+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0550 started at 11:39:06 on 14-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0550 in P2(1)/n CELL 0.71073 11.5254 14.3958 20.4783 90.000 95.396 90.000 ZERR 4.00 0.0009 0.0011 0.0012 0.000 0.006 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H P CL FE PD UNIT 116 196 8 20 4 4 V = 3382.65 F(000) = 1640.0 Mu = 1.47 mm-1 Cell Wt = 3196.49 Rho = 1.569 MERG 2 OMIT -3.00 55.00 OMIT 1 2 0 OMIT -1 2 1 OMIT 0 1 3 OMIT 1 2 1 OMIT 0 0 4 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.10 0.26 0.32 ACTA BOND $H WGHT 0.02880 1.75880 L.S. 15 TEMP -153.00 FVAR 0.24740 0.64516 MOLE 1 C1 1 0.198776 0.701858 0.075119 11.00000 0.01839 0.01031 = 0.01804 0.00270 0.00031 -0.00054 C2 1 0.322036 0.701582 0.074468 11.00000 0.01739 0.01200 = 0.01274 0.00234 0.00070 0.00029 C3 1 0.348499 0.693546 0.007698 11.00000 0.02011 0.01570 = 0.01734 0.00011 0.00430 -0.00077 AFIX 43 H3 2 0.424248 0.692327 -0.006998 11.00000 -1.20000 AFIX 0 C4 1 0.241618 0.687732 -0.032592 11.00000 0.02669 0.01687 = 0.01408 -0.00177 0.00083 -0.00348 AFIX 43 H4 2 0.233303 0.680936 -0.078940 11.00000 -1.20000 AFIX 0 C5 1 0.148930 0.693870 0.008640 11.00000 0.01827 0.01515 = 0.02216 0.00252 -0.00155 -0.00334 AFIX 43 H5 2 0.068054 0.692838 -0.005542 11.00000 -1.20000 AFIX 0 C6 1 0.241714 0.931555 0.067633 11.00000 0.05649 0.01576 = 0.01919 0.00362 0.00525 0.00419 AFIX 43 H6 2 0.239963 0.937816 0.113712 11.00000 -1.20000 AFIX 0 C7 1 0.341810 0.929070 0.034501 11.00000 0.01930 0.01190 = 0.08981 -0.00025 -0.00981 -0.00295 AFIX 43 H7 2 0.420073 0.933359 0.053476 11.00000 -1.20000 AFIX 0 C8 1 0.304202 0.918893 -0.033055 11.00000 0.10360 0.01370 = 0.05765 0.00473 0.06349 0.00119 AFIX 43 H8 2 0.352599 0.915025 -0.068034 11.00000 -1.20000 AFIX 0 C9 1 0.182232 0.915621 -0.038474 11.00000 0.08786 0.01985 = 0.03091 0.00536 -0.02644 0.00007 AFIX 43 H9 2 0.133038 0.909044 -0.078103 11.00000 -1.20000 AFIX 0 C10 1 0.146101 0.923479 0.022799 11.00000 0.02592 0.01822 = 0.06407 0.00855 0.00429 0.00318 AFIX 43 H10 2 0.067284 0.923375 0.032831 11.00000 -1.20000 AFIX 0 C11 1 0.138926 0.714172 0.136595 11.00000 0.01436 0.01233 = 0.01790 0.00334 0.00075 -0.00053 AFIX 23 H11A 2 0.059986 0.739243 0.124047 11.00000 -1.20000 H11B 2 0.182231 0.761810 0.163925 11.00000 -1.20000 AFIX 0 C12 1 0.406887 0.713744 0.133624 11.00000 0.01456 0.01434 = 0.01657 -0.00077 0.00508 -0.00092 AFIX 23 H12A 2 0.376682 0.763760 0.160564 11.00000 -1.20000 H12B 2 0.480705 0.736629 0.118360 11.00000 -1.20000 AFIX 0 C13 1 0.011876 0.536443 0.136746 11.00000 0.01382 0.01843 = 0.01859 -0.00150 0.00076 -0.00490 C14 1 0.082351 0.471031 0.096114 11.00000 0.02090 0.02330 = 0.02389 -0.00654 0.00116 -0.00350 AFIX 137 H14A 2 0.130013 0.429572 0.125610 11.00000 -1.50000 H14B 2 0.133097 0.507823 0.070292 11.00000 -1.50000 H14C 2 0.028843 0.434022 0.066553 11.00000 -1.50000 AFIX 0 C15 1 -0.068457 0.595483 0.089653 11.00000 0.01550 0.02745 = 0.02423 0.00426 -0.00047 -0.00607 AFIX 137 H15A 2 -0.125096 0.555187 0.064732 11.00000 -1.50000 H15B 2 -0.021941 0.628389 0.059317 11.00000 -1.50000 H15C 2 -0.109782 0.640681 0.114750 11.00000 -1.50000 AFIX 0 C16 1 -0.068780 0.478444 0.175934 11.00000 0.01950 0.02225 = 0.02535 -0.00160 0.00088 -0.00597 AFIX 137 H16A 2 -0.119561 0.519845 0.198416 11.00000 -1.50000 H16B 2 -0.021849 0.440817 0.208401 11.00000 -1.50000 H16C 2 -0.116542 0.437556 0.146060 11.00000 -1.50000 AFIX 0 C17 1 0.058082 0.663569 0.261087 11.00000 0.01676 0.01451 = 0.01699 -0.00120 0.00231 0.00019 C18 1 0.030168 0.593017 0.313467 11.00000 0.03262 0.02400 = 0.02216 0.00212 0.01012 0.00149 AFIX 137 H18A 2 0.101166 0.559069 0.328975 11.00000 -1.50000 H18B 2 -0.028756 0.549164 0.294546 11.00000 -1.50000 H18C 2 0.000252 0.625722 0.350362 11.00000 -1.50000 AFIX 0 C19 1 0.149775 0.729730 0.294414 11.00000 0.02153 0.02574 = 0.01660 -0.00583 0.00058 -0.00166 AFIX 137 H19A 2 0.164510 0.780283 0.264225 11.00000 -1.50000 H19B 2 0.222279 0.695556 0.306164 11.00000 -1.50000 H19C 2 0.121103 0.755610 0.334141 11.00000 -1.50000 AFIX 0 C20 1 -0.052310 0.718630 0.239562 11.00000 0.01502 0.02133 = 0.02561 -0.00584 0.00283 0.00096 AFIX 137 H20A 2 -0.084486 0.744669 0.278233 11.00000 -1.50000 H20B 2 -0.109923 0.677375 0.216339 11.00000 -1.50000 H20C 2 -0.033306 0.769152 0.210312 11.00000 -1.50000 AFIX 0 C21 1 0.513792 0.527665 0.134288 11.00000 0.01740 0.01829 = 0.01906 -0.00254 0.00449 0.00556 C22 1 0.574682 0.444399 0.170296 11.00000 0.02625 0.01786 = 0.02919 -0.00207 0.00516 0.00583 AFIX 137 H22A 2 0.600855 0.400620 0.138096 11.00000 -1.50000 H22B 2 0.519864 0.413193 0.196814 11.00000 -1.50000 H22C 2 0.642041 0.466442 0.198872 11.00000 -1.50000 AFIX 0 C23 1 0.603937 0.576080 0.095393 11.00000 0.02139 0.02511 = 0.02322 -0.00056 0.00945 0.00305 AFIX 137 H23A 2 0.664905 0.603741 0.125914 11.00000 -1.50000 H23B 2 0.565564 0.624891 0.067858 11.00000 -1.50000 H23C 2 0.638905 0.530522 0.067568 11.00000 -1.50000 AFIX 0 C24 1 0.415134 0.485815 0.087605 11.00000 0.02784 0.01994 = 0.02483 -0.00486 0.00418 0.00222 AFIX 137 H24A 2 0.371773 0.535880 0.063834 11.00000 -1.50000 H24B 2 0.362349 0.450398 0.113016 11.00000 -1.50000 H24C 2 0.448415 0.444499 0.056217 11.00000 -1.50000 AFIX 0 C25 1 0.554026 0.672705 0.250700 11.00000 0.01601 0.01829 = 0.01803 -0.00071 0.00057 -0.00072 C26 1 0.486145 0.703382 0.308346 11.00000 0.01996 0.02459 = 0.01929 -0.00401 -0.00229 0.00009 AFIX 137 H26A 2 0.455880 0.648487 0.329402 11.00000 -1.50000 H26B 2 0.421112 0.743478 0.291947 11.00000 -1.50000 H26C 2 0.538270 0.737692 0.340352 11.00000 -1.50000 AFIX 0 C27 1 0.654886 0.609082 0.276372 11.00000 0.01733 0.02641 = 0.02750 -0.00067 -0.00341 0.00105 AFIX 137 H27A 2 0.701281 0.592895 0.240294 11.00000 -1.50000 H27B 2 0.623569 0.552325 0.294470 11.00000 -1.50000 H27C 2 0.704264 0.641369 0.310759 11.00000 -1.50000 AFIX 0 C28 1 0.609632 0.759898 0.222867 11.00000 0.01988 0.02215 = 0.02533 -0.00288 0.00073 -0.00517 AFIX 137 H28A 2 0.669943 0.784241 0.255306 11.00000 -1.50000 H28B 2 0.549553 0.807332 0.212973 11.00000 -1.50000 H28C 2 0.644723 0.743513 0.182643 11.00000 -1.50000 AFIX 0 P1 3 0.123597 0.609753 0.188250 11.00000 0.01360 0.01251 = 0.01503 0.00053 0.00231 -0.00036 P2 3 0.443115 0.613488 0.188515 11.00000 0.01314 0.01379 = 0.01490 -0.00044 0.00194 0.00076 CL1 4 0.171566 0.413686 0.262990 11.00000 0.02048 0.01610 = 0.02853 0.00570 0.00385 -0.00162 CL2 4 0.437414 0.462247 0.302795 11.00000 0.01998 0.02166 = 0.02407 0.00715 -0.00139 0.00211 FE1 5 0.250350 0.809129 0.018287 11.00000 0.02004 0.01459 = 0.01419 0.00186 0.00224 -0.00083 PD1 6 0.292754 0.533401 0.230958 11.00000 0.01364 0.01221 = 0.01530 0.00145 0.00237 0.00040 MOLE 2 PART 1 C31 1 0.763976 0.843210 0.009032 21.00000 0.02664 0.01224 = 0.03603 0.01632 0.00031 0.00241 AFIX 13 H31 2 0.775167 0.904889 -0.011944 21.00000 -1.20000 AFIX 0 CL31 4 0.613834 0.824688 0.008203 21.00000 0.01971 0.03137 = 0.06810 0.00940 0.00761 -0.00115 CL32 4 0.835077 0.847544 0.088175 21.00000 0.04453 0.03808 = 0.02805 0.00259 -0.00307 0.01224 CL33 4 0.822619 0.758981 -0.039693 21.00000 0.05612 0.06088 = 0.03730 -0.00475 -0.01029 0.02817 PART 2 SAME C31 > CL33 C36 1 0.764303 0.857190 0.005044 -21.00000 0.01452 0.03850 = 0.02682 0.00292 0.00198 -0.01242 AFIX 13 H36 2 0.761394 0.921270 -0.013890 -21.00000 -1.20000 AFIX 0 CL36 4 0.623628 0.814930 0.013714 -21.00000 0.05307 0.11449 = 0.11688 0.04836 0.01078 -0.03150 CL37 4 0.838998 0.855988 0.083973 -21.00000 0.09848 0.03156 = 0.05378 0.01015 -0.02612 0.01672 CL38 4 0.838258 0.780296 -0.043543 -21.00000 0.05243 0.15427 = 0.03569 -0.00320 0.01282 0.05801 HKLF 4 Covalent radii and connectivity table for 04src0550 in P2(1)/n C 0.770 H 0.320 P 1.100 CL 0.990 FE 1.240 PD 1.380 C1 - C2 C5 C11 Fe1 C2 - C1 C3 C12 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C10 C7 Fe1 C7 - C6 C8 Fe1 C8 - C9 C7 Fe1 C9 - C10 C8 Fe1 C10 - C9 C6 Fe1 C11 - C1 P1 C12 - C2 P2 C13 - C15 C16 C14 P1 C14 - C13 C15 - C13 C16 - C13 C17 - C20 C18 C19 P1 C18 - C17 C19 - C17 C20 - C17 C21 - C23 C24 C22 P2 C22 - C21 C23 - C21 C24 - C21 C25 - C27 C26 C28 P2 C26 - C25 C27 - C25 C28 - C25 P1 - C11 C17 C13 Pd1 P2 - C12 C21 C25 Pd1 Cl1 - Pd1 Cl2 - Pd1 Fe1 - C8 C5 C4 C7 C3 C9 C6 C10 C1 C2 Pd1 - P2 P1 Cl1 Cl2 C31_a - Cl33_a Cl32_a Cl31_a Cl31_a - C31_a Cl32_a - C31_a Cl33_a - C31_a C36_b - Cl36_b Cl37_b Cl38_b Cl36_b - C36_b Cl37_b - C36_b Cl38_b - C36_b 33765 Reflections read, of which 746 rejected -14 =< h =< 12, -17 =< k =< 18, -26 =< l =< 26, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 7725 Unique reflections, of which 0 suppressed R(int) = 0.0569 R(sigma) = 0.0638 Friedel opposites merged Maximum memory for data reduction = 4559 / 76228 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 = 5740 / 503475 wR2 = 0.0765 before cycle 1 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.004 OSF 2 0.64526 0.04146 0.002 FVAR 2 Mean shift/esd = 0.002 Maximum = 0.028 for U22 Pd1 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl37_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 2 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.002 OSF 2 0.64524 0.04145 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.010 for U22 Pd1 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 3 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 -0.001 OSF 2 0.64524 0.04147 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H36_b Max. dU = 0.000 for Cl37_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 4 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.001 OSF 2 0.64525 0.04146 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for y Pd1 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl37_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 5 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64536 