Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Howard Colquhoun' _publ_contact_author_address ; School of Chemistry The University of Reading Whiteknights Reading RG6 6AD UNITED KINGDOM ; _publ_contact_author_email H.M.COLQUHOUN@RDG.AC.UK _publ_section_title ; The oxadiazolyldiazenido(1-) ligand: a remarkably versatile platform for the synthesis of heteropolynuclear transition metal complexes ; loop_ _publ_author_name 'Howard Colquhoun' 'Kareem Abd El Kader' 'C. Cardin' 'Sam Y. F. Chan' 'M. Drew' 'Yu. Gan' ; T.M.White ; data_2 _database_code_depnum_ccdc_archive 'CCDC 651020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H56 Br N5 O4 P4 W' _chemical_formula_weight 1310.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.759(14) _cell_length_b 17.125(19) _cell_length_c 24.16(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.651(10) _cell_angle_gamma 90.00 _cell_volume 5934(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 2.778 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37027 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.79 _reflns_number_total 10751 _reflns_number_gt 9211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+11.3012P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10751 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.885786(17) 0.172902(14) 0.181015(10) 0.03073(9) Uani 1 1 d . . . Br2 Br 0.77820(5) 0.09706(5) 0.23591(3) 0.0517(2) Uani 1 1 d . . . P1 P 0.84055(13) 0.06843(10) 0.10541(8) 0.0413(4) Uani 1 1 d . . . P2 P 0.75653(12) 0.27136(10) 0.14898(7) 0.0365(4) Uani 1 1 d . . . P3 P 0.91735(13) 0.26328(10) 0.26535(7) 0.0399(4) Uani 1 1 d . . . P4 P 1.01829(13) 0.07834(11) 0.21435(9) 0.0488(5) Uani 1 1 d . . . C11 C 0.7371(6) 0.0049(4) 0.0983(3) 0.0487(18) Uani 1 1 d . . . C12 C 0.7397(7) -0.0733(5) 0.0847(3) 0.068(2) Uani 1 1 d . . . H12 H 0.7956 -0.0965 0.0824 0.081 Uiso 1 1 calc R . . C13 C 0.6564(10) -0.1180(6) 0.0743(4) 0.089(4) Uani 1 1 d . . . H13 H 0.6585 -0.1712 0.0670 0.107 Uiso 1 1 calc R . . C14 C 0.5743(10) -0.0839(7) 0.0747(5) 0.095(4) Uani 1 1 d . . . H14 H 0.5195 -0.1128 0.0653 0.114 Uiso 1 1 calc R . . C15 C 0.5716(7) -0.0082(7) 0.0887(4) 0.085(3) Uani 1 1 d . . . H15 H 0.5150 0.0146 0.0900 0.101 Uiso 1 1 calc R . . C16 C 0.6530(6) 0.0367(5) 0.1013(4) 0.068(2) Uani 1 1 d . . . H16 H 0.6501 0.0887 0.1118 0.081 Uiso 1 1 calc R . . C21 C 0.8288(6) 0.0972(4) 0.0303(3) 0.0503(18) Uani 1 1 d . . . C22 C 0.7416(7) 0.1047(6) -0.0078(4) 0.077(3) Uani 1 1 d . . . H22 H 0.6880 0.0941 0.0048 0.093 Uiso 1 1 calc R . . C23 C 0.7330(10) 0.1278(8) -0.0646(5) 0.112(4) Uani 1 1 d . . . H23 H 0.6746 0.1309 -0.0897 0.134 Uiso 1 1 calc R . . C24 C 0.8126(12) 0.1458(8) -0.0824(5) 0.106(4) Uani 1 1 d . . . H24 H 0.8078 0.1615 -0.1198 0.127 Uiso 1 1 calc R . . C25 C 0.8984(9) 0.1408(6) -0.0459(5) 0.090(4) Uani 1 1 d . . . H25 H 0.9516 0.1534 -0.0584 0.108 Uiso 1 1 calc R . . C26 C 0.9062(7) 0.1167(5) 0.0105(4) 0.070(2) Uani 1 1 d . . . H26 H 0.9650 0.1137 0.0351 0.083 Uiso 1 1 calc R . . C31 C 0.6345(5) 0.2411(4) 0.1336(3) 0.0447(16) Uani 1 1 d . . . C32 C 0.5923(6) 0.2207(5) 0.1780(4) 0.065(2) Uani 1 1 d . . . H32 H 0.6260 0.2266 0.2155 0.078 Uiso 1 1 calc R . . C33 C 0.5026(7) 0.1922(7) 0.1677(6) 0.092(3) Uani 1 1 d . . . H33 H 0.4763 0.1786 0.1978 0.111 Uiso 1 1 calc R . . C34 C 0.4527(8) 0.1843(7) 0.1125(7) 0.105(4) Uani 1 1 d . . . H34 H 0.3923 0.1648 0.1053 0.126 Uiso 1 1 calc R . . C35 C 0.4907(7) 0.2049(7) 0.0667(5) 0.093(4) Uani 1 1 d . . . H35 H 0.4558 0.1998 0.0294 0.112 Uiso 1 1 calc R . . C36 C 0.5823(6) 0.2335(5) 0.0778(4) 0.066(2) Uani 1 1 d . . . H36 H 0.6084 0.2474 0.0478 0.079 Uiso 1 1 calc R . . C41 C 0.7613(5) 0.3331(4) 0.0866(3) 0.0487(17) Uani 1 1 d . . . C42 C 0.8016(5) 0.3053(5) 0.0447(3) 0.0483(17) Uani 1 1 d . . . H42 H 0.8237 0.2543 0.0468 0.058 Uiso 1 1 calc R . . C43 C 0.8100(7) 0.3523(6) -0.0007(4) 0.069(2) Uani 1 1 d . . . H43 H 0.8384 0.3326 -0.0282 0.083 Uiso 1 1 calc R . . C44 C 0.7771(8) 0.4275(6) -0.0054(5) 0.086(3) Uani 1 1 d . . . H44 H 0.7827 0.4589 -0.0358 0.103 Uiso 1 1 calc R . . C45 C 0.7357(9) 0.4554(6) 0.0360(5) 0.097(4) Uani 1 1 d . . . H45 H 0.7136 0.5064 0.0334 0.117 Uiso 1 1 calc R . . C46 C 0.7261(7) 0.4086(6) 0.0819(4) 0.075(3) Uani 1 1 d . . . H46 H 0.6964 0.4280 0.1090 0.090 Uiso 1 1 calc R . . C51 C 1.0047(6) 0.3414(4) 0.2661(3) 0.0520(19) Uani 1 1 d . . . C52 C 0.9957(7) 0.4135(5) 0.2893(4) 0.072(3) Uani 1 1 d . . . H52 H 0.9442 0.4245 0.3039 0.087 Uiso 1 1 calc R . . C53 C 1.0651(9) 0.4705(6) 0.2908(5) 0.095(4) Uani 1 1 d . . . H53 H 1.0588 0.5198 0.3056 0.114 Uiso 1 1 calc R . . C54 C 1.1413(9) 0.4535(7) 0.2704(5) 0.097(4) Uani 1 1 d . . . H54 H 1.1870 0.4913 0.2719 0.117 Uiso 1 1 calc R . . C55 C 1.1516(7) 0.3811(7) 0.2478(5) 0.084(3) Uani 1 1 d . . . H55 H 1.2040 0.3700 0.2341 0.100 Uiso 1 1 calc R . . C56 C 1.0830(6) 0.3252(5) 0.2456(4) 0.065(2) Uani 1 1 d . . . H56 H 1.0895 0.2763 0.2302 0.078 Uiso 1 1 calc R . . C61 C 0.9491(6) 0.2255(4) 0.3392(3) 0.0503(18) Uani 1 1 d . . . C62 C 0.8824(8) 0.1928(5) 0.3641(4) 0.068(2) Uani 1 1 d . . . H62 H 0.8198 0.1931 0.3450 0.082 Uiso 1 1 calc R . . C63 C 0.9105(11) 0.1592(6) 0.4188(5) 0.100(4) Uani 1 1 d . . . H63 H 0.8656 0.1378 0.4356 0.120 Uiso 1 1 calc R . . C64 C 0.9996(13) 0.1575(8) 0.4471(5) 0.120(6) Uani 1 1 d . . . H64 H 1.0167 0.1342 0.4828 0.144 Uiso 1 1 calc R . . C65 C 1.0644(11) 0.1896(8) 0.4234(5) 0.114(5) Uani 1 1 d . . . H65 H 1.1264 0.1892 0.4437 0.137 Uiso 1 1 calc R . . C66 C 1.0419(7) 0.2240(6) 0.3689(4) 0.080(3) Uani 1 1 d . . . H66 H 1.0882 0.2452 0.3532 0.096 Uiso 1 1 calc R . . C71 C 1.1376(5) 0.1180(5) 0.2380(3) 0.0518(18) Uani 1 1 d . . . C72 C 1.1839(6) 0.1184(6) 0.2937(4) 0.078(3) Uani 1 1 d . . . H72 H 1.1566 0.0957 0.3208 0.094 Uiso 1 1 calc R . . C73 C 1.2730(8) 0.1531(9) 0.3111(6) 0.112(4) Uani 1 1 d . . . H73 H 1.3034 0.1531 0.3495 0.135 Uiso 1 1 calc R . . C74 C 1.3140(8) 0.1856(8) 0.2736(7) 0.113(5) Uani 1 1 d . . . H74 H 1.3729 0.2077 0.2857 0.136 Uiso 1 1 calc R . . C75 C 1.2708(7) 0.1866(7) 0.2181(6) 0.091(4) Uani 1 1 d . . . H75 H 1.3000 0.2098 0.1921 0.109 Uiso 1 1 calc R . . C76 C 1.1810(6) 0.1528(6) 0.1984(4) 0.075(3) Uani 1 1 d . . . H76 H 1.1515 0.1537 0.1599 0.090 Uiso 1 1 calc R . . C81 C 1.0214(6) 0.0033(5) 0.2680(4) 0.066(2) Uani 1 1 d . . . C82 C 0.9873(6) 0.0188(5) 0.3155(4) 0.066(2) Uani 1 1 d . . . H82 H 0.9554 0.0653 0.3170 0.080 Uiso 1 1 calc R . . C83 C 0.9992(8) -0.0330(7) 0.3613(5) 0.096(4) Uani 1 1 d . . . H83 H 0.9776 -0.0212 0.3935 0.115 Uiso 1 1 calc R . . C84 C 1.0445(12) -0.1027(8) 0.3566(9) 0.159(8) Uani 1 1 d . . . H84 H 1.0523 -0.1391 0.3859 0.191 Uiso 1 1 calc R . . C85 C 1.0778(18) -0.1189(11) 0.3101(11) 0.245(15) Uani 1 1 d . . . H85 H 1.1098 -0.1653 0.3085 0.293 Uiso 1 1 calc R . . C86 C 1.0644(11) -0.0666(7) 0.2648(8) 0.145(7) Uani 1 1 d . . . H86 H 1.0848 -0.0793 0.2323 0.174 Uiso 1 1 calc R . . C1 C 0.9373(6) -0.0040(5) 0.1172(4) 0.070(3) Uani 1 1 d . . . H1A H 0.9212 -0.0480 0.1384 0.084 Uiso 1 1 calc R . . H1B H 0.9435 -0.0234 0.0806 0.084 Uiso 1 1 calc R . . C2 C 1.0273(6) 0.0276(6) 0.1482(4) 0.077(3) Uani 1 1 d . . . H2A H 1.0500 0.0640 0.1238 0.092 Uiso 1 1 calc R . . H2B H 1.0720 -0.0146 0.1577 0.092 Uiso 1 1 calc R . . C3 C 0.7646(5) 0.3470(5) 0.2059(3) 0.0515(19) Uani 1 1 d . . . H3A H 0.8017 0.3905 0.1980 0.062 Uiso 1 1 calc R . . H3B H 0.7026 0.3664 0.2051 0.062 Uiso 1 1 calc R . . C4 C 0.8076(5) 0.3156(4) 0.2644(3) 0.0505(18) Uani 1 1 d . . . H4A H 0.7641 0.2803 0.2760 0.061 Uiso 1 1 calc R . . H4B H 0.8200 0.3584 0.2915 0.061 Uiso 1 1 calc R . . N101 N 0.9578(3) 0.2189(3) 0.1410(2) 0.0356(12) Uani 1 1 d . . . N102 N 1.0139(4) 0.2395(3) 0.1089(3) 0.0492(15) Uani 1 1 d . . . C101 C 1.0263(5) 0.3142(4) 0.0992(3) 0.0488(18) Uani 1 1 d . . . N103 N 1.0785(6) 0.3418(4) 0.0659(4) 0.079(3) Uani 1 1 d . . . N104 N 1.0702(6) 0.4223(4) 0.0658(4) 0.079(2) Uani 1 1 d . . . C102 C 1.0147(6) 0.4406(5) 0.0978(3) 0.0544(19) Uani 1 1 d . . . O101 O 0.9835(3) 0.3746(3) 0.1211(2) 0.0427(11) Uani 1 1 d . . . C103 C 0.9850(5) 0.5177(4) 0.1106(3) 0.0489(17) Uani 1 1 d . . . C104 C 1.0067(7) 0.5798(5) 0.0784(4) 0.067(2) Uani 1 1 d . . . H104 H 1.0355 0.5705 0.0486 0.080 Uiso 1 1 calc R . . C105 C 0.9847(7) 0.6548(5) 0.0912(4) 0.073(3) Uani 1 1 d . . . H105 H 1.0015 0.6970 0.0715 0.087 Uiso 1 1 calc R . . C106 C 0.9379(6) 0.6669(5) 0.1331(3) 0.0535(19) Uani 1 1 d . . . C107 C 0.9142(6) 0.6059(5) 0.1634(4) 0.063(2) Uani 1 1 d . . . H107 H 0.8818 0.6148 0.1915 0.076 Uiso 1 1 calc R . . C108 C 0.9388(6) 0.5310(5) 0.1520(4) 0.061(2) Uani 1 1 d . . . H108 H 0.9236 0.4894 0.1727 0.073 Uiso 1 1 calc R . . N105 N 0.9166(6) 0.7470(4) 0.1470(3) 0.069(2) Uani 1 1 d . . . O102 O 0.9562(8) 0.7992(4) 0.1301(5) 0.139(4) Uani 1 1 d . . . O103 O 0.8627(6) 0.7586(5) 0.1763(4) 0.117(3) Uani 1 1 d . . . O201 O 1.200(2) 0.2485(17) 0.0143(12) 0.176(10) Uiso 0.50 1 d P . . H201 H 1.1447 0.2553 -0.0008 0.211 Uiso 0.50 1 calc PR . . C202 C 1.245(2) 0.3094(17) 0.0098(13) 0.119(9) Uiso 0.50 1 d P . . H20A H 1.2021 0.3507 -0.0052 0.143 Uiso 0.50 1 calc PR . . H20B H 1.2851 0.3000 -0.0154 0.143 Uiso 0.50 1 calc PR . . H20C H 1.2816 0.3242 0.0466 0.143 Uiso 0.50 1 calc PR . . O301 O 1.163(2) 0.1290(18) 0.0377(14) 0.197(11) Uiso 0.50 1 d P . . H301 H 1.1085 0.1145 0.0279 0.236 Uiso 0.50 1 calc PR . . C302 C 1.208(2) 0.0792(18) 0.0588(13) 0.129(10) Uiso 0.50 1 d P . . H30A H 1.2577 0.0710 0.0401 0.154 Uiso 0.50 1 calc PR . . H30B H 1.1708 0.0326 0.0560 0.154 Uiso 0.50 1 calc PR . . H30C H 1.2333 0.0914 0.0981 0.154 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02611(14) 0.03301(15) 0.03293(14) -0.00351(10) 0.00668(9) -0.00109(10) Br2 0.0497(4) 0.0609(5) 0.0477(4) 0.0032(3) 0.0181(3) -0.0061(3) P1 0.0419(10) 0.0389(10) 0.0420(10) -0.0095(7) 0.0078(8) -0.0008(7) P2 0.0301(9) 0.0444(10) 0.0350(9) -0.0019(7) 0.0078(7) 0.0054(7) P3 0.0395(10) 0.0429(10) 0.0344(9) -0.0070(7) 0.0030(7) 0.0018(7) P4 0.0361(10) 0.0477(11) 0.0586(12) -0.0081(9) 0.0029(9) 0.0102(8) C11 0.069(5) 0.042(4) 0.035(4) -0.003(3) 0.010(3) -0.013(3) C12 0.098(7) 0.050(5) 0.050(5) -0.007(4) 0.008(5) -0.014(4) C13 0.144(11) 0.048(6) 0.070(7) -0.008(4) 0.014(7) -0.041(6) C14 0.112(10) 0.096(9) 0.084(8) -0.029(6) 0.035(7) -0.067(8) C15 0.076(7) 0.096(8) 0.088(7) -0.019(6) 0.031(6) -0.039(6) C16 0.065(6) 0.061(6) 0.080(6) -0.018(4) 0.024(5) -0.024(4) C21 0.058(5) 0.052(5) 0.045(4) -0.011(3) 0.020(4) -0.005(3) C22 0.066(6) 0.116(8) 0.050(5) 0.009(5) 0.015(5) -0.012(6) C23 0.123(11) 0.148(12) 0.054(6) 0.020(7) 0.002(7) -0.007(9) C24 0.144(13) 0.126(10) 0.057(7) 0.001(7) 0.042(8) -0.017(9) C25 0.120(10) 0.083(7) 0.091(8) -0.017(6) 0.076(8) -0.019(7) C26 0.078(6) 0.080(6) 0.060(5) -0.019(4) 0.036(5) -0.014(5) C31 0.032(4) 0.057(4) 0.045(4) -0.002(3) 0.009(3) 0.005(3) C32 0.040(4) 0.091(7) 0.067(5) 0.013(5) 0.019(4) 0.003(4) C33 0.040(5) 0.118(9) 0.121(10) 0.018(7) 0.024(6) -0.005(5) C34 0.044(6) 0.107(9) 0.162(13) 0.001(8) 0.020(8) -0.026(6) C35 0.057(6) 0.104(8) 0.100(9) -0.020(7) -0.019(6) -0.004(6) C36 0.049(5) 0.073(6) 0.070(6) -0.008(4) 0.004(4) -0.006(4) C41 0.033(4) 0.056(5) 0.056(4) 0.008(3) 0.008(3) 0.007(3) C42 0.048(4) 0.058(5) 0.040(4) 0.006(3) 0.013(3) 0.004(3) C43 0.072(6) 0.081(6) 0.057(5) 0.018(4) 0.020(5) -0.007(5) C44 0.113(9) 0.073(7) 0.078(7) 0.036(5) 0.033(6) 0.013(6) C45 0.143(11) 0.062(7) 0.092(8) 0.030(5) 0.037(8) 0.036(6) C46 0.085(7) 0.074(6) 0.071(6) 0.016(5) 0.028(5) 0.033(5) C51 0.060(5) 0.050(4) 0.040(4) -0.010(3) 0.000(4) -0.011(3) C52 0.095(7) 0.050(5) 0.072(6) -0.017(4) 0.021(5) -0.011(5) C53 0.122(10) 0.046(6) 0.108(9) -0.016(5) 0.012(8) -0.024(6) C54 0.089(8) 0.077(8) 0.116(10) -0.004(6) 0.004(7) -0.046(6) C55 0.063(6) 0.094(8) 0.090(7) -0.011(6) 0.011(5) -0.030(5) C56 0.047(5) 0.069(6) 0.075(6) -0.021(4) 0.009(4) -0.016(4) C61 0.063(5) 0.045(4) 0.036(4) -0.005(3) -0.002(4) 0.002(3) C62 0.097(7) 0.060(5) 0.048(5) -0.001(4) 0.017(5) -0.004(5) C63 0.165(14) 0.082(8) 0.053(6) 0.007(5) 0.026(8) -0.017(8) C64 0.192(17) 0.096(9) 0.050(7) 0.014(6) -0.014(9) -0.023(10) C65 0.136(12) 0.105(10) 0.068(7) 0.018(7) -0.042(8) 0.000(8) C66 0.082(7) 0.079(7) 0.058(6) 0.002(5) -0.023(5) -0.002(5) C71 0.039(4) 0.053(5) 0.063(5) 0.003(4) 0.011(4) 0.007(3) C72 0.049(5) 0.108(8) 0.071(6) 0.005(5) 0.002(5) -0.022(5) C73 0.066(7) 0.172(13) 0.089(8) -0.006(8) 0.001(6) -0.037(8) C74 0.049(6) 0.155(13) 0.129(12) 0.003(9) 0.007(7) -0.025(7) C75 0.041(5) 0.118(9) 0.120(10) 0.019(7) 0.031(6) -0.001(5) C76 0.048(5) 0.103(8) 0.078(6) 0.012(5) 0.020(5) 0.015(5) C81 0.052(5) 0.045(5) 0.101(7) 0.011(4) 0.016(5) 0.001(4) C82 0.059(5) 0.054(5) 0.076(6) 0.010(4) -0.005(5) 0.003(4) C83 0.074(7) 0.089(8) 0.116(9) 0.035(7) 0.008(6) -0.006(6) C84 0.159(15) 0.103(11) 0.24(2) 0.116(13) 0.091(14) 0.054(10) C85 0.34(3) 0.129(15) 0.34(3) 0.152(18) 0.24(3) 0.145(18) C86 0.176(15) 0.071(8) 0.226(17) 0.069(9) 