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 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Howard Colquhoun' ; Dept of Chemistry University of Reading Whiteknights Reading Berks RG6 6AD ; ; ? #footnote for author 1 ; 'Sam Y. F. Chan' ; Dept of Chemistry University of Reading Whiteknights Reading Berks RG6 6AD ; ; ? # footnote 2 ; 'Ann M. Chippendale' ; Dept of Chemistry University of Reading Whiteknights Reading Berks RG6 6AD ; ; ? ; 'Michael G. B. Drew' ; Dept of Chemistry Imperial College South Kensington London SW7 2AZ ; ; ? ; 'David J. Williams' '' '' _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 ; Extended-chain, multinuclear transition metal complexes bridged by cyanodiazenido(1-), [N=N-CN]-, ligands ; data_1 _database_code_depnum_ccdc_archive 'CCDC 641370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H48 Br N3 P4 W' _chemical_formula_weight 1114.58 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 13.283(14) _cell_length_b 12.077(14) _cell_length_c 29.76(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.159(10) _cell_angle_gamma 90.00 _cell_volume 4747(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14561 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 26.07 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _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 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 3.450 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.539 _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 not-applicable _diffrn_standards_interval_time 2m _diffrn_standards_decay_% not-applicable _diffrn_reflns_number 14561 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.07 _reflns_number_total 8540 _reflns_number_gt 5700 _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. the nitrogen atoms in the ligand bonded to the tungsten atom could not be refined anisotropically and so were given isotropic thermal parameters. In addition the W-N100 and N100-N101 bonds were constrained to expected values. From a study of the electron density, we believe this problem is due to the proximity of N(100) to the heavy atom W and the relatively poor quality of the data, rather than to any structural disorder. ; _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^)+(0.1080P)^2^+21.2188P] 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 8540 _refine_ls_number_parameters 539 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1966 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.002 _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 0.62113(3) 0.28225(4) 0.872675(14) 0.04312(19) Uani 1 1 d D . . Br2 Br 0.46938(13) 0.20106(15) 0.91308(5) 0.0771(5) Uani 1 1 d . . . P1 P 0.7229(3) 0.1084(3) 0.87692(11) 0.0540(8) Uani 1 1 d . . . C2 C 0.7156(14) 0.0439(17) 0.8206(5) 0.097(6) Uani 1 1 d . . . H2A H 0.7833 0.0412 0.8112 0.116 Uiso 1 1 calc R . . H2B H 0.6927 -0.0319 0.8231 0.116 Uiso 1 1 calc R . . C3 C 0.6505(12) 0.0978(14) 0.7858(5) 0.074(4) Uani 1 1 d . . . H3A H 0.6188 0.0406 0.7663 0.089 Uiso 1 1 calc R . . H3B H 0.6931 0.1408 0.7678 0.089 Uiso 1 1 calc R . . P4 P 0.5499(3) 0.1896(3) 0.80119(10) 0.0503(8) Uani 1 1 d . . . C11 C 0.7002(11) -0.0101(11) 0.9125(5) 0.059(3) Uani 1 1 d . . . C12 C 0.7419(17) -0.1115(15) 0.9053(7) 0.100(6) Uani 1 1 d . . . H12 H 0.7762 -0.1226 0.8801 0.120 Uiso 1 1 calc R . . C13 C 0.733(2) -0.1992(15) 0.9360(8) 0.112(7) Uani 1 1 d . . . H13 H 0.7630 -0.2671 0.9308 0.134 Uiso 1 1 calc R . . C14 C 0.6859(19) -0.1879(18) 0.9704(9) 0.116(8) Uani 1 1 d . . . H14 H 0.6825 -0.2469 0.9902 0.139 Uiso 1 1 calc R . . C15 C 0.6384(16) -0.0871(16) 0.9791(6) 0.094(6) Uani 1 1 d . . . H15 H 0.6008 -0.0791 1.0035 0.112 Uiso 1 1 calc R . . C16 C 0.6501(13) -0.0016(13) 0.9500(5) 0.075(4) Uani 1 1 d . . . H16 H 0.6222 0.0666 0.9562 0.090 Uiso 1 1 calc R . . C21 C 0.8627(11) 0.1244(11) 0.8906(5) 0.060(3) Uani 1 1 d . . . C22 C 0.9152(13) 0.1745(15) 0.8600(7) 0.091(5) Uani 1 1 d . . . H22 H 0.8817 0.1979 0.8326 0.109 Uiso 1 1 calc R . . C23 C 1.0229(16) 0.1918(15) 0.8695(9) 0.110(7) Uani 1 1 d . . . H23 H 1.0607 0.2214 0.8478 0.132 Uiso 1 1 calc R . . C24 C 1.0678(17) 0.1628(19) 0.9122(10) 0.113(8) Uani 1 1 d . . . H24 H 1.1360 0.1782 0.9202 0.136 Uiso 1 1 calc R . . C25 C 1.0147(16) 0.1135(18) 0.9413(7) 0.099(6) Uani 1 1 d . . . H25 H 1.0467 0.0904 0.9690 0.118 Uiso 1 1 calc R . . C26 C 0.9111(11) 0.0954(14) 0.9312(5) 0.073(4) Uani 1 1 d . . . H26 H 0.8747 0.0629 0.9527 0.088 Uiso 1 1 calc R . . C31 C 0.5258(11) 0.2677(13) 0.7477(4) 0.058(3) Uani 1 1 d . . . C32 C 0.5342(12) 0.3809(15) 0.7480(4) 0.072(4) Uani 1 1 d . . . H32 H 0.5476 0.4186 0.7753 0.086 Uiso 1 1 calc R . . C33 C 0.5226(12) 0.4391(15) 0.7077(5) 0.081(5) Uani 1 1 d . . . H33 H 0.5305 0.5156 0.7079 0.097 Uiso 1 1 calc R . . C34 C 0.4996(13) 0.3850(14) 0.6676(4) 0.075(5) Uani 1 1 d . . . H34 H 0.4904 0.4246 0.6406 0.090 Uiso 1 1 calc R . . C36 C 0.5026(14) 0.2154(14) 0.7067(5) 0.081(5) Uani 1 1 d . . . H36 H 0.4953 0.1388 0.7058 0.097 Uiso 1 1 calc R . . C35 C 0.4904(15) 0.2753(16) 0.6673(5) 0.092(6) Uani 1 1 d . . . H35 H 0.4754 0.2385 0.6399 0.110 Uiso 1 1 calc R . . C41 C 0.4380(11) 0.1037(12) 0.8003(4) 0.059(3) Uani 1 1 d . . . C42 C 0.3465(16) 0.136(2) 0.7775(7) 0.115(7) Uani 1 1 d . . . H42 H 0.3451 0.1997 0.7602 0.139 Uiso 1 1 calc R . . C43 C 0.2538(17) 0.076(3) 0.7789(9) 0.137(10) Uani 1 1 d . . . H43 H 0.1910 0.1042 0.7677 0.164 Uiso 1 1 calc R . . C44 C 0.2669(18) -0.031(3) 0.7988(9) 0.151(13) Uani 1 1 d . . . H44 H 0.2104 -0.0763 0.7979 0.181 Uiso 1 1 calc R . . C45 C 0.351(2) -0.069(2) 0.8182(9) 0.138(10) Uani 1 1 d . . . H45 H 0.3551 -0.1401 0.8298 0.166 Uiso 1 1 calc R . . C46 C 0.4415(16) 0.0019(15) 0.8216(6) 0.095(6) Uani 1 1 d . . . H46 H 0.5010 -0.0218 0.8381 0.114 Uiso 1 1 calc R . . P5 P 0.5274(2) 0.4643(3) 0.87282(10) 0.0487(8) Uani 1 1 d . . . C6 C 0.5595(11) 0.5327(11) 0.9294(4) 0.061(3) Uani 1 1 d . . . H6A H 0.6179 0.5802 0.9282 0.073 Uiso 1 1 calc R . . H6B H 0.5031 0.5785 0.9362 0.073 Uiso 1 1 calc R . . C7 C 0.5825(10) 0.4463(12) 0.9671(4) 0.061(4) Uani 1 1 d . . . H7A H 0.5219 0.4044 0.9713 0.073 Uiso 1 1 calc R . . H7B H 0.6055 0.4829 0.9954 0.073 Uiso 1 1 calc R . . P8 P 0.6809(3) 0.3540(3) 0.95055(10) 0.0506(8) Uani 1 1 d . . . C51 C 0.3893(9) 0.4732(13) 0.8641(4) 0.058(4) Uani 1 1 d . . . C52 C 0.3373(15) 0.3945(18) 0.8373(6) 0.100(6) Uani 1 1 d . . . H52 H 0.3720 0.3365 0.8254 0.120 Uiso 1 1 calc R . . C53 C 0.2290(14) 0.402(2) 0.8279(7) 0.110(7) Uani 1 1 d . . . H53 H 0.1939 0.3515 0.8086 0.132 Uiso 1 1 calc R . . C54 C 0.1793(15) 0.483(2) 0.8468(8) 0.121(8) Uani 1 1 d . . . H54 H 0.1089 0.4846 0.8425 0.145 Uiso 1 1 calc R . . C55 C 0.2287(18) 0.558(4) 0.8713(10) 0.21(2) Uani 1 1 d . . . H55 H 0.1922 0.6162 0.8823 0.249 Uiso 1 1 calc R . . C56 C 0.3354(15) 0.557(2) 0.8821(8) 0.138(10) Uani 1 1 d . . . H56 H 0.3680 0.6116 0.9005 0.166 Uiso 1 1 calc R . . C62 C 0.5003(16) 0.6328(14) 0.8063(5) 0.086(5) Uani 1 1 d . . . H62 H 0.4316 0.6161 0.8036 0.104 Uiso 1 1 calc R . . C63 C 0.538(3) 0.7145(18) 0.7800(6) 0.120(9) Uani 1 1 d . . . H63 H 0.4939 0.7538 0.7594 0.144 Uiso 1 1 calc R . . C65 C 0.7087(17) 0.6810(16) 0.8154(7) 0.102(7) Uani 1 1 d . . . H65 H 0.7773 0.6985 0.8180 0.123 Uiso 1 1 calc R . . C64 C 0.636(3) 0.7369(17) 0.7841(7) 0.129(11) Uani 1 1 d . . . H64 H 0.6589 0.7916 0.7658 0.155 Uiso 1 1 calc R . . C66 C 0.6708(13) 0.6006(15) 0.8409(5) 0.079(5) Uani 1 1 d . . . H66 H 0.7146 0.5613 0.8616 0.095 Uiso 1 1 calc R . . C72 C 0.6250(13) 0.2217(14) 1.0230(5) 0.074(4) Uani 1 1 d . . . H72 H 0.5581 0.2412 1.0141 0.088 Uiso 1 1 calc R . . C73 C 0.646(2) 0.1541(16) 1.0579(5) 0.102(7) Uani 1 1 d . . . H73 H 0.5935 0.1313 1.0741 0.123 Uiso 1 1 calc R . . C74 C 0.7421(18) 0.1164(19) 1.0710(6) 0.106(7) Uani 1 1 d . . . H74 H 0.7533 0.0646 1.0941 0.127 Uiso 1 1 calc R . . C75 C 0.8222(16) 0.1563(17) 1.0495(5) 0.094(6) Uani 1 1 d . . . H75 H 0.8880 0.1337 1.0589 0.113 Uiso 1 1 calc R . . C76 C 0.8034(12) 0.2308(12) 1.0135(5) 0.066(4) Uani 1 1 d . . . H76 H 0.8561 0.2586 0.9987 0.079 Uiso 1 1 calc R . . C82 C 0.8579(13) 0.4417(17) 0.9229(5) 0.085(5) Uani 1 1 d . . . H82 H 0.8512 0.3895 0.8998 0.102 Uiso 1 1 calc R . . C83 C 0.9347(15) 0.520(2) 0.9262(7) 0.105(7) Uani 1 1 d . . . H83 H 0.9793 0.5209 0.9041 0.125 Uiso 1 1 calc R . . C84 C 0.9468(16) 0.592(2) 0.9594(9) 0.117(9) Uani 1 1 d . . . H84 H 0.9987 0.6437 0.9595 0.141 Uiso 1 1 calc R . . C85 C 0.8863(16) 0.5946(15) 0.9939(8) 0.105(7) Uani 1 1 d . . . H85 H 0.8987 0.6434 1.0180 0.126 Uiso 1 1 calc R . . C86 C 0.8038(13) 0.5195(14) 0.9910(6) 0.083(5) Uani 1 1 d . . . H86 H 0.7587 0.5206 1.0129 0.099 Uiso 1 1 calc R . . C61 C 0.5690(12) 0.5765(11) 0.8369(4) 0.058(3) Uani 1 1 d . . . C71 C 0.7004(11) 0.2633(12) 1.0001(4) 0.057(3) Uani 1 1 d . . . C81 C 0.7906(11) 0.4454(11) 0.9562(4) 0.059(4) Uani 1 1 d . . . N100 N 0.7103(8) 0.3352(10) 0.8399(3) 0.069(3) Uiso 1 1 d D . . N101 N 0.7579(5) 0.3764(6) 0.8145(2) 0.0227(15) Uiso 1 1 d D . . C102 C 0.8482(8) 0.4109(14) 0.8128(5) 0.073(4) Uiso 1 1 d D . . N103 N 0.9279(12) 0.4467(14) 0.8151(5) 0.101(5) Uiso 1 1 d . . . 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 0.0450(3) 0.0436(3) 0.0404(3) -0.0022(2) 0.00283(18) 0.0001(3) Br2 0.0798(11) 0.0802(12) 0.0721(9) 0.0089(8) 0.0122(8) -0.0063(9) P1 0.062(2) 0.046(2) 0.0530(18) -0.0055(15) -0.0018(15) 0.0114(17) C2 0.110(14) 0.121(16) 0.062(9) -0.015(9) 0.021(9) 0.056(13) C3 0.086(11) 0.071(11) 0.061(8) -0.012(7) -0.006(7) 0.032(9) P4 0.0528(19) 0.050(2) 0.0472(16) -0.0055(13) 0.0010(14) -0.0048(15) C11 0.062(8) 0.032(8) 0.078(9) 0.006(6) -0.009(7) -0.007(6) C12 0.133(17) 0.065(13) 0.102(13) -0.014(10) 0.017(12) 0.003(12) C13 0.15(2) 0.043(12) 0.148(19) 0.028(11) 0.031(16) 0.019(12) C14 0.13(2) 0.063(15) 0.16(2) 0.035(14) 0.005(16) -0.012(13) C15 0.127(16) 0.065(12) 0.095(12) 0.014(9) 0.043(11) -0.009(11) C16 0.089(12) 0.049(10) 0.087(10) 0.008(8) 0.009(9) 0.003(8) C21 0.063(8) 0.032(8) 0.086(9) -0.004(6) 0.009(7) 0.001(6) C22 0.068(11) 0.061(11) 0.145(16) 0.006(11) 0.022(11) 0.012(9) C23 0.093(15) 0.051(12) 0.19(2) -0.003(12) 0.056(15) -0.003(10) C24 0.082(14) 0.074(14) 0.18(2) -0.022(15) -0.021(15) -0.012(12) C25 0.100(15) 0.085(15) 0.107(14) -0.009(11) -0.007(12) -0.013(12) C26 0.063(9) 0.082(12) 0.069(9) -0.022(8) -0.014(7) -0.020(8) C31 0.060(8) 0.056(10) 0.059(8) -0.005(6) 0.005(6) 0.005(7) C32 0.084(11) 0.089(13) 0.042(7) -0.009(7) 0.007(6) -0.012(9) C33 0.092(12) 0.084(12) 0.064(9) 0.014(8) -0.004(8) -0.039(10) C34 0.099(12) 0.078(12) 0.046(7) 0.022(7) -0.006(7) -0.007(9) C36 0.115(14) 0.061(10) 0.062(9) -0.003(8) -0.011(9) 0.007(10) C35 0.136(16) 0.088(14) 0.047(8) -0.016(8) -0.015(9) -0.018(12) C41 0.062(8) 0.061(10) 0.053(7) -0.014(6) -0.001(6) -0.012(7) C42 0.101(15) 0.14(2) 0.101(14) 0.006(13) -0.025(11) -0.021(14) C43 0.062(13) 0.19(3) 0.15(2) -0.01(2) 0.012(13) -0.022(17) C44 0.059(13) 0.26(4) 0.13(2) 0.02(2) 0.004(13) -0.02(2) C45 0.18(3) 0.081(16) 0.16(2) 0.013(15) 0.08(2) -0.049(18) C46 0.107(15) 0.069(12) 0.105(13) 0.004(10) -0.004(11) -0.015(11) P5 0.0481(18) 0.0403(19) 0.0577(17) -0.0010(14) 0.0055(14) 0.0053(15) C6 0.071(9) 0.041(8) 0.071(8) -0.001(6) 0.010(7) 0.012(7) C7 0.061(8) 0.063(9) 0.057(7) -0.005(6) 0.002(6) 0.018(7) P8 0.0562(19) 0.048(2) 0.0458(16) -0.0082(14) -0.0012(14) 0.0053(16) C51 0.042(7) 0.079(10) 0.053(7) 0.015(7) 0.004(5) 0.019(7) C52 0.097(14) 0.101(15) 0.099(13) -0.027(11) -0.002(10) -0.013(12) C53 0.054(10) 0.130(19) 0.142(17) 0.001(15) -0.015(11) -0.016(12) C54 0.056(11) 0.17(2) 0.141(18) 0.017(17) 0.011(12) 0.053(14) C55 0.063(14) 0.35(5) 0.21(3) -0.15(3) 0.004(16) 0.05(2) C56 0.075(13) 0.18(3) 0.159(19) -0.072(18) 0.002(13) 0.048(15) C62 0.127(15) 0.052(10) 0.082(10) 0.002(8) 0.016(10) 0.000(10) C63 0.23(3) 0.074(14) 0.058(10) 0.005(9) 0.005(14) -0.041(18) C65 0.130(17) 0.077(13) 0.115(14) 0.020(11) 0.081(14) 0.009(12) C64 0.27(4) 0.050(12) 0.076(13) -0.017(9) 0.075(19) -0.037(18) C66 0.089(12) 0.079(12) 0.071(9) -0.027(8) 0.018(8) -0.002(10) C72 0.088(11) 0.075(11) 0.059(8) -0.008(8) 0.010(8) 0.011(10) C73 0.18(2) 0.078(13) 0.048(8) 0.005(8) 0.009(11) -0.011(14) C74 0.127(18) 0.112(17) 0.077(12) 0.036(11) 0.001(12) 0.001(14) C75 0.116(15) 0.097(14) 0.062(9) -0.002(9) -0.019(10) 0.032(12) C76 0.080(10) 0.047(8) 0.066(8) -0.006(7) -0.012(7) 0.015(8) C82 0.074(11) 0.107(15) 0.070(9) 0.013(9) -0.010(8) -0.022(10) C83 0.097(14) 0.128(19) 0.083(12) 0.020(12) -0.015(10) -0.041(14) C84 0.082(14) 0.107(18) 0.15(2) 0.057(17) -0.040(14) -0.025(13) C85 0.101(15) 0.054(11) 0.147(18) -0.032(12) -0.045(13) 0.024(11) C86 0.074(10) 0.061(11) 0.106(12) -0.026(9) -0.019(9) 0.001(9) C61 0.077(10) 0.042(8) 0.055(7) -0.008(6) 0.016(6) -0.001(7) C71 0.072(9) 0.049(8) 0.051(7) -0.007(6) 0.005(6) 0.013(7) C81 0.078(9) 0.036(8) 0.058(7) -0.006(6) -0.021(7) 0.005(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 W1 N100 1.736(7) . ? W1 P1 2.493(4) . ? W1 P4 2.498(4) . ? W1 P8 2.522(4) . ? W1 P5 2.527(4) . ? W1 Br2 2.644(3) . ? P1 C11 1.825(14) . ? P1 C2 1.842(15) . ? P1 C21 1.868(15) . ? C2 C3 1.43(2) . ? C3 P4 1.832(14) . ? P4 C41 1.811(14) . ? P4 C31 1.847(14) . ? C11 C16 1.36(2) . ? C11 C12 1.37(2) . ? C12 C13 1.41(3) . ? C13 C14 1.27(3) . ? C14 C15 1.41(3) . ? C15 C16 1.37(2) . ? C21 C26 1.35(2) . ? C21 C22 1.35(2) . ? C22 C23 1.44(3) . ? C23 C24 1.39(3) . ? C24 C25 1.32(3) . ? C25 C26 1.39(2) . ? C31 C36 1.38(2) . ? C31 C32 1.37(2) . ? C32 C33 1.38(2) . ? C33 C34 1.37(2) . ? C34 C35 1.33(2) . ? C36 C35 1.37(2) . ? C41 C42 1.38(2) . ? C41 C46 1.38(2) . ? C42 C43 1.43(3) . ? C43 C44 1.42(4) . ? C44 C45 1.29(3) . ? C45 C46 1.46(3) . ? P5 C51 1.828(13) . ? P5 C61 1.847(14) . ? P5 C6 1.882(13) . ? C6 C7 1.540(18) . ? C7 P8 1.826(13) . ? P8 C81 1.821(15) . ? P8 C71 1.833(14) . ? C51 C52 1.38(2) . ? C51 C56 1.38(2) . ? C52 C53 1.44(2) . ? C53 C54 1.33(3) . ? C54 C55 1.30(4) . ? C55 C56 1.42(3) . ? C62 C63 1.38(3) . ? C62 C61 1.39(2) . ? C63 C64 1.32(4) . ? C65 C66 1.36(2) . ? C65 C64 1.44(3) . ? C66 C61 1.38(2) . ? C72 C73 1.33(2) . ? C72 C71 1.37(2) . ? C73 C74 1.37(3) . ? C74 C75 1.39(3) . ? C75 C76 1.40(2) . ? C76 C71 1.44(2) . ? C82 C83 1.38(3) . ? C82 C81 1.40(2) . ? C83 C84 1.32(3) . ? C84 C85 1.37(3) . ? C85 C86 1.42(3) . ? C86 C81 1.367(19) . ? N100 N101 1.149(7) . ? N101 C102 1.276(9) . ? C102 N103 1.138(18) . ? 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 P1 86.5(4) . . ? N100 W1 P4 84.6(4) . . ? P1 W1 P4 79.63(12) . . ? N100 W1 P8 102.9(4) . . ? P1 W1 P8 97.31(11) . . ? P4 W1 P8 171.82(12) . . ? N100 W1 P5 92.7(4) . . ? P1 W1 P5 175.76(11) . . ? P4 W1 P5 104.44(12) . . ? P8 W1 P5 78.81(11) . . ? N100 W1 Br2 172.7(4) . . ? P1 W1 Br2 95.78(12) . . ? P4 W1 Br2 89.07(11) . . ? P8 W1 Br2 83.67(11) . . ? P5 W1 Br2 85.54(11) . . ? C11 P1 C2 101.5(9) . . ? C11 P1 C21 100.2(6) . . ? C2 P1 C21 101.3(8) . . ? C11 P1 W1 124.6(5) . . ? C2 P1 W1 109.6(6) . . ? C21 P1 W1 116.5(4) . . ? C3 C2 P1 115.7(12) . . ? C2 C3 P4 119.7(10) . . ? C41 P4 C3 105.6(8) . . ? C41 P4 C31 102.4(7) . . ? C3 P4 C31 99.1(7) . . ? C41 P4 W1 120.3(4) . . ? C3 P4 W1 105.3(5) . . ? C31 P4 W1 121.3(5) . . ? C16 C11 C12 115.8(15) . . ? C16 C11 P1 122.8(11) . . ? C12 C11 P1 121.1(14) . . ? C11 C12 C13 120.6(19) . . ? C14 C13 C12 122(2) . . ? C13 C14 C15 121(2) . . ? C16 C15 C14 116.9(18) . . ? C15 C16 C11 124.1(16) . . ? C26 C21 C22 119.3(15) . . ? C26 C21 P1 122.3(12) . . ? C22 C21 P1 118.1(12) . . ? C21 C22 C23 120.4(19) . . ? C24 C23 C22 117(2) . . ? C25 C24 C23 120(2) . . ? C24 C25 C26 121(2) . . ? C21 C26 C25 121.1(17) . . ? C36 C31 C32 118.2(13) . . ? C36 C31 P4 122.0(12) . . ? C32 C31 P4 119.8(10) . . ? C31 C32 C33 119.9(13) . . ? C34 C33 C32 120.5(16) . . ? C35 C34 C33 119.6(13) . . ? C35 C36 C31 120.7(16) . . ? C34 C35 C36 121.1(14) . . ? C42 C41 C46 117.2(17) . . ? C42 C41 P4 121.7(14) . . ? C46 C41 P4 121.1(13) . . ? C41 C42 C43 124(2) . . ? C44 C43 C42 114(2) . . ? C45 C44 C43 125(3) . . ? C44 C45 C46 119(3) . . ? C41 C46 C45 120(2) . . ? C51 P5 C61 103.5(7) . . ? C51 P5 C6 103.2(6) . . ? C61 P5 C6 98.2(6) . . ? C51 P5 W1 122.5(5) . . ? C61 P5 W1 117.3(5) . . ? C6 P5 W1 108.6(4) . . ? C7 C6 P5 111.3(9) . . ? C6 C7 P8 107.9(9) . . ? C81 P8 C7 101.2(7) . . ? C81 P8 C71 104.2(6) . . ? C7 P8 C71 101.0(6) . . ? C81 P8 W1 117.6(4) . . ? C7 P8 W1 107.1(4) . . ? C71 P8 W1 122.5(5) . . ? C52 C51 C56 118.9(16) . . ? C52 C51 P5 118.4(13) . . ? C56 C51 P5 122.7(14) . . ? C51 C52 C53 119.8(19) . . ? C54 C53 C52 120(2) . . ? C55 C54 C53 120(2) . . ? C54 C55 C56 123(3) . . ? C51 C56 C55 118(2) . . ? C63 C62 C61 118(2) . . ? C64 C63 C62 120(3) . . ? C66 C65 C64 116(2) . . ? C63 C64 C65 123(2) . . ? C65 C66 C61 121.4(19) . . ? C73 C72 C71 120.9(18) . . ? C72 C73 C74 123(2) . . ? C73 C74 C75 119.4(18) . . ? C74 C75 C76 119.6(18) . . ? C75 C76 C71 118.3(17) . . ? C83 C82 C81 116.7(18) . . ? C84 C83 C82 122(2) . . ? C83 C84 C85 123(2) . . ? C84 C85 C86 116.9(19) . . ? C81 C86 C85 120.0(18) . . ? C66 C61 C62 121.4(15) . . ? C66 C61 P5 117.2(12) . . ? C62 C61 P5 121.4(13) . . ? C72 C71 C76 119.2(14) . . ? C72 C71 P8 125.0(12) . . ? C76 C71 P8 115.7(11) . . ? C86 C81 C82 121.1(16) . . ? C86 C81 P8 120.2(13) . . ? C82 C81 P8 118.7(11) . . ? N101 N100 W1 170.4(11) . . ? N100 N101 C102 138.8(11) . . ? N103 C102 N101 173.4(18) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 2.766 _refine_diff_density_min -1.707 _refine_diff_density_rms 0.168 _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_2 _database_code_depnum_ccdc_archive 'CCDC 641371' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C114 H108 N6 O8 P8 Br2 Rh2 W2 . 2.7(C H2 Cl2)' _chemical_formula_sum 'C116.70 H113.40 Br2 Cl5.40 N6 O8 P8 Rh2 W2' _chemical_formula_weight 2900.46 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' Rh Rh 0.0927 3.6045 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 27.888(4) _cell_length_b 13.2256(11) _cell_length_c 17.4034(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.467(8) _cell_angle_gamma 90.00 _cell_volume 6122.