+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 10:32:21 on 08-Jun-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in P2(1)/c CELL 0.71073 23.0236 12.4019 15.5740 90.000 109.102 90.000 ZERR 4.00 0.0022 0.0006 0.0010 0.000 0.007 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P CL FE PD O UNIT 152 304 8 8 4 4 24 V = 4202.08 F(000) = 1952.0 Mu = 1.02 mm-1 Cell Wt = 3696.31 Rho = 1.461 MERG 2 OMIT -3.00 55.00 OMIT -1 1 2 OMIT 4 0 0 SHEL 7 0.77 DFIX 0.84 0.02 O51 H51A O51 H51B O52 H52A O52 H52B O53 H53A O53 H53B DFIX 0.84 0.02 O54 H54A O54 H54B O55 H55A O55 H55B DFIX 0.84 0.005 O56 H56A O56 H56B DANG 1.35 0.02 H51A H51B H52A H52B H53A H53B H54A H54B H55A H55B DANG 1.35 0.005 H56A H56B EQIV $1 -X+1, Y+1/2, -Z-1/2 EQIV $2 X, -Y-1/2, Z+1/2 EQIV $3 -X+1, Y-1/2, -Z-1/2 EQIV $4 X, -Y+1/2, Z+1/2 EQIV $5 X, Y+1, Z EQIV $6 -X+2, -Y+1, -Z HTAB O51 CL11_$1 HTAB O51 O54_$1 HTAB O52 CL11_$2 HTAB O52 O51_$4 HTAB O53 CL11 HTAB O53 O52 HTAB O54 O55_$3 HTAB O54 CL11_$1 HTAB O55 O54_$4 HTAB O55 O53_$5 HTAB O56 CL1 HTAB O56 CL1_$6 FMAP 2 PLAN 5 SIZE 0.02 0.18 0.24 ACTA BOND $H WGHT 0.03230 6.38760 L.S. 10 TEMP -153.00 FVAR 0.23199 MOLE 1 C1 1 0.864674 0.023522 0.084048 11.00000 0.01063 0.01175 = 0.01354 -0.00043 0.00380 -0.00078 C2 1 0.845080 0.011586 -0.014468 11.00000 0.01066 0.01472 = 0.01373 -0.00120 0.00378 -0.00064 C3 1 0.842839 -0.100501 -0.034558 11.00000 0.01307 0.01520 = 0.01859 -0.00558 0.00399 -0.00022 C4 1 0.858451 -0.159029 0.047987 11.00000 0.01435 0.01133 = 0.02414 -0.00213 0.00136 0.00188 C5 1 0.871467 -0.084043 0.121970 11.00000 0.01138 0.00979 = 0.01770 0.00026 0.00068 -0.00044 C6 1 0.696867 0.009750 0.001276 11.00000 0.01155 0.01181 = 0.01339 0.00176 0.00440 -0.00068 C7 1 0.695792 -0.081618 -0.057490 11.00000 0.01003 0.01349 = 0.01614 -0.00036 0.00072 -0.00141 C8 1 0.710918 -0.175485 -0.002336 11.00000 0.01285 0.01197 = 0.02348 0.00153 0.00166 -0.00374 C9 1 0.723401 -0.144980 0.089879 11.00000 0.01394 0.01740 = 0.02109 0.00651 0.00236 -0.00349 C10 1 0.715155 -0.031875 0.094316 11.00000 0.01185 0.01913 = 0.01389 0.00122 0.00369 -0.00427 C11 1 0.833444 0.097022 -0.086180 11.00000 0.01759 0.01886 = 0.01199 -0.00007 0.00508 -0.00002 AFIX 137 H11A 2 0.862531 0.088456 -0.119669 11.00000 -1.50000 H11B 2 0.838846 0.168323 -0.057511 11.00000 -1.50000 H11C 2 0.791345 0.090156 -0.128255 11.00000 -1.50000 AFIX 0 C12 1 0.830312 -0.149491 -0.126589 11.00000 0.02163 0.02425 = 0.02365 -0.01297 0.00589 -0.00178 AFIX 137 H12A 2 0.869257 -0.169898 -0.134874 11.00000 -1.50000 H12B 2 0.808923 -0.096989 -0.173253 11.00000 -1.50000 H12C 2 0.804547 -0.213693 -0.131955 11.00000 -1.50000 AFIX 0 C13 1 0.863781 -0.279088 0.056187 11.00000 0.02536 0.01163 = 0.04217 -0.00515 -0.00050 0.00165 AFIX 137 H13A 2 0.836140 -0.312430 0.000818 11.00000 -1.50000 H13B 2 0.852471 -0.302823 0.108618 11.00000 -1.50000 H13C 2 0.906223 -0.300658 0.064495 11.00000 -1.50000 AFIX 0 C14 1 0.891556 -0.118747 0.219344 11.00000 0.01958 0.01505 = 0.01937 0.00493 -0.00089 -0.00092 AFIX 137 H14A 2 0.879257 -0.193791 0.223049 11.00000 -1.50000 H14B 2 0.872211 -0.072476 0.253249 11.00000 -1.50000 H14C 2 0.936354 -0.112697 0.245496 11.00000 -1.50000 AFIX 0 C15 1 0.680446 -0.085490 -0.158358 11.00000 0.01875 0.02116 = 0.01533 -0.00335 0.00082 0.00265 AFIX 137 H15A 2 0.698224 -0.150641 -0.175274 11.00000 -1.50000 H15B 2 0.697347 -0.021670 -0.178806 11.00000 -1.50000 H15C 2 0.635698 -0.086698 -0.187164 11.00000 -1.50000 AFIX 0 C16 1 0.708174 -0.288152 -0.036308 11.00000 0.02226 0.01247 = 0.03404 -0.00231 -0.00024 -0.00220 AFIX 137 H16A 2 0.734327 -0.334427 0.011939 11.00000 -1.50000 H16B 2 0.722718 -0.290092 -0.088806 11.00000 -1.50000 H16C 2 0.665669 -0.314134 -0.054428 11.00000 -1.50000 AFIX 0 C17 1 0.738872 -0.219676 0.169471 11.00000 0.02504 0.02410 = 0.02841 0.01250 0.00427 -0.00312 AFIX 137 H17A 2 0.701652 -0.235406 0.184623 11.00000 -1.50000 H17B 2 0.769463 -0.185686 0.221698 11.00000 -1.50000 H17C 2 0.755647 -0.286927 0.154295 11.00000 -1.50000 AFIX 0 C18 1 0.716851 0.021362 0.181315 11.00000 0.01747 0.02611 = 0.01349 0.00157 0.00591 -0.00517 AFIX 137 H18A 2 0.676551 0.014573 0.189407 11.00000 -1.50000 H18B 2 0.727002 0.097850 0.179256 11.00000 -1.50000 H18C 2 0.748109 -0.013468 0.232264 11.00000 -1.50000 AFIX 0 C19 1 0.977947 0.138867 0.124595 11.00000 0.01254 0.01989 = 0.01474 -0.00049 0.00471 -0.00062 AFIX 13 H19 2 1.002029 0.201819 0.158113 11.00000 -1.20000 AFIX 0 C20 1 0.975948 0.149591 0.026009 11.00000 0.01843 0.03149 = 0.01706 0.00005 0.00960 -0.00108 AFIX 137 H20A 2 1.017771 0.159295 0.024183 11.00000 -1.50000 H20B 2 0.950816 0.212135 -0.001852 11.00000 -1.50000 H20C 2 0.957974 0.084228 -0.007585 11.00000 -1.50000 AFIX 0 C21 1 1.013506 0.037670 0.167689 11.00000 0.01643 0.02805 = 0.02565 0.00521 0.00947 0.00553 AFIX 137 H21A 2 0.990438 -0.026477 0.138868 11.00000 -1.50000 H21B 2 1.019094 0.036826 0.232828 11.00000 -1.50000 H21C 2 1.053784 0.037778 0.159001 11.00000 -1.50000 AFIX 0 C22 1 0.921004 0.135620 0.262528 11.00000 0.01571 0.01682 = 0.01188 -0.00155 0.00391 -0.00178 AFIX 13 H22 2 0.941897 0.064663 0.281484 11.00000 -1.20000 AFIX 0 C23 1 0.865507 0.140327 0.295299 11.00000 0.02000 0.02931 = 0.01653 -0.00044 0.00750 -0.00072 AFIX 137 H23A 2 0.878251 0.121739 0.359975 11.00000 -1.50000 H23B 2 0.834315 0.088937 0.260555 11.00000 -1.50000 H23C 2 0.848275 0.213333 0.286436 11.00000 -1.50000 AFIX 0 C24 1 0.966165 0.224789 0.309082 11.00000 0.02804 0.03464 = 0.01589 -0.01001 0.00511 -0.01261 AFIX 137 H24A 2 0.947372 0.295273 0.289034 11.00000 -1.50000 H24B 2 1.003713 0.217661 0.292951 11.00000 -1.50000 H24C 2 0.976366 0.218604 0.375110 11.00000 -1.50000 AFIX 0 C25 1 0.613789 0.156327 -0.149815 11.00000 0.01467 0.01904 = 0.01511 0.00167 0.00195 0.00011 AFIX 13 H25 2 0.593457 