Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Sylvia M. Draper' _publ_contact_author_address ; School of Chemistry Trinity College Dublin Dublin Ireland ; _publ_contact_author_email smdraper@tcd.ie _publ_contact_author_phone 353(1)6082026 loop_ _publ_author_name _publ_author_address Cecile.M.A.Ollangier ;School of Chemistry Trinity College Dublin Dublin Ireland ; S.D.Perera ;Department of Chemistry The Open University of Sri Lanka Sri Lanka ; C.M.Fitchett ;School of Chemistry Trinity College Dublin Dublin Ireland ; D.S.Draper ;School of Chemistry Trinity College Dublin Dublin Ireland ; _publ_section_title ; Rhodium and Palladium Complexes of a Pyridyl-centred Polyphenylene Derivative ; data_2 _database_code_depnum_ccdc_archive 'CCDC 644544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H24 N2, C H2 Cl2' _chemical_formula_sum 'C35 H26 Cl2 N2' _chemical_formula_weight 545.48 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall F2-2d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 25.057(3) _cell_length_b 43.374(4) _cell_length_c 10.3758(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11276.7(19) _cell_formula_units_Z 16 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 1607 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 17.80 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9041 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22078 _diffrn_reflns_av_R_equivalents 0.1035 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4968 _reflns_number_gt 3184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(10) _refine_ls_number_reflns 4968 _refine_ls_number_parameters 352 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 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 N1 N 0.48957(14) 0.87333(7) 0.7202(4) 0.0372(9) Uani 1 1 d . . . C2 C 0.50247(16) 0.84322(9) 0.7227(4) 0.0335(11) Uani 1 1 d . . . C3 C 0.46998(15) 0.82053(8) 0.6658(4) 0.0289(10) Uani 1 1 d . . . C4 C 0.42138(16) 0.82972(8) 0.6112(4) 0.0282(10) Uani 1 1 d . . . C5 C 0.40725(15) 0.86113(9) 0.6110(4) 0.0290(10) Uani 1 1 d . . . C6 C 0.44404(16) 0.88224(8) 0.6626(4) 0.0317(10) Uani 1 1 d . . . C7 C 0.55263(17) 0.83580(9) 0.7931(5) 0.0342(11) Uani 1 1 d . . . N8 N 0.59587(17) 0.85191(9) 0.7560(4) 0.0545(12) Uani 1 1 d . . . C9 C 0.6416(2) 0.84623(12) 0.8222(6) 0.0607(16) Uani 1 1 d . . . H9A H 0.6725 0.8575 0.7976 0.073 Uiso 1 1 calc R . . C10 C 0.6469(2) 0.82605(12) 0.9193(6) 0.0578(15) Uani 1 1 d . . . H10A H 0.6803 0.8227 0.9599 0.069 Uiso 1 1 calc R . . C11 C 0.6002(2) 0.80989(10) 0.9592(5) 0.0542(14) Uani 1 1 d . . . H11A H 0.6011 0.7961 1.0301 0.065 Uiso 1 1 calc R . . C12 C 0.55435(18) 0.81492(9) 0.8925(5) 0.0411(12) Uani 1 1 d . . . H12A H 0.5230 0.8038 0.9149 0.049 Uiso 1 1 calc R . . C13 C 0.48826(16) 0.78752(8) 0.6637(4) 0.0305(10) Uani 1 1 d . . . C14 C 0.45914(17) 0.76452(9) 0.7257(4) 0.0365(11) Uani 1 1 d . . . H14A H 0.4275 0.7697 0.7714 0.044 Uiso 1 1 calc R . . C15 C 0.47600(18) 0.73413(9) 0.7210(4) 0.0394(12) Uani 1 1 d . . . H15A H 0.4563 0.7186 0.7644 0.047 Uiso 1 1 calc R . . C16 C 0.52149(19) 