.05 (0.26) 107.69 (0.25) 119.64 (0.24) P2 - C35 C21 C29 FMAP and GRID set by program FMAP 2 3 36 GRID -1.515 -2 -2 1.515 2 2 R1 = 0.0764 for 7716 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 3.37 at 0.4010 0.4191 0.2422 [ 0.91 A from PT1 ] Deepest hole -1.99 at 0.5504 0.4540 0.2274 [ 0.86 A from PT1 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 4278 / 32136 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5990 0.5809 0.7578 1.00000 0.05 3.37 0.91 PT1 1.72 CL1 1.92 CL2 2.89 P1 Q2 1 0.4567 0.6315 0.7786 1.00000 0.05 2.97 0.89 PT1 1.68 P2 1.92 P1 2.52 H20 Q3 1 0.5411 0.6209 0.7178 1.00000 0.05 2.55 0.84 PT1 2.21 CL1 2.24 H2 2.26 P1 Q4 1 0.5230 0.5721 0.8213 1.00000 0.05 2.06 0.90 PT1 2.17 CL2 2.26 H39 2.31 H40 Q5 1 0.5573 0.8002 1.3081 1.00000 0.05 1.81 1.53 H38 2.10 C38 2.42 H8A 2.61 H13 Shortest distances between peaks (including symmetry equivalents) 1 3 1.06 1 4 1.27 2 3 1.32 2 4 1.33 3 4 1.73 1 2 1.79 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 10.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 10.28: Structure factors and derivatives 30.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.16: Apply other restraints 6.41: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.25: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0043 finished at 09:36:09 Total CPU time: 57.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++