0.227620 -0.150002 11.00000 -1.20000 AFIX 0 C26 1 0.645327 0.170243 -0.222076 11.00000 0.02729 0.02221 = 0.01433 0.00127 0.00527 0.00004 AFIX 137 H26A 2 0.648117 0.100118 -0.249468 11.00000 -1.50000 H26B 2 0.686724 0.199542 -0.193616 11.00000 -1.50000 H26C 2 0.621266 0.219950 -0.269257 11.00000 -1.50000 AFIX 0 C27 1 0.559604 0.076920 -0.178897 11.00000 0.02069 0.02785 = 0.02439 0.00094 0.00147 -0.00453 AFIX 137 H27A 2 0.545716 0.068369 -0.245087 11.00000 -1.50000 H27B 2 0.525766 0.104878 -0.160204 11.00000 -1.50000 H27C 2 0.572776 0.006874 -0.149947 11.00000 -1.50000 AFIX 0 C28 1 0.612670 0.164012 0.037120 11.00000 0.01484 0.02020 = 0.01986 -0.00124 0.00881 -0.00202 AFIX 13 H28 2 0.640289 0.172845 0.101323 11.00000 -1.20000 AFIX 0 C29 1 0.570797 0.067225 0.036565 11.00000 0.01917 0.02696 = 0.03008 0.00310 0.01289 -0.00394 AFIX 137 H29A 2 0.553759 0.074763 0.086263 11.00000 -1.50000 H29B 2 0.594754 0.000454 0.044632 11.00000 -1.50000 H29C 2 0.537194 0.064779 -0.021552 11.00000 -1.50000 AFIX 0 C30 1 0.574554 0.267884 0.012353 11.00000 0.02060 0.02334 = 0.03411 -0.00090 0.01546 0.00382 AFIX 137 H30A 2 0.546285 0.262663 -0.050138 11.00000 -1.50000 H30B 2 0.602082 0.329567 0.017417 11.00000 -1.50000 H30C 2 0.550963 0.277730 0.053970 11.00000 -1.50000 AFIX 0 C31 1 0.723836 0.243967 -0.014108 11.00000 0.01262 0.01205 = 0.01378 -0.00022 0.00509 -0.00056 AFIX 13 H31 2 0.749782 0.218334 -0.050468 11.00000 -1.20000 AFIX 0 C32 1 0.767637 0.249404 0.084403 11.00000 0.01155 0.01294 = 0.01342 0.00042 0.00393 -0.00156 AFIX 13 H32 2 0.773644 0.174692 0.109954 11.00000 -1.20000 AFIX 0 C33 1 0.745329 0.321298 0.147262 11.00000 0.01755 0.01798 = 0.01656 -0.00254 0.00750 -0.00041 AFIX 23 H33A 2 0.766869 0.299437 0.210903 11.00000 -1.20000 H33B 2 0.700891 0.308160 0.134585 11.00000 -1.20000 AFIX 0 C34 1 0.755256 0.442984 0.138436 11.00000 0.02580 0.01649 = 0.02059 -0.00472 0.00905 0.00243 AFIX 23 H34A 2 0.716375 0.475774 0.099404 11.00000 -1.20000 H34B 2 0.765977 0.476719 0.199254 11.00000 -1.20000 AFIX 0 C35 1 0.805388 0.466781 0.098530 11.00000 0.02155 0.00703 = 0.02531 -0.00180 0.00454 0.00072 AFIX 43 H35 2 0.843279 0.491920 0.139631 11.00000 -1.20000 AFIX 0 C36 1 0.802377 0.456234 0.010097 11.00000 0.01839 0.00849 = 0.02560 0.00244 0.00632 0.00111 AFIX 43 H36 2 0.839395 0.470986 -0.002139 11.00000 -1.20000 AFIX 0 C37 1 0.748473 0.424449 -0.070686 11.00000 0.02079 0.01285 = 0.01772 0.00281 0.00581 0.00069 AFIX 23 H37A 2 0.764649 0.386239 -0.113893 11.00000 -1.20000 H37B 2 0.728750 0.491487 -0.101009 11.00000 -1.20000 AFIX 0 C38 1 0.698443 0.354035 -0.055399 11.00000 0.01795 0.01210 = 0.01762 0.00239 0.00348 0.00007 AFIX 23 H38A 2 0.665373 0.342554 -0.114095 11.00000 -1.20000 H38B 2 0.680382 0.391743 -0.014111 11.00000 -1.20000 AFIX 0 P1 3 0.900793 0.147204 0.137742 11.00000 0.01063 0.01002 = 0.01035 -0.00138 0.00308 -0.00141 P2 3 0.662955 0.140652 -0.031535 11.00000 0.01054 0.01120 = 0.01310 -0.00009 0.00354 -0.00043 CL1 4 0.947448 0.404458 0.104455 11.00000 0.01864 0.02110 = 0.03129 0.00140 0.00584 -0.00873 FE1 5 0.782437 -0.062295 0.035333 11.00000 0.01115 0.00862 = 0.01209 0.00016 0.00121 -0.00098 PD1 6 0.852376 0.310353 0.089815 11.00000 0.01244 0.00865 = 0.01486 -0.00054 0.00379 -0.00218 MOLE 2 CL11 4 0.538259 -0.224485 -0.146316 11.00000 0.03528 0.02810 = 0.03578 0.00295 0.01725 0.00159 MOLE 3 O51 7 0.569384 0.420469 -0.227120 11.00000 0.02897 0.03461 = 0.03845 0.00170 0.00393 0.00989 H51A 2 0.538325 0.387070 -0.262703 11.00000 -1.50000 H51B 2 0.554982 0.449091 -0.189457 11.00000 -1.50000 MOLE 4 O52 7 0.601896 -0.133702 0.231606 11.00000 0.03948 0.04310 = 0.04802 0.00723 0.02560 0.00188 H52A 2 0.586751 -0.178986 0.258827 11.00000 -1.50000 H52B 2 0.592514 -0.072072 0.245546 11.00000 -1.50000 MOLE 5 O53 7 0.588549 -0.251164 0.074350 11.00000 0.05027 0.05185 = 0.03740 0.00043 0.00639 -0.01435 H53A 2 0.575611 -0.219845 0.023855 11.00000 -1.50000 H53B 2 0.584598 -0.207446 0.113026 11.00000 -1.50000 MOLE 6 O54 7 0.467480 0.031129 -0.404011 11.00000 0.06340 0.02847 = 0.02474 -0.00208 0.01061 0.00277 H54A 2 0.444447 0.025120 -0.458347 11.00000 -1.50000 H54B 2 0.463030 0.096683 -0.390985 11.00000 -1.50000 MOLE 7 O55 7 0.588281 0.528874 0.092829 11.00000 0.05713 0.03650 = 0.03374 0.00781 0.00317 -0.00136 H55A 2 0.556223 0.526858 0.108667 11.00000 -1.50000 H55B 2 0.594903 0.594728 0.090159 11.00000 -1.50000 MOLE 8 O56 7 1.071595 0.423804 0.057835 11.00000 0.08071 0.14168 = 0.08524 0.01944 0.04529 0.01139 H56A 2 1.038273 0.413978 0.068751 11.00000 -1.50000 H56B 2 1.061366 0.452413 0.005486 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for s93 in P2(1)/c C 0.770 H 0.320 P 1.100 CL 0.990 FE 1.240 PD 1.380 O 0.660 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 - C7 C10 P2 Fe1 C7 - C8 C6 C15 Fe1 C8 - C9 C7 C16 Fe1 C9 - C10 C8 C17 Fe1 C10 - C9 C6 C18 Fe1 C11 - C2 C12 - C3 C13 - C4 C14 - C5 C15 - C7 C16 - C8 C17 - C9 C18 - C10 C19 - C20 C21 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 C31 - C32 C38 P2 C32 - C33 C31 Pd1 C33 - C32 C34 C34 - C35 C33 C35 - C36 C34 Pd1 C36 - C35 C37 Pd1 C37 - C36 C38 C38 - C37 C31 P1 - C1 C22 C19 Pd1 P2 - C6 C25 C28 C31 Cl1 - Pd1 Fe1 - C7 C2 C6 C5 C4 C10 C3 C1 C9 C8 Pd1 - C32 C35 C36 P1 Cl1 Cl11 - no bonds found O51 - no bonds found O52 - no bonds found O53 - no bonds found O54 - no bonds found O55 - no bonds found O56 - no bonds found Operators for generating equivalent atoms: $1 -x+1, y+1/2, -z-1/2 $2 x, -y-1/2, z+1/2 $3 -x+1, y-1/2, -z-1/2 $4 x, -y+1/2, z+1/2 $5 x, y+1, z $6 -x+2, -y+1, -z 43879 Reflections read, of which 1490 rejected -29 =< h =< 29, -15 =< k =< 16, -17 =< l =< 20, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 12 1 10.64 3.41 2 22.61 -3 12 1 33.70 1.89 4 11.41 -8 5 8 10.72 0.44 5 2.33 0 8 8 69.06 1.26 