0.72653(10) 0.6532(5) 0.0410(12) Uani 1 1 d . . . H16A H 0.5326 0.7056 0.6483 0.049 Uiso 1 1 calc R . . C17 C 0.55057(18) 0.74898(10) 0.5930(5) 0.0422(12) Uani 1 1 d . . . H17A H 0.5821 0.7436 0.5475 0.051 Uiso 1 1 calc R . . C18 C 0.53450(17) 0.77955(9) 0.5978(4) 0.0332(11) Uani 1 1 d . . . H18A H 0.5551 0.7950 0.5561 0.040 Uiso 1 1 calc R . . C19 C 0.38541(16) 0.80605(8) 0.5524(4) 0.0274(10) Uani 1 1 d . . . C20 C 0.33402(17) 0.80167(9) 0.6010(5) 0.0346(11) Uani 1 1 d . . . H20A H 0.3217 0.8138 0.6711 0.042 Uiso 1 1 calc R . . C21 C 0.30111(18) 0.77956(10) 0.5471(5) 0.0420(12) Uani 1 1 d . . . H21A H 0.2658 0.7770 0.5783 0.050 Uiso 1 1 calc R . . C22 C 0.31960(17) 0.76131(10) 0.4480(5) 0.0406(12) Uani 1 1 d . . . H22A H 0.2974 0.7456 0.4136 0.049 Uiso 1 1 calc R . . C23 C 0.37032(17) 0.76574(9) 0.3983(5) 0.0364(11) Uani 1 1 d . . . H23A H 0.3828 0.7535 0.3285 0.044 Uiso 1 1 calc R . . C24 C 0.40246(15) 0.78818(9) 0.4518(4) 0.0293(10) Uani 1 1 d . . . H24A H 0.4373 0.7913 0.4180 0.035 Uiso 1 1 calc R . . C25 C 0.35473(16) 0.87159(9) 0.5580(5) 0.0306(10) Uani 1 1 d . . . C26 C 0.31883(17) 0.88556(9) 0.6451(5) 0.0420(12) Uani 1 1 d . . . H26A H 0.3284 0.8887 0.7327 0.050 Uiso 1 1 calc R . . C27 C 0.26889(19) 0.89464(10) 0.5989(6) 0.0517(15) Uani 1 1 d . . . H27A H 0.2440 0.9040 0.6558 0.062 Uiso 1 1 calc R . . C28 C 0.25549(18) 0.89016(10) 0.4728(6) 0.0538(15) Uani 1 1 d . . . H28A H 0.2215 0.8967 0.4429 0.065 Uiso 1 1 calc R . . C29 C 0.29055(18) 0.87633(10) 0.3875(5) 0.0437(12) Uani 1 1 d . . . H29A H 0.2807 0.8731 0.3002 0.052 Uiso 1 1 calc R . . C30 C 0.34039(16) 0.86725(9) 0.4321(5) 0.0347(11) Uani 1 1 d . . . H30A H 0.3649 0.8579 0.3743 0.042 Uiso 1 1 calc R . . C31 C 0.43618(15) 0.91660(8) 0.6558(5) 0.0327(11) Uani 1 1 d . . . C32 C 0.44356(18) 0.93410(10) 0.7654(5) 0.0447(13) Uani 1 1 d . . . H32A H 0.4517 0.9244 0.8452 0.054 Uiso 1 1 calc R . . C33 C 0.4389(2) 0.96622(12) 0.7582(6) 0.0620(16) Uani 1 1 d . . . H33A H 0.4428 0.9786 0.8331 0.074 Uiso 1 1 calc R . . C34 C 0.42853(19) 0.97965(11) 0.6385(8) 0.0646(18) Uani 1 1 d . . . H34A H 0.4260 1.0015 0.6325 0.078 Uiso 1 1 calc R . . C35 C 0.42200(19) 0.96267(11) 0.5320(6) 0.0522(14) Uani 1 1 d . . . H35A H 0.4148 0.9723 0.4516 0.063 Uiso 1 1 calc R . . C36 C 0.42584(17) 0.93076(10) 0.5407(5) 0.0402(12) Uani 1 1 d . . . H36A H 0.4212 0.9186 0.4654 0.048 Uiso 1 1 calc R . . Cl42 Cl 0.39304(6) 0.82380(4) 0.93498(16) 0.0775(5) Uani 1 1 d . . . Cl41 Cl 0.32761(7) 0.80778(4) 1.15450(17) 0.0897(6) Uani 1 1 d . . . C40 C 0.3288(2) 0.82181(13) 0.9970(6) 0.0683(17) Uani 1 1 d . . . H40A H 0.3069 0.8082 0.9415 0.082 Uiso 1 1 calc R . . H40B H 0.3126 0.8426 0.9953 0.082 Uiso 1 1 calc R . . 