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 11.21 _cell_measurement_theta_max 25.27 _exptl_crystal_description Platy_Rhombs _exptl_crystal_colour Orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2879 _exptl_absorpt_coefficient_mu 8.805 _exptl_absorpt_correction_type 'Lamina (0 0 1)' _exptl_absorpt_correction_T_min 0.24794 _exptl_absorpt_correction_T_max 0.80952 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8737 _diffrn_reflns_av_R_equivalents 0.1036 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 60.01 _reflns_number_total 8405 _reflns_number_gt 6415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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. Restraints were used for the phenyl rings which were refined as rigid groups. Also for two of the dichloromethane molecules which were disordered with each having two resolved overlapping orientations while the remainder have ordered partial occupancy single site orientations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+24.1000P] 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 SHELXL _refine_ls_extinction_coef 0.00017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8405 _refine_ls_number_parameters 660 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.053 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.218575(15) 0.49615(3) 0.13878(3) 0.03669(18) Uani 1 d . . . Rh Rh 0.45813(3) 0.50985(7) 0.45566(5) 0.0524(2) Uani 1 d . . . Br Br 0.13860(4) 0.43600(9) 0.02457(7) 0.0533(3) Uani 1 d . . . P1 P 0.26445(9) 0.38414(18) 0.06894(15) 0.0405(5) Uani 1 d . . . P2 P 0.22480(10) 0.60515(19) 0.02424(16) 0.0457(6) Uani 1 d . . . P3 P 0.16722(9) 0.60538(19) 0.19980(16) 0.0409(5) Uani 1 d . . . P4 P 0.20518(10) 0.38235(19) 0.24455(17) 0.0445(6) Uani 1 d . . . O1 O 0.4327(3) 0.4532(7) 0.5459(6) 0.070(2) Uani 1 d . . . O2 O 0.4623(3) 0.3667(7) 0.4158(6) 0.069(2) Uani 1 d . . . O3 O 0.5110(3) 0.4364(8) 0.6282(6) 0.074(3) Uani 1 d . . . O4 O 0.5411(3) 0.3483(6) 0.4985(6) 0.068(2) Uani 1 d . . . N1 N 0.2703(3) 0.5421(6) 0.2152(5) 0.0425(18) Uani 1 d . . . C1 C 0.3453(4) 0.5519(8) 0.3215(8) 0.054(3) Uani 1 d . . . N3 N 0.3812(3) 0.5307(8) 0.3694(7) 0.066(3) Uani 1 d . . . N2 N 0.3036(4) 0.5931(7) 0.2724(7) 0.064(3) Uani 1 d . . . C2 C 0.3314(2) 0.4086(6) 0.1023(4) 0.047(2) Uani 1 d G . . C3 C 0.3574(3) 0.4422(8) 0.0505(4) 0.070(3) Uani 1 d G . . H3A H 0.3407 0.4504 -0.0040 0.083 Uiso 1 calc R . . C4 C 0.4085(3) 0.4633(9) 0.0802(6) 0.117(7) Uani 1 d G . . H4A H 0.4259 0.4858 0.0455 0.141 Uiso 1 calc R . . C5 C 0.4335(2) 0.4510(9) 0.1617(6) 0.115(7) Uani 1 d G . . H5A H 0.4677 0.4651 0.1815 0.138 Uiso 1 calc R . . C6 C 0.4075(3) 0.4174(8) 0.2135(4) 0.084(5) Uani 1 d G . . H6A H 0.4242 0.4091 0.2681 0.101 Uiso 1 calc R . . C7 C 0.3564(3) 0.3962(7) 0.1838(4) 0.067(3) Uani 1 d G . . H7A H 0.3390 0.3737 0.2185 0.081 Uiso 1 calc R . . C8 C 0.2608(3) 0.2456(4) 0.0638(6) 0.053(3) Uani 1 d G . . C9 C 0.2142(2) 0.2000(5) 0.0516(6) 0.064(3) Uani 1 d G . . H9A H 0.1858 0.2395 0.0468 0.076 Uiso 1 calc R . . C10 C 0.2099(3) 0.0953(5) 0.0467(6) 0.076(4) Uani 1 d G . . H10A H 0.1788 0.0648 0.0386 0.091 Uiso 1 calc R . . C11 C 0.2523(4) 0.0363(4) 0.0540(6) 0.086(5) Uani 1 d G . . H11A H 0.2495 -0.0338 0.0507 0.103 Uiso 1 calc R . . C12 C 0.2989(3) 0.0819(5) 0.0661(7) 0.085(5) Uani 1 d G . . H12A H 0.3272 0.0424 0.0710 0.103 Uiso 1 calc R . . C13 C 0.3031(2) 0.1866(5) 0.0711(6) 0.071(4) Uani 1 d G . . H13A H 0.3343 0.2171 0.0792 0.085 Uiso 1 calc R . . C14 C 0.2433(4) 0.4146(8) -0.0365(7) 0.052(3) Uani 1 d . . . H14A H 0.2668 0.3858 -0.0616 0.062 Uiso 1 calc R . . H14B H 0.2111 0.3819 -0.0602 0.062 Uiso 1 calc R . . C15 C 0.2375(6) 0.5268(9) -0.0571(8) 0.072(4) Uani 1 d . . . H15A H 0.2101 0.5356 -0.1064 0.087 Uiso 1 calc R . . H15B H 0.2680 0.5510 -0.0668 0.087 Uiso 1 calc R . . C16 C 0.2756(3) 0.6973(6) 0.0385(5) 0.055(3) Uani 1 d G . . C17 C 0.2750(3) 0.7626(8) -0.0244(5) 0.090(5) Uani 1 d G . . H17A H 0.2478 0.7624 -0.0711 0.108 Uiso 1 calc R . . C18 C 0.3151(4) 0.8280(7) -0.0176(7) 0.117(8) Uani 1 d G . . H18A H 0.3147 0.8717 -0.0597 0.140 Uiso 1 calc R . . C19 C 0.3558(4) 0.8282(7) 0.0521(8) 0.103(7) Uani 1 d G . . H19A H 0.3826 0.8720 0.0567 0.124 Uiso 1 calc R . . C20 C 0.3564(3) 0.7630(9) 0.1150(7) 0.132(8) Uani 1 d G . . H20A H 0.3836 0.7631 0.1617 0.159 Uiso 1 calc R . . C21 C 0.3163(4) 0.6975(8) 0.1082(5) 0.092(5) Uani 1 d G . . H21A H 0.3167 0.6539 0.1503 0.111 Uiso 1 calc R . . C22 C 0.1698(2) 0.6823(5) -0.0269(4) 0.052(3) Uani 1 d G . . C23 C 0.1648(3) 0.7759(5) 0.0062(4) 0.055(3) Uani 1 d G . . H23A H 0.1899 0.7995 0.0507 0.066 Uiso 1 calc R . . C24 C 0.1221(3) 0.8341(5) -0.0272(6) 0.074(4) Uani 1 d G . . H24A H 0.1187 0.8967 -0.0050 0.088 Uiso 1 calc R . . C25 C 0.0844(3) 0.7987(7) -0.0937(6) 0.086(5) Uani 1 d G . . H25A H 0.0559 0.8376 -0.1161 0.103 Uiso 1 calc R . . C26 C 0.0895(3) 0.7051(8) -0.1268(5) 0.094(5) Uani 1 d G . . H26A H 0.0643 0.6814 -0.1714 0.113 Uiso 1 calc R . . C27 C 0.1322(3) 0.6469(5) -0.0934(5) 0.072(4) Uani 1 d G . . H27A H 0.1355 0.5843 -0.1156 0.087 Uiso 1 calc R . . C28 C 0.1746(3) 0.7434(4) 0.2058(5) 0.052(3) Uani 1 d G . . C29 C 0.1340(2) 0.8086(6) 0.1942(6) 0.071(4) Uani 1 d G . . H29A H 0.1016 0.7826 0.1834 0.085 Uiso 1 calc R . . C30 C 0.1416(3) 0.9125(5) 0.1987(7) 0.092(5) Uani 1 d G . . H30A H 0.1144 0.9562 0.1909 0.110 Uiso 1 calc R . . C31 C 0.1900(4) 0.9513(4) 0.2147(6) 0.082(4) Uani 1 d G . . H31A H 0.1951 1.0209 0.2177 0.098 Uiso 1 calc R . . C32 C 0.2306(3) 0.8861(6) 0.2264(7) 0.085(4) Uani 1 d G . . H32A H 0.2630 0.9121 0.2371 0.102 Uiso 1 calc R . . C33 C 0.2230(2) 0.7822(5) 0.2219(6) 0.066(3) Uani 1 d G . . H33A H 0.2502 0.7386 0.2297 0.079 Uiso 1 calc R . . C34 C 0.0998(2) 0.5886(6) 0.1684(4) 0.050(3) Uani 1 d G . . C35 C 0.0752(3) 0.5459(7) 0.2190(5) 0.081(4) Uani 1 d G . . H35A H 0.0932 0.5283 0.2715 0.097 Uiso 1 calc R . . C36 C 0.0236(3) 0.5295(8) 0.1913(7) 0.107(6) Uani 1 d G . . H36A H 0.0071 0.5009 0.2251 0.128 Uiso 1 calc R . . C37 C -0.0034(2) 0.5558(9) 0.1129(7) 0.112(7) Uani 1 d G . . H37A H -0.0379 0.5449 0.0943 0.134 Uiso 1 calc R . . C38 C 0.0213(3) 0.5985(8) 0.0622(5) 0.088(5) Uani 1 d G . . H38A H 0.0033 0.6162 0.0098 0.105 Uiso 1 calc R . . C39 C 0.0729(3) 0.6149(6) 0.0900(4) 0.066(3) Uani 1 d G . . H39A H 0.0894 0.6435 0.0561 0.080 Uiso 1 calc R . . C40 C 0.1887(4) 0.5740(8) 0.3073(7) 0.051(2) Uani 1 d . . . H40A H 0.2209 0.6064 0.3312 0.061 Uiso 1 calc R . . H40B H 0.1651 0.6029 0.3325 0.061 Uiso 1 calc R . . C41 C 0.1943(6) 0.4619(9) 0.3278(8) 0.071(4) Uani 1 d . . . H41A H 0.1641 0.4384 0.3390 0.086 Uiso 1 calc R . . H41B H 0.2222 0.4527 0.3763 0.086 Uiso 1 calc R . . C42 C 0.2603(2) 0.3060(5) 0.2950(4) 0.049(2) Uani 1 d G . . C43 C 0.2983(3) 0.3441(5) 0.3598(5) 0.065(3) Uani 1 d G . . H43A H 0.2943 0.4063 0.3820 0.078 Uiso 1 calc R . . C44 C 0.3423(3) 0.2891(8) 0.3914(5) 0.083(4) Uani 1 d G . . H44A H 0.3678 0.3146 0.4347 0.099 Uiso 1 calc R . . C45 C 0.3483(2) 0.1961(7) 0.3582(6) 0.089(5) Uani 1 d G . . H45A H 0.3778 0.1594 0.3794 0.107 Uiso 1 calc R . . C46 C 0.3103(3) 0.1580(5) 0.2934(6) 0.083(4) Uani 1 d G . . H46A H 0.3143 0.0958 0.2713 0.100 Uiso 1 calc R . . C47 C 0.2663(3) 0.2129(5) 0.2618(4) 0.061(3) Uani 1 d G . . H47A H 0.2408 0.1875 0.2185 0.073 Uiso 1 calc R . . C48 C 0.1528(7) 0.2927(18) 0.2320(15) 0.08(2) Uani 0.60 d PGU A 1 C49 C 0.1583(8) 0.212(2) 0.2854(16) 0.091(13) Uani 0.60 d PGU A 1 H49A H 0.1895 0.1988 0.3223 0.109 Uiso 0.60 calc PR A 1 C50 C 0.1172(12) 0.152(2) 0.284(2) 0.114(18) Uani 0.60 d PGU A 1 H50A H 0.1208 0.0982 0.3194 0.136 Uiso 0.60 calc PR A 1 C51 C 0.0706(10) 0.172(2) 0.229(2) 0.13(2) Uani 0.60 d PGU A 1 H51A H 0.0430 0.1317 0.2273 0.158 Uiso 0.60 calc PR A 1 C52 C 0.0651(7) 0.252(2) 0.1751(15) 0.087(10) Uani 0.60 d PGU A 1 H52A H 0.0339 0.2659 0.1382 0.104 Uiso 0.60 calc PR A 1 C53 C 0.1062(8) 0.3128(17) 0.1769(12) 0.063(7) Uani 0.60 d PGU A 1 H53A H 0.1026 0.3666 0.1412 0.076 Uiso 0.60 calc PR A 1 C48' C 0.1544(10) 0.290(2) 0.2347(15) 0.05(2) Uani 0.40 d PGU A 2 C49' C 0.1528(11) 0.239(3) 0.3033(15) 0.081(18) Uani 0.40 d PGU A 2 H49B H 0.1783 0.2472 0.3515 0.097 Uiso 0.40 calc PR A 2 C50' C 0.1130(13) 0.174(3) 0.300(2) 0.069(14) Uani 0.40 d PGU A 2 H50B H 0.1119 0.1390 0.3459 0.082 Uiso 0.40 calc PR A 2 C51' C 0.0748(11) 0.161(3) 0.228(2) 0.09(2) Uani 0.40 d PGU A 2 H51B H 0.0481 0.1175 0.2257 0.103 Uiso 0.40 calc PR A 2 C52' C 0.0764(11) 0.213(3) 0.1594(17) 0.12(3) Uani 0.40 d PGU A 2 H52B H 0.0508 0.2042 0.1112 0.144 Uiso 0.40 calc PR A 2 C53' C 0.1162(13) 0.278(3) 0.1627(13) 0.11(2) Uani 0.40 d PGU A 2 H53B H 0.1173 0.3124 0.1168 0.138 Uiso 0.40 calc PR A 2 C54 C 0.4645(5) 0.4285(11) 0.6110(8) 0.067(3) Uani 1 d . . . C55 C 0.4442(7) 0.3858(16) 0.6746(11) 0.107(6) Uani 1 d . . . H55A H 0.4696 0.3889 0.7259 0.160 Uiso 1 calc R . . H55B H 0.4344 0.3168 0.6620 0.160 Uiso 1 calc R . . H55C H 0.4155 0.4245 0.6768 0.160 Uiso 1 calc R . . C56 C 0.5023(5) 0.3173(10) 0.4474(9) 0.070(4) Uani 1 d . . . C57 C 0.5037(7) 0.2089(12) 0.4172(14) 0.117(8) Uani 1 d . . . H57A H 0.5171 0.1647 0.4623 0.175 Uiso 1 calc R . . H57B H 0.5247 0.2063 0.3824 0.175 Uiso 1 calc R . . H57C H 0.4703 0.1878 0.3880 0.175 Uiso 1 calc R . . C58 C 0.5994(7) 0.2997(16) 0.1454(18) 0.113(10) Uani 0.70 d PD . . H58A H 0.6174 0.2568 0.1899 0.135 Uiso 0.70 calc PR . . H58B H 0.5895 0.2582 0.0973 0.135 Uiso 0.70 calc PR . . Cl1 Cl 0.6367(5) 0.3872(8) 0.1336(9) 0.187(5) Uani 0.70 d PDU . . Cl2 Cl 0.5492(5) 0.3419(12) 0.1630(12) 0.256(9) Uani 0.70 d PDU . . C59 C 0.052(3) 0.169(5) -0.102(3) 0.10(2) Uiso 0.25 d PD B 1 H59A H 0.0789 0.1557 -0.1262 0.117 Uiso 0.25 calc PR B 1 H59B H 0.0463 0.2413 -0.1047 0.117 Uiso 0.25 calc PR B 1 Cl3 Cl 0.0711(13) 0.135(4) -0.009(2) 0.25(3) Uani 0.25 d PDU B 1 Cl4 Cl 0.0019(17) 0.111(5) -0.153(2) 0.25(3) Uani 0.25 d PDU B 1 C59' C 0.0287(10) 0.155(5) -0.121(4) 0.13(2) Uiso 0.40 d PD C 2 H59C H 0.0193 0.1444 -0.1787 0.156 Uiso 0.40 calc PR C 2 H59D H 0.0250 0.2259 -0.1111 0.156 Uiso 0.40 calc PR C 2 Cl3' Cl 0.0868(8) 0.122(2) -0.0816(19) 0.213(11) Uani 0.40 d PDU C 2 Cl4' Cl -0.0088(9) 0.090(3) -0.084(4) 0.34(2) Uani 0.40 d PDU C 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 W 0.0341(3) 0.0366(3) 0.0416(3) 0.00291(18) 0.01467(18) -0.00076(17) Rh 0.0315(4) 0.0607(5) 0.0601(5) -0.0065(4) 0.0061(3) 0.0062(3) Br 0.0410(5) 0.0620(7) 0.0538(6) -0.0043(5) 0.0096(4) -0.0044(5) P1 0.0408(12) 0.0408(12) 0.0427(13) -0.0016(10) 0.0166(10) 0.0009(10) P2 0.0503(14) 0.0438(13) 0.0468(15) 0.0089(11) 0.0204(11) 0.0019(11) P3 0.0378(12) 0.0413(12) 0.0464(14) -0.0036(10) 0.0172(10) -0.0007(10) P4 0.0475(13) 0.0416(12) 0.0477(14) 0.0082(11) 0.0195(11) -0.0016(11) O1 0.039(4) 0.087(6) 0.079(6) 0.002(5) 0.012(4) 0.000(4) O2 0.046(4) 0.072(5) 0.080(6) -0.011(5) 0.006(4) 0.005(4) O3 0.043(4) 0.108(7) 0.066(6) 0.008(5) 0.010(4) -0.006(5) O4 0.041(4) 0.063(5) 0.092(7) -0.013(5) 0.006(4) 0.007(4) N1 0.050(4) 0.039(4) 0.045(5) -0.002(4) 0.023(4) -0.002(4) C1 0.038(6) 0.045(6) 0.075(8) -0.008(5) 0.012(6) 0.001(5) N3 0.036(5) 0.076(7) 0.069(6) -0.013(5) -0.010(5) 0.011(5) N2 0.050(5) 0.056(5) 0.070(7) -0.006(5) -0.005(5) 0.005(5) C2 0.040(5) 0.052(6) 0.052(6) -0.004(5) 0.019(4) 0.009(5) C3 0.043(6) 0.103(10) 0.066(8) 0.002(7) 0.022(6) -0.007(7) C4 0.061(9) 0.171(19) 0.127(17) -0.028(15) 0.039(10) -0.040(11) C5 0.035(7) 0.146(16) 0.159(19) -0.045(15) 0.024(9) -0.007(9) C6 0.050(7) 0.128(13) 0.070(9) -0.027(9) 0.011(6) 0.004(8) C7 0.046(6) 0.078(8) 0.073(8) -0.012(7) 0.011(6) 0.014(6) C8 0.057(6) 0.044(5) 0.061(7) 0.002(5) 0.020(5) -0.004(5) C9 0.070(7) 0.051(6) 0.076(9) -0.010(6) 0.030(7) -0.013(6) C10 0.085(9) 0.054(7) 0.088(10) -0.005(7) 0.025(8) -0.015(7) C11 0.126(14) 0.058(7) 0.069(9) -0.001(7) 0.022(9) 0.004(9) C12 0.073(9) 0.048(7) 0.136(15) 0.000(8) 0.032(9) 0.006(7) C13 0.055(7) 0.053(7) 0.100(11) -0.005(7) 0.014(7) 0.004(6) C14 0.056(6) 0.060(6) 0.046(6) -0.004(5) 0.023(5) 0.000(5) C15 0.105(11) 0.069(7) 0.058(8) 0.013(6) 0.048(8) 0.016(8) C16 0.057(6) 0.051(6) 0.065(7) 0.007(5) 0.030(6) -0.003(5) C17 0.069(9) 0.085(10) 0.121(14) 0.056(10) 0.037(9) 0.006(8) C18 0.109(14) 0.084(11) 0.19(2) 0.062(13) 0.095(16) 0.002(10) C19 0.092(12) 0.067(9) 0.18(2) -0.008(11) 0.089(14) -0.021(9) C20 0.103(14) 0.17(2) 0.135(18) -0.019(15) 0.047(13) -0.079(15) C21 0.083(10) 0.102(11) 0.095(12) 0.005(9) 0.031(9) -0.048(9) C22 0.061(6) 0.053(6) 0.042(6) 0.013(5) 0.016(5) 0.004(5) C23 0.058(6) 0.058(6) 0.051(6) 0.012(5) 0.019(5) 0.006(5) C24 0.071(8) 0.067(8) 0.088(10) 0.014(7) 0.031(8) 0.017(7) C25 0.068(9) 0.096(11) 0.096(12) 0.041(9) 0.028(8) 0.026(8) C26 0.063(8) 0.112(13) 0.091(12) 0.012(10) -0.003(8) -0.008(9) C27 0.074(8) 0.081(9) 0.053(7) 0.004(6) 0.006(6) -0.006(7) C28 0.059(6) 0.045(5) 0.055(7) 0.003(5) 0.020(5) 0.004(5) C29 0.077(8) 0.053(7) 0.080(9) -0.007(6) 0.018(7) 0.008(6) C30 0.120(13) 0.054(7) 0.112(13) -0.010(8) 0.049(11) 0.022(9) C31 0.112(12) 0.047(7) 0.089(11) -0.004(7) 0.033(9) -0.018(8) C32 0.085(10) 0.061(8) 0.100(12) -0.003(7) 0.015(8) -0.029(8) C33 0.064(7) 0.055(7) 0.077(9) 0.001(6) 0.019(6) -0.007(6) C34 0.039(5) 0.056(6) 0.058(7) -0.015(5) 0.019(5) -0.006(5) C35 0.049(7) 0.096(10) 0.105(12) 0.010(9) 0.033(7) 0.002(7) C36 0.067(10) 0.125(14) 0.146(18) -0.036(13) 0.057(11) -0.030(10) C37 0.035(7) 0.159(17) 0.137(17) -0.069(15) 0.021(9) -0.008(9) C38 0.051(7) 0.094(10) 0.100(12) -0.029(9) -0.004(7) 0.025(7) C39 0.055(7) 0.077(8) 0.065(8) -0.014(7) 0.015(6) 0.009(6) C40 0.048(5) 0.055(6) 0.050(6) -0.006(5) 0.015(5) 0.001(5) C41 0.099(10) 0.063(7) 0.064(8) 0.006(6) 0.041(8) 0.012(7) C42 0.042(5) 0.052(6) 0.054(6) 0.011(5) 0.017(5) -0.002(5) C43 0.055(7) 0.069(7) 0.065(8) 0.007(6) 0.009(6) -0.008(6) C44 0.049(7) 0.098(11) 0.090(11) 0.029(9) 0.005(7) -0.009(7) C45 0.046(7) 0.123(13) 0.101(12) 0.053(11) 0.025(7) 0.020(8) C46 0.072(9) 0.081(9) 0.106(12) 0.035(9) 0.042(9) 0.031(8) C47 0.058(7) 0.057(6) 0.068(8) 0.018(6) 0.019(6) 0.006(6) C48 0.06(2) 0.09(3) 0.11(4) 0.07(2) 0.06(2) 0.029(18) C49 0.050(16) 0.068(16) 0.15(3) 0.041(18) 0.022(19) 0.002(14) C50 0.09(3) 0.054(15) 0.20(5) 0.03(2) 0.05(3) -0.007(18) C51 0.11(4) 0.14(4) 0.16(5) 0.08(3) 0.08(3) 0.00(3) C52 0.060(15) 0.12(2) 0.09(2) 0.008(18) 0.023(15) -0.021(16) C53 0.050(12) 0.093(17) 0.042(12) 0.016(13) 0.007(10) -0.020(13) C48' 0.05(3) 0.03(2) 0.06(3) -0.03(2) 0.00(2) -0.02(2) C49' 0.039(18) 0.11(4) 0.09(3) 0.09(3) 0.023(19) 0.02(2) C50' 0.05(2) 0.09(3) 0.07(2) 0.07(2) 0.027(18) 0.00(2) C51' 0.04(2) 0.06(2) 0.15(6) -0.03(3) 0.03(3) -0.04(2) C52' 0.10(4) 0.18(6) 0.09(3) 0.00(4) 0.05(3) -0.09(4) C53' 0.09(4) 0.17(5) 0.09(3) -0.04(3) 0.04(3) -0.09(4) C54 0.053(7) 0.092(9) 0.058(7) 0.009(7) 0.019(6) 0.003(7) C55 0.076(10) 0.151(17) 0.099(13) 0.020(12) 0.037(9) -0.022(11) C56 0.062(8) 0.065(7) 0.086(10) -0.017(7) 0.028(7) 0.002(6) C57 0.088(11) 0.073(10) 0.18(2) -0.058(12) 0.021(12) 0.005(9) C58 0.11(2) 0.084(15) 0.13(2) -0.026(15) 0.021(18) 0.034(15) Cl1 0.164(9) 0.154(8) 0.247(14) -0.041(9) 0.069(10) -0.063(8) Cl2 0.130(9) 0.276(16) 0.37(2) -0.114(16) 0.088(12) 0.036(10) Cl3 0.15(3) 0.33(5) 0.27(5) -0.16(4) 0.04(3) 0.03(3) Cl4 0.18(4) 0.39(7) 0.14(3) -0.12(4) -0.02(2) 0.01(4) Cl3' 0.147(16) 0.24(2) 0.28(3) 0.01(2) 0.113(19) 0.045(17) Cl4' 0.119(17) 0.35(4) 0.55(7) 0.10(5) 0.11(3) 0.00(2) _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 W N1 1.751(9) . ? W P3 2.486(2) . ? W P4 2.491(3) . ? W P1 2.498(2) . ? W P2 2.508(3) . ? W Br 2.6261(12) . ? Rh O2 2.031(9) . ? Rh O3 2.033(9) 3_666 ? Rh O4 2.036(8) 3_666 ? Rh O1 2.049(9) . ? Rh N3 2.235(9) . ? Rh Rh 2.3960(15) 3_666 ? P1 C14 1.796(11) . ? P1 C2 1.810(6) . ? P1 C8 1.836(5) . ? P2 C16 1.830(6) . ? P2 C22 1.835(6) . ? P2 C15 1.871(13) . ? P3 C34 1.807(6) . ? P3 C40 1.833(11) . ? P3 C28 1.837(6) . ? P4 C42 1.828(6) . ? P4 C48' 1.835(19) . ? P4 C48 1.843(18) . ? P4 C41 1.888(13) . ? O1 C54 1.255(15) . ? O2 C56 1.267(16) . ? O3 C54 1.245(15) . ? O4 C56 1.247(16) . ? N1 N2 1.324(13) . ? C1 N3 1.130(15) . ? C1 N2 1.336(15) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C14 C15 1.524(16) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C40 C41 1.522(16) . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C48' C49' 1.3900 . ? C48' C53' 1.3900 . ? C49' C50' 1.3900 . ? C50' C51' 1.3900 . ? C51' C52' 1.3900 . ? C52' C53' 1.3900 . ? C54 O3 1.245(15) . ? C54 C55 1.50(2) . ? C56 O4 1.247(16) . ? C56 C57 1.531(18) . ? C58 Cl1 1.611(14) . ? C58 Cl2 1.618(14) . ? C59 Cl3 1.615(15) . ? C59 Cl4 1.616(15) . ? C59' Cl3' 1.616(15) . ? C59' Cl4' 1.617(15) . ? 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 N1 W P3 85.6(3) . . ? N1 W P4 85.4(3) . . ? P3 W P4 78.58(9) . . ? N1 W P1 98.6(3) . . ? P3 W P1 175.76(8) . . ? P4 W P1 102.33(9) . . ? N1 W P2 99.6(3) . . ? P3 W P2 101.05(9) . . ? P4 W P2 174.94(9) . . ? P1 W P2 77.67(8) . . ? N1 W Br 177.0(3) . . ? P3 W Br 91.84(7) . . ? P4 W Br 95.43(7) . . ? P1 W Br 83.96(7) . . ? P2 W Br 79.52(7) . . ? O2 Rh O3 90.1(4) . 3_666 ? O2 Rh O4 175.9(3) . 3_666 ? O3 Rh O4 90.1(4) 3_666 3_666 ? O2 Rh O1 89.4(4) . . ? O3 Rh O1 175.4(3) 3_666 . ? O4 Rh O1 90.1(4) 3_666 . ? O2 Rh N3 91.6(4) . . ? O3 Rh N3 90.1(4) 3_666 . ? O4 Rh N3 92.5(4) 3_666 . ? O1 Rh N3 94.4(4) . . ? O2 Rh Rh 88.5(2) . 3_666 ? O3 Rh Rh 87.7(2) 3_666 3_666 ? O4 Rh Rh 87.4(2) 3_666 3_666 ? O1 Rh Rh 87.8(2) . 3_666 ? N3 Rh Rh 177.8(3) . 3_666 ? C14 P1 C2 106.2(4) . . ? C14 P1 C8 100.2(5) . . ? C2 P1 C8 103.4(4) . . ? C14 P1 W 107.7(4) . . ? C2 P1 W 111.6(3) . . ? C8 P1 W 125.9(3) . . ? C16 P2 C22 101.3(4) . . ? C16 P2 C15 99.0(6) . . ? C22 P2 C15 105.1(5) . . ? C16 P2 W 120.7(3) . . ? C22 P2 W 117.3(3) . . ? C15 P2 W 110.9(4) . . ? C34 P3 C40 105.8(4) . . ? C34 P3 C28 103.2(4) . . ? C40 P3 C28 99.8(4) . . ? C34 P3 W 118.7(3) . . ? C40 P3 W 104.5(3) . . ? C28 P3 W 122.2(3) . . ? C42 P4 C48' 101.1(10) . . ? C42 P4 C48 102.9(8) . . ? C48' P4 C48 1.9(15) . . ? C42 P4 C41 104.2(5) . . ? C48' P4 C41 98.2(10) . . ? C48 P4 C41 98.3(10) . . ? C42 P4 W 113.4(3) . . ? C48' P4 W 127.9(9) . . ? C48 P4 W 126.2(7) . . ? C41 P4 W 109.0(4) . . ? C54 O1 Rh 118.3(8) . . ? C56 O2 Rh 117.8(8) . . ? C54 O3 Rh 119.4(9) . 3_666 ? C56 O4 Rh 119.1(8) . 3_666 ? N2 N1 W 168.4(7) . . ? N3 C1 N2 169.4(13) . . ? C1 N3 Rh 170.4(11) . . ? N1 N2 C1 123.6(10) . . ? C3 C2 C7 120.0 . . ? C3 C2 P1 122.6(4) . . ? C7 C2 P1 117.4(4) . . ? C4 C3 C2 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C6 C7 C2 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 118.5(4) . . ? C13 C8 P1 121.5(4) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C8 120.0 . . ? C15 C14 P1 116.0(8) . . ? C14 C15 P2 113.1(8) . . ? C17 C16 C21 120.0 . . ? C17 C16 P2 118.8(5) . . ? C21 C16 P2 121.0(5) . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C16 120.0 . . ? C23 C22 C27 120.0 . . ? C23 C22 P2 117.9(4) . . ? C27 C22 P2 122.0(4) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.0 . . ? C29 C28 C33 120.0 . . ? C29 C28 P3 122.4(4) . . ? C33 C28 P3 117.6(4) . . ? C30 C29 C28 120.0 . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C32 C33 C28 120.0 . . ? C35 C34 C39 120.0 . . ? C35 C34 P3 121.7(5) . . ? C39 C34 P3 118.2(5) . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C34 120.0 . . ? C41 C40 P3 116.0(8) . . ? C40 C41 P4 113.1(8) . . ? C43 C42 C47 120.0 . . ? C43 C42 P4 121.1(4) . . ? C47 C42 P4 118.6(4) . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C46 C47 C42 120.0 . . ? C49 C48 C53 120.0 . . ? C49 C48 P4 119.3(13) . . ? C53 C48 P4 120.1(13) . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C52 C53 C48 120.0 . . ? C49' C48' C53' 120.0 . . ? C49' C48' P4 118.1(16) . . ? C53' C48' P4 121.8(16) . . ? C48' C49' C50' 120.0 . . ? C51' C50' C49' 120.0 . . ? C52' C51' C50' 120.0 . . ? C51' C52' C53' 120.0 . . ? C52' C53' C48' 120.0 . . ? O3 C54 O1 126.8(12) . . ? O3 C54 C55 116.9(13) . . ? O1 C54 C55 116.4(12) . . ? O4 C56 O2 127.1(12) . . ? O4 C56 C57 116.5(13) . . ? O2 C56 C57 116.4(13) . . ? Cl1 C58 Cl2 113.9(14) . . ? Cl3 C59 Cl4 112.9(16) . . ? Cl3' C59' Cl4' 112.3(16) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 60.01 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 1.780 _refine_diff_density_min -3.363 _refine_diff_density_rms 0.159 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 641372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C106 H96 Br2 Cl2 N6 P8 Pd W2 . 10(C H CL3)' _chemical_formula_sum 'C116 H106 Br2 Cl32 N6 P8 Pd W2' _chemical_formula_weight 3600.15 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' Pd Pd 0.1215 3.9337 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4189(8) _cell_length_b 16.2144(11) _cell_length_c 18.3904(6) _cell_angle_alpha 81.823(5) _cell_angle_beta 83.808(5) _cell_angle_gamma 79.185(5) _cell_volume 3587.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.07 _cell_measurement_theta_max 27.98 _exptl_crystal_description 'rhombic needles' _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 11.251 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3791 _exptl_absorpt_correction_T_max 0.7847 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11832 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 62.00 _reflns_number_total 11241 _reflns_number_gt 8924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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. Restraints were used for the phenyl rings which were refined as rigid groups. Also for two of the ten included chloroform molecules are disordered and adopt resolved overlapping partial occupancy orientations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+8.9548P] 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 SHELXL _refine_ls_extinction_coef 0.00026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11241 _refine_ls_number_parameters 690 _refine_ls_number_restraints 153 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.18117(3) 0.306781(19) 0.216788(16) 0.02707(12) Uani 1 d . . . Br Br 0.23210(7) 0.16601(5) 0.15713(4) 0.0404(2) Uani 1 d . . . Pd Pd 0.0000 0.5000 0.5000 0.0441(2) Uani 1 d S . . Cl Cl -0.1183(2) 0.62264(15) 0.46189(12) 0.0584(5) Uani 1 d . . . N1 N 0.1494(5) 0.4036(4) 0.2529(3) 0.0336(13) Uani 1 d . . . N2 N 0.1283(7) 0.4807(4) 0.2723(3) 0.0459(17) Uani 1 d . . . N3 N 0.0780(8) 0.5016(5) 0.4010(4) 0.056(2) Uani 1 d . . . C1 C 0.0992(7) 0.4883(5) 0.3405(5) 0.0428(18) Uani 1 d . . . P1 P 0.31690(16) 0.36014(11) 0.11887(9) 0.0319(4) Uani 1 d . . . C2 C 0.3509(5) 0.4635(3) 0.1275(3) 0.0417(18) Uani 1 d G . . C3 C 0.3651(7) 0.5223(4) 0.0660(2) 0.063(3) Uani 1 d G . . H3A H 0.3546 0.5105 0.0195 0.076 Uiso 1 calc R . . C4 C 0.3952(8) 0.5987(3) 0.0740(3) 0.087(4) Uani 1 d G . . H4A H 0.4047 0.6380 0.0329 0.105 Uiso 1 calc R . . C5 C 0.4109(7) 0.6162(3) 0.1435(4) 0.079(4) Uani 1 d G . . H5A H 0.4310 0.6674 0.1489 0.095 Uiso 1 calc R . . C6 C 0.3967(7) 0.5574(4) 0.2050(3) 0.063(3) Uani 1 d G . . H6A H 0.4073 0.5692 0.2515 0.076 Uiso 1 calc R . . C7 C 0.3667(6) 0.4810(3) 0.1970(2) 0.054(2) Uani 1 d G . . H7A H 0.3572 0.4417 0.2381 0.065 Uiso 1 calc R . . C8 C 0.4505(4) 0.2985(3) 0.0942(3) 0.0381(16) Uani 1 d G . . C9 C 0.4583(4) 0.2361(3) 0.0484(3) 0.0479(19) Uani 1 d G . . H9A H 0.3964 0.2294 0.0270 0.057 Uiso 1 calc R . . C10 C 0.5585(5) 0.1837(3) 0.0345(3) 0.063(3) Uani 1 d G . . H10A H 0.5637 0.1420 0.0038 0.076 Uiso 1 calc R . . C11 C 0.6509(4) 0.1938(4) 0.0665(4) 0.072(3) Uani 1 d G . . H11A H 0.7180 0.1587 0.0572 0.086 Uiso 1 calc R . . C12 C 0.6431(4) 0.2562(4) 0.1123(4) 0.068(3) Uani 1 d G . . H12A H 0.7050 0.2629 0.1337 0.082 Uiso 1 calc R . . C13 C 0.5429(5) 0.3086(3) 0.1262(3) 0.052(2) Uani 1 d G . . H13A H 0.5377 0.3503 0.1568 0.062 Uiso 1 calc R . . C14 C 0.2493(7) 0.3792(5) 0.0318(4) 0.0429(18) Uani 1 d . . . H14A H 0.2914 0.4106 -0.0062 0.051 Uiso 1 calc R . . H14B H 0.2451 0.3257 0.0154 0.051 Uiso 1 calc R . . C15 C 0.1344(7) 0.4294(5) 0.0457(4) 0.0439(18) Uani 1 d . . . H15A H 0.0980 0.4422 0.0003 0.053 Uiso 1 calc R . . H15B H 0.1386 0.4823 0.0632 0.053 Uiso 1 calc R . . P2 P 0.05601(16) 0.36492(11) 0.11578(10) 0.0330(4) Uani 1 d . . . C16 C -0.0688(4) 0.4416(3) 0.1367(3) 0.0370(16) Uani 1 d G . . C17 C -0.1724(4) 0.4226(3) 0.1327(3) 0.051(2) Uani 1 d G . . H17A H -0.1790 0.3718 0.1171 0.061 Uiso 1 calc R . . C18 C -0.2662(3) 0.4795(4) 0.1519(4) 0.060(2) Uani 1 d G . . H18A H -0.3355 0.4667 0.1492 0.072 Uiso 1 calc R . . C19 C -0.2563(4) 0.5554(4) 0.1752(4) 0.062(3) Uani 1 d G . . H19A H -0.3191 0.5934 0.1881 0.075 Uiso 1 calc R . . C20 C -0.1528(5) 0.5745(3) 0.1793(3) 0.060(2) Uani 1 d G . . H20A H -0.1462 0.6253 0.1948 0.072 Uiso 1 calc R . . C21 C -0.0590(4) 0.5176(3) 0.1600(3) 0.0427(18) Uani 1 d G . . H21A H 0.0103 0.5303 0.1627 0.051 Uiso 1 calc R . . C22 C 0.0038(5) 0.2974(3) 0.0608(3) 0.0391(16) Uani 1 d G . . C23 C -0.0206(6) 0.3257(3) -0.0115(3) 0.066(3) Uani 1 d G . . H23A H -0.0101 0.3795 -0.0328 0.079 Uiso 1 calc R . . C24 C -0.0606(7) 0.2737(5) -0.0521(2) 0.081(4) Uani 1 d G . . H24A H -0.0770 0.2927 -0.1004 0.097 Uiso 1 calc R . . C25 C -0.0763(6) 0.1933(4) -0.0203(3) 0.076(3) Uani 1 d G . . H25A H -0.1031 0.1585 -0.0475 0.092 Uiso 1 calc R . . C26 C -0.0519(6) 0.1649(3) 0.0520(4) 0.062(3) Uani 1 d G . . H26A H -0.0623 0.1112 0.0732 0.074 Uiso 1 calc R . . C27 C -0.0118(5) 0.2170(3) 0.0925(2) 0.0465(19) Uani 1 d G . . H27A H 0.0045 0.1980 0.1409 0.056 Uiso 1 calc R . . P3 P 0.05146(15) 0.23586(11) 0.30961(9) 0.0310(4) Uani 1 d . . . C28 C -0.0489(4) 0.3065(3) 0.3630(3) 0.0358(16) Uani 1 d G . . C29 C -0.0850(5) 0.2804(3) 0.4353(3) 0.059(2) Uani 1 d G . . H29A H -0.0565 0.2268 0.4578 0.071 Uiso 1 calc R . . C30 C -0.1636(6) 0.3344(4) 0.4740(2) 0.073(3) Uani 1 d G . . H30A H -0.1877 0.3169 0.5224 0.087 Uiso 1 calc R . . C31 C -0.2061(5) 0.4145(4) 0.4404(3) 0.060(3) Uani 1 d G . . H31A H -0.2587 0.4506 0.4663 0.072 Uiso 1 calc R . . C32 C -0.1700(5) 0.4406(3) 0.3681(3) 0.055(2) Uani 1 d G . . H32A H -0.1984 0.4942 0.3456 0.066 Uiso 1 calc R . . C33 C -0.0914(5) 0.3866(3) 0.3294(2) 0.0474(19) Uani 1 d G . . H33A H -0.0672 0.4041 0.2810 0.057 Uiso 1 calc R . . C34 C -0.0318(4) 0.1624(3) 0.2866(3) 0.0371(16) Uani 1 d G . . C35 C 0.0179(3) 0.0806(3) 0.2749(3) 0.0448(18) Uani 1 d G . . H35A H 0.0928 0.0629 0.2796 0.054 Uiso 1 calc R . . C36 C -0.0443(5) 0.0251(3) 0.2561(4) 0.060(3) Uani 1 d G . . H36A H -0.0110 -0.0296 0.2482 0.072 Uiso 1 calc R . . C37 C -0.1562(5) 0.0515(3) 0.2490(4) 0.060(2) Uani 1 d G . . H37A H -0.1979 0.0144 0.2364 0.072 Uiso 1 calc R . . C38 C -0.2059(3) 0.1333(4) 0.2607(4) 0.058(2) Uani 1 d G . . H38A H -0.2808 0.1509 0.2559 0.069 Uiso 1 calc R . . C39 C -0.1437(4) 0.1887(3) 0.2795(3) 0.050(2) Uani 1 d G . . H39A H -0.1770 0.2434 0.2873 0.060 Uiso 1 calc R . . C40 C 0.1339(7) 0.1706(5) 0.3806(4) 0.0439(18) Uani 1 d . . . H40A H 0.0867 0.1561 0.4243 0.053 Uiso 1 calc R . . H40B H 0.1719 0.1186 0.3625 0.053 Uiso 1 calc R . . C41 C 0.2172(7) 0.2212(6) 0.3993(4) 0.0431(18) Uani 1 d . . . H41A H 0.2599 0.1891 0.4384 0.052 Uiso 1 calc R . . H41B H 0.1792 0.2739 0.4162 0.052 Uiso 1 calc R . . P4 P 0.30833(16) 0.24323(11) 0.31622(10) 0.0339(4) Uani 1 d . . . C42 C 0.3946(4) 0.3102(3) 0.3461(3) 0.0397(17) Uani 1 d G . . C43 C 0.3450(4) 0.3777(4) 0.3839(3) 0.050(2) Uani 1 d G . . H43A H 0.2698 0.3855 0.3974 0.060 Uiso 1 calc R . . C44 C 0.4078(5) 0.4334(4) 0.4016(4) 0.068(3) Uani 1 d G . . H44A H 0.3746 0.4785 0.4270 0.081 Uiso 1 calc R . . C45 C 0.5202(5) 0.4216(4) 0.3814(5) 0.078(4) Uani 1 d G . . H45A H 0.5622 0.4589 0.3933 0.093 Uiso 1 calc R . . C46 C 0.5698(4) 0.3542(4) 0.3435(5) 0.080(4) Uani 1 d G . . H46A H 0.6451 0.3463 0.3300 0.096 Uiso 1 calc R . . C47 C 0.5070(4) 0.2985(3) 0.3259(4) 0.057(2) Uani 1 d G . . H47A H 0.5402 0.2533 0.3005 0.069 Uiso 1 calc R . . C48 C 0.4022(4) 0.1427(3) 0.3094(3) 0.0410(17) Uani 1 d G . . C49 C 0.4621(4) 0.1288(3) 0.2426(2) 0.0434(18) Uani 1 d G . . H49A H 0.4519 0.1693 0.2016 0.052 Uiso 1 calc R . . C50 C 0.5374(5) 0.0543(3) 0.2371(3) 0.054(2) Uani 1 d G . . H50A H 0.5775 0.0450 0.1925 0.065 Uiso 1 calc R . . C51 C 0.5527(5) -0.0063(3) 0.2984(4) 0.072(3) Uani 1 d G . . H51A H 0.6030 -0.0561 0.2948 0.086 Uiso 1 calc R . . C52 C 0.4927(6) 0.0076(4) 0.3652(3) 0.085(4) Uani 1 d G . . H52A H 0.5030 -0.0329 0.4062 0.102 Uiso 1 calc R . . C53 C 0.4175(6) 0.0821(4) 0.3707(3) 0.065(3) Uani 1 d G . . H53A H 0.3773 0.0914 0.4154 0.078 Uiso 1 calc R . . C54 C 0.2026(7) -0.0595(4) 0.5455(5) 0.100(5) Uani 1 d D . . H54A H 0.1556 -0.0806 0.5877 0.120 Uiso 1 calc R . . Cl1 Cl 0.2179(4) 0.0413(2) 0.55729(19) 0.1076(13) Uani 1 d D . . Cl2 Cl 0.3270(6) -0.1278(4) 0.5434(5) 0.194(3) Uani 1 d D . . Cl3 Cl 0.1387(8) -0.0584(4) 0.4666(3) 0.203(4) Uani 1 d D . . C55 C 0.2367(5) 0.1041(3) -0.0366(4) 0.067(3) Uani 1 d D . . H55A H 0.1921 0.1203 0.0082 0.080 Uiso 1 calc R . . Cl4 Cl 0.1671(4) 0.0405(3) -0.0750(3) 0.1326(18) Uani 1 d D . . Cl5 Cl 0.3616(3) 0.0487(2) -0.0092(2) 0.0987(11) Uani 1 d D . . Cl6 Cl 0.2512(4) 0.1969(2) -0.0930(2) 0.1113(13) Uani 1 d D . . C56 C 0.3235(4) -0.0691(6) 0.1953(3) 0.082(4) Uani 1 d D . . H56A H 0.3326 -0.0098 0.1837 0.099 Uiso 1 calc R . . Cl7 Cl 0.2171(5) -0.0822(4) 0.1473(3) 0.152(2) Uani 1 d D . . Cl8 Cl 0.4461(4) -0.1304(3) 0.1669(3) 0.1353(18) Uani 1 d D . . Cl9 Cl 0.2894(5) -0.0870(4) 0.2889(2) 0.1405(19) Uani 1 d D . . C57 C 0.0235(7) 0.7347(5) 0.3169(4) 0.121(7) Uani 1 d D . . H57A H -0.0110 0.6906 0.3475 0.146 Uiso 1 calc R . . Cl10 Cl 0.0315(5) 0.8129(2) 0.3697(2) 0.1190(16) Uani 1 d D . . Cl11 Cl -0.0562(9) 0.7782(5) 0.2449(4) 0.225(5) Uani 1 d D . . Cl12 Cl 0.1536(8) 0.6906(3) 0.2833(5) 0.253(6) Uani 1 d D . . C58 C 0.6393(13) -0.2987(8) 0.3935(7) 0.090(8) Uani 0.55 d PD A 1 H58A H 0.6999 -0.3299 0.4218 0.108 Uiso 0.55 calc PR A 1 Cl13 Cl 0.5593(18) -0.2230(11) 0.4425(9) 0.160(8) Uani 0.55 d PD A 1 Cl14 Cl 0.5561(15) -0.3666(7) 0.3760(10) 0.179(6) Uani 0.55 d PD A 1 Cl15 Cl 0.6897(15) -0.2494(8) 0.3109(9) 0.194(8) Uani 0.55 d PD A 1 C58A C 0.6038(19) -0.3125(13) 0.4109(10) 0.122(16) Uiso 0.45 d PD B 2 H58B H 0.6546 -0.3571 0.4378 0.147 Uiso 0.45 calc PR B 2 Cl16 Cl 0.4692(19) -0.3282(17) 0.4261(17) 0.255(12) Uani 0.45 d PD B 2 Cl17 Cl 0.633(2) -0.307(2) 0.3165(10) 0.268(14) Uani 0.45 d PD B 2 Cl18 Cl 0.603(2) -0.2136(10) 0.4355(12) 0.202(14) Uani 0.45 d PD B 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 W 0.03438(18) 0.02147(16) 0.02631(17) -0.00023(10) 0.00230(11) -0.01212(11) Br 0.0476(5) 0.0294(4) 0.0467(4) -0.0076(3) 0.0026(3) -0.0145(3) Pd 0.0572(5) 0.0439(4) 0.0343(4) -0.0164(3) 0.0030(4) -0.0119(4) Cl 0.0731(15) 0.0513(12) 0.0476(11) -0.0115(9) 0.0020(10) -0.0028(10) N1 0.043(3) 0.022(3) 0.034(3) 0.007(2) 0.004(3) -0.016(2) N2 0.080(5) 0.026(3) 0.032(3) -0.009(2) 0.006(3) -0.012(3) N3 0.080(6) 0.046(4) 0.039(4) -0.011(3) 0.011(4) -0.004(4) C1 0.050(5) 0.030(4) 0.045(5) -0.005(3) 0.003(4) -0.002(3) P1 0.0402(10) 0.0269(8) 0.0291(8) -0.0001(6) 0.0090(7) -0.0161(7) C2 0.051(5) 0.027(4) 0.046(4) -0.002(3) 0.010(4) -0.013(3) C3 0.103(8) 0.039(5) 0.052(5) -0.002(4) 0.012(5) -0.036(5) C4 0.147(13) 0.045(6) 0.075(7) 0.001(5) 0.027(8) -0.059(7) C5 0.097(9) 0.036(5) 0.108(9) -0.009(5) 0.018(7) -0.040(6) C6 0.094(8) 0.044(5) 0.065(6) -0.022(4) 0.004(5) -0.038(5) C7 0.075(6) 0.041(5) 0.050(5) -0.002(4) 0.006(4) -0.028(4) C8 0.041(4) 0.032(4) 0.040(4) 0.005(3) 0.006(3) -0.013(3) C9 0.049(5) 0.041(4) 0.052(5) -0.006(4) 0.008(4) -0.014(4) C10 0.058(6) 0.043(5) 0.084(7) -0.016(5) 0.024(5) -0.006(4) C11 0.054(6) 0.045(5) 0.107(9) -0.004(5) 0.022(6) -0.002(4) C12 0.042(5) 0.065(6) 0.096(8) 0.009(6) -0.008(5) -0.020(5) C13 0.052(5) 0.042(4) 0.063(5) -0.002(4) 0.005(4) -0.018(4) C14 0.051(5) 0.044(4) 0.031(4) 0.005(3) 0.009(3) -0.015(4) C15 0.048(5) 0.044(4) 0.037(4) 0.011(3) -0.004(3) -0.014(4) P2 0.0421(10) 0.0281(8) 0.0287(8) 0.0022(7) 0.0000(7) -0.0113(7) C16 0.050(4) 0.032(4) 0.030(3) 0.006(3) -0.001(3) -0.016(3) C17 0.046(5) 0.048(5) 0.056(5) -0.003(4) 0.000(4) -0.008(4) C18 0.047(5) 0.059(6) 0.073(6) -0.010(5) -0.002(5) -0.005(4) C19 0.062(6) 0.062(6) 0.055(5) -0.008(4) 0.003(5) 0.009(5) C20 0.083(7) 0.040(5) 0.051(5) -0.005(4) -0.007(5) 0.001(5) C21 0.050(5) 0.031(4) 0.043(4) 0.000(3) -0.006(3) -0.001(3) C22 0.044(4) 0.037(4) 0.034(4) -0.005(3) 0.003(3) -0.007(3) C23 0.096(8) 0.067(6) 0.043(5) 0.001(4) -0.018(5) -0.032(6) C24 0.110(10) 0.105(9) 0.041(5) -0.023(6) -0.017(6) -0.036(8) C25 0.074(7) 0.105(9) 0.068(7) -0.047(7) 0.009(6) -0.040(7) C26 0.061(6) 0.059(6) 0.075(7) -0.019(5) -0.004(5) -0.027(5) C27 0.053(5) 0.049(5) 0.044(4) -0.003(4) -0.008(4) -0.025(4) P3 0.0362(9) 0.0281(8) 0.0290(8) 0.0037(6) 0.0032(7) -0.0154(7) C28 0.040(4) 0.038(4) 0.033(4) -0.002(3) 0.004(3) -0.020(3) C29 0.075(7) 0.050(5) 0.044(5) 0.002(4) 0.013(4) -0.003(5) C30 0.086(8) 0.092(8) 0.032(4) -0.007(5) 0.012(5) -0.006(6) C31 0.054(5) 0.086(7) 0.049(5) -0.039(5) 0.013(4) -0.019(5) C32 0.055(5) 0.048(5) 0.061(5) -0.016(4) 0.012(4) -0.004(4) C33 0.057(5) 0.042(4) 0.042(4) -0.004(3) 0.006(4) -0.009(4) C34 0.045(4) 0.034(4) 0.031(3) 0.004(3) 0.003(3) -0.015(3) C35 0.045(4) 0.032(4) 0.058(5) -0.003(3) 0.005(4) -0.015(3) C36 0.076(7) 0.042(5) 0.068(6) -0.011(4) 0.009(5) -0.029(5) C37 0.067(6) 0.053(5) 0.069(6) -0.012(5) 0.002(5) -0.034(5) C38 0.052(5) 0.071(6) 0.059(5) -0.009(5) -0.007(4) -0.032(5) C39 0.048(5) 0.050(5) 0.054(5) -0.008(4) 0.002(4) -0.016(4) C40 0.049(5) 0.042(4) 0.039(4) 0.014(3) -0.001(3) -0.019(4) C41 0.045(4) 0.054(5) 0.030(4) 0.009(3) -0.005(3) -0.017(4) P4 0.0377(10) 0.0310(9) 0.0338(9) 0.0010(7) -0.0008(7) -0.0126(8) C42 0.041(4) 0.041(4) 0.041(4) -0.003(3) -0.003(3) -0.017(3) C43 0.054(5) 0.057(5) 0.046(4) -0.016(4) -0.010(4) -0.017(4) C44 0.062(6) 0.065(6) 0.083(7) -0.035(6) -0.003(5) -0.012(5) C45 0.057(6) 0.065(7) 0.128(10) -0.048(7) -0.009(6) -0.026(5) C46 0.045(6) 0.081(8) 0.128(11) -0.052(7) -0.004(6) -0.022(5) C47 0.043(5) 0.050(5) 0.084(7) -0.025(5) -0.002(5) -0.009(4) C48 0.038(4) 0.036(4) 0.049(4) 0.003(3) -0.002(3) -0.017(3) C49 0.036(4) 0.030(4) 0.063(5) -0.006(3) -0.006(4) -0.001(3) C50 0.046(5) 0.035(4) 0.080(6) -0.012(4) 0.005(4) -0.007(4) C51 0.059(6) 0.036(5) 0.112(9) 0.004(5) -0.005(6) 0.002(4) C52 0.090(9) 0.055(6) 0.089(8) 0.029(6) 0.001(7) 0.009(6) C53 0.073(7) 0.054(6) 0.053(5) 0.017(4) 0.004(5) 0.004(5) C54 0.132(13) 0.092(10) 0.067(8) 0.013(7) 0.011(8) -0.026(9) Cl1 0.158(4) 0.092(2) 0.0713(19) 0.0082(17) -0.002(2) -0.036(2) Cl2 0.157(6) 0.133(5) 0.256(8) -0.013(5) 0.075(6) 0.009(4) Cl3 0.384(12) 0.138(4) 0.123(4) 0.038(3) -0.094(6) -0.140(6) C55 0.081(7) 0.058(6) 0.068(6) -0.030(5) 0.004(5) -0.019(5) Cl4 0.130(4) 0.100(3) 0.195(5) -0.080(3) -0.031(3) -0.033(3) Cl5 0.099(3) 0.0664(18) 0.129(3) -0.0196(18) -0.009(2) -0.0055(17) Cl6 0.159(4) 0.074(2) 0.105(3) -0.0030(18) -0.037(3) -0.022(2) C56 0.106(10) 0.067(7) 0.084(8) -0.020(6) 0.008(7) -0.041(7) Cl7 0.142(4) 0.199(6) 0.146(4) -0.067(4) -0.015(3) -0.071(4) Cl8 0.117(3) 0.140(4) 0.156(4) -0.080(3) 0.024(3) -0.014(3) Cl9 0.128(4) 0.200(6) 0.088(3) -0.017(3) 0.018(3) -0.031(4) C57 0.23(2) 0.068(8) 0.074(8) -0.015(7) 0.028(11) -0.067(11) Cl10 0.219(5) 0.0691(19) 0.074(2) -0.0114(15) -0.024(3) -0.030(3) Cl11 0.369(13) 0.230(8) 0.128(5) -0.006(5) -0.084(6) -0.162(9) Cl12 0.333(11) 0.080(3) 0.284(9) -0.003(4) 0.177(9) -0.007(5) C58 0.11(2) 0.038(10) 0.12(2) -0.004(11) -0.022(17) 0.000(12) Cl13 0.247(18) 0.096(9) 0.118(9) -0.030(6) 0.015(11) 0.017(9) Cl14 0.224(15) 0.112(7) 0.232(15) -0.033(8) -0.081(13) -0.061(9) Cl15 0.229(16) 0.106(7) 0.204(14) 0.015(8) 0.069(12) 0.007(8) Cl16 0.180(19) 0.23(2) 0.35(3) 0.01(2) -0.01(2) -0.072(18) Cl17 0.26(3) 0.42(4) 0.147(14) -0.17(2) 0.062(15) -0.07(3) Cl18 0.35(3) 0.050(5) 0.22(2) -0.039(9) -0.21(2) 0.040(11) _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 W N1 1.752(6) . ? W P1 2.5064(16) . ? W P2 2.5159(19) . ? W P3 2.5248(16) . ? W P4 2.5250(19) . ? W Br 2.6143(8) . ? Pd N3 1.968(7) . ? Pd N3 1.968(7) 2_566 ? Pd Cl 2.309(2) 2_566 ? Pd Cl 2.309(2) . ? N1 N2 1.320(9) . ? N2 C1 1.284(10) . ? N3 C1 1.155(11) . ? P1 C8 1.817(4) . ? P1 C2 1.834(4) . ? P1 C14 1.848(8) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C14 C15 1.520(12) . ? C15 P2 1.852(8) . ? P2 C22 1.834(4) . ? P2 C16 1.839(4) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? P3 C28 1.830(4) . ? P3 C40 1.833(8) . ? P3 C34 1.835(4) . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C40 C41 1.530(11) . ? C41 P4 1.835(8) . ? P4 C48 1.829(4) . ? P4 C42 1.834(4) . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C54 Cl2 1.724(4) . ? C54 Cl3 1.725(4) . ? C54 Cl1 1.727(4) . ? C55 Cl5 1.728(4) . ? C55 Cl4 1.728(4) . ? C55 Cl6 1.729(4) . ? C56 Cl9 1.724(4) . ? C56 Cl7 1.727(4) . ? C56 Cl8 1.728(4) . ? C57 Cl10 1.726(4) . ? C57 Cl12 1.727(4) . ? C57 Cl11 1.728(4) . ? C58 Cl13 1.724(4) . ? C58 Cl15 1.725(4) . ? C58 Cl14 1.725(4) . ? C58A Cl18 1.725(4) . ? C58A Cl16 1.726(4) . ? C58A Cl17 1.726(4) . ? 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 N1 W P1 92.51(18) . . ? N1 W P2 90.3(2) . . ? P1 W P2 80.13(6) . . ? N1 W P3 94.43(18) . . ? P1 W P3 173.04(6) . . ? P2 W P3 100.26(6) . . ? N1 W P4 91.8(2) . . ? P1 W P4 99.80(6) . . ? P2 W P4 177.86(6) . . ? P3 W P4 79.54(6) . . ? N1 W Br 177.31(17) . . ? P1 W Br 84.97(4) . . ? P2 W Br 88.31(5) . . ? P3 W Br 88.10(5) . . ? P4 W Br 89.55(5) . . ? N3 Pd N3 180.000(2) . 2_566 ? N3 Pd Cl 89.5(2) . 2_566 ? N3 Pd Cl 90.5(2) 2_566 2_566 ? N3 Pd Cl 90.5(2) . . ? N3 Pd Cl 89.5(2) 2_566 . ? Cl Pd Cl 180.0 2_566 . ? N2 N1 W 173.4(5) . . ? C1 N2 N1 117.6(6) . . ? C1 N3 Pd 158.8(8) . . ? N3 C1 N2 173.6(9) . . ? C8 P1 C2 102.6(3) . . ? C8 P1 C14 103.1(3) . . ? C2 P1 C14 103.5(3) . . ? C8 P1 W 123.25(18) . . ? C2 P1 W 115.96(19) . . ? C14 P1 W 106.2(2) . . ? C3 C2 C7 120.0 . . ? C3 C2 P1 121.4(3) . . ? C7 C2 P1 118.6(3) . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C7 C6 C5 120.0 . . ? C6 C7 C2 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 119.7(3) . . ? C13 C8 P1 120.1(3) . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C15 C14 P1 108.2(5) . . ? C14 C15 P2 108.3(5) . . ? C22 P2 C16 101.6(3) . . ? C22 P2 C15 103.0(3) . . ? C16 P2 C15 101.8(3) . . ? C22 P2 W 122.97(19) . . ? C16 P2 W 118.37(18) . . ? C15 P2 W 106.3(3) . . ? C17 C16 C21 120.0 . . ? C17 C16 P2 120.6(3) . . ? C21 C16 P2 119.4(3) . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C16 120.0 . . ? C23 C22 C27 120.0 . . ? C23 C22 P2 120.9(3) . . ? C27 C22 P2 119.1(3) . . ? C24 C23 C22 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.0 . . ? C28 P3 C40 102.8(3) . . ? C28 P3 C34 102.5(3) . . ? C40 P3 C34 102.4(3) . . ? C28 P3 W 115.72(17) . . ? C40 P3 W 107.4(3) . . ? C34 P3 W 123.53(18) . . ? C29 C28 C33 120.0 . . ? C29 C28 P3 121.1(3) . . ? C33 C28 P3 118.9(3) . . ? C28 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C28 120.0 . . ? C35 C34 C39 120.0 . . ? C35 C34 P3 119.7(3) . . ? C39 C34 P3 120.3(3) . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C34 120.0 . . ? C41 C40 P3 108.2(5) . . ? C40 C41 P4 108.5(5) . . ? C48 P4 C42 103.3(3) . . ? C48 P4 C41 103.8(3) . . ? C42 P4 C41 102.8(3) . . ? C48 P4 W 121.1(2) . . ? C42 P4 W 118.3(2) . . ? C41 P4 W 105.1(3) . . ? C43 C42 C47 120.0 . . ? C43 C42 P4 119.1(3) . . ? C47 C42 P4 120.6(3) . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C46 C47 C42 120.0 . . ? C49 C48 C53 120.0 . . ? C49 C48 P4 119.1(3) . . ? C53 C48 P4 120.8(3) . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C50 C51 C52 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C48 120.0 . . ? Cl2 C54 Cl3 110.2(7) . . ? Cl2 C54 Cl1 111.6(5) . . ? Cl3 C54 Cl1 111.0(4) . . ? Cl5 C55 Cl4 111.1(4) . . ? Cl5 C55 Cl6 111.8(4) . . ? Cl4 C55 Cl6 113.0(4) . . ? Cl9 C56 Cl7 110.2(4) . . ? Cl9 C56 Cl8 113.2(4) . . ? Cl7 C56 Cl8 111.3(5) . . ? Cl10 C57 Cl12 110.1(5) . . ? Cl10 C57 Cl11 109.0(4) . . ? Cl12 C57 Cl11 110.2(8) . . ? Cl13 C58 Cl15 108.7(11) . . ? Cl13 C58 Cl14 107.8(11) . . ? Cl15 C58 Cl14 109.1(11) . . ? Cl18 C58A Cl16 105.6(18) . . ? Cl18 C58A Cl17 107.7(14) . . ? Cl16 C58A Cl17 104.9(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 62.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.439 _refine_diff_density_min -1.591 _refine_diff_density_rms 0.129 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 641373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H114 Br2 F12 Mn N6 O4 P8 W2' _chemical_formula_weight 2882.49 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 12.3745(2) _cell_length_b 16.13710(10) _cell_length_c 18.3672(2) _cell_angle_alpha 66.3210(10) _cell_angle_beta 77.5070(10) _cell_angle_gamma 72.3760(10) _cell_volume 3182.37(7) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1439 _exptl_absorpt_coefficient_mu 2.700 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SORTAV ' _exptl_absorpt_correction_T_min 0.62755 _exptl_absorpt_correction_T_max 0.69199 _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 CCD' _diffrn_measurement_method '303 frames, counting time 20 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65258 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14468 _reflns_number_gt 12795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker-Nonius' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0487P)^2^+6.5477P] 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 14468 _refine_ls_number_parameters 747 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.003 _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 0.817379(11) 0.744176(9) 0.748364(8) 0.01263(5) Uani 1 1 d . . . Br2 Br 0.87660(3) 0.64582(3) 0.65653(2) 0.02060(8) Uani 1 1 d . . . P1 P 0.96396(8) 0.62459(6) 0.83830(5) 0.01556(18) Uani 1 1 d . . . C11 C 1.0310(4) 0.6634(3) 0.8947(2) 0.0220(8) Uani 1 1 d . . . C12 C 1.1474(4) 0.6561(3) 0.8836(3) 0.0282(9) Uani 1 1 d . . . H12 H 1.1938 0.6282 0.8485 0.034 Uiso 1 1 calc R . . C13 C 1.1963(5) 0.6900(3) 0.9243(3) 0.0416(12) Uani 1 1 d . . . H13 H 1.2744 0.6855 0.9158 0.050 Uiso 1 1 calc R . . C14 C 1.1286(6) 0.7298(3) 0.9768(3) 0.0481(15) Uani 1 1 d . . . H14 H 1.1610 0.7516 1.0047 0.058 Uiso 1 1 calc R . . C15 C 1.0134(6) 0.7379(3) 0.9887(3) 0.0474(15) Uani 1 1 d . . . H15 H 0.9682 0.7653 1.0245 0.057 Uiso 1 1 calc R . . C16 C 0.9626(4) 0.7052(3) 0.9478(2) 0.0317(10) Uani 1 1 d . . . H16 H 0.8842 0.7114 0.9559 0.038 Uiso 1 1 calc R . . C21 C 1.0851(3) 0.5458(3) 0.8038(2) 0.0192(7) Uani 1 1 d U . . C22 C 1.1368(4) 0.4594(3) 0.8567(3) 0.0314(9) Uani 1 1 d U . . H22 H 1.1076 0.4405 0.9104 0.038 Uiso 1 1 calc R . . C23 C 1.2309(4) 0.4013(3) 0.8309(3) 0.0382(11) Uani 1 1 d U . . H23 H 1.2653 0.3441 0.8670 0.046 Uiso 1 1 calc R . . C24 C 1.2735(4) 0.4290(3) 0.7506(3) 0.0358(10) Uani 1 1 d U . . H24 H 1.3351 0.3895 0.7324 0.043 Uiso 1 1 calc R . . C25 C 1.2244(4) 0.5147(3) 0.6982(3) 0.0318(9) Uani 1 1 d U . . H25 H 1.2535 0.5336 0.6445 0.038 Uiso 1 1 calc R . . C26 C 1.1313(3) 0.5736(3) 0.7248(2) 0.0244(8) Uani 1 1 d U . . H26 H 1.0999 0.6322 0.6890 0.029 Uiso 1 1 calc R . . C2 C 0.8885(3) 0.5426(3) 0.9194(2) 0.0223(8) Uani 1 1 d . . . H2A H 0.9430 0.4869 0.9475 0.027 Uiso 1 1 calc R . . H2B H 0.8442 0.5714 0.9573 0.027 Uiso 1 1 calc R . . C3 C 0.8095(3) 0.5171(3) 0.8822(2) 0.0223(8) Uani 1 1 d . . . H3A H 0.7704 0.4723 0.9232 0.027 Uiso 1 1 calc R . . H3B H 0.8533 0.4897 0.8432 0.027 Uiso 1 1 calc R . . P4 P 0.70599(8) 0.62492(6) 0.83365(5) 0.01582(18) Uani 1 1 d . . . C31 C 0.6203(3) 0.5858(3) 0.7901(2) 0.0207(8) Uani 1 1 d . . . C36 C 0.5052(4) 0.6286(3) 0.7841(2) 0.0253(8) Uani 1 1 d . . . H36 H 0.4695 0.6735 0.8069 0.030 Uiso 1 1 calc R . . C35 C 0.4432(4) 0.6044(3) 0.7439(3) 0.0336(10) Uani 1 1 d . . . H35 H 0.3661 0.6330 0.7403 0.040 Uiso 1 1 calc R . . C34 C 0.4954(5) 0.5383(4) 0.7096(3) 0.0399(12) Uani 1 1 d . . . H34 H 0.4540 0.5235 0.6818 0.048 Uiso 1 1 calc R . . C32 C 0.6716(4) 0.5173(3) 0.7568(2) 0.0271(9) Uani 1 1 d . . . H32 H 0.7482 0.4870 0.7615 0.033 Uiso 1 1 calc R . . C33 C 0.6089(5) 0.4941(3) 0.7166(3) 0.0377(11) Uani 1 1 d . . . H33 H 0.6437 0.4486 0.6944 0.045 Uiso 1 1 calc R . . C41 C 0.6083(3) 0.6479(3) 0.9174(2) 0.0188(7) Uani 1 1 d . . . C45 C 0.5168(5) 0.5983(3) 1.0524(3) 0.0447(13) Uani 1 1 d . . . H45 H 0.5095 0.5514 1.1021 0.054 Uiso 1 1 calc R . . C42 C 0.5409(4) 0.7370(3) 0.9056(2) 0.0246(8) Uani 1 1 d . . . H42 H 0.5493 0.7844 0.8564 0.029 Uiso 1 1 calc R . . C43 C 0.4609(4) 0.7570(3) 0.9660(3) 0.0306(9) Uani 1 1 d . . . H43 H 0.4154 0.8170 0.9568 0.037 Uiso 1 1 calc R . . C44 C 0.4492(4) 0.6872(3) 1.0397(3) 0.0328(10) Uani 1 1 d . . . H44 H 0.3961 0.7001 1.0805 0.039 Uiso 1 1 calc R . . C46 C 0.5956(4) 0.5780(3) 0.9917(3) 0.0361(11) Uani 1 1 d . . . H46 H 0.6400 0.5176 1.0008 0.043 Uiso 1 1 calc R . . P5 P 0.67220(8) 0.85847(6) 0.65685(5) 0.01410(17) Uani 1 1 d . . . C6 C 0.7272(3) 0.9637(2) 0.6028(2) 0.0181(7) Uani 1 1 d . . . H6A H 0.6799 1.0076 0.5609 0.022 Uiso 1 1 calc R . . H6B H 0.7272 0.9937 0.6391 0.022 Uiso 1 1 calc R . . C7 C 0.8489(3) 0.9324(3) 0.5666(2) 0.0181(7) Uani 1 1 d . . . H7A H 0.8807 0.9860 0.5353 0.022 Uiso 1 1 calc R . . H7B H 0.8491 0.9004 0.5317 0.022 Uiso 1 1 calc R . . P8 P 0.93459(8) 0.85320(6) 0.64986(5) 0.01448(18) Uani 1 1 d . . . C51 C 0.5321(3) 0.9030(2) 0.7033(2) 0.0163(7) Uani 1 1 d . . . C52 C 0.5236(3) 0.9593(3) 0.7466(2) 0.0187(7) Uani 1 1 d . . . H52 H 0.5878 0.9765 0.7488 0.022 Uiso 1 1 calc R . . C53 C 0.4196(3) 0.9898(3) 0.7864(2) 0.0222(8) Uani 1 1 d . . . H53 H 0.4146 1.0266 0.8156 0.027 Uiso 1 1 calc R . . C54 C 0.3234(4) 0.9652(3) 0.7826(2) 0.0270(9) Uani 1 1 d . . . H54 H 0.2535 0.9865 0.8085 0.032 Uiso 1 1 calc R . . C55 C 0.3315(4) 0.9091(3) 0.7404(3) 0.0285(9) Uani 1 1 d . . . H55 H 0.2673 0.8916 0.7388 0.034 Uiso 1 1 calc R . . C56 C 0.4351(3) 0.8788(3) 0.7002(2) 0.0227(8) Uani 1 1 d . . . H56 H 0.4396 0.8420 0.6710 0.027 Uiso 1 1 calc R . . C61 C 0.6375(3) 0.8353(3) 0.5758(2) 0.0171(7) Uani 1 1 d . . . C62 C 0.6264(3) 0.9021(3) 0.4991(2) 0.0242(8) Uani 1 1 d . . . H62 H 0.6395 0.9603 0.4870 0.029 Uiso 1 1 calc R . . C63 C 0.5956(4) 0.8819(3) 0.4403(2) 0.0284(9) Uani 1 1 d . . . H63 H 0.5892 0.9266 0.3890 0.034 Uiso 1 1 calc R . . C64 C 0.5748(4) 0.7968(3) 0.4573(2) 0.0263(9) Uani 1 1 d . . . H64 H 0.5541 0.7840 0.4179 0.032 Uiso 1 1 calc R . . C65 C 0.5848(3) 0.7300(3) 0.5337(2) 0.0236(8) Uani 1 1 d . . . H65 H 0.5697 0.6726 0.5458 0.028 Uiso 1 1 calc R . . C66 C 0.6173(3) 0.7487(3) 0.5918(2) 0.0198(7) Uani 1 1 d . . . H66 H 0.6258 0.7028 0.6424 0.024 Uiso 1 1 calc R . . C71 C 1.0720(3) 0.8167(2) 0.5958(2) 0.0173(7) Uani 1 1 d . . . C76 C 1.0772(3) 0.7764(3) 0.5402(2) 0.0202(7) Uani 1 1 d . . . H76 H 1.0107 0.7697 0.5297 0.024 Uiso 1 1 calc R . . C75 C 1.1817(4) 0.7463(3) 0.5005(2) 0.0256(8) Uani 1 1 d . . . H75 H 1.1848 0.7194 0.4636 0.031 Uiso 1 1 calc R . . C72 C 1.1725(3) 0.8260(3) 0.6109(2) 0.0254(8) Uani 1 1 d . . . H72 H 1.1703 0.8523 0.6480 0.030 Uiso 1 1 calc R . . C73 C 1.2763(4) 0.7958(3) 0.5704(3) 0.0317(10) Uani 1 1 d . . . H73 H 1.3431 0.8024 0.5805 0.038 Uiso 1 1 calc R . . C74 C 1.2810(4) 0.7561(3) 0.5156(3) 0.0286(9) Uani 1 1 d . . . H74 H 1.3507 0.7360 0.4888 0.034 Uiso 1 1 calc R . . C81 C 0.9623(2) 0.93338(14) 0.68798(13) 0.0172(7) Uani 1 1 d G . . C82 C 0.9971(2) 0.89660(12) 0.76410(13) 0.0202(7) Uani 1 1 d G . . H82 H 1.0040 0.8336 0.7945 0.024 Uiso 1 1 calc R . . C83 C 1.0217(2) 0.95400(16) 0.79480(11) 0.0238(8) Uani 1 1 d G . . H83 H 1.0450 0.9294 0.8457 0.029 Uiso 1 1 calc R . . C84 C 1.0114(3) 1.04818(15) 0.74939(15) 0.0268(9) Uani 1 1 d G . . H84 H 1.0278 1.0866 0.7699 0.032 Uiso 1 1 calc R . . C85 C 0.9765(3) 1.08496(12) 0.67327(15) 0.0348(10) Uani 1 1 d G . . H85 H 0.9696 1.1480 0.6429 0.042 Uiso 1 1 calc R . . C86 C 0.9520(3) 1.02756(15) 0.64257(11) 0.0292(9) Uani 1 1 d G . . H86 H 0.9287 1.0522 0.5916 0.035 Uiso 1 1 calc R . . N100 N 0.7785(3) 0.8125(2) 0.80950(17) 0.0158(6) Uani 1 1 d U . . N101 N 0.7669(3) 0.8679(3) 0.8468(2) 0.0271(7) Uani 1 1 d U . . C102 C 0.6812(3) 0.8824(3) 0.8979(2) 0.0234(8) Uani 1 1 d U . . N103 N 0.6108(3) 0.9037(3) 0.9448(2) 0.0382(10) Uani 1 1 d U . . Mn1 Mn 0.5000 1.0000 1.0000 0.0290(2) Uani 1 2 d S . . O91 O 0.4882(3) 0.8907(2) 1.11863(19) 0.0365(7) Uani 1 1 d . . . C92 C 0.3998(4) 0.8663(3) 1.1551(2) 0.0299(9) Uani 1 1 d D . . C93 C 0.2943(4) 0.8877(3) 1.1273(3) 0.0305(9) Uani 1 1 d . . . H93 H 0.2341 0.8671 1.1635 0.037 Uiso 1 1 calc R . . C94 C 0.2763(3) 0.9386(3) 1.0474(2) 0.0255(8) Uani 1 1 d D . . O95 O 0.3446(2) 0.9725(2) 0.98996(17) 0.0280(6) Uani 1 1 d . . . C921 C 0.4072(5) 0.8045(4) 1.2445(3) 0.0459(13) Uani 1 1 d D . . F922 F 0.4554(10) 0.7134(5) 1.2457(5) 0.073(3) Uani 0.50 1 d PD . . F923 F 0.4762(16) 0.8214(10) 1.2765(6) 0.114(7) Uani 0.50 1 d PD . . F924 F 0.3094(7) 0.7977(11) 1.2883(5) 0.109(5) Uani 0.50 1 d PD . . F925 F 0.3522(12) 0.8598(6) 1.2897(4) 0.079(3) Uani 0.50 1 d PD . . F926 F 0.5152(8) 0.7780(11) 1.2625(7) 0.106(6) Uani 0.50 1 d PD . . F927 F 0.3587(17) 0.7381(9) 1.2682(6) 0.125(6) Uani 0.50 1 d PD . . C941 C 0.1575(4) 0.9564(3) 1.0247(3) 0.0311(9) Uani 1 1 d D . . F942 F 0.0927(3) 0.9030(3) 1.08087(18) 0.0582(9) Uani 1 1 d D . . F943 F 0.1630(2) 0.9400(2) 0.95832(16) 0.0443(7) Uani 1 1 d D . . F944 F 0.1009(3) 1.0446(2) 1.0121(2) 0.0617(10) Uani 1 1 d D . . C111 C -0.5723(4) 0.5675(4) 1.4461(3) 0.0400(11) Uiso 1 1 d . . . H111 H -0.6205 0.6134 1.4093 0.048 Uiso 1 1 calc R . . C112 C -0.4627(4) 0.5752(4) 1.4431(3) 0.0409(11) Uiso 1 1 d . . . H112 H -0.4379 0.6263 1.4045 0.049 Uiso 1 1 calc R A 1 C113 C -0.3898(5) 0.5069(4) 1.4975(3) 0.0410(11) Uiso 0.50 1 d P . 1 H113 H -0.3161 0.5118 1.4955 0.049 Uiso 0.50 1 calc PR . 1 C114 C -0.3898(5) 0.5069(4) 1.4975(3) 0.0410(11) Uiso 0.50 1 d P . 2 C115 C -0.2661(11) 0.5180(9) 1.4933(8) 0.056(3) Uiso 0.50 1 d P B 2 H11A H -0.2610 0.5315 1.5386 0.068 Uiso 0.50 1 calc PR B 2 H11B H -0.2507 0.5680 1.4449 0.068 Uiso 0.50 1 calc PR B 2 H11C H -0.2114 0.4611 1.4938 0.068 Uiso 0.50 1 calc PR B 2 C121 C 0.1003(6) 1.2740(5) 0.7170(4) 0.0154(13) Uiso 0.50 1 d PD . . C122 C 0.0171(9) 1.3546(7) 0.6995(6) 0.041(2) Uiso 0.50 1 d PD . . H122 H -0.0168 1.3789 0.7394 0.050 Uiso 0.50 1 calc PR . . C123 C -0.0181(9) 1.4008(8) 0.6248(6) 0.045(2) Uiso 0.50 1 d P . . H123 H -0.0739 1.4566 0.6147 0.054 Uiso 0.50 1 calc PR . . C124 C 0.0277(7) 1.3663(6) 0.5640(5) 0.0254(17) Uiso 0.50 1 d P . . H124 H -0.0007 1.3952 0.5145 0.031 Uiso 0.50 1 calc PR . . C125 C 0.1157(5) 1.2887(4) 0.5789(4) 0.0080(11) Uiso 0.50 1 d P . . H125 H 0.1525 1.2665 0.5381 0.010 Uiso 0.50 1 calc PR . . C126 C 0.1502(5) 1.2429(4) 0.6552(3) 0.0083(12) Uiso 0.50 1 d PD . . H126 H 0.2092 1.1892 0.6648 0.010 Uiso 0.50 1 calc PR . . C127 C 0.1383(7) 1.2220(6) 0.8004(4) 0.0291(18) Uiso 0.50 1 d PD . . H12A H 0.2188 1.1944 0.7964 0.035 Uiso 0.50 1 calc PR . . H12B H 0.0980 1.1740 0.8297 0.035 Uiso 0.50 1 calc PR . . H12C H 0.1222 1.2648 0.8278 0.035 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 0.01525(8) 0.01212(8) 0.00936(7) -0.00318(5) -0.00062(5) -0.00315(5) Br2 0.02358(19) 0.02149(19) 0.01827(17) -0.01042(15) 0.00015(14) -0.00482(14) P1 0.0181(5) 0.0145(4) 0.0113(4) -0.0029(3) -0.0027(3) -0.0018(3) C11 0.036(2) 0.0144(18) 0.0129(16) -0.0005(14) -0.0101(15) -0.0036(15) C12 0.037(2) 0.023(2) 0.026(2) -0.0039(17) -0.0117(18) -0.0105(17) C13 0.056(3) 0.035(3) 0.040(3) -0.004(2) -0.023(2) -0.019(2) C14 0.088(5) 0.030(3) 0.037(3) -0.003(2) -0.035(3) -0.022(3) C15 0.104(5) 0.019(2) 0.020(2) -0.0062(18) -0.019(3) -0.006(2) C16 0.054(3) 0.021(2) 0.0161(18) -0.0050(16) -0.0075(18) -0.0025(19) C21 0.0204(18) 0.0180(17) 0.0197(17) -0.0069(14) -0.0039(14) -0.0038(14) C22 0.035(2) 0.024(2) 0.0228(19) -0.0032(17) -0.0013(17) 0.0010(17) C23 0.039(3) 0.024(2) 0.039(2) -0.0072(19) -0.003(2) 0.0030(18) C24 0.031(2) 0.030(2) 0.043(2) -0.019(2) 0.0031(19) 0.0001(18) C25 0.025(2) 0.039(2) 0.027(2) -0.0158(18) 0.0048(17) -0.0033(17) C26 0.023(2) 0.026(2) 0.0191(18) -0.0063(16) -0.0019(15) -0.0025(15) C2 0.023(2) 0.0197(19) 0.0169(17) 0.0005(15) -0.0039(15) -0.0033(15) C3 0.026(2) 0.0156(18) 0.0204(18) -0.0012(15) -0.0024(15) -0.0057(15) P4 0.0193(5) 0.0138(4) 0.0125(4) -0.0025(3) -0.0002(3) -0.0057(3) C31 0.027(2) 0.0209(19) 0.0139(16) -0.0025(15) 0.0023(15) -0.0129(15) C36 0.032(2) 0.026(2) 0.0189(18) -0.0048(16) -0.0010(16) -0.0131(17) C35 0.031(2) 0.047(3) 0.027(2) -0.007(2) -0.0034(18) -0.023(2) C34 0.050(3) 0.055(3) 0.031(2) -0.019(2) 0.001(2) -0.035(3) C32 0.037(2) 0.024(2) 0.023(2) -0.0105(17) 0.0007(17) -0.0114(17) C33 0.053(3) 0.040(3) 0.033(2) -0.021(2) 0.001(2) -0.024(2) C41 0.0209(19) 0.0220(19) 0.0148(16) -0.0068(15) 0.0023(14) -0.0096(15) C45 0.063(3) 0.034(3) 0.023(2) -0.004(2) 0.017(2) -0.015(2) C42 0.031(2) 0.0209(19) 0.0175(18) -0.0055(16) 0.0044(16) -0.0069(16) C43 0.034(2) 0.027(2) 0.030(2) -0.0146(19) 0.0063(18) -0.0073(18) C44 0.039(3) 0.038(2) 0.024(2) -0.0156(19) 0.0131(18) -0.017(2) C46 0.046(3) 0.026(2) 0.023(2) -0.0030(18) 0.0103(19) -0.0082(19) P5 0.0157(4) 0.0139(4) 0.0112(4) -0.0034(3) -0.0017(3) -0.0030(3) C6 0.0193(18) 0.0155(17) 0.0149(16) -0.0007(14) -0.0020(14) -0.0044(14) C7 0.0211(19) 0.0175(18) 0.0117(16) -0.0004(14) -0.0014(14) -0.0061(14) P8 0.0155(4) 0.0153(4) 0.0111(4) -0.0031(3) -0.0007(3) -0.0045(3) C51 0.0188(18) 0.0153(17) 0.0115(15) -0.0033(14) 0.0007(13) -0.0031(13) C52 0.0206(19) 0.0206(18) 0.0137(16) -0.0053(14) -0.0042(14) -0.0030(14) C53 0.027(2) 0.0223(19) 0.0164(17) -0.0095(15) -0.0049(15) 0.0008(15) C54 0.024(2) 0.034(2) 0.0216(19) -0.0138(18) 0.0014(16) -0.0022(17) C55 0.021(2) 0.037(2) 0.032(2) -0.0184(19) 0.0008(17) -0.0079(17) C56 0.0207(19) 0.026(2) 0.0243(19) -0.0119(17) 0.0000(15) -0.0074(15) C61 0.0167(18) 0.0210(18) 0.0135(16) -0.0074(14) -0.0012(13) -0.0031(14) C62 0.029(2) 0.024(2) 0.0192(18) -0.0076(16) -0.0066(16) -0.0022(16) C63 0.036(2) 0.029(2) 0.0169(18) -0.0068(17) -0.0105(17) 0.0003(17) C64 0.026(2) 0.036(2) 0.0208(19) -0.0150(18) -0.0063(16) -0.0044(17) C65 0.024(2) 0.030(2) 0.0218(19) -0.0120(17) -0.0009(15) -0.0108(16) C66 0.024(2) 0.0201(18) 0.0144(16) -0.0037(15) -0.0008(14) -0.0090(15) C71 0.0197(18) 0.0158(17) 0.0136(16) -0.0034(14) 0.0001(14) -0.0043(14) C76 0.0205(19) 0.0213(19) 0.0151(17) -0.0028(15) -0.0012(14) -0.0059(15) C75 0.029(2) 0.026(2) 0.0218(19) -0.0124(17) 0.0012(16) -0.0042(16) C72 0.021(2) 0.032(2) 0.027(2) -0.0155(18) -0.0006(16) -0.0057(16) C73 0.018(2) 0.043(3) 0.040(2) -0.024(2) -0.0004(18) -0.0061(18) C74 0.019(2) 0.033(2) 0.032(2) -0.0158(19) 0.0052(17) -0.0039(16) C81 0.0165(18) 0.0194(18) 0.0160(17) -0.0076(15) 0.0032(13) -0.0065(14) C82 0.0221(19) 0.0186(18) 0.0196(18) -0.0043(15) -0.0034(15) -0.0071(14) C83 0.024(2) 0.030(2) 0.0198(18) -0.0097(17) -0.0017(15) -0.0092(16) C84 0.030(2) 0.026(2) 0.032(2) -0.0173(18) -0.0017(17) -0.0105(17) C85 0.054(3) 0.017(2) 0.036(2) -0.0030(18) -0.014(2) -0.0141(19) C86 0.041(3) 0.024(2) 0.023(2) -0.0039(17) -0.0070(18) -0.0123(18) N100 0.0155(15) 0.0173(15) 0.0145(14) -0.0053(12) -0.0009(11) -0.0050(11) N101 0.0193(17) 0.035(2) 0.0319(19) -0.0226(16) 0.0064(14) -0.0050(14) C102 0.026(2) 0.025(2) 0.026(2) -0.0129(17) -0.0085(17) -0.0061(16) N103 0.034(2) 0.059(3) 0.041(2) -0.041(2) 0.0135(18) -0.0193(19) Mn1 0.0230(5) 0.0498(6) 0.0287(5) -0.0302(4) 0.0072(4) -0.0138(4) O91 0.0270(17) 0.055(2) 0.0322(16) -0.0238(16) -0.0051(13) -0.0037(14) C92 0.034(2) 0.030(2) 0.028(2) -0.0159(18) -0.0035(18) -0.0029(18) C93 0.030(2) 0.034(2) 0.029(2) -0.0141(19) 0.0012(18) -0.0086(18) C94 0.020(2) 0.033(2) 0.029(2) -0.0204(18) 0.0014(16) -0.0049(16) O95 0.0267(15) 0.0402(17) 0.0253(14) -0.0194(13) 0.0012(12) -0.0119(13) C921 0.050(3) 0.042(3) 0.042(3) -0.008(2) -0.018(2) -0.006(2) F922 0.106(7) 0.032(4) 0.056(5) 0.002(3) -0.012(5) -0.002(4) F923 0.23(2) 0.114(10) 0.038(5) 0.018(6) -0.065(10) -0.125(12) F924 0.050(5) 0.153(12) 0.027(4) 0.020(6) 0.005(3) 0.029(7) F925 0.118(9) 0.083(6) 0.025(3) -0.016(4) -0.001(5) -0.021(6) F926 0.068(6) 0.141(13) 0.057(6) -0.010(7) -0.036(5) 0.034(8) F927 0.26(2) 0.077(8) 0.068(8) 0.024(6) -0.071(11) -0.116(11) C941 0.028(2) 0.043(3) 0.030(2) -0.020(2) 0.0004(18) -0.0113(19) F942 0.0366(17) 0.105(3) 0.0387(16) -0.0195(18) 0.0038(13) -0.0396(18) F943 0.0360(15) 0.082(2) 0.0351(14) -0.0373(15) 0.0013(12) -0.0231(14) F944 0.0368(17) 0.058(2) 0.102(3) -0.047(2) -0.0293(18) 0.0125(14) _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(3) . ? W1 P5 2.5029(9) . ? W1 P4 2.5116(9) . ? W1 P8 2.5150(9) . ? W1 P1 2.5217(9) . ? W1 Br2 2.6100(4) . ? P1 C21 1.830(4) . ? P1 C11 1.832(4) . ? P1 C2 1.845(4) . ? C11 C12 1.386(6) . ? C11 C16 1.396(6) . ? C12 C13 1.396(6) . ? C13 C14 1.366(8) . ? C14 C15 1.368(9) . ? C15 C16 1.400(7) . ? C21 C26 1.381(5) . ? C21 C22 1.392(5) . ? C22 C23 1.386(6) . ? C23 C24 1.389(7) . ? C24 C25 1.373(7) . ? C25 C26 1.391(6) . ? C2 C3 1.533(5) . ? C3 P4 1.833(4) . ? P4 C31 1.827(4) . ? P4 C41 1.830(4) . ? C31 C36 1.389(6) . ? C31 C32 1.397(6) . ? C36 C35 1.394(6) . ? C35 C34 1.378(7) . ? C34 C33 1.377(8) . ? C32 C33 1.390(6) . ? C41 C42 1.383(5) . ? C41 C46 1.392(5) . ? C45 C44 1.378(7) . ? C45 C46 1.390(6) . ? C42 C43 1.391(6) . ? C43 C44 1.383(6) . ? P5 C51 1.830(4) . ? P5 C61 1.834(4) . ? P5 C6 1.841(4) . ? C6 C7 1.530(5) . ? C7 P8 1.846(4) . ? P8 C71 1.832(4) . ? P8 C81 1.8390(19) . ? C51 C56 1.389(5) . ? C51 C52 1.398(5) . ? C52 C53 1.389(5) . ? C53 C54 1.387(6) . ? C54 C55 1.381(6) . ? C55 C56 1.389(6) . ? C61 C62 1.393(5) . ? C61 C66 1.397(5) . ? C62 C63 1.399(5) . ? C63 C64 1.373(6) . ? C64 C65 1.388(6) . ? C65 C66 1.382(5) . ? C71 C72 1.392(5) . ? C71 C76 1.397(5) . ? C76 C75 1.392(6) . ? C75 C74 1.382(6) . ? C72 C73 1.393(6) . ? C73 C74 1.378(6) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? N100 N101 1.289(4) . ? N101 C102 1.286(5) . ? C102 N103 1.162(5) . ? N103 Mn1 2.168(4) . ? Mn1 O95 2.161(3) . ? Mn1 O95 2.161(3) 2_677 ? Mn1 N103 2.168(4) 2_677 ? Mn1 O91 2.193(3) . ? Mn1 O91 2.193(3) 2_677 ? O91 C92 1.238(6) . ? C92 C93 1.399(6) . ? C92 C921 1.547(6) . ? C93 C94 1.394(6) . ? C94 O95 1.247(5) . ? C94 C941 1.526(6) . ? C921 F927 1.265(9) . ? C921 F923 1.277(9) . ? C921 F924 1.309(9) . ? C921 F926 1.345(10) . ? C921 F925 1.390(9) . ? C921 F922 1.403(8) . ? C941 F943 1.331(5) . ? C941 F944 1.331(5) . ? C941 F942 1.341(5) . ? C111 C114 1.367(7) 2_468 ? C111 C113 1.367(7) 2_468 ? C111 C112 1.387(7) . ? C112 C114 1.389(7) . ? C112 C113 1.389(7) . ? C113 C111 1.367(7) 2_468 ? C114 C111 1.367(7) 2_468 ? C114 C115 1.575(13) . ? C121 C122 1.361(12) . ? C121 C126 1.374(9) . ? C121 C127 1.521(9) . ? C122 C123 1.366(14) . ? C123 C124 1.383(14) . ? C124 C125 1.364(10) . ? C125 C126 1.389(8) . ? 