0.124(13) 0.061(9) C1 0.059(5) 0.064(6) 0.079(6) -0.025(4) 0.000(5) 0.019(4) C2 0.059(6) 0.083(7) 0.087(7) -0.031(5) 0.014(5) 0.020(5) C3 0.047(4) 0.059(5) 0.045(4) -0.014(3) 0.002(3) 0.012(3) C4 0.053(5) 0.059(5) 0.041(4) -0.009(3) 0.012(3) 0.011(3) N101 0.027(3) 0.033(3) 0.047(3) -0.005(2) 0.008(2) 0.002(2) N102 0.045(3) 0.045(4) 0.069(4) 0.001(3) 0.036(3) -0.004(3) C101 0.041(4) 0.055(5) 0.057(5) 0.002(3) 0.025(4) -0.008(3) N103 0.084(6) 0.061(5) 0.117(7) 0.013(4) 0.072(5) 0.000(4) N104 0.092(6) 0.053(5) 0.116(7) 0.016(4) 0.071(5) -0.001(4) C102 0.057(5) 0.053(5) 0.059(5) 0.010(4) 0.025(4) -0.009(4) O101 0.041(3) 0.042(3) 0.050(3) 0.003(2) 0.020(2) -0.009(2) C103 0.053(5) 0.044(4) 0.054(4) 0.005(3) 0.021(4) -0.008(3) C104 0.088(7) 0.055(5) 0.073(6) 0.000(4) 0.049(5) -0.009(4) C105 0.099(7) 0.052(5) 0.085(7) 0.017(4) 0.057(6) -0.001(5) C106 0.058(5) 0.056(5) 0.053(5) 0.003(3) 0.025(4) 0.003(4) C107 0.075(6) 0.064(6) 0.064(5) 0.000(4) 0.044(5) -0.010(4) C108 0.080(6) 0.050(5) 0.064(5) 0.012(4) 0.036(5) -0.015(4) N105 0.079(5) 0.058(5) 0.081(5) 0.010(4) 0.043(5) 0.007(4) O102 0.211(10) 0.051(5) 0.208(10) 0.009(5) 0.159(9) 0.005(5) O103 0.157(8) 0.085(6) 0.149(8) 0.002(5) 0.116(7) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N101 1.780(5) . ? W1 P3 2.513(3) . ? W1 P4 2.520(3) . ? W1 P2 2.527(2) . ? W1 P1 2.531(3) . ? W1 Br2 2.6385(18) . ? P1 C11 1.850(8) . ? P1 C21 1.850(8) . ? P1 C1 1.862(8) . ? P2 C31 1.825(7) . ? P2 C41 1.857(8) . ? P2 C3 1.872(7) . ? P3 C4 1.847(8) . ? P3 C61 1.851(8) . ? P3 C51 1.855(8) . ? P4 C81 1.817(9) . ? P4 C71 1.847(8) . ? P4 C2 1.851(9) . ? C11 C16 1.372(12) . ? C11 C12 1.382(11) . ? C12 C13 1.418(14) . ? C13 C14 1.347(16) . ? C14 C15 1.342(15) . ? C15 C16 1.398(12) . ? C21 C26 1.379(11) . ? C21 C22 1.401(12) . ? C22 C23 1.404(13) . ? C23 C24 1.378(17) . ? C24 C25 1.365(17) . ? C25 C26 1.402(14) . ? C31 C36 1.392(11) . ? C31 C32 1.406(10) . ? C32 C33 1.378(12) . ? C33 C34 1.370(18) . ? C34 C35 1.400(17) . ? C35 C36 1.403(13) . ? C41 C42 1.374(10) . ? C41 C46 1.388(11) . ? C42 C43 1.389(11) . ? C43 C44 1.371(13) . ? C44 C45 1.373(15) . ? C45 C46 1.404(13) . ? C51 C52 1.375(11) . ? C51 C56 1.390(12) . ? C52 C53 1.410(14) . ? C53 C54 1.360(16) . ? C54 C55 1.378(15) . ? C55 C56 1.385(12) . ? C61 C66 1.389(12) . ? C61 C62 1.388(12) . ? C62 C63 1.411(14) . ? C63 C64 1.33(2) . ? C64 C65 1.34(2) . ? C65 C66 1.408(14) . ? C71 C72 1.358(12) . ? C71 C76 1.405(12) . ? C72 C73 1.413(13) . ? C73 C74 1.325(17) . ? C74 C75 1.341(17) . ? C75 C76 1.421(14) . ? C81 C86 1.366(13) . ? C81 C82 1.383(13) . ? C82 C83 1.396(13) . ? C83 C84 1.386(18) . ? C84 C85 1.36(2) . ? C85 C86 1.39(2) . ? C1 C2 1.466(12) . ? C3 C4 1.506(10) . ? N101 N102 1.309(7) . ? N102 C101 1.321(9) . ? C101 N103 1.325(9) . ? C101 O101 1.381(9) . ? N103 N104 1.384(10) . ? N104 C102 1.292(10) . ? C102 O101 1.389(8) . ? C102 C103 1.446(11) . ? C103 C108 1.355(11) . ? C103 C104 1.399(10) . ? C104 C105 1.378(12) . ? C105 C106 1.371(11) . ? C106 C107 1.367(11) . ? C106 N105 1.463(10) . ? C107 C108 1.378(12) . ? N105 O102 1.192(10) . ? N105 O103 1.199(9) . ? O201 C202 1.25(3) . ? O301 C302 1.13(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N101 W1 P3 98.47(18) . . ? N101 W1 P4 86.56(18) . . ? P3 W1 P4 98.93(8) . . ? N101 W1 P2 92.46(18) . . ? P3 W1 P2 79.60(8) . . ? P4 W1 P2 178.10(6) . . ? N101 W1 P1 90.62(18) . . ? P3 W1 P1 170.81(6) . . ? P4 W1 P1 80.16(9) . . ? P2 W1 P1 101.48(8) . . ? N101 W1 Br2 176.37(16) . . ? P3 W1 Br2 85.07(8) . . ? P4 W1 Br2 92.10(9) . . ? P2 W1 Br2 88.97(8) . . ? P1 W1 Br2 85.83(8) . . ? C11 P1 C21 100.5(3) . . ? C11 P1 C1 102.0(4) . . ? C21 P1 C1 102.6(4) . . ? C11 P1 W1 123.6(2) . . ? C21 P1 W1 117.9(3) . . ? C1 P1 W1 107.4(3) . . ? C31 P2 C41 102.8(3) . . ? C31 P2 C3 103.5(3) . . ? C41 P2 C3 101.2(4) . . ? C31 P2 W1 120.7(3) . . ? C41 P2 W1 117.3(2) . . ? C3 P2 W1 108.9(2) . . ? C4 P3 C61 101.7(4) . . ? C4 P3 C51 104.8(4) . . ? C61 P3 C51 103.0(3) . . ? C4 P3 W1 107.1(2) . . ? C61 P3 W1 121.5(3) . . ? C51 P3 W1 116.6(3) . . ? C81 P4 C71 100.2(4) . . ? C81 P4 C2 106.8(5) . . ? C71 P4 C2 100.5(4) . . ? C81 P4 W1 124.7(3) . . ? C71 P4 W1 118.3(3) . . ? C2 P4 W1 103.5(3) . . ? C16 C11 C12 118.2(8) . . ? C16 C11 P1 119.9(6) . . ? C12 C11 P1 121.6(7) . . ? C11 C12 C13 119.6(10) . . ? C14 C13 C12 120.5(10) . . ? C15 C14 C13 120.1(10) . . ? C14 C15 C16 120.7(11) . . ? C11 C16 C15 120.8(9) . . ? C26 C21 C22 117.3(8) . . ? C26 C21 P1 120.8(7) . . ? C22 C21 P1 121.9(6) . . ? C21 C22 C23 121.7(10) . . ? C24 C23 C22 118.7(12) . . ? C25 C24 C23 121.0(11) . . ? C24 C25 C26 119.8(10) . . ? C21 C26 C25 121.6(10) . . ? C36 C31 C32 118.1(7) . . ? C36 C31 P2 121.2(6) . . ? C32 C31 P2 120.6(6) . . ? C33 C32 C31 122.1(9) . . ? C34 C33 C32 118.9(11) . . ? C33 C34 C35 121.5(10) . . ? C34 C35 C36 118.9(10) . . ? C31 C36 C35 120.5(9) . . ? C42 C41 C46 118.8(8) . . ? C42 C41 P2 120.5(6) . . ? C46 C41 P2 120.7(6) . . ? C41 C42 C43 121.0(8) . . ? C44 C43 C42 120.9(9) . . ? C43 C44 C45 118.4(9) . . ? C44 C45 C46 121.5(9) . . ? C41 C46 C45 119.3(9) . . ? C52 C51 C56 119.6(8) . . ? C52 C51 P3 121.2(7) . . ? C56 C51 P3 119.1(6) . . ? C51 C52 C53 119.5(10) . . ? C54 C53 C52 120.0(10) . . ? C53 C54 C55 120.9(10) . . ? C54 C55 C56 119.3(11) . . ? C55 C56 C51 120.6(9) . . ? C66 C61 C62 118.9(8) . . ? C66 C61 P3 119.9(7) . . ? C62 C61 P3 121.0(6) . . ? C61 C62 C63 119.3(11) . . ? C64 C63 C62 121.8(13) . . ? C63 C64 C65 119.3(12) . . ? C64 C65 C66 122.3(13) . . ? C61 C66 C65 118.5(11) . . ? C72 C71 C76 118.0(8) . . ? C72 C71 P4 121.9(7) . . ? C76 C71 P4 120.0(7) . . ? C71 C72 C73 120.8(10) . . ? C74 C73 C72 121.1(12) . . ? C73 C74 C75 120.2(11) . . ? C74 C75 C76 121.0(11) . . ? C71 C76 C75 119.0(10) . . ? C86 C81 C82 118.6(10) . . ? C86 C81 P4 120.9(9) . . ? C82 C81 P4 120.2(7) . . ? C81 C82 C83 122.2(10) . . ? C84 C83 C82 117.1(13) . . ? C85 C84 C83 121.4(13) . . ? C84 C85 C86 120.5(14) . . ? C81 C86 C85 120.1(15) . . ? C2 C1 P1 113.6(6) . . ? C1 C2 P4 111.9(6) . . ? C4 C3 P2 112.5(5) . . ? C3 C4 P3 111.0(5) . . ? N102 N101 W1 169.3(5) . . ? N101 N102 C101 120.0(6) . . ? N102 C101 N103 125.3(7) . . ? N102 C101 O101 124.2(6) . . ? N103 C101 O101 110.4(7) . . ? C101 N103 N104 107.1(7) . . ? C102 N104 N103 108.0(6) . . ? N104 C102 O101 111.3(7) . . ? N104 C102 C103 128.1(7) . . ? O101 C102 C103 120.7(6) . . ? C101 O101 C102 103.3(5) . . ? C108 C103 C104 120.2(7) . . ? C108 C103 C102 122.8(7) . . ? C104 C103 C102 117.0(7) . . ? C105 C104 C103 119.1(8) . . ? C106 C105 C104 119.6(7) . . ? C107 C106 C105 121.1(8) . . ? C107 C106 N105 119.9(7) . . ? C105 C106 N105 118.9(7) . . ? C106 C107 C108 119.4(7) . . ? C103 C108 C107 120.5(7) . . ? O102 N105 O103 121.7(9) . . ? O102 N105 C106 118.4(8) . . ? O103 N105 C106 119.8(7) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.79 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.059 _refine_diff_density_min -1.629 _refine_diff_density_rms 0.183 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1997) SHELX97 program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 651021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H57 Br N4 O3 P4 W' _chemical_formula_weight 1281.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.690(9) _cell_length_b 17.330(3) _cell_length_c 20.190(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.54(4) _cell_angle_gamma 90.00 _cell_volume 5839.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36225 _cell_measurement_theta_min 5.56 _cell_measurement_theta_max 54.22 _exptl_crystal_description shard _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 5.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;Oxford Diffraction Ltd. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_absorpt_correction_T_min 0.9091 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_standards_number 0 _diffrn_radiation_type 'Cu k\a' _diffrn_radiation_source 'Focused (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method 'calculated strategy' _diffrn_detector_area_resol_mean 16.2086 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36225 _diffrn_reflns_av_R_equivalents 0.2051 _diffrn_reflns_av_sigmaI/netI 0.2155 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.56 _diffrn_reflns_theta_max 54.22 _reflns_number_total 6991 _reflns_number_gt 3479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'Crysalis Red, Oxford Diffraction Ltd' _computing_data_reduction 'Crysalis Red, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6991 _refine_ls_number_parameters 665 _refine_ls_number_restraints 432 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1804 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W001 W 0.16840(5) -0.81941(4) 0.11424(3) 0.0285(3) Uani 1 1 d U . . Br02 Br 0.04219(11) -0.90515(9) 0.08859(8) 0.0352(5) Uani 1 1 d U . . P003 P 0.2014(3) -0.8498(2) -0.00495(19) 0.0307(11) Uani 1 1 d U . . P004 P 0.1094(3) -0.7976(2) 0.22765(18) 0.0288(11) Uani 1 1 d U . . P005 P 0.2303(3) -0.9293(2) 0.17464(19) 0.0303(11) Uani 1 1 d U . . P006 P 0.0957(3) -0.7149(2) 0.05454(18) 0.0301(11) Uani 1 1 d U . . N101 N 0.2530(7) -0.7703(8) 0.1385(6) 0.033(3) Uani 1 1 d U . . O008 O 0.4037(7) -0.7647(7) 0.0899(5) 0.046(3) Uani 1 1 d U . . N102 N 0.3083(9) -0.7268(8) 0.1695(6) 0.042(4) Uani 1 1 d U . . O101 O 0.6474(8) -0.7029(7) 0.0694(6) 0.074(4) Uani 1 1 d U . . H101 H 0.6155 -0.6924 0.0986 0.112 Uiso 1 1 calc R . . C101 C 0.0116(10) -0.8845(9) 0.3121(7) 0.032(4) Uani 1 1 d U . . H101' H 0.0571 -0.8963 0.3370 0.038 Uiso 1 1 calc R . . C102 C 0.3793(12) -0.7260(10) 0.1470(8) 0.046(5) Uani 1 1 d U . . N014 N 0.4437(9) -0.6852(9) 0.1747(7) 0.052(4) Uani 1 1 d U . . C015 C 0.0938(9) -0.6993(8) 0.2582(7) 0.027(4) Uani 1 1 d U . . C016 C -0.0052(9) -0.6939(8) 0.0754(6) 0.026(4) Uani 1 1 d U . . C017 C -0.1492(10) -0.7166(9) 0.0700(8) 0.039(5) Uani 1 1 d U . . H017 H -0.1910 -0.7434 0.0497 0.047 Uiso 1 1 calc R . . C019 C 0.1639(10) -0.9946(9) -0.0593(7) 0.032(4) Uani 1 1 d U . . H019 H 0.1117 -0.9763 -0.0631 0.039 Uiso 1 1 calc R . . C020 C 0.1108(9) -0.8221(9) -0.0524(6) 0.029(4) Uani 1 1 d U . . H02A H 0.1206 -0.8273 -0.0995 0.035 Uiso 1 1 calc R . . H02B H 0.0666 -0.8558 -0.0409 0.035 Uiso 1 1 calc R . . C021 C 0.2770(10) -0.7915(9) -0.0477(7) 0.032(4) Uani 1 1 d U . . C023 C 0.0170(9) -0.8411(8) 0.2525(7) 0.027(4) Uani 1 1 d U . . C024 C -0.1008(10) -0.6282(9) 0.1476(8) 0.038(4) Uani 1 1 d U . . H024 H -0.1092 -0.5924 0.1812 0.046 Uiso 1 1 calc R . . C025 C -0.1314(10) -0.8497(9) 0.2417(7) 0.032(4) Uani 1 1 d U . . H025 H -0.1771 -0.8374 0.2171 0.039 Uiso 1 1 calc R . . C026 C 0.3408(10) -0.9275(9) 0.1755(7) 0.037(4) Uani 1 1 d U . . C027 C 0.1838(11) -1.0712(9) -0.0796(7) 0.038(4) Uani 1 1 d U . . H027 H 0.1443 -1.1042 -0.0959 0.045 Uiso 1 1 calc R . . C028 C 0.3053(9) -0.8115(9) -0.1123(6) 0.032(4) Uani 1 1 d U . . H028 H 0.2890 -0.8578 -0.1313 0.038 Uiso 1 1 calc R . . C029 C 0.1863(9) -0.8335(8) 0.2827(7) 0.031(4) Uani 1 1 d U . . H02C H 0.2338 -0.8016 0.2793 0.037 Uiso 1 1 calc R . . H02D H 0.1678 -0.8314 0.3281 0.037 Uiso 1 1 calc R . . C030 C -0.0544(9) -0.8249(9) 0.2208(7) 0.034(4) Uani 1 1 d U . . H030 H -0.0520 -0.7951 0.1825 0.041 Uiso 1 1 calc R . . C031 C 0.1619(10) -0.6489(9) 0.2551(7) 0.035(4) Uani 1 1 d U . . H031 H 0.2109 -0.6673 0.2403 0.042 Uiso 1 1 calc R . . N103 N 0.5101(9) -0.6994(8) 0.1343(7) 0.049(4) Uani 1 1 d U . . C033 C -0.1369(10) -0.8925(9) 0.2993(7) 0.038(4) Uani 1 1 d U . . H033 H -0.1861 -0.9092 0.3152 0.046 Uiso 1 1 calc R . . C034 C 0.1005(10) -0.5642(9) 0.0051(7) 0.035(4) Uani 1 1 d U . . H034 H 0.0554 -0.5788 -0.0193 0.042 Uiso 1 1 calc R . . C035 C 0.2240(10) -0.9484(9) -0.0339(7) 0.029(4) Uani 1 1 d U . . C036 C 0.2353(11) -0.5176(10) 0.0768(9) 0.052(5) Uani 1 1 d U . . H036 H 0.2806 -0.5025 0.1007 0.062 Uiso 1 1 calc R . . C037 C 0.2072(9) -0.9185(8) 0.2642(6) 0.028(4) Uani 1 1 d U . . H03A H 0.1623 -0.9515 0.2751 0.034 Uiso 1 1 calc R . . H03B H 0.2531 -0.9352 0.2903 0.034 Uiso 1 1 calc R . . C038 C -0.0651(11) -0.9093(9) 0.3324(8) 0.042(5) Uani 1 1 d U . . H038 H -0.0680 -0.9391 0.3706 0.050 Uiso 1 1 calc R . . C039 C 0.1362(10) -0.6153(9) 0.0510(8) 0.037(4) Uani 1 1 d U . . C040 C 0.1775(9) -1.1873(10) 0.1417(7) 0.041(4) Uani 1 1 d U . . H040 H 0.1654 -1.2391 0.1351 0.049 Uiso 1 1 calc R . . C041 C 0.2611(10) -1.0950(9) -0.0750(7) 0.036(4) Uani 1 1 d U . . H041 H 0.2743 -1.1441 -0.0900 0.043 Uiso 1 1 calc R . . C042 C 0.1768(9) -1.0566(9) 0.1004(7) 0.035(4) Uani 1 1 d U . . H042 H 0.1663 -1.0215 0.0666 0.042 Uiso 1 1 calc R . . C043 C 0.0220(9) -0.6730(9) 0.2834(6) 0.027(4) Uani 1 1 d U . . H043 H -0.0206 -0.7072 0.2875 0.032 Uiso 1 1 calc R . . C044 C -0.0231(10) -0.6414(9) 0.1281(7) 0.032(4) Uani 1 1 d U . . H044 H 0.0186 -0.6158 0.1497 0.039 Uiso 1 1 calc R . . C045 C 0.3219(10) -1.0480(9) -0.0481(7) 0.038(4) Uani 1 1 d U . . H045 H 0.3737 -1.0669 -0.0432 