+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0437r started at 11:44:26 on 08-Jun-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0437r in P2(1)/c CELL 0.71073 19.4376 11.1178 30.2758 90.000 91.579 90.000 ZERR 8.00 0.0015 0.0011 0.0027 0.000 0.008 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P CL FE PD UNIT 244 424 16 24 8 8 V = 6540.22 F(000) = 3112.0 Mu = 1.36 mm-1 Cell Wt = 6002.15 Rho = 1.524 MERG 2 OMIT -3.00 55.00 OMIT 1 0 4 OMIT -8 11 3 OMIT 2 1 33 OMIT -6 10 3 OMIT 1 0 32 OMIT -8 11 11 OMIT -7 12 10 OMIT -7 12 16 OMIT 0 1 35 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.16 0.40 0.56 ACTA BOND $H WGHT 0.02430 7.47680 L.S. 10 TEMP -153.00 FVAR 0.19213 MOLE 1 C1 1 0.163739 0.515676 0.867719 11.00000 0.01204 0.01144 = 0.01503 -0.00013 0.00041 -0.00211 C2 1 0.135586 0.549892 0.909733 11.00000 0.01466 0.01532 = 0.01679 -0.00414 0.00220 -0.00106 C3 1 0.075845 0.621853 0.900348 11.00000 0.01676 0.01376 = 0.02398 -0.00624 0.00317 -0.00068 C4 1 0.066381 0.631787 0.853819 11.00000 0.01503 0.01194 = 0.02559 0.00266 0.00265 0.00078 C5 1 0.120430 0.568384 0.833241 11.00000 0.01548 0.01242 = 0.01913 0.00371 0.00148 -0.00056 C6 1 0.069933 0.274083 0.863660 11.00000 0.01218 0.01046 = 0.01356 0.00087 -0.00157 -0.00014 C7 1 0.043258 0.303512 0.906637 11.00000 0.01517 0.01363 = 0.01717 0.00272 0.00365 0.00032 C8 1 -0.017515 0.374598 0.899248 11.00000 0.01346 0.01397 = 0.02386 0.00045 0.00544 -0.00169 C9 1 -0.029319 0.387814 0.853120 11.00000 0.01093 0.01742 = 0.02650 -0.00281 -0.00195 -0.00050 C10 1 0.024209 0.328734 0.830733 11.00000 0.01534 0.01465 = 0.01675 -0.00225 -0.00515 -0.00003 C11 1 0.160244 0.525229 0.956117 11.00000 0.01787 0.03706 = 0.01370 -0.00874 0.00099 0.00038 AFIX 137 H11A 2 0.189887 0.591319 0.966481 11.00000 -1.50000 H11B 2 0.186369 0.449835 0.956956 11.00000 -1.50000 H11C 2 0.120622 0.518383 0.975286 11.00000 -1.50000 AFIX 0 C12 1 0.033282 0.682649 0.934192 11.00000 0.02483 0.02457 = 0.03600 -0.00998 0.00803 0.00279 AFIX 137 H12A 2 0.051141 0.763853 0.939724 11.00000 -1.50000 H12B 2 0.035406 0.636236 0.961714 11.00000 -1.50000 H12C 2 -0.014582 0.687686 0.923309 11.00000 -1.50000 AFIX 0 C13 1 0.008985 0.697697 0.830299 11.00000 0.02243 0.02041 = 0.03944 0.01169 0.00276 0.00803 AFIX 137 H13A 2 -0.030850 0.701936 0.849386 11.00000 -1.50000 H13B 2 -0.003885 0.654970 0.802990 11.00000 -1.50000 H13C 2 0.024150 0.779293 0.823135 11.00000 -1.50000 AFIX 0 C14 1 0.131153 0.567553 0.784381 11.00000 0.01708 0.02814 = 0.01849 0.00855 0.00168 0.00339 AFIX 137 H14A 2 0.086455 0.571411 0.768662 11.00000 -1.50000 H14B 2 0.154988 0.493467 0.776223 11.00000 -1.50000 H14C 2 0.159022 0.637238 0.776329 11.00000 -1.50000 AFIX 0 C15 1 0.068469 0.270479 0.951991 11.00000 0.02775 0.02103 = 0.01529 0.00344 0.00419 0.00422 AFIX 137 H15A 2 0.061160 0.338094 0.972091 11.00000 -1.50000 H15B 2 0.117682 0.251575 0.951441 11.00000 -1.50000 H15C 2 0.043133 0.200056 0.962249 11.00000 -1.50000 AFIX 0 C16 1 -0.063046 0.422668 0.934279 11.00000 0.02182 0.02311 = 0.03616 -0.00210 0.01496 0.00161 AFIX 137 H16A 2 -0.087296 0.494221 0.923119 11.00000 -1.50000 H16B 2 -0.034973 0.444125 0.960487 11.00000 -1.50000 H16C 2 -0.096647 0.361095 0.942141 11.00000 -1.50000 AFIX 0 C17 1 -0.090499 0.447159 0.831371 11.00000 0.01727 0.02533 = 0.04134 -0.00583 -0.01237 0.00559 AFIX 137 H17A 2 -0.127965 0.388636 0.827920 11.00000 -1.50000 H17B 2 -0.078014 0.477367 0.802258 11.00000 -1.50000 H17C 2 -0.105580 0.514333 0.849695 11.00000 -1.50000 AFIX 0 C18 1 0.027541 0.319638 0.781501 11.00000 0.02563 0.02271 = 0.01663 -0.00179 -0.00853 0.00451 AFIX 137 H18A 2 -0.001615 0.253043 0.771006 11.00000 -1.50000 H18B 2 0.075194 0.304955 0.773211 11.00000 -1.50000 H18C 2 0.011225 0.394963 0.768059 11.00000 -1.50000 AFIX 0 C19 1 0.293162 0.562020 0.830328 11.00000 0.01772 0.01688 = 0.01888 0.00296 0.00156 -0.00399 AFIX 13 H19 2 0.274903 0.575111 0.799500 11.00000 -1.20000 AFIX 0 C20 1 0.282814 0.681475 0.854602 11.00000 0.02995 0.01598 = 0.03022 0.00177 0.00289 -0.00743 AFIX 137 H20A 2 0.299666 0.673746 0.885277 11.00000 -1.50000 H20B 2 0.233740 0.701797 0.854147 11.00000 -1.50000 H20C 2 0.308425 0.745206 0.839893 11.00000 -1.50000 AFIX 0 C21 1 0.369456 0.534301 0.826155 11.00000 0.01605 0.03247 = 0.02271 0.00079 0.00182 -0.00803 AFIX 137 H21A 2 0.390248 0.593371 0.806544 11.00000 -1.50000 H21B 2 0.374935 0.453449 0.813847 11.00000 -1.50000 H21C 2 0.392269 0.538250 0.855392 11.00000 -1.50000 AFIX 0 C22 1 0.287657 0.380349 0.903156 11.00000 0.01568 0.01728 = 0.01340 0.00187 -0.00126 -0.00085 AFIX 13 H22 2 0.253054 0.335584 0.920643 11.00000 -1.20000 AFIX 0 C23 1 0.343218 0.289059 0.891399 11.00000 0.02072 0.02410 = 0.02358 -0.00437 -0.00665 0.00651 AFIX 137 H23A 2 0.382878 0.331451 0.879547 11.00000 -1.50000 H23B 2 0.324648 0.232896 0.869153 11.00000 -1.50000 H23C 2 0.357691 0.244401 0.917971 11.00000 -1.50000 AFIX 0 C24 1 0.319770 0.474555 0.934371 11.00000 0.01916 0.02153 = 0.01585 -0.00325 -0.00383 0.00018 AFIX 137 H24A 2 0.329969 0.437742 0.963225 11.00000 -1.50000 H24B 2 0.287442 0.541284 0.937908 11.00000 -1.50000 H24C 2 0.362441 0.504899 0.921948 11.00000 -1.50000 AFIX 0 C25 1 0.090858 0.061272 0.813627 11.00000 0.01529 0.01548 = 0.01619 -0.00323 0.00095 -0.00193 AFIX 13 H25 2 0.082271 0.095785 0.783475 11.00000 -1.20000 AFIX 0 C26 1 0.019593 0.032566 0.831303 11.00000 0.01291 0.02004 = 0.02974 -0.00428 0.00085 -0.00477 AFIX 137 H26A 2 -0.005614 -0.018817 0.810120 11.00000 -1.50000 H26B 2 -0.005948 0.107547 0.835426 11.00000 -1.50000 H26C 2 0.024762 -0.009391 0.859667 11.00000 -1.50000 AFIX 0 C27 1 0.132141 -0.054671 0.806535 11.00000 0.02088 0.01553 = 0.02127 -0.00624 0.00236 -0.00115 AFIX 137 H27A 2 0.133038 -0.102341 0.833772 11.00000 -1.50000 H27B 2 0.179314 -0.034087 0.798760 11.00000 -1.50000 H27C 2 0.110402 -0.101530 0.782549 11.00000 -1.50000 AFIX 0 C28 1 0.179912 0.101792 0.893372 11.00000 0.01732 0.01528 = 0.01462 0.00309 -0.00290 0.00060 AFIX 13 H28 2 0.194773 0.166415 0.914536 11.00000 -1.20000 AFIX 0 C29 1 0.245658 0.032485 0.881561 11.00000 0.01683 0.02356 = 0.03309 0.00365 -0.00127 0.00461 AFIX 137 H29A 2 0.276725 0.028338 0.907565 11.00000 -1.50000 H29B 2 0.268686 0.074227 0.857588 11.00000 -1.50000 H29C 2 0.233327 -0.049135 0.872027 11.00000 -1.50000 AFIX 0 C30 1 0.132042 0.018688 0.918729 11.00000 0.02683 0.01864 = 0.01772 0.00518 -0.00108 -0.00149 AFIX 137 H30A 2 0.127483 -0.058277 0.903143 11.00000 -1.50000 H30B 2 0.086654 0.056363 0.920728 11.00000 -1.50000 H30C 2 0.151375 0.004829 0.948531 11.00000 -1.50000 AFIX 0 P1 3 0.241593 0.435470 0.853087 11.00000 0.01043 0.01314 = 0.01026 -0.00026 -0.00006 -0.00021 P2 3 0.139806 0.178881 0.845214 11.00000 0.01091 0.01121 = 0.01218 -0.00041 0.00042 -0.00013 CL1 4 0.288313 0.376655 0.750951 11.00000 0.01956 0.02517 = 0.01348 0.00098 0.00561 -0.00434 CL2 4 