2 10.95 -19 8 9 5.69 3.01 2 16.94 -1 5 17 60.26 4.90 3 25.73 6 Inconsistent equivalents 9597 Unique reflections, of which 0 suppressed R(int) = 0.0319 R(sigma) = 0.0326 Friedel opposites merged Maximum memory for data reduction = 6415 / 96634 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 = 7968 / 667889 wR2 = 0.0799 before cycle 1 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.010 OSF Mean shift/esd = 0.003 Maximum = 0.045 for U23 Pd1 Max. shift = 0.000 A for H56A Max. dU = 0.000 for O56 Least-squares cycle 2 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 2 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.016 for U23 Pd1 Max. shift = 0.000 A for H51B Max. dU = 0.000 for O56 Least-squares cycle 3 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 3 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H56B Max. dU = 0.000 for O56 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 4 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H54A Max. dU = 0.000 for O56 Least-squares cycle 5 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 5 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H54A Max. dU = 0.000 for O56 Least-squares cycle 6 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 6 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H54A Max. dU = 0.000 for O56 Least-squares cycle 7 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 7 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H54A Max. dU = 0.000 for C36 Least-squares cycle 8 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 8 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H54A Max. dU = 0.000 for O56 Least-squares cycle 9 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 9 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H55A Max. dU = 0.000 for O56 Least-squares cycle 10 Maximum vector length = 511 Memory required = 7968 / 667889 wR2 = 0.0799 before cycle 10 for 9597 data and 503 / 503 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23199 0.00020 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x Pd1 Max. shift = 0.000 A for H56B Max. dU = 0.000 for O51 Largest correlation matrix elements 0.970 z H56B / y H56B 0.781 z H55A / x H55A 0.578 z H51B / x H51B 0.916 z H56A / x H56A 0.634 y H52B / y H52A 0.551 U13 O56 / U11 O56 -0.906 x H56B / x H56A 0.627 z H53B / z H53A 0.534 U13 O56 / U33 O56 -0.817 x H56B / z H56A 0.580 z H52A / x H52A 0.514 U13 O52 / U11 O52 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H11A 0.8625 0.0885 -0.1197 137 0.980 0.000 C11 C2 H11A H11B 0.8388 0.1683 -0.0575 137 0.980 0.000 C11 C2 H11A H11C 0.7913 0.0902 -0.1283 137 0.980 0.000 C11 C2 H11A H12A 0.8693 -0.1699 -0.1349 137 0.980 0.000 C12 C3 H12A H12B 0.8089 -0.0970 -0.1733 137 0.980 0.000 C12 C3 H12A H12C 0.8045 -0.2137 -0.1320 137 0.980 0.000 C12 C3 H12A H13A 0.8361 -0.3124 0.0008 137 0.980 0.000 C13 C4 H13A H13B 0.8525 -0.3028 0.1086 137 0.980 0.000 C13 C4 H13A H13C 0.9062 -0.3007 0.0645 137 0.980 0.000 C13 C4 H13A H14A 0.8793 -0.1938 0.2231 137 0.980 0.000 C14 C5 H14A H14B 0.8722 -0.0725 0.2532 137 0.980 0.000 C14 C5 H14A H14C 0.9364 -0.1127 0.2455 137 0.980 0.000 C14 C5 H14A H15A 0.6982 -0.1506 -0.1753 137 0.980 0.000 C15 C7 H15A H15B 0.6973 -0.0217 -0.1788 137 0.980 0.000 C15 C7 H15A H15C 0.6357 -0.0867 -0.1872 137 0.980 0.000 C15 C7 H15A H16A 0.7343 -0.3344 0.0119 137 0.980 0.000 C16 C8 H16A H16B 0.7227 -0.2901 -0.0888 137 0.980 0.000 C16 C8 H16A H16C 0.6657 -0.3141 -0.0544 137 0.980 0.000 C16 C8 H16A H17A 0.7017 -0.2354 0.1846 137 0.980 0.000 C17 C9 H17A H17B 0.7695 -0.1857 0.2217 137 0.980 0.000 C17 C9 H17A H17C 0.7556 -0.2869 0.1543 137 0.980 0.000 C17 C9 H17A H18A 0.6766 0.0146 0.1894 137 0.980 0.000 C18 C10 H18A H18B 0.7270 0.0978 0.1793 137 0.980 0.000 C18 C10 H18A H18C 0.7481 -0.0135 0.2323 137 0.980 0.000 C18 C10 H18A H19 1.0020 0.2018 0.1581 13 1.000 0.000 C19 C20 C21 P1 H20A 1.0178 0.1593 0.0242 137 0.980 0.000 C20 C19 H20A H20B 0.9508 0.2121 -0.0019 137 0.980 0.000 C20 C19 H20A H20C 0.9580 0.0842 -0.0076 137 0.980 0.000 C20 C19 H20A H21A 0.9904 -0.0265 0.1389 137 0.980 0.000 C21 C19 H21A H21B 1.0191 0.0368 0.2328 137 0.980 0.000 C21 C19 H21A H21C 1.0538 0.0378 0.1590 137 0.980 0.000 C21 C19 H21A H22 0.9419 0.0647 0.2815 13 1.000 0.000 C22 C23 C24 P1 H23A 0.8783 0.1217 0.3600 137 0.980 0.000 C23 C22 H23A H23B 0.8343 0.0889 0.2606 137 0.980 0.000 C23 C22 H23A H23C 0.8483 0.2133 0.2864 137 0.980 0.000 C23 C22 H23A H24A 0.9474 0.2953 0.2890 137 0.980 0.000 C24 C22 H24A H24B 1.0037 0.2177 0.2930 137 0.980 0.000 C24 C22 H24A H24C 0.9764 0.2186 0.3751 137 0.980 0.000 C24 C22 H24A H25 0.5935 0.2276 -0.1500 13 1.000 0.000 C25 C26 C27 P2 H26A 0.6481 0.1001 -0.2495 137 0.980 0.000 C26 C25 H26A H26B 0.6867 0.1995 -0.1936 137 0.980 0.000 C26 C25 H26A H26C 0.6213 0.2200 -0.2693 137 0.980 0.000 C26 C25 H26A H27A 0.5457 0.0684 -0.2451 137 0.980 0.000 C27 C25 H27A H27B 0.5258 0.1049 -0.1602 137 0.980 0.000 C27 C25 H27A H27C 0.5728 0.0069 -0.1499 137 0.980 0.000 C27 C25 H27A H28 0.6403 0.1728 0.1013 13 1.000 0.000 C28 C30 C29 P2 H29A 0.5538 0.0748 0.0863 137 0.980 0.000 C29 C28 H29A H29B 0.5948 0.0005 0.0446 137 0.980 0.000 C29 C28 H29A H29C 0.5372 0.0648 -0.0216 137 0.980 0.000 C29 C28 H29A H30A 0.5463 0.2627 -0.0501 137 0.980 0.000 C30 C28 H30A H30B 0.6021 0.3296 0.0174 137 0.980 0.000 C30 C28 H30A H30C 0.5510 0.2777 0.0540 137 0.980 0.000 C30 C28 H30A H31 0.7498 0.2183 -0.0505 13 1.000 0.000 C31 C32 C38 P2 H32 0.7736 0.1747 0.1100 13 1.000 0.000 C32 C33 C31 Pd1 H33A 0.7669 0.2994 0.2109 23 0.990 0.000 C33 C32 C34 H33B 0.7009 0.3082 0.1346 23 0.990 0.000 C33 C32 C34 H34A 0.7164 0.4758 0.0994 23 0.990 0.000 C34 C35 C33 H34B 0.7660 0.4767 0.1993 23 0.990 0.000 C34 C35 C33 ** Bond(s) to Pd1 ignored in idealizing H-atoms attached to C35 ** H35 0.8433 0.4919 0.1396 43 0.950 0.000 C35 C36 C34 ** Bond(s) to Pd1 ignored in idealizing H-atoms attached to C36 ** H36 0.8394 0.4710 -0.0021 43 0.950 0.000 C36 C35 C37 H37A 0.7646 0.3862 -0.1139 23 0.990 0.000 C37 C36 C38 H37B 0.7287 0.4915 -0.1010 23 0.990 0.000 C37 C36 C38 H38A 0.6654 0.3426 -0.1141 23 0.990 0.000 C38 C37 C31 H38B 0.6804 0.3917 -0.0141 23 0.990 0.000 C38 C37 C31 s93 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86467 0.02352 0.08405 1.00000 0.01063 0.01175 0.01354 -0.00043 0.00380 -0.00078 0.01201 0.00411 0.00009 0.00018 0.00014 0.00000 0.00094 0.00104 0.00099 0.00082 0.00078 0.00078 0.00041 C2 0.84508 0.01159 -0.01447 1.00000 0.01066 0.01472 0.01373 -0.00120 0.00378 -0.00064 0.01309 0.00417 0.00009 0.00018 0.00014 0.00000 0.00095 0.00108 0.00098 0.00085 0.00078 0.00080 0.00042 C3 0.84284 -0.10050 -0.03456 1.00000 0.01307 0.01520 0.01858 -0.00558 0.00399 -0.00022 0.01591 0.00431 0.00010 0.00019 0.00015 0.00000 0.00100 0.00110 0.00107 0.00090 0.00084 0.00084 0.00044 C4 0.85845 -0.15903 0.04799 1.00000 0.01434 0.01133 0.02414 -0.00212 0.00136 0.00189 0.01781 0.00447 0.00010 0.00018 0.00016 0.00000 0.00105 0.00108 0.00116 0.00092 0.00088 0.00084 0.00046 C5 0.87147 -0.08404 0.12197 1.00000 0.01137 0.00979 0.01770 0.00026 0.00068 -0.00044 0.01395 0.00421 0.00010 0.00017 0.00015 0.00000 0.00097 0.00103 0.00104 0.00085 0.00081 0.00079 0.00043 C6 0.69687 0.00975 0.00128 1.00000 0.01155 0.01181 0.01339 0.00176 0.00440 -0.00068 0.01217 0.00417 0.00009 0.00017 0.00014 0.00000 0.00095 0.00103 0.00098 0.00082 0.00078 0.00079 0.00041 C7 0.69579 -0.08162 -0.05749 1.00000 0.01003 0.01348 0.01614 -0.00037 0.00072 -0.00141 0.01409 0.00416 0.00009 0.00018 0.00015 0.00000 0.00096 0.00108 0.00103 0.00086 0.00080 0.00080 0.00043 C8 0.71092 -0.17548 -0.00234 1.00000 0.01285 0.01197 0.02348 0.00152 0.00166 -0.00374 0.01715 0.00439 0.00010 0.00018 0.00016 0.00000 0.00103 0.00109 0.00114 0.00091 0.00087 0.00083 0.00046 C9 0.72340 -0.14498 0.08988 1.00000 0.01394 0.01740 0.02109 0.00651 0.00236 -0.00349 0.01830 0.00457 0.00010 0.00019 0.00016 0.00000 0.00104 0.00115 0.00113 0.00095 0.00087 0.00088 0.00047 C10 0.71516 -0.03188 0.09432 1.00000 0.01185 0.01913 0.01389 0.00122 0.00369 -0.00427 0.01508 0.00427 0.00010 0.00019 0.00014 0.00000 0.00098 0.00115 0.00101 0.00089 0.00080 0.00084 0.00044 C11 0.83344 0.09702 -0.08618 1.00000 0.01759 0.01887 0.01199 -0.00007 0.00507 -0.00002 0.01609 0.00445 0.00010 0.00019 0.00014 0.00000 0.00106 0.00116 0.00098 0.00088 0.00083 0.00089 0.00044 H11A 0.86253 0.08846 -0.11967 1.00000 0.02414 0.00000 0.00000 H11B 0.83885 0.16832 -0.05751 1.00000 0.02414 0.00000 0.00000 H11C 0.79135 0.09015 -0.12826 1.00000 0.02414 0.00000 0.00000 C12 0.83031 -0.14949 -0.12659 1.00000 0.02163 0.02425 0.02365 -0.01297 0.00589 -0.00179 0.02355 0.00467 0.00011 0.00021 0.00017 0.00000 0.00120 0.00131 0.00122 0.00105 0.00097 0.00100 0.00053 H12A 0.86926 -0.16990 -0.13487 1.00000 0.03532 0.00000 0.00000 H12B 0.80892 -0.09699 -0.17325 1.00000 0.03532 0.00000 0.00000 H12C 0.80455 -0.21369 -0.13195 1.00000 0.03532 0.00000 0.00000 C13 0.86378 -0.27909 0.05619 1.00000 0.02536 0.01163 0.04217 -0.00515 -0.00050 0.00165 0.02921 0.00512 0.00012 0.00020 0.00020 0.00000 0.00132 0.00118 0.00156 0.00112 0.00115 0.00099 0.00060 H13A 0.83614 -0.31243 0.00082 1.00000 0.04381 0.00000 0.00000 H13B 0.85247 -0.30282 0.10862 1.00000 0.04381 0.00000 0.00000 H13C 0.90622 -0.30066 0.06449 1.00000 0.04381 0.00000 0.00000 C14 0.89156 -0.11875 0.21934 1.00000 0.01958 0.01504 0.01937 0.00493 -0.00089 -0.00092 0.01977 0.00458 0.00011 0.00019 0.00016 0.00000 0.00114 0.00115 0.00113 0.00093 0.00090 0.00090 0.00048 H14A 0.87926 -0.19379 0.22305 1.00000 0.02966 0.00000 0.00000 H14B 0.87221 -0.07248 0.25325 1.00000 0.02966 0.00000 0.00000 H14C 0.93635 -0.11270 0.24550 1.00000 0.02966 0.00000 0.00000 C15 0.68045 -0.08549 -0.15836 1.00000 0.01875 0.02116 0.01533 -0.00335 0.00082 0.00265 0.01957 0.00451 0.00011 0.00020 0.00015 0.00000 0.00112 0.00123 0.00107 0.00094 0.00088 0.00093 0.00048 H15A 0.69822 -0.15064 -0.17527 1.00000 0.02936 0.00000 0.00000 H15B 0.69735 -0.02167 -0.17881 1.00000 0.02936 0.00000 0.00000 H15C 0.63570 -0.08670 -0.18716 1.00000 0.02936 0.00000 0.00000 C16 0.70817 -0.28815 -0.03631 1.00000 0.02226 0.01247 0.03403 -0.00231 -0.00024 -0.00220 0.02523 0.00483 0.00012 0.00020 0.00018 0.00000 0.00123 0.00116 0.00139 0.00103 0.00104 0.00094 0.00055 H16A 0.73433 -0.33443 0.01194 1.00000 0.03785 0.00000 0.00000 H16B 0.72272 -0.29009 -0.08881 1.00000 0.03785 0.00000 0.00000 H16C 0.66567 -0.31413 -0.05443 1.00000 0.03785 0.00000 0.00000 C17 0.73887 -0.21968 0.16947 1.00000 0.02504 0.02410 0.02841 0.01249 0.00427 -0.00312 0.02694 0.00537 0.00012 0.00022 0.00018 0.00000 0.00128 0.00133 0.00131 0.00111 0.00105 0.00105 0.00056 H17A 0.70165 -0.23541 0.18462 1.00000 0.04041 0.00000 0.00000 H17B 0.76946 -0.18569 0.22170 1.00000 0.04041 0.00000 0.00000 H17C 0.75565 -0.28693 0.15429 1.00000 0.04041 0.00000 0.00000 C18 0.71685 0.02136 0.18131 1.00000 0.01747 0.02611 0.01349 0.00158 0.00591 -0.00517 0.01882 0.00452 0.00011 0.00020 0.00015 0.00000 0.00107 0.00128 0.00102 0.00095 0.00086 0.00094 0.00047 H18A 0.67655 0.01457 0.18941 1.00000 0.02823 0.00000 0.00000 H18B 0.72700 0.09785 0.17926 1.00000 0.02823 0.00000 0.00000 H18C 0.74811 -0.01347 0.23226 1.00000 0.02823 0.00000 0.00000 C19 0.97795 0.13887 0.12459 1.00000 0.01254 0.01989 0.01474 -0.00049 0.00471 -0.00062 0.01566 0.00443 0.00010 0.00019 0.00015 0.00000 0.00100 0.00117 0.00101 0.00090 0.00081 0.00086 0.00044 H19 1.00203 0.20182 0.15811 1.00000 0.01879 0.00000 0.00000 C20 0.97595 0.14959 0.02601 1.00000 0.01843 0.03149 0.01706 0.00005 0.00960 -0.00108 0.02140 0.00489 0.00011 0.00022 0.00015 0.00000 0.00113 