0.046 Uiso 1 1 calc R . . C046 C 0.3839(11) -0.9694(10) 0.1266(8) 0.043(5) Uani 1 1 d U . . H046 H 0.3561 -1.0003 0.0966 0.051 Uiso 1 1 calc R . . C047 C 0.2006(10) -0.5921(10) 0.0859(8) 0.042(5) Uani 1 1 d U . . H047 H 0.2232 -0.6254 0.1170 0.050 Uiso 1 1 calc R . . C048 C -0.1676(11) -0.6649(9) 0.1202(7) 0.041(5) Uani 1 1 d U . . H048 H -0.2196 -0.6556 0.1342 0.049 Uiso 1 1 calc R . . C049 C 0.0124(9) -0.5958(9) 0.3029(7) 0.030(4) Uani 1 1 d U . . H049 H -0.0365 -0.5783 0.3188 0.036 Uiso 1 1 calc R . . C050 C 0.1347(11) -0.4900(10) -0.0029(8) 0.045(5) Uani 1 1 d U . . H050 H 0.1121 -0.4549 -0.0325 0.054 Uiso 1 1 calc R . . C051' C 0.5314(11) -0.7710(10) 0.0274(8) 0.044(5) Uani 1 1 d U . . C052 C -0.0724(10) -0.7303(9) 0.0487(8) 0.041(5) Uani 1 1 d U . . H052 H -0.0651 -0.7658 0.0147 0.049 Uiso 1 1 calc R . . C053 C 0.2009(10) -0.4707(10) 0.0331(8) 0.041(4) Uani 1 1 d U . . H053 H 0.2232 -0.4221 0.0267 0.049 Uiso 1 1 calc R . . C054 C 0.4879(12) -0.7452(11) 0.0886(9) 0.056(5) Uani 1 1 d U . . C055 C 0.2312(10) -1.0864(9) 0.2103(8) 0.043(5) Uani 1 1 d U . . H055 H 0.2581 -1.0703 0.2484 0.052 Uiso 1 1 calc R . . C056 C 0.2985(10) -0.7199(10) -0.0203(8) 0.040(4) Uani 1 1 d U . . H056 H 0.2802 -0.7054 0.0213 0.048 Uiso 1 1 calc R . . C057 C 0.2088(9) -1.0329(9) 0.1605(7) 0.031(4) Uani 1 1 d U . . C058 C 0.3841(11) -0.8812(10) 0.2197(8) 0.042(5) Uani 1 1 d U . . H058 H 0.3573 -0.8547 0.2529 0.051 Uiso 1 1 calc R . . C059 C 0.0797(10) -0.5443(9) 0.2977(7) 0.032(4) Uani 1 1 d U . . H059 H 0.0737 -0.4929 0.3097 0.039 Uiso 1 1 calc R . . C060 C 0.3041(10) -0.9737(9) -0.0291(7) 0.035(4) Uani 1 1 d U . . H060 H 0.3441 -0.9410 -0.0133 0.042 Uiso 1 1 calc R . . C061 C 0.1539(10) -0.5703(9) 0.2750(7) 0.035(4) Uani 1 1 d U . . H061 H 0.1973 -0.5368 0.2730 0.042 Uiso 1 1 calc R . . C062 C 0.1606(10) -1.1351(9) 0.0921(7) 0.040(4) Uani 1 1 d U . . H062 H 0.1382 -1.1524 0.0524 0.048 Uiso 1 1 calc R . . C063 C 0.6090(12) -0.7494(11) 0.0205(9) 0.056(5) Uani 1 1 d U . . C064 C 0.0892(10) -0.7369(9) -0.0358(7) 0.034(4) Uani 1 1 d U . . H06A H 0.0351 -0.7264 -0.0514 0.041 Uiso 1 1 calc R . . H06B H 0.1252 -0.7029 -0.0594 0.041 Uiso 1 1 calc R . . C065 C 0.4656(11) -0.8743(10) 0.2148(8) 0.047(5) Uani 1 1 d U . . H065 H 0.4939 -0.8418 0.2433 0.056 Uiso 1 1 calc R . . C067 C 0.4658(11) -0.9649(10) 0.1232(8) 0.050(5) Uani 1 1 d U . . H067 H 0.4931 -0.9941 0.0921 0.060 Uiso 1 1 calc R . . C068 C 0.3559(11) -0.7642(11) -0.1469(8) 0.050(5) Uani 1 1 d U . . H068 H 0.3750 -0.7786 -0.1882 0.060 Uiso 1 1 calc R . . C069 C 0.6511(12) -0.7718(11) -0.0381(9) 0.057(5) Uani 1 1 d U . . H069 H 0.7040 -0.7562 -0.0433 0.068 Uiso 1 1 calc R . . C070 C 0.3492(10) -0.6698(10) -0.0574(7) 0.043(5) Uani 1 1 d U . . H070 H 0.3628 -0.6214 -0.0409 0.052 Uiso 1 1 calc R . . C073 C 0.4952(11) -0.8176(11) -0.0225(8) 0.059(5) Uani 1 1 d U . . H073 H 0.4430 -0.8352 -0.0173 0.071 Uiso 1 1 calc R . . C074 C 0.2115(11) -1.1648(10) 0.2005(8) 0.049(5) Uani 1 1 d U . . H074 H 0.2216 -1.2008 0.2336 0.059 Uiso 1 1 calc R . . C075 C 0.6152(12) -0.8158(12) -0.0870(9) 0.064(6) Uani 1 1 d U . . H075 H 0.6442 -0.8302 -0.1241 0.077 Uiso 1 1 calc R . . C077 C 0.5389(11) -0.8376(10) -0.0811(8) 0.053(5) Uani 1 1 d U . . H077 H 0.5140 -0.8657 -0.1148 0.063 Uiso 1 1 calc R . . C078 C 0.5070(11) -0.9178(11) 0.1652(9) 0.053(5) Uani 1 1 d U . . H078 H 0.5623 -0.9137 0.1618 0.064 Uiso 1 1 calc R . . C080 C 0.3778(10) -0.6937(10) -0.1182(7) 0.045(5) Uani 1 1 d U . . H080 H 0.4130 -0.6616 -0.1409 0.054 Uiso 1 1 calc R . . O501 O 0.490(3) -0.494(3) -0.0266(17) 0.140(15) Uiso 0.50 1 d P . 1 O501' O 0.453(3) -0.459(3) 0.074(2) 0.19(2) Uiso 0.50 1 d P A 2 C501'' C 0.479(3) -0.503(3) -0.102(3) 0.113(19) Uiso 0.50 1 d P B 1 C501''' C 0.422(3) -0.418(3) 0.134(3) 0.114(19) Uiso 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W001 0.0407(5) 0.0260(4) 0.0189(4) 0.0001(4) 0.0073(3) -0.0005(4) Br02 0.0459(13) 0.0310(10) 0.0288(9) -0.0019(8) 0.0084(9) -0.0025(8) P003 0.035(3) 0.034(2) 0.023(2) -0.0007(18) 0.008(2) -0.0027(19) P004 0.039(3) 0.026(2) 0.022(2) -0.0015(17) 0.005(2) -0.0019(18) P005 0.039(3) 0.027(2) 0.025(2) -0.0003(18) 0.009(2) 0.002(2) P006 0.046(3) 0.027(2) 0.017(2) 0.0004(17) 0.007(2) -0.002(2) N101 0.030(7) 0.045(7) 0.025(6) 0.023(6) -0.003(6) 0.012(6) O008 0.054(7) 0.048(6) 0.036(6) -0.001(5) -0.003(5) 0.005(5) N102 0.037(7) 0.042(7) 0.046(7) -0.002(6) 0.000(6) -0.002(6) O101 0.072(8) 0.076(8) 0.076(7) -0.010(6) 0.003(6) -0.001(6) C101 0.038(8) 0.032(7) 0.025(7) 0.002(6) 0.009(6) -0.001(6) C102 0.046(9) 0.050(8) 0.043(8) -0.004(7) 0.008(7) -0.004(7) N014 0.055(8) 0.053(7) 0.047(7) -0.011(7) 0.007(6) -0.010(7) C015 0.027(8) 0.026(7) 0.028(7) 0.000(6) 0.004(6) -0.001(6) C016 0.031(8) 0.029(7) 0.017(6) 0.012(6) 0.003(6) -0.005(6) C017 0.041(9) 0.039(8) 0.037(7) 0.004(7) -0.005(7) -0.004(7) C019 0.034(8) 0.036(8) 0.027(7) 0.001(6) 0.003(6) -0.011(6) C020 0.039(8) 0.032(7) 0.016(6) -0.007(6) 0.005(6) 0.004(7) C021 0.032(8) 0.034(8) 0.029(7) -0.005(6) 0.006(6) -0.004(6) C023 0.030(8) 0.025(7) 0.026(7) -0.008(6) 0.008(6) 0.003(6) C024 0.044(8) 0.036(8) 0.035(7) 0.005(7) 0.003(7) 0.001(7) C025 0.035(8) 0.035(7) 0.028(7) -0.009(6) 0.001(7) 0.000(6) C026 0.042(8) 0.038(8) 0.033(7) 0.004(6) 0.004(7) 0.002(7) C027 0.047(9) 0.032(8) 0.033(7) -0.006(6) 0.000(7) -0.008(7) C028 0.038(8) 0.038(7) 0.019(6) 0.001(6) 0.016(6) -0.006(7) C029 0.038(8) 0.029(7) 0.027(7) -0.003(6) 0.006(6) 0.007(6) C030 0.047(8) 0.026(7) 0.030(7) -0.009(6) -0.002(7) 0.004(7) C031 0.040(8) 0.036(8) 0.029(7) -0.001(6) 0.013(7) 0.003(6) N103 0.047(8) 0.055(8) 0.044(7) -0.018(6) -0.002(6) -0.014(6) C033 0.043(8) 0.032(7) 0.039(7) -0.007(6) 0.005(7) -0.002(7) C034 0.045(8) 0.039(8) 0.021(7) -0.001(6) 0.013(6) 0.004(7) C035 0.036(8) 0.030(7) 0.022(7) -0.001(6) 0.009(6) -0.001(6) C036 0.055(9) 0.046(8) 0.054(8) -0.008(7) 0.005(7) -0.004(7) C037 0.038(8) 0.030(7) 0.016(6) 0.003(6) 0.014(6) 0.004(6) C038 0.056(9) 0.034(8) 0.035(7) -0.003(6) 0.014(7) 0.003(7) C039 0.046(8) 0.031(7) 0.035(7) 0.011(6) 0.011(7) 0.005(7) C040 0.043(8) 0.036(8) 0.045(7) -0.008(7) 0.010(7) 0.000(7) C041 0.041(8) 0.036(8) 0.031(7) -0.004(6) 0.015(7) 0.001(7) C042 0.042(8) 0.034(7) 0.030(7) -0.005(6) 0.002(7) -0.001(7) C043 0.028(7) 0.026(7) 0.027(6) 0.005(6) 0.006(6) -0.004(6) C044 0.031(8) 0.035(7) 0.031(7) 0.003(6) 0.002(7) -0.003(6) C045 0.037(8) 0.038(8) 0.040(7) 0.006(7) 0.005(7) 0.003(7) C046 0.048(9) 0.038(8) 0.041(8) -0.009(7) -0.003(7) -0.004(7) C047 0.045(8) 0.040(8) 0.041(8) 0.006(7) 0.001(7) -0.004(7) C048 0.045(8) 0.042(8) 0.036(7) 0.006(7) 0.003(7) 0.002(7) C049 0.034(8) 0.030(7) 0.027(7) 0.000(6) 0.006(6) 0.000(6) C050 0.059(9) 0.036(8) 0.040(8) 0.005(7) 0.006(7) -0.002(7) C051 0.046(9) 0.043(8) 0.044(8) 0.000(7) 0.008(7) -0.001(7) C052 0.049(9) 0.034(8) 0.041(8) 0.003(7) 0.001(7) 0.002(7) C053 0.045(8) 0.033(8) 0.046(8) 0.004(7) 0.006(7) -0.004(7) C054 0.055(9) 0.052(9) 0.061(9) 0.010(7) 0.013(8) 0.000(7) C055 0.054(9) 0.035(8) 0.041(8) 0.002(7) 0.005(7) 0.004(7) C056 0.044(8) 0.046(8) 0.031(7) 0.005(7) 0.011(7) -0.007(7) C057 0.038(8) 0.026(7) 0.030(7) 0.001(6) 0.012(6) -0.001(6) C058 0.048(9) 0.049(8) 0.030(7) -0.001(7) 0.006(7) 0.003(7) C059 0.039(8) 0.033(7) 0.025(7) 0.004(6) 0.011(6) 0.004(7) C060 0.035(8) 0.034(8) 0.037(7) -0.001(6) -0.002(7) -0.008(6) C061 0.038(8) 0.039(8) 0.029(7) 0.004(6) 0.015(7) -0.007(7) C062 0.051(9) 0.035(8) 0.033(7) -0.008(6) 0.004(7) -0.001(7) C063 0.056(9) 0.052(9) 0.060(9) 0.003(7) -0.001(8) -0.002(7) C064 0.042(8) 0.032(7) 0.028(7) 0.005(6) 0.001(6) 0.005(6) C065 0.052(9) 0.052(8) 0.036(7) -0.003(7) -0.005(7) -0.003(7) C067 0.055(9) 0.046(8) 0.048(8) -0.011(7) 0.010(7) -0.001(7) C068 0.054(9) 0.054(9) 0.042(8) 0.001(7) 0.012(7) -0.002(7) C069 0.052(9) 0.064(9) 0.055(8) 0.000(7) 0.017(8) 0.004(7) C070 0.049(8) 0.049(8) 0.032(7) 0.000(7) 0.014(7) -0.005(7) C073 0.060(9) 0.057(9) 0.061(8) 0.006(8) 0.004(8) -0.004(8) C074 0.060(9) 0.041(8) 0.047(8) 0.007(7) 0.016(7) 0.003(7) C075 0.061(9) 0.067(9) 0.065(9) -0.008(8) 0.007(8) -0.002(8) C077 0.051(9) 0.058(9) 0.049(8) -0.007(7) 0.013(7) 0.004(7) C078 0.043(9) 0.061(9) 0.056(8) 0.006(7) 0.009(7) 0.008(7) C080 0.043(8) 0.056(9) 0.036(7) 0.010(7) 0.010(7) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W001 N101 1.717(14) . ? W001 P005 2.481(4) . ? W001 P006 2.485(4) . ? W001 P003 2.529(4) . ? W001 P004 2.529(4) . ? W001 Br02 2.6254(19) . ? P003 C021 1.838(16) . ? P003 C035 1.846(15) . ? P003 C020 1.846(14) . ? P004 C023 1.793(15) . ? P004 C029 1.802(14) . ? P004 C015 1.831(14) . ? P005 C057 1.853(15) . ? P005 C037 1.862(12) . ? P005 C026 1.845(17) . ? P006 C016 1.777(16) . ? P006 C064 1.866(14) . ? P006 C039 1.855(16) . ? N101 N102 1.341(17) . ? O008 C102 1.397(19) . ? O008 C054 1.45(2) . ? N102 C102 1.273(19) . ? O101 C063 1.42(2) . ? C101 C038 1.41(2) . ? C101 C023 1.424(19) . ? C102 N014 1.40(2) . ? N014 N103 1.403(18) . ? C015 C043 1.383(19) . ? C015 C031 1.43(2) . ? C016 C052 1.39(2) . ? C016 C044 1.43(2) . ? C017 C052 1.38(2) . ? C017 C048 1.39(2) . ? C019 C035 1.38(2) . ? C019 C027 1.43(2) . ? C020 C064 1.56(2) . ? C021 C056 1.40(2) . ? C021 C028 1.434(19) . ? C023 C030 1.37(2) . ? C024 C044 1.38(2) . ? C024 C048 1.39(2) . ? C025 C033 1.38(2) . ? C025 C030 1.42(2) . ? C026 C058 1.40(2) . ? C026 C046 1.42(2) . ? C027 C041 1.36(2) . ? C028 C068 1.37(2) . ? C029 C037 1.558(19) . ? C031 C061 1.43(2) . ? N103 C054 1.27(2) . ? C033 C038 1.40(2) . ? C034 C039 1.41(2) . ? C034 C050 1.42(2) . ? C035 C060 1.41(2) . ? C036 C053 1.33(2) . ? C036 C047 1.43(2) . ? C039 C047 1.34(2) . ? C040 C074 1.37(2) . ? C040 C062 1.38(2) . ? C041 C045 1.41(2) . ? C042 C057 1.38(2) . ? C042 C062 1.40(2) . ? C043 C049 1.41(2) . ? C045 C060 1.38(2) . ? C046 C067 1.37(2) . ? C049 C059 1.44(2) . ? C050 C053 1.36(2) . ? C051 C063 1.36(2) . ? C051 C073 1.42(2) . ? C051 C054 1.51(2) . ? C055 C074 1.41(2) . ? C055 C057 1.41(2) . ? C056 C070 1.43(2) . ? C058 C065 1.37(2) . ? C059 C061 1.398(19) . ? C063 C069 1.44(2) . ? C065 C078 1.44(2) . ? C067 C078 1.36(2) . ? C068 C080 1.40(2) . ? C069 C075 1.38(2) . ? C070 C080 1.39(2) . ? C073 C077 1.44(2) . ? C075 C077 1.34(2) . ? O501 O501 1.14(7) 3_645 ? O501 C501 1.54(6) . ? O501 C501 1.49(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N101 W001 P005 84.4(4) . . ? N101 W001 P006 100.0(4) . . ? P005 W001 P006 175.31(15) . . ? N101 W001 P003 100.9(4) . . ? P005 W001 P003 102.38(13) . . ? P006 W001 P003 78.47(13) . . ? N101 W001 P004 89.6(4) . . ? P005 W001 P004 80.43(13) . . ? P006 W001 P004 97.91(13) . . ? P003 W001 P004 169.29(14) . . ? N101 W001 Br02 173.4(4) . . ? P005 W001 Br02 89.55(11) . . ? P006 W001 Br02 85.97(11) . . ? P003 W001 Br02 82.87(11) . . ? P004 W001 Br02 86.83(10) . . ? C021 P003 C035 102.6(7) . . ? C021 P003 C020 100.1(7) . . ? C035 P003 C020 104.2(7) . . ? C021 P003 W001 119.3(5) . . ? C035 P003 W001 122.8(5) . . ? C020 P003 W001 104.8(4) . . ? C023 P004 C029 107.0(7) . . ? C023 P004 C015 99.9(7) . . ? C029 P004 C015 102.5(7) . . ? C023 P004 W001 122.3(5) . . ? C029 P004 W001 103.0(5) . . ? C015 P004 W001 120.1(5) . . ? C057 P005 C037 101.9(6) . . ? C057 P005 C026 102.1(7) . . ? C037 P005 C026 101.9(7) . . ? C057 P005 W001 126.1(5) . . ? C037 P005 W001 108.1(5) . . ? C026 P005 W001 113.8(5) . . ? C016 P006 C064 103.1(7) . . ? C016 P006 C039 99.5(7) . . ? C064 P006 C039 99.8(7) . . ? C016 P006 W001 119.6(5) . . ? C064 P006 W001 110.4(5) . . ? C039 P006 W001 121.4(6) . . ? N102 N101 W001 166.5(12) . . ? C102 O008 C054 101.2(14) . . ? C102 N102 N101 118.6(14) . . ? C038 C101 C023 118.0(15) . . ? N102 C102 N014 125.3(16) . . ? N102 C102 O008 124.6(16) . . ? N014 C102 O008 110.1(16) . . ? C102 N014 N103 106.6(13) . . ? C043 C015 C031 120.3(14) . . ? C043 C015 P004 123.8(11) . . ? C031 C015 P004 115.9(12) . . ? C052 C016 C044 113.7(15) . . ? C052 C016 P006 125.3(13) . . ? C044 C016 P006 120.7(12) . . ? C052 C017 C048 123.5(17) . . ? C035 C019 C027 118.4(16) . . ? C064 C020 P003 109.0(10) . . ? C056 C021 C028 119.2(14) . . ? C056 C021 P003 118.4(11) . . ? C028 C021 P003 121.9(12) . . ? C030 C023 C101 116.1(15) . . ? C030 C023 P004 121.8(12) . . ? C101 C023 P004 121.4(12) . . ? C044 C024 C048 124.2(16) . . ? C033 C025 C030 118.6(15) . . ? C058 C026 C046 118.3(16) . . ? C058 C026 P005 121.8(13) . . ? C046 C026 P005 119.8(13) . . ? C041 C027 C019 119.0(15) . . ? C068 C028 C021 121.9(16) . . ? C037 C029 P004 109.8(10) . . ? C023 C030 C025 125.5(15) . . ? C061 C031 C015 119.5(15) . . ? C054 N103 N014 107.8(15) . . ? C025 C033 C038 116.8(16) . . ? C039 C034 C050 118.5(16) . . ? C019 C035 C060 122.1(15) . . ? C019 C035 P003 120.3(13) . . ? C060 C035 P003 117.5(12) . . ? C053 C036 C047 117.7(18) . . ? C029 C037 P005 112.1(10) . . ? C101 C038 C033 124.9(15) . . ? C047 C039 C034 119.2(16) . . ? C047 C039 P006 123.3(13) . . ? C034 C039 P006 117.3(13) . . ? C074 C040 C062 121.6(16) . . ? C027 C041 C045 122.1(16) . . ? C057 C042 C062 117.9(15) . . ? C049 C043 C015 121.2(14) . . ? C024 C044 C016 121.4(15) . . ? C041 C045 C060 119.6(16) . . ? C067 C046 C026 121.1(16) . . ? C039 C047 C036 121.9(17) . . ? C017 C048 C024 113.8(16) . . ? C043 C049 C059 118.6(15) . . ? C053 C050 C034 119.4(16) . . ? C063 C051 C073 118.9(17) . . ? C063 C051 C054 118.1(17) . . ? C073 C051 C054 122.9(17) . . ? C017 C052 C016 123.4(16) . . ? C036 C053 C050 123.3(17) . . ? N103 C054 O008 114.1(16) . . ? N103 C054 C051 129.9(18) . . ? O008 C054 C051 115.0(16) . . ? C074 C055 C057 118.1(16) . . ? C070 C056 C021 118.7(15) . . ? C042 C057 C055 121.7(14) . . ? C042 C057 P005 119.7(11) . . ? C055 C057 P005 118.4(12) . . ? C065 C058 C026 120.8(16) . . ? C061 C059 C049 121.3(15) . . ? C035 C060 C045 118.6(15) . . ? C059 C061 C031 119.0(15) . . ? C040 C062 C042 121.0(15) . . ? C051 C063 O101 120.6(17) . . ? C051 C063 C069 119.1(18) . . ? O101 C063 C069 120.3(18) . . ? C020 C064 P006 113.1(10) . . ? C058 C065 C078 119.3(17) . . ? C078 C067 C046 120.1(17) . . ? C028 C068 C080 118.1(16) . . ? C075 C069 C063 121.8(19) . . ? C080 C070 C056 119.7(17) . . ? C077 C073 C051 120.3(17) . . ? C040 C074 C055 119.4(17) . . ? C077 C075 C069 120.0(19) . . ? C075 C077 C073 119.8(18) . . ? C067 C078 C065 120.5(18) . . ? C068 C080 C070 122.4(16) . . ? O501' O501 C501 160(7) 3_645 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 54.22 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.183 _refine_diff_density_min -0.911 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 651022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C123 H114 Br2 Cl2 N10 O6 P8 Pd W2' _chemical_formula_weight 2780.