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 90.40(10) . . ? N100 W1 P4 97.10(10) . . ? P5 W1 P4 99.87(3) . . ? N100 W1 P8 90.38(10) . . ? P5 W1 P8 79.19(3) . . ? P4 W1 P8 172.47(3) . . ? N100 W1 P1 91.67(10) . . ? P5 W1 P1 177.84(3) . . ? P4 W1 P1 79.25(3) . . ? P8 W1 P1 101.43(3) . . ? N100 W1 Br2 178.97(10) . . ? P5 W1 Br2 89.34(2) . . ? P4 W1 Br2 83.92(2) . . ? P8 W1 Br2 88.59(2) . . ? P1 W1 Br2 88.60(2) . . ? C21 P1 C11 102.23(18) . . ? C21 P1 C2 102.23(18) . . ? C11 P1 C2 101.73(18) . . ? C21 P1 W1 122.60(12) . . ? C11 P1 W1 118.18(12) . . ? C2 P1 W1 106.96(12) . . ? C12 C11 C16 118.7(4) . . ? C12 C11 P1 121.9(3) . . ? C16 C11 P1 119.3(3) . . ? C11 C12 C13 121.1(5) . . ? C14 C13 C12 119.6(5) . . ? C13 C14 C15 120.5(4) . . ? C14 C15 C16 120.8(5) . . ? C11 C16 C15 119.3(5) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 P1 120.1(3) . . ? C22 C21 P1 121.2(3) . . ? C23 C22 C21 121.1(4) . . ? C24 C23 C22 119.5(4) . . ? C25 C24 C23 119.8(4) . . ? C24 C25 C26 120.4(4) . . ? C21 C26 C25 120.6(4) . . ? C3 C2 P1 108.3(3) . . ? C2 C3 P4 107.3(3) . . ? C31 P4 C41 102.49(17) . . ? C31 P4 C3 102.96(18) . . ? C41 P4 C3 103.62(18) . . ? C31 P4 W1 121.62(12) . . ? C41 P4 W1 117.03(12) . . ? C3 P4 W1 106.97(13) . . ? C36 C31 C32 118.9(4) . . ? C36 C31 P4 120.6(3) . . ? C32 C31 P4 120.3(3) . . ? C31 C36 C35 120.1(4) . . ? C34 C35 C36 120.5(4) . . ? C35 C34 C33 119.9(4) . . ? C33 C32 C31 120.4(4) . . ? C34 C33 C32 120.2(4) . . ? C42 C41 C46 118.7(4) . . ? C42 C41 P4 118.9(3) . . ? C46 C41 P4 122.4(3) . . ? C44 C45 C46 120.8(4) . . ? C41 C42 C43 121.1(4) . . ? C44 C43 C42 119.8(4) . . ? C45 C44 C43 119.5(4) . . ? C45 C46 C41 120.1(4) . . ? C51 P5 C61 103.30(16) . . ? C51 P5 C6 103.00(16) . . ? C61 P5 C6 102.67(17) . . ? C51 P5 W1 117.17(11) . . ? C61 P5 W1 121.99(12) . . ? C6 P5 W1 106.28(12) . . ? C7 C6 P5 107.0(2) . . ? C6 C7 P8 107.7(2) . . ? C71 P8 C81 103.14(15) . . ? C71 P8 C7 101.46(16) . . ? C81 P8 C7 103.16(14) . . ? C71 P8 W1 124.71(12) . . ? C81 P8 W1 114.22(9) . . ? C7 P8 W1 107.57(12) . . ? C56 C51 C52 119.0(3) . . ? C56 C51 P5 121.9(3) . . ? C52 C51 P5 118.9(3) . . ? C53 C52 C51 120.3(4) . . ? C54 C53 C52 120.1(4) . . ? C55 C54 C53 119.9(4) . . ? C54 C55 C56 120.3(4) . . ? C55 C56 C51 120.4(4) . . ? C62 C61 C66 118.4(3) . . ? C62 C61 P5 122.4(3) . . ? C66 C61 P5 119.1(3) . . ? C61 C62 C63 120.0(4) . . ? C64 C63 C62 120.8(4) . . ? C63 C64 C65 119.5(4) . . ? C66 C65 C64 120.2(4) . . ? C65 C66 C61 121.0(3) . . ? C72 C71 C76 119.1(3) . . ? C72 C71 P8 121.1(3) . . ? C76 C71 P8 119.8(3) . . ? C75 C76 C71 120.0(4) . . ? C74 C75 C76 120.5(4) . . ? C71 C72 C73 120.1(4) . . ? C74 C73 C72 120.6(4) . . ? C73 C74 C75 119.7(4) . . ? C82 C81 C86 120.0 . . ? C82 C81 P8 117.86(13) . . ? C86 C81 P8 122.12(13) . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? N101 N100 W1 169.3(3) . . ? C102 N101 N100 123.9(4) . . ? N103 C102 N101 171.0(4) . . ? C102 N103 Mn1 154.8(4) . . ? O95 Mn1 O95 179.999(1) . 2_677 ? O95 Mn1 N103 94.61(13) . . ? O95 Mn1 N103 85.39(13) 2_677 . ? O95 Mn1 N103 85.39(13) . 2_677 ? O95 Mn1 N103 94.61(13) 2_677 2_677 ? N103 Mn1 N103 179.999(2) . 2_677 ? O95 Mn1 O91 83.34(12) . . ? O95 Mn1 O91 96.66(11) 2_677 . ? N103 Mn1 O91 93.54(14) . . ? N103 Mn1 O91 86.46(15) 2_677 . ? O95 Mn1 O91 96.66(11) . 2_677 ? O95 Mn1 O91 83.34(12) 2_677 2_677 ? N103 Mn1 O91 86.46(15) . 2_677 ? N103 Mn1 O91 93.54(14) 2_677 2_677 ? O91 Mn1 O91 180.000(2) . 2_677 ? C92 O91 Mn1 125.0(3) . . ? O91 C92 C93 129.3(4) . . ? O91 C92 C921 114.9(4) . . ? C93 C92 C921 115.7(4) . . ? C94 C93 C92 122.3(4) . . ? O95 C94 C93 129.0(4) . . ? O95 C94 C941 113.8(4) . . ? C93 C94 C941 117.2(4) . . ? C94 O95 Mn1 125.2(3) . . ? F923 C921 F924 113.3(9) . . ? F927 C921 F926 113.9(9) . . ? F927 C921 F925 106.5(9) . . ? F926 C921 F925 102.3(7) . . ? F923 C921 F922 105.3(9) . . ? F924 C921 F922 102.6(8) . . ? F927 C921 C92 114.0(6) . . ? F923 C921 C92 113.3(6) . . ? F924 C921 C92 115.6(5) . . ? F926 C921 C92 110.9(7) . . ? F925 C921 C92 108.2(5) . . ? F922 C921 C92 105.2(5) . . ? F943 C941 F944 108.0(4) . . ? F943 C941 F942 106.2(4) . . ? F944 C941 F942 106.7(4) . . ? F943 C941 C94 111.4(3) . . ? F944 C941 C94 110.5(4) . . ? F942 C941 C94 113.7(4) . . ? C114 C111 C112 120.6(5) 2_468 . ? C113 C111 C112 120.6(5) 2_468 . ? C111 C112 C114 120.2(5) . . ? C111 C112 C113 120.2(5) . . ? C111 C113 C112 119.2(5) 2_468 . ? C111 C114 C112 119.2(5) 2_468 . ? C111 C114 C115 121.7(6) 2_468 . ? C112 C114 C115 119.1(6) . . ? C122 C121 C126 116.7(7) . . ? C122 C121 C127 121.7(7) . . ? C126 C121 C127 121.5(6) . . ? C121 C122 C123 121.8(10) . . ? C122 C123 C124 121.2(10) . . ? C125 C124 C123 117.9(8) . . ? C124 C125 C126 119.7(6) . . ? C121 C126 C125 122.4(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.655 _refine_diff_density_min -1.881 _refine_diff_density_rms 0.130 _publ_section_references ; Hooft, R., Bruker-Nonius Ltd, (1998) COLLECT Program. Otwinowski, Z., and Minor.W., (1997) DENZO program. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands Blessing, R.H., SORTAV program, J.Appl.Cryst. 1997 30 421-426. ; #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 641374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H114 Br2 F12 N6 Ni O4 P8 W2' _chemical_formula_weight 2886.36 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 12.550(14) _cell_length_b 16.589(18) _cell_length_c 18.41(2) _cell_angle_alpha 66.441(10) _cell_angle_beta 77.086(10) _cell_angle_gamma 72.451(10) _cell_volume 3327(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _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 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 2.630 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.659 _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 19961 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.1738 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.84 _reflns_number_total 11318 _reflns_number_gt 7519 _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. The CF3 groups were disordered and two sets of fluorines were refined with distance constraints. ; _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^)+(0.0413P)^2^+42.5124P] 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 11318 _refine_ls_number_parameters 697 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.1892 _refine_ls_wR_factor_gt 0.1675 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.076 _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 0.81299(4) 0.74732(4) 0.75078(3) 0.01877(15) Uani 1 1 d . . . Br2 Br 0.87594(13) 0.65394(12) 0.65607(9) 0.0436(4) Uani 1 1 d . . . P1 P 0.9591(3) 0.6294(3) 0.8385(2) 0.0323(9) Uani 1 1 d . . . C11 C 1.0289(13) 0.6653(11) 0.8948(8) 0.043(4) Uani 1 1 d . . . C12 C 1.1457(15) 0.6562(13) 0.8824(11) 0.064(5) Uani 1 1 d . . . H12 H 1.1899 0.6281 0.8474 0.077 Uiso 1 1 calc R . . C13 C 1.196(2) 0.6884(16) 0.9215(16) 0.088(7) Uani 1 1 d . . . H13 H 1.2732 0.6846 0.9105 0.106 Uiso 1 1 calc R . . C14 C 1.135(3) 0.7248(18) 0.9746(15) 0.102(9) Uani 1 1 d . . . H14 H 1.1707 0.7451 1.0011 0.123 Uiso 1 1 calc R . . C15 C 1.021(2) 0.7330(14) 0.9914(11) 0.076(6) Uani 1 1 d . . . H15 H 0.9798 0.7570 1.0299 0.091 Uiso 1 1 calc R . . C16 C 0.9647(17) 0.7047(12) 0.9496(9) 0.062(5) Uani 1 1 d . . . H16 H 0.8870 0.7125 0.9587 0.075 Uiso 1 1 calc R . . C21 C 1.0748(13) 0.5539(11) 0.8026(9) 0.044(3) Uani 1 1 d U . . C22 C 1.1210(15) 0.4674(12) 0.8501(11) 0.067(4) Uani 1 1 d U . . H22 H 1.0891 0.4451 0.9027 0.080 Uiso 1 1 calc R . . C23 C 1.2139(16) 0.4121(13) 0.8223(12) 0.084(5) Uani 1 1 d U . . H23 H 1.2445 0.3544 0.8565 0.101 Uiso 1 1 calc R . . C24 C 1.2600(16) 0.4421(13) 0.7452(12) 0.075(5) Uani 1 1 d U . . H24 H 1.3191 0.4037 0.7256 0.090 Uiso 1 1 calc R . . C25 C 1.2203(14) 0.5277(12) 0.6969(11) 0.060(4) Uani 1 1 d U . . H25 H 1.2537 0.5493 0.6446 0.072 Uiso 1 1 calc R . . C26 C 1.1286(12) 0.5840(11) 0.7258(9) 0.047(3) Uani 1 1 d U . . H26 H 1.1031 0.6434 0.6925 0.056 Uiso 1 1 calc R . . C2 C 0.8824(12) 0.5511(10) 0.9203(8) 0.042(4) Uani 1 1 d . . . H2A H 0.9354 0.4973 0.9491 0.051 Uiso 1 1 calc R . . H2B H 0.8384 0.5803 0.9574 0.051 Uiso 1 1 calc R . . C3 C 0.8044(12) 0.5250(9) 0.8839(8) 0.037(4) Uani 1 1 d . . . H3A H 0.7648 0.4824 0.9255 0.045 Uiso 1 1 calc R . . H3B H 0.8481 0.4968 0.8460 0.045 Uiso 1 1 calc R . . P4 P 0.7036(3) 0.6288(3) 0.8334(2) 0.0301(9) Uani 1 1 d . . . C31 C 0.6220(12) 0.5898(11) 0.7903(8) 0.037(4) Uani 1 1 d . . . C36 C 0.5080(13) 0.6263(12) 0.7852(9) 0.051(4) Uani 1 1 d . . . H36 H 0.4709 0.6690 0.8089 0.061 Uiso 1 1 calc R . . C35 C 0.4464(15) 0.6021(14) 0.7465(10) 0.062(5) Uani 1 1 d . . . H35 H 0.3704 0.6294 0.7425 0.075 Uiso 1 1 calc R . . C34 C 0.501(2) 0.5364(16) 0.7144(12) 0.081(7) Uani 1 1 d . . . H34 H 0.4615 0.5180 0.6894 0.097 Uiso 1 1 calc R . . C32 C 0.6737(14) 0.5253(12) 0.7568(9) 0.048(4) Uani 1 1 d . . . H32 H 0.7502 0.4988 0.7593 0.058 Uiso 1 1 calc R . . C33 C 0.612(2) 0.4985(16) 0.7186(12) 0.083(7) Uani 1 1 d . . . H33 H 0.6476 0.4545 0.6962 0.100 Uiso 1 1 calc R . . C41 C 0.6040(12) 0.6511(9) 0.9182(7) 0.031(3) Uani 1 1 d . . . C45 C 0.508(2) 0.6027(18) 1.0489(12) 0.107(9) Uani 1 1 d . . . H45 H 0.5002 0.5561 1.0976 0.128 Uiso 1 1 calc R . . C42 C 0.5400(13) 0.7383(12) 0.9086(9) 0.049(4) Uani 1 1 d . . . H42 H 0.5505 0.7854 0.8607 0.059 Uiso 1 1 calc R . . C43 C 0.4605(14) 0.7561(13) 0.9697(10) 0.066(6) Uani 1 1 d . . . H43 H 0.4185 0.8149 0.9626 0.079 Uiso 1 1 calc R . . C44 C 0.4436(19) 0.6855(17) 1.0416(11) 0.079(7) Uani 1 1 d . . . H44 H 0.3896 0.6956 1.0828 0.095 Uiso 1 1 calc R . . C46 C 0.5861(18) 0.5819(13) 0.9891(11) 0.081(7) Uani 1 1 d . . . H46 H 0.6256 0.5225 0.9965 0.097 Uiso 1 1 calc R . . P5 P 0.6705(3) 0.8583(3) 0.6585(2) 0.0304(9) Uani 1 1 d . . . C6 C 0.7228(11) 0.9624(10) 0.6080(8) 0.036(4) Uani 1 1 d . . . H6A H 0.6765 1.0057 0.5667 0.043 Uiso 1 1 calc R . . H6B H 0.7212 0.9899 0.6460 0.043 Uiso 1 1 calc R . . C7 C 0.8454(11) 0.9333(10) 0.5710(7) 0.038(4) Uani 1 1 d . . . H7A H 0.8761 0.9860 0.5411 0.046 Uiso 1 1 calc R . . H7B H 0.8467 0.9034 0.5349 0.046 Uiso 1 1 calc R . . P8 P 0.9300(3) 0.8551(3) 0.6530(2) 0.0289(9) Uani 1 1 d . . . C51 C 0.5314(12) 0.9014(10) 0.7044(8) 0.035(3) Uani 1 1 d . . . C52 C 0.5194(12) 0.9566(10) 0.7483(8) 0.038(4) Uani 1 1 d . . . H52 H 0.5826 0.9726 0.7516 0.046 Uiso 1 1 calc R . . C53 C 0.4168(12) 0.9882(12) 0.7871(8) 0.046(4) Uani 1 1 d . . . H53 H 0.4114 1.0243 0.8161 0.055 Uiso 1 1 calc R . . C54 C 0.3229(13) 0.9648(14) 0.7816(10) 0.061(5) Uani 1 1 d . . . H54 H 0.2533 0.9865 0.8065 0.073 Uiso 1 1 calc R . . C55 C 0.3305(13) 0.9106(14) 0.7403(11) 0.070(6) Uani 1 1 d . . . H55 H 0.2668 0.8943 0.7384 0.083 Uiso 1 1 calc R . . C56 C 0.4343(13) 0.8794(12) 0.7008(9) 0.052(5) Uani 1 1 d . . . H56 H 0.4385 0.8436 0.6717 0.062 Uiso 1 1 calc R . . C61 C 0.6366(10) 0.8355(11) 0.5769(8) 0.034(4) Uani 1 1 d . . . C62 C 0.6243(14) 0.9006(12) 0.5013(9) 0.053(5) Uani 1 1 d . . . H62 H 0.6358 0.9576 0.4896 0.064 Uiso 1 1 calc R . . C63 C 0.5950(16) 0.8806(14) 0.4435(10) 0.068(6) Uani 1 1 d . . . H63 H 0.5904 0.9240 0.3924 0.081 Uiso 1 1 calc R . . C64 C 0.5728(15) 0.8005(15) 0.4584(10) 0.064(5) Uani 1 1 d . . . H64 H 0.5492 0.7902 0.4191 0.077 Uiso 1 1 calc R . . C65 C 0.5857(14) 0.7331(12) 0.5337(10) 0.053(5) Uani 1 1 d . . . H65 H 0.5724 0.6768 0.5453 0.064 Uiso 1 1 calc R . . C66 C 0.6201(13) 0.7530(12) 0.5928(8) 0.046(4) Uani 1 1 d . . . H66 H 0.6312 0.7084 0.6428 0.056 Uiso 1 1 calc R . . C71 C 1.0662(11) 0.8205(10) 0.5990(8) 0.037(4) Uani 1 1 d . . . C76 C 1.0744(13) 0.7849(11) 0.5412(8) 0.048(4) Uani 1 1 d . . . H76 H 1.0094 0.7783 0.5302 0.058 Uiso 1 1 calc R . . C75 C 1.1763(14) 0.7588(13) 0.4994(9) 0.058(5) Uani 1 1 d . . . H75 H 1.1786 0.7376 0.4592 0.070 Uiso 1 1 calc R . . C72 C 1.1669(12) 0.8272(13) 0.6161(10) 0.056(5) Uani 1 1 d . . . H72 H 1.1651 0.8494 0.6555 0.068 Uiso 1 1 calc R . . C73 C 1.2689(13) 0.8000(14) 0.5734(12) 0.071(6) Uani 1 1 d . . . H73 H 1.3346 0.8066 0.5834 0.085 Uiso 1 1 calc R . . C74 C 1.2748(15) 0.7641(14) 0.5172(12) 0.071(6) Uani 1 1 d . . . H74 H 1.3440 0.7435 0.4912 0.085 Uiso 1 1 calc R . . C81 C 0.9582(9) 0.9322(6) 0.6920(6) 0.036(4) Uani 1 1 d G . . C82 C 0.9885(8) 0.8957(6) 0.7689(5) 0.044(4) Uani 1 1 d G . . H82 H 0.9918 0.8349 0.7992 0.053 Uiso 1 1 calc R . . C83 C 1.0140(9) 0.9500(8) 0.8006(5) 0.054(5) Uani 1 1 d G . . H83 H 1.0343 0.9255 0.8521 0.065 Uiso 1 1 calc R . . C84 C 1.0091(11) 1.0408(8) 0.7554(7) 0.070(6) Uani 1 1 d G . . H84 H 1.0262 1.0772 0.7767 0.084 Uiso 1 1 calc R . . C85 C 0.9788(11) 1.0774(6) 0.6786(7) 0.081(6) Uani 1 1 d G . . H85 H 0.9755 1.1381 0.6483 0.097 Uiso 1 1 calc R . . C86 C 0.9533(11) 1.0230(7) 0.6468(5) 0.077(7) Uani 1 1 d G . . H86 H 0.9330 1.0475 0.5954 0.093 Uiso 1 1 calc R . . N100 N 0.7714(8) 0.8108(8) 0.8162(6) 0.030(3) Uani 1 1 d U . . N101 N 0.7611(12) 0.8580(11) 0.8612(10) 0.067(4) Uani 1 1 d U . . C102 C 0.6685(13) 0.8825(11) 0.9019(9) 0.043(4) Uani 1 1 d U . . N103 N 0.6001(12) 0.9132(10) 0.9432(8) 0.054(4) Uani 1 1 d U . . Ni1 Ni 0.5000 1.0000 1.0000 0.0395(7) Uani 1 2 d S . . O91 O 0.4935(9) 0.8968(8) 1.1094(6) 0.056(3) Uani 1 1 d . . . C92 C 0.4085(14) 0.8679(10) 1.1488(7) 0.061(5) Uani 1 1 d D . . C93 C 0.3045(15) 0.8933(13) 1.1163(10) 0.061(5) Uani 1 1 d . . . H93 H 0.2453 0.8710 1.1512 0.073 Uiso 1 1 calc R . . C94 C 0.2815(9) 0.9479(11) 1.0380(8) 0.051(5) Uani 1 1 d D . . O95 O 0.3518(9) 0.9845(8) 0.9834(6) 0.053(3) Uani 1 1 d . . . C921 C 0.4217(14) 0.7980(13) 1.2409(12) 0.114(9) Uani 1 1 d D . . F922 F 0.489(2) 0.7203(12) 1.2281(14) 0.118(4) Uiso 0.489(11) 1 d PD . . F923 F 0.472(2) 0.8373(17) 1.2710(13) 0.118(4) Uiso 0.489(11) 1 d PD . . F924 F 0.3158(15) 0.7897(19) 1.2741(12) 0.118(4) Uiso 0.489(11) 1 d PD . . F925 F 0.360(2) 0.8555(15) 1.2828(12) 0.118(4) Uiso 0.511(11) 1 d PD . . F926 F 0.5326(14) 0.7738(18) 1.2469(13) 0.118(4) Uiso 0.511(11) 1 d PD . . F927 F 0.371(2) 0.7329(14) 1.2506(13) 0.118(4) Uiso 0.511(11) 1 d PD . . C941 C 0.1623(14) 0.9655(10) 1.0128(8) 0.072(6) Uiso 1 1 d D . . F942 F 0.1133(14) 0.8980(12) 1.0747(9) 0.079(3) Uiso 0.563(12) 1 d PD . . F943 F 0.1754(14) 0.9554(14) 0.9432(8) 0.079(3) Uiso 0.563(12) 1 d PD . . F944 F 0.1048(13) 1.0491(10) 1.0150(12) 0.079(3) Uiso 0.563(12) 1 d PD . . F945 F 0.1412(18) 1.0535(11) 0.9571(13) 0.079(3) Uiso 0.437(12) 1 d PD . . F946 F 0.1822(17) 0.9045(15) 0.9725(13) 0.079(3) Uiso 0.437(12) 1 d PD . . F947 F 0.0844(14) 0.9514(18) 1.0749(11) 0.079(3) Uiso 0.437(12) 1 d PD . . C111 C -0.572(2) 0.5660(18) 1.4504(14) 0.098(7) Uiso 1 1 d . . . H111 H -0.6203 0.6121 1.4157 0.118 Uiso 1 1 calc R . . C112 C -0.464(2) 0.5744(19) 1.4461(16) 0.114(9) Uiso 1 1 d . . . H112 H -0.4411 0.6253 1.4090 0.136 Uiso 1 1 calc R A 1 C113 C -0.391(2) 0.506(2) 1.4977(16) 0.114(9) Uiso 0.50 1 d P . 1 H113 H -0.3184 0.5105 1.4960 0.137 Uiso 0.50 1 calc PR . 1 C114 C -0.391(2) 0.506(2) 1.4977(16) 0.114(9) Uiso 0.50 1 d P . 