0.04147 0.003 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for FVAR 2 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl36_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 6 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64517 0.04146 -0.005 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.005 for FVAR 2 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl36_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 7 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64530 0.04147 0.003 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for y Cl38_b Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 8 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64522 0.04147 -0.002 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.002 for U13 Cl33_a Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 9 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.001 OSF 2 0.64530 0.04147 0.002 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for x Cl38_b Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 10 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64526 0.04146 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for y Pd1 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 11 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64525 0.04148 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for y Pd1 Max. shift = 0.000 A for H36_b Max. dU = 0.000 for Cl37_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 12 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64538 0.04147 0.003 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for FVAR 2 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl36_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 13 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.000 OSF 2 0.64528 0.04146 -0.002 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.003 for x Cl38_b Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl38_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 14 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 0.001 OSF 2 0.64532 0.04147 0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for U13 Cl33_a Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl36_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 5740 / 503475 wR2 = 0.0765 before cycle 15 for 7725 data and 392 / 392 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24740 0.00022 -0.001 OSF 2 0.64519 0.04146 -0.003 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.003 for FVAR 2 Max. shift = 0.000 A for Cl38_b Max. dU = 0.000 for Cl36_b Largest correlation matrix elements 0.932 y Cl38_b / FVAR 2 0.819 y Cl38_b / U22 Cl31_a 0.785 y Cl38_b / U22 Cl33_a 0.916 U22 Cl33_a / FVAR 2 0.816 U22 Cl33_a / U22 Cl31_a -0.773 U12 Cl38_b / x Cl38_b -0.884 U11 C36_b / U11 C31_a -0.815 z Cl38_b / z Cl33_a -0.752 y Cl38_b / y Cl36_b 0.884 U22 Cl31_a / FVAR 2 0.812 U23 Cl38_b / z Cl33_a -0.745 y Cl36_b / U22 Cl33_a -0.881 U23 Cl38_b / z Cl38_b -0.807 y Cl36_b / FVAR 2 -0.733 U12 Cl37_b / U12 Cl32_a -0.864 x Cl37_b / x Cl32_a 0.806 U22 C36_b / y C31_a 0.721 x Cl36_b / FVAR 2 -0.852 U13 C36_b / U13 C31_a -0.791 x C36_b / x C31_a 0.721 U22 Cl38_b / y Cl33_a -0.850 U33 C36_b / U33 C31_a -0.786 U22 Cl36_b / y Cl31_a -0.719 z C36_b / z C31_a Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.4242 0.6923 -0.0070 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.2333 0.6809 -0.0789 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.0681 0.6928 -0.0055 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.2400 0.9378 0.1137 43 0.950 0.000 C6 C10 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.4201 0.9334 0.0535 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.3526 0.9150 -0.0680 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.1330 0.9090 -0.0781 43 0.950 0.000 C9 C10 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.0673 0.9234 0.0328 43 0.950 0.000 C10 C9 C6 H11A 0.0600 0.7392 0.1240 23 0.990 0.000 C11 C1 P1 H11B 0.1822 0.7618 0.1639 23 0.990 0.000 C11 C1 P1 H12A 0.3767 0.7638 0.1606 23 0.990 0.000 C12 C2 P2 H12B 0.4807 0.7366 0.1184 23 0.990 0.000 C12 C2 P2 H14A 0.1300 0.4296 0.1256 137 0.980 0.000 C14 C13 H14A H14B 0.1331 0.5078 0.0703 137 0.980 0.000 C14 C13 H14A H14C 0.0288 0.4340 0.0666 137 0.980 0.000 C14 C13 H14A H15A -0.1251 0.5552 0.0647 137 0.980 0.000 C15 C13 H15A H15B -0.0219 0.6284 0.0593 137 0.980 0.000 C15 C13 H15A H15C -0.1098 0.6407 0.1148 137 0.980 0.000 C15 C13 H15A H16A -0.1196 0.5198 0.1984 137 0.980 0.000 C16 C13 H16A H16B -0.0218 0.4408 0.2084 137 0.980 0.000 C16 C13 H16A H16C -0.1165 0.4376 0.1461 137 0.980 0.000 C16 C13 H16A H18A 0.1012 0.5591 0.3290 137 0.980 0.000 C18 C17 H18A H18B -0.0288 0.5492 0.2945 137 0.980 0.000 C18 C17 H18A H18C 0.0003 0.6257 0.3504 137 0.980 0.000 C18 C17 H18A H19A 0.1645 0.7803 0.2642 137 0.980 0.000 C19 C17 H19A H19B 0.2223 