0.192114 0.151285 0.743095 11.00000 0.03230 0.02554 = 0.01486 -0.00761 0.00539 -0.00875 FE1 5 0.066392 0.454255 0.871806 11.00000 0.01036 0.01161 = 0.01095 0.00065 -0.00023 0.00150 PD1 6 0.216124 0.284273 0.801881 11.00000 0.01144 0.01362 = 0.00889 -0.00071 0.00095 -0.00017 MOLE 2 C31 1 0.421234 0.574939 0.614561 11.00000 0.00868 0.01314 = 0.01383 0.00032 0.00045 0.00106 C32 1 0.423359 0.648627 0.654099 11.00000 0.01229 0.01378 = 0.01685 -0.00176 -0.00245 0.00116 C33 1 0.441147 0.767961 0.640452 11.00000 0.00900 0.01494 = 0.02355 -0.00292 -0.00167 -0.00066 C34 1 0.448776 0.769448 0.593794 11.00000 0.01036 0.01564 = 0.02196 0.00042 0.00226 -0.00064 C35 1 0.436448 0.651015 0.577482 11.00000 0.01092 0.01550 = 0.01462 0.00162 0.00333 0.00035 C36 1 0.258717 0.630667 0.600300 11.00000 0.01010 0.01355 = 0.01301 -0.00095 -0.00071 0.00022 C37 1 0.258991 0.704332 0.639595 11.00000 0.00995 0.01159 = 0.01600 -0.00263 0.00103 0.00030 C38 1 0.273780 0.825033 0.626451 11.00000 0.01099 0.01290 = 0.02252 -0.00235 -0.00058 0.00276 C39 1 0.282125 0.827609 0.580079 11.00000 0.01239 0.01342 = 0.02591 0.00471 -0.00321 0.00115 C40 1 0.273453 0.708542 0.563205 11.00000 0.01268 0.01667 = 0.01634 0.00309 -0.00285 -0.00045 C41 1 0.410246 0.619455 0.701304 11.00000 0.02065 0.01860 = 0.01634 -0.00258 -0.00129 0.00303 AFIX 137 H41A 2 0.453821 0.599236 0.716585 11.00000 -1.50000 H41B 2 0.378778 0.550772 0.702694 11.00000 -1.50000 H41C 2 0.389537 0.689224 0.715591 11.00000 -1.50000 AFIX 0 C42 1 0.454046 0.871563 0.670912 11.00000 0.01976 0.01515 = 0.03199 -0.00810 -0.00279 -0.00143 AFIX 137 H42A 2 0.501190 0.867068 0.683131 11.00000 -1.50000 H42B 2 0.421486 0.868573 0.695032 11.00000 -1.50000 H42C 2 0.447932 0.947078 0.654575 11.00000 -1.50000 AFIX 0 C43 1 0.469984 0.875014 0.566429 11.00000 0.02229 0.01565 = 0.03294 0.00456 0.00724 -0.00363 AFIX 137 H43A 2 0.519627 0.871302 0.561752 11.00000 -1.50000 H43B 2 0.458977 0.949782 0.581856 11.00000 -1.50000 H43C 2 0.445194 0.872888 0.537812 11.00000 -1.50000 AFIX 0 C44 1 0.443793 0.614733 0.530365 11.00000 0.02381 0.01983 = 0.01612 0.00143 0.00583 0.00131 AFIX 137 H44A 2 0.428765 0.680921 0.511021 11.00000 -1.50000 H44B 2 0.415340 0.543639 0.524139 11.00000 -1.50000 H44C 2 0.492096 0.595825 0.525008 11.00000 -1.50000 AFIX 0 C45 1 0.244187 0.671918 0.686404 11.00000 0.01888 0.01717 = 0.01769 -0.00209 0.00275 -0.00350 AFIX 137 H45A 2 0.272160 0.722147 0.706527 11.00000 -1.50000 H45B 2 0.255412 0.587029 0.691515 11.00000 -1.50000 H45C 2 0.195304 0.685370 0.691797 11.00000 -1.50000 AFIX 0 C46 1 0.278122 0.932865 0.656019 11.00000 0.01753 0.01296 = 0.03093 -0.00521 0.00039 0.00043 AFIX 137 H46A 2 0.317502 0.982497 0.647949 11.00000 -1.50000 H46B 2 0.283993 0.906631 0.686794 11.00000 -1.50000 H46C 2 0.235713 0.980050 0.652668 11.00000 -1.50000 AFIX 0 C47 1 0.294674 0.938572 0.553269 11.00000 0.02729 0.01881 = 0.02966 0.00962 -0.00642 -0.00124 AFIX 137 H47A 2 0.250607 0.977254 0.545695 11.00000 -1.50000 H47B 2 0.317888 0.916484 0.526112 11.00000 -1.50000 H47C 2 0.323723 0.994455 0.570489 11.00000 -1.50000 AFIX 0 C48 1 0.274339 0.676295 0.515199 11.00000 0.02529 0.02242 = 0.01485 0.00411 -0.00178 -0.00115 AFIX 137 H48A 2 0.228818 0.691239 0.501581 11.00000 -1.50000 H48B 2 0.286062 0.591035 0.512103 11.00000 -1.50000 H48C 2 0.308719 0.725509 0.500499 11.00000 -1.50000 AFIX 0 C49 1 0.399664 0.341836 0.658620 11.00000 0.02040 0.01438 = 0.01414 0.00284 -0.00036 -0.00203 AFIX 13 H49 2 0.361207 0.385576 0.672900 11.00000 -1.20000 AFIX 0 C50 1 0.375458 0.210960 0.653152 11.00000 0.03975 0.01671 = 0.02930 0.00627 -0.00261 -0.00827 AFIX 137 H50A 2 0.415527 0.157443 0.653333 11.00000 -1.50000 H50B 2 0.349665 0.202392 0.625058 11.00000 -1.50000 H50C 2 0.345747 0.189587 0.677577 11.00000 -1.50000 AFIX 0 C51 1 0.461095 0.348177 0.691334 11.00000 0.02623 0.02098 = 0.01775 0.00160 -0.00382 0.00469 AFIX 137 H51A 2 0.445259 0.334283 0.721359 11.00000 -1.50000 H51B 2 0.482477 0.427826 0.689714 11.00000 -1.50000 H51C 2 0.494850 0.286481 0.683857 11.00000 -1.50000 AFIX 0 C52 1 0.497874 0.372505 0.584865 11.00000 0.01376 0.01827 = 0.01704 -0.00201 -0.00015 0.00415 AFIX 13 H52 2 0.496199 0.386803 0.552244 11.00000 -1.20000 AFIX 0 C53 1 0.557486 0.448846 0.603186 11.00000 0.01322 0.03569 = 0.02837 -0.00638 -0.00121 0.00113 AFIX 137 H53A 2 0.564510 0.432219 0.634777 11.00000 -1.50000 H53B 2 0.546687 0.534249 0.598974 11.00000 -1.50000 H53C 2 0.599491 0.429026 0.587556 11.00000 -1.50000 AFIX 0 C54 1 0.514956 0.238455 0.590969 11.00000 0.03060 0.02373 = 0.02937 -0.00213 0.00115 0.01456 AFIX 137 H54A 2 0.553401 0.216892 0.572250 11.00000 -1.50000 H54B 2 0.474575 0.189969 0.582564 11.00000 -1.50000 H54C 2 0.527785 0.223027 0.621983 11.00000 -1.50000 AFIX 0 C55 1 0.155028 0.498176 0.555672 11.00000 0.01271 0.02117 = 0.01937 -0.00138 -0.00476 -0.00069 AFIX 13 H55 2 0.169454 0.514071 0.524763 11.00000 -1.20000 AFIX 0 C56 1 0.106086 0.390730 0.552850 11.00000 0.02032 0.03145 = 0.02366 -0.00643 -0.00434 -0.00997 AFIX 137 H56A 2 0.084247 0.379629 0.581354 11.00000 -1.50000 H56B 2 0.132003 0.318139 0.545527 11.00000 -1.50000 H56C 2 0.070619 0.405510 0.529857 11.00000 -1.50000 AFIX 0 C57 1 0.114485 0.609117 0.569635 11.00000 0.01285 0.02554 = 0.04268 -0.00086 -0.00685 0.00476 AFIX 137 H57A 2 0.074993 0.620776 0.549262 11.00000 -1.50000 H57B 2 0.144330 0.680094 0.568912 11.00000 -1.50000 H57C 2 0.098155 0.597564 0.599676 11.00000 -1.50000 AFIX 0 C58 1 0.212691 0.391774 0.639535 11.00000 0.01670 0.01381 = 0.01363 -0.00147 0.00151 -0.00101 AFIX 13 H58 2 0.252633 0.399038 0.660900 11.00000 -1.20000 AFIX 0 C59 1 0.204643 0.256829 0.628998 11.00000 0.03066 0.01637 = 0.02511 0.00376 0.00871 -0.00237 AFIX 137 H59A 2 0.209161 0.210222 0.656399 11.00000 -1.50000 H59B 2 0.240437 0.232079 0.608716 11.00000 -1.50000 H59C 2 0.159212 0.242363 0.615178 11.00000 -1.50000 AFIX 0 C60 1 0.149400 0.434446 0.663816 11.00000 0.01602 0.02346 = 0.02018 -0.00345 0.00447 -0.00397 AFIX 137 H60A 2 0.107696 0.407917 0.647699 11.00000 -1.50000 H60B 2 0.149757 0.522448 0.665663 11.00000 -1.50000 H60C 2 0.150102 0.400376 0.693678 11.00000 -1.50000 AFIX 0 P31 3 0.410882 0.414831 0.604833 11.00000 0.01174 0.00978 = 0.01167 -0.00080 -0.00012 0.00056 P32 3 0.236566 0.474429 0.589158 11.00000 0.01079 0.01139 = 0.01202 -0.00166 0.00027 -0.00043 CL31 4 0.398418 0.252667 0.513997 11.00000 0.01666 0.04665 = 0.03789 -0.03039 0.00166 0.00159 CL32 4 0.242490 0.315478 0.498138 11.00000 0.02380 0.04278 = 0.02125 -0.01712 -0.01028 0.00825 FE31 5 0.351571 0.709301 0.609098 11.00000 0.01023 0.00974 = 0.01261 0.00029 0.00046 -0.00048 PD31 6 0.322438 0.369247 0.554102 11.00000 0.01169 0.01242 = 0.01007 -0.00257 0.00025 -0.00079 MOLE 3 C71 1 0.363674 0.058701 0.759044 11.00000 0.03706 0.03204 = 0.02127 0.00340 0.00162 0.00378 AFIX 23 H71A 2 0.392403 0.052374 0.732646 11.00000 -1.20000 H71B 2 0.320822 0.101740 0.750338 11.00000 -1.20000 AFIX 0 CL71 4 0.342886 -0.087641 0.777733 11.00000 0.04910 0.03371 = 0.03056 0.00365 -0.00047 -0.00666 CL72 4 0.407908 0.140661 0.799834 11.00000 0.03547 0.03258 = 0.03798 -0.00106 -0.00566 0.00266 HKLF 4 Covalent radii and connectivity table for 04src0437r in P2(1)/c C 0.770 H 0.320 P 1.100 CL 0.990 FE 1.240 PD 1.380 C1 - C5 C2 P1 Fe1 C2 - C3 C1 C11 Fe1 C3 - C4 C2 C12 Fe1 C4 - C3 C5 C13 Fe1 C5 - C4 C1 C14 Fe1 C6 - C10 C7 P2 Fe1 C7 - C8 C6 C15 Fe1 C8 - C9 C7 C16 Fe1 C9 - C8 C10 C17 Fe1 C10 - C9 C6 C18 Fe1 C11 - C2 C12 - C3 C13 - C4 C14 - C5 C15 - C7 C16 - C8 C17 - C9 C18 - C10 C19 - C21 C20 P1 C20 - C19 C21 - C19 C22 - C23 C24 P1 C23 - C22 C24 - C22 C25 - C26 C27 P2 C26 - C25 C27 - C25 C28 - C30 C29 P2 C29 - C28 C30 - C28 P1 - C1 C22 C19 Pd1 P2 - C6 C28 C25 Pd1 Cl1 - Pd1 Cl2 - Pd1 Fe1 - C1 C6 C10 C5 C7 C2 C4 C8 C3 C9 Pd1 - P2 P1 Cl1 Cl2 C31 - C35 C32 P31 Fe31 C32 - C33 C31 C41 Fe31 C33 - C34 C32 C42 Fe31 C34 - C35 C33 C43 Fe31 C35 - C34 C31 C44 Fe31 C36 - C37 C40 P32 Fe31 C37 - C38 C36 C45 Fe31 C38 - C39 C37 C46 Fe31 C39 - C38 C40 C47 Fe31 C40 - C39 C36 C48 Fe31 C41 - C32 C42 - C33 C43 - C34 C44 - C35 C45 - C37 C46 - C38 C47 - C39 C48 - C40 C49 - C51 C50 P31 C50 - C49 C51 - C49 C52 - C53 C54 P31 C53 - C52 C54 - C52 C55 - C56 C57 P32 C56 - C55 C57 - C55 C58 - C60 C59 P32 C59 - C58 C60 - C58 P31 - C31 C49 C52 Pd31 P32 - C36 C58 C55 Pd31 Cl31 - Pd31 Cl32 - Pd31 Fe31 - C36 C31 C40 C35 C32 C37 C39 C38 C33 C34 Pd31 - P32 P31 Cl31 Cl32 C71 - Cl72 Cl71 Cl71 - C71 Cl72 - C71 50486 Reflections read, of which 1682 rejected -22 =< h =< 25, -14 =< k =< 14, -39 =< l =< 35, 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) 2 0 20 902.91 32.19 2 162.97 1 Inconsistent equivalents 14858 Unique reflections, of which 0 suppressed R(int) = 0.0337 R(sigma) = 0.0373 Friedel opposites merged Maximum memory for data reduction = 8555 / 148778 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 = 10772 / 1001017 wR2 = 0.0689 before cycle 1 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 -0.045 OSF Mean shift/esd = 0.003 Maximum = 0.065 for z Pd1 Max. shift = 0.000 A for H50A Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 2 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19212 0.00011 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.022 for z Pd1 Max. shift = 0.000 A for H50A Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 3 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19212 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H13B Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 4 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H13A Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 5 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H24C Max. dU = 0.000 for C4 Least-squares cycle 6 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 6 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H26B Max. dU = 0.000 for C60 Least-squares cycle 7 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 7 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C17 Least-squares cycle 8 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 8 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H42B Max. dU = 0.000 for C39 Least-squares cycle 9 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 9 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for C44 Max. dU = 0.000 for C57 Least-squares cycle 10 Maximum vector length = 511 Memory required = 10772 / 1001017 wR2 = 0.0689 before cycle 10 for 14858 data and 708 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19213 0.00011 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for z Pd31 Max. shift = 0.000 A for H12B Max. dU = 0.000 for C51 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H11A 0.1899 0.5913 0.9665 137 0.980 0.000 C11 C2 H11A H11B 0.1864 0.4498 0.9570 137 0.980 0.000 C11 C2 H11A H11C 0.1206 0.5184 0.9753 137 0.980 0.000 C11 C2 H11A H12A 0.0511 0.7639 0.9397 137 0.980 0.000 C12 C3 H12A H12B 0.0354 0.6362 0.9617 137 0.980 0.000 C12 C3 H12A H12C -0.0146 0.6877 0.9233 137 0.980 0.000 C12 C3 H12A H13A -0.0308 0.7019 0.8494 137 0.980 0.000 C13 C4 H13A H13B -0.0039 0.6550 0.8030 137 0.980 0.000 C13 C4 H13A H13C 0.0242 0.7793 0.8231 137 0.980 0.000 C13 C4 H13A H14A 0.0865 0.5714 0.7687 137 0.980 0.000 C14 C5 H14A H14B 0.1550 0.4935 0.7762 137 0.980 0.000 C14 C5 H14A H14C 0.1590 0.6372 0.7763 137 0.980 0.000 C14 C5 H14A H15A 0.0612 0.3381 0.9721 137 0.980 0.000 C15 C7 H15A H15B 0.1177 0.2516 0.9514 137 0.980 0.000 C15 C7 H15A H15C 0.0431 0.2001 0.9622 137 0.980 0.000 C15 C7 H15A H16A -0.0873 0.4942 0.9231 137 0.980 0.000 C16 C8 H16A H16B -0.0350 0.4441 0.9605 137 0.980 0.000 C16 C8 H16A H16C -0.0966 0.3611 0.9421 137 0.980 0.000 C16 C8 H16A H17A -0.1280 0.3886 0.8279 137 0.980 0.000 C17 C9 H17A H17B -0.0780 0.4774 0.8023 137 0.980 0.000 C17 C9 H17A H17C -0.1056 0.5143 0.8497 137 0.980 0.000 C17 C9 H17A H18A -0.0016 0.2530 0.7710 137 0.980 0.000 C18 C10 H18A H18B 0.0752 0.3050 0.7732 137 0.980 0.000 C18 C10 H18A H18C 0.0112 0.3950 0.7681 137 0.980 0.000 C18 C10 H18A H19 0.2749 0.5751 0.7995 13 1.000 0.000 C19 C21 C20 P1 H20A 0.2997 0.6737 0.8853 137 0.980 0.000 C20 C19 H20A H20B 0.2337 0.7018 0.8541 137 0.980 0.000 C20 C19 H20A H20C 0.3084 0.7452 0.8399 137 0.980 0.000 C20 C19 H20A H21A 0.3902 0.5934 0.8065 137 0.980 0.000 C21 C19 H21A H21B 0.3749 0.4535 0.8138 137 0.980 0.000 C21 C19 H21A H21C 0.3923 0.5382 0.8554 137 0.980 0.000 C21 C19 H21A H22 0.2531 0.3356 0.9206 13 1.000 0.000 C22 C23 C24 P1 H23A 0.3829 0.3315 0.8795 137 0.980 0.000 C23 C22 H23A H23B 0.3246 0.2329 0.8692 137 0.980 0.000 C23 C22 H23A H23C 0.3577 0.2444 0.9180 137 0.980 0.000 C23 C22 H23A H24A 0.3300 0.4377 0.9632 137 0.980 0.000 C24 C22 H24A H24B 0.2874 0.5413 0.9379 137 0.980 0.000 C24 C22 H24A H24C 0.3624 0.5049 0.9219 137 0.980 0.000 C24 C22 H24A H25 0.0823 0.0958 0.7835 13 1.000 0.000 C25 C26 C27 P2 H26A -0.0056 -0.0188 0.8101 137 0.980 0.000 C26 C25 H26A H26B -0.0059 0.1075 0.8354 137 0.980 0.000 C26 C25 H26A H26C 0.0248 -0.0094 0.8597 137 0.980 0.000 C26 C25 H26A H27A 0.1330 -0.1023 0.8338 137 0.980 0.000 C27 C25 H27A H27B 0.1793 -0.0341 0.7988 137 0.980 0.000 C27 C25 H27A H27C 0.1104 -0.1015 0.7825 137 0.980 0.000 C27 C25 H27A H28 0.1948 0.1664 0.9145 13 1.000 0.000 C28 C30 C29 P2 H29A 0.2767 0.0283 0.9076 137 0.980 0.000 C29 C28 H29A H29B 0.2687 0.0742 0.8576 137 0.980 0.000 C29 C28 H29A H29C 0.2333 -0.0491 0.8720 137 0.980 0.000 C29 C28 H29A H30A 0.1275 -0.0583 0.9031 137 0.980 0.000 C30 C28 H30A H30B 0.0867 0.0564 0.9207 137 0.980 0.000 C30 C28 H30A H30C 0.1514 0.0048 0.9485 137 0.980 0.000 C30 C28 H30A H41A 0.4538 0.5992 0.7166 137 0.980 0.000 C41 C32 H41A H41B 0.3788 0.5508 0.7027 137 0.980 0.000 C41 C32 H41A H41C 0.3895 0.6892 0.7156 137 0.980 0.000 C41 C32 H41A H42A 