0.00138 0.00109 0.00102 0.00091 0.00100 0.00050 H20A 1.01777 0.15929 0.02418 1.00000 0.03209 0.00000 0.00000 H20B 0.95082 0.21213 -0.00185 1.00000 0.03209 0.00000 0.00000 H20C 0.95797 0.08423 -0.00759 1.00000 0.03209 0.00000 0.00000 C21 1.01351 0.03767 0.16769 1.00000 0.01643 0.02805 0.02565 0.00521 0.00947 0.00553 0.02275 0.00524 0.00011 0.00021 0.00017 0.00000 0.00111 0.00136 0.00122 0.00106 0.00095 0.00099 0.00051 H21A 0.99044 -0.02648 0.13887 1.00000 0.03412 0.00000 0.00000 H21B 1.01909 0.03683 0.23283 1.00000 0.03412 0.00000 0.00000 H21C 1.05378 0.03778 0.15900 1.00000 0.03412 0.00000 0.00000 C22 0.92100 0.13562 0.26253 1.00000 0.01571 0.01682 0.01188 -0.00155 0.00391 -0.00178 0.01495 0.00424 0.00010 0.00019 0.00014 0.00000 0.00103 0.00113 0.00097 0.00086 0.00081 0.00086 0.00043 H22 0.94190 0.06466 0.28148 1.00000 0.01794 0.00000 0.00000 C23 0.86551 0.14033 0.29530 1.00000 0.02000 0.02931 0.01653 -0.00044 0.00750 -0.00072 0.02157 0.00487 0.00011 0.00022 0.00016 0.00000 0.00116 0.00137 0.00109 0.00100 0.00091 0.00100 0.00050 H23A 0.87825 0.12174 0.35997 1.00000 0.03236 0.00000 0.00000 H23B 0.83432 0.08894 0.26055 1.00000 0.03236 0.00000 0.00000 H23C 0.84828 0.21333 0.28644 1.00000 0.03236 0.00000 0.00000 C24 0.96616 0.22479 0.30908 1.00000 0.02804 0.03463 0.01589 -0.01001 0.00511 -0.01261 0.02670 0.00464 0.00012 0.00023 0.00016 0.00000 0.00133 0.00150 0.00112 0.00107 0.00099 0.00114 0.00057 H24A 0.94737 0.29527 0.28903 1.00000 0.04004 0.00000 0.00000 H24B 1.00371 0.21766 0.29295 1.00000 0.04004 0.00000 0.00000 H24C 0.97637 0.21860 0.37511 1.00000 0.04004 0.00000 0.00000 C25 0.61379 0.15633 -0.14981 1.00000 0.01467 0.01904 0.01511 0.00167 0.00195 0.00011 0.01699 0.00443 0.00010 0.00020 0.00015 0.00000 0.00105 0.00116 0.00103 0.00090 0.00084 0.00088 0.00045 H25 0.59346 0.22762 -0.15000 1.00000 0.02038 0.00000 0.00000 C26 0.64533 0.17024 -0.22208 1.00000 0.02729 0.02221 0.01433 0.00127 0.00527 0.00004 0.02165 0.00489 0.00012 0.00021 0.00016 0.00000 0.00126 0.00126 0.00105 0.00095 0.00094 0.00100 0.00050 H26A 0.64812 0.10012 -0.24947 1.00000 0.03248 0.00000 0.00000 H26B 0.68672 0.19954 -0.19362 1.00000 0.03248 0.00000 0.00000 H26C 0.62127 0.21995 -0.26926 1.00000 0.03248 0.00000 0.00000 C27 0.55960 0.07692 -0.17890 1.00000 0.02069 0.02785 0.02439 0.00094 0.00147 -0.00452 0.02575 0.00487 0.00011 0.00022 0.00017 0.00000 0.00121 0.00140 0.00125 0.00108 0.00099 0.00103 0.00055 H27A 0.54572 0.06837 -0.24509 1.00000 0.03863 0.00000 0.00000 H27B 0.52577 0.10488 -0.16021 1.00000 0.03863 0.00000 0.00000 H27C 0.57278 0.00688 -0.14994 1.00000 0.03863 0.00000 0.00000 C28 0.61267 0.16401 0.03712 1.00000 0.01484 0.02020 0.01986 -0.00124 0.00881 -0.00202 0.01754 0.00462 0.00010 0.00019 0.00016 0.00000 0.00105 0.00119 0.00109 0.00093 0.00088 0.00089 0.00046 H28 0.64029 0.17284 0.10132 1.00000 0.02104 0.00000 0.00000 C29 0.57080 0.06723 0.03657 1.00000 0.01917 0.02696 0.03007 0.00310 0.01289 -0.00393 0.02422 0.00512 0.00011 0.00021 0.00018 0.00000 0.00117 0.00136 0.00130 0.00109 0.00102 0.00100 0.00053 H29A 0.55376 0.07476 0.08626 1.00000 0.03633 0.00000 0.00000 H29B 0.59475 0.00045 0.04463 1.00000 0.03633 0.00000 0.00000 H29C 0.53719 0.06478 -0.02155 1.00000 0.03633 0.00000 0.00000 C30 0.57455 0.26788 0.01235 1.00000 0.02060 0.02334 0.03411 -0.00090 0.01546 0.00382 0.02443 0.00536 0.00011 0.00021 0.00018 0.00000 0.00119 0.00131 0.00136 0.00111 0.00105 0.00100 0.00053 H30A 0.54629 0.26266 -0.05014 1.00000 0.03665 0.00000 0.00000 H30B 0.60208 0.32957 0.01742 1.00000 0.03665 0.00000 0.00000 H30C 0.55096 0.27773 0.05397 1.00000 0.03665 0.00000 0.00000 C31 0.72384 0.24397 -0.01411 1.00000 0.01262 0.01205 0.01378 -0.00022 0.00509 -0.00056 0.01263 0.00414 0.00009 0.00017 0.00014 0.00000 0.00097 0.00104 0.00099 0.00083 0.00080 0.00081 0.00041 H31 0.74978 0.21833 -0.05047 1.00000 0.01515 0.00000 0.00000 C32 0.76764 0.24940 0.08440 1.00000 0.01155 0.01294 0.01342 0.00042 0.00393 -0.00156 0.01268 0.00414 0.00009 0.00018 0.00014 0.00000 0.00096 0.00104 0.00097 0.00083 0.00079 0.00080 0.00041 H32 0.77364 0.17469 0.10995 1.00000 0.01521 0.00000 0.00000 C33 0.74533 0.32130 0.14726 1.00000 0.01755 0.01798 0.01656 -0.00254 0.00750 -0.00041 0.01689 0.00451 0.00011 0.00018 0.00015 0.00000 0.00108 0.00116 0.00104 0.00091 0.00087 0.00088 0.00045 H33A 0.76687 0.29944 0.21090 1.00000 0.02027 0.00000 0.00000 H33B 0.70089 0.30816 0.13459 1.00000 0.02027 0.00000 0.00000 C34 0.75526 0.44298 0.13844 1.00000 0.02580 0.01649 0.02059 -0.00472 0.00905 0.00243 0.02060 0.00483 0.00011 0.00019 0.00016 0.00000 0.00123 0.00118 0.00115 0.00095 0.00096 0.00096 0.00049 H34A 0.71638 0.47577 0.09940 1.00000 0.02472 0.00000 0.00000 H34B 0.76598 0.47672 0.19925 1.00000 0.02472 0.00000 0.00000 C35 0.80539 0.46678 0.09853 1.00000 0.02155 0.00703 0.02531 -0.00180 0.00454 0.00072 0.01873 0.00467 0.00011 0.00018 0.00016 0.00000 0.00114 0.00103 0.00119 0.00091 0.00094 0.00086 0.00047 H35 0.84328 0.49192 0.13963 1.00000 0.02247 0.00000 0.00000 C36 0.80238 0.45623 0.01010 1.00000 0.01839 0.00849 0.02560 0.00244 0.00632 0.00111 0.01771 0.00459 0.00011 0.00018 0.00016 0.00000 0.00110 0.00104 0.00118 0.00091 0.00092 0.00085 0.00046 H36 0.83939 0.47099 -0.00214 1.00000 0.02125 0.00000 0.00000 C37 0.74847 0.42445 -0.07069 1.00000 0.02079 0.01285 0.01772 0.00281 0.00581 0.00069 0.01724 0.00451 0.00011 0.00019 0.00015 0.00000 0.00112 0.00109 0.00107 0.00089 0.00089 0.00088 0.00045 H37A 0.76465 0.38624 -0.11389 1.00000 0.02068 0.00000 0.00000 H37B 0.72875 0.49149 -0.10101 1.00000 0.02068 0.00000 0.00000 C38 0.69844 0.35403 -0.05540 1.00000 0.01795 0.01210 0.01762 0.00239 0.00348 0.00007 0.01646 0.00448 0.00010 0.00018 0.00015 0.00000 0.00108 0.00107 0.00107 0.00088 0.00087 0.00086 0.00045 H38A 0.66537 0.34255 -0.11409 1.00000 