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 17.84(2) _cell_length_b 14.861(17) _cell_length_c 27.18(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.124(10) _cell_angle_gamma 90.00 _cell_volume 7072(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 2.491 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24323 _diffrn_reflns_av_R_equivalents 0.1374 _diffrn_reflns_av_sigmaI/netI 0.3025 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 26.41 _reflns_number_total 9167 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+17.0860P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9167 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2836 _refine_ls_R_factor_gt 0.1381 _refine_ls_wR_factor_ref 0.3051 _refine_ls_wR_factor_gt 0.2638 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.26247(7) 0.18532(8) 0.02089(4) 0.0503(4) Uani 1 1 d . . . Br2 Br 0.3615(2) 0.0518(2) 0.01906(14) 0.0982(13) Uani 1 1 d . . . N100 N 0.2024(14) 0.2709(15) 0.0241(8) 0.075(8) Uiso 1 1 d . . . N101 N 0.1437(12) 0.3374(14) 0.0186(7) 0.052(6) Uiso 1 1 d . . . C102 C 0.1513(19) 0.410(2) 0.0467(11) 0.076(10) Uiso 1 1 d . . . N103 N 0.1059(15) 0.4745(19) 0.0441(9) 0.093(9) Uiso 1 1 d . . . N104 N 0.1348(19) 0.538(2) 0.0825(12) 0.127(11) Uiso 1 1 d . . . C105 C 0.201(2) 0.506(2) 0.0980(11) 0.086(10) Uiso 1 1 d . . . O106 O 0.2160(11) 0.4286(13) 0.0783(7) 0.072(6) Uiso 1 1 d . . . C111 C 0.2635(11) 0.5530(13) 0.1381(6) 0.062(8) Uiso 1 1 d G . . C112 C 0.2402(9) 0.6229(14) 0.1657(8) 0.121(13) Uiso 1 1 d G . . H112 H 0.1889 0.6385 0.1609 0.145 Uiso 1 1 calc R . . C113 C 0.2938(14) 0.6694(11) 0.2004(7) 0.117(12) Uiso 1 1 d G . . H113 H 0.2782 0.7161 0.2189 0.141 Uiso 1 1 calc R . . C114 C 0.3705(12) 0.6460(13) 0.2075(6) 0.070(9) Uiso 1 1 d G . . C115 C 0.3938(8) 0.5761(14) 0.1799(7) 0.103(11) Uiso 1 1 d G . . H115 H 0.4451 0.5605 0.1847 0.124 Uiso 1 1 calc R . . C116 C 0.3402(12) 0.5296(10) 0.1452(6) 0.072(9) Uiso 1 1 d G . . H116 H 0.3558 0.4829 0.1268 0.087 Uiso 1 1 calc R . . C117 C 0.428(2) 0.692(3) 0.2404(16) 0.145(16) Uiso 1 1 d . . . N118 N 0.4712(18) 0.736(2) 0.2674(12) 0.140(13) Uiso 1 1 d . . . Pd1 Pd 0.0000 0.5000 0.0000 0.0790(12) Uani 1 2 d S . . Cl1 Cl 0.0588(5) 0.5762(7) -0.0551(4) 0.129(4) Uani 1 1 d . . . P1 P 0.3272(5) 0.2043(5) 0.1123(3) 0.061(2) Uani 1 1 d . . . C2 C 0.4219(14) 0.2698(17) 0.1117(9) 0.064(8) Uiso 1 1 d . . . H2A H 0.4144 0.3326 0.1193 0.077 Uiso 1 1 calc R . . H2B H 0.4616 0.2461 0.1379 0.077 Uiso 1 1 calc R . . C3 C 0.4456(16) 0.2645(19) 0.0673(10) 0.080(10) Uiso 1 1 d . . . H3A H 0.4699 0.2063 0.0662 0.096 Uiso 1 1 calc R . . H3B H 0.4849 0.3097 0.0677 0.096 Uiso 1 1 calc R . . P4 P 0.3795(5) 0.2772(5) 0.0104(3) 0.073(3) Uani 1 1 d . . . C11 C 0.2857(12) 0.2644(11) 0.1570(7) 0.057(8) Uiso 1 1 d G . . C12 C 0.3277(8) 0.3024(13) 0.2004(8) 0.108(11) Uiso 1 1 d G . . H12 H 0.3805 0.2954 0.2080 0.129 Uiso 1 1 calc R . . C13 C 0.2909(13) 0.3508(12) 0.2325(6) 0.109(12) Uiso 1 1 d G . . H13 H 0.3190 0.3763 0.2616 0.131 Uiso 1 1 calc R . . C14 C 0.2120(13) 0.3613(11) 0.2212(7) 0.116(13) Uiso 1 1 d G . . H14 H 0.1873 0.3937 0.2427 0.139 Uiso 1 1 calc R . . C15 C 0.1700(8) 0.3233(13) 0.1778(8) 0.112(12) Uiso 1 1 d G . . H15 H 0.1172 0.3302 0.1702 0.134 Uiso 1 1 calc R . . C16 C 0.2068(11) 0.2748(12) 0.1457(6) 0.073(9) Uiso 1 1 d G . . H16 H 0.1787 0.2494 0.1167 0.088 Uiso 1 1 calc R . . C21 C 0.3621(15) 0.1060(12) 0.1579(7) 0.075(9) Uiso 1 1 d G . . C22 C 0.4330(14) 0.0681(17) 0.1570(8) 0.141(15) Uiso 1 1 d G . . H22 H 0.4643 0.0932 0.1369 0.169 Uiso 1 1 calc R . . C23 C 0.4572(11) -0.0072(17) 0.1860(10) 0.20(2) Uiso 1 1 d G . . H23 H 0.5047 -0.0325 0.1854 0.237 Uiso 1 1 calc R . . C24 C 0.4105(17) -0.0447(12) 0.2160(8) 0.129(14) Uiso 1 1 d G . . H24 H 0.4267 -0.0951 0.2355 0.155 Uiso 1 1 calc R . . C25 C 0.3396(15) -0.0069(16) 0.2169(8) 0.156(17) Uiso 1 1 d G . . H25 H 0.3083 -0.0320 0.2370 0.188 Uiso 1 1 calc R . . C26 C 0.3153(11) 0.0685(16) 0.1879(9) 0.122(13) Uiso 1 1 d G . . H26 H 0.2679 0.0938 0.1885 0.146 Uiso 1 1 calc R . . C31 C 0.4285(12) 0.2618(14) -0.0421(7) 0.076(9) Uiso 1 1 d G . . C32 C 0.4022(10) 0.3034(12) -0.0880(9) 0.107(11) Uiso 1 1 d G . . H32 H 0.3620 0.3442 -0.0914 0.128 Uiso 1 1 calc R . . C33 C 0.4359(13) 0.2841(14) -0.1288(6) 0.133(14) Uiso 1 1 d G . . H33 H 0.4183 0.3119 -0.1595 0.160 Uiso 1 1 calc R . . C34 C 0.4960(13) 0.2231(15) -0.1237(8) 0.113(13) Uiso 1 1 d G . . H34 H 0.5185 0.2101 -0.1510 0.136 Uiso 1 1 calc R . . C35 C 0.5223(10) 0.1815(12) -0.0778(10) 0.157(16) Uiso 1 1 d G . . H35 H 0.5625 0.1407 -0.0744 0.188 Uiso 1 1 calc R . . C36 C 0.4886(13) 0.2008(14) -0.0370(7) 0.104(11) Uiso 1 1 d G . . H36 H 0.5062 0.1730 -0.0063 0.125 Uiso 1 1 calc R . . C41 C 0.3621(15) 0.4055(11) 0.0090(7) 0.070(9) Uiso 1 1 d G . . C42 C 0.2935(11) 0.4438(17) -0.0146(7) 0.115(13) Uiso 1 1 d G . . H42 H 0.2535 0.4073 -0.0301 0.138 Uiso 1 1 calc R . . C43 C 0.2848(12) 0.5368(19) -0.0152(8) 0.138(15) Uiso 1 1 d G . . H43 H 0.2389 0.5625 -0.0311 0.166 Uiso 1 1 calc R . . C44 C 0.3446(17) 0.5914(11) 0.0078(9) 0.185(19) Uiso 1 1 d G . . H44 H 0.3387 0.6536 0.0074 0.222 Uiso 1 1 calc R . . C45 C 0.4131(14) 0.5530(16) 0.0315(8) 0.114(13) Uiso 1 1 d G . . H45 H 0.4532 0.5895 0.0469 0.137 Uiso 1 1 calc R . . C46 C 0.4219(10) 0.4600(17) 0.0321(7) 0.107(12) Uiso 1 1 d G . . H46 H 0.4678 0.4344 0.0479 0.128 Uiso 1 1 calc R . . P5 P 0.2003(6) 0.1551(6) -0.0726(4) 0.104(4) Uani 1 1 d . . . C6 C 0.098(2) 0.142(2) -0.0668(13) 0.131(14) Uiso 1 1 d . . . H6A H 0.0800 0.1964 -0.0535 0.157 Uiso 1 1 calc R . . H6B H 0.0666 0.1312 -0.0998 0.157 Uiso 1 1 calc R . . C7 C 0.088(2) 0.062(2) -0.0322(13) 0.129(14) Uiso 1 1 d . . . H7A H 0.0959 0.0060 -0.0486 0.154 Uiso 1 1 calc R . . H7B H 0.0368 0.0623 -0.0253 0.154 Uiso 1 1 calc R . . P8 P 0.1612(6) 0.0722(6) 0.0300(4) 0.095(3) Uani 1 1 d . . . C61 C 0.1769(17) 0.2565(17) -0.1175(10) 0.115(13) Uiso 1 1 d G . . C62 C 0.2144(13) 0.2576(17) -0.1578(12) 0.150(16) Uiso 1 1 d G . . H62 H 0.2454 0.2095 -0.1629 0.181 Uiso 1 1 calc R . . C63 C 0.2057(16) 0.331(2) -0.1904(9) 0.20(2) Uiso 1 1 d G . . H63 H 0.2308 0.3313 -0.2173 0.243 Uiso 1 1 calc R . . C64 C 0.1595(18) 0.4024(17) -0.1827(12) 0.172(18) Uiso 1 1 d G . . H64 H 0.1536 0.4513 -0.2045 0.206 Uiso 1 1 calc R . . C65 C 0.1219(14) 0.4013(18) -0.1424(14) 0.21(2) Uiso 1 1 d G . . H65 H 0.0910 0.4494 -0.1372 0.256 Uiso 1 1 calc R . . C66 C 0.1306(16) 0.328(3) -0.1098(10) 0.23(2) Uiso 1 1 d G . . H66 H 0.1055 0.3277 -0.0828 0.271 Uiso 1 1 calc R . . C51 C 0.2339(18) 0.0769(14) -0.1105(8) 0.088(10) Uiso 1 1 d G . . C52 C 0.3113(16) 0.0757(16) -0.1118(9) 0.132(14) Uiso 1 1 d G . . H52 H 0.3445 0.1147 -0.0914 0.159 Uiso 1 1 calc R . . C53 C 0.3392(12) 0.016(2) -0.1434(12) 0.22(2) Uiso 1 1 d G . . H53 H 0.3911 0.0155 -0.1442 0.264 Uiso 1 1 calc R . . C54 C 0.290(2) -0.0419(16) -0.1738(9) 0.21(2) Uiso 1 1 d G . . H54 H 0.3083 -0.0817 -0.1950 0.246 Uiso 1 1 calc R . . C55 C 0.2121(19) -0.0408(16) -0.1725(9) 0.177(18) Uiso 1 1 d G . . H55 H 0.1790 -0.0797 -0.1928 0.213 Uiso 1 1 calc R . . C56 C 0.1842(11) 0.019(2) -0.1409(11) 0.159(16) Uiso 1 1 d G . . H56 H 0.1324 0.0194 -0.1400 0.191 Uiso 1 1 calc R . . C71 C 0.0955(10) 0.0949(15) 0.0748(7) 0.061(8) Uiso 1 1 d G . . C72 C 0.0972(11) 0.0443(11) 0.1180(9) 0.115(12) Uiso 1 1 d G . . H72 H 0.1284 -0.0062 0.1240 0.138 Uiso 1 1 calc R . . C73 C 0.0524(13) 0.0692(15) 0.1523(7) 0.127(14) Uiso 1 1 d G . . H73 H 0.0535 0.0354 0.1812 0.153 Uiso 1 1 calc R . . C74 C 0.0058(11) 0.1447(16) 0.1433(8) 0.121(13) Uiso 1 1 d G . . H74 H -0.0242 0.1614 0.1662 0.146 Uiso 1 1 calc R . . C75 C 0.0040(10) 0.1953(12) 0.1000(9) 0.122(13) Uiso 1 1 d G . . H75 H -0.0271 0.2458 0.0940 0.146 Uiso 1 1 calc R . . C76 C 0.0489(12) 0.1704(14) 0.0658(7) 0.124(13) Uiso 1 1 d G . . H76 H 0.0477 0.2042 0.0369 0.149 Uiso 1 1 calc R . . C81 C 0.1845(14) -0.0521(12) 0.0427(8) 0.069(9) Uiso 1 1 d G . . C82 C 0.2498(12) -0.0772(17) 0.0767(8) 0.111(12) Uiso 1 1 d G . . H82 H 0.2832 -0.0335 0.0925 0.134 Uiso 1 1 calc R . . C83 C 0.2650(12) -0.168(2) 0.0870(8) 0.153(16) Uiso 1 1 d G . . H83 H 0.3087 -0.1845 0.1097 0.184 Uiso 1 1 calc R . . C84 C 0.2149(19) -0.2331(12) 0.0633(11) 0.173(18) Uiso 1 1 d G . . H84 H 0.2251 -0.2936 0.0702 0.207 Uiso 1 1 calc R . . C85 C 0.1497(16) -0.2079(17) 0.0294(10) 0.189(19) Uiso 1 1 d G . . H85 H 0.1162 -0.2517 0.0136 0.226 Uiso 1 1 calc R . . C86 C 0.1344(10) -0.117(2) 0.0191(7) 0.148(16) Uiso 1 1 d G . . H86 H 0.0908 -0.1006 -0.0036 0.177 Uiso 1 1 calc R . . O100 O 0.683(5) 0.291(6) 0.118(4) 0.24(4) Uiso 0.50 1 d P A 1 H100 H 0.6644 0.2455 0.1275 0.291 Uiso 0.50 1 calc PR A 1 C101 C 0.644(5) 0.382(5) 0.137(3) 0.16(3) Uiso 0.50 1 d P A 1 H10A H 0.6752 0.4023 0.1681 0.188 Uiso 0.50 1 calc PR A 1 H10B H 0.5940 0.3670 0.1430 0.188 Uiso 0.50 1 calc PR A 1 H10C H 0.6403 0.4279 0.1124 0.188 Uiso 0.50 1 calc PR A 1 O300 O 0.748(5) 0.261(6) 0.091(3) 0.29(4) Uiso 0.50 1 d P B 2 O400 O 0.731(6) 0.343(7) 0.148(4) 0.33(5) Uiso 0.50 1 d P C 2 O200 O 0.916(5) 0.303(5) 0.259(3) 0.31(4) Uiso 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0516(8) 0.0439(8) 0.0547(7) -0.0029(7) 0.0086(5) 0.0047(8) Br2 0.092(3) 0.071(3) 0.134(4) -0.004(2) 0.029(2) 0.004(2) Pd1 0.061(3) 0.061(3) 0.107(3) -0.010(2) -0.004(2) 0.009(2) Cl1 0.109(9) 0.125(9) 0.146(10) 0.003(7) 0.003(7) 0.002(7) P1 0.081(7) 0.033(6) 0.069(6) 0.002(4) 0.014(4) 0.004(5) P4 0.083(8) 0.032(6) 0.108(8) -0.001(4) 0.031(5) -0.005(5) P5 0.141(11) 0.069(8) 0.099(9) -0.027(5) 0.015(7) -0.024(7) P8 0.104(9) 0.080(8) 0.100(8) 0.003(6) 0.014(6) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N100 1.68(2) . ? W1 P8 2.516(10) . ? W1 P1 2.544(8) . ? W1 P4 2.557(9) . ? W1 P5 2.609(10) . ? W1 Br2 2.665(4) . ? N100 N101 1.43(3) . ? N101 C102 1.32(3) . ? C102 N103 1.25(3) . ? C102 O106 1.33(3) . ? N103 N104 1.43(3) . ? N103 Pd1 2.07(3) . ? N104 C105 1.26(4) . ? C105 O106 1.32(3) . ? C105 C111 1.57(3) . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C114 C117 1.41(5) . ? C115 C116 1.3900 . ? C117 N118 1.15(4) . ? Pd1 N103 2.07(3) 3_565 ? Pd1 Cl1 2.289(11) . ? Pd1 Cl1 2.289(11) 3_565 ? P1 C11 1.782(15) . ? P1 C21 1.939(18) . ? P1 C2 1.95(2) . ? C2 C3 1.36(3) . ? C3 P4 1.76(3) . ? P4 C31 1.826(17) . ? P4 C41 1.930(18) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? P5 C51 1.73(2) . ? P5 C6 1.88(3) . ? P5 C61 1.93(2) . ? C6 C7 1.54(4) . ? C7 P8 1.93(3) . ? P8 C71 1.875(17) . ? P8 C81 1.909(19) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? O100 C101 1.66(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N100 W1 P8 91.3(8) . . ? N100 W1 P1 92.3(8) . . ? P8 W1 P1 100.2(3) . . ? N100 W1 P4 98.4(8) . . ? P8 W1 P4 170.3(3) . . ? P1 W1 P4 79.8(3) . . ? N100 W1 P5 91.5(8) . . ? P8 W1 P5 78.6(3) . . ? P1 W1 P5 176.1(3) . . ? P4 W1 P5 100.7(3) . . ? N100 W1 Br2 177.7(8) . . ? P8 W1 Br2 89.8(3) . . ? P1 W1 Br2 85.57(19) . . ? P4 W1 Br2 80.6(2) . . ? P5 W1 Br2 90.7(2) . . ? N101 N100 W1 169.6(19) . . ? C102 N101 N100 121(2) . . ? N103 C102 N101 127(3) . . ? N103 C102 O106 111(3) . . ? N101 C102 O106 122(3) . . ? C102 N103 N104 109(3) . . ? C102 N103 Pd1 133(3) . . ? N104 N103 Pd1 118(2) . . ? C105 N104 N103 100(3) . . ? N104 C105 O106 116(3) . . ? N104 C105 C111 124(3) . . ? O106 C105 C111 120(3) . . ? C105 O106 C102 103(3) . . ? C112 C111 C116 120.0 . . ? C112 C111 C105 117(2) . . ? C116 C111 C105 123(2) . . ? C111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 C117 123(2) . . ? C115 C114 C117 117(2) . . ? C116 C115 C114 120.0 . . ? C115 C116 C111 120.0 . . ? N118 C117 C114 175(5) . . ? N103 Pd1 N103 180.0(13) 3_565 . ? N103 Pd1 Cl1 90.7(7) 3_565 . ? N103 Pd1 Cl1 89.3(7) . . ? N103 Pd1 Cl1 89.3(7) 3_565 3_565 ? N103 Pd1 Cl1 90.7(7) . 