0.5012 0.8671 0.6831 137 0.980 0.000 C42 C33 H42A H42B 0.4215 0.8686 0.6950 137 0.980 0.000 C42 C33 H42A H42C 0.4479 0.9471 0.6546 137 0.980 0.000 C42 C33 H42A H43A 0.5196 0.8713 0.5618 137 0.980 0.000 C43 C34 H43A H43B 0.4590 0.9498 0.5819 137 0.980 0.000 C43 C34 H43A H43C 0.4452 0.8729 0.5378 137 0.980 0.000 C43 C34 H43A H44A 0.4288 0.6809 0.5110 137 0.980 0.000 C44 C35 H44A H44B 0.4153 0.5436 0.5241 137 0.980 0.000 C44 C35 H44A H44C 0.4921 0.5958 0.5250 137 0.980 0.000 C44 C35 H44A H45A 0.2722 0.7221 0.7065 137 0.980 0.000 C45 C37 H45A H45B 0.2554 0.5870 0.6915 137 0.980 0.000 C45 C37 H45A H45C 0.1953 0.6854 0.6918 137 0.980 0.000 C45 C37 H45A H46A 0.3175 0.9825 0.6479 137 0.980 0.000 C46 C38 H46A H46B 0.2840 0.9066 0.6868 137 0.980 0.000 C46 C38 H46A H46C 0.2357 0.9801 0.6527 137 0.980 0.000 C46 C38 H46A H47A 0.2506 0.9773 0.5457 137 0.980 0.000 C47 C39 H47A H47B 0.3179 0.9165 0.5261 137 0.980 0.000 C47 C39 H47A H47C 0.3237 0.9945 0.5705 137 0.980 0.000 C47 C39 H47A H48A 0.2288 0.6912 0.5016 137 0.980 0.000 C48 C40 H48A H48B 0.2861 0.5910 0.5121 137 0.980 0.000 C48 C40 H48A H48C 0.3087 0.7255 0.5005 137 0.980 0.000 C48 C40 H48A H49 0.3612 0.3856 0.6729 13 1.000 0.000 C49 C51 C50 P31 H50A 0.4155 0.1574 0.6533 137 0.980 0.000 C50 C49 H50A H50B 0.3497 0.2024 0.6251 137 0.980 0.000 C50 C49 H50A H50C 0.3458 0.1896 0.6776 137 0.980 0.000 C50 C49 H50A H51A 0.4453 0.3343 0.7214 137 0.980 0.000 C51 C49 H51A H51B 0.4825 0.4278 0.6897 137 0.980 0.000 C51 C49 H51A H51C 0.4949 0.2865 0.6839 137 0.980 0.000 C51 C49 H51A H52 0.4962 0.3868 0.5522 13 1.000 0.000 C52 C53 C54 P31 H53A 0.5645 0.4322 0.6348 137 0.980 0.000 C53 C52 H53A H53B 0.5467 0.5342 0.5990 137 0.980 0.000 C53 C52 H53A H53C 0.5995 0.4290 0.5876 137 0.980 0.000 C53 C52 H53A H54A 0.5534 0.2169 0.5723 137 0.980 0.000 C54 C52 H54A H54B 0.4746 0.1900 0.5826 137 0.980 0.000 C54 C52 H54A H54C 0.5278 0.2230 0.6220 137 0.980 0.000 C54 C52 H54A H55 0.1695 0.5141 0.5248 13 1.000 0.000 C55 C56 C57 P32 H56A 0.0842 0.3796 0.5814 137 0.980 0.000 C56 C55 H56A H56B 0.1320 0.3181 0.5455 137 0.980 0.000 C56 C55 H56A H56C 0.0706 0.4055 0.5299 137 0.980 0.000 C56 C55 H56A H57A 0.0750 0.6208 0.5493 137 0.980 0.000 C57 C55 H57A H57B 0.1443 0.6801 0.5689 137 0.980 0.000 C57 C55 H57A H57C 0.0982 0.5976 0.5997 137 0.980 0.000 C57 C55 H57A H58 0.2526 0.3990 0.6609 13 1.000 0.000 C58 C60 C59 P32 H59A 0.2092 0.2102 0.6564 137 0.980 0.000 C59 C58 H59A H59B 0.2404 0.2321 0.6087 137 0.980 0.000 C59 C58 H59A H59C 0.1592 0.2424 0.6152 137 0.980 0.000 C59 C58 H59A H60A 0.1077 0.4079 0.6477 137 0.980 0.000 C60 C58 H60A H60B 0.1498 0.5224 0.6657 137 0.980 0.000 C60 C58 H60A H60C 0.1501 0.4004 0.6937 137 0.980 0.000 C60 C58 H60A H71A 0.3924 0.0524 0.7326 23 0.990 0.000 C71 Cl72 Cl71 H71B 0.3208 0.1017 0.7503 23 0.990 0.000 C71 Cl72 Cl71 04src0437r in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.16374 0.51568 0.86772 1.00000 0.01204 0.01143 0.01503 -0.00013 0.00041 -0.00211 0.01283 0.00380 0.00011 0.00020 0.00007 0.00000 0.00105 0.00106 0.00113 0.00089 0.00084 0.00084 0.00044 C2 0.13559 0.54989 0.90973 1.00000 0.01466 0.01532 0.01679 -0.00414 0.00220 -0.00106 0.01556 0.00397 0.00012 0.00021 0.00008 0.00000 0.00110 0.00115 0.00118 0.00094 0.00089 0.00090 0.00047 C3 0.07584 0.62185 0.90035 1.00000 0.01676 0.01376 0.02398 -0.00624 0.00317 -0.00068 0.01812 0.00412 0.00012 0.00021 0.00008 0.00000 0.00117 0.00116 0.00131 0.00099 0.00096 0.00091 0.00050 C4 0.06638 0.63179 0.85382 1.00000 0.01503 0.01194 0.02559 0.00266 0.00265 0.00078 0.01748 0.00426 0.00012 0.00021 0.00008 0.00000 0.00114 0.00111 0.00132 0.00099 0.00095 0.00089 0.00049 C5 0.12043 0.56838 0.83324 1.00000 0.01548 0.01242 0.01913 0.00371 0.00148 -0.00056 0.01566 0.00410 0.00012 0.00021 0.00008 0.00000 0.00111 0.00112 0.00121 0.00094 0.00090 0.00089 0.00047 C6 0.06993 0.27408 0.86366 1.00000 0.01218 0.01046 0.01356 0.00087 -0.00157 -0.00014 0.01210 0.00379 0.00011 0.00020 0.00007 0.00000 0.00105 0.00106 0.00111 0.00088 0.00084 0.00083 0.00044 C7 0.04326 0.30351 0.90664 1.00000 0.01517 0.01363 0.01717 0.00272 0.00365 0.00031 0.01526 0.00413 0.00012 0.00021 0.00008 0.00000 0.00111 0.00114 0.00119 0.00092 0.00089 0.00088 0.00047 C8 -0.01751 0.37460 0.89925 1.00000 0.01346 0.01397 0.02386 0.00045 0.00544 -0.00169 0.01700 0.00419 0.00012 0.00021 0.00008 0.00000 0.00112 0.00114 0.00130 0.00099 0.00093 0.00089 0.00049 C9 -0.02932 0.38781 0.85312 1.00000 0.01093 0.01742 0.02650 -0.00281 -0.00195 -0.00050 0.01833 0.00410 0.00012 0.00022 0.00008 0.00000 0.00110 0.00121 0.00134 0.00102 0.00094 0.00090 0.00050 C10 0.02421 0.32873 0.83073 1.00000 0.01534 0.01466 0.01675 -0.00225 -0.00515 -0.00003 0.01568 0.00394 0.00012 0.00021 0.00008 0.00000 0.00113 0.00113 0.00119 0.00094 0.00090 0.00089 0.00047 C11 0.16024 0.52523 0.95612 1.00000 0.01787 0.03706 0.01370 -0.00874 0.00099 0.00038 0.02286 0.00433 0.00013 0.00026 0.00008 0.00000 0.00120 0.00153 0.00119 0.00111 0.00093 0.00108 0.00055 H11A 0.18989 0.59132 0.96648 1.00000 0.03430 0.00000 0.00000 H11B 0.18637 0.44983 0.95696 1.00000 0.03430 0.00000 0.00000 H11C 0.12062 0.51838 0.97529 1.00000 0.03430 0.00000 0.00000 C12 0.03328 0.68265 0.93419 1.00000 0.02483 0.02457 0.03600 -0.00998 0.00803 0.00279 0.02834 0.00492 0.00014 0.00025 0.00010 0.00000 0.00139 0.00141 0.00162 0.00123 0.00118 0.00111 0.00062 H12A 0.05114 0.76385 0.93973 1.00000 0.04250 0.00000 0.00000 H12B 0.03540 0.63623 0.96171 1.00000 0.04250 0.00000 0.00000 H12C -0.01458 0.68769 0.92331 1.00000 0.04250 0.00000 0.00000 C13 0.00899 0.69770 0.83030 1.00000 0.02243 0.02040 0.03943 0.01169 0.00276 0.00803 0.02739 0.00518 0.00013 0.00024 0.00010 0.00000 0.00134 0.00135 0.00165 0.00120 0.00116 0.00106 0.00061 H13A -0.03085 0.70194 0.84939 1.00000 0.04108 0.00000 0.00000 H13B -0.00389 0.65497 0.80299 1.00000 0.04108 0.00000 0.00000 H13C 0.02415 0.77929 0.82313 1.00000 0.04108 0.00000 0.00000 C14 0.13115 0.56755 0.78438 1.00000 0.01708 0.02814 0.01849 0.00855 0.00168 0.00339 0.02121 0.00457 0.00012 0.00024 0.00008 0.00000 0.00118 0.00140 0.00126 0.00108 0.00094 0.00102 0.00053 H14A 0.08645 0.57141 0.76866 1.00000 0.03182 0.00000 0.00000 H14B 0.15499 0.49347 0.77622 1.00000 0.03182 0.00000 0.00000 H14C 0.15902 0.63724 0.77633 1.00000 0.03182 0.00000 0.00000 C15 0.06847 0.27048 0.95199 1.00000 0.02775 0.02102 0.01529 0.00344 0.00419 0.00422 0.02129 0.00457 0.00013 0.00023 0.00008 0.00000 0.00136 0.00129 0.00122 0.00102 0.00100 0.00105 0.00053 H15A 0.06116 0.33809 0.97209 1.00000 0.03193 0.00000 0.00000 H15B 0.11768 0.25158 0.95144 1.00000 0.03193 0.00000 0.00000 H15C 0.04313 0.20006 0.96225 1.00000 0.03193 0.00000 0.00000 C16 -0.06305 0.42267 0.93428 1.00000 0.02182 0.02311 0.03616 -0.00210 0.01496 0.00161 0.02677 0.00502 0.00013 0.00024 0.00009 0.00000 0.00132 0.00138 0.00158 0.00120 0.00114 0.00107 0.00060 H16A -0.08730 