0.6956 0.3062 137 0.980 0.000 C19 C17 H19A H19C 0.1211 0.7556 0.3341 137 0.980 0.000 C19 C17 H19A H20A -0.0845 0.7447 0.2782 137 0.980 0.000 C20 C17 H20A H20B -0.1099 0.6774 0.2163 137 0.980 0.000 C20 C17 H20A H20C -0.0333 0.7692 0.2103 137 0.980 0.000 C20 C17 H20A H22A 0.6009 0.4006 0.1381 137 0.980 0.000 C22 C21 H22A H22B 0.5199 0.4132 0.1968 137 0.980 0.000 C22 C21 H22A H22C 0.6420 0.4664 0.1989 137 0.980 0.000 C22 C21 H22A H23A 0.6649 0.6037 0.1259 137 0.980 0.000 C23 C21 H23A H23B 0.5656 0.6249 0.0679 137 0.980 0.000 C23 C21 H23A H23C 0.6389 0.5305 0.0676 137 0.980 0.000 C23 C21 H23A H24A 0.3718 0.5359 0.0638 137 0.980 0.000 C24 C21 H24A H24B 0.3623 0.4504 0.1130 137 0.980 0.000 C24 C21 H24A H24C 0.4484 0.4445 0.0562 137 0.980 0.000 C24 C21 H24A H26A 0.4559 0.6485 0.3294 137 0.980 0.000 C26 C25 H26A H26B 0.4211 0.7435 0.2919 137 0.980 0.000 C26 C25 H26A H26C 0.5383 0.7377 0.3404 137 0.980 0.000 C26 C25 H26A H27A 0.7013 0.5929 0.2403 137 0.980 0.000 C27 C25 H27A H27B 0.6236 0.5523 0.2945 137 0.980 0.000 C27 C25 H27A H27C 0.7043 0.6414 0.3108 137 0.980 0.000 C27 C25 H27A H28A 0.6699 0.7842 0.2553 137 0.980 0.000 C28 C25 H28A H28B 0.5496 0.8073 0.2130 137 0.980 0.000 C28 C25 H28A H28C 0.6447 0.7435 0.1826 137 0.980 0.000 C28 C25 H28A H31 0.7752 0.9049 -0.0119 13 1.000 0.000 C31_a Cl33_a Cl32_a Cl31_a H36 0.7614 0.9213 -0.0139 13 1.000 0.000 C36_b Cl36_b Cl37_b Cl38_b 04src0550 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.19878 0.70186 0.07512 1.00000 0.01839 0.01031 0.01804 0.00270 0.00032 -0.00054 0.01567 0.00501 0.00025 0.00017 0.00014 0.00000 0.00165 0.00130 0.00161 0.00118 0.00132 0.00110 0.00063 C2 0.32204 0.70158 0.07447 1.00000 0.01739 0.01200 0.01274 0.00234 0.00070 0.00029 0.01409 0.00496 0.00025 0.00017 0.00014 0.00000 0.00162 0.00130 0.00149 0.00115 0.00126 0.00110 0.00061 C3 0.34850 0.69355 0.00770 1.00000 0.02011 0.01570 0.01734 0.00011 0.00430 -0.00076 0.01756 0.00514 0.00026 0.00018 0.00014 0.00000 0.00169 0.00140 0.00160 0.00124 0.00134 0.00115 0.00065 H3 0.42425 0.69233 -0.00700 1.00000 0.02107 0.00000 0.00000 C4 0.24162 0.68773 -0.03259 1.00000 0.02669 0.01687 0.01409 -0.00177 0.00083 -0.00348 0.01928 0.00513 0.00026 0.00018 0.00015 0.00000 0.00184 0.00141 0.00157 0.00123 0.00139 0.00122 0.00067 H4 0.23330 0.68094 -0.07894 1.00000 0.02314 0.00000 0.00000 C5 0.14893 0.69387 0.00864 1.00000 0.01827 0.01515 0.02217 0.00252 -0.00155 -0.00334 0.01875 0.00520 0.00027 0.00018 0.00014 0.00000 0.00166 0.00139 0.00171 0.00125 0.00137 0.00115 0.00066 H5 0.06805 0.69284 -0.00554 1.00000 0.02250 0.00000 0.00000 C6 0.24171 0.93156 0.06763 1.00000 0.05649 0.01576 0.01920 0.00362 0.00526 0.00420 0.03037 0.00625 0.00033 0.00020 0.00016 0.00000 0.00257 0.00149 0.00179 0.00136 0.00179 0.00153 0.00083 H6 0.23996 0.93782 0.11371 1.00000 0.03645 0.00000 0.00000 C7 0.34181 0.92907 0.03450 1.00000 0.01931 0.01191 0.08982 -0.00025 -0.00981 -0.00295 0.04129 0.00647 0.00030 0.00020 0.00023 0.00000 0.00196 0.00152 0.00349 0.00184 0.00207 0.00130 0.00107 H7 0.42007 0.93336 0.05348 1.00000 0.04955 0.00000 0.00000 C8 0.30420 0.91889 -0.03306 1.00000 0.10361 0.01370 0.05765 0.00473 0.06348 0.00120 0.05478 0.00899 0.00045 0.00022 0.00022 0.00000 0.00394 0.00169 0.00293 0.00180 0.00289 0.00197 0.00137 H8 0.35260 0.91503 -0.06803 1.00000 0.06574 0.00000 0.00000 C9 0.18223 0.91562 -0.03847 1.00000 0.08784 0.01986 0.03091 0.00536 -0.02644 0.00007 0.04823 0.00681 0.00043 0.00022 0.00019 0.00000 0.00358 0.00176 0.00232 0.00165 0.00236 0.00193 0.00115 H9 0.13304 0.90904 -0.07810 1.00000 0.05788 0.00000 0.00000 C10 0.14610 0.92348 0.02280 1.00000 0.02592 0.01822 0.06407 0.00854 0.00429 0.00318 0.03607 0.00666 0.00031 0.00021 0.00020 0.00000 0.00204 0.00163 0.00284 0.00175 0.00199 0.00137 0.00091 H10 0.06728 0.92338 0.03283 1.00000 0.04328 0.00000 0.00000 C11 0.13893 0.71417 0.13660 1.00000 0.01436 0.01233 0.01790 0.00334 0.00075 -0.00053 0.01491 0.00506 0.00025 0.00017 0.00014 0.00000 0.00156 0.00129 0.00158 0.00120 0.00127 0.00109 0.00061 H11A 0.05998 0.73924 0.12405 1.00000 0.01789 0.00000 0.00000 H11B 0.18223 0.76181 0.16393 1.00000 0.01789 0.00000 0.00000 C12 0.40689 0.71374 0.13362 1.00000 0.01456 0.01434 0.01657 -0.00077 0.00508 -0.00092 0.01493 0.00492 0.00024 0.00018 0.00014 0.00000 0.00156 0.00134 0.00156 0.00120 0.00129 0.00110 0.00062 H12A 0.37668 0.76376 0.16056 1.00000 0.01792 0.00000 0.00000 H12B 0.48071 0.73663 0.11836 1.00000 0.01792 0.00000 0.00000 C13 0.01188 0.53644 0.13675 1.00000 0.01382 0.01843 0.01859 -0.00150 0.00076 -0.00490 0.01699 0.00492 0.00024 0.00018 0.00014 0.00000 0.00156 0.00140 0.00159 0.00127 0.00127 0.00115 0.00063 C14 0.08235 0.47103 0.09611 1.00000 0.02090 0.02330 0.02389 -0.00654 0.00116 -0.00350 0.02276 0.00528 0.00026 0.00020 0.00015 0.00000 0.00174 0.00154 0.00174 0.00138 0.00141 0.00128 0.00069 H14A 0.13001 0.42957 0.12561 1.00000 0.03414 0.00000 0.00000 