2 C115 C -0.271(5) 0.516(5) 1.499(4) 0.18(3) Uiso 0.50 1 d P B 2 H11A H -0.2676 0.5192 1.5499 0.213 Uiso 0.50 1 calc PR B 2 H11B H -0.2573 0.5707 1.4572 0.213 Uiso 0.50 1 calc PR B 2 H11C H -0.2149 0.4651 1.4923 0.213 Uiso 0.50 1 calc PR B 2 C121 C 0.101(4) 1.272(3) 0.713(2) 0.096(15) Uiso 0.50 1 d PD . . C122 C -0.001(4) 1.333(3) 0.706(3) 0.121(19) Uiso 0.50 1 d PD . . H122 H -0.0481 1.3433 0.7497 0.145 Uiso 0.50 1 calc PR . . C123 C -0.026(6) 1.376(5) 0.634(4) 0.17(3) Uiso 0.50 1 d P . . H123 H -0.0851 1.4280 0.6245 0.203 Uiso 0.50 1 calc PR . . C124 C 0.026(4) 1.352(4) 0.572(3) 0.110(17) Uiso 0.50 1 d P . . H124 H -0.0022 1.3763 0.5229 0.132 Uiso 0.50 1 calc PR . . C125 C 0.110(4) 1.297(3) 0.584(2) 0.075(12) Uiso 0.50 1 d P . . H125 H 0.1581 1.2847 0.5418 0.090 Uiso 0.50 1 calc PR . . C126 C 0.135(4) 1.258(3) 0.649(2) 0.082(13) Uiso 0.50 1 d PD . . H126 H 0.1922 1.2051 0.6540 0.098 Uiso 0.50 1 calc PR . . C127 C 0.141(5) 1.217(4) 0.796(2) 0.19(3) Uiso 0.50 1 d PD . . H12A H 0.1931 1.1615 0.7957 0.224 Uiso 0.50 1 calc PR . . H12B H 0.0775 1.2044 0.8352 0.224 Uiso 0.50 1 calc PR . . H12C H 0.1776 1.2519 0.8096 0.224 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 0.0243(3) 0.0167(3) 0.0125(2) -0.00232(19) -0.00153(16) -0.00539(19) Br2 0.0470(9) 0.0511(11) 0.0388(9) -0.0254(8) -0.0013(6) -0.0101(8) P1 0.039(2) 0.028(2) 0.0244(19) -0.0045(17) -0.0077(15) -0.0038(17) C11 0.053(10) 0.045(11) 0.026(8) -0.006(7) -0.008(7) -0.012(8) C12 0.067(13) 0.060(14) 0.085(14) -0.031(11) -0.013(10) -0.034(10) C13 0.093(18) 0.073(18) 0.11(2) -0.020(15) -0.037(15) -0.036(14) C14 0.15(3) 0.09(2) 0.085(18) -0.004(15) -0.070(18) -0.049(19) C15 0.14(2) 0.061(15) 0.046(11) -0.027(10) -0.024(12) -0.028(14) C16 0.101(15) 0.052(13) 0.033(9) -0.013(9) -0.026(9) -0.007(11) C21 0.050(7) 0.032(7) 0.051(7) -0.018(6) -0.011(5) -0.003(5) C22 0.067(8) 0.035(7) 0.070(8) -0.013(6) 0.000(6) 0.015(6) C23 0.080(8) 0.041(8) 0.087(8) -0.007(7) 0.006(7) 0.015(7) C24 0.069(8) 0.048(8) 0.079(8) -0.019(7) 0.011(7) 0.006(7) C25 0.055(7) 0.052(8) 0.062(7) -0.021(6) 0.004(6) -0.006(6) C26 0.042(7) 0.041(7) 0.055(7) -0.019(6) -0.007(5) -0.003(5) C2 0.051(9) 0.035(10) 0.028(8) 0.001(7) -0.004(6) -0.012(7) C3 0.049(9) 0.022(9) 0.041(8) -0.010(7) 0.001(6) -0.013(7) P4 0.042(2) 0.026(2) 0.0222(18) -0.0078(17) -0.0001(15) -0.0120(17) C31 0.045(9) 0.039(10) 0.035(8) -0.018(7) 0.000(6) -0.018(7) C36 0.046(10) 0.050(12) 0.058(11) -0.027(9) 0.006(7) -0.012(8) C35 0.053(11) 0.080(16) 0.059(11) -0.014(11) -0.016(9) -0.031(10) C34 0.102(18) 0.10(2) 0.073(14) -0.055(14) 0.008(12) -0.049(15) C32 0.052(10) 0.058(12) 0.050(10) -0.028(9) 0.001(7) -0.028(9) C33 0.094(18) 0.094(19) 0.092(16) -0.062(15) 0.015(13) -0.045(15) C41 0.049(9) 0.021(8) 0.022(7) -0.006(6) 0.002(6) -0.017(7) C45 0.13(2) 0.09(2) 0.060(14) -0.010(14) 0.057(13) -0.043(17) C42 0.060(11) 0.044(11) 0.041(9) -0.019(8) 0.019(7) -0.021(8) C43 0.058(12) 0.056(13) 0.069(12) -0.018(10) 0.028(9) -0.023(9) C44 0.104(17) 0.099(19) 0.053(12) -0.041(13) 0.040(11) -0.066(15) C46 0.122(18) 0.037(12) 0.060(12) -0.017(10) 0.032(11) -0.017(11) P5 0.030(2) 0.032(3) 0.0257(19) -0.0072(17) -0.0058(14) -0.0043(16) C6 0.048(9) 0.028(9) 0.031(8) -0.009(7) -0.017(6) 0.000(7) C7 0.041(9) 0.030(9) 0.023(7) 0.013(6) -0.001(6) -0.015(7) P8 0.0299(19) 0.031(2) 0.0217(18) -0.0047(16) 0.0005(13) -0.0102(16) C51 0.042(9) 0.033(9) 0.033(8) -0.013(7) -0.009(6) -0.007(7) C52 0.040(9) 0.036(10) 0.043(9) -0.020(7) -0.013(6) 0.000(7) C53 0.044(9) 0.066(13) 0.031(8) -0.026(8) 0.010(6) -0.016(8) C54 0.034(10) 0.093(16) 0.062(11) -0.050(12) 0.002(7) 0.000(9) C55 0.024(10) 0.100(18) 0.089(14) -0.049(13) 0.006(8) -0.010(9) C56 0.048(10) 0.071(14) 0.050(10) -0.027(9) 0.001(7) -0.030(9) C61 0.024(7) 0.053(11) 0.026(7) -0.025(7) 0.004(5) -0.001(6) C62 0.072(12) 0.043(11) 0.042(9) -0.007(8) -0.032(8) -0.002(9) C63 0.091(14) 0.065(15) 0.037(10) -0.014(10) -0.029(9) 0.004(12) C64 0.081(13) 0.084(17) 0.038(10) -0.034(11) -0.019(9) -0.008(12) C65 0.070(12) 0.048(12) 0.059(11) -0.029(9) -0.016(9) -0.020(9) C66 0.065(11) 0.058(12) 0.025(8) -0.012(8) -0.026(7) -0.016(9) C71 0.036(8) 0.034(10) 0.026(7) 0.001(7) -0.004(6) -0.005(7) C76 0.053(10) 0.054(12) 0.027(8) 0.001(8) 0.001(7) -0.024(8) C75 0.053(11) 0.070(14) 0.043(10) -0.016(9) 0.005(8) -0.013(9) C72 0.032(9) 0.083(15) 0.067(12) -0.039(11) 0.002(7) -0.022(9) C73 0.019(9) 0.105(18) 0.099(15) -0.059(14) 0.013(8) -0.013(9) C74 0.042(12) 0.087(17) 0.087(15) -0.052(13) 0.026(9) -0.015(10) C81 0.037(8) 0.033(9) 0.032(8) -0.004(7) -0.007(6) -0.007(7) C82 0.055(10) 0.028(10) 0.051(10) -0.012(8) -0.017(7) -0.008(7) C83 0.063(11) 0.065(14) 0.035(9) -0.009(9) -0.003(7) -0.030(10) C84 0.084(14) 0.079(17) 0.072(14) -0.042(12) -0.008(11) -0.032(12) C85 0.135(19) 0.037(13) 0.074(14) -0.009(11) -0.029(13) -0.027(12) C86 0.15(2) 0.033(12) 0.061(12) 0.002(9) -0.041(12) -0.045(12) N100 0.023(6) 0.036(8) 0.033(6) -0.019(6) -0.005(4) 0.002(5) N101 0.059(9) 0.090(12) 0.097(11) -0.082(10) -0.004(8) -0.016(8) C102 0.049(9) 0.049(10) 0.041(8) -0.030(8) -0.006(7) -0.004(7) N103 0.064(9) 0.056(10) 0.052(8) -0.036(8) 0.000(7) -0.011(7) Ni1 0.0318(15) 0.057(2) 0.0406(15) -0.0326(15) 0.0007(11) -0.0083(13) O91 0.058(8) 0.066(9) 0.048(7) -0.024(6) -0.011(5) -0.013(6) C92 0.067(13) 0.047(12) 0.061(12) -0.014(9) 0.009(9) -0.024(10) C93 0.060(12) 0.080(15) 0.057(11) -0.032(11) 0.013(9) -0.043(10) C94 0.037(9) 0.084(15) 0.059(11) -0.058(11) 0.008(7) -0.016(9) O95 0.050(7) 0.077(9) 0.053(7) -0.046(7) -0.005(5) -0.014(6) C921 0.091(19) 0.12(3) 0.096(19) -0.004(17) -0.003(14) -0.036(17) _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 1.799(11) . ? W1 P5 2.519(4) . ? W1 P4 2.523(4) . ? W1 P8 2.534(4) . ? W1 P1 2.537(4) . ? W1 Br2 2.621(3) . ? P1 C21 1.803(16) . ? P1 C11 1.845(16) . ? P1 C2 1.849(14) . ? C11 C16 1.39(2) . ? C11 C12 1.40(2) . ? C12 C13 1.39(3) . ? C13 C14 1.33(3) . ? C14 C15 1.38(3) . ? C15 C16 1.43(2) . ? C21 C22 1.37(2) . ? C21 C26 1.38(2) . ? C22 C23 1.39(2) . ? C23 C24 1.36(2) . ? C24 C25 1.35(2) . ? C25 C26 1.40(2) . ? C2 C3 1.542(19) . ? C3 P4 1.833(14) . ? P4 C31 1.809(15) . ? P4 C41 1.856(13) . ? C31 C32 1.37(2) . ? C31 C36 1.38(2) . ? C36 C35 1.39(2) . ? C35 C34 1.38(3) . ? C34 C33 1.34(3) . ? C32 C33 1.41(2) . ? C41 C46 1.38(2) . ? C41 C42 1.39(2) . ? C45 C44 1.34(3) . ? C45 C46 1.38(2) . ? C42 C43 1.39(2) . ? C43 C44 1.40(2) . ? P5 C51 1.829(14) . ? P5 C6 1.845(15) . ? P5 C61 1.848(14) . ? C6 C7 1.552(18) . ? C7 P8 1.846(13) . ? P8 C71 1.828(14) . ? P8 C81 1.844(9) . ? C51 C56 1.395(19) . ? C51 C52 1.403(19) . ? C52 C53 1.386(19) . ? C53 C54 1.38(2) . ? C54 C55 1.36(2) . ? C55 C56 1.40(2) . ? C61 C66 1.35(2) . ? C61 C62 1.386(19) . ? C62 C63 1.38(2) . ? C63 C64 1.35(3) . ? C64 C65 1.40(2) . ? C65 C66 1.436(19) . ? C71 C76 1.38(2) . ? C71 C72 1.41(2) . ? C76 C75 1.38(2) . ? C75 C74 1.38(2) . ? C72 C73 1.40(2) . ? C73 C74 1.36(2) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? N100 N101 1.312(16) . ? N101 C102 1.283(19) . ? C102 N103 1.153(18) . ? N103 Ni1 2.066(13) . ? Ni1 O95 2.056(11) 2_677 ? Ni1 O95 2.056(11) . ? Ni1 O91 2.062(11) . ? Ni1 O91 2.062(11) 2_677 ? Ni1 N103 2.066(13) 2_677 ? O91 C92 1.256(17) . ? C92 C93 1.43(2) . ? C92 C921 1.64(2) . ? C93 C94 1.40(2) . ? C94 O95 1.263(17) . ? C94 C941 1.574(19) . ? C921 F926 1.345(16) . ? C921 F927 1.348(15) . ? C921 F923 1.352(15) . ? C921 F924 1.356(15) . ? C921 F922 1.388(16) . ? C921 F925 1.409(15) . ? C941 F947 1.319(14) . ? C941 F943 1.326(14) . ? C941 F944 1.369(14) . ? C941 F945 1.395(15) . ? C941 F946 1.415(15) . ? C941 F942 1.418(14) . ? C111 C114 1.33(3) 2_468 ? C111 C113 1.33(3) 2_468 ? C111 C112 1.38(3) . ? C112 C114 1.39(3) . ? C112 C113 1.39(3) . ? C113 C111 1.33(3) 2_468 ? C114 C111 1.33(3) 2_468 ? C114 C115 1.58(6) . ? C121 C126 1.25(5) . ? C121 C122 1.37(5) . ? C121 C127 1.538(19) . ? C122 C123 1.29(7) . ? C123 C124 1.33(7) . ? C124 C125 1.16(6) . ? C125 C126 1.18(5) . ? 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 91.8(3) . . ? N100 W1 P4 96.3(4) . . ? P5 W1 P4 99.82(15) . . ? N100 W1 P8 92.0(4) . . ? P5 W1 P8 79.19(14) . . ? P4 W1 P8 171.62(13) . . ? N100 W1 P1 91.7(3) . . ? P5 W1 P1 176.42(15) . . ? P4 W1 P1 79.38(15) . . ? P8 W1 P1 101.08(14) . . ? N100 W1 Br2 179.3(3) . . ? P5 W1 Br2 88.81(13) . . ? P4 W1 Br2 83.82(12) . . ? P8 W1 Br2 87.84(12) . . ? P1 W1 Br2 87.64(12) . . ? C21 P1 C11 102.1(7) . . ? C21 P1 C2 103.0(7) . . ? C11 P1 C2 101.5(7) . . ? C21 P1 W1 122.5(5) . . ? C11 P1 W1 118.6(5) . . ? C2 P1 W1 106.2(5) . . ? C16 C11 C12 118.5(16) . . ? C16 C11 P1 119.9(13) . . ? C12 C11 P1 121.6(13) . . ? C13 C12 C11 121(2) . . ? C14 C13 C12 120(2) . . ? C13 C14 C15 121(2) . . ? C14 C15 C16 120(2) . . ? C11 C16 C15 119(2) . . ? C22 C21 C26 116.0(15) . . ? C22 C21 P1 123.1(13) . . ? C26 C21 P1 120.6(12) . . ? C21 C22 C23 122.2(18) . . ? C24 C23 C22 120.0(18) . . ? C25 C24 C23 120.0(18) . . ? C24 C25 C26 119.7(17) . . ? C21 C26 C25 121.9(16) . . ? C3 C2 P1 108.6(9) . . ? C2 C3 P4 107.8(10) . . ? C31 P4 C3 103.3(7) . . ? C31 P4 C41 102.5(6) . . ? C3 P4 C41 102.4(6) . . ? C31 P4 W1 122.7(5) . . ? C3 P4 W1 107.5(5) . . ? C41 P4 W1 115.9(5) . . ? C32 C31 C36 117.1(15) . . ? C32 C31 P4 120.2(12) . . ? C36 C31 P4 122.6(12) . . ? C31 C36 C35 123.0(17) . . ? C34 C35 C36 117.9(19) . . ? C33 C34 C35 121(2) . . ? C31 C32 C33 120.5(18) . . ? C34 C33 C32 120(2) . . ? C46 C41 C42 118.8(14) . . ? C46 C41 P4 121.5(12) . . ? C42 C41 P4 119.6(10) . . ? C44 C45 C46 124(2) . . ? C41 C42 C43 120.9(15) . . ? C42 C43 C44 119.9(19) . . ? C45 C44 C43 117.4(18) . . ? C41 C46 C45 118.6(19) . . ? C51 P5 C6 101.3(7) . . ? C51 P5 C61 102.7(6) . . ? C6 P5 C61 104.6(7) . . ? C51 P5 W1 117.2(5) . . ? C6 P5 W1 106.0(4) . . ? C61 P5 W1 122.5(5) . . ? C7 C6 P5 106.3(10) . . ? C6 C7 P8 108.3(8) . . ? C71 P8 C81 102.4(6) . . ? C71 P8 C7 102.3(6) . . ? C81 P8 C7 102.9(6) . . ? C71 P8 W1 124.6(5) . . ? C81 P8 W1 114.7(4) . . ? C7 P8 W1 107.4(4) . . ? C56 C51 C52 116.9(13) . . ? C56 C51 P5 123.1(12) . . ? C52 C51 P5 120.0(11) . . ? C53 C52 C51 122.5(14) . . ? C54 C53 C52 118.6(15) . . ? C55 C54 C53 121.1(15) . . ? C54 C55 C56 120.0(16) . . ? C51 C56 C55 120.9(16) . . ? C66 C61 C62 119.3(14) . . ? C66 C61 P5 118.3(11) . . ? C62 C61 P5 122.4(13) . . ? C63 C62 C61 119.7(17) . . ? C64 C63 C62 122.5(17) . . ? C63 C64 C65 119.0(16) . . ? C64 C65 C66 118.3(17) . . ? C61 C66 C65 121.0(14) . . ? C76 C71 C72 117.7(13) . . ? C76 C71 P8 120.9(11) . . ? C72 C71 P8 121.4(12) . . ? C75 C76 C71 121.9(15) . . ? C76 C75 C74 120.2(17) . . ? C73 C72 C71 119.4(16) . . ? C74 C73 C72 121.7(16) . . ? C73 C74 C75 118.9(15) . . ? C82 C81 C86 120.0 . . ? C82 C81 P8 117.5(6) . . ? C86 C81 P8 122.5(6) . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C84 C85 C86 120.0 . . ? C85 C86 C81 120.0 . . ? N101 N100 W1 169.2(10) . . ? C102 N101 N100 123.7(14) . . ? N103 C102 N101 164.6(18) . . ? C102 N103 Ni1 163.0(14) . . ? O95 Ni1 O95 179.998(2) 2_677 . ? O95 Ni1 O91 91.6(4) 2_677 . ? O95 Ni1 O91 88.4(4) . . ? O95 Ni1 O91 88.4(4) 2_677 2_677 ? O95 Ni1 O91 91.6(4) . 2_677 ? O91 Ni1 O91 180.000(4) . 2_677 ? O95 Ni1 N103 94.1(5) 2_677 2_677 ? O95 Ni1 N103 85.9(5) . 2_677 ? O91 Ni1 N103 87.1(5) . 2_677 ? O91 Ni1 N103 92.9(5) 2_677 2_677 ? O95 Ni1 N103 85.9(5) 2_677 . ? O95 Ni1 N103 94.1(5) . . ? O91 Ni1 N103 92.9(5) . . ? O91 Ni1 N103 87.1(5) 2_677 . ? N103 Ni1 N103 179.999(3) 2_677 . ? C92 O91 Ni1 126.9(9) . . ? O91 C92 C93 122.9(12) . . ? O91 C92 C921 116.5(12) . . ? C93 C92 C921 120.6(12) . . ? C94 C93 C92 127.6(13) . . ? O95 C94 C93 124.4(11) . . ? O95 C94 C941 115.5(11) . . ? C93 C94 C941 120.1(12) . . ? C94 O95 Ni1 125.6(8) . . ? F926 C921 F927 118.0(16) . . ? F923 C921 F922 115.0(16) . . ? F924 C921 F922 112.6(15) . . ? F926 C921 F925 113.1(15) . . ? F927 C921 F925 112.8(15) . . ? F926 C921 C92 105.3(14) . . ? F927 C921 C92 104.9(14) . . ? F923 C921 C92 104.2(14) . . ? F924 C921 C92 105.0(14) . . ? F922 C921 C92 100.6(14) . . ? F925 C921 C92 100.4(14) . . ? F943 C941 F944 116.2(14) . . ? F947 C941 F946 113.4(14) . . ? F945 C941 F946 108.4(13) . . ? F943 C941 F942 111.3(13) . . ? F944 C941 F942 109.7(13) . . ? F945 C941 F947 114.0(14) . . ? F947 C941 C94 112.1(13) . . ? F943 C941 C94 109.0(12) . . ? F944 C941 C94 105.8(12) . . ? F945 C941 C94 105.8(12) . . ? F946 C941 C94 102.3(12) . . ? F942 C941 C94 104.0(12) . . ? C114 C111 C112 122(3) 2_468 . ? C113 C111 C112 122(3) 2_468 . ? C111 C112 C114 120(3) . . ? C111 C112 C113 120(3) . . ? C111 C113 C112 118(3) 2_468 . ? C111 C114 C112 118(3) 2_468 . ? C111 C114 C115 121(4) 2_468 . ? C112 C114 C115 121(4) . . ? C126 C121 C122 109(4) . . ? C126 C121 C127 130(4) . . ? C122 C121 C127 120(4) . . ? C123 C122 C121 115(6) . . ? C122 C123 C124 124(8) . . ? C125 C124 C123 114(6) . . ? C124 C125 C126 122(5) . . ? C125 C126 C121 133(5) . . ? C121 C126 C124 105(4) . . ? _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_full 0.879 _refine_diff_density_max 1.096 _refine_diff_density_min -2.266 _refine_diff_density_rms 0.206 _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_7 _database_code_depnum_ccdc_archive 'CCDC 641375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H114 Br2 F12 N6 O4 P8 W2 Zn' _chemical_formula_weight 2892.92 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 12.3596(15) _cell_length_b 16.162(2) _cell_length_c 18.3412(19) _cell_angle_alpha 66.374(10) _cell_angle_beta 77.310(10) _cell_angle_gamma 72.154(10) _cell_volume 3175.4(7) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 2.796 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SORTAV _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 CCD System' _diffrn_measurement_method '431 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51339 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14463 _reflns_number_gt 10889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker-Nonius' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO and Scalepack (Otwinowski & Minor 1997i)' _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. The CF3 groups were disordered and two sets of fluorines were refined with distance constraints.; ; _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^)+(0.0413P)^2^+42.5124P] 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 14463 _refine_ls_number_parameters 733 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.776 _refine_ls_restrained_S_all 0.795 _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 0.815880(19) 0.744792(16) 0.749070(14) 0.01548(7) Uani 1 1 d . . . Br2 Br 0.87675(5) 0.64678(4) 0.65683(4) 0.02316(13) Uani 1 1 d . . . P1 P 0.96313(12) 0.62559(10) 0.83880(9) 0.0180(3) Uani 1 1 d . . . C11 C 1.0315(5) 0.6636(4) 0.8950(3) 0.0234(13) Uani 1 1 d . . . C12 C 1.1485(6) 0.6570(5) 0.8826(4) 0.0320(15) Uani 1 1 d . . . H12 H 1.1947 0.6299 0.8467 0.038 Uiso 1 1 calc R . . C13 C 1.1970(7) 0.6904(5) 0.9234(5) 0.0411(18) Uani 1 1 d . . . H13 H 1.2753 0.6859 0.9143 0.049 Uiso 1 1 calc R . . C14 C 1.1309(8) 0.7297(5) 0.9765(5) 0.046(2) Uani 1 1 d . . . H14 H 1.1643 0.7512 1.0040 0.055 Uiso 1 1 calc R . . C15 C 1.0144(8) 0.7380(5) 0.9896(4) 0.048(2) Uani 1 1 d . . . H15 H 0.9696 0.7651 1.0258 0.058 Uiso 1 1 calc R . . C16 C 0.9633(7) 0.7056(4) 0.9485(4) 0.0334(16) Uani 1 1 d . . . H16 H 0.8846 0.7120 0.9568 0.040 Uiso 1 1 calc R . . C21 C 1.0844(5) 0.5464(4) 0.8038(4) 0.0206(12) Uani 1 1 d U . . C22 C 1.1354(6) 0.4598(4) 0.8561(4) 0.0326(15) Uani 1 1 d U . . H22 H 1.1058 0.4403 0.9098 0.039 Uiso 1 1 calc R . . C23 C 1.2299(6) 0.4020(5) 0.8296(5) 0.0421(17) Uani 1 1 d U . . H23 H 1.2638 0.3446 0.8656 0.050 Uiso 1 1 calc R . . C24 C 1.2741(6) 0.4292(5) 0.7494(5) 0.0374(16) Uani 1 1 d U . . H24 H 1.3353 0.3896 0.7307 0.045 Uiso 1 1 calc R . . C25 C 1.2249(6) 0.5167(5) 0.6979(4) 0.0348(15) Uani 1 1 d U . . H25 H 1.2554 0.5365 0.6445 0.042 Uiso 1 1 calc R . . C26 C 1.1318(5) 0.5753(4) 0.7239(4) 0.0261(13) Uani 1 1 d U . . H26 H 1.1006 0.6339 0.6883 0.031 Uiso 1 1 calc R . . C2 C 0.8872(5) 0.5440(4) 0.9204(3) 0.0223(13) Uani 1 1 d . . . H2A H 0.9419 0.4887 0.9490 0.027 Uiso 1 1 calc R . . H2B H 0.8421 0.5733 0.9580 0.027 Uiso 1 1 calc R . . C3 C 0.8096(5) 0.5180(4) 0.8834(4) 0.0219(12) Uani 1 1 d . . . H3A H 0.7706 0.4733 0.9245 0.026 Uiso 1 1 calc R . . H3B H 0.8542 0.4904 0.8446 0.026 Uiso 1 1 calc R . . P4 P 0.70508(13) 0.62562(10) 0.83419(9) 0.0180(3) Uani 1 1 d . . . C31 C 0.6200(5) 0.5858(4) 0.7909(3) 0.0206(12) Uani 1 1 d . . . C36 C 0.5047(5) 0.6281(4) 0.7847(4) 0.0265(14) Uani 1 1 d . . . H36 H 0.4682 0.6729 0.8077 0.032 Uiso 1 1 calc R . . C35 C 0.4434(6) 0.6040(5) 0.7445(4) 0.0333(16) Uani 1 1 d . . . H35 H 0.3660 0.6325 0.7407 0.040 Uiso 1 1 calc R . . C34 C 0.4974(7) 0.5373(6) 0.7101(4) 0.0397(18) Uani 1 1 d . . . H34 H 0.4564 0.5217 0.6827 0.048 Uiso 1 1 calc R . . C32 C 0.6727(6) 0.5172(4) 0.7570(4) 0.0277(14) Uani 1 1 d . . . H32 H 0.7495 0.4870 0.7619 0.033 Uiso 1 1 calc R . . C33 C 0.6116(7) 0.4940(5) 0.7164(4) 0.0391(17) Uani 1 1 d . . . H33 H 0.6476 0.4492 0.6934 0.047 Uiso 1 1 calc R . . C41 C 0.6061(5) 0.6489(4) 0.9179(4) 0.0223(12) Uani 1 1 d . . . C45 C 0.5138(7) 0.5998(5) 1.0536(4) 0.045(2) Uani 1 1 d . . . H45 H 0.5071 0.5533 1.1036 0.054 Uiso 1 1 calc R . . C42 C 0.5381(5) 0.7377(4) 0.9066(4) 0.0265(14) Uani 1 1 d . . . H42 H 0.5467 0.7851 0.8575 0.032 Uiso 1 1 calc R . . C43 C 0.4569(6) 0.7579(5) 0.9669(4) 0.0328(15) Uani 1 1 d . . . H43 H 0.4109 0.8179 0.9576 0.039 Uiso 1 1 calc R . . C44 C 0.4451(6) 0.6888(5) 1.0401(4) 0.0352(16) Uani 1 1 d . . . H44 H 0.3909 0.7018 1.0806 0.042 Uiso 1 1 calc R . . C46 C 0.5925(7) 0.5798(5) 0.9928(4) 0.0396(18) Uani 1 1 d . . . H46 H 0.6369 0.5193 1.0019 0.047 Uiso 1 1 calc R . . P5 P 0.67053(12) 0.85901(10) 0.65745(9) 0.0168(3) Uani 1 1 d . . . C6 C 0.7247(5) 0.9646(4) 0.6035(4) 0.0208(12) Uani 1 1 d . . . H6A H 0.6774 1.0082 0.5616 0.025 Uiso 1 1 calc R . . H6B H 0.7238 0.9947 0.6400 0.025 Uiso 1 1 calc R . . C7 C 0.8477(5) 0.9335(4) 0.5673(3) 0.0203(12) Uani 1 1 d . . . H7A H 0.8792 0.9872 0.5364 0.024 Uiso 1 1 calc R . . H7B H 0.8487 0.9017 0.5320 0.024 Uiso 1 1 calc R . . P8 P 0.93278(12) 0.85423(10) 0.65084(9) 0.0167(3) Uani 1 1 d . . . C51 C 0.5300(5) 0.9036(4) 0.7034(3) 0.0199(12) Uani 1 1 d . . . C52 C 0.5195(5) 0.9590(4) 0.7483(3) 0.0215(12) Uani 1 1 d . . . H52 H 0.5838 0.9750 0.7519 0.026 Uiso 1 1 calc R . . C53 C 0.4152(5) 0.9904(4) 0.7875(4) 0.0268(14) Uani 1 1 d . . . H53 H 0.4096 1.0273 0.8168 0.032 Uiso 1 1 calc R . . C54 C 0.3191(5) 0.9663(5) 0.7827(4) 0.0292(14) Uani 1 1 d . . . H54 H 0.2487 0.9876 0.8085 0.035 Uiso 1 1 calc R . . C55 C 0.3274(5) 0.9112(5) 0.7399(4) 0.0310(15) Uani 1 1 d . . . H55 H 0.2628 0.8948 0.7374 0.037 Uiso 1 1 calc R . . C56 C 0.4325(5) 0.8796(4) 0.7002(4) 0.0252(13) Uani 1 1 d . . . H56 H 0.4374 0.8423 0.6714 0.030 Uiso 1 1 calc R . . C61 C 0.6358(5) 0.8358(4) 0.5763(3) 0.0192(12) Uani 1 1 d . . . C62 C 0.6260(5) 0.9021(4) 0.4991(4) 0.0274(14) Uani 1 1 d . . . H62 H 0.6389 0.9602 0.4868 0.033 Uiso 1 1 calc R . . C63 C 0.5968(6) 0.8812(4) 0.4404(4) 0.0301(15) Uani 1 1 d . . . H63 H 0.5914 0.9256 0.3890 0.036 Uiso 1 1 calc R . . C64 C 0.5760(5) 0.7970(5) 0.4569(4) 0.0280(14) Uani 1 1 d . . . H64 H 0.5549 0.7844 0.4175 0.034 Uiso 1 1 calc R . . C65 C 0.5868(5) 0.7303(4) 0.5332(4) 0.0259(13) Uani 1 1 d . . . H65 H 0.5738 0.6723 0.5449 0.031 Uiso 1 1 calc R . . C66 C 0.6170(5) 0.7496(4) 0.5922(4) 0.0223(12) Uani 1 1 d . . . H66 H 0.6246 0.7042 0.6430 0.027 Uiso 1 1 calc R . . C71 C 1.0707(5) 0.8175(4) 0.5961(3) 0.0198(12) Uani 1 1 d . . . C76 C 1.0777(5) 0.7775(4) 0.5403(3) 0.0212(12) Uani 1 1 d . . . H76 H 1.0114 0.7710 0.5295 0.025 Uiso 1 1 calc R . . C75 C 1.1822(5) 0.7472(4) 0.5007(4) 0.0259(13) Uani 1 1 d . . . H75 H 1.1855 0.7202 0.4637 0.031 Uiso 1 1 calc R . . C72 C 1.1710(5) 0.8266(5) 0.6121(4) 0.0281(14) Uani 1 1 d . . . H72 H 1.1681 0.8529 0.6494 0.034 Uiso 1 1 calc R . . C73 C 1.2764(6) 0.7958(5) 0.5714(4) 0.0341(16) Uani 1 1 d . . . H73 H 1.3432 0.8016 0.5821 0.041 Uiso 1 1 calc R . . C74 C 1.2814(5) 0.7570(5) 0.5156(4) 0.0323(15) Uani 1 1 d . . . H74 H 1.3513 0.7375 0.4883 0.039 Uiso 1 1 calc R . . C81 C 0.9609(4) 0.9341(2) 0.6893(2) 0.0202(12) Uani 1 1 d G . . C82 C 0.9931(3) 0.89822(19) 0.7662(2) 0.0233(13) Uani 1 1 d G . . H82 H 0.9988 0.8356 0.7971 0.028 Uiso 1 1 calc R . . C83 C 1.0168(4) 0.9560(3) 0.79681(18) 0.0261(13) Uani 1 1 d G . . H83 H 1.0384 0.9320 0.8482 0.031 Uiso 1 1 calc R . . C84 C 1.0083(4) 1.0496(2) 0.7506(2) 0.0312(15) Uani 1 1 d G . . H84 H 1.0242 1.0882 0.7711 0.037 Uiso 1 1 calc R . . C85 C 0.9761(4) 1.08542(19) 0.6737(2) 0.0399(18) Uani 1 1 d G . . H85 H 0.9704 1.1480 0.6428 0.048 Uiso 1 1 calc R . . C86 C 0.9524(4) 1.0277(3) 0.64309(18) 0.0334(16) Uani 1 1 d G . . H86 H 0.9308 1.0517 0.5917 0.040 Uiso 1 1 calc R . . N100 N 0.7741(4) 0.8132(3) 0.8123(3) 0.0217(11) Uani 1 1 d U . . N101 N 0.7631(5) 0.8658(4) 0.8515(4) 0.0341(13) Uani 1 1 d U . . C102 C 0.6749(6) 0.8842(5) 0.8994(4) 0.0296(14) Uani 1 1 d U . . N103 N 0.6030(5) 0.9064(5) 0.9464(4) 0.0398(15) Uani 1 1 d U . . ZN1 Zn 0.5000 1.0000 1.0000 0.0298(2) Uani 1 2 d S . . O91 O 0.4952(4) 0.8938(3) 1.1151(3) 0.0370(11) Uani 1 1 d . . . C92 C 0.4061(6) 0.8692(5) 1.1527(4) 0.0359(16) Uani 1 1 d D . . C93 C 0.2994(6) 0.8915(5) 1.1249(4) 0.0329(15) Uani 1 1 d . . . H93 H 0.2393 0.8710 1.1615 0.039 Uiso 1 1 calc R . . C94 C 0.2796(5) 0.9426(4) 1.0453(4) 0.0284(14) Uani 1 1 d D . . O95 O 0.3477(4) 0.9782(3) 0.9871(3) 0.0302(10) Uani 1 1 d . . . C921 C 0.4155(6) 0.8057(5) 1.2411(5) 0.051(2) Uani 1 1 d D . . F922 F 0.4540(14) 0.7141(7) 1.2411(9) 0.082(5) Uani 0.50 1 d PD . . F923 F 0.4982(15) 0.8176(12) 1.2701(10) 0.091(7) Uani 0.50 1 d PD . . F924 F 0.3185(10) 0.8097(14) 1.2883(7) 0.117(8) Uani 0.50 1 d PD . . F925 F 0.3571(13) 0.8607(9) 1.2871(7) 0.077(5) Uani 0.50 1 d PD . . F926 F 0.5249(11) 0.7787(11) 1.2578(10) 0.074(5) Uani 0.50 1 d PD . . F927 F 0.369(2) 0.7353(11) 1.2630(8) 0.116(8) Uani 0.50 1 d PD . . C941 C 0.1618(6) 0.9586(4) 1.0228(4) 0.0330(15) Uiso 1 1 d D . . F942 F 0.1043(7) 0.8929(7) 1.0801(5) 0.0365(8) Uiso 0.558(17) 1 d PD . . F943 F 0.1645(8) 0.9511(7) 0.9524(5) 0.0365(8) Uiso 0.558(17) 1 d PD . . F944 F 0.0978(7) 1.0416(6) 1.0214(7) 0.0365(8) Uiso 0.558(17) 1 d PD . . F945 F 0.1142(9) 1.0553(6) 0.9909(9) 0.0365(8) Uiso 0.442(17) 1 d PD . . F946 F 0.1753(9) 0.9237(8) 0.9635(6) 0.0365(8) Uiso 0.442(17) 1 d PD . . F947 F 0.0870(8) 0.9236(10) 1.0816(5) 0.0365(8) Uiso 0.442(17) 1 d PD . . C111 C -0.5726(7) 0.5673(5) 1.4463(5) 0.0435(18) Uiso 1 1 d . . . H111 H -0.6207 0.6134 1.4096 0.052 Uiso 1 1 calc R . . C112 C -0.4620(7) 0.5744(6) 1.4434(5) 0.0436(18) Uiso 1 1 d . . . H112 H -0.4371 0.6252 1.4048 0.052 Uiso 1 1 calc R A 1 C113 C -0.3891(7) 0.5070(5) 1.4972(5) 0.0432(18) Uiso 0.50 1 d P . 