0.01975 0.00000 0.00000 H38B 0.68038 0.39174 -0.01411 1.00000 0.01975 0.00000 0.00000 P1 0.90079 0.14720 0.13774 1.00000 0.01063 0.01002 0.01035 -0.00138 0.00308 -0.00141 0.01042 0.00104 0.00002 0.00004 0.00004 0.00000 0.00024 0.00026 0.00024 0.00020 0.00019 0.00020 0.00011 P2 0.66295 0.14065 -0.03154 1.00000 0.01054 0.01120 0.01310 -0.00009 0.00354 -0.00043 0.01169 0.00107 0.00002 0.00005 0.00004 0.00000 0.00025 0.00027 0.00025 0.00021 0.00020 0.00020 0.00011 Cl1 0.94745 0.40446 0.10445 1.00000 0.01864 0.02110 0.03129 0.00140 0.00584 -0.00873 0.02425 0.00115 0.00003 0.00005 0.00004 0.00000 0.00027 0.00030 0.00031 0.00025 0.00023 0.00023 0.00013 Fe1 0.78244 -0.06229 0.03533 1.00000 0.01115 0.00862 0.01209 0.00016 0.00121 -0.00098 0.01125 0.00058 0.00001 0.00002 0.00002 0.00000 0.00015 0.00015 0.00014 0.00012 0.00011 0.00011 0.00007 Pd1 0.85238 0.31035 0.08981 1.00000 0.01244 0.00865 0.01486 -0.00054 0.00379 -0.00218 0.01215 0.00031 0.00001 0.00001 0.00001 0.00000 0.00009 0.00009 0.00009 0.00006 0.00006 0.00006 0.00005 Cl11 0.53826 -0.22448 -0.14632 1.00000 0.03528 0.02810 0.03578 0.00295 0.01725 0.00159 0.03168 0.00143 0.00003 0.00006 0.00005 0.00000 0.00036 0.00034 0.00035 0.00028 0.00029 0.00028 0.00015 O51 0.56938 0.42047 -0.22712 1.00000 0.02897 0.03461 0.03844 0.00170 0.00393 0.00989 0.03574 0.00429 0.00009 0.00018 0.00015 0.00000 0.00105 0.00119 0.00115 0.00094 0.00087 0.00089 0.00047 H51A 0.53832 0.38707 -0.26270 1.00000 0.05361 0.03407 0.00123 0.00267 0.00194 0.00000 0.00000 H51B 0.55499 0.44909 -0.18945 1.00000 0.05361 0.05911 0.00148 0.00277 0.00188 0.00000 0.00000 O52 0.60190 -0.13370 0.23161 1.00000 0.03948 0.04310 0.04803 0.00723 0.02560 0.00188 0.04078 0.00493 0.00010 0.00019 0.00016 0.00000 0.00122 0.00132 0.00130 0.00111 0.00102 0.00105 0.00052 H52A 0.58675 -0.17898 0.25883 1.00000 0.06117 0.07518 0.00173 0.00212 0.00246 0.00000 0.00000 H52B 0.59251 -0.07207 0.24554 1.00000 0.06117 0.07406 0.00182 0.00158 0.00262 0.00000 0.00000 O53 0.58855 -0.25116 0.07435 1.00000 0.05027 0.05186 0.03740 0.00043 0.00639 -0.01435 0.04845 0.00466 0.00012 0.00020 0.00016 0.00000 0.00142 0.00155 0.00121 0.00111 0.00111 0.00119 0.00060 H53A 0.57561 -0.21985 0.02385 1.00000 0.07268 0.07551 0.00192 0.00297 0.00145 0.00000 0.00000 H53B 0.58460 -0.20745 0.11303 1.00000 0.07268 0.07202 0.00204 0.00274 0.00189 0.00000 0.00000 O54 0.46748 0.03113 -0.40401 1.00000 0.06340 0.02847 0.02474 -0.00208 0.01061 0.00277 0.03980 0.00448 0.00011 0.00017 0.00014 0.00000 0.00151 0.00111 0.00099 0.00089 0.00099 0.00105 0.00052 H54A 0.44444 0.02512 -0.45834 1.00000 0.05970 0.04506 0.00153 0.00277 0.00142 0.00000 0.00000 H54B 0.46303 0.09669 -0.39099 1.00000 0.05970 0.05825 0.00170 0.00172 0.00225 0.00000 0.00000 O55 0.58828 0.52887 0.09283 1.00000 0.05713 0.03650 0.03374 0.00781 0.00317 -0.00136 0.04531 0.00480 0.00012 0.00019 0.00015 0.00000 0.00151 0.00126 0.00115 0.00103 0.00105 0.00113 0.00056 H55A 0.55622 0.52685 0.10866 1.00000 0.06797 0.07791 0.00132 0.00301 0.00281 0.00000 0.00000 H55B 0.59490 0.59473 0.09016 1.00000 0.06797 0.07183 0.00172 0.00167 0.00285 0.00000 0.00000 O56 1.07159 0.42380 0.05783 1.00000 0.08072 0.14170 0.08526 0.01945 0.04530 0.01139 0.09813 0.00891 0.00016 0.00041 0.00025 0.00000 0.00239 0.00365 0.00249 0.00247 0.00203 0.00244 0.00121 H56A 1.03827 0.41400 0.06876 1.00000 0.14719 0.11798 0.00136 0.00561 0.00377 0.00000 0.00000 H56B 1.06137 0.45243 0.00549 1.00000 0.14719 0.12222 0.00244 0.00535 0.00213 0.00000 0.00000 Final Structure Factor Calculation for s93 in P2(1)/c Total number of l.s. parameters = 503 Maximum vector length = 511 Memory required = 7465 / 26061 wR2 = 0.0799 before cycle 11 for 9597 data and 0 / 503 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 6. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.018 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0323 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0320 for 8501 Fo > 4sig(Fo) and 0.0389 for all 9597 data wR2 = 0.0799, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 76.00 for hydrogen atoms Principal mean square atomic displacements U 0.0137 0.0121 0.0102 C1 0.0155 0.0132 0.0106 C2 0.0235 0.0131 0.0111 C3 0.0292 0.0139 0.0103 C4 0.0217 0.0105 0.0096 C5 0.0147 0.0120 0.0098 C6 0.0196 0.0138 0.0089 C7 0.0280 0.0149 0.0086 C8 0.0301 0.0140 0.0108 C9 0.0220 0.0136 0.0096 C10 0.0189 0.0177 0.0117 C11 0.0376 0.0221 0.0110 C12 0.0546 0.0223 0.0107 C13 0.0318 0.0162 0.0113 C14 0.0281 0.0177 0.0129 C15 0.0439 0.0202 0.0115 C16 0.0441 0.0236 0.0131 C17 0.0291 0.0158 0.0115 C18 0.0200 0.0147 0.0123 C19 0.0316 0.0206 0.0120 C20 0.0330 0.0218 0.0134 C21 0.0181 0.0153 0.0114 C22 0.0294 0.0201 0.0152 C23 0.0446 0.0250 0.0106 C24 0.0206 0.0179 0.0125 C25 0.0285 0.0224 0.0141 C26 0.0346 0.0257 0.0170 C27 0.0222 0.0188 0.0116 C28 0.0320 0.0281 0.0126 C29 0.0352 0.0252 0.0129 C30 0.0141 0.0123 0.0115 C31 0.0146 0.0131 0.0104 C32 0.0202 0.0173 0.0132 C33 0.0265 0.0237 0.0116 C34 0.0288 0.0205 0.0068 C35 0.0265 0.0185 0.0081 C36 0.0212 0.0190 0.0116 C37 0.0217 0.0165 0.0112 C38 0.0119 0.0110 0.0084 P1 0.0133 0.0114 0.0103 P2 0.0353 0.0268 0.0107 Cl1 0.0156 0.0099 0.0083 Fe1 0.0154 0.0134 0.0077 Pd1 0.0404 0.0284 0.0262 Cl11 0.0481 0.0383 0.0209 O51 0.0562 0.0408 0.0254 O52 0.0702 0.0414 0.0338 O53 0.0667 0.0293 0.0234 O54 0.0689 0.0403 0.0268 O55 0.1492 0.0898 0.0554 O56 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.030 0.044 0.061 0.078 0.098 0.121 0.151 0.201 1.000 Number in group 1015. 961. 904. 1005. 929. 971. 959. 941. 946. 966. GooF 1.028 1.066 1.031 1.061 1.085 0.968 0.994 1.034 1.037 1.026 K 2.232 1.134 1.029 0.989 0.987 0.991 0.999 1.007 1.010 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 974. 963. 962. 962. 954. 942. 956. 962. 962. 