H14B 0.13310 0.50782 0.07029 1.00000 0.03414 0.00000 0.00000 H14C 0.02884 0.43402 0.06655 1.00000 0.03414 0.00000 0.00000 C15 -0.06846 0.59548 0.08965 1.00000 0.01550 0.02745 0.02423 0.00426 -0.00047 -0.00607 0.02254 0.00531 0.00025 0.00020 0.00015 0.00000 0.00169 0.00163 0.00180 0.00141 0.00139 0.00125 0.00070 H15A -0.12510 0.55519 0.06473 1.00000 0.03381 0.00000 0.00000 H15B -0.02194 0.62839 0.05932 1.00000 0.03381 0.00000 0.00000 H15C -0.10978 0.64068 0.11475 1.00000 0.03381 0.00000 0.00000 C16 -0.06878 0.47844 0.17593 1.00000 0.01950 0.02225 0.02535 -0.00160 0.00088 -0.00597 0.02244 0.00523 0.00026 0.00019 0.00015 0.00000 0.00172 0.00157 0.00178 0.00135 0.00141 0.00124 0.00070 H16A -0.11956 0.51985 0.19842 1.00000 0.03366 0.00000 0.00000 H16B -0.02185 0.44082 0.20840 1.00000 0.03366 0.00000 0.00000 H16C -0.11654 0.43756 0.14606 1.00000 0.03366 0.00000 0.00000 C17 0.05808 0.66357 0.26109 1.00000 0.01677 0.01451 0.01700 -0.00120 0.00231 0.00019 0.01605 0.00496 0.00024 0.00018 0.00014 0.00000 0.00161 0.00136 0.00159 0.00122 0.00128 0.00112 0.00063 C18 0.03017 0.59302 0.31347 1.00000 0.03262 0.02400 0.02216 0.00213 0.01011 0.00149 0.02578 0.00582 0.00028 0.00020 0.00015 0.00000 0.00199 0.00160 0.00177 0.00140 0.00151 0.00137 0.00074 H18A 0.10117 0.55907 0.32898 1.00000 0.03868 0.00000 0.00000 H18B -0.02876 0.54916 0.29455 1.00000 0.03868 0.00000 0.00000 H18C 0.00025 0.62572 0.35036 1.00000 0.03868 0.00000 0.00000 C19 0.14978 0.72973 0.29441 1.00000 0.02153 0.02574 0.01660 -0.00583 0.00058 -0.00166 0.02137 0.00496 0.00026 0.00020 0.00014 0.00000 0.00175 0.00158 0.00165 0.00135 0.00138 0.00128 0.00068 H19A 0.16451 0.78028 0.26423 1.00000 0.03205 0.00000 0.00000 H19B 0.22228 0.69556 0.30616 1.00000 0.03205 0.00000 0.00000 H19C 0.12110 0.75561 0.33414 1.00000 0.03205 0.00000 0.00000 C20 -0.05231 0.71863 0.23956 1.00000 0.01502 0.02133 0.02561 -0.00584 0.00283 0.00096 0.02059 0.00527 0.00024 0.00019 0.00015 0.00000 0.00164 0.00151 0.00177 0.00135 0.00138 0.00118 0.00068 H20A -0.08449 0.74467 0.27823 1.00000 0.03089 0.00000 0.00000 H20B -0.10992 0.67738 0.21634 1.00000 0.03089 0.00000 0.00000 H20C -0.03331 0.76915 0.21031 1.00000 0.03089 0.00000 0.00000 C21 0.51379 0.52767 0.13429 1.00000 0.01740 0.01829 0.01906 -0.00254 0.00449 0.00556 0.01807 0.00521 0.00025 0.00019 0.00014 0.00000 0.00163 0.00142 0.00161 0.00127 0.00131 0.00117 0.00064 C22 0.57468 0.44440 0.17030 1.00000 0.02626 0.01787 0.02919 -0.00207 0.00516 0.00583 0.02428 0.00568 0.00027 0.00019 0.00016 0.00000 0.00188 0.00147 0.00187 0.00135 0.00151 0.00125 0.00073 H22A 0.60086 0.40062 0.13810 1.00000 0.03641 0.00000 0.00000 H22B 0.51986 0.41319 0.19681 1.00000 0.03641 0.00000 0.00000 H22C 0.64204 0.46644 0.19887 1.00000 0.03641 0.00000 0.00000 C23 0.60394 0.57608 0.09539 1.00000 0.02138 0.02511 0.02322 -0.00056 0.00945 0.00305 0.02277 0.00559 0.00026 0.00020 0.00015 0.00000 0.00177 0.00158 0.00177 0.00139 0.00142 0.00129 0.00070 H23A 0.66491 0.60374 0.12591 1.00000 0.03416 0.00000 0.00000 H23B 0.56556 0.62489 0.06786 1.00000 0.03416 0.00000 0.00000 H23C 0.63891 0.53052 0.06757 1.00000 0.03416 0.00000 0.00000 C24 0.41513 0.48581 0.08760 1.00000 0.02784 0.01995 0.02483 -0.00486 0.00418 0.00222 0.02410 0.00527 0.00027 0.00020 0.00015 0.00000 0.00186 0.00154 0.00180 0.00135 0.00149 0.00128 0.00072 H24A 0.37177 0.53588 0.06383 1.00000 0.03615 0.00000 0.00000 H24B 0.36235 0.45040 0.11302 1.00000 0.03615 0.00000 0.00000 H24C 0.44841 0.44450 0.05622 1.00000 0.03615 0.00000 0.00000 C25 0.55403 0.67271 0.25070 1.00000 0.01601 0.01829 0.01803 -0.00071 0.00056 -0.00072 0.01751 0.00506 0.00025 0.00019 0.00014 0.00000 0.00163 0.00143 0.00161 0.00126 0.00130 0.00116 0.00064 C26 0.48614 0.70338 0.30835 1.00000 0.01996 0.02459 0.01929 -0.00401 -0.00228 0.00009 0.02154 0.00528 0.00026 0.00020 0.00015 0.00000 0.00174 0.00157 0.00168 0.00133 0.00139 0.00126 0.00069 H26A 0.45588 0.64849 0.32940 1.00000 0.03231 0.00000 0.00000 H26B 0.42111 0.74348 0.29195 1.00000 0.03231 0.00000 0.00000 H26C 0.53827 0.73769 0.34035 1.00000 0.03231 0.00000 0.00000 C27 0.65489 0.60908 0.27637 1.00000 0.01733 0.02641 0.02750 -0.00068 -0.00341 0.00106 0.02410 0.00543 0.00026 0.00020 0.00015 0.00000 0.00173 0.00163 0.00185 0.00142 0.00143 0.00128 0.00072 H27A 0.70128 0.59290 0.24029 1.00000 0.03615 0.00000 0.00000 H27B 0.62357 0.55232 0.29447 1.00000 0.03615 0.00000 0.00000 H27C 0.70426 0.64137 0.31076 1.00000 0.03615 0.00000 0.00000 C28 0.60963 0.75990 0.22287 1.00000 0.01988 0.02215 0.02533 -0.00288 0.00073 -0.00517 0.02254 0.00527 0.00026 0.00019 0.00015 0.00000 0.00170 0.00153 0.00179 0.00138 0.00143 0.00126 0.00069 H28A 0.66994 0.78424 0.25531 1.00000 0.03381 0.00000 0.00000 H28B 0.54955 0.80733 0.21297 1.00000 0.03381 0.00000 0.00000 H28C 0.64472 0.74351 0.18264 1.00000 0.03381 0.00000 0.00000 P1 0.12360 0.60975 0.18825 1.00000 0.01360 0.01251 0.01503 0.00053 