3_565 ? Cl1 Pd1 Cl1 179.998(1) . 3_565 ? C11 P1 C21 93.8(10) . . ? C11 P1 C2 103.3(11) . . ? C21 P1 C2 102.1(12) . . ? C11 P1 W1 123.5(8) . . ? C21 P1 W1 124.7(7) . . ? C2 P1 W1 106.2(8) . . ? C3 C2 P1 113(2) . . ? C2 C3 P4 120(2) . . ? C3 P4 C31 109.3(13) . . ? C3 P4 C41 101.6(12) . . ? C31 P4 C41 102.0(10) . . ? C3 P4 W1 105.5(10) . . ? C31 P4 W1 123.0(7) . . ? C41 P4 W1 113.4(8) . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 123.8(14) . . ? C16 C11 P1 116.2(14) . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 118.3(17) . . ? C26 C21 P1 121.5(17) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P4 121.0(16) . . ? C36 C31 P4 118.7(16) . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P4 122.6(17) . . ? C46 C41 P4 117.4(17) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C51 P5 C6 115.6(16) . . ? C51 P5 C61 101.9(14) . . ? C6 P5 C61 92.3(15) . . ? C51 P5 W1 124.3(11) . . ? C6 P5 W1 100.1(12) . . ? C61 P5 W1 118.7(9) . . ? C7 C6 P5 111(3) . . ? C6 C7 P8 110(2) . . ? C71 P8 C81 101.4(10) . . ? C71 P8 C7 100.4(13) . . ? C81 P8 C7 99.9(14) . . ? C71 P8 W1 119.6(7) . . ? C81 P8 W1 121.9(9) . . ? C7 P8 W1 110.0(12) . . ? C62 C61 C66 120.0 . . ? C62 C61 P5 115(2) . . ? C66 C61 P5 125(2) . . ? C63 C62 C61 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P5 119(2) . . ? C56 C51 P5 121(2) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P8 122.4(15) . . ? C76 C71 P8 117.3(15) . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? C82 C81 C86 120.0 . . ? C82 C81 P8 120.4(18) . . ? C86 C81 P8 119.6(18) . . ? C81 C82 C83 120.0 . . ? C82 C83 C84 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? _diffrn_measured_fraction_theta_max 0.631 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.631 _refine_diff_density_max 1.252 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.117 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1997) SHELX97 program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 651023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H160 Br2 Cl4 N10 O26 P8 Rh2 W2' _chemical_formula_weight 3425.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2326(15) _cell_length_b 26.598(3) _cell_length_c 21.292(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.357(10) _cell_angle_gamma 90.00 _cell_volume 7650.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3452 _exptl_absorpt_coefficient_mu 2.453 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Bruker-Nonius Kappa System' _diffrn_measurement_method '343 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68619 _diffrn_reflns_av_R_equivalents 0.1101 _diffrn_reflns_av_sigmaI/netI 0.1568 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.56 _reflns_number_total 17419 _reflns_number_gt 9676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker-Nonius' _computing_cell_refinement 'COLLECT, Bruker-Nonius' _computing_data_reduction 'DENZO, Bruker-Nonius' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+27.4787P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17419 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.1939 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.45678(3) 0.238067(15) 0.917325(19) 0.02391(13) Uani 1 1 d . . . Rh1 Rh 0.01674(6) 0.01466(3) 0.55565(4) 0.0335(2) Uani 1 1 d . . . Br2 Br 0.55737(8) 0.31325(4) 0.89205(5) 0.0351(3) Uani 1 1 d . . . N100 N 0.3914(6) 0.1888(3) 0.9421(4) 0.0296(19) Uani 1 1 d . . . N101 N 0.3526(7) 0.1573(3) 0.9746(4) 0.031(2) Uani 1 1 d . . . C102 C 0.2859(8) 0.1251(4) 0.9401(5) 0.034(2) Uani 1 1 d . . . N103 N 0.2390(8) 0.0913(3) 0.9651(5) 0.048(3) Uani 1 1 d . . . O106 O 0.2539(5) 0.1225(2) 0.8719(3) 0.0290(16) Uani 1 1 d . . . N104 N 0.1741(8) 0.0659(3) 0.9118(5) 0.048(3) Uani 1 1 d . . . C105 C 0.1864(9) 0.0850(4) 0.8583(5) 0.038(3) Uani 1 1 d . . . C107 C 0.1397(8) 0.0703(4) 0.7910(5) 0.035(3) Uani 1 1 d . . . C108 C 0.1584(9) 0.0972(4) 0.7410(6) 0.044(3) Uani 1 1 d . . . H108 H 0.1994 0.1253 0.7507 0.053 Uiso 1 1 calc R . . C112 C 0.0799(10) 0.0286(5) 0.7734(6) 0.056(4) Uani 1 1 d . . . H112 H 0.0679 0.0089 0.8061 0.067 Uiso 1 1 calc R . . C109 C 0.1150(9) 0.0817(4) 0.6758(6) 0.045(3) Uani 1 1 d . . . H109 H 0.1269 0.1004 0.6421 0.054 Uiso 1 1 calc R . . C111 C 0.0382(11) 0.0159(5) 0.7087(7) 0.065(4) Uani 1 1 d . . . H111 H -0.0050 -0.0113 0.6980 0.078 Uiso 1 1 calc R . . N110 N 0.0572(7) 0.0414(3) 0.6598(4) 0.039(2) Uani 1 1 d . . . P1 P 0.3142(2) 0.28158(10) 0.83661(13) 0.0284(6) Uani 1 1 d . . . C2 C 0.3362(8) 0.2811(4) 0.7561(5) 0.032(2) Uani 1 1 d . . . H2A H 0.2768 0.2918 0.7218 0.039 Uiso 1 1 calc R . . H2B H 0.3890 0.3044 0.7569 0.039 Uiso 1 1 calc R . . C3 C 0.3646(8) 0.2279(4) 0.7413(5) 0.033(2) Uani 1 1 d . . . H3A H 0.3868 0.2291 0.7027 0.039 Uiso 1 1 calc R . . H3B H 0.3064 0.2067 0.7308 0.039 Uiso 1 1 calc R . . P4 P 0.4629(2) 0.19960(10) 0.81069(13) 0.0287(6) Uani 1 1 d . . . C11 C 0.1953(8) 0.2492(4) 0.8227(5) 0.031(2) Uani 1 1 d . . . C12 C 0.1723(8) 0.2312(4) 0.8778(6) 0.039(3) Uani 1 1 d . . . H12 H 0.2158 0.2365 0.9201 0.047 Uiso 1 1 calc R . . C13 C 0.0842(9) 0.2055(5) 0.8693(7) 0.051(3) Uani 1 1 d . . . H13 H 0.0682 0.1935 0.9057 0.061 Uiso 1 1 calc R . . C14 C 0.0227(9) 0.1981(5) 0.8077(8) 0.063(4) Uani 1 1 d . . . H14 H -0.0361 0.1809 0.8026 0.075 Uiso 1 1 calc R . . C15 C 0.0417(10) 0.2145(6) 0.7521(7) 0.065(4) Uani 1 1 d . . . H15 H -0.0024 0.2079 0.7103 0.078 Uiso 1 1 calc R . . C16 C 0.1313(9) 0.2421(5) 0.7597(6) 0.048(3) Uani 1 1 d . . . H16 H 0.1457 0.2549 0.7231 0.058 Uiso 1 1 calc R . . C21 C 0.2826(8) 0.3483(4) 0.8426(5) 0.036(3) Uani 1 1 d . . . C22 C 0.3325(9) 0.3857(4) 0.8201(6) 0.046(3) Uani 1 1 d . . . H22 H 0.3825 0.3776 0.8023 0.055 Uiso 1 1 calc R . . C23 C 0.3056(11) 0.4351(5) 0.8248(6) 0.057(4) Uani 1 1 d . . . H23 H 0.3392 0.4605 0.8109 0.069 Uiso 1 1 calc R . . C24 C 0.2295(10) 0.4479(5) 0.8499(6) 0.055(3) Uani 1 1 d . . . H24 H 0.2117 0.4814 0.8516 0.066 Uiso 1 1 calc R . . C26 C 0.2076(9) 0.3609(4) 0.8687(6) 0.045(3) Uani 1 1 d . . . H26 H 0.1744 0.3360 0.8840 0.054 Uiso 1 1 calc R . . C25 C 0.1826(10) 0.4119(5) 0.8714(7) 0.060(4) Uani 1 1 d . . . H25 H 0.1323 0.4206 0.8886 0.072 Uiso 1 1 calc R . . C31 C 0.5748(8) 0.2071(4) 0.7867(5) 0.036(3) Uani 1 1 d . . . C32 C 0.6415(8) 0.1684(4) 0.7941(5) 0.038(3) Uani 1 1 d . . . H32 H 0.6279 0.1374 0.8095 0.046 Uiso 1 1 calc R . . C34 C 0.7495(9) 0.2211(5) 0.7561(6) 0.051(3) Uani 1 1 d . . . H34 H 0.8071 0.2256 0.7450 0.061 Uiso 1 1 calc R . . C33 C 0.7287(9) 0.1748(5) 0.7791(5) 0.044(3) Uani 1 1 d . . . H33 H 0.7731 0.1482 0.7843 0.053 Uiso 1 1 calc R . . C35 C 0.6843(9) 0.2598(5) 0.7501(5) 0.043(3) Uani 1 1 d . . . H35 H 0.7003 0.2913 0.7373 0.051 Uiso 1 1 calc R . . C36 C 0.5950(8) 0.2538(4) 0.7623(5) 0.037(3) Uani 1 1 d . . . H36 H 0.5494 0.2799 0.7547 0.044 Uiso 1 1 calc R . . C41 C 0.4380(8) 0.1322(4) 0.7958(5) 0.031(2) Uani 1 1 d . . . C42 C 0.4455(8) 0.0997(4) 0.8468(6) 0.039(3) Uani 1 1 d . . . H42 H 0.4656 0.1118 0.8899 0.047 Uiso 1 1 calc R . . C43 C 0.4236(11) 0.0487(4) 0.8358(7) 0.057(4) Uani 1 1 d . . . H43 H 0.4297 0.0267 0.8708 0.069 Uiso 1 1 calc R . . C44 C 0.3921(13) 0.0318(5) 0.7701(9) 0.080(5) Uani 1 1 d . . . H44 H 0.3734 -0.0016 0.7613 0.096 Uiso 1 1 calc R . . C45 C 0.3885(12) 0.0634(5) 0.7189(8) 0.073(4) Uani 1 1 d . . . H45 H 0.3724 0.0511 0.6760 0.087 Uiso 1 1 calc R . . C46 C 0.4093(9) 0.1147(5) 0.7314(5) 0.048(3) Uani 1 1 d . . . H46 H 0.4037 0.1367 0.6966 0.058 Uiso 1 1 calc R . . P5 P 0.6145(2) 0.20412(10) 0.99579(13) 0.0275(6) Uani 1 1 d . . . C6 C 0.6216(8) 0.2257(4) 1.0800(5) 0.032(2) Uani 1 1 d . . . H6A H 0.6544 0.2001 1.1118 0.039 Uiso 1 1 calc R . . H6B H 0.6614 0.2560 1.0903 0.039 Uiso 1 1 calc R . . C7 C 0.5198(7) 0.2364(4) 1.0867(5) 0.030(2) Uani 1 1 d . . . H7A H 0.5272 0.2512 1.1296 0.035 Uiso 1 1 calc R . . H7B H 0.4831 0.2053 1.0833 0.035 Uiso 1 1 calc R . . P8 P 0.4516(2) 0.27993(10) 1.02094(12) 0.0256(6) Uani 1 1 d . . . C51 C 0.6197(9) 0.1357(4) 1.0056(5) 0.037(3) Uani 1 1 d . . . C52 C 0.5663(10) 0.1105(4) 1.0391(6) 0.052(3) Uani 1 1 d . . . H52 H 0.5268 0.1288 1.0583 0.062 Uiso 1 1 calc R . . C53 C 0.5690(13) 0.0596(5) 1.0452(8) 0.078(5) Uani 1 1 d . . . H53 H 0.5336 0.0437 1.0696 0.094 Uiso 1 1 calc R . . C54 C 0.6251(13) 0.0313(5) 1.0149(8) 0.075(5) Uani 1 1 d . . . H54 H 0.6279 -0.0035 1.0191 0.089 Uiso 1 1 calc R . . C55 C 0.6749(11) 0.0551(5) 0.9796(7) 0.065(4) Uani 1 1 d . . . H55 H 0.7130 0.0367 0.9595 0.078 Uiso 1 1 calc R . . C56 C 0.6696(10) 0.1074(4) 0.9731(6) 0.052(3) Uani 1 1 d . . . H56 H 0.7008 0.1233 0.9460 0.062 Uiso 1 1 calc R . . C61 C 0.7412(8) 0.2152(4) 0.9947(5) 0.033(2) Uani 1 1 d . . . C62 C 0.7600(8) 0.2312(4) 0.9392(5) 0.035(3) Uani 1 1 d . . . H62 H 0.7077 0.2396 0.9018 0.042 Uiso 1 1 calc R . . C63 C 0.8572(8) 0.2353(4) 0.9378(6) 0.041(3) Uani 1 1 d . . . H63 H 0.8695 0.2451 0.8992 0.049 Uiso 1 1 calc R . . C64 C 0.9336(9) 0.2246(5) 0.9933(6) 0.053(3) Uani 1 1 d . . . H64 H 0.9985 0.2280 0.9930 0.064 Uiso 1 1 calc R . . C65 C 0.9150(9) 0.2087(6) 1.0501(7) 0.065(4) Uani 1 1 d . . . H65 H 0.9676 0.2008 1.0876 0.079 Uiso 1 1 calc R . . C66 C 0.8204(8) 0.2045(5) 1.0518(6) 0.050(3) Uani 1 1 d . . . H66 H 0.8084 0.1946 1.0904 0.060 Uiso 1 1 calc R . . C72 C 0.4860(8) 0.3806(4) 1.0007(5) 0.036(3) Uani 1 1 d . . . H72 H 0.4506 0.3737 0.9568 0.043 Uiso 1 1 calc R . . C73 C 0.5163(8) 0.4286(4) 1.0183(6) 0.037(3) Uani 1 1 d . . . H73 H 0.5011 0.4541 0.9867 0.044 Uiso 1 1 calc R . . C74 C 0.5700(8) 0.4394(4) 1.0837(6) 0.038(3) Uani 1 1 d . . . H74 H 0.5905 0.4721 1.0961 0.046 Uiso 1 1 calc R . . C75 C 0.5924(9) 0.4018(4) 1.1296(6) 0.043(3) Uani 1 1 d . . . H75 H 0.6290 0.4090 1.1732 0.051 Uiso 1 1 calc R . . C76 C 0.5604(7) 0.3523(4) 1.1114(5) 0.032(2) Uani 1 1 d . . . H76 H 0.5755 0.3266 1.1427 0.039 Uiso 1 1 calc R . . C71 C 0.5060(7) 0.3421(3) 1.0459(5) 0.025(2) Uani 1 1 d . . . C81 C 0.3341(7) 0.2869(4) 1.0397(5) 0.028(2) Uani 1 1 d . . . C82 C 0.2905(8) 0.3346(4) 1.0364(6) 0.040(3) Uani 1 1 d . . . H82 H 0.3191 0.3625 1.0235 0.048 Uiso 1 1 calc R . . C83 C 0.2051(8) 0.3392(4) 1.0526(6) 0.041(3) Uani 1 1 d . . . H83 H 0.1757 0.3707 1.0504 0.049 Uiso 1 1 calc R . . C84 C 0.1618(8) 0.2980(5) 1.0720(5) 0.043(3) Uani 1 1 d . . . H84 H 0.1042 0.3022 1.0832 0.052 Uiso 1 1 calc R . . C85 C 0.2028(8) 0.2516(4) 1.0749(5) 0.038(3) Uani 1 1 d . . . H85 H 0.1724 0.2240 1.0873 0.045 Uiso 1 1 calc R . . C86 C 0.2894(8) 0.2453(4) 1.0596(5) 0.033(2) Uani 1 1 d . . . H86 H 0.3181 0.2136 1.0624 0.040 Uiso 1 1 calc R . . O93 O 0.0053(6) -0.0858(3) 0.4808(4) 0.0409(19) Uani 1 1 d . . . C92 C 0.0294(9) -0.0930(5) 0.5416(7) 0.049(3) Uani 1 1 d . . . O91 O 0.0373(6) -0.0585(3) 0.5854(4) 0.0413(19) Uani 1 1 d . . . C94 C 0.0507(12) -0.1465(5) 0.5672(7) 0.073(4) Uani 1 1 d . . . H94A H -0.0090 -0.1660 0.5524 0.088 Uiso 1 1 calc R . . H94B H 0.0746 -0.1461 0.6147 0.088 Uiso 1 1 calc R . . H94C H 0.0999 -0.1611 0.5506 0.088 Uiso 1 1 calc R . . C96 C 0.1882(9) 0.0064(4) 0.5129(6) 0.045(3) Uani 1 1 d . . . O95 O 0.1614(5) 0.0193(3) 0.5627(4) 0.0391(18) Uani 1 1 d . . . C98 C 0.2970(9) 0.0089(6) 0.5213(7) 0.062(4) Uani 1 1 d . . . H98A H 0.3281 -0.0219 0.5407 0.075 Uiso 1 1 calc R . . H98B H 0.3262 0.0365 0.5498 0.075 Uiso 1 1 calc R . . H98C H 0.3062 0.0136 0.4789 0.075 Uiso 1 1 calc R . . O97 O 0.1302(5) -0.0087(3) 0.4573(4) 0.0407(19) Uani 1 1 d . . . C401 C 0.1696(12) 0.6158(5) 0.9043(7) 0.0675(9) Uiso 0.716(4) 1 d P A 1 H40A H 0.1226 0.5984 0.9211 0.081 Uiso 0.716(4) 1 calc PR A 1 H40B H 0.2355 0.6044 0.9295 0.081 Uiso 0.716(4) 1 calc PR A 1 Cl41 Cl 0.1613(4) 0.67715(19) 0.9154(3) 0.0675(9) Uiso 0.716(4) 1 d P A 1 Cl42 Cl 0.1457(4) 0.5998(2) 0.8187(3) 0.0675(9) Uiso 0.716(4) 1 d P A 1 C402 C 0.1696(12) 0.6158(5) 0.9043(7) 0.0675(9) Uiso 0.284(4) 1 d P A 2 H40C H 0.1930 0.5817 0.9026 0.081 Uiso 0.284(4) 1 calc PR A 2 H40D H 0.1035 0.6130 0.9078 0.081 Uiso 0.284(4) 1 calc PR A 2 Cl43 Cl 0.2440(10) 0.6417(5) 0.9787(6) 0.0675(9) Uiso 0.284(4) 1 d P A 2 Cl44 Cl 0.1587(10) 0.6392(5) 0.8380(7) 0.0675(9) Uiso 0.284(4) 1 d P A 2 O100 O 0.1336(10) 0.1512(5) 0.1503(7) 0.108(4) Uani 1 1 d . B 1 H100 H 0.1388 0.1366 0.1176 0.130 Uiso 1 1 calc R B 1 C101 C 0.0804(18) 0.1193(8) 0.1832(10) 0.127(8) Uani 1 1 d . B 1 H10A H 0.1259 0.0964 0.2124 0.152 Uiso 1 1 calc R B 1 H10B H 0.0305 0.1006 0.1507 0.152 Uiso 1 1 