960. GooF 1.026 0.951 0.881 0.875 0.845 0.859 0.837 0.868 0.944 1.837 K 0.964 0.994 1.022 1.020 1.024 1.021 1.016 1.000 1.000 0.994 R1 0.079 0.068 0.060 0.044 0.037 0.034 0.028 0.024 0.022 0.032 Recommended weighting scheme: WGHT 0.0324 6.3849 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) 5 0 2 -2.18 307.25 8.04 0.040 3.30 4 3 0 920.75 404.15 7.91 0.045 3.29 0 2 1 3813.35 7128.02 7.87 0.191 5.71 -3 1 5 1070.13 590.64 6.37 0.055 3.01 0 1 3 3589.08 2519.45 6.33 0.114 4.56 -5 2 1 1772.83 1116.81 6.26 0.076 3.70 6 3 0 2038.67 3018.04 6.11 0.124 2.73 -3 1 3 6313.56 4687.90 6.08 0.155 4.53 2 5 2 1436.54 879.89 6.06 0.067 2.25 -3 2 2 109.01 10.12 5.74 0.007 4.42 6 0 4 341.42 118.07 5.71 0.025 2.24 -3 0 4 4193.84 3044.53 5.68 0.125 3.82 0 3 4 3974.44 2984.57 5.31 0.124 2.75 6 6 1 885.26 524.40 5.14 0.052 1.75 -4 1 3 37.56 185.98 4.86 0.031 4.18 0 6 0 716.67 351.27 4.73 0.042 2.07 -3 2 7 5060.32 3996.14 4.63 0.143 2.09 4 0 2 761.98 1166.72 4.52 0.077 3.82 5 1 1 4450.94 5625.46 4.52 0.170 3.67 2 2 5 57.45 2.21 4.47 0.003 2.42 -5 2 6 2453.05 3226.13 4.46 0.129 2.33 -4 2 1 16473.67 19671.28 4.43 0.317 4.22 -3 3 6 222.85 75.32 4.41 0.020 2.20 6 1 1 236.49 98.45 4.34 0.022 3.17 2 2 3 6676.60 5453.62 4.34 0.167 3.37 3 0 6 8772.34 7251.30 4.31 0.193 2.12 -12 0 2 2570.60 3441.99 4.31 0.133 1.91 -2 2 2 5242.02 6465.76 4.26 0.182 4.73 6 1 0 4498.45 3593.13 4.26 0.136 3.48 -6 4 3 7255.04 8783.37 4.22 0.212 2.33 -9 1 3 91.73 15.41 4.10 0.009 2.47 3 3 4 247.52 111.33 4.10 0.024 2.38 -1 4 1 6562.73 5423.56 4.05 0.167 3.03 -1 2 2 4637.52 5695.72 4.02 0.171 4.85 7 0 2 15971.58 18832.43 4.02 0.311 2.58 1 5 2 860.04 579.54 3.96 0.054 2.31 4 2 1 1245.61 1692.66 3.95 0.093 3.71 -3 1 1 269.75 124.81 3.95 0.025 6.45 2 1 5 1148.86 817.51 3.90 0.065 2.57 4 4 1 550.10 340.71 3.84 0.042 2.58 2 1 2 6055.08 7300.51 3.82 0.193 4.90 3 3 2 11965.23 13977.52 3.76 0.268 3.04 3 3 0 13983.19 12020.92 3.74 0.248 3.59 -2 1 3 835.48 1173.87 3.71 0.078 4.75 6 3 4 1408.87 1047.43 3.67 0.073 1.97 -8 6 3 338.17 181.78 3.64 0.031 1.66 -5 3 2 12074.96 14077.79 3.64 0.268 3.02 -8 1 9 4178.38 3426.73 3.63 0.132 1.65 -7 0 8 3593.21 4435.05 3.60 0.151 1.87 2 0 4 1826.49 1414.03 3.59 0.085 3.18 Bond lengths and angles C1 - Distance Angles C5 1.4465 (0.0030) C2 1.4582 (0.0028) 106.91 (0.18) P1 1.8134 (0.0022) 128.30 (0.16) 120.55 (0.16) Fe1 2.0864 (0.0021) 69.02 (0.12) 68.54 (0.12) 145.47 (0.12) C1 - C5 C2 P1 C2 - Distance Angles C3 1.4221 (0.0031) C1 1.4582 (0.0028) 107.89 (0.19) C11 1.4987 (0.0030) 122.85 (0.19) 129.10 (0.20) Fe1 2.0624 (0.0021) 70.67 (0.13) 70.31 (0.12) 128.16 (0.15) C2 - C3 C1 C11 C3 - Distance Angles C4 1.4164 (0.0033) C2 1.4221 (0.0031) 108.73 (0.19) C12 1.4954 (0.0031) 125.01 (0.21) 126.14 (0.21) Fe1 2.0818 (0.0022) 69.92 (0.13) 69.20 (0.12) 129.89 (0.16) C3 - C4 C2 C12 C4 - Distance Angles C3 1.4164 (0.0033) C5 1.4340 (0.0032) 108.73 (0.20) C13 1.4960 (0.0033) 125.23 (0.22) 125.96 (0.22) Fe1 2.0773 (0.0023) 70.26 (0.13) 69.50 (0.12) 128.75 (0.18) C4 - C3 C5 C13 C5 - Distance Angles C4 1.4340 (0.0032) C1 1.4465 (0.0030) 107.69 (0.19) C14 1.4966 (0.0031) 122.80 (0.20) 129.43 (0.20) Fe1 2.0700 (0.0021) 70.05 (0.12) 70.25 (0.12) 127.57 (0.16) C5 - C4 C1 C14 C6 - Distance Angles C7 1.4517 (0.0030) C10 1.4643 (0.0029) 106.78 (0.19) P2 1.8014 (0.0022) 127.46 (0.16) 123.78 (0.16) Fe1 2.0681 (0.0021) 69.07 (0.12) 69.67 (0.12) 138.61 (0.12) C6 - C7 C10 P2 C7 - Distance Angles C8 1.4207 (0.0031) C6 1.4517 (0.0030) 107.95 (0.19) C15 1.4939 (0.0030) 122.43 (0.20) 129.60 (0.20) Fe1 2.0590 (0.0021) 71.42 (0.12) 69.74 (0.12) 125.69 (0.16) C7 - C8 C6 C15 C8 - Distance Angles C9 1.4206 (0.0033) C7 1.4207 (0.0031) 108.75 (0.20) C16 1.4881 (0.0033) 125.48 (0.22) 125.52 (0.21) Fe1 2.0962 (0.0022) 70.01 (0.13) 68.60 (0.12) 131.79 (0.17) C8 - C9 C7 C16 C9 - Distance Angles C10 1.4202 (0.0033) C8 1.4206 (0.0033) 109.04 (0.20) C17 1.4942 (0.0033) 124.84 (0.23) 126.02 (0.23) Fe1 2.0920 (0.0023) 69.55 (0.13) 70.33 (0.13) 129.09 (0.17) C9 - C10 C8 C17 C10 - Distance Angles C9 1.4202 (0.0033) C6 1.4643 (0.0029) 107.44 (0.19) C18 1.4962 (0.0031) 121.04 (0.20) 130.87 (0.21) Fe1 2.0778 (0.0022) 70.63 (0.13) 68.97 (0.12) 132.70 (0.15) C10 - C9 C6 C18 C11 - Distance Angles C2 1.4987 (0.0030) 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 1.4954 (0.0031) 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 1.4960 (0.0033) 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 1.4966 (0.0031) 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 1.4939 (0.0030) 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 1.4881 (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 1.4942 (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 1.4962 (0.0031) 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 C20 1.5267 (0.0030) C21 1.5285 (0.0033) 110.41 (0.19) P1 1.8564 (0.0022) 113.02 (0.15) 113.06 (0.16) H19 1.0000 106.62 106.62 106.62 C19 - C20 C21 P1 C20 - Distance Angles C19 1.5267 (0.0030) 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 1.5285 (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 1.5243 (0.0031) C24 1.5285 (0.0032) 109.15 (0.19) P1 1.8499 (0.0022) 113.49 (0.15) 109.90 (0.16) H22 1.0000 108.05 108.05 108.05 C22 - C23 C24 P1 C23 - Distance Angles C22 1.5243 (0.0031) 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 1.5285 (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 1.5357 (0.0032) C27 1.5367 (0.0033) 112.89 (0.20) P2 1.8297 (0.0022) 117.69 (0.16) 113.81 (0.16) H25 1.0000 103.39 103.39 103.39 C25 - C26 C27 P2 C26 - Distance Angles C25 1.5357 (0.0032) 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 1.5367 (0.0033) 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 1.5352 (0.0034) C29 1.5378 (0.0033) 110.35 (0.19) P2 1.8379 (0.0023) 113.78 (0.16) 112.76 (0.17) H28 