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 N1 0.034(2) 0.0195(18) 0.058(3) -0.0015(17) -0.009(2) -0.0019(15) C2 0.031(2) 0.024(2) 0.046(3) -0.001(2) -0.002(2) -0.0014(19) C3 0.026(2) 0.024(2) 0.037(3) 0.001(2) -0.003(2) -0.0027(17) C4 0.029(2) 0.023(2) 0.033(3) -0.0029(18) 0.0021(19) -0.0048(18) C5 0.022(2) 0.027(2) 0.038(3) 0.0000(19) 0.001(2) -0.0016(17) C6 0.028(2) 0.023(2) 0.044(3) -0.005(2) -0.001(2) -0.0008(18) C7 0.034(3) 0.023(2) 0.045(3) -0.004(2) -0.007(2) -0.0014(19) N8 0.048(3) 0.047(2) 0.069(3) 0.001(2) -0.014(2) -0.010(2) C9 0.041(3) 0.061(4) 0.081(5) -0.003(3) -0.019(3) -0.009(3) C10 0.045(3) 0.054(3) 0.075(4) -0.007(3) -0.027(3) 0.007(3) C11 0.070(4) 0.039(3) 0.053(3) 0.004(3) -0.020(3) 0.014(3) C12 0.038(3) 0.032(2) 0.053(3) -0.003(2) -0.001(3) -0.003(2) C13 0.031(2) 0.022(2) 0.038(3) 0.000(2) -0.010(2) -0.0014(17) C14 0.036(3) 0.031(3) 0.042(3) 0.002(2) 0.002(2) 0.001(2) C15 0.043(3) 0.025(2) 0.049(3) 0.006(2) -0.007(3) -0.008(2) C16 0.045(3) 0.023(2) 0.055(3) -0.006(2) -0.004(3) 0.003(2) C17 0.033(3) 0.040(3) 0.053(3) -0.005(2) 0.003(2) 0.010(2) C18 0.032(3) 0.025(2) 0.043(3) 0.002(2) -0.003(2) -0.0040(19) C19 0.024(2) 0.018(2) 0.040(3) 0.0008(19) -0.005(2) -0.0016(16) C20 0.033(3) 0.022(2) 0.048(3) 0.001(2) 0.006(2) -0.0002(18) C21 0.029(3) 0.036(3) 0.061(4) 0.003(3) 0.004(2) -0.015(2) C22 0.041(3) 0.032(2) 0.049(3) -0.008(2) -0.005(2) -0.018(2) C23 0.035(3) 0.031(2) 0.043(3) -0.003(2) -0.002(2) -0.0004(19) C24 0.023(2) 0.024(2) 0.040(3) 0.000(2) 0.001(2) -0.0022(17) C25 0.023(2) 0.018(2) 0.051(3) -0.0039(19) 0.001(2) -0.0029(17) C26 0.040(3) 0.028(2) 0.058(3) -0.013(2) 0.000(3) -0.003(2) C27 0.035(3) 0.033(3) 0.087(5) -0.023(3) 0.004(3) 0.002(2) C28 0.027(3) 0.029(3) 0.105(5) -0.005(3) -0.020(3) 0.003(2) C29 0.042(3) 0.037(3) 0.052(3) 0.007(2) -0.022(3) -0.008(2) C30 0.029(2) 0.032(2) 0.043(3) 0.004(2) -0.002(2) -0.0036(19) C31 0.017(2) 0.024(2) 0.057(3) -0.003(2) -0.003(2) -0.0028(17) C32 0.047(3) 0.031(3) 0.056(4) -0.002(2) 0.004(3) 0.000(2) C33 0.058(4) 0.039(3) 0.089(5) -0.014(3) -0.006(3) 0.005(3) C34 0.035(3) 0.027(3) 0.131(6) -0.006(4) -0.012(4) 0.005(2) C35 0.042(3) 0.037(3) 0.077(4) 0.008(3) -0.013(3) -0.011(2) C36 0.032(3) 0.026(2) 0.062(4) -0.003(2) -0.012(2) -0.0023(19) Cl42 0.0837(11) 0.0734(9) 0.0755(12) 0.0006(8) 0.0094(9) 0.0351(8) Cl41 0.0899(12) 0.1122(13) 0.0670(11) 0.0077(10) -0.0054(9) 0.0322(10) C40 0.066(4) 0.054(3) 0.084(5) 0.001(3) -0.010(3) 0.019(3) _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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:53.1(2), B:62.2(1), C:61.4(2), D:61.9(2), E: 51.4(2). ; 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 N1 C2 1.345(5) . ? N1 C6 1.345(5) . ? C2 C3 1.407(5) . ? C2 C7 1.489(6) . ? C3 C4 1.401(6) . ? C3 C13 1.503(5) . ? C4 C5 1.408(5) . ? C4 C19 1.496(5) . ? C5 C6 1.405(5) . ? C5 C25 1.497(6) . ? C6 C31 1.505(5) . ? C7 N8 1.345(6) . ? C7 C12 1.373(6) . ? N8 C9 1.359(6) . ? C9 C10 1.341(7) . ? C9 H9A 0.9500 . ? C10 C11 1.425(7) . ? C10 H10A 0.9500 . ? C11 C12 1.358(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.389(6) . ? C13 C14 1.393(6) . ? C14 C15 1.385(6) . ? C14 H14A 0.9500 . ? C15 C16 1.379(6) . ? C15 H15A 0.9500 . ? C16 C17 1.367(6) . ? C16 H16A 0.9500 . ? C17 C18 1.386(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.369(6) . ? C19 C20 1.396(6) . ? C20 C21 1.383(6) . ? C20 H20A 0.9500 . ? C21 C22 1.378(6) . ? C21 H21A 0.9500 . ? C22 C23 1.385(6) . ? C22 H22A 0.9500 . ? C23 C24 