0.49422 0.92312 1.00000 0.04015 0.00000 0.00000 H16B -0.03497 0.44412 0.96049 1.00000 0.04015 0.00000 0.00000 H16C -0.09665 0.36110 0.94214 1.00000 0.04015 0.00000 0.00000 C17 -0.09050 0.44716 0.83137 1.00000 0.01727 0.02533 0.04134 -0.00583 -0.01237 0.00559 0.02822 0.00456 0.00013 0.00025 0.00010 0.00000 0.00126 0.00141 0.00169 0.00126 0.00114 0.00107 0.00062 H17A -0.12796 0.38864 0.82792 1.00000 0.04233 0.00000 0.00000 H17B -0.07801 0.47737 0.80226 1.00000 0.04233 0.00000 0.00000 H17C -0.10558 0.51433 0.84969 1.00000 0.04233 0.00000 0.00000 C18 0.02754 0.31964 0.78150 1.00000 0.02563 0.02272 0.01663 -0.00179 -0.00853 0.00451 0.02183 0.00435 0.00013 0.00024 0.00008 0.00000 0.00134 0.00131 0.00125 0.00104 0.00101 0.00104 0.00054 H18A -0.00162 0.25304 0.77101 1.00000 0.03274 0.00000 0.00000 H18B 0.07519 0.30495 0.77321 1.00000 0.03274 0.00000 0.00000 H18C 0.01123 0.39496 0.76806 1.00000 0.03274 0.00000 0.00000 C19 0.29316 0.56202 0.83033 1.00000 0.01772 0.01688 0.01888 0.00296 0.00156 -0.00399 0.01781 0.00418 0.00012 0.00021 0.00008 0.00000 0.00117 0.00119 0.00123 0.00099 0.00093 0.00094 0.00049 H19 0.27490 0.57511 0.79950 1.00000 0.02137 0.00000 0.00000 C20 0.28281 0.68148 0.85460 1.00000 0.02995 0.01598 0.03022 0.00177 0.00289 -0.00743 0.02535 0.00457 0.00014 0.00023 0.00009 0.00000 0.00145 0.00125 0.00150 0.00110 0.00115 0.00107 0.00058 H20A 0.29967 0.67375 0.88528 1.00000 0.03802 0.00000 0.00000 H20B 0.23374 0.70180 0.85415 1.00000 0.03802 0.00000 0.00000 H20C 0.30842 0.74521 0.83989 1.00000 0.03802 0.00000 0.00000 C21 0.36946 0.53430 0.82616 1.00000 0.01605 0.03247 0.02271 0.00079 0.00182 -0.00803 0.02372 0.00445 0.00012 0.00025 0.00009 0.00000 0.00120 0.00149 0.00134 0.00114 0.00098 0.00106 0.00056 H21A 0.39025 0.59337 0.80654 1.00000 0.03558 0.00000 0.00000 H21B 0.37494 0.45345 0.81385 1.00000 0.03558 0.00000 0.00000 H21C 0.39227 0.53825 0.85539 1.00000 0.03558 0.00000 0.00000 C22 0.28766 0.38035 0.90316 1.00000 0.01568 0.01727 0.01340 0.00187 -0.00126 -0.00085 0.01548 0.00399 0.00012 0.00021 0.00008 0.00000 0.00112 0.00119 0.00114 0.00093 0.00088 0.00091 0.00047 H22 0.25305 0.33558 0.92064 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0.00092 0.00048 H49 0.36121 0.38558 0.67290 1.00000 0.01959 0.00000 0.00000 C50 0.37546 0.21096 0.65315 1.00000 0.03975 0.01671 0.02930 0.00627 -0.00261 -0.00827 0.02865 0.00472 0.00015 0.00023 0.00009 0.00000 0.00163 0.00130 0.00151 0.00113 0.00123 0.00115 0.00062 H50A 0.41553 0.15744 0.65333 1.00000 0.04298 0.00000 0.00000 H50B 0.34966 0.20239 0.62506 1.00000 0.04298 0.00000 0.00000 H50C 0.34575 0.18958 0.67758 1.00000 0.04298 0.00000 0.00000 C51 0.46110 0.34818 0.69133 1.00000 0.02623 0.02098 0.01775 0.00160 -0.00383 0.00469 0.02174 0.00438 0.00013 0.00023 0.00008 0.00000 0.00134 0.00130 0.00126 0.00103 0.00101 0.00104 0.00053 H51A 0.44526 0.33428 0.72136 1.00000 0.03261 0.00000 0.00000 H51B 0.48248 0.42783 0.68972 1.00000 0.03261 0.00000 0.00000 H51C 0.49485 0.28648 0.68386 1.00000 0.03261 0.00000 0.00000 C52 0.49787 0.37250 0.58487 1.00000 0.01375 0.01827 0.01704 -0.00201 -0.00015 0.00415 0.01636 0.00410 0.00012 0.00021 0.00008 0.00000 0.00111 0.00120 0.00119 0.00097 0.00089 0.00092 0.00048 H52 0.49620 0.38680 0.55224 1.00000 0.01964 0.00000 0.00000 C53 0.55749 0.44885 0.60319 1.00000 0.01322 0.03569 0.02836 -0.00638 -0.00121 0.00113 0.02579 0.00442 0.00012 0.00026 0.00009 0.00000 0.00118 0.00156 0.00144 0.00122 0.00101 0.00108 0.00059 H53A 0.56451 0.43222 0.63478 1.00000 0.03868 0.00000 0.00000 H53B 0.54669 0.53425 0.59897 1.00000 0.03868 0.00000 0.00000 H53C 0.59949 0.42903 0.58756 1.00000 0.03868 0.00000 0.00000 C54 0.51496 0.23845 0.59097 1.00000 0.03060 0.02373 0.02937 -0.00213 0.00115 0.01455 0.02789 0.00507 0.00014 0.00024 0.00009 0.00000 0.00148 0.00140 0.00150 0.00117 0.00116 0.00114 0.00061 H54A 0.55340 0.21689 0.57225 1.00000 0.04184 0.00000 0.00000 H54B 0.47458 0.18997 0.58256 1.00000 0.04184 0.00000 0.00000 H54C 0.52778 0.22303 0.62198 1.00000 0.04184 0.00000 0.00000 C55 0.15503 0.49818 0.55567 1.00000 0.01271 0.02117 0.01937 -0.00138 -0.00476 -0.00069 0.01784 0.00398 0.00012 0.00022 0.00008 0.00000 0.00111 0.00127 0.00122 0.00101 0.00091 0.00094 0.00050 H55 0.16945 0.51407 0.52476 1.00000 0.02141 0.00000 0.00000 C56 0.10609 0.39073 0.55285 1.00000 0.02032 0.03144 0.02366 -0.00643 -0.00434 -0.00997 0.02523 0.00419 0.00013 0.00025 0.00009 0.00000 0.00129 0.00150 0.00138 0.00116 0.00103 0.00110 0.00058 H56A 0.08425 0.37963 0.58135 1.00000 0.03785 0.00000 0.00000 H56B 0.13200 0.31814 0.54553 1.00000 0.03785 0.00000 0.00000 H56C 0.07062 0.40551 0.52986 1.00000 0.03785 0.00000 0.00000 C57 0.11449 0.60912 0.56963 1.00000 0.01285 0.02554 0.04268 -0.00086 -0.00685 0.00476 0.02716 0.00470 0.00013 0.00024 0.00010 0.00000 0.00119 0.00141 0.00169 0.00123 0.00111 0.00102 0.00061 H57A 0.07499 0.62078 0.54926 1.00000 0.04074 0.00000 0.00000 H57B 0.14433 0.68009 0.56891 1.00000 0.04074 0.00000 0.00000 H57C 0.09815 0.59756 0.59968 1.00000 0.04074 0.00000 0.00000 C58 0.21269 0.39177 0.63954 1.00000 0.01670 0.01381 0.01363 -0.00147 0.00151 -0.00101 0.01469 0.00401 0.00012 0.00020 0.00008 0.00000 0.00114 0.00113 0.00114 0.00091 0.00088 0.00089 0.00046 H58 0.25263 0.39904 0.66090 1.00000 0.01763 0.00000 0.00000 C59 0.20464 0.25683 0.62900 1.00000 0.03065 0.01637 0.02511 0.00376 0.00871 -0.00237 0.02390 0.00471 0.00014 0.00022 0.00009 0.00000 0.00143 0.00124 0.00139 0.00107 0.00111 0.00105 0.00056 H59A 0.20916 0.21022 0.65640 1.00000 0.03585 0.00000 0.00000 H59B 0.24044 0.23208 0.60872 1.00000 0.03585 0.00000 0.00000 H59C 0.15921 0.24236 0.61518 1.00000 0.03585 0.00000 0.00000 C60 0.14940 0.43445 0.66382 1.00000 0.01602 0.02346 0.02018 -0.00345 0.00447 -0.00397 0.01981 0.00426 0.00012 0.00023 0.00008 0.00000 0.00116 0.00131 0.00127 0.00104 0.00094 0.00098 0.00051 H60A 0.10770 0.40792 0.64770 1.00000 0.02972 0.00000 0.00000 H60B 0.14976 0.52245 0.66566 1.00000 0.02972 0.00000 0.00000 H60C 0.15010 0.40037 0.69368 1.00000 0.02972 0.00000 0.00000 P31 0.41088 0.41483 0.60483 1.00000 0.01174 0.00978 0.01167 -0.00080 -0.00012 0.00056 0.01107 0.00098 0.00003 0.00005 0.00002 0.00000 0.00027 0.00027 0.00028 0.00022 0.00021 0.00021 0.00011 P32 0.23657 0.47443 0.58916 1.00000 0.01079 0.01139 0.01202 -0.00166 0.00027 -0.00043 0.01140 0.00098 0.00003 0.00005 0.00002 0.00000 0.00026 0.00027 0.00028 0.00022 0.00021 0.00021 0.00011 Cl31 0.39842 0.25267 0.51400 1.00000 0.01666 0.04665 0.03789 -0.03039 0.00166 0.00159 0.03371 0.00111 0.00003 0.00007 0.00002 0.00000 0.00030 0.00043 0.00039 0.00034 0.00027 0.00028 0.00017 Cl32 0.24249 0.31548 0.49814 1.00000 0.02380 0.04278 0.02125 -0.01712 -0.01028 0.00825 0.02948 0.00109 0.00003 0.00007 0.00002 0.00000 0.00032 0.00040 0.00032 0.00029 0.00025 0.00028 0.00016 Fe31 0.35157 0.70930 0.60910 1.00000 0.01023 0.00974 0.01261 0.00029 