calc R B 1 H10C H 0.0497 0.1399 0.2083 0.152 Uiso 1 1 calc R B 1 O300 O 0.4324(13) 0.1383(6) 0.1673(8) 0.146(6) Uiso 1 1 d . C 3 H300 H 0.4449 0.1665 0.1834 0.175 Uiso 1 1 calc R C 3 C301 C 0.504(2) 0.1049(11) 0.2030(15) 0.189(12) Uiso 1 1 d . C 3 H30A H 0.5643 0.1227 0.2237 0.227 Uiso 1 1 calc R C 3 H30B H 0.5149 0.0798 0.1737 0.227 Uiso 1 1 calc R C 3 H30C H 0.4816 0.0890 0.2363 0.227 Uiso 1 1 calc R C 3 O200 O 0.2563(9) 0.0936(4) 0.0992(6) 0.099(4) Uiso 1 1 d . D 4 O201 O 0.3440(12) 0.9742(5) 0.1981(7) 0.129(5) Uiso 1 1 d . E 4 O202 O 0.1740(14) 0.9588(7) 0.2234(9) 0.062(5) Uiso 0.50 1 d P F 4 O203 O 0.2941(13) 0.5916(6) 0.1680(8) 0.151(6) Uiso 1 1 d . G 4 O204 O 0.0871(9) 0.6711(4) 0.2452(6) 0.092(3) Uiso 1 1 d . H 4 O205 O 0.0453(14) 0.9867(6) -0.0796(9) 0.062(5) Uiso 0.50 1 d P I 4 O206 O 0.2207(11) 0.5953(5) 0.3091(7) 0.126(5) Uiso 1 1 d . J 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0228(2) 0.0281(2) 0.0208(2) -0.00074(17) 0.00694(16) 0.00113(18) Rh1 0.0264(5) 0.0397(5) 0.0364(5) -0.0121(4) 0.0128(4) -0.0075(4) Br2 0.0374(7) 0.0357(6) 0.0365(6) -0.0003(5) 0.0177(5) -0.0019(5) N100 0.023(5) 0.046(5) 0.018(4) -0.002(4) 0.004(4) 0.007(4) N101 0.036(5) 0.032(5) 0.025(5) 0.004(4) 0.008(4) -0.003(4) C102 0.040(7) 0.035(6) 0.025(6) -0.005(5) 0.007(5) 0.001(5) N103 0.064(8) 0.043(6) 0.038(6) -0.002(5) 0.018(5) -0.020(5) O106 0.025(4) 0.032(4) 0.030(4) -0.001(3) 0.008(3) 0.000(3) N104 0.054(7) 0.042(6) 0.043(6) -0.007(5) 0.009(5) -0.019(5) C105 0.043(7) 0.039(6) 0.030(6) -0.011(5) 0.009(5) -0.007(6) C107 0.024(6) 0.036(6) 0.044(7) -0.001(5) 0.009(5) -0.001(5) C108 0.043(8) 0.041(7) 0.047(7) -0.005(5) 0.012(6) -0.020(6) C112 0.077(10) 0.055(8) 0.039(7) -0.018(6) 0.025(7) -0.036(7) C109 0.054(8) 0.042(7) 0.037(7) -0.011(5) 0.009(6) -0.011(6) C111 0.069(10) 0.075(9) 0.060(9) -0.026(7) 0.032(8) -0.036(8) N110 0.039(6) 0.047(6) 0.034(5) -0.019(4) 0.015(5) -0.009(5) P1 0.0258(15) 0.0349(14) 0.0253(14) 0.0009(11) 0.0092(12) 0.0041(12) C2 0.038(7) 0.039(6) 0.020(5) 0.006(4) 0.009(5) 0.017(5) C3 0.024(6) 0.049(7) 0.024(5) 0.006(5) 0.006(5) 0.010(5) P4 0.0253(15) 0.0346(15) 0.0257(14) -0.0030(11) 0.0074(12) 0.0029(12) C11 0.027(6) 0.034(6) 0.035(6) 0.002(4) 0.014(5) 0.002(4) C12 0.021(6) 0.056(7) 0.039(7) 0.005(5) 0.009(5) 0.015(5) C13 0.030(7) 0.072(9) 0.054(8) 0.007(7) 0.018(7) 0.005(6) C14 0.024(7) 0.087(10) 0.077(11) -0.018(8) 0.017(7) -0.014(7) C15 0.051(9) 0.097(11) 0.041(8) -0.022(8) 0.005(7) -0.008(8) C16 0.032(7) 0.075(9) 0.030(6) -0.009(6) -0.001(5) -0.005(6) C21 0.039(7) 0.037(6) 0.031(6) 0.004(5) 0.012(5) 0.011(5) C22 0.048(8) 0.050(7) 0.038(7) 0.004(6) 0.013(6) 0.007(6) C23 0.078(11) 0.044(7) 0.054(8) 0.009(6) 0.026(8) 0.009(7) C24 0.062(9) 0.047(8) 0.058(9) 0.006(6) 0.020(7) 0.014(7) C26 0.053(8) 0.039(6) 0.050(7) 0.000(5) 0.027(7) -0.002(6) C25 0.057(9) 0.052(8) 0.082(10) 0.006(7) 0.037(8) 0.018(7) C31 0.038(7) 0.044(7) 0.026(6) -0.005(5) 0.008(5) 0.004(5) C32 0.034(7) 0.047(7) 0.034(6) -0.007(5) 0.010(5) -0.003(5) C34 0.034(7) 0.092(10) 0.030(7) -0.009(6) 0.015(6) 0.005(7) C33 0.031(7) 0.063(8) 0.035(7) -0.007(6) 0.006(6) 0.007(6) C35 0.043(7) 0.055(7) 0.029(6) -0.004(5) 0.008(5) -0.023(6) C36 0.026(6) 0.056(7) 0.028(6) -0.009(5) 0.007(5) 0.012(5) C41 0.032(6) 0.029(5) 0.034(6) -0.003(5) 0.012(5) 0.004(5) C42 0.028(6) 0.037(6) 0.047(7) -0.008(5) 0.003(5) 0.003(5) C43 0.069(10) 0.035(7) 0.066(10) 0.006(6) 0.019(8) 0.004(7) C44 0.108(15) 0.046(9) 0.091(13) -0.014(9) 0.038(11) -0.010(9) C45 0.094(13) 0.052(9) 0.064(10) -0.029(8) 0.013(9) -0.007(8) C46 0.058(9) 0.057(8) 0.027(6) -0.006(5) 0.011(6) -0.007(7) P5 0.0254(15) 0.0331(14) 0.0249(14) 0.0033(11) 0.0093(12) 0.0015(12) C6 0.032(6) 0.046(6) 0.017(5) 0.005(4) 0.005(5) -0.002(5) C7 0.030(6) 0.038(6) 0.023(5) 0.001(4) 0.013(5) -0.003(5) P8 0.0237(14) 0.0293(13) 0.0237(14) -0.0016(10) 0.0077(12) 0.0016(11) C51 0.045(7) 0.025(5) 0.037(6) 0.001(5) 0.007(6) 0.009(5) C52 0.062(9) 0.034(7) 0.071(9) 0.013(6) 0.037(8) 0.008(6) C53 0.097(13) 0.047(8) 0.110(13) 0.026(8) 0.060(11) 0.008(8) C54 0.090(13) 0.044(8) 0.091(12) 0.008(8) 0.031(10) 0.019(8) C55 0.058(10) 0.058(9) 0.077(10) -0.013(8) 0.018(8) 0.017(8) C56 0.064(9) 0.045(7) 0.046(8) 0.008(6) 0.016(7) 0.008(7) C61 0.021(6) 0.043(6) 0.037(6) -0.004(5) 0.011(5) 0.001(5) C62 0.032(6) 0.038(6) 0.032(6) -0.004(5) 0.005(5) 0.004(5) C63 0.028(6) 0.060(8) 0.032(6) -0.008(5) 0.007(5) -0.009(6) C64 0.024(7) 0.089(10) 0.049(8) 0.002(7) 0.014(6) -0.005(7) C65 0.018(7) 0.118(12) 0.047(8) 0.018(8) -0.008(6) -0.001(7) C66 0.026(7) 0.091(10) 0.033(7) 0.010(6) 0.007(6) 0.007(7) C72 0.028(6) 0.053(7) 0.031(6) -0.003(5) 0.015(5) -0.001(5) C73 0.036(7) 0.031(6) 0.052(7) -0.001(5) 0.026(6) 0.002(5) C74 0.031(7) 0.034(6) 0.049(7) -0.010(5) 0.012(6) -0.006(5) C75 0.044(8) 0.045(7) 0.038(7) -0.008(5) 0.013(6) -0.004(6) C76 0.023(6) 0.042(6) 0.032(6) 0.000(5) 0.007(5) -0.001(5) C71 0.028(6) 0.021(5) 0.024(6) -0.004(4) 0.005(5) 0.002(4) C81 0.025(6) 0.039(6) 0.020(5) -0.006(4) 0.008(4) -0.004(5) C82 0.023(6) 0.046(7) 0.049(7) -0.006(5) 0.007(5) 0.006(5) C83 0.028(6) 0.048(7) 0.049(7) 0.001(6) 0.014(6) 0.006(5) C84 0.026(6) 0.068(8) 0.042(7) 0.001(6) 0.020(6) 0.008(6) C85 0.034(7) 0.059(8) 0.020(5) -0.002(5) 0.007(5) -0.007(5) C86 0.032(6) 0.041(6) 0.025(6) -0.003(4) 0.007(5) -0.003(5) O93 0.044(5) 0.044(4) 0.035(5) -0.013(4) 0.014(4) -0.011(4) C92 0.038(8) 0.047(8) 0.062(9) -0.011(7) 0.018(7) -0.008(6) O91 0.044(5) 0.039(4) 0.038(4) -0.003(4) 0.010(4) -0.005(4) C94 0.093(13) 0.049(8) 0.066(10) -0.010(7) 0.008(9) -0.010(8) C96 0.034(7) 0.049(7) 0.055(8) -0.016(6) 0.016(7) -0.005(6) O95 0.023(4) 0.055(5) 0.039(4) -0.017(4) 0.010(4) -0.012(4) C98 0.029(7) 0.103(11) 0.062(9) -0.042(8) 0.025(7) -0.021(7) O97 0.026(4) 0.052(5) 0.048(5) -0.018(4) 0.018(4) -0.010(4) O100 0.070(9) 0.130(11) 0.112(11) 0.012(8) 0.011(8) -0.009(8) C101 0.17(2) 0.115(17) 0.105(16) 0.003(13) 0.052(17) 0.028(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N100 1.781(8) . ? W1 P8 2.493(2) . ? W1 P1 2.493(3) . ? W1 P5 2.506(3) . ? W1 P4 2.517(2) . ? W1 Br2 2.6121(11) . ? Rh1 O91 2.038(7) . ? Rh1 O95 2.021(7) . ? Rh1 O93 2.031(8) 3_556 ? Rh1 O97 2.028(7) 3_556 ? Rh1 N110 2.225(8) . ? Rh1 Rh1 2.3956(16) 3_556 ? N100 N101 1.314(11) . ? N101 C102 1.318(13) . ? C102 N103 1.325(13) . ? C102 O106 1.380(12) . ? N103 N104 1.393(13) . ? O106 C105 1.352(12) . ? N104 C105 1.309(13) . ? C105 C107 1.430(15) . ? C107 C112 1.375(15) . ? C107 C108 1.377(15) . ? C108 C109 1.393(15) . ? C112 C111 1.360(17) . ? C109 N110 1.330(14) . ? C111 N110 1.339(15) . ? P1 C2 1.836(9) . ? P1 C21 1.846(10) . ? P1 C11 1.838(11) . ? C2 C3 1.531(14) . ? C3 P4 1.845(10) . ? P4 C31 1.830(11) . ? P4 C41 1.835(10) . ? C11 C16 1.376(15) . ? C11 C12 1.398(14) . ? C12 C13 1.389(16) . ? C13 C14 1.341(18) . ? C14 C15 1.367(18) . ? C15 C16 1.436(18) . ? C21 C22 1.391(15) . ? C21 C26 1.390(14) . ? C22 C23 1.381(16) . ? C23 C24 1.391(17) . ? C24 C25 1.328(17) . ? C26 C25 1.409(16) . ? C31 C32 1.375(15) . ? C31 C36 1.410(15) . ? C32 C33 1.387(15) . ? C34 C35 1.366(17) . ? C34 C33 1.391(17) . ? C35 C36 1.385(15) . ? C41 C42 1.367(15) . ? C41 C46 1.382(14) . ? C42 C43 1.394(15) . ? C43 C44 1.40(2) . ? C44 C45 1.37(2) . ? C45 C46 1.401(17) . ? P5 C61 1.835(10) . ? P5 C51 1.832(10) . ? P5 C6 1.854(10) . ? C6 C7 1.528(13) . ? C7 P8 1.839(10) . ? P8 C71 1.833(10) . ? P8 C81 1.846(10) . ? C51 C52 1.370(15) . ? C51 C56 1.363(15) . ? C52 C53 1.359(16) . ? C53 C54 1.394(19) . ? C54 C55 1.343(19) . ? C55 C56 1.399(17) . ? C61 C62 1.360(14) . ? C61 C66 1.401(15) . ? C62 C63 1.397(15) . ? C63 C64 1.360(16) . ? C64 C65 1.384(17) . ? C65 C66 1.363(16) . ? C72 C71 1.372(14) . ? C72 C73 1.362(14) . ? C73 C74 1.392(15) . ? C74 C75 1.363(15) . ? C75 C76 1.409(15) . ? C76 C71 1.390(14) . ? C81 C86 1.407(14) . ? C81 C82 1.404(14) . ? C82 C83 1.368(14) . ? C83 C84 1.383(15) . ? C84 C85 1.359(15) . ? C85 C86 1.381(15) . ? O93 C92 1.245(14) . ? O93 Rh1 2.031(8) 3_556 ? C92 O91 1.290(14) . ? C92 C94 1.518(18) . ? C96 O97 1.276(14) . ? C96 O95 1.281(12) . ? C96 C98 1.503(15) . ? O97 Rh1 2.028(7) 3_556 ? C401 Cl41 1.659(14) . ? C401 Cl42 1.796(15) . ? C402 Cl44 1.505(18) . ? C402 Cl43 1.75(2) . ? O100 C101 1.46(2) . ? O300 C301 1.38(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N100 W1 P8 84.4(2) . . ? N100 W1 P1 99.1(3) . . ? P8 W1 P1 99.09(8) . . ? N100 W1 P5 88.8(3) . . ? P8 W1 P5 80.85(8) . . ? P1 W1 P5 172.07(9) . . ? N100 W1 P4 97.9(2) . . ? P8 W1 P4 177.45(9) . . ? P1 W1 P4 79.56(9) . . ? P5 W1 P4 100.17(9) . . ? N100 W1 Br2 174.8(2) . . ? P8 W1 Br2 90.65(6) . . ? P1 W1 Br2 83.25(7) . . ? P5 W1 Br2 88.82(6) . . ? P4 W1 Br2 87.04(7) . . ? O91 Rh1 O95 89.6(3) . . ? O91 Rh1 O93 175.9(3) . 3_556 ? O95 Rh1 O93 90.2(3) . 3_556 ? O91 Rh1 O97 90.5(3) . 3_556 ? O95 Rh1 O97 176.5(3) . 3_556 ? O93 Rh1 O97 89.6(3) 3_556 3_556 ? O91 Rh1 N110 91.6(3) . . ? O95 Rh1 N110 88.2(3) . . ? O93 Rh1 N110 92.5(3) 3_556 . ? O97 Rh1 N110 95.3(3) 3_556 . ? O91 Rh1 Rh1 87.8(2) . 3_556 ? O95 Rh1 Rh1 88.5(2) . 3_556 ? O93 Rh1 Rh1 88.1(2) 3_556 3_556 ? O97 Rh1 Rh1 88.0(2) 3_556 3_556 ? N110 Rh1 Rh1 176.6(2) . 3_556 ? N101 N100 W1 166.2(7) . . ? N100 N101 C102 118.1(8) . . ? N101 C102 N103 125.6(9) . . ? N101 C102 O106 124.0(9) . . ? N103 C102 O106 110.4(9) . . ? C102 N103 N104 106.8(9) . . ? C105 O106 C102 103.8(8) . . ? C105 N104 N103 106.6(9) . . ? N104 C105 O106 112.3(9) . . ? N104 C105 C107 128.2(10) . . ? O106 C105 C107 119.5(9) . . ? C112 C107 C108 117.5(11) . . ? C112 C107 C105 123.1(10) . . ? C108 C107 C105 119.3(10) . . ? C107 C108 C109 118.9(10) . . ? C111 C112 C107 120.8(12) . . ? N110 C109 C108 122.6(11) . . ? C112 C111 N110 122.1(12) . . ? C109 N110 C111 118.0(10) . . ? C109 N110 Rh1 117.3(7) . . ? C111 N110 Rh1 124.2(8) . . ? C2 P1 C21 100.8(4) . . ? C2 P1 C11 105.3(5) . . ? C21 P1 C11 103.3(5) . . ? C2 P1 W1 107.4(3) . . ? C21 P1 W1 124.2(4) . . ? C11 P1 W1 113.7(3) . . ? C3 C2 P1 109.4(6) . . ? C2 C3 P4 113.3(7) . . ? C31 P4 C41 101.3(5) . . ? C31 P4 C3 103.9(5) . . ? C41 P4 C3 101.8(5) . . ? C31 P4 W1 119.2(4) . . ? C41 P4 W1 119.6(3) . . ? C3 P4 W1 108.8(3) . . ? C16 C11 C12 120.8(10) . . ? C16 C11 P1 121.0(8) . . ? C12 C11 P1 118.2(9) . . ? C13 C12 C11 120.0(11) . . ? C14 C13 C12 118.9(12) . . ? C13 C14 C15 123.6(13) . . ? C14 C15 C16 118.4(12) . . ? C11 C16 C15 118.2(11) . . ? C22 C21 C26 120.4(10) . . ? C22 C21 P1 120.0(8) . . ? C26 C21 P1 119.6(8) . . ? C23 C22 C21 118.0(11) . . ? C22 C23 C24 121.9(12) . . ? C25 C24 C23 119.5(12) . . ? C21 C26 C25 118.9(11) . . ? C24 C25 C26 121.3(12) . . ? C32 C31 C36 119.2(10) . . ? C32 C31 P4 121.1(8) . . ? C36 C31 P4 119.7(8) . . ? C31 C32 C33 121.3(11) . . ? C35 C34 C33 119.2(11) . . ? C34 C33 C32 119.6(11) . . ? C34 C35 C36 122.1(11) . . ? C35 C36 C31 118.5(10) . . ? C42 C41 C46 119.9(10) . . ? C42 C41 P4 121.2(8) . . ? C46 C41 P4 118.8(8) . . ? C41 C42 C43 121.7(11) . . ? C42 C43 C44 117.6(12) . . ? C45 C44 C43 121.2(13) . . ? C44 C45 C46 119.7(13) . . ? C41 C46 C45 119.7(12) . . ? C61 P5 C51 99.0(5) . . ? C61 P5 C6 101.9(5) . . ? C51 P5 C6 102.1(5) . . ? C61 P5 W1 127.7(4) . . ? C51 P5 W1 115.5(4) . . ? C6 P5 W1 107.3(3) . . ? C7 C6 P5 112.5(7) . . ? C6 C7 P8 109.6(6) . . ? C71 P8 C7 105.9(5) . . ? C71 P8 C81 100.1(4) . . ? C7 P8 C81 101.2(4) . . ? C71 P8 W1 122.2(3) . . ? C7 P8 W1 103.7(3) . . ? C81 P8 W1 121.2(3) . . ? C52 C51 C56 117.3(10) . . ? C52 C51 P5 122.4(8) . . ? C56 C51 P5 119.9(9) . . ? C51 C52 C53 122.2(12) . . ? C52 C53 C54 119.8(13) . . ? C55 C54 C53 119.0(13) . . ? C54 C55 C56 120.2(13) . . ? C51 C56 C55 121.1(12) . . ? C62 C61 C66 119.5(10) . . ? C62 C61 P5 121.6(9) . . ? C66 C61 P5 118.8(8) . . ? C61 C62 C63 120.7(11) . . ? C64 C63 C62 119.4(10) . . ? C63 C64 C65 120.2(11) . . ? C66 C65 C64 120.7(12) . . ? C65 C66 C61 119.5(11) . . ? C71 C72 C73 121.9(10) . . ? C72 C73 C74 119.6(10) . . ? C75 C74 C73 119.8(10) . . ? C74 C75 C76 120.4(11) . . ? C71 C76 C75 119.2(10) . . ? C72 C71 C76 119.1(9) . . ? C72 C71 P8 119.6(8) . . ? C76 C71 P8 121.1(7) . . ? C86 C81 C82 119.4(9) . . ? C86 C81 P8 120.9(8) . . ? C82 C81 P8 119.7(8) . . ? C83 C82 C81 118.9(11) . . ? C82 C83 C84 121.2(11) . . ? C85 C84 C83 120.6(10) . . ? C84 C85 C86 120.2(10) . . ? C81 C86 C85 119.8(10) . . ? C92 O93 Rh1 120.1(7) . 3_556 ? O93 C92 O91 125.0(11) . . ? O93 C92 C94 118.5(11) . . ? O91 C92 C94 116.5(12) . . ? C92 O91 Rh1 119.0(8) . . ? O97 C96 O95 125.3(10) . . ? O97 C96 C98 117.7(10) . . ? O95 C96 C98 116.9(11) . . ? C96 O95 Rh1 118.9(7) . . ? C96 O97 Rh1 119.3(7) . 3_556 ? Cl41 C401 Cl42 112.2(8) . . ? Cl44 C402 Cl43 122.8(11) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.188 _refine_diff_density_min -1.455 _refine_diff_density_rms 0.207 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 651024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H76 Br Fe N5 O4 P4 Pd W' _chemical_formula_weight 1661.