1.0000 106.47 106.47 106.47 C28 - C30 C29 P2 C29 - Distance Angles C28 1.5378 (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 1.5352 (0.0034) 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 C31 - Distance Angles C32 1.5371 (0.0028) C38 1.5403 (0.0030) 114.41 (0.18) P2 1.8523 (0.0022) 113.23 (0.14) 112.72 (0.14) H31 1.0000 105.12 105.12 105.12 C31 - C32 C38 P2 C32 - Distance Angles C33 1.5318 (0.0030) C31 1.5371 (0.0028) 114.57 (0.18) Pd1 2.0682 (0.0021) 105.69 (0.14) 111.02 (0.14) H32 1.0000 108.46 108.46 108.46 C32 - C33 C31 Pd1 C33 - Distance Angles C32 1.5318 (0.0030) C34 1.5392 (0.0033) 115.02 (0.19) H33A 0.9900 108.51 108.51 H33B 0.9900 108.51 108.51 107.52 C33 - C32 C34 H33A C34 - Distance Angles C35 1.5083 (0.0034) C33 1.5392 (0.0033) 112.62 (0.19) H34A 0.9900 109.07 109.07 H34B 0.9900 109.07 109.07 107.83 C34 - C35 C33 H34A C35 - Distance Angles C36 1.3624 (0.0034) C34 1.5083 (0.0033) 127.23 (0.22) Pd1 2.2469 (0.0022) 73.88 (0.13) 107.72 (0.15) H35 0.9500 116.38 116.38 88.28 C35 - C36 C34 Pd1 C36 - Distance Angles C35 1.3624 (0.0034) C37 1.5022 (0.0032) 128.80 (0.22) Pd1 2.2813 (0.0022) 71.11 (0.13) 112.28 (0.15) H36 0.9500 115.60 115.60 86.32 C36 - C35 C37 Pd1 C37 - Distance Angles C36 1.5022 (0.0032) C38 1.5250 (0.0031) 118.60 (0.19) H37A 0.9900 107.66 107.66 H37B 0.9900 107.66 107.66 107.07 C37 - C36 C38 H37A C38 - Distance Angles C37 1.5250 (0.0031) C31 1.5403 (0.0030) 111.70 (0.18) H38A 0.9900 109.28 109.28 H38B 0.9900 109.28 109.28 107.94 C38 - C37 C31 H38A P1 - Distance Angles C1 1.8134 (0.0022) C22 1.8499 (0.0022) 109.78 (0.10) C19 1.8564 (0.0022) 102.30 (0.10) 101.00 (0.10) Pd1 2.3128 (0.0006) 119.43 (0.07) 109.63 (0.08) 113.00 (0.08) P1 - C1 C22 C19 P2 - Distance Angles C6 1.8014 (0.0022) C25 1.8297 (0.0022) 116.70 (0.10) C28 1.8379 (0.0023) 105.91 (0.10) 105.61 (0.11) C31 1.8523 (0.0022) 110.17 (0.10) 105.26 (0.10) 113.35 (0.10) P2 - C6 C25 C28 Cl1 - Distance Angles Pd1 2.4246 (0.0006) Cl1 - Fe1 - Distance Angles C7 2.0590 (0.0021) C2 2.0624 (0.0021) 115.07 (0.09) C6 2.0681 (0.0021) 41.19 (0.08) 115.87 (0.08) C5 2.0700 (0.0021) 165.40 (0.09) 68.77 (0.08) 151.70 (0.09) C4 2.0773 (0.0023) 126.30 (0.09) 67.74 (0.09) 167.45 (0.09) 40.46 (0.09) C10 2.0778 (0.0022) 68.92 (0.09) 143.12 (0.09) 41.36 (0.08) 117.26 (0.09) 142.16 (0.09) C3 2.0818 (0.0022) 105.42 (0.09) 40.13 (0.09) 135.03 (0.09) 67.83 (0.09) 39.82 (0.09) 174.11 (0.09) C1 2.0864 (0.0021) 150.47 (0.09) 41.15 (0.08) 123.22 (0.09) 40.73 (0.08) 67.91 (0.09) 117.76 (0.08) 67.93 (0.08) C9 2.0920 (0.0023) 67.61 (0.09) 176.16 (0.09) 67.97 (0.09) 107.93 (0.09) 108.52 (0.09) 39.82 (0.09) 137.28 (0.09) C8 2.0962 (0.0022) 39.98 (0.09) 140.74 (0.09) 67.81 (0.09) 127.94 (0.09) 101.54 (0.09) 67.31 (0.09) 107.41 (0.09) Fe1 - C7 C2 C6 C5 C4 C10 C3 Pd1 - Distance Angles C32 2.0682 (0.0021) C35 2.2469 (0.0022) 81.47 (0.09) C36 2.2813 (0.0022) 88.07 (0.08) 35.01 (0.09) P1 2.3128 (0.0006) 92.41 (0.06) 157.91 (0.06) 166.78 (0.06) Cl1 2.4246 (0.0006) 172.03 (0.06) 90.94 (0.06) 87.06 (0.06) 93.77 (0.02) Pd1 - C32 C35 C36 P1 O51 - Distance Angles H51A 0.8548 (0.0172) H51B 0.8410 (0.0173) 102.69 (2.33) O51 - H51A O52 - Distance Angles H52A 0.8447 (0.0176) H52B 0.8419 (0.0176) 106.94 (2.52) O52 - H52A O53 - Distance Angles H53A 0.8395 (0.0179) H53B 0.8372 (0.0180) 106.60 (2.68) O53 - H53A O54 - Distance Angles H54A 0.8421 (0.0175) H54B 0.8522 (0.0176) 103.79 (2.41) O54 - H54A O55 - Distance Angles H55A 0.8517 (0.0178) H55B 0.8343 (0.0179) 103.47 (2.53) O55 - H55A O56 - Distance Angles H56A 0.8472 (0.0051) H56B 0.8488 (0.0051) 105.55 (0.85) O56 - H56A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.855(17) 2.323(18) 3.172(2) 172(3) O51-H51A...Cl11_$1 0.841(17) 1.978(17) 2.812(3) 171(3) O51-H51B...O54_$1 0.845(18) 2.44(2) 3.268(2) 168(3) O52-H52A...Cl11_$2 0.842(18) 2.037(18) 2.878(3) 177(4) O52-H52B...O51_$4 0.839(18) 2.50(2) 3.264(2) 151(3) O53-H53A...Cl11 0.837(18) 1.98(2) 2.779(3) 159(4) O53-H53B...O52 0.842(17) 1.98(2) 2.797(3) 163(4) O54-H54A...O55_$3 0.852(18) 2.295(18) 3.144(2) 174(4) O54-H54B...Cl11_$1 0.852(18) 2.11(2) 2.895(4) 152(4) O55-H55A...O54_$4 0.834(18) 1.93(2) 2.743(3) 166(4) O55-H55B...O53_$5 0.847(5) 2.336(10) 3.180(4) 174(7) O56-H56A...Cl1 0.849(5) 2.43(3) 3.224(4) 156(7) O56-H56B...Cl1_$6 FMAP and GRID set by program FMAP 2 3 39 GRID -1.389 -1 -2 1.389 1 2 R1 = 0.0381 for 9597 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.0708 0.4249 0.0582 [ 0.03 A from O56 ] Deepest hole -0.92 at 0.0505 0.4437 0.0297 [ 0.53 A from H56B ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 7417 / 67305 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6611 0.1388 0.0225 1.00000 0.05 0.48 0.86 P2 1.25 C28 1.52 H28 1.88 C6 Q2 1 0.8555 0.2993 0.0474 1.00000 0.05 0.47 0.70 PD1 2.25 H11B 2.25 H36 2.27 C36 Q3 1 0.9797 0.1440 0.0724 1.00000 0.05 0.42 0.70 C20 0.83 C19 1.34 H20A 1.39 H20C Q4 1 0.6315 0.1594 0.0009 1.00000 0.05 0.41 0.82 C28 1.04 P2 1.52 H28 1.93 C30 Q5 1 0.8635 0.0210 0.0268 1.00000 0.05 0.37 0.65 C2 0.88 C1 1.76 C3 1.91 C11 Shortest distances between peaks (including symmetry equivalents) 1 4 0.70 3 5 2.96 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.05: Interpret restraints etc. 0.00: 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 0.00: Analyse other restraints etc. 3.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.11: Set up l.s. refinement 0.02: Generate idealized H-atoms 28.33: Structure factors and derivatives 57.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 5.41: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.13: Merge reflections for Fourier and .fcf 0.27: Fourier summations 0.27: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 10:34:11 Total CPU time: 96.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++