0.00231 -0.00036 0.01365 0.00131 0.00006 0.00005 0.00004 0.00000 0.00040 0.00033 0.00040 0.00030 0.00032 0.00028 0.00016 P2 0.44312 0.61349 0.18852 1.00000 0.01314 0.01379 0.01490 -0.00044 0.00195 0.00076 0.01391 0.00131 0.00006 0.00005 0.00004 0.00000 0.00040 0.00034 0.00040 0.00030 0.00032 0.00028 0.00016 Cl1 0.17157 0.41369 0.26299 1.00000 0.02048 0.01610 0.02853 0.00570 0.00385 -0.00162 0.02161 0.00132 0.00006 0.00005 0.00004 0.00000 0.00041 0.00034 0.00043 0.00031 0.00033 0.00028 0.00017 Cl2 0.43741 0.46225 0.30279 1.00000 0.01998 0.02166 0.02407 0.00715 -0.00139 0.00211 0.02212 0.00133 0.00006 0.00005 0.00004 0.00000 0.00041 0.00036 0.00041 0.00032 0.00033 0.00029 0.00017 Fe1 0.25035 0.80913 0.01829 1.00000 0.02004 0.01459 0.01419 0.00186 0.00224 -0.00083 0.01624 0.00074 0.00004 0.00003 0.00002 0.00000 0.00024 0.00020 0.00023 0.00017 0.00019 0.00016 0.00011 Pd1 0.29275 0.53340 0.23096 1.00000 0.01364 0.01221 0.01530 0.00145 0.00237 0.00040 0.01365 0.00038 0.00002 0.00001 0.00001 0.00000 0.00013 0.00011 0.00013 0.00009 0.00009 0.00008 0.00007 C31_a 0.76398 0.84321 0.00903 0.64519 0.02665 0.01224 0.03604 0.01632 0.00030 0.00240 0.02515 0.01842 0.00081 0.00099 0.00057 0.04146 0.00659 0.00353 0.00703 0.00362 0.00480 0.00323 0.00358 H31_a 0.77517 0.90489 -0.01195 0.64519 0.03017 0.04146 0.00000 Cl31_a 0.61383 0.82469 0.00820 0.64519 0.01971 0.03137 0.06810 0.00940 0.00761 -0.00115 0.03951 0.00834 0.00041 0.00031 0.00029 0.04146 0.00177 0.00230 0.00243 0.00139 0.00130 0.00122 0.00167 Cl32_a 0.83508 0.84754 0.08817 0.64519 0.04453 0.03808 0.02805 0.00258 -0.00306 0.01223 0.03730 0.01253 0.00049 0.00062 0.00035 0.04146 0.00273 0.00245 0.00206 0.00160 0.00167 0.00147 0.00133 Cl33_a 0.82262 0.75898 -0.03969 0.64519 0.05612 0.06088 0.03730 -0.00475 -0.01029 0.02817 0.05236 0.01432 0.00076 0.00046 0.00040 0.04146 0.00260 0.00318 0.00232 0.00118 0.00217 0.00150 0.00138 C36_b 0.76430 0.85719 0.00505 0.35481 0.01451 0.03848 0.02683 0.00290 0.00200 -0.01242 0.02660 0.03206 0.00132 0.00204 0.00093 0.04146 0.01069 0.01229 0.01141 0.00822 0.00806 0.00713 0.00668 H36_b 0.76139 0.92127 -0.01389 0.35481 0.03193 0.04146 0.00000 Cl36_b 0.62363 0.81493 0.01372 0.35481 0.05307 0.11448 0.11688 0.04837 0.01078 -0.03150 0.09464 0.02284 0.00138 0.00126 0.00082 0.04146 0.00556 0.00862 0.00728 0.00652 0.00458 0.00457 0.00494 Cl37_b 0.83900 0.85599 0.08398 0.35481 0.09848 0.03155 0.05379 0.01015 -0.02613 0.01671 0.06338 0.02889 0.00127 0.00135 0.00073 0.04146 0.00833 0.00340 0.00602 0.00324 0.00488 0.00372 0.00407 Cl38_b 0.83826 0.78030 -0.04354 0.35481 0.05244 0.15426 0.03569 -0.00321 0.01281 0.05801 0.08025 0.04960 0.00189 0.00243 0.00084 0.04146 0.00481 0.01117 0.00324 0.00647 0.00332 0.00688 0.00440 Final Structure Factor Calculation for 04src0550 in P2(1)/n Total number of l.s. parameters = 392 Maximum vector length = 511 Memory required = 5348 / 25039 wR2 = 0.0765 before cycle 16 for 7725 data and 0 / 392 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.013; Restrained GooF = 1.013 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0288 * P )^2 + 1.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0366 for 5708 Fo > 4sig(Fo) and 0.0651 for all 7725 data wR2 = 0.0765, GooF = S = 1.013, Restrained GooF = 1.013 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 49.00 for hydrogen atoms Principal mean square atomic displacements U 0.0203 0.0172 0.0095 C1 0.0176 0.0147 0.0100 C2 0.0215 0.0161 0.0151 C3 0.0279 0.0170 0.0129 C4 0.0261 0.0172 0.0130 C5 0.0569 0.0208 0.0134 C6 0.0945 0.0187 0.0107 C7 0.1364 0.0174 0.0106 C8 0.1056 0.0244 0.0147 C9 0.0657 0.0266 0.0160 C10 0.0197 0.0143 0.0107 C11 0.0193 0.0141 0.0114 C12 0.0217 0.0187 0.0106 C13 0.0303 0.0224 0.0155 C14 0.0332 0.0215 0.0130 C15 0.0270 0.0257 0.0146 C16 0.0178 0.0165 0.0139 C17 0.0363 0.0238 0.0172 C18 0.0286 0.0219 0.0135 C19 0.0297 0.0180 0.0141 C20 0.0234 0.0206 0.0102 C21 0.0306 0.0282 0.0140 C22 0.0296 0.0252 0.0135 C23 0.0285 0.0278 0.0160 C24 0.0189 0.0182 0.0154 C25 0.0277 0.0220 0.0150 C26 0.0308 0.0262 0.0153 C27 0.0274 0.0251 0.0152 C28 0.0155 0.0134 0.0121 P1 0.0151 0.0143 0.0123 P2 0.0308 0.0210 0.0130 Cl1 0.0305 0.0221 0.0138 Cl2 0.0202 0.0163 0.0123 Fe1 0.0162 0.0131 0.0116 Pd1 0.0447 0.0270 0.0037 C31_a 0.0704 0.0296 0.0186 Cl31_a 0.0549 0.0340 0.0230 Cl32_a 0.0918 0.0393 0.0260 Cl33_a 0.0445 0.0264 0.0090 C36_b 0.1699 0.0841 0.0299 Cl36_b 0.1208 0.0511 0.0182 Cl37_b 0.1807 0.0415 0.0186 Cl38_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.039 0.058 0.079 0.103 0.130 0.162 0.204 0.274 1.000 Number in group 772. 809. 736. 789. 775. 754. 772. 775. 771. 772. GooF 0.857 0.998 0.975 1.008 1.126 1.093 1.013 1.047 0.998 0.994 K 1.231 0.970 0.893 0.956 0.955 0.972 0.990 0.997 1.016 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 793. 771. 759. 786. 754. 774. 783. 764. 769. 