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1773(7) _cell_length_b 14.9382(10) _cell_length_c 20.6774(12) _cell_angle_alpha 72.028(6) _cell_angle_beta 87.447(5) _cell_angle_gamma 74.688(5) _cell_volume 3448.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 2.855 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 1.323 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23947 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 30.14 _reflns_number_total 18968 _reflns_number_gt 12714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18968 _refine_ls_number_parameters 831 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.892361(17) -0.140049(14) 0.265128(10) 0.01939(6) Uani 1 1 d . . . Br1 Br 1.07316(5) -0.28241(4) 0.26512(3) 0.03595(14) Uani 1 1 d . . . P1 P 0.75148(10) -0.23250(9) 0.25659(6) 0.0203(3) Uani 1 1 d . . . C2 C 0.6746(4) -0.2400(4) 0.3362(3) 0.0287(11) Uani 1 1 d . . . H2A H 0.6314 -0.1752 0.3360 0.034 Uiso 1 1 calc R . . H2B H 0.6217 -0.2796 0.3399 0.034 Uiso 1 1 calc R . . C3 C 0.7593(4) -0.2848(4) 0.3962(3) 0.0279(11) Uani 1 1 d . . . H3A H 0.7941 -0.3525 0.3997 0.034 Uiso 1 1 calc R . . H3B H 0.7190 -0.2833 0.4376 0.034 Uiso 1 1 calc R . . P4 P 0.87306(11) -0.22100(9) 0.38957(6) 0.0215(3) Uani 1 1 d . . . P5 P 0.91795(11) -0.07520(9) 0.14087(7) 0.0233(3) Uani 1 1 d . . . C6 C 1.0618(4) -0.0547(4) 0.1305(3) 0.0280(11) Uani 1 1 d . . . H6A H 1.1190 -0.1169 0.1411 0.034 Uiso 1 1 calc R . . H6B H 1.0699 -0.0178 0.0837 0.034 Uiso 1 1 calc R . . C7 C 1.0797(4) 0.0017(4) 0.1782(3) 0.0275(11) Uani 1 1 d . . . H7A H 1.0340 0.0686 0.1608 0.033 Uiso 1 1 calc R . . H7B H 1.1590 0.0028 0.1781 0.033 Uiso 1 1 calc R . . P8 P 1.04117(11) -0.05195(9) 0.26746(7) 0.0218(3) Uani 1 1 d . . . C11 C 0.7828(4) -0.3592(4) 0.2564(3) 0.0264(11) Uani 1 1 d . . . C12 C 0.8899(5) -0.4157(4) 0.2513(3) 0.0388(14) Uani 1 1 d . . . H12 H 0.9522 -0.3898 0.2480 0.047 Uiso 1 1 calc R . . C13 C 0.9064(6) -0.5131(4) 0.2510(3) 0.0480(17) Uani 1 1 d . . . H13 H 0.9795 -0.5505 0.2476 0.058 Uiso 1 1 calc R . . C14 C 0.8177(6) -0.5522(4) 0.2558(3) 0.0471(17) Uani 1 1 d . . . H14 H 0.8294 -0.6160 0.2552 0.057 Uiso 1 1 calc R . . C15 C 0.7114(6) -0.4985(5) 0.2613(3) 0.0505(17) Uani 1 1 d . . . H15 H 0.6501 -0.5256 0.2646 0.061 Uiso 1 1 calc R . . C16 C 0.6932(5) -0.4023(4) 0.2621(3) 0.0416(15) Uani 1 1 d . . . H16 H 0.6197 -0.3665 0.2666 0.050 Uiso 1 1 calc R . . C21 C 0.6360(4) -0.1746(4) 0.1908(3) 0.0253(11) Uani 1 1 d . . . C22 C 0.5425(4) -0.1014(4) 0.1971(3) 0.0333(12) Uani 1 1 d . . . H22 H 0.5354 -0.0827 0.2363 0.040 Uiso 1 1 calc R . . C23 C 0.4596(5) -0.0562(4) 0.1449(3) 0.0406(14) Uani 1 1 d . . . H23 H 0.3977 -0.0065 0.1490 0.049 Uiso 1 1 calc R . . C24 C 0.4686(5) -0.0845(5) 0.0873(3) 0.0474(16) Uani 1 1 d . . . H24 H 0.4114 -0.0554 0.0532 0.057 Uiso 1 1 calc R . . C25 C 0.5619(5) -0.1556(5) 0.0797(3) 0.0443(15) Uani 1 1 d . . . H25 H 0.5684 -0.1730 0.0399 0.053 Uiso 1 1 calc R . . C26 C 0.6460(5) -0.2014(4) 0.1306(3) 0.0351(13) Uani 1 1 d . . . H26 H 0.7088 -0.2496 0.1253 0.042 Uiso 1 1 calc R . . C31 C 0.9797(4) -0.3139(3) 0.4513(3) 0.0269(11) Uani 1 1 d . . . C32 C 0.9448(5) -0.3651(4) 0.5133(3) 0.0374(13) Uani 1 1 d . . . H32 H 0.8674 -0.3570 0.5207 0.045 Uiso 1 1 calc R . . C33 C 1.0242(6) -0.4286(4) 0.5646(3) 0.0437(15) Uani 1 1 d . . . H33 H 0.9994 -0.4631 0.6056 0.052 Uiso 1 1 calc R . . C34 C 1.1387(6) -0.4405(4) 0.5548(3) 0.0457(16) Uani 1 1 d . . . H34 H 1.1919 -0.4804 0.5895 0.055 Uiso 1 1 calc R . . C35 C 1.1733(5) -0.3922(4) 0.4926(4) 0.0473(17) Uani 1 1 d . . . H35 H 1.2508 -0.4017 0.4850 0.057 Uiso 1 1 calc R . . C36 C 1.0950(5) -0.3296(4) 0.4407(3) 0.0382(14) Uani 1 1 d . . . H36 H 1.1205 -0.2983 0.3989 0.046 Uiso 1 1 calc R . . C41 C 0.8174(4) -0.1362(4) 0.4385(3) 0.0266(11) Uani 1 1 d . . . C42 C 0.8898(5) -0.1169(4) 0.4805(3) 0.0388(14) Uani 1 1 d . . . H42 H 0.9671 -0.1490 0.4848 0.047 Uiso 1 1 calc R . . C43 C 0.8472(6) -0.0507(5) 0.5155(3) 0.0493(17) Uani 1 1 d . . . H43 H 0.8956 -0.0388 0.5436 0.059 Uiso 1 1 calc R . . C44 C 0.7336(7) -0.0025(5) 0.5090(3) 0.0539(19) Uani 1 1 d . . . H44 H 0.7051 0.0416 0.5329 0.065 Uiso 1 1 calc R . . C45 C 0.6610(6) -0.0193(4) 0.4666(3) 0.0473(16) Uani 1 1 d . . . H45 H 0.5842 0.0140 0.4620 0.057 Uiso 1 1 calc R . . C46 C 0.7028(5) -0.0854(4) 0.4316(3) 0.0350(13) Uani 1 1 d . . . H46 H 0.6540 -0.0961 0.4031 0.042 Uiso 1 1 calc R . . C51 C 0.9108(5) -0.1436(4) 0.0819(3) 0.0296(12) Uani 1 1 d . . . C52 C 0.8355(5) -0.1067(5) 0.0265(3) 0.0390(14) Uani 1 1 d . . . H52 H 0.7920 -0.0422 0.0151 0.047 Uiso 1 1 calc R . . C53 C 0.8235(6) -0.1648(5) -0.0130(3) 0.0471(16) Uani 1 1 d . . . H53 H 0.7721 -0.1387 -0.0502 0.057 Uiso 1 1 calc R . . C54 C 0.8866(6) -0.2594(5) 0.0027(4) 0.0533(18) Uani 1 1 d . . . H54 H 0.8778 -0.2977 -0.0236 0.064 Uiso 1 1 calc R . . C55 C 0.9620(7) -0.2976(5) 0.0566(4) 0.062(2) Uani 1 1 d . . . H55 H 1.0059 -0.3618 0.0667 0.075 Uiso 1 1 calc R . . C56 C 0.9741(6) -0.2409(5) 0.0972(3) 0.0496(17) Uani 1 1 d . . . H56 H 1.0248 -0.2683 0.1347 0.060 Uiso 1 1 calc R . . C61 C 0.8222(4) 0.0441(4) 0.0992(3) 0.0288(11) Uani 1 1 d . . . C62 C 0.7042(5) 0.0543(4) 0.1078(3) 0.0299(12) Uani 1 1 d . . . H62 H 0.6789 0.0012 0.1338 0.036 Uiso 1 1 calc R . . C63 C 0.6267(5) 0.1418(4) 0.0781(3) 0.0379(14) Uani 1 1 d . . . H63 H 0.5492 0.1478 0.0837 0.045 Uiso 1 1 calc R . . C64 C 0.6644(6) 0.2221(4) 0.0393(3) 0.0464(16) Uani 1 1 d . . . H64 H 0.6121 0.2817 0.0195 0.056 Uiso 1 1 calc R . . C65 C 0.7786(6) 0.2127(5) 0.0306(3) 0.0487(17) Uani 1 1 d . . . H65 H 0.8031 0.2668 0.0055 0.058 Uiso 1 1 calc R . . C66 C 0.8582(5) 0.1244(4) 0.0585(3) 0.0356(13) Uani 1 1 d . . . H66 H 0.9351 0.1184 0.0503 0.043 Uiso 1 1 calc R . . C71 C 1.1802(4) -0.1225(3) 0.3103(3) 0.0236(10) Uani 1 1 d . . . C72 C 1.1933(5) -0.1377(4) 0.3797(3) 0.0306(12) Uani 1 1 d . . . H72 H 1.1346 -0.1074 0.4023 0.037 Uiso 1 1 calc R . . C73 C 1.2930(5) -0.1976(4) 0.4155(3) 0.0352(13) Uani 1 1 d . . . H73 H 1.3014 -0.2070 0.4618 0.042 Uiso 1 1 calc R . . C74 C 1.3801(5) -0.2434(4) 0.3819(3) 0.0400(14) Uani 1 1 d . . . H74 H 1.4464 -0.2852 0.4058 0.048 Uiso 1 1 calc R . . C75 C 1.3682(5) -0.2270(4) 0.3134(3) 0.0407(14) Uani 1 1 d . . . H75 H 1.4273 -0.2565 0.2906 0.049 Uiso 1 1 calc R . . C76 C 1.2688(4) -0.1668(4) 0.2779(3) 0.0326(12) Uani 1 1 d . . . H76 H 1.2618 -0.1561 0.2314 0.039 Uiso 1 1 calc R . . C81 C 1.0110(5) 0.0534(4) 0.2995(3) 0.0302(12) Uani 1 1 d . . . C82 C 1.0870(5) 0.1120(4) 0.2878(3) 0.0368(13) Uani 1 1 d . . . H82 H 1.1518 0.0981 0.2633 0.044 Uiso 1 1 calc R . . C83 C 1.0652(6) 0.1905(4) 0.3127(3) 0.0468(17) Uani 1 1 d . . . H83 H 1.1154 0.2298 0.3048 0.056 Uiso 1 1 calc R . . C84 C 0.9683(6) 0.2110(4) 0.3495(3) 0.0471(17) Uani 1 1 d . . . H84 H 0.9540 0.2641 0.3660 0.057 Uiso 1 1 calc R . . C85 C 0.8947(6) 0.1543(4) 0.3615(3) 0.0429(16) Uani 1 1 d . . . H85 H 0.8303 0.1686 0.3862 0.051 Uiso 1 1 calc R . . C86 C 0.9153(5) 0.0738(4) 0.3367(3) 0.0300(12) Uani 1 1 d . . . H86 H 0.8651 0.0346 0.3452 0.036 Uiso 1 1 calc R . . N100 N 0.7714(3) -0.0438(3) 0.2669(2) 0.0196(8) Uani 1 1 d . . . N101 N 0.6769(3) 0.0161(3) 0.2730(2) 0.0234(9) Uani 1 1 d . . . C102 C 0.6608(4) 0.1127(4) 0.2454(3) 0.0235(10) Uani 1 1 d . . . N103 N 0.5657(4) 0.1800(3) 0.2439(2) 0.0272(9) Uani 1 1 d . . . N104 N 0.5930(4) 0.2688(3) 0.2097(2) 0.0297(10) Uani 1 1 d . . . O105 O 0.7473(3) 0.1523(2) 0.21383(17) 0.0240(7) Uani 1 1 d . . . C106 C 0.6942(4) 0.2522(3) 0.1927(2) 0.0206(10) Uani 1 1 d . . . C107 C 0.7637(5) 0.3155(3) 0.1557(3) 0.0274(11) Uani 1 1 d . . . C108 C 0.7095(5) 0.4120(4) 0.1152(3) 0.0332(12) Uani 1 1 d . . . C109 C 0.8828(5) 0.2817(4) 0.1591(3) 0.0380(14) Uani 1 1 d . . . H109 H 0.9170 0.2182 0.1857 0.046 Uiso 1 1 calc R . . C110 C 0.7817(6) 0.4682(4) 0.0783(3) 0.0456(16) Uani 1 1 d . . . H110 H 0.7494 0.5308 0.0497 0.055 Uiso 1 1 calc R . . C111 C 0.8996(6) 0.4324(5) 0.0835(4) 0.0538(18) Uani 1 1 d . . . H111 H 0.9447 0.4717 0.0591 0.065 Uiso 1 1 calc R . . C112 C 0.9502(5) 0.3396(4) 0.1243(3) 0.0438(15) Uani 1 1 d . . . H112 H 1.0292 0.3163 0.1283 0.053 Uiso 1 1 calc R . . O113 O 0.5993(3) 0.4493(3) 0.1117(2) 0.0373(9) Uani 1 1 d . . . Pd1 Pd 0.49299(3) 0.40592(3) 0.19115(2) 0.02861(10) Uani 1 1 d . . . Fe1 Fe 0.41245(7) 0.35788(6) 0.36709(4) 0.03406(19) Uani 1 1 d . . . C171 C 0.3872(4) 0.3792(4) 0.2645(3) 0.0320(13) Uani 1 1 d . . . C172 C 0.3283(5) 0.4641(4) 0.2833(3) 0.0373(14) Uani 1 1 d . . . C173 C 0.2501(5) 0.4402(5) 0.3335(3) 0.0403(14) Uani 1 1 d . . . H173 H 0.2009 0.4821 0.3537 0.048 Uiso 1 1 calc R . . C174 C 0.2619(5) 0.3379(5) 0.3473(3) 0.0436(16) Uani 1 1 d . . . H174 H 0.2215 0.3013 0.3792 0.052 Uiso 1 1 calc R . . C175 C 0.3441(5) 0.3011(5) 0.3051(3) 0.0401(14) Uani 1 1 d . . . H175 H 0.3661 0.2371 0.3040 0.048 Uiso 1 1 calc R . . C176 C 0.3550(5) 0.5594(4) 0.2430(3) 0.0412(15) Uani 1 1 d . . . H17A H 0.2879 0.6137 0.2377 0.049 Uiso 1 1 calc R . . H17B H 0.4152 0.5707 0.2661 0.049 Uiso 1 1 calc R . . N177 N 0.3921(4) 0.5495(3) 0.1747(2) 0.0365(11) Uani 1 1 d . . . C178 C 0.4488(6) 0.6251(4) 0.1403(3) 0.0488(17) Uani 1 1 d . . . H17A' H 0.5161 0.6166 0.1663 0.073 Uiso 1 1 calc R . . H17B' H 0.3981 0.6881 0.1360 0.073 Uiso 1 1 calc R . . H17C H 0.4694 0.6203 0.0959 0.073 Uiso 1 1 calc R . . C179 C 0.2883(6) 0.5613(5) 0.1344(4) 0.0536(18) Uani 1 1 d . . . H17D H 0.3096 0.5543 0.0905 0.080 Uiso 1 1 calc R . . H17E H 0.2378 0.6248 0.1287 0.080 Uiso 1 1 calc R . . H17F H 0.2505 0.5123 0.1578 0.080 Uiso 1 1 calc R . . C181 C 0.4651(6) 0.2707(5) 0.4634(3) 0.0512(17) Uani 1 1 d . . . H181 H 0.4284 0.2271 0.4919 0.061 Uiso 1 1 calc R . . C182 C 0.5488(6) 0.2486(5) 0.4176(4) 0.0525(18) Uani 1 1 d . . . H182 H 0.5767 0.1882 0.4107 0.063 Uiso 1 1 calc R . . C183 C 0.5831(6) 0.3331(6) 0.3843(4) 0.0554(19) Uani 1 1 d . . . H183 H 0.6373 0.3385 0.3511 0.066 Uiso 1 1 calc R . . C184 C 0.5206(7) 0.4096(6) 0.4098(4) 0.061(2) Uani 1 1 d . . . H184 H 0.5272 0.4733 0.3968 0.074 Uiso 1 1 calc R . . C185 C 0.4458(6) 0.3697(6) 0.4593(4) 0.0574(19) Uani 1 1 d . . . H185 H 0.3942 0.4030 0.4840 0.069 Uiso 1 1 calc R . . O91 O 0.3849(4) 0.0888(4) 0.2542(3) 0.0643(14) Uani 1 1 d . . . H91 H 0.3228 0.0934 0.2378 0.077 Uiso 1 1 calc R . . C92 C 0.3940(6) 0.0314(5) 0.3237(4) 0.0595(19) Uani 1 1 d . . . H92A H 0.4692 0.0209 0.3418 0.071 Uiso 1 1 calc R . . H92B H 0.3801 -0.0303 0.3274 0.071 Uiso 1 1 calc R . . H92C H 0.3389 0.0648 0.3488 0.071 Uiso 1 1 calc R . . O93 O 0.2589(13) 0.2178(11) 0.1435(8) 0.112(5) Uiso 0.50 1 d P . . H93 H 0.3118 0.1684 0.1559 0.134 Uiso 0.50 1 calc PR . . C94 C 0.2996(10) 0.2943(8) 0.1189(6) 0.033(2) Uiso 0.50 1 d P . . H94A H 0.3556 0.2943 0.1508 0.040 Uiso 0.50 1 calc PR . . H94B H 0.2387 0.3539 0.1111 0.040 Uiso 0.50 1 calc PR . . C95 C 0.3483(14) 0.2888(12) 0.0596(8) 0.066(4) Uiso 0.50 1 d P . . H95A H 0.3960 0.2241 0.0659 0.079 Uiso 0.50 1 calc PR . . H95B H 0.3936 0.3348 0.0455 0.079 Uiso 0.50 1 calc PR . . H95C H 0.2900 0.3037 0.0253 0.079 Uiso 0.50 1 calc PR . . O96 O 0.5468(9) 0.5681(7) -0.0156(5) 0.060(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01857(10) 0.01535(9) 0.02478(11) -0.00851(7) 0.00258(7) -0.00287(7) Br1 0.0264(3) 0.0289(3) 0.0538(4) -0.0211(3) 0.0040(2) 0.0002(2) P1 0.0204(6) 0.0169(6) 0.0238(6) -0.0068(5) 0.0002(5) -0.0043(5) C2 0.026(3) 0.033(3) 0.030(3) -0.015(2) 0.009(2) -0.008(2) C3 0.032(3) 0.028(3) 0.022(3) -0.002(2) 0.001(2) -0.010(2) P4 0.0224(6) 0.0179(6) 0.0227(6) -0.0074(5) -0.0001(5) -0.0012(5) P5 0.0245(7) 0.0228(6) 0.0237(7) -0.0090(5) 0.0034(5) -0.0063(5) C6 0.029(3) 0.025(3) 0.028(3) -0.008(2) 0.002(2) -0.005(2) C7 0.024(3) 0.031(3) 0.030(3) -0.006(2) 0.002(2) -0.014(2) P8 0.0223(6) 0.0175(6) 0.0256(7) -0.0070(5) -0.0002(5) -0.0047(5) C11 0.029(3) 0.020(2) 0.034(3) -0.013(2) -0.001(2) -0.007(2) C12 0.032(3) 0.033(3) 0.058(4) -0.024(3) 0.003(3) -0.007(2) C13 0.051(4) 0.027(3) 0.063(5) -0.020(3) -0.001(3) 0.002(3) C14 0.059(4) 0.020(3) 0.059(4) -0.008(3) -0.022(3) -0.005(3) C15 0.067(5) 0.033(3) 0.058(4) -0.010(3) -0.002(4) -0.027(3) C16 0.034(3) 0.026(3) 0.064(4) -0.014(3) 0.000(3) -0.005(2) C21 0.024(3) 0.021(2) 0.026(3) -0.001(2) -0.005(2) -0.006(2) C22 0.024(3) 0.035(3) 0.038(3) -0.009(3) 0.001(2) -0.006(2) C23 0.027(3) 0.039(3) 0.043(4) 0.001(3) -0.003(3) -0.004(3) C24 0.037(4) 0.055(4) 0.040(4) 0.003(3) -0.014(3) -0.014(3) C25 0.048(4) 0.057(4) 0.031(3) -0.011(3) -0.003(3) -0.020(3) C26 0.038(3) 0.035(3) 0.031(3) -0.006(2) -0.007(2) -0.011(3) C31 0.030(3) 0.017(2) 0.032(3) -0.009(2) -0.005(2) -0.001(2) C32 0.038(3) 0.035(3) 0.035(3) -0.013(3) -0.002(3) 0.001(3) C33 0.055(4) 0.036(3) 0.033(3) -0.004(3) -0.005(3) -0.007(3) C34 0.051(4) 0.024(3) 0.053(4) -0.002(3) -0.021(3) -0.001(3) C35 0.028(3) 0.037(3) 0.067(5) -0.005(3) -0.016(3) -0.002(3) C36 0.042(3) 0.027(3) 0.040(3) -0.002(2) -0.006(3) -0.008(3) C41 0.031(3) 0.024(3) 0.022(3) -0.007(2) 0.003(2) -0.001(2) C42 0.046(4) 