1 H113 H -0.3154 0.5119 1.4952 0.052 Uiso 0.50 1 calc PR . 1 C114 C -0.3891(7) 0.5070(5) 1.4972(5) 0.0432(18) Uiso 0.50 1 d P . 2 C115 C -0.2645(16) 0.5173(13) 1.4929(12) 0.062(5) Uiso 0.50 1 d P B 2 H11A H -0.2620 0.5387 1.5342 0.074 Uiso 0.50 1 calc PR B 2 H11B H -0.2449 0.5613 1.4416 0.074 Uiso 0.50 1 calc PR B 2 H11C H -0.2109 0.4580 1.5004 0.074 Uiso 0.50 1 calc PR B 2 C121 C 0.0981(9) 1.2746(7) 0.7165(6) 0.013(2) Uiso 0.50 1 d PD . . C122 C 0.0164(13) 1.3540(10) 0.6983(9) 0.045(4) Uiso 0.50 1 d PD . . H122 H -0.0179 1.3784 0.7382 0.054 Uiso 0.50 1 calc PR . . C123 C -0.0188(14) 1.4005(12) 0.6243(10) 0.050(4) Uiso 0.50 1 d P . . H123 H -0.0735 1.4569 0.6139 0.059 Uiso 0.50 1 calc PR . . C124 C 0.0257(10) 1.3650(8) 0.5649(7) 0.023(3) Uiso 0.50 1 d P . . H124 H -0.0041 1.3924 0.5160 0.028 Uiso 0.50 1 calc PR . . C125 C 0.1137(8) 1.2892(6) 0.5793(6) 0.0070(18) Uiso 0.50 1 d P . . H125 H 0.1512 1.2674 0.5383 0.008 Uiso 0.50 1 calc PR . . C126 C 0.1484(8) 1.2436(7) 0.6550(5) 0.0082(19) Uiso 0.50 1 d PD . . H126 H 0.2080 1.1902 0.6644 0.010 Uiso 0.50 1 calc PR . . C127 C 0.1371(10) 1.2229(8) 0.8002(6) 0.028(3) Uiso 0.50 1 d PD . . H12A H 0.2190 1.2027 0.7958 0.034 Uiso 0.50 1 calc PR . . H12B H 0.1050 1.1698 0.8273 0.034 Uiso 0.50 1 calc PR . . H12C H 0.1116 1.2638 0.8300 0.034 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 0.01586(11) 0.01474(11) 0.01339(12) -0.00271(8) -0.00172(8) -0.00350(8) Br2 0.0241(3) 0.0241(3) 0.0220(3) -0.0100(2) -0.0009(2) -0.0056(2) P1 0.0193(7) 0.0179(7) 0.0144(7) -0.0036(6) -0.0027(6) -0.0037(6) C11 0.033(3) 0.014(3) 0.014(3) 0.002(2) -0.007(3) 0.000(2) C12 0.038(4) 0.030(3) 0.028(4) -0.005(3) -0.009(3) -0.012(3) C13 0.050(5) 0.034(4) 0.042(5) -0.004(3) -0.021(4) -0.015(3) C14 0.076(6) 0.029(4) 0.042(5) -0.005(3) -0.031(4) -0.018(4) C15 0.093(7) 0.024(4) 0.028(4) -0.011(3) -0.017(4) -0.005(4) C16 0.054(4) 0.022(3) 0.021(3) -0.008(3) -0.005(3) -0.003(3) C21 0.022(3) 0.022(3) 0.023(3) -0.014(2) -0.002(2) -0.005(2) C22 0.036(3) 0.026(3) 0.026(3) -0.007(3) -0.001(3) 0.001(3) C23 0.040(4) 0.026(3) 0.046(4) -0.008(3) -0.005(3) 0.004(3) C24 0.036(3) 0.030(3) 0.047(4) -0.019(3) 0.000(3) -0.004(3) C25 0.027(3) 0.037(3) 0.035(4) -0.012(3) -0.003(3) -0.003(3) C26 0.021(3) 0.029(3) 0.024(3) -0.005(2) -0.003(2) -0.007(2) C2 0.024(3) 0.021(3) 0.015(3) 0.002(2) -0.007(2) -0.005(2) C3 0.021(3) 0.017(3) 0.024(3) -0.003(2) -0.003(2) -0.006(2) P4 0.0208(7) 0.0160(7) 0.0147(7) -0.0030(6) -0.0008(6) -0.0056(6) C31 0.027(3) 0.022(3) 0.012(3) -0.002(2) 0.002(2) -0.014(2) C36 0.030(3) 0.032(3) 0.020(3) -0.007(3) 0.001(3) -0.016(3) C35 0.028(3) 0.046(4) 0.026(4) -0.003(3) -0.006(3) -0.020(3) C34 0.046(4) 0.059(5) 0.030(4) -0.019(4) 0.000(3) -0.032(4) C32 0.034(3) 0.030(3) 0.022(3) -0.011(3) 0.004(3) -0.015(3) C33 0.054(5) 0.044(4) 0.033(4) -0.022(3) 0.004(3) -0.026(4) C41 0.025(3) 0.025(3) 0.018(3) -0.007(2) 0.002(2) -0.012(2) C45 0.057(5) 0.036(4) 0.026(4) -0.001(3) 0.016(3) -0.018(4) C42 0.030(3) 0.024(3) 0.019(3) -0.005(3) 0.005(3) -0.007(3) C43 0.034(4) 0.028(3) 0.032(4) -0.015(3) 0.009(3) -0.005(3) C44 0.041(4) 0.038(4) 0.027(4) -0.014(3) 0.015(3) -0.020(3) C46 0.050(4) 0.026(3) 0.030(4) -0.002(3) 0.006(3) -0.008(3) P5 0.0164(7) 0.0178(7) 0.0145(7) -0.0039(6) -0.0015(6) -0.0046(6) C6 0.021(3) 0.016(3) 0.022(3) -0.003(2) -0.003(2) -0.005(2) C7 0.021(3) 0.024(3) 0.012(3) -0.002(2) -0.001(2) -0.006(2) P8 0.0160(7) 0.0184(7) 0.0135(7) -0.0030(6) -0.0008(6) -0.0053(6) C51 0.020(3) 0.019(3) 0.019(3) -0.004(2) -0.007(2) -0.003(2) C52 0.020(3) 0.027(3) 0.016(3) -0.005(2) -0.002(2) -0.007(2) C53 0.030(3) 0.033(3) 0.017(3) -0.012(3) -0.002(3) -0.002(3) C54 0.018(3) 0.039(4) 0.029(4) -0.017(3) 0.000(3) -0.002(3) C55 0.021(3) 0.039(4) 0.035(4) -0.016(3) 0.001(3) -0.009(3) C56 0.024(3) 0.027(3) 0.025(3) -0.012(3) 0.000(3) -0.006(3) C61 0.016(3) 0.026(3) 0.015(3) -0.008(2) -0.001(2) -0.003(2) C62 0.035(4) 0.021(3) 0.022(3) -0.006(3) -0.006(3) -0.002(3) C63 0.039(4) 0.027(3) 0.017(3) -0.003(3) -0.010(3) 0.000(3) C64 0.024(3) 0.041(4) 0.023(3) -0.016(3) -0.004(3) -0.005(3) C65 0.027(3) 0.027(3) 0.028(4) -0.013(3) -0.001(3) -0.009(3) C66 0.019(3) 0.026(3) 0.022(3) -0.010(3) -0.005(2) -0.003(2) C71 0.021(3) 0.018(3) 0.013(3) 0.002(2) 0.000(2) -0.007(2) C76 0.023(3) 0.021(3) 0.020(3) -0.004(2) -0.002(2) -0.010(2) C75 0.028(3) 0.027(3) 0.024(3) -0.012(3) 0.003(3) -0.006(3) C72 0.026(3) 0.035(4) 0.027(3) -0.014(3) -0.001(3) -0.009(3) C73 0.022(3) 0.043(4) 0.039(4) -0.021(3) 0.000(3) -0.005(3) C74 0.022(3) 0.032(4) 0.042(4) -0.019(3) 0.000(3) -0.001(3) C81 0.022(3) 0.019(3) 0.020(3) -0.006(2) 0.002(2) -0.011(2) C82 0.023(3) 0.024(3) 0.021(3) -0.005(3) -0.002(2) -0.007(2) C83 0.029(3) 0.030(3) 0.020(3) -0.008(3) 0.001(3) -0.010(3) C84 0.032(4) 0.029(3) 0.037(4) -0.015(3) -0.003(3) -0.011(3) C85 0.062(5) 0.025(3) 0.034(4) -0.001(3) -0.015(4) -0.020(3) C86 0.050(4) 0.023(3) 0.024(4) -0.001(3) -0.009(3) -0.012(3) N100 0.019(2) 0.021(2) 0.022(3) -0.003(2) -0.004(2) -0.007(2) N101 0.028(3) 0.041(3) 0.037(3) -0.026(3) 0.009(3) -0.006(3) C102 0.031(3) 0.033(3) 0.032(4) -0.014(3) -0.008(3) -0.009(3) N103 0.032(3) 0.056(4) 0.047(4) -0.039(3) 0.003(3) -0.008(3) ZN1 0.0240(5) 0.0427(6) 0.0328(6) -0.0251(5) 0.0036(4) -0.0107(5) O91 0.028(2) 0.046(3) 0.039(3) -0.019(2) -0.008(2) -0.005(2) C92 0.038(4) 0.037(4) 0.037(4) -0.018(3) -0.004(3) -0.007(3) C93 0.030(3) 0.032(4) 0.035(4) -0.013(3) 0.002(3) -0.009(3) C94 0.027(3) 0.035(4) 0.028(4) -0.020(3) 0.002(3) -0.007(3) O95 0.026(2) 0.043(3) 0.028(3) -0.020(2) -0.0006(19) -0.011(2) C921 0.047(5) 0.043(5) 0.053(5) -0.005(4) -0.016(4) -0.008(4) F922 0.129(13) 0.048(7) 0.052(9) 0.003(6) -0.021(9) -0.018(8) F923 0.152(19) 0.093(14) 0.052(9) -0.006(9) -0.048(11) -0.065(13) F924 0.066(9) 0.147(17) 0.031(7) 0.022(10) 0.008(6) 0.039(10) F925 0.115(13) 0.078(9) 0.032(6) -0.016(6) -0.001(7) -0.023(8) F926 0.070(8) 0.071(11) 0.064(10) -0.006(8) -0.033(7) 0.002(7) F927 0.24(3) 0.085(12) 0.052(10) 0.016(8) -0.050(14) -0.115(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 1.803(5) . ? W1 P5 2.5032(15) . ? W1 P4 2.5079(15) . ? W1 P8 2.5160(15) . ? W1 P1 2.5214(15) . ? W1 Br2 2.6068(7) . ? P1 C21 1.832(6) . ? P1 C11 1.834(6) . ? P1 C2 1.849(6) . ? C11 C12 1.391(9) . ? C11 C16 1.397(9) . ? C12 C13 1.390(10) . ? C13 C14 1.359(11) . ? C14 C15 1.380(12) . ? C15 C16 1.403(10) . ? C21 C22 1.388(8) . ? C21 C26 1.397(8) . ? C22 C23 1.386(9) . ? C23 C24 1.390(10) . ? C24 C25 1.384(10) . ? C25 C26 1.379(9) . ? C2 C3 1.524(8) . ? C3 P4 1.840(6) . ? P4 C31 1.828(6) . ? P4 C41 1.831(6) . ? C31 C36 1.386(9) . ? C31 C32 1.406(8) . ? C36 C35 1.388(9) . ? C35 C34 1.388(10) . ? C34 C33 1.377(11) . ? C32 C33 1.380(9) . ? C41 C42 1.381(8) . ? C41 C46 1.395(9) . ? C45 C44 1.382(10) . ? C45 C46 1.383(10) . ? C42 C43 1.392(9) . ? C43 C44 1.373(9) . ? P5 C51 1.823(6) . ? P5 C61 1.835(6) . ? P5 C6 1.842(6) . ? C6 C7 1.536(8) . ? C7 P8 1.845(6) . ? P8 C71 1.836(6) . ? P8 C81 1.843(3) . ? C51 C56 1.394(8) . ? C51 C52 1.404(8) . ? C52 C53 1.385(8) . ? C53 C54 1.388(9) . ? C54 C55 1.374(9) . ? C55 C56 1.398(9) . ? C61 C66 1.387(8) . ? C61 C62 1.396(8) . ? C62 C63 1.392(9) . ? C63 C64 1.365(9) . ? C64 C65 1.387(9) . ? C65 C66 1.389(8) . ? C71 C76 1.389(8) . ? C71 C72 1.397(8) . ? C76 C75 1.387(8) . ? C75 C74 1.380(9) . ? C72 C73 1.404(9) . ? C73 C74 1.381(9) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? N100 N101 1.277(7) . ? N101 C102 1.281(8) . ? C102 N103 1.173(8) . ? N103 ZN1 2.083(6) . ? ZN1 N103 2.083(6) 2_677 ? ZN1 O95 2.095(4) . ? ZN1 O95 2.095(4) 2_677 ? ZN1 O91 2.124(5) 2_677 ? ZN1 O91 2.124(5) . ? O91 C92 1.249(8) . ? C92 C93 1.409(9) . ? C92 C921 1.539(10) . ? C93 C94 1.394(9) . ? C94 O95 1.260(7) . ? C94 C941 1.519(8) . ? C921 F927 1.308(11) . ? C921 F924 1.317(11) . ? C921 F923 1.345(12) . ? C921 F926 1.351(12) . ? C921 F925 1.402(12) . ? C921 F922 1.409(12) . ? C941 F947 1.316(10) . ? C941 F944 1.326(9) . ? C941 F943 1.336(9) . ? C941 F946 1.372(10) . ? C941 F942 1.406(9) . ? C941 F945 1.409(10) . ? C111 C114 1.370(11) 2_468 ? C111 C113 1.370(11) 2_468 ? C111 C112 1.394(11) . ? C112 C114 1.377(11) . ? C112 C113 1.377(11) . ? C113 C111 1.370(11) 2_468 ? C114 C111 1.370(11) 2_468 ? C114 C115 1.581(19) . ? C121 C122 1.338(17) . ? C121 C126 1.366(13) . ? C121 C127 1.527(12) . ? C122 C123 1.36(2) . ? C123 C124 1.36(2) . ? C124 C125 1.343(15) . ? C125 C126 1.378(13) . ? 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 90.44(15) . . ? N100 W1 P4 96.35(15) . . ? P5 W1 P4 100.01(5) . . ? N100 W1 P8 90.94(15) . . ? P5 W1 P8 79.07(5) . . ? P4 W1 P8 172.67(5) . . ? N100 W1 P1 91.63(15) . . ? P5 W1 P1 177.88(5) . . ? P4 W1 P1 79.29(5) . . ? P8 W1 P1 101.36(5) . . ? N100 W1 Br2 179.62(16) . . ? P5 W1 Br2 89.39(4) . . ? P4 W1 Br2 84.01(4) . . ? P8 W1 Br2 88.70(4) . . ? P1 W1 Br2 88.55(4) . . ? C21 P1 C11 102.0(3) . . ? C21 P1 C2 102.3(3) . . ? C11 P1 C2 101.7(3) . . ? C21 P1 W1 122.4(2) . . ? C11 P1 W1 118.72(18) . . ? C2 P1 W1 106.81(19) . . ? C12 C11 C16 118.9(6) . . ? C12 C11 P1 122.0(5) . . ? C16 C11 P1 119.1(5) . . ? C13 C12 C11 120.6(7) . . ? C14 C13 C12 120.5(8) . . ? C13 C14 C15 120.2(7) . . ? C14 C15 C16 120.4(7) . . ? C11 C16 C15 119.4(7) . . ? C22 C21 C26 118.6(6) . . ? C22 C21 P1 121.4(5) . . ? C26 C21 P1 119.8(5) . . ? C23 C22 C21 120.9(6) . . ? C22 C23 C24 120.4(7) . . ? C25 C24 C23 118.4(7) . . ? C26 C25 C24 121.6(7) . . ? C25 C26 C21 119.9(6) . . ? C3 C2 P1 108.1(4) . . ? C2 C3 P4 107.4(4) . . ? C31 P4 C41 102.3(3) . . ? C31 P4 C3 103.1(3) . . ? C41 P4 C3 103.5(3) . . ? C31 P4 W1 121.84(19) . . ? C41 P4 W1 116.95(19) . . ? C3 P4 W1 106.93(19) . . ? C36 C31 C32 118.8(6) . . ? C36 C31 P4 120.8(5) . . ? C32 C31 P4 120.3(5) . . ? C31 C36 C35 120.4(6) . . ? C36 C35 C34 120.0(6) . . ? C33 C34 C35 120.2(6) . . ? C33 C32 C31 120.6(6) . . ? C34 C33 C32 119.9(7) . . ? C42 C41 C46 117.7(6) . . ? C42 C41 P4 119.3(5) . . ? C46 C41 P4 122.9(5) . . ? C44 C45 C46 120.1(6) . . ? C41 C42 C43 121.6(6) . . ? C44 C43 C42 119.6(6) . . ? C43 C44 C45 119.9(6) . . ? C45 C46 C41 121.0(7) . . ? C51 P5 C61 102.8(3) . . ? C51 P5 C6 102.6(3) . . ? C61 P5 C6 102.8(3) . . ? C51 P5 W1 117.43(19) . . ? C61 P5 W1 122.10(19) . . ? C6 P5 W1 106.52(19) . . ? C7 C6 P5 107.0(4) . . ? C6 C7 P8 107.6(4) . . ? C71 P8 C81 103.2(2) . . ? C71 P8 C7 101.0(3) . . ? C81 P8 C7 103.3(2) . . ? C71 P8 W1 124.32(18) . . ? C81 P8 W1 114.56(14) . . ? C7 P8 W1 107.87(19) . . ? C56 C51 C52 118.1(5) . . ? C56 C51 P5 122.2(5) . . ? C52 C51 P5 119.6(4) . . ? C53 C52 C51 121.3(6) . . ? C52 C53 C54 119.6(6) . . ? C55 C54 C53 120.3(6) . . ? C54 C55 C56 120.4(6) . . ? C51 C56 C55 120.4(6) . . ? C66 C61 C62 118.5(5) . . ? C66 C61 P5 119.0(4) . . ? C62 C61 P5 122.5(5) . . ? C63 C62 C61 119.9(6) . . ? C64 C63 C62 121.3(6) . . ? C63 C64 C65 119.1(6) . . ? C64 C65 C66 120.3(6) . . ? C61 C66 C65 120.8(6) . . ? C76 C71 C72 118.9(5) . . ? C76 C71 P8 120.8(4) . . ? C72 C71 P8 120.3(5) . . ? C75 C76 C71 120.9(6) . . ? C74 C75 C76 120.4(6) . . ? C71 C72 C73 119.7(6) . . ? C74 C73 C72 120.5(6) . . ? C75 C74 C73 119.6(6) . . ? C82 C81 C86 120.0 . . ? C82 C81 P8 118.3(2) . . ? C86 C81 P8 121.7(2) . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? N101 N100 W1 168.9(4) . . ? N100 N101 C102 124.3(6) . . ? N103 C102 N101 170.8(7) . . ? C102 N103 ZN1 154.2(6) . . ? N103 ZN1 N103 179.999(2) 2_677 . ? N103 ZN1 O95 86.4(2) 2_677 . ? N103 ZN1 O95 93.6(2) . . ? N103 ZN1 O95 93.6(2) 2_677 2_677 ? N103 ZN1 O95 86.4(2) . 2_677 ? O95 ZN1 O95 180.00(5) . 2_677 ? N103 ZN1 O91 92.6(2) 2_677 2_677 ? N103 ZN1 O91 87.4(2) . 2_677 ? O95 ZN1 O91 92.69(18) . 2_677 ? O95 ZN1 O91 87.31(18) 2_677 2_677 ? N103 ZN1 O91 87.4(2) 2_677 . ? N103 ZN1 O91 92.6(2) . . ? O95 ZN1 O91 87.31(18) . . ? O95 ZN1 O91 92.69(18) 2_677 . ? O91 ZN1 O91 179.998(2) 2_677 . ? C92 O91 ZN1 123.4(4) . . ? O91 C92 C93 128.7(6) . . ? O91 C92 C921 115.0(6) . . ? C93 C92 C921 116.3(6) . . ? C94 C93 C92 123.2(6) . . ? O95 C94 C93 128.5(6) . . ? O95 C94 C941 113.7(5) . . ? C93 C94 C941 117.8(6) . . ? C94 O95 ZN1 123.7(4) . . ? F924 C921 F923 112.1(12) . . ? F927 C921 F926 112.5(11) . . ? F927 C921 F925 108.2(11) . . ? F926 C921 F925 104.5(10) . . ? F924 C921 F922 106.8(11) . . ? F923 C921 F922 105.1(10) . . ? F927 C921 C92 113.3(8) . . ? F924 C921 C92 115.1(7) . . ? F923 C921 C92 111.3(9) . . ? F926 C921 C92 110.9(9) . . ? F925 C921 C92 106.8(7) . . ? F922 C921 C92 105.6(8) . . ? F944 C941 F943 109.2(6) . . ? F947 C941 F946 109.9(7) . . ? F944 C941 F942 106.4(6) . . ? F943 C941 F942 106.4(6) . . ? F947 C941 F945 106.5(7) . . ? F946 C941 F945 107.8(7) . . ? F947 C941 C94 116.0(7) . . ? F944 C941 C94 110.5(6) . . ? F943 C941 C94 113.4(6) . . ? F946 C941 C94 107.8(6) . . ? F942 C941 C94 110.7(6) . . ? F945 C941 C94 108.6(6) . . ? C114 C111 C112 120.5(8) 2_468 . ? C113 C111 C112 120.5(8) 2_468 . ? C114 C112 C111 120.8(8) . . ? C113 C112 C111 120.8(8) . . ? C111 C113 C112 118.7(7) 2_468 . ? C111 C114 C112 118.7(7) 2_468 . ? C111 C114 C115 121.6(10) 2_468 . ? C112 C114 C115 119.7(10) . . ? C122 C121 C126 116.0(10) . . ? C122 C121 C127 122.5(11) . . ? C126 C121 C127 121.4(9) . . ? C121 C122 C123 123.1(15) . . ? C122 C123 C124 120.4(16) . . ? C125 C124 C123 118.0(12) . . ? C124 C125 C126 120.0(10) . . ? C121 C126 C125 122.1(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.320 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.148 _publ_section_references ; Hooft, R., Bruker-Nonius Ltd, (1998) COLLECT Program. Otwinowski, Z., and Minor.W., (1997) DENZO program. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands Blessing, R.H., SORTAV program, J.Appl.Cryst. 1997 30 421-426. ; #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 641376' _audit_creation_date 07-14-03 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================================== _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 13.4062(3) _cell_angle_alpha 94.185(1) _cell_length_b 13.6587(3) _cell_angle_beta 110.576(1) _cell_length_c 16.5249(5) _cell_angle_gamma 105.6456(13) _cell_volume 2680.26(12) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B #The carbon atoms of one of the phenyl rings have large temperature #factors indicative of thermal motion. _cell_formula_units_Z 2 _chemical_formula_sum ' C54 H53 B Br Cl2 F4 N3 O P4 W ' _chemical_formula_moiety ; ' C53 H51 Br N3 O P4 W, 0.5(C2 H4 Cl4), B F4 ' ; _chemical_compound_source ; ? ; _chemical_formula_weight 1305.39 _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange-red ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1300.000 _exptl_absorpt_coefficient_mu 3.175 # Sheldrick geometric definitions 0.54 0.63 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.63 _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 20719 _reflns_number_total 12141 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 12141 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12334 _diffrn_reflns_theta_min 5.108 _diffrn_reflns_theta_max 27.516 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.828 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.26 _refine_diff_density_max 2.32 _refine_ls_number_reflns 6454 _refine_ls_number_parameters 617 #_refine_ls_R_factor_ref 0.0530 _refine_ls_wR_factor_ref 0.0584 _refine_ls_goodness_of_fit_ref 1.1188 #_reflns_number_all 12141 _refine_ls_R_factor_all 0.1152 _refine_ls_wR_factor_all 0.1075 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6454 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_gt 0.0583 _refine_ls_shift/su_max 0.001228 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 0.516 0.958E-01 0.280 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens W1 W 0.83799(3) 0.30666(3) 0.69940(3) 0.0204 1.0000 Uani . P1 P 0.88145(19) 0.50147(18) 0.74549(15) 0.0250 1.0000 Uani . P2 P 1.01077(19) 0.34464(18) 0.83976(15) 0.0256 1.0000 Uani . P3 P 0.8214(2) 0.12256(18) 0.64749(16) 0.0272 1.0000 Uani . P4 P 0.67232(19) 0.26379(18) 0.55226(15) 0.0248 1.0000 Uani . Br1 Br 0.96066(8) 0.34257(8) 0.60838(6) 0.0341 1.0000 Uani . B1 B 0.5643(8) 0.9850(8) 0.2455(7) 0.0539 1.0000 Uani . O1 O 0.7638(7) 0.3822(6) 0.9134(5) 0.0527 1.0000 Uani . N1 N 0.7464(6) 0.2781(5) 0.7590(5) 0.0252 1.0000 Uani . N2 N 0.6748(8) 0.2523(7) 0.7930(5) 0.0429 1.0000 Uani . N3 N 0.5866(9) 0.2816(8) 0.8851(7) 0.0579 1.0000 Uani . C1 C 1.0082(8) 0.5452(7) 0.8478(6) 0.0310 1.0000 Uani . C2 C 1.0125(7) 0.4615(7) 0.9046(6) 0.0271 1.0000 Uani . C3 C 0.7350(8) 0.0887(7) 0.5293(6) 0.0317 1.0000 Uani . C4 C 0.6340(8) 0.1246(7) 0.5133(6) 0.0321 1.0000 Uani . C5 C 0.6906(7) 0.3257(7) 0.4618(6) 0.0287 1.0000 Uani . C6 C 0.7542(9) 0.4290(8) 0.4803(7) 0.0363 1.0000 Uani . C7 C 0.7681(9) 0.4790(8) 0.4129(8) 0.0423 1.0000 Uani . C8 C 0.7161(9) 0.426(1) 0.3260(8) 0.0443 1.0000 Uani . C9 C 0.652(1) 0.3230(9) 0.3073(7) 0.0467 1.0000 Uani . C10 C 0.6384(9) 0.2728(9) 0.3741(7) 0.0431 1.0000 Uani . C11 C 0.5387(7) 0.2763(7) 0.5486(6) 0.0303 1.0000 Uani . C12 C 0.4900(8) 0.3448(8) 0.5039(6) 0.0326 1.0000 Uani . C13 C 0.3897(9) 0.3537(9) 0.5050(7) 0.0451 1.0000 Uani . C14 C 0.336(1) 0.292(1) 0.5500(8) 0.0493 1.0000 Uani . C15 C 0.383(1) 0.222(1) 0.5960(8) 0.0494 1.0000 Uani . C16 C 0.4828(8) 0.2145(9) 0.5944(7) 0.0393 1.0000 Uani . C17 C 0.9459(9) 0.0873(8) 0.6561(7) 0.0427 1.0000 Uani . C18 C 0.992(1) 0.101(1) 0.5921(9) 0.0574 1.0000 Uani . C19 C 1.0893(12) 0.0795(12) 0.6019(14) 0.0820 1.0000 Uani . C20 C 1.1437(12) 0.0456(13) 0.674(2) 0.1024 1.0000 Uani . C21 C 1.1005(13) 0.0312(13) 0.7435(15) 0.0942 1.0000 Uani . C22 C 