772. GooF 0.954 0.914 0.913 0.975 0.960 1.001 0.996 0.999 0.960 1.377 K 0.962 0.990 1.003 1.006 1.014 1.011 1.011 1.015 1.016 0.990 R1 0.159 0.144 0.115 0.102 0.074 0.058 0.041 0.032 0.024 0.021 Recommended weighting scheme: WGHT 0.0288 1.7431 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) -4 4 3 1019.33 1396.37 5.69 0.117 2.18 0 4 4 1112.35 1480.18 5.25 0.121 2.94 3 2 5 282.82 98.50 5.14 0.031 2.50 -6 6 10 566.41 891.16 4.99 0.094 1.25 0 2 4 4505.25 3736.65 4.96 0.192 4.16 0 4 7 241.46 95.66 4.94 0.031 2.26 -3 1 7 798.33 554.35 4.83 0.074 2.40 -4 3 7 463.67 738.74 4.70 0.085 1.96 -4 5 6 745.00 975.47 4.54 0.098 1.80 4 3 1 3287.51 3948.50 4.45 0.198 2.42 2 2 0 3925.39 3381.51 3.95 0.183 4.49 4 7 11 699.83 1065.27 3.91 0.103 1.21 -12 5 16 1240.37 2856.77 3.87 0.168 0.77 4 1 6 2180.09 1699.60 3.68 0.130 2.07 3 1 7 166.47 43.67 3.65 0.021 2.19 -1 1 4 2920.37 3389.45 3.65 0.183 4.58 -9 10 11 1276.89 2081.04 3.61 0.143 0.87 -11 1 18 5618.52 4215.82 3.50 0.204 0.80 9 9 11 607.10 1373.99 3.42 0.117 0.85 -10 2 6 2367.85 3218.85 3.41 0.178 1.11 -5 8 3 46.65 134.94 3.41 0.037 1.40 1 5 2 856.71 1054.36 3.41 0.102 2.68 4 1 2 486.34 313.15 3.40 0.056 2.65 -2 2 3 3213.65 3683.54 3.38 0.191 3.88 -5 3 4 2131.63 1813.32 3.38 0.134 1.98 0 1 4 1507.68 1280.40 3.34 0.113 4.80 0 2 8 2733.19 2370.97 3.32 0.153 2.40 -2 10 8 996.56 1449.97 3.16 0.120 1.24 5 4 3 2390.84 2755.65 3.15 0.165 1.82 4 3 5 3252.45 2837.33 3.15 0.167 2.04 12 10 3 407.36 1052.77 3.13 0.102 0.78 -2 0 8 326.42 205.56 3.11 0.045 2.41 4 3 3 148.19 246.21 3.11 0.049 2.26 5 15 8 891.90 1608.95 3.09 0.126 0.83 -9 10 6 932.69 1288.95 3.06 0.113 0.94 3 1 0 4304.59 4823.35 3.05 0.218 3.70 -2 5 6 6811.36 6070.98 3.04 0.245 2.09 0 17 5 -148.91 211.42 3.03 0.046 0.83 4 5 4 6475.78 7210.19 3.00 0.267 1.85 0 0 6 981.68 1191.08 3.00 0.109 3.40 0 14 7 381.53 631.27 3.00 0.079 0.97 -6 9 17 1826.67 2790.68 2.97 0.166 0.88 1 0 7 3751.81 3299.11 2.96 0.181 2.76 -14 5 4 659.39 1171.97 2.94 0.108 0.79 7 7 16 485.44 1077.42 2.92 0.103 0.87 1 10 10 3040.41 2615.31 2.91 0.161 1.16 2 2 1 2957.46 2633.46 2.89 0.161 4.32 -8 11 16 2370.96 3137.30 2.87 0.176 0.79 0 5 3 102.86 172.33 2.86 0.041 2.65 1 8 16 408.92 709.35 2.86 0.084 1.03 Bond lengths and angles C1 - Distance Angles C2 1.4219 (0.0040) C5 1.4316 (0.0041) 107.63 (0.26) C11 1.5018 (0.0038) 123.11 (0.26) 129.18 (0.27) Fe1 2.0549 (0.0026) 69.78 (0.15) 68.49 (0.15) 124.48 (0.18) C1 - C2 C5 C11 C2 - Distance Angles C1 1.4219 (0.0040) C3 1.4333 (0.0039) 108.16 (0.26) C12 1.4939 (0.0040) 124.78 (0.25) 126.96 (0.26) Fe1 2.0553 (0.0026) 69.74 (0.15) 68.73 (0.15) 124.31 (0.18) C2 - C1 C3 C12 C3 - Distance Angles C4 1.4192 (0.0041) C2 1.4333 (0.0039) 107.96 (0.25) Fe1 2.0350 (0.0027) 69.47 (0.16) 70.25 (0.15) H3 0.9500 126.02 126.02 125.84 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4192 (0.0041) C5 1.4253 (0.0040) 108.05 (0.25) Fe1 2.0323 (0.0027) 69.68 (0.16) 69.31 (0.15) H4 0.9500 125.97 125.97 126.60 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4253 (0.0040) C1 1.4316 (0.0041) 108.19 (0.26) Fe1 2.0286 (0.0027) 69.59 (0.15) 70.47 (0.16) H5 0.9500 125.90 125.90 125.62 C5 - C4 C1 Fe1 C6 - Distance Angles C10 1.3713 (0.0048) C7 1.3928 (0.0049) 108.78 (0.32) Fe1 2.0387 (0.0031) 70.64 (0.19) 69.82 (0.18) H6 0.9500 125.61 125.61 125.52 C6 - C10 C7 Fe1 C7 - Distance Angles C6 1.3928 (0.0049) C8 1.4179 (0.0056) 106.66 (0.32) Fe1 2.0339 (0.0031) 70.19 (0.18) 69.32 (0.19) H7 0.9500 126.67 126.67 125.42 C7 - C6 C8 Fe1 C8 - Distance Angles C9 1.4005 (0.0059) C7 1.4179 (0.0056) 107.05 (0.33) Fe1 2.0274 (0.0032) 70.18 (0.20) 69.81 (0.19) H8 0.9500 126.47 126.47 125.13 C8 - C9 C7 Fe1 C9 - Distance Angles C10 1.3634 (0.0053) C8 1.4005 (0.0059) 108.39 (0.35) Fe1 2.0362 (0.0034) 70.84 (0.20) 69.50 (0.21) H9 0.9500 125.81 125.81 125.43 C9 - C10 C8 Fe1 C10 - Distance Angles C9 1.3634 (0.0053) C6 1.3713 (0.0048) 109.11 (0.34) Fe1 2.0452 (0.0032) 70.13 (0.21) 70.12 (0.19) H10 0.9500 125.44 125.44 125.89 C10 - C9 C6 Fe1 C11 - Distance Angles C1 1.5018 (0.0038) P1 1.8561 (0.0026) 117.26 (0.18) H11A 0.9900 107.99 107.99 H11B 0.9900 107.99 107.99 107.24 C11 - C1 P1 H11A C12 - Distance Angles C2 1.4939 (0.0039) P2 1.8527 (0.0027) 119.58 (0.18) H12A 0.9900 107.42 107.42 H12B 0.9900 107.42 107.42 106.95 C12 - C2 P2 H12A C13 - Distance Angles C15 1.5303 (0.0040) C16 1.5315 (0.0038) 105.78 (0.23) C14 1.5382 (0.0039) 108.55 (0.24) 109.09 (0.22) P1 1.9049 (0.0028) 112.25 (0.19) 115.08 (0.20) 105.95 (0.19) C13 - C15 C16 C14 C14 - Distance Angles C13 1.5382 (0.0039) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles C13 1.5303 (0.0040) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C13 H15A H15B C16 - Distance Angles C13 1.5315 (0.0038) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C13 H16A H16B C17 - Distance Angles C20 1.5284 (0.0039) C18 1.5331 (0.0039) 108.76 (0.24) C19 1.5343 (0.0039) 109.04 (0.23) 106.33 (0.24) P1 1.8992 (0.0028) 