0.030(3) 0.039(3) -0.014(3) -0.006(3) -0.003(3) C43 0.075(5) 0.037(3) 0.036(4) -0.017(3) -0.013(3) -0.004(3) C44 0.084(5) 0.033(3) 0.044(4) -0.025(3) 0.007(4) 0.001(3) C45 0.050(4) 0.036(3) 0.056(4) -0.026(3) 0.016(3) 0.000(3) C46 0.041(3) 0.027(3) 0.034(3) -0.011(2) 0.006(2) -0.002(2) C51 0.035(3) 0.037(3) 0.025(3) -0.017(2) 0.009(2) -0.015(2) C52 0.042(3) 0.043(3) 0.037(3) -0.020(3) 0.005(3) -0.011(3) C53 0.046(4) 0.067(5) 0.038(4) -0.026(3) 0.002(3) -0.020(3) C54 0.070(5) 0.056(4) 0.053(4) -0.038(4) 0.007(4) -0.026(4) C55 0.083(6) 0.047(4) 0.059(5) -0.030(4) 0.000(4) -0.003(4) C56 0.060(4) 0.045(4) 0.048(4) -0.030(3) -0.007(3) -0.002(3) C61 0.030(3) 0.029(3) 0.027(3) -0.009(2) -0.002(2) -0.004(2) C62 0.033(3) 0.031(3) 0.024(3) -0.005(2) 0.000(2) -0.009(2) C63 0.032(3) 0.040(3) 0.035(3) -0.011(3) -0.010(2) 0.002(3) C64 0.054(4) 0.032(3) 0.040(4) -0.002(3) -0.018(3) 0.002(3) C65 0.065(5) 0.034(3) 0.042(4) 0.002(3) -0.009(3) -0.018(3) C66 0.037(3) 0.037(3) 0.028(3) -0.002(2) -0.002(2) -0.012(3) C71 0.018(2) 0.019(2) 0.034(3) -0.008(2) 0.001(2) -0.0049(19) C72 0.029(3) 0.027(3) 0.034(3) -0.008(2) 0.002(2) -0.006(2) C73 0.034(3) 0.033(3) 0.038(3) -0.006(3) -0.007(2) -0.011(2) C74 0.027(3) 0.037(3) 0.053(4) -0.008(3) -0.007(3) -0.010(3) C75 0.022(3) 0.043(4) 0.056(4) -0.018(3) 0.004(3) -0.005(3) C76 0.024(3) 0.038(3) 0.039(3) -0.016(3) 0.001(2) -0.009(2) C81 0.036(3) 0.021(2) 0.033(3) -0.011(2) -0.013(2) -0.001(2) C82 0.044(3) 0.027(3) 0.044(4) -0.012(3) -0.005(3) -0.015(3) C83 0.063(4) 0.030(3) 0.053(4) -0.009(3) -0.019(3) -0.021(3) C84 0.066(4) 0.018(3) 0.054(4) -0.016(3) -0.020(3) 0.004(3) C85 0.052(4) 0.031(3) 0.043(4) -0.020(3) -0.010(3) 0.006(3) C86 0.034(3) 0.018(2) 0.037(3) -0.010(2) -0.004(2) -0.003(2) N100 0.021(2) 0.0147(18) 0.023(2) -0.0066(16) 0.0031(16) -0.0040(16) N101 0.026(2) 0.0130(19) 0.030(2) -0.0023(17) 0.0027(18) -0.0082(16) C102 0.021(2) 0.025(2) 0.026(3) -0.012(2) 0.0035(19) -0.004(2) N103 0.025(2) 0.017(2) 0.034(3) -0.0040(18) 0.0058(18) -0.0003(17) N104 0.027(2) 0.026(2) 0.032(2) -0.0105(19) 0.0049(19) 0.0024(18) O105 0.0235(18) 0.0172(16) 0.0295(19) -0.0079(14) 0.0039(14) -0.0022(14) C106 0.028(3) 0.014(2) 0.020(2) -0.0050(18) 0.0013(19) -0.0048(19) C107 0.035(3) 0.017(2) 0.030(3) -0.008(2) 0.003(2) -0.005(2) C108 0.042(3) 0.022(3) 0.030(3) -0.006(2) 0.008(2) -0.004(2) C109 0.035(3) 0.031(3) 0.051(4) -0.021(3) 0.011(3) -0.005(2) C110 0.058(4) 0.028(3) 0.041(4) 0.000(3) 0.013(3) -0.011(3) C111 0.057(5) 0.044(4) 0.060(5) -0.012(3) 0.027(4) -0.022(3) C112 0.035(3) 0.036(3) 0.061(4) -0.018(3) 0.011(3) -0.010(3) O113 0.037(2) 0.027(2) 0.036(2) 0.0004(17) 0.0033(17) 0.0005(17) Pd1 0.0295(2) 0.01940(19) 0.0307(2) -0.00753(17) -0.00023(17) 0.00391(16) Fe1 0.0312(4) 0.0313(4) 0.0382(5) -0.0113(4) 0.0056(3) -0.0057(3) C171 0.023(3) 0.027(3) 0.045(3) -0.018(3) 0.004(2) 0.002(2) C172 0.025(3) 0.037(3) 0.051(4) -0.025(3) 0.005(3) 0.003(2) C173 0.022(3) 0.048(4) 0.052(4) -0.021(3) 0.008(3) -0.005(3) C174 0.040(4) 0.056(4) 0.047(4) -0.014(3) 0.000(3) -0.035(3) C175 0.035(3) 0.041(3) 0.051(4) -0.026(3) 0.015(3) -0.009(3) C176 0.046(4) 0.020(3) 0.047(4) -0.011(3) 0.001(3) 0.011(2) N177 0.036(3) 0.025(2) 0.035(3) -0.005(2) -0.006(2) 0.011(2) C178 0.060(4) 0.024(3) 0.048(4) -0.005(3) 0.003(3) 0.006(3) C179 0.045(4) 0.043(4) 0.059(5) -0.013(3) -0.010(3) 0.011(3) C181 0.055(4) 0.051(4) 0.039(4) -0.001(3) 0.005(3) -0.015(3) C182 0.043(4) 0.044(4) 0.055(4) -0.002(3) -0.003(3) 0.001(3) C183 0.032(4) 0.073(5) 0.047(4) -0.002(4) -0.003(3) -0.008(3) C184 0.067(5) 0.062(5) 0.051(5) 0.000(4) -0.013(4) -0.028(4) C185 0.055(5) 0.073(5) 0.044(4) -0.020(4) 0.000(3) -0.014(4) O91 0.051(3) 0.070(4) 0.073(4) -0.027(3) 0.003(3) -0.013(3) C92 0.055(5) 0.051(4) 0.073(6) -0.016(4) 0.009(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N100 1.774(4) . ? W1 P5 2.4877(14) . ? W1 P1 2.5120(13) . ? W1 P4 2.5129(13) . ? W1 P8 2.5149(13) . ? W1 Br1 2.6263(6) . ? P1 C11 1.831(5) . ? P1 C21 1.838(5) . ? P1 C2 1.845(5) . ? C2 C3 1.513(7) . ? C3 P4 1.856(5) . ? P4 C31 1.829(5) . ? P4 C41 1.834(5) . ? P5 C61 1.823(5) . ? P5 C51 1.834(5) . ? P5 C6 1.849(5) . ? C6 C7 1.537(7) . ? C7 P8 1.865(5) . ? P8 C81 1.836(5) . ? P8 C71 1.838(5) . ? C11 C12 1.373(7) . ? C11 C16 1.391(8) . ? C12 C13 1.418(8) . ? C13 C14 1.343(9) . ? C14 C15 1.351(9) . ? C15 C16 1.400(8) . ? C21 C22 1.388(7) . ? C21 C26 1.411(7) . ? C22 C23 1.388(8) . ? C23 C24 1.372(9) . ? C24 C25 1.377(9) . ? C25 C26 1.381(8) . ? C31 C36 1.380(8) . ? C31 C32 1.390(8) . ? C32 C33 1.394(8) . ? C33 C34 1.372(9) . ? C34 C35 1.375(9) . ? C35 C36 1.391(8) . ? C41 C46 1.391(7) . ? C41 C42 1.405(7) . ? C42 C43 1.382(8) . ? C43 C44 1.371(9) . ? C44 C45 1.391(9) . ? C45 C46 1.380(7) . ? C51 C52 1.378(8) . ? C51 C56 1.397(8) . ? C52 C53 1.397(8) . ? C53 C54 1.364(9) . ? C54 C55 1.353(10) . ? C55 C56 1.401(8) . ? C61 C66 1.400(8) . ? C61 C62 1.412(7) . ? C62 C63 1.372(7) . ? C63 C64 1.399(9) . ? C64 C65 1.370(10) . ? C65 C66 1.386(8) . ? C71 C76 1.372(7) . ? C71 C72 1.392(7) . ? C72 C73 1.385(7) . ? C73 C74 1.386(8) . ? C74 C75 1.367(8) . ? C75 C76 1.382(8) . ? C81 C86 1.385(8) . ? C81 C82 1.398(8) . ? C82 C83 1.382(8) . ? C83 C84 1.393(9) . ? C84 C85 1.354(9) . ? C85 C86 1.408(7) . ? N100 N101 1.286(5) . ? N101 C102 1.341(6) . ? C102 N103 1.313(6) . ? C102 O105 1.384(6) . ? N103 N104 1.414(6) . ? N104 C106 1.248(6) . ? N104 Pd1 2.017(4) . ? O105 C106 1.396(5) . ? C106 C107 1.454(7) . ? C107 C109 1.401(8) . ? C107 C108 1.419(7) . ? C108 O113 1.307(7) . ? C108 C110 1.412(8) . ? C109 C112 1.371(8) . ? C110 C111 1.390(9) . ? C111 C112 1.374(9) . ? O113 Pd1 2.095(4) . ? Pd1 C171 1.960(6) . ? Pd1 N177 2.103(4) . ? Fe1 C174 2.013(6) . ? Fe1 C181 2.037(7) . ? Fe1 C185 2.036(7) . ? Fe1 C183 2.040(6) . ? Fe1 C172 2.042(6) . ? Fe1 C184 2.043(7) . ? Fe1 C182 2.046(6) . ? Fe1 C175 2.048(6) . ? Fe1 C173 2.052(6) . ? Fe1 C171 2.071(6) . ? C171 C175 1.421(8) . ? C171 C172 1.441(7) . ? C172 C173 1.406(8) . ? C172 C176 1.522(8) . ? C173 C174 1.435(9) . ? C174 C175 1.412(8) . ? C176 N177 1.502(7) . ? N177 C178 1.459(8) . ? N177 C179 1.487(8) . ? C181 C182 1.405(9) . ? C181 C185 1.411(10) . ? C182 C183 1.399(10) . ? C183 C184 1.429(10) . ? C184 C185 1.435(10) . ? O91 C92 1.419(8) . ? O93 C94 1.314(17) . ? C94 C95 1.356(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N100 W1 P5 94.94(13) . . ? N100 W1 P1 85.68(13) . . ? P5 W1 P1 96.76(4) . . ? N100 W1 P4 89.45(13) . . ? P5 W1 P4 174.73(4) . . ? P1 W1 P4 80.63(4) . . ? N100 W1 P8 97.25(13) . . ? P5 W1 P8 80.32(4) . . ? P1 W1 P8 176.00(4) . . ? P4 W1 P8 102.05(4) . . ? N100 W1 Br1 178.69(12) . . ? P5 W1 Br1 86.07(3) . . ? P1 W1 Br1 95.05(3) . . ? P4 W1 Br1 89.59(3) . . ? P8 W1 Br1 82.07(3) . . ? C11 P1 C21 100.4(2) . . ? C11 P1 C2 100.8(2) . . ? C21 P1 C2 102.8(2) . . ? C11 P1 W1 127.19(17) . . ? C21 P1 W1 118.83(17) . . ? C2 P1 W1 103.07(17) . . ? C3 C2 P1 109.4(4) . . ? C2 C3 P4 113.0(4) . . ? C31 P4 C41 99.9(2) . . ? C31 P4 C3 100.6(2) . . ? C41 P4 C3 102.4(2) . . ? C31 P4 W1 128.88(18) . . ? C41 P4 W1 114.47(17) . . ? C3 P4 W1 107.03(16) . . ? C61 P5 C51 102.6(2) . . ? C61 P5 C6 104.4(2) . . ? C51 P5 C6 104.1(2) . . ? C61 P5 W1 114.42(17) . . ? C51 P5 W1 122.45(18) . . ? C6 P5 W1 107.18(17) . . ? C7 C6 P5 109.5(3) . . ? C6 C7 P8 113.1(4) . . ? C81 P8 C71 100.9(2) . . ? C81 P8 C7 101.9(2) . . ? C71 P8 C7 102.8(2) . . ? C81 P8 W1 121.46(19) . . ? C71 P8 W1 118.80(16) . . ? C7 P8 W1 108.37(16) . . ? C12 C11 C16 117.1(5) . . ? C12 C11 P1 124.4(4) . . ? C16 C11 P1 118.5(4) . . ? C11 C12 C13 120.7(6) . . ? C14 C13 C12 120.8(6) . . ? C13 C14 C15 119.9(6) . . ? C14 C15 C16 120.4(6) . . ? C11 C16 C15 121.2(6) . . ? C22 C21 C26 119.2(5) . . ? C22 C21 P1 121.7(4) . . ? C26 C21 P1 119.0(4) . . ? C23 C22 C21 120.0(5) . . ? C24 C23 C22 120.4(6) . . ? C23 C24 C25 120.3(6) . . ? C24 C25 C26 120.5(6) . . ? C25 C26 C21 119.5(6) . . ? C36 C31 C32 118.4(5) . . ? C36 C31 P4 122.2(4) . . ? C32 C31 P4 119.2(4) . . ? C31 C32 C33 120.9(6) . . ? C34 C33 C32 120.3(6) . . ? C33 C34 C35 118.8(6) . . ? C34 C35 C36 121.5(6) . . ? C31 C36 C35 120.0(6) . . ? C46 C41 C42 118.6(5) . . ? C46 C41 P4 120.2(4) . . ? C42 C41 P4 121.1(4) . . ? C43 C42 C41 120.5(6) . . ? C44 C43 C42 120.1(6) . . ? C43 C44 C45 120.2(5) . . ? C46 C45 C44 120.1(6) . . ? C45 C46 C41 120.5(6) . . ? C52 C51 C56 117.6(5) . . ? C52 C51 P5 122.5(4) . . ? C56 C51 P5 119.5(4) . . ? C51 C52 C53 120.9(6) . . ? C54 C53 C52 120.5(6) . . ? C55 C54 C53 120.0(6) . . ? C54 C55 C56 120.3(7) . . ? C51 C56 C55 120.7(6) . . ? C66 C61 C62 118.8(5) . . ? C66 C61 P5 124.1(4) . . ? C62 C61 P5 117.1(4) . . ? C63 C62 C61 120.6(5) . . ? C62 C63 C64 119.9(6) . . ? C65 C64 C63 119.8(6) . . ? C64 C65 C66 121.3(6) . . ? C65 C66 C61 119.5(6) . . ? C76 C71 C72 118.5(5) . . ? C76 C71 P8 122.7(4) . . ? C72 C71 P8 118.6(4) . . ? C73 C72 C71 120.7(5) . . ? C72 C73 C74 119.6(6) . . ? C75 C74 C73 119.8(5) . . ? C74 C75 C76 120.3(5) . . ? C71 C76 C75 121.0(5) . . ? C86 C81 C82 119.9(5) . . ? C86 C81 P8 120.5(4) . . ? C82 C81 P8 119.6(4) . . ? C83 C82 C81 119.7(6) . . ? C82 C83 C84 120.1(6) . . ? C85 C84 C83 120.6(5) . . ? C84 C85 C86 120.3(6) . . ? C81 C86 C85 119.5(5) . . ? N101 N100 W1 171.7(3) . . ? N100 N101 C102 121.0(4) . . ? N103 C102 N101 126.3(5) . . ? N103 C102 O105 112.0(4) . . ? N101 C102 O105 121.7(4) . . ? C102 N103 N104 104.3(4) . . ? C106 N104 N103 110.1(4) . . ? C106 N104 Pd1 121.7(4) . . ? N103 N104 Pd1 128.2(3) . . ? C102 O105 C106 102.6(4) . . ? N104 C106 O105 111.1(4) . . ? N104 C106 C107 132.7(5) . . ? O105 C106 C107 116.2(4) . . ? C109 C107 C108 120.2(5) . . ? C109 C107 C106 120.6(5) . . ? C108 C107 C106 119.3(5) . . ? O113 C108 C110 120.4(5) . . ? O113 C108 C107 123.3(5) . . ? C110 C108 C107 116.4(5) . . ? C112 C109 C107 121.8(6) . . ? C111 C110 C108 121.8(6) . . ? C112 C111 C110 120.8(6) . . ? C109 C112 C111 119.1(6) . . ? C108 O113 Pd1 123.3(3) . . ? C171 Pd1 N104 97.94(19) . . ? C171 Pd1 O113 174.28(18) . . ? N104 Pd1 O113 87.63(16) . . ? C171 Pd1 N177 81.7(2) . . ? N104 Pd1 N177 177.87(18) . . ? O113 Pd1 N177 92.64(17) . . ? C174 Fe1 C181 107.2(3) . . ? C174 Fe1 C185 120.1(3) . . ? C181 Fe1 C185 40.5(3) . . ? C174 Fe1 C183 161.0(3) . . ? C181 Fe1 C183 67.8(3) . . ? C185 Fe1 C183 68.9(3) . . ? C174 Fe1 C172 67.9(3) . . ? C181 Fe1 C172 165.2(3) . . ? C185 Fe1 C172 128.6(3) . . ? C183 Fe1 C172 121.3(3) . . ? C174 Fe1 C184 156.2(3) . . ? C181 Fe1 C184 68.3(3) . . ? C185 Fe1 C184 41.2(3) . . ? C183 Fe1 C184 41.0(3) . . ? C172 Fe1 C184 110.1(3) . . ? C174 Fe1 C182 124.5(3) . . ? C181 Fe1 C182 40.3(3) . . ? C185 Fe1 C182 68.3(3) . . ? C183 Fe1 C182 40.0(3) . . ? C172 Fe1 C182 154.0(3) . . ? C184 Fe1 C182 68.2(3) . . ? C174 Fe1 C175 40.7(2) . . ? C181 Fe1 C175 118.0(3) . . ? C185 Fe1 C175 153.3(3) . . ? C183 Fe1 C175 124.0(3) . . ? C172 Fe1 C175 68.1(2) . . ? C184 Fe1 C175 162.6(3) . . ? C182 Fe1 C175 105.4(3) . . ? C174 Fe1 C173 41.3(2) . . ? C181 Fe1 C173 127.1(3) . . ? C185 Fe1 C173 109.0(3) . . ? C183 Fe1 C173 156.0(3) . . ? C172 Fe1 C173 40.2(2) . . ? C184 Fe1 C173 121.5(3) . . ? C182 Fe1 C173 163.3(3) . . ? C175 Fe1 C173 69.1(2) . . ? C174 Fe1 C171 68.3(2) . . ? C181 Fe1 C171 151.9(2) . . ? C185 Fe1 C171 165.8(3) . . ? C183 Fe1 C171 106.9(3) . . ? C172 Fe1 C171 41.00(19) . . ? C184 Fe1 C171 126.9(3) . . ? C182 Fe1 C171 117.8(2) . . ? C175 Fe1 C171 40.3(2) . . ? C173 Fe1 C171 68.9(2) . . ? C175 C171 C172 106.4(5) . . ? C175 C171 Pd1 140.0(4) . . ? C172 C171 Pd1 113.5(4) . . ? C175 C171 Fe1 69.0(3) . . ? C172 C171 Fe1 68.4(3) . . ? Pd1 C171 Fe1 128.2(3) . . ? C173 C172 C171 110.1(5) . . ? C173 C172 C176 133.6(5) . . ? C171 C172 C176 116.1(5) . . ? C173 C172 Fe1 70.3(4) . . ? C171 C172 Fe1 70.6(3) . . ? C176 C172 Fe1 129.3(4) . . ? C172 C173 C174 105.8(5) . . ? C172 C173 Fe1 69.5(3) . . ? C174 C173 Fe1 67.9(3) . . ? C175 C174 C173 109.6(6) . . ? C175 C174 Fe1 71.0(3) . . ? C173 C174 Fe1 70.8(3) . . ? C174 C175 C171 108.1(5) . . ? C174 C175 Fe1 68.3(3) . . ? C171 C175 Fe1 70.7(3) . . ? N177 C176 C172 106.6(4) . . ? C178 N177 C179 109.9(5) . . ? C178 N177 C176 109.8(5) . . ? C179 N177 C176 107.6(5) . . ? C178 N177 Pd1 114.6(4) . . ? C179 N177 Pd1 107.4(4) . . ? C176 N177 Pd1 107.3(3) . . ? C182 C181 C185 109.0(7) . . ? C182 C181 Fe1 70.2(4) . . ? C185 C181 Fe1 69.7(4) . . ? C181 C182 C183 108.4(6) . . ? C181 C182 Fe1 69.5(4) . . ? C183 C182 Fe1 69.8(4) . . ? C182 C183 C184 108.3(7) . . ? C182 C183 Fe1 70.2(4) . . ? C184 C183 Fe1 69.6(4) . . ? C183 C184 C185 107.2(7) . . ? C183 C184 Fe1 69.4(4) . . ? C185 C184 Fe1 69.2(4) . . ? C181 C185 C184 107.2(7) . . ? C181 C185 Fe1 69.8(4) . . ? C184 C185 Fe1 69.7(4) . . ? O93 C94 C95 107.4(12) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 30.14 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 2.831 _refine_diff_density_min -2.200 _refine_diff_density_rms 0.151 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END