0.00046 -0.00048 0.01086 0.00054 0.00002 0.00003 0.00001 0.00000 0.00015 0.00015 0.00016 0.00012 0.00012 0.00012 0.00007 Pd31 0.32244 0.36925 0.55410 1.00000 0.01169 0.01242 0.01007 -0.00257 0.00025 -0.00079 0.01139 0.00029 0.00001 0.00002 0.00001 0.00000 0.00008 0.00009 0.00008 0.00007 0.00006 0.00006 0.00004 C71 0.36367 0.05870 0.75904 1.00000 0.03706 0.03203 0.02127 0.00340 0.00163 0.00378 0.03011 0.00499 0.00015 0.00026 0.00009 0.00000 0.00159 0.00156 0.00140 0.00120 0.00116 0.00126 0.00063 H71A 0.39240 0.05237 0.73265 1.00000 0.03613 0.00000 0.00000 H71B 0.32082 0.10174 0.75034 1.00000 0.03613 0.00000 0.00000 Cl71 0.34289 -0.08764 0.77773 1.00000 0.04911 0.03371 0.03056 0.00365 -0.00047 -0.00666 0.03782 0.00133 0.00004 0.00007 0.00002 0.00000 0.00046 0.00039 0.00039 0.00032 0.00032 0.00034 0.00017 Cl72 0.40791 0.14066 0.79983 1.00000 0.03547 0.03258 0.03799 -0.00106 -0.00566 0.00266 0.03547 0.00129 0.00004 0.00007 0.00003 0.00000 0.00039 0.00039 0.00041 0.00032 0.00031 0.00030 0.00017 Final Structure Factor Calculation for 04src0437r in P2(1)/c Total number of l.s. parameters = 708 Maximum vector length = 511 Memory required = 10064 / 25039 wR2 = 0.0689 before cycle 11 for 14858 data and 0 / 708 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 7.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0293 for 12455 Fo > 4sig(Fo) and 0.0401 for all 14858 data wR2 = 0.0689, GooF = S = 1.038, Restrained GooF = 1.038 for all data Occupancy sum of asymmetric unit = 75.00 for non-hydrogen and 106.00 for hydrogen atoms Principal mean square atomic displacements U 0.0150 0.0139 0.0096 C1 0.0209 0.0140 0.0118 C2 0.0275 0.0161 0.0107 C3 0.0264 0.0146 0.0114 C4 0.0208 0.0156 0.0106 C5 0.0151 0.0111 0.0101 C6 0.0203 0.0141 0.0114 C7 0.0257 0.0148 0.0105 C8 0.0277 0.0168 0.0105 C9 0.0222 0.0148 0.0100 C10 0.0400 0.0179 0.0107 C11 0.0430 0.0274 0.0146 C12 0.0460 0.0250 0.0111 C13 0.0338 0.0165 0.0134 C14 0.0311 0.0194 0.0134 C15 0.0445 0.0236 0.0121 C16 0.0500 0.0235 0.0112 C17 0.0337 0.0206 0.0111 C18 0.0220 0.0194 0.0119 C19 0.0336 0.0301 0.0124 C20 0.0358 0.0229 0.0125 C21 0.0188 0.0154 0.0122 C22 0.0351 0.0195 0.0141 C23 0.0242 0.0203 0.0123 C24 0.0197 0.0150 0.0122 C25 0.0315 0.0208 0.0104 C26 0.0260 0.0200 0.0115 C27 0.0201 0.0167 0.0106 C28 0.0344 0.0253 0.0140 C29 0.0280 0.0223 0.0130 C30 0.0132 0.0107 0.0100 P1 0.0123 0.0111 0.0109 P2 0.0277 0.0205 0.0097 Cl1 0.0407 0.0208 0.0109 Cl2 0.0126 0.0113 0.0090 Fe1 0.0138 0.0115 0.0086 Pd1 0.0140 0.0132 0.0084 C31 0.0191 0.0130 0.0110 C32 0.0247 0.0143 0.0086 C33 0.0222 0.0157 0.0099 C34 0.0175 0.0143 0.0091 C35 0.0144 0.0125 0.0098 C36 0.0172 0.0108 0.0095 C37 0.0233 0.0141 0.0090 C38 0.0282 0.0140 0.0097 C39 0.0206 0.0147 0.0106 C40 0.0241 0.0170 0.0146 C41 0.0358 0.0201 0.0112 C42 0.0362 0.0227 0.0116 C43 0.0268 0.0194 0.0132 C44 0.0232 0.0160 0.0144 C45 0.0324 0.0176 0.0115 C46 0.0395 0.0239 0.0128 C47 0.0271 0.0228 0.0129 C48 0.0215 0.0162 0.0113 C49 0.0446 0.0289 0.0125 C50 0.0299 0.0211 0.0142 C51 0.0217 0.0162 0.0112 C52 0.0396 0.0248 0.0130 C53 0.0423 0.0295 0.0119 C54 0.0229 0.0208 0.0099 C55 0.0380 0.0273 0.0104 C56 0.0449 0.0266 0.0100 C57 0.0176 0.0143 0.0122 C58 0.0361 0.0225 0.0131 C59 0.0280 0.0182 0.0132 C60 0.0125 0.0113 0.0094 P31 0.0134 0.0109 0.0099 P32 0.0730 0.0173 0.0108 Cl31 0.0574 0.0218 0.0093 Cl32 0.0126 0.0105 0.0094 Fe31 0.0142 0.0116 0.0084 Pd31 0.0393 0.0307 0.0203 C71 0.0520 0.0337 0.0278 Cl71 0.0443 0.0327 0.0294 Cl72 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.033 0.050 0.068 0.087 0.110 0.139 0.175 0.234 1.000 Number in group 1497. 1526. 1490. 1490. 1445. 1496. 1476. 1458. 1495. 1485. GooF 0.919 0.985 0.983 1.059 1.054 1.115 1.086 1.094 1.091 0.982 K 1.663 1.018 0.979 0.982 0.978 0.986 0.995 1.005 1.010 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 1504. 1466. 1498. 1482. 1473. 1489. 1483. 1480. 1493. 1490. GooF 1.027 0.983 1.027 1.001 0.927 0.958 0.918 0.994 0.940 1.486 K 0.979 1.001 1.006 1.017 1.013 1.013 1.006 1.003 0.999 0.989 R1 0.086 0.071 0.066 0.054 0.042 0.034 0.028 0.027 0.020 0.024 Recommended weighting scheme: WGHT 0.0243 7.4746 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -3 10 4 716.57 2136.92 8.56 0.086 1.09 -1 7 16 1042.88 2712.10 8.18 0.097 1.22 -3 0 2 5205.30 8543.90 7.92 0.172 6.01 1 2 35 3136.64 5712.01 7.69 0.140 0.85 16 6 16 959.31 2392.50 6.92 0.091 0.89 6 0 32 369.80 1547.45 6.88 0.073 0.90 -10 1 13 3346.87 5437.17 6.84 0.137 1.50 -2 5 25 8483.34 11507.15 6.27 0.199 1.06 -4 7 33 5830.07 9112.59 6.20 0.177 0.79 -1 4 34 3073.25 5428.97 6.17 0.137 0.85 -2 5 33 6404.37 9091.14 5.94 0.177 0.85 4 5 20 6874.84 9300.78 5.94 0.179 1.20 0 2 8 856.23 439.02 5.80 0.039 3.13 -8 10 25 5861.55 10695.58 5.75 0.192 0.78 0 0 12 458.05 923.67 5.57 0.056 2.52 2 0 4 3306.03 4874.85 5.39 0.130 5.89 -9 10 1 4405.33 6308.21 5.17 0.148 0.99 0 6 32 1460.50 2959.02 5.16 0.101 0.84 -7 9 21 2627.99 3970.88 5.03 0.117 0.89 0 0 6 2755.70 3983.16 4.98 0.117 5.04 -7 12 9 1876.62 3521.27 4.87 0.110 0.85 -3 9 8 690.54 1439.10 4.77 0.070 1.16 4 12 0 502.73 1502.79 4.60 0.072 0.91 -2 5 29 6723.54 9177.21 4.59 0.178 0.94 -1 0 36 20063.89 25961.51 4.52 0.299 0.84 0 7 14 1396.24 2370.07 4.48 0.090 1.28 -1 5 26 7827.79 10183.00 4.45 0.188 1.03 2 4 8 3136.94 2383.18 4.42 0.091 2.17 7 0 0 2097.88 2969.36 4.25 0.101 2.78 -1 1 15 6301.62 7603.95 4.15 0.162 1.98 -1 3 30 6931.36 10427.27 4.13 0.190 0.97 0 2 37 838.48 1739.29 4.10 0.077 0.81 -2 5 2 102.09 295.68 4.08 0.032 2.15 0 0 8 14619.91 17235.29 4.02 0.244 3.78 6 5 2 384.23 175.51 3.97 0.025 1.82 -7 10 2 375.16 845.98 3.96 0.054 1.03 -8 0 8 434.00 843.95 3.94 0.054 2.07 -7 10 4 294.21 934.52 3.90 0.057 1.02 5 2 12 6365.08 5333.92 3.83 0.136 1.96 -9 0 4 40.19 487.35 3.82 0.041 2.09 -3 4 2 7568.86 6414.53 3.81 0.149 2.52 -2 2 8 7468.69 6274.33 3.81 0.147 3.00 -3 3 9 3825.27 3077.59 3.80 0.103 2.34 -1 1 8 224.34 92.52 3.77 0.018 3.54 -5 8 31 4283.73 5607.31 3.77 0.139 0.79 3 3 0 10813.70 9337.49 3.73 0.180 3.22 -1 4 9 14620.86 12624.32 3.69 0.209 2.13 -2 0 16 25264.90 21972.03 3.65 0.275 1.87 -9 10 13 2539.04 3668.32 3.64 0.113 0.91 -4 9 23 2791.77 3958.87 3.63 0.117 0.89 Bond lengths and angles C1 - Distance Angles C5 1.4468 (0.0032) C2 1.4493 (0.0031) 107.50 (0.19) P1 1.8217 (0.0023) 119.57 (0.17) 132.70 (0.17) Fe1 2.0186 (0.0022) 69.73 (0.13) 69.99 (0.13) 129.47 (0.12) C1 - C5 C2 P1 C2 - Distance Angles C3 1.4322 (0.0032) C1 1.4493 (0.0031) 107.23 (0.20) C11 1.4966 (0.0033) 121.70 (0.21) 131.04 (0.21) Fe1 2.0428 (0.0023) 70.22 (0.13) 68.20 (0.12) 128.39 (0.18) C2 - C3 C1 C11 C3 - Distance Angles C4 1.4199 (0.0035) C2 1.4322 (0.0033) 108.81 (0.20) C12 1.4960 (0.0034) 125.83 (0.23) 125.25 (0.23) Fe1 2.0600 (0.0023) 69.30 (0.13) 68.92 (0.13) 130.65 (0.18) C3 - C4 C2 C12 C4 - Distance Angles C3 1.4199 (0.0035) C5 1.4230 (0.0033) 108.59 (0.21) C13 1.4983 (0.0033) 125.73 (0.23) 125.68 (0.23) Fe1 2.0475 (0.0023) 70.25 (0.14) 69.16 (0.13) 126.33 (0.18) C4 - C3 C5 C13 C5 - Distance Angles C4 1.4230 (0.0032) C1 1.4468 (0.0032) 107.86 (0.21) C14 1.4996 (0.0033) 124.01 (0.21) 127.97 (0.21) Fe1 2.0357 (0.0023) 70.05 (0.13) 68.46 (0.13) 130.53 (0.18) C5 - C4 C1 C14 C6 - Distance Angles C10 1.4505 (0.0031) C7 1.4512 (0.0031) 107.13 (0.19) P2 1.8217 (0.0023) 118.72 (0.17) 133.92 (0.17) Fe1 2.0196 (0.0022) 69.28 (0.13) 69.68 (0.13) 129.93 (0.12) C6 - C10 C7 P2 C7 - Distance Angles C8 1.4337 (0.0032) C6 1.4512 (0.0031) 107.31 (0.20) C15 1.4911 (0.0033) 121.86 (0.21) 130.82 (0.21) Fe1 2.0369 (0.0023) 70.02 (0.13) 68.40 (0.13) 127.43 (0.17) C7 - C8 C6 C15 C8 - Distance Angles C9 1.4166 (0.0035) C7 1.4337 (0.0032) 108.75 (0.21) C16 1.4985 (0.0033) 125.31 (0.22) 125.90 (0.23) Fe1 2.0516 (0.0023) 70.43 (0.14) 68.92 (0.13) 128.63 (0.18) C8 - C9 C7 C16 C9 - Distance Angles C8 1.4166 (0.0035) C10 1.4186 (0.0033) 108.78 (0.20) C17 1.4966 (0.0033) 125.77 (0.23) 125.33 (0.23) Fe1 2.0661 (0.0023) 69.33 (0.13) 68.26 (0.13) 131.41 (0.18) C9 - C8 C10 C17 C10 - Distance Angles C9 1.4186 (0.0033) C6 1.4505 (0.0031) 108.01 (0.21) C18 1.4972 (0.0033) 124.01 (0.21) 127.84 (0.21) Fe1 2.0273 (0.0023) 71.20 (0.14) 68.72 (0.13) 129.00 (0.18) C10 - C9 C6 C18 C11 - Distance Angles C2 1.4966 (0.0033) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C2 H11A H11B C12 - Distance Angles C3 1.4960 (0.0034) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C3 H12A H12B C13 - Distance Angles C4 1.4983 (0.0034) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C4 H13A H13B C14 - Distance Angles C5 1.4996 (0.0033) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C5 H14A H14B C15 - Distance Angles C7 1.4911 (0.0033) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C7 H15A H15B C16 - Distance Angles C8 1.4985 (0.0033) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C8 H16A H16B C17 - Distance Angles C9 1.4966 (0.0033) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C9 H17A H17B C18 - Distance Angles C10 1.4972 (0.0033) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C10 H18A H18B C19 - Distance Angles C21 1.5233 (0.0033) C20 1.5338 (0.0035) 110.84 (0.21) P1 1.8701 (0.0024) 114.28 (0.17) 113.34 (0.17) H19 1.0000 105.86 105.86 105.86 C19 - C21 C20 P1 C20 - Distance Angles C19 1.5338 (0.0035) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C19 H20A H20B C21 - Distance Angles C19 1.5233 (0.0033) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C19 H21A H21B C22 - Distance Angles C23 1.5311 (0.0033) C24 1.5321 (0.0032) 108.58 (0.19) P1 1.8440 (0.0023) 111.03 (0.16) 117.40 (0.17) H22 1.0000 106.39 106.39 106.39 C22 - C23 C24 P1 C23 - Distance Angles C22 1.5311 (0.0032) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C24 - Distance Angles C22 1.5321 (0.0032) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B C25 - Distance Angles C26 1.5323 (0.0031) C27 1.5366 (0.0032) 110.77 (0.20) P2 1.8653 (0.0023) 114.85 (0.16) 113.50 (0.16) H25 1.0000 105.60 105.60 105.60 C25 - C26 C27 P2 C26 - Distance Angles C25 1.5323 (0.0031) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5366 (0.0032) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C25 H27A H27B C28 - Distance Angles C30 1.5324 (0.0033) C29 1.5427 (0.0033) 109.47 (0.20) P2 1.8454 (0.0023) 115.26 (0.16) 112.55 (0.17) H28 1.0000 106.31 106.31 106.31 C28 - C30 C29 P2 C29 - Distance Angles C28 1.5427 (0.0033) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C28 H29A H29B C30 - Distance Angles C28 1.5324 (0.0033) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C28 H30A H30B P1 - Distance Angles C1 1.8217 (0.0023) C22 1.8440 (0.0023) 110.52 (0.11) C19 1.8701 (0.0024) 100.29 (0.11) 107.45 (0.11) Pd1 2.3306 (0.0006) 110.62 (0.07) 113.36 (0.08) 113.81 (0.08) P1 - C1 C22 C19 P2 - Distance Angles C6 1.8217 (0.0023) C28 1.8454 (0.0023) 109.26 (0.11) C25 1.8653 (0.0023) 100.98 (0.10) 106.14 (0.11) Pd1 2.3242 (0.0006) 111.90 (0.07) 114.70 (0.08) 112.86 (0.08) P2 - C6 C28 C25 Cl1 - Distance Angles Pd1 2.3496 (0.0006) Cl1 - Cl2 - Distance Angles Pd1 2.3507 (0.0006) Cl2 - Fe1 - Distance Angles C1 2.0186 (0.0022) C6 2.0196 (0.0022) 107.03 (0.09) C10 2.0273 (0.0023) 124.00 (0.09) 42.01 (0.09) C5 2.0357 (0.0023) 41.81 (0.09) 121.89 (0.09) 106.48 (0.10) C7 2.0369 (0.0023) 122.05 (0.09) 41.92 (0.09) 70.11 (0.10) 159.15 (0.09) C2 2.0428 (0.0023) 41.81 (0.09) 124.11 (0.09) 162.17 (0.09) 69.87 (0.10) 106.77 (0.10) C4 2.0475 (0.0024) 69.56 (0.09) 157.42 (0.10) 120.22 (0.10) 40.79 (0.09) 158.82 (0.09) 69.08 (0.10) C8 2.0516 (0.0023) 158.09 (0.10) 69.60 (0.09) 68.82 (0.10) 158.40 (0.10) 41.05 (0.09) 121.03 (0.10) 121.98 (0.09) C3 2.0600 (0.0024) 69.32 (0.09) 160.98 (0.10) 155.48 (0.10) 68.61 (0.10) 123.06 (0.10) 40.86 (0.09) 40.45 (0.10) C9 2.0661 (0.0023) 160.50 (0.10) 69.23 (0.09) 40.54 (0.09) 122.73 (0.10) 68.75 (0.10) 156.06 (0.09) 106.16 (0.10) Fe1 - C1 C6 C10 C5 C7 C2 C4 Pd1 - Distance Angles P2 2.3242 (0.0006) P1 2.3306 (0.0006) 96.62 (0.02) Cl1 2.3496 (0.0006) 173.12 (0.02) 90.09 (0.02) Cl2 2.3507 (0.0006) 89.64 (0.02) 172.47 (0.02) 83.56 (0.02) Pd1 - P2 P1 Cl1 C31 - Distance Angles C35 1.4427 (0.0031) C32 1.4502 (0.0031) 108.02 (0.19) P31 1.8145 (0.0023) 118.23 (0.17) 133.52 (0.17) Fe31 2.0199 (0.0022) 69.76 (0.12) 69.73 (0.12) 129.87 (0.12) C31 - C35 C32 P31 C32 - Distance Angles C33 1.4347 (0.0032) C31 1.4502 (0.0031) 106.64 (0.20) C41 1.4942 (0.0033) 121.67 (0.21) 131.69 (0.21) Fe31 2.0381 (0.0023) 70.57 (0.13) 68.39 (0.12) 125.42 (0.16) C32 - C33 C31 C41 C33 - Distance Angles C34 1.4245 (0.0034) C32 1.4347 (0.0032) 109.20 (0.20) C42 1.4924 (0.0033) 125.70 (0.22) 124.99 (0.22) Fe31 2.0657 (0.0022) 69.97 (0.13) 68.51 (0.13) 130.75 (0.17) C33 - C34 C32 C42 C34 - Distance Angles C35 1.4243 (0.0033) C33 1.4245 (0.0034) 108.18 (0.20) C43 1.5009 (0.0033) 125.29 (0.22) 126.45 (0.22) Fe31 2.0688 (0.0022) 68.46 (0.13) 69.73 (0.13) 130.00 (0.17) C34 - C35 C33 C43 C35 - Distance Angles C34 1.4243 (0.0033) C31 1.4427 (0.0031) 107.96 (0.20) C44 1.4931 (0.0032) 124.16 (0.21) 127.74 (0.21) Fe31 2.0359 (0.0022) 70.94 (0.13) 68.57 (0.12) 129.44 (0.17) C35 - C34 C31 C44 C36 - Distance Angles C37 1.4442 (0.0031) C40 1.4528 (0.0032) 107.61 (0.19) P32 1.8189 (0.0023) 133.62 (0.17) 118.45 (0.17) Fe31 2.0165 (0.0022) 70.27 (0.12) 69.45 (0.12) 130.16 (0.12) C36 - C37 C40 P32 C37 - Distance Angles C38 1.4311 (0.0032) C36 1.4442 (0.0031) 107.39 (0.20) C45 1.4979 (0.0032) 122.28 (0.20) 130.28 (0.20) Fe31 2.0458 (0.0022) 70.32 (0.13) 68.09 (0.12) 128.89 (0.16) C37 - C38 C36 C45 C38 - Distance Angles C39 1.4180 (0.0034) C37 1.4311 (0.0032) 108.88 (0.20) C46 1.4972 (0.0033) 124.73 (0.22) 126.37 (0.22) Fe31 2.0644 (0.0022) 69.88 (0.13) 68.93 (0.12) 128.44 (0.16) C38 - C39 C37 C46 C39 - Distance Angles C38 1.4180 (0.0034) C40 1.4272 (0.0033) 108.67 (0.21) C47 1.5004 (0.0033) 125.24 (0.23) 126.04 (0.23) Fe31 2.0637 (0.0023) 69.94 (0.13) 68.32 (0.13) 129.81 (0.17) C39 - C38 C40 C47 C40 - Distance Angles C39 1.4272 (0.0033) C36 1.4528 (0.0031) 107.45 (0.20) C48 1.4975 (0.0033) 124.40 (0.21) 127.98 (0.21) Fe31 2.0298 (0.0023) 70.88 (0.13) 68.47 (0.12) 129.57 (0.17) C40 - C39 C36 C48 C41 - Distance Angles C32 1.4942 (0.0033) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C32 H41A H41B C42 - Distance Angles C33 1.4924 (0.0033) H42A 0.9800 109.47 H42B 0.9800 109.47 109.47 H42C 0.9800 109.47 109.47 109.47 C42 - C33 H42A H42B C43 - Distance Angles C34 1.5009 (0.0033) H43A 0.9800 109.47 H43B 0.9800 109.47 109.47 H43C 0.9800 109.47 109.47 109.47 C43 - C34 H43A H43B C44 - Distance Angles C35 1.4931 (0.0032) H44A 0.9800 109.47 H44B 0.9800 109.47 109.47 H44C 0.9800 109.47 109.47 109.47 C44 - C35 H44A H44B C45 - Distance Angles C37 1.4979 (0.0032) H45A 0.9800 109.47 H45B 0.9800 109.47 109.47 H45C 0.9800 109.47 109.47 109.47 C45 - C37 H45A H45B C46 - Distance Angles C38 1.4972 (0.0032) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C38 H46A H46B C47 - Distance Angles C39 1.5004 (0.0033) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C39 H47A H47B C48 - Distance Angles C40 1.4975 (0.0033) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C40 H48A H48B C49 - Distance Angles C51 1.5319 (0.0033) C50 1.5368 (0.0033) 110.13 (0.20) P31 1.8378 (0.0024) 116.31 (0.17) 111.48 (0.17) H49 1.0000 106.06 106.06 106.06 C49 - C51 C50 P31 C50 - Distance Angles C49 1.5368 (0.0033) H50A 0.9800 109.47 H50B 0.9800 109.47 109.47 H50C 0.9800 109.47 109.47 109.47 C50 - C49 H50A H50B C51 - Distance Angles C49 1.5319 (0.0033) H51A 0.9800 109.47 H51B 0.9800 109.47 109.47 H51C 0.9800 109.47 109.47 109.47 C51 - C49 H51A H51B C52 - Distance Angles C53 1.5282 (0.0033) C54 1.5369 (0.0034) 109.62 (0.21) P31 1.8715 (0.0023) 115.21 (0.17) 113.52 (0.18) H52 1.0000 105.90 105.90 105.90 C52 - C53 C54 P31 C53 - Distance Angles C52 1.5282 (0.0033) H53A 0.9800 109.47 H53B 0.9800 109.47 109.47 H53C 0.9800 109.47 109.47 109.47 C53 - C52 H53A H53B C54 - Distance Angles C52 1.5369 (0.0034) H54A 0.9800 109.47 H54B 0.9800 109.47 109.47 H54C 0.9800 109.47 109.47 109.47 C54 - C52 H54A H54B C55 - Distance Angles C56 1.5280 (0.0033) C57 1.5295 (0.0034) 108.73 (0.20) P32 1.8764 (0.0023) 115.82 (0.18) 113.46 (0.17) H55 1.0000 106.02 106.02 106.02 C55 - C56 C57 P32 C56 - Distance Angles C55 1.5280 (0.0033) H56A 0.9800 109.47 H56B 0.9800 109.47 109.47 H56C 0.9800 109.47 109.47 109.47 C56 - C55 H56A H56B C57 - Distance Angles C55 1.5295 (0.0034) H57A 0.9800 109.47 H57B 0.9800 109.47 109.47 H57C 0.9800 109.47 109.47 109.47 C57 - C55 H57A H57B C58 - Distance Angles C60 1.5260 (0.0031) C59 1.5409 (0.0033) 108.89 (0.20) P32 1.8507 (0.0023) 117.80 (0.17) 109.83 (0.16) H58 1.0000 106.57 106.57 106.57 C58 - C60 C59 P32 C59 - Distance Angles C58 1.5409 (0.0033) H59A 0.9800 109.47 H59B 0.9800 109.47 109.47 H59C 0.9800 109.47 109.47 109.47 C59 - C58 H59A H59B C60 - Distance Angles C58 1.5260 (0.0031) H60A 0.9800 109.47 H60B 0.9800 109.47 109.47 H60C 0.9800 109.47 109.47 109.47 C60 - C58 H60A H60B P31 - Distance Angles C31 1.8145 (0.0023) C49 1.8378 (0.0024) 107.74 (0.11) C52 1.8715 (0.0023) 101.65 (0.10) 107.79 (0.11) Pd31 2.3293 (0.0006) 113.39 (0.07) 112.63 (0.08) 112.91 (0.08) P31 - C31 C49 C52 P32 - Distance Angles C36 1.8189 (0.0023) C58 1.8507 (0.0023) 112.63 (0.10) C55 1.8764 (0.0023) 99.09 (0.10) 106.73 (0.11) Pd31 2.3190 (0.0006) 113.38 (0.07) 109.07 (0.08) 115.57 (0.08) P32 - C36 C58 C55 Cl31 - Distance Angles Pd31 2.3311 (0.0007) Cl31 - Cl32 - Distance Angles Pd31 2.3448 (0.0006) Cl32 - Fe31 - Distance Angles C36 2.0165 (0.0022) C31 2.0199 (0.0022) 106.60 (0.09) C40 2.0298 (0.0023) 42.08 (0.09) 122.69 (0.09) C35 2.0359 (0.0022) 122.27 (0.09) 41.67 (0.09) 106.11 (0.09) C32 2.0381 (0.0023) 122.59 (0.09) 41.87 (0.09) 160.34 (0.09) 70.13 (0.09) C37 2.0458 (0.0022) 41.64 (0.09) 122.62 (0.09) 70.01 (0.09) 159.69 (0.09) 106.49 (0.09) C39 2.0637 (0.0023) 69.36 (0.09) 159.29 (0.10) 40.80 (0.09) 122.12 (0.10) 157.42 (0.10) 68.66 (0.09) C38 2.0644 (0.0022) 69.19 (0.09) 159.09 (0.09) 68.74 (0.09) 157.93 (0.10) 121.94 (0.09) 40.75 (0.09) 40.18 (0.10) C33 2.0657 (0.0023) 159.66 (0.09) 68.97 (0.09) 157.08 (0.10) 68.46 (0.09) 40.92 (0.09) 122.81 (0.09) 121.84 (0.09) C34 2.0688 (0.0023) 158.46 (0.09) 69.09 (0.09) 121.24 (0.09) 40.60 (0.09) 69.15 (0.09) 158.42 (0.09) 106.82 (0.09) Fe31 - C36 C31 C40 C35 C32 C37 C39 Pd31 - Distance Angles P32 2.3190 (0.0006) P31 2.3293 (0.0006) 96.66 (0.02) Cl31 2.3311 (0.0007) 173.26 (0.02) 89.87 (0.02) Cl32 2.3448 (0.0006) 89.33 (0.02) 173.90 (0.02) 84.18 (0.02) Pd31 - P32 P31 Cl31 C71 - Distance Angles Cl72 1.7425 (0.0029) Cl71 1.7729 (0.0029) 111.47 (0.15) H71A 0.9900 109.33 109.33 H71B 0.9900 109.33 109.33 107.97 C71 - Cl72 Cl71 H71A Cl71 - Distance Angles C71 1.7729 (0.0030) Cl71 - Cl72 - Distance Angles C71 1.7425 (0.0029) Cl72 - FMAP and GRID set by program FMAP 2 3 65 GRID -0.806 -1 -2 0.806 1 2 R1 = 0.0393 for 14858 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.52 at 0.3898 0.1805 0.0071 [ 0.79 A from CL31 ] Deepest hole -0.70 at 0.3424 0.1777 0.0382 [ 0.81 A from PD31 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 9302 / 84110 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3898 0.3195 0.5071 1.00000 0.05 0.52 0.79 CL31 2.04 PD31 2.56 H52 2.59 H44B Q2 1 0.4249 0.1156 0.7717 1.00000 0.05 0.50 0.96 CL72 1.39 C71 1.50 H71A 2.11 H71B Q3 1 0.2811 0.4438 0.5788 1.00000 0.05 0.47 0.99 P32 1.39 PD31 2.22 C36 2.37 C58 Q4 1 0.4178 0.5015 0.6113 1.00000 0.05 0.46 0.82 C31 0.99 P31 1.99 C35 2.09 C32 Q5 1 0.1737 0.2078 0.8226 1.00000 0.05 0.46 1.01 P2 1.35 PD1 2.30 C25 2.45 C28 Q6 1 0.3830 0.3437 0.5734 1.00000 0.05 0.45 1.33 PD31 1.34 P31 2.09 CL31 2.27 C52 Q7 1 0.3928 0.2777 0.6533 1.00000 0.05 0.45 0.74 C49 0.81 C50 1.41 H50A 1.45 H50B Q8 1 0.2395 0.3586 0.8378 1.00000 0.05 0.45 0.97 P1 1.43 PD1 2.18 C22 2.35 H23B Q9 1 0.2575 0.7638 0.6297 1.00000 0.05 0.45 0.73 C37 0.76 C38 1.73 C36 1.74 C39 Q10 1 0.4412 0.7031 0.6472 1.00000 0.05 0.43 0.73 C32 0.75 C33 1.77 C31 1.79 C34 Shortest distances between peaks (including symmetry equivalents) 1 6 2.03 5 8 2.15 4 6 2.19 3 6 2.28 4 10 2.53 6 7 2.53 4 7 2.84 3 4 2.88 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 3.92: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.00: Generate idealized H-atoms 62.02: Structure factors and derivatives 172.56: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 13.69: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.44: Analysis of variance 0.20: Merge reflections for Fourier and .fcf 0.61: Fourier summations 0.42: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0437r finished at 11:49:21 Total CPU time: 254.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++