111.51 (0.20) 113.85 (0.19) 107.13 (0.19) C17 - C20 C18 C19 C18 - Distance Angles C17 1.5331 (0.0039) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B C19 - Distance Angles C17 1.5343 (0.0039) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C17 H19A H19B C20 - Distance Angles C17 1.5284 (0.0039) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C17 H20A H20B C21 - Distance Angles C23 1.5347 (0.0039) C24 1.5380 (0.0041) 110.63 (0.24) C22 1.5414 (0.0038) 107.55 (0.24) 105.63 (0.23) P2 1.8956 (0.0027) 110.93 (0.19) 106.63 (0.19) 115.34 (0.20) C21 - C23 C24 C22 C22 - Distance Angles C21 1.5414 (0.0038) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C21 H22A H22B C23 - Distance Angles C21 1.5347 (0.0039) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C21 H23A H23B C24 - Distance Angles C21 1.5380 (0.0041) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C21 H24A H24B C25 - Distance Angles C27 1.5335 (0.0039) C26 1.5409 (0.0039) 109.37 (0.24) C28 1.5427 (0.0038) 106.55 (0.24) 107.96 (0.23) P2 1.9174 (0.0029) 113.50 (0.19) 106.35 (0.19) 112.99 (0.20) C25 - C27 C26 C28 C26 - Distance Angles C25 1.5409 (0.0039) 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 1.5335 (0.0039) 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 C25 1.5427 (0.0038) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C25 H28A H28B P1 - Distance Angles C11 1.8561 (0.0026) C17 1.8992 (0.0028) 100.57 (0.12) C13 1.9049 (0.0028) 103.22 (0.13) 111.28 (0.13) Pd1 2.3352 (0.0008) 118.28 (0.09) 106.11 (0.09) 116.34 (0.09) P1 - C11 C17 C13 P2 - Distance Angles C12 1.8527 (0.0027) C21 1.8956 (0.0027) 103.71 (0.12) C25 1.9174 (0.0029) 98.90 (0.12) 112.49 (0.13) Pd1 2.3176 (0.0007) 118.77 (0.09) 105.85 (0.09) 116.58 (0.09) P2 - C12 C21 C25 Cl1 - Distance Angles Pd1 2.3502 (0.0007) Cl1 - Cl2 - Distance Angles Pd1 2.3520 (0.0008) Cl2 - Fe1 - Distance Angles C8 2.0274 (0.0033) C5 2.0286 (0.0027) 142.06 (0.17) C4 2.0323 (0.0027) 114.03 (0.14) 41.10 (0.11) C7 2.0339 (0.0031) 40.87 (0.16) 174.45 (0.15) 144.45 (0.15) C3 2.0350 (0.0028) 112.44 (0.14) 69.01 (0.12) 40.84 (0.11) 115.26 (0.13) C9 2.0362 (0.0034) 40.32 (0.17) 111.87 (0.15) 110.91 (0.13) 67.67 (0.15) 138.00 (0.15) C6 2.0387 (0.0031) 67.35 (0.14) 134.49 (0.13) 174.36 (0.14) 40.00 (0.14) 144.41 (0.14) 66.29 (0.14) C10 2.0452 (0.0032) 66.79 (0.15) 109.10 (0.13) 135.59 (0.14) 66.86 (0.13) 176.13 (0.14) 39.03 (0.15) 39.24 (0.14) C1 2.0549 (0.0026) 176.76 (0.16) 41.04 (0.11) 68.97 (0.11) 135.94 (0.15) 68.85 (0.11) 140.59 (0.16) 109.80 (0.12) C2 2.0553 (0.0026) 138.66 (0.17) 68.65 (0.11) 68.72 (0.11) 111.91 (0.13) 41.02 (0.11) 178.82 (0.17) 114.18 (0.12) Fe1 - C8 C5 C4 C7 C3 C9 C6 Pd1 - Distance Angles P2 2.3176 (0.0007) P1 2.3352 (0.0008) 104.64 (0.03) Cl1 2.3502 (0.0007) 162.64 (0.03) 87.28 (0.03) Cl2 2.3520 (0.0008) 86.57 (0.03) 163.13 (0.03) 84.89 (0.03) Pd1 - P2 P1 Cl1 C31_a - Distance Angles Cl33_a 1.7463 (0.0085) Cl32_a 1.7471 (0.0083) 112.45 (0.70) Cl31_a 1.7494 (0.0083) 108.92 (0.64) 113.06 (0.67) H31_a 1.0000 107.37 107.37 107.37 C31_a - Cl33_a Cl32_a Cl31_a Cl31_a - Distance Angles C31_a 1.7494 (0.0083) Cl31_a - Cl32_a - Distance Angles C31_a 1.7471 (0.0083) Cl32_a - Cl33_a - Distance Angles C31_a 1.7463 (0.0085) Cl33_a - C36_b - Distance Angles Cl36_b 1.7563 (0.0140) Cl37_b 1.7585 (0.0136) 106.29 (1.30) Cl38_b 1.7611 (0.0135) 109.87 (1.21) 106.98 (1.28) H36_b 1.0000 111.17 111.17 111.17 C36_b - Cl36_b Cl37_b Cl38_b Cl36_b - Distance Angles C36_b 1.7563 (0.0141) Cl36_b - Cl37_b - Distance Angles C36_b 1.7585 (0.0136) Cl37_b - Cl38_b - Distance Angles C36_b 1.7611 (0.0135) Cl38_b - FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0641 for 7725 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.59 at 0.2532 0.2573 0.0193 [ 1.03 A from CL33 ] Deepest hole -0.87 at 0.2449 0.4988 0.2353 [ 0.75 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 5115 / 30553 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7468 0.7427 -0.0193 1.00000 0.05 0.59 1.03 CL33 1.32 CL38 1.56 C31 1.73 C36 Q2 1 0.1956 0.5364 0.1756 1.00000 0.05 0.48 1.38 P1 1.52 PD1 1.96 H14A 2.19 C13 Q3 1 0.1237 0.5355 0.3077 1.00000 0.05 0.48 0.63 H18A 1.37 C18 1.76 H18B 2.08 CL1 Q4 1 0.2536 0.6958 0.0870 1.00000 0.05 0.44 0.66 C1 0.86 C2 1.76 C11 1.92 C5 Q5 1 0.2182 0.5846 0.2725 1.00000 0.05 0.43 1.46 PD1 1.74 H19B 1.89 H18A 1.99 P1 Shortest distances between peaks (including symmetry equivalents) 3 5 1.53 2 5 2.09 2 3 2.90 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 2.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.02: Generate idealized H-atoms 22.67: Structure factors and derivatives 42.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 3.88: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.13: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0550 finished at 11:40:23 Total CPU time: 73.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++