1.001(1) 0.051(1) 0.732(1) 0.0591 1.0000 Uani . C23 C 0.7525(8) 0.0232(7) 0.6952(6) 0.0268 1.0000 Uani . C24 C 0.7022(9) -0.0795(7) 0.6530(6) 0.0359 1.0000 Uani . C25 C 0.662(1) -0.1563(8) 0.6967(7) 0.0453 1.0000 Uani . C26 C 0.6727(11) -0.1296(8) 0.7827(8) 0.0460 1.0000 Uani . C27 C 0.725(1) -0.0283(9) 0.8253(7) 0.0472 1.0000 Uani . C28 C 0.7641(9) 0.0488(7) 0.7823(7) 0.0385 1.0000 Uani . C29 C 0.7708(7) 0.5313(7) 0.7719(6) 0.0263 1.0000 Uani . C30 C 0.7906(9) 0.5890(9) 0.8532(7) 0.0426 1.0000 Uani . C31 C 0.7018(9) 0.613(1) 0.8657(7) 0.0450 1.0000 Uani . C32 C 0.5964(9) 0.5811(8) 0.8019(8) 0.0426 1.0000 Uani . C33 C 0.5768(8) 0.5237(9) 0.7219(8) 0.0474 1.0000 Uani . C34 C 0.6641(9) 0.4997(9) 0.7083(7) 0.0438 1.0000 Uani . C35 C 0.9211(8) 0.6047(7) 0.6872(6) 0.0302 1.0000 Uani . C36 C 0.8756(8) 0.6850(8) 0.6780(7) 0.0377 1.0000 Uani . C37 C 0.916(1) 0.7675(9) 0.6417(9) 0.0512 1.0000 Uani . C38 C 1.0006(11) 0.769(1) 0.6135(8) 0.0536 1.0000 Uani . C39 C 1.049(1) 0.6918(8) 0.6218(8) 0.0443 1.0000 Uani . C40 C 1.0103(8) 0.6110(7) 0.6600(7) 0.0379 1.0000 Uani . C41 C 1.1527(8) 0.3758(7) 0.8406(6) 0.0304 1.0000 Uani . C42 C 1.1754(8) 0.3158(8) 0.7828(7) 0.0344 1.0000 Uani . C43 C 1.2846(9) 0.3315(9) 0.7871(8) 0.0438 1.0000 Uani . C44 C 1.3722(9) 0.4095(9) 0.8500(8) 0.0447 1.0000 Uani . C45 C 1.3505(8) 0.4722(9) 0.9076(8) 0.0473 1.0000 Uani . C46 C 1.2423(8) 0.4579(8) 0.9035(7) 0.0393 1.0000 Uani . C47 C 1.0179(8) 0.2568(7) 0.9188(6) 0.0311 1.0000 Uani . C48 C 0.9412(9) 0.2452(8) 0.9619(6) 0.0399 1.0000 Uani . C49 C 0.9467(11) 0.183(1) 1.0246(7) 0.0531 1.0000 Uani . C50 C 1.0247(15) 0.131(1) 1.0429(8) 0.0662 1.0000 Uani . C51 C 1.0969(12) 0.140(1) 1.0011(9) 0.0571 1.0000 Uani . C52 C 1.093(1) 0.2028(8) 0.9389(7) 0.0432 1.0000 Uani . C53 C 0.6802(9) 0.3112(8) 0.8670(7) 0.0383 1.0000 Uani . F1 F 0.4913(7) 0.9603(7) 0.2892(6) 0.080(2) 1.0000 Uiso . F2 F 0.6644(9) 1.0566(9) 0.3082(7) 0.114(4) 1.0000 Uiso . F3 F 0.5892(9) 0.8955(8) 0.2208(7) 0.102(3) 1.0000 Uiso . F4 F 0.5115(14) 1.0110(14) 0.1633(9) 0.172(6) 1.0000 Uiso . Cl1 Cl 0.2871(4) -0.2672(4) 0.8897(4) 0.0415(12) 0.5000 Uiso . Cl2 Cl 0.3034(7) -0.0565(7) 0.9303(6) 0.080(2) 0.5000 Uiso . Cl3 Cl 0.4293(5) 0.2340(5) 1.0192(4) 0.0551(14) 0.5000 Uiso . Cl4 Cl 0.2994(7) 0.0121(7) 0.9542(6) 0.076(2) 0.5000 Uiso . C54 C 0.244(2) -0.165(1) 0.8420(9) 0.059(6) 0.5000 Uiso . C55 C 0.4331(11) 0.1065(8) 1.0059(16) 0.057(6) 0.5000 Uiso . H11 H 1.0079 0.6086 0.8819 0.0348 1.0000 Uiso . H12 H 1.0761 0.5619 0.8326 0.0348 1.0000 Uiso . H21 H 1.0828 0.4863 0.9590 0.0297 1.0000 Uiso . H22 H 0.9458 0.4451 0.9213 0.0297 1.0000 Uiso . H31 H 0.7794 0.1237 0.4961 0.0371 1.0000 Uiso . H32 H 0.7101 0.0120 0.5094 0.0371 1.0000 Uiso . H41 H 0.5887 0.0865 0.5448 0.0304 1.0000 Uiso . H42 H 0.5878 0.1083 0.4487 0.0304 1.0000 Uiso . H61 H 0.7901 0.4678 0.5424 0.0458 1.0000 Uiso . H71 H 0.8155 0.5532 0.4267 0.0566 1.0000 Uiso . H81 H 0.7255 0.4619 0.2774 0.0608 1.0000 Uiso . H91 H 0.6142 0.2848 0.2450 0.0546 1.0000 Uiso . H101 H 0.5915 0.1984 0.3601 0.0500 1.0000 Uiso . H121 H 0.5280 0.3883 0.4704 0.0360 1.0000 Uiso . H131 H 0.3565 0.4042 0.4734 0.0502 1.0000 Uiso . H141 H 0.2628 0.2977 0.5497 0.0571 1.0000 Uiso . H151 H 0.3447 0.1792 0.6293 0.0558 1.0000 Uiso . H161 H 0.5160 0.1642 0.6262 0.0459 1.0000 Uiso . H181 H 0.9531 0.1264 0.5384 0.0670 1.0000 Uiso . H191 H 1.1204 0.0893 0.5551 0.0911 1.0000 Uiso . H201 H 1.2145 0.0300 0.6803 0.1169 1.0000 Uiso . H211 H 1.1415 0.0077 0.7978 0.0976 1.0000 Uiso . H221 H 0.9673 0.0396 0.7769 0.0654 1.0000 Uiso . H241 H 0.6944 -0.0993 0.5911 0.0404 1.0000 Uiso . H251 H 0.6258 -0.2301 0.6657 0.0475 1.0000 Uiso . H261 H 0.6425 -0.1836 0.8133 0.0543 1.0000 Uiso . H271 H 0.7355 -0.0093 0.8880 0.0523 1.0000 Uiso . H281 H 0.8004 0.1224 0.8139 0.0449 1.0000 Uiso . H301 H 0.8672 0.6125 0.9013 0.0498 1.0000 Uiso . H311 H 0.7160 0.6551 0.9231 0.0543 1.0000 Uiso . H321 H 0.5338 0.5987 0.8126 0.0541 1.0000 Uiso . H331 H 0.4999 0.4999 0.6743 0.0506 1.0000 Uiso . H341 H 0.6490 0.4582 0.6504 0.0496 1.0000 Uiso . H361 H 0.8129 0.6835 0.6979 0.0440 1.0000 Uiso . H371 H 0.8837 0.8257 0.6362 0.0633 1.0000 Uiso . H381 H 1.0279 0.8277 0.5861 0.0620 1.0000 Uiso . H391 H 1.1110 0.6941 0.6007 0.0562 1.0000 Uiso . H401 H 1.0468 0.5555 0.6685 0.0400 1.0000 Uiso . H421 H 1.1121 0.2595 0.7367 0.0401 1.0000 Uiso . H431 H 1.2992 0.2865 0.7449 0.0568 1.0000 Uiso . H441 H 1.4509 0.4210 0.8543 0.0548 1.0000 Uiso . H451 H 1.4144 0.5288 0.9529 0.0502 1.0000 Uiso . H461 H 1.2277 0.5048 0.9443 0.0448 1.0000 Uiso . H481 H 0.8838 0.2820 0.9470 0.0441 1.0000 Uiso . H491 H 0.8945 0.1752 1.0562 0.0570 1.0000 Uiso . H501 H 1.0282 0.0852 1.0879 0.0739 1.0000 Uiso . H511 H 1.1528 0.1017 1.0154 0.0693 1.0000 Uiso . H521 H 1.1458 0.2087 0.9080 0.0508 1.0000 Uiso . H541 H 0.1604 -0.1842 0.8164 0.0709 0.5000 Uiso . H542 H 0.2735 -0.1488 0.7949 0.0709 0.5000 Uiso . H551 H 0.4709 0.0914 1.0653 0.0687 0.5000 Uiso . H552 H 0.4778 0.1012 0.9694 0.0687 0.5000 Uiso . H23 H 0.6192 0.1945 0.7688 0.0479 1.0000 Uiso . H33 H 0.5833 0.3150 0.9307 0.0675 1.0000 Uiso . H34 H 0.5291 0.2292 0.8512 0.0675 1.0000 Uiso . 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 0.02072(18) 0.01967(18) 0.01843(17) 0.00049(12) 0.00657(13) 0.00484(12) P1 0.0236(12) 0.0234(11) 0.0254(12) -0.0002(9) 0.009(1) 0.0050(9) P2 0.0245(12) 0.0263(12) 0.0220(11) -0.0004(9) 0.0065(9) 0.0066(9) P3 0.0272(12) 0.0252(12) 0.0255(12) -0.0000(9) 0.007(1) 0.008(1) P4 0.0233(12) 0.0252(12) 0.0202(11) 0.0018(9) 0.0052(9) 0.0040(9) Br1 0.0329(5) 0.0399(6) 0.0314(5) 0.0045(4) 0.0171(4) 0.0089(4) B1 0.019(6) 0.066(9) 0.07(1) 0.037(8) 0.007(6) 0.012(6) O1 0.056(5) 0.048(5) 0.048(5) -0.008(4) 0.028(4) 0.002(4) N1 0.023(4) 0.012(3) 0.030(4) 0.005(3) -0.000(3) 0.003(3) N2 0.054(6) 0.046(5) 0.019(4) -0.012(4) 0.004(4) 0.020(5) N3 0.057(6) 0.060(7) 0.053(6) -0.006(5) 0.032(5) 0.004(5) C1 0.027(5) 0.024(4) 0.037(5) -0.009(4) 0.009(4) 0.006(4) C2 0.029(5) 0.022(4) 0.024(4) -0.004(3) 0.003(4) 0.009(4) C3 0.039(5) 0.023(4) 0.030(5) -0.004(4) 0.011(4) 0.011(4) C4 0.029(5) 0.025(5) 0.021(5) -0.004(4) -0.004(4) -0.003(4) C5 0.025(5) 0.030(5) 0.032(5) 0.008(4) 0.010(4) 0.011(4) C6 0.041(6) 0.029(5) 0.044(6) 0.016(4) 0.018(5) 0.016(4) C7 0.044(6) 0.040(6) 0.057(7) 0.024(5) 0.029(6) 0.020(5) C8 0.045(6) 0.062(7) 0.045(6) 0.029(6) 0.026(5) 0.030(6) C9 0.058(7) 0.045(6) 0.034(6) 0.007(5) 0.015(5) 0.015(5) C10 0.041(6) 0.052(7) 0.031(5) 0.006(5) 0.013(5) 0.010(5) C11 0.023(5) 0.035(5) 0.024(5) -0.003(4) 0.005(4) 0.004(4) C12 0.028(5) 0.034(5) 0.028(5) 0.005(4) 0.008(4) 0.002(4) C13 0.042(6) 0.041(6) 0.043(6) 0.003(5) 0.006(5) 0.013(5) C14 0.038(6) 0.054(7) 0.050(7) -0.002(6) 0.017(5) 0.010(5) C15 0.044(7) 0.047(7) 0.049(7) -0.002(6) 0.026(6) -0.007(5) C16 0.026(5) 0.051(6) 0.039(6) 0.009(5) 0.011(4) 0.009(4) C17 0.035(6) 0.032(5) 0.045(6) -0.018(5) 0.004(5) 0.007(4) C18 0.043(6) 0.057(7) 0.068(8) -0.031(6) 0.031(6) 0.007(5) C19 0.038(7) 0.063(9) 0.127(15) -0.04(1) 0.034(9) -0.001(7) C20 0.031(7) 0.06(1) 0.20(2) -0.022(12) 0.036(12) 0.015(7) C21 0.046(8) 0.07(1) 0.132(16) 0.01(1) -0.02(1) 0.027(7) C22 0.043(7) 0.043(7) 0.078(9) 0.011(6) 0.005(6) 0.017(5) C23 0.027(5) 0.021(4) 0.027(5) 0.005(4) 0.006(4) 0.005(4) C24 0.040(5) 0.028(5) 0.033(5) -0.002(4) 0.008(4) 0.011(4) C25 0.059(7) 0.020(5) 0.040(6) 0.003(4) 0.006(5) 0.004(5) C26 0.063(7) 0.028(5) 0.046(6) 0.013(5) 0.020(6) 0.011(5) C27 0.055(7) 0.043(6) 0.033(6) 0.006(5) 0.009(5) 0.009(5) C28 0.057(7) 0.021(4) 0.034(5) 0.007(4) 0.010(5) 0.016(4) C29 0.024(4) 0.021(4) 0.030(5) 0.005(4) 0.009(4) 0.005(3) C30 0.036(6) 0.053(7) 0.036(6) -0.004(5) 0.010(5) 0.017(5) C31 0.037(6) 0.066(7) 0.033(5) -0.001(5) 0.013(5) 0.021(5) C32 0.042(6) 0.030(5) 0.062(7) 0.001(5) 0.031(6) 0.010(5) C33 0.024(5) 0.046(6) 0.057(7) -0.009(5) 0.005(5) 0.006(4) C34 0.035(6) 0.052(7) 0.037(6) -0.009(5) 0.008(5) 0.015(5) C35 0.038(5) 0.027(5) 0.027(5) 0.003(4) 0.016(4) 0.008(4) C36 0.033(5) 0.034(5) 0.043(6) 0.006(4) 0.012(5) 0.009(4) C37 0.054(7) 0.040(6) 0.064(8) 0.026(6) 0.022(6) 0.018(5) C38 0.058(8) 0.047(7) 0.050(7) 0.016(6) 0.018(6) 0.010(6) C39 0.053(7) 0.036(6) 0.051(7) 0.012(5) 0.037(6) 0.002(5) C40 0.033(5) 0.022(5) 0.044(6) 0.003(4) 0.011(5) -0.007(4) C41 0.030(5) 0.029(5) 0.028(5) 0.005(4) 0.007(4) 0.010(4) C42 0.029(5) 0.032(5) 0.039(5) 0.003(4) 0.012(4) 0.007(4) C43 0.039(6) 0.049(7) 0.054(7) 0.014(5) 0.025(5) 0.020(5) C44 0.026(5) 0.058(7) 0.053(7) 0.017(6) 0.012(5) 0.020(5) C45 0.016(5) 0.047(6) 0.063(7) 0.004(5) 0.002(5) 0.004(4) C46 0.032(5) 0.039(6) 0.041(6) -0.003(4) 0.006(4) 0.015(4) C47 0.037(5) 0.028(5) 0.018(4) 0.005(4) 0.006(4) 0.001(4) C48 0.052(6) 0.038(6) 0.020(5) 0.006(4) 0.009(4) 0.006(5) C49 0.069(8) 0.045(7) 0.028(6) -0.002(5) 0.020(6) -0.008(6) C50 0.111(12) 0.037(6) 0.037(7) 0.022(5) 0.014(7) 0.018(7) C51 0.074(9) 0.048(7) 0.051(7) 0.027(6) 0.019(7) 0.025(6) C52 0.052(7) 0.036(6) 0.040(6) 0.014(5) 0.012(5) 0.015(5) C53 0.034(5) 0.039(6) 0.050(6) 0.009(5) 0.024(5) 0.014(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . P1 . 2.560(2) yes W1 . P2 . 2.533(2) yes W1 . P3 . 2.521(2) yes W1 . P4 . 2.546(2) yes W1 . Br1 . 2.573(1) yes W1 . N1 . 1.810(8) yes P1 . C1 . 1.841(9) yes P1 . C29 . 1.820(9) yes P1 . C35 . 1.83(1) yes P2 . C2 . 1.846(8) yes P2 . C41 . 1.83(1) yes P2 . C47 . 1.832(9) yes P3 . C3 . 1.83(1) yes P3 . C17 . 1.820(11) yes P3 . C23 . 1.818(9) yes P4 . C4 . 1.832(9) yes P4 . C5 . 1.83(1) yes P4 . C11 . 1.825(9) yes B1 . F1 . 1.396(8) yes B1 . F2 . 1.413(9) yes B1 . F3 . 1.419(9) yes B1 . F4 . 1.415(9) yes O1 . C53 . 1.219(13) yes N1 . N2 . 1.260(12) yes N2 . C53 . 1.381(13) yes N2 . H23 . 0.875 no N3 . C53 . 1.355(14) yes N3 . H33 . 0.872 no N3 . H34 . 0.872 no C1 . C2 . 1.532(14) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.505(14) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . C6 . 1.384(13) yes C5 . C10 . 1.404(14) yes C6 . C7 . 1.390(15) yes C6 . H61 . 1.000 no C7 . C8 . 1.395(17) yes C7 . H71 . 1.000 no C8 . C9 . 1.381(17) yes C8 . H81 . 1.000 no C9 . C10 . 1.380(16) yes C9 . H91 . 1.000 no C10 . H101 . 1.000 no C11 . C12 . 1.392(14) yes C11 . C16 . 1.414(14) yes C12 . C13 . 1.389(15) yes C12 . H121 . 1.000 no C13 . C14 . 1.385(17) yes C13 . H131 . 1.000 no C14 . C15 . 1.408(18) yes C14 . H141 . 1.000 no C15 . C16 . 1.379(16) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.400(17) yes C17 . C22 . 1.407(18) yes C18 . C19 . 1.371(19) yes C18 . H181 . 1.000 no C19 . C20 . 1.35(3) yes C19 . H191 . 1.000 no C20 . C21 . 1.46(3) yes C20 . H201 . 1.000 no C21 . C22 . 1.39(2) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.388(13) yes C23 . C28 . 1.399(14) yes C24 . C25 . 1.411(15) yes C24 . H241 . 1.000 no C25 . C26 . 1.387(16) yes C25 . H251 . 1.000 no C26 . C27 . 1.375(15) yes C26 . H261 . 1.000 no C27 . C28 . 1.400(15) yes C27 . H271 . 1.000 no C28 . H281 . 1.000 no C29 . C30 . 1.407(14) yes C29 . C34 . 1.372(14) yes C30 . C31 . 1.393(14) yes C30 . H301 . 1.000 no C31 . C32 . 1.361(15) yes C31 . H311 . 1.000 no C32 . C33 . 1.388(16) yes C32 . H321 . 1.000 no C33 . C34 . 1.381(15) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no C35 . C36 . 1.385(14) yes C35 . C40 . 1.403(14) yes C36 . C37 . 1.387(15) yes C36 . H361 . 1.000 no C37 . C38 . 1.363(18) yes C37 . H371 . 1.000 no C38 . C39 . 1.369(17) yes C38 . H381 . 1.000 no C39 . C40 . 1.383(14) yes C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . C42 . 1.378(13) yes C41 . C46 . 1.417(14) yes C42 . C43 . 1.396(14) yes C42 . H421 . 1.000 no C43 . C44 . 1.379(16) yes C43 . H431 . 1.000 no C44 . C45 . 1.389(16) yes C44 . H441 . 1.000 no C45 . C46 . 1.387(14) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C47 . C48 . 1.426(15) yes C47 . C52 . 1.367(15) yes C48 . C49 . 1.385(16) yes C48 . H481 . 1.000 no C49 . C50 . 1.38(2) yes C49 . H491 . 1.000 no C50 . C51 . 1.36(2) yes C50 . H501 . 1.000 no C51 . C52 . 1.381(16) yes C51 . H511 . 1.000 no C52 . H521 . 1.000 no Cl2 . Cl4 . 1.01(1) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no C55 . H551 . 1.000 no C55 . H552 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . W1 . P2 . 79.53(8) yes P1 . W1 . P3 . 171.06(7) yes P2 . W1 . P3 . 97.83(8) yes P1 . W1 . P4 . 102.59(8) yes P2 . W1 . P4 . 175.73(8) yes P3 . W1 . P4 . 79.51(8) yes P1 . W1 . Br1 . 90.06(6) yes P2 . W1 . Br1 . 90.91(6) yes P3 . W1 . Br1 . 81.42(6) yes P4 . W1 . Br1 . 85.40(6) yes P1 . W1 . N1 . 91.3(2) yes P2 . W1 . N1 . 91.5(2) yes P3 . W1 . N1 . 97.3(2) yes P4 . W1 . N1 . 92.2(2) yes Br1 . W1 . N1 . 177.4(2) yes W1 . P1 . C1 . 107.2(3) yes W1 . P1 . C29 . 112.1(3) yes C1 . P1 . C29 . 106.2(4) yes W1 . P1 . C35 . 128.0(3) yes C1 . P1 . C35 . 98.3(4) yes C29 . P1 . C35 . 102.7(4) yes W1 . P2 . C2 . 104.4(3) yes W1 . P2 . C41 . 122.5(3) yes C2 . P2 . C41 . 104.3(4) yes W1 . P2 . C47 . 120.8(3) yes C2 . P2 . C47 . 101.1(4) yes C41 . P2 . C47 . 100.7(5) yes W1 . P3 . C3 . 107.5(3) yes W1 . P3 . C17 . 120.5(3) yes C3 . P3 . C17 . 103.7(5) yes W1 . P3 . C23 . 116.9(3) yes C3 . P3 . C23 . 105.0(4) yes C17 . P3 . C23 . 101.5(5) yes W1 . P4 . C4 . 106.1(3) yes W1 . P4 . C5 . 119.2(3) yes C4 . P4 . C5 . 105.8(4) yes W1 . P4 . C11 . 119.6(3) yes C4 . P4 . C11 . 101.7(4) yes C5 . P4 . C11 . 102.5(4) yes F1 . B1 . F2 . 105.4(9) yes F1 . B1 . F3 . 109.8(9) yes F2 . B1 . F3 . 108.1(9) yes F1 . B1 . F4 . 111.3(10) yes F2 . B1 . F4 . 119.5(12) yes F3 . B1 . F4 . 102.5(11) yes W1 . N1 . N2 . 174.0(6) yes N1 . N2 . C53 . 122.9(9) yes N1 . N2 . H23 . 118.636 no C53 . N2 . H23 . 118.472 no C53 . N3 . H33 . 120.253 no C53 . N3 . H34 . 120.226 no H33 . N3 . H34 . 119.521 no P1 . C1 . C2 . 111.2(6) yes P1 . C1 . H11 . 109.037 no C2 . C1 . H11 . 109.011 no P1 . C1 . H12 . 109.038 no C2 . C1 . H12 . 109.018 no H11 . C1 . H12 . 109.469 no P2 . C2 . C1 . 108.2(6) yes P2 . C2 . H21 . 109.783 no C1 . C2 . H21 . 109.790 no P2 . C2 . H22 . 109.773 no C1 . C2 . H22 . 109.776 no H21 . C2 . H22 . 109.485 no P3 . C3 . C4 . 108.3(6) yes P3 . C3 . H31 . 109.759 no C4 . C3 . H31 . 109.752 no P3 . C3 . H32 . 109.771 no C4 . C3 . H32 . 109.775 no H31 . C3 . H32 . 109.471 no P4 . C4 . C3 . 112.6(6) yes P4 . C4 . H41 . 108.677 no C3 . C4 . H41 . 108.669 no P4 . C4 . H42 . 108.695 no C3 . C4 . H42 . 108.689 no H41 . C4 . H42 . 109.455 no P4 . C5 . C6 . 118.6(7) yes P4 . C5 . C10 . 121.9(7) yes C6 . C5 . C10 . 119.4(9) yes C5 . C6 . C7 . 120.1(10) yes C5 . C6 . H61 . 119.951 no C7 . C6 . H61 . 119.916 no C6 . C7 . C8 . 120.1(10) yes C6 . C7 . H71 . 119.940 no C8 . C7 . H71 . 119.940 no C7 . C8 . C9 . 119.8(10) yes C7 . C8 . H81 . 120.117 no C9 . C8 . H81 . 120.122 no C8 . C9 . C10 . 120.3(10) yes C8 . C9 . H91 . 119.845 no C10 . C9 . H91 . 119.811 no C5 . C10 . C9 . 120.2(10) yes C5 . C10 . H101 . 119.878 no C9 . C10 . H101 . 119.876 no P4 . C11 . C12 . 123.2(7) yes P4 . C11 . C16 . 118.4(7) yes C12 . C11 . C16 . 118.4(9) yes C11 . C12 . C13 . 121.1(9) yes C11 . C12 . H121 . 119.417 no C13 . C12 . H121 . 119.448 no C12 . C13 . C14 . 119.7(10) yes C12 . C13 . H131 . 120.168 no C14 . C13 . H131 . 120.171 no C13 . C14 . C15 . 120.6(10) yes C13 . C14 . H141 . 119.713 no C15 . C14 . H141 . 119.715 no C14 . C15 . C16 . 119.1(11) yes C14 . C15 . H151 . 120.432 no C16 . C15 . H151 . 120.426 no C11 . C16 . C15 . 121.0(10) yes C11 . C16 . H161 . 119.490 no C15 . C16 . H161 . 119.477 no P3 . C17 . C18 . 121.6(10) yes P3 . C17 . C22 . 119.0(10) yes C18 . C17 . C22 . 119.3(11) yes C17 . C18 . C19 . 121.0(16) yes C17 . C18 . H181 . 119.481 no C19 . C18 . H181 . 119.482 no C18 . C19 . C20 . 120.5(17) yes C18 . C19 . H191 . 119.700 no C20 . C19 . H191 . 119.764 no C19 . C20 . C21 . 120.8(13) yes C19 . C20 . H201 . 119.534 no C21 . C20 . H201 . 119.630 no C20 . C21 . C22 . 117.7(16) yes C20 . C21 . H211 . 121.067 no C22 . C21 . H211 . 121.195 no C17 . C22 . C21 . 120.6(16) yes C17 . C22 . H221 . 119.741 no C21 . C22 . H221 . 119.708 no P3 . C23 . C24 . 122.5(7) yes P3 . C23 . C28 . 118.3(7) yes C24 . C23 . C28 . 118.7(9) yes C23 . C24 . C25 . 120.6(9) yes C23 . C24 . H241 . 119.680 no C25 . C24 . H241 . 119.696 no C24 . C25 . C26 . 120.1(9) yes C24 . C25 . H251 . 119.960 no C26 . C25 . H251 . 119.930 no C25 . C26 . C27 . 119.3(10) yes C25 . C26 . H261 . 120.337 no C27 . C26 . H261 . 120.348 no C26 . C27 . C28 . 121.1(10) yes C26 . C27 . H271 . 119.442 no C28 . C27 . H271 . 119.475 no C23 . C28 . C27 . 120.2(9) yes C23 . C28 . H281 . 119.930 no C27 . C28 . H281 . 119.899 no P1 . C29 . C30 . 123.0(7) yes P1 . C29 . C34 . 118.5(7) yes C30 . C29 . C34 . 118.5(9) yes C29 . C30 . C31 . 118.9(9) yes C29 . C30 . H301 . 120.525 no C31 . C30 . H301 . 120.550 no C30 . C31 . C32 . 121.8(10) yes C30 . C31 . H311 . 119.090 no C32 . C31 . H311 . 119.080 no C31 . C32 . C33 . 119.2(9) yes C31 . C32 . H321 . 120.424 no C33 . C32 . H321 . 120.386 no C32 . C33 . C34 . 119.7(10) yes C32 . C33 . H331 . 120.147 no C34 . C33 . H331 . 120.141 no C29 . C34 . C33 . 121.8(9) yes C29 . C34 . H341 . 119.085 no C33 . C34 . H341 . 119.075 no P1 . C35 . C36 . 122.4(7) yes P1 . C35 . C40 . 119.5(7) yes C36 . C35 . C40 . 117.7(9) yes C35 . C36 . C37 . 120.7(10) yes C35 . C36 . H361 . 119.648 no C37 . C36 . H361 . 119.642 no C36 . C37 . C38 . 119.6(11) yes C36 . C37 . H371 . 120.196 no C38 . C37 . H371 . 120.183 no C37 . C38 . C39 . 122.0(11) yes C37 . C38 . H381 . 118.979 no C39 . C38 . H381 . 118.993 no C38 . C39 . C40 . 118.1(10) yes C38 . C39 . H391 . 120.914 no C40 . C39 . H391 . 120.952 no C35 . C40 . C39 . 121.8(10) yes C35 . C40 . H401 . 119.121 no C39 . C40 . H401 . 119.092 no P2 . C41 . C42 . 120.3(7) yes P2 . C41 . C46 . 120.8(7) yes C42 . C41 . C46 . 118.8(9) yes C41 . C42 . C43 . 121.7(9) yes C41 . C42 . H421 . 119.168 no C43 . C42 . H421 . 119.159 no C42 . C43 . C44 . 119.4(10) yes C42 . C43 . H431 . 120.276 no C44 . C43 . H431 . 120.278 no C43 . C44 . C45 . 119.7(9) yes C43 . C44 . H441 . 120.175 no C45 . C44 . H441 . 120.172 no C44 . C45 . C46 . 121.5(10) yes C44 . C45 . H451 . 119.277 no C46 . C45 . H451 . 119.268 no C41 . C46 . C45 . 118.9(9) yes C41 . C46 . H461 . 120.531 no C45 . C46 . H461 . 120.571 no P2 . C47 . C48 . 117.8(8) yes P2 . C47 . C52 . 123.6(8) yes C48 . C47 . C52 . 118.6(9) yes C47 . C48 . C49 . 119.6(11) yes C47 . C48 . H481 . 120.207 no C49 . C48 . H481 . 120.194 no C48 . C49 . C50 . 119.4(12) yes C48 . C49 . H491 . 120.289 no C50 . C49 . H491 . 120.343 no C49 . C50 . C51 . 121.4(11) yes C49 . C50 . H501 . 119.267 no C51 . C50 . H501 . 119.349 no C50 . C51 . C52 . 119.9(12) yes C50 . C51 . H511 . 120.052 no C52 . C51 . H511 . 120.049 no C47 . C52 . C51 . 121.2(11) yes C47 . C52 . H521 . 119.426 no C51 . C52 . H521 . 119.423 no O1 . C53 . N2 . 122.5(9) yes O1 . C53 . N3 . 122.8(10) yes N2 . C53 . N3 . 114.6(10) yes H541 . C54 . H542 . 109.458 no H551 . C55 . H552 . 109.468 no