1.380(5) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.368(6) . ? C25 C26 1.412(6) . ? C26 C27 1.397(7) . ? C26 H26A 0.9500 . ? C27 C28 1.365(7) . ? C27 H27A 0.9500 . ? C28 C29 1.383(7) . ? C28 H28A 0.9500 . ? C29 C30 1.389(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.368(6) . ? C31 C32 1.380(6) . ? C32 C33 1.400(7) . ? C32 H32A 0.9500 . ? C33 C34 1.397(8) . ? C33 H33A 0.9500 . ? C34 C35 1.338(8) . ? C34 H34A 0.9500 . ? C35 C36 1.391(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? Cl42 C40 1.736(6) . ? Cl41 C40 1.744(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 C2 N1 C6 119.5(3) . . ? N1 C2 C3 122.1(4) . . ? N1 C2 C7 115.0(4) . . ? C3 C2 C7 122.9(4) . . ? C4 C3 C2 118.2(3) . . ? C4 C3 C13 122.0(3) . . ? C2 C3 C13 119.7(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 C19 119.6(3) . . ? C5 C4 C19 120.8(4) . . ? C6 C5 C4 117.7(4) . . ? C6 C5 C25 121.3(3) . . ? C4 C5 C25 121.0(3) . . ? N1 C6 C5 122.6(3) . . ? N1 C6 C31 114.6(3) . . ? C5 C6 C31 122.8(4) . . ? N8 C7 C12 122.2(4) . . ? N8 C7 C2 115.3(4) . . ? C12 C7 C2 122.5(4) . . ? C7 N8 C9 116.1(4) . . ? C10 C9 N8 125.5(5) . . ? C10 C9 H9A 117.3 . . ? N8 C9 H9A 117.3 . . ? C9 C10 C11 117.3(5) . . ? C9 C10 H10A 121.4 . . ? C11 C10 H10A 121.4 . . ? C12 C11 C10 117.9(5) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? C11 C12 C7 121.0(4) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? C18 C13 C14 119.1(4) . . ? C18 C13 C3 119.9(4) . . ? C14 C13 C3 121.0(4) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C13 119.9(4) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? C24 C19 C20 119.1(4) . . ? C24 C19 C4 120.8(4) . . ? C20 C19 C4 120.1(4) . . ? C21 C20 C19 119.9(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C24 C23 C22 118.9(4) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C19 C24 C23 121.6(4) . . ? C19 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C30 C25 C26 120.2(4) . . ? C30 C25 C5 122.7(4) . . ? C26 C25 C5 117.1(4) . . ? C27 C26 C25 118.2(5) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C28 C27 C26 120.6(5) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C27 C28 C29 121.2(4) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C28 C29 C30 118.8(5) . . ? C28 C29 H29A 120.6 . . ? C30 C29 H29A 120.6 . . ? C25 C30 C29 121.0(4) . . ? C25 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C36 C31 C32 119.9(4) . . ? C36 C31 C6 120.7(4) . . ? C32 C31 C6 119.3(4) . . ? C31 C32 C33 119.5(5) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? C32 C33 C34 118.6(5) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C35 C34 C33 121.9(5) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C34 C35 C36 119.1(5) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? C31 C36 C35 121.1(5) . . ? C31 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? Cl42 C40 Cl41 112.3(3) . . ? Cl42 C40 H40A 109.1 . . ? Cl41 C40 H40A 109.1 . . ? Cl42 C40 H40B 109.1 . . ? Cl41 C40 H40B 109.1 . . ? H40A C40 H40B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 C3 0.5(7) . . . . ? C6 N1 C2 C7 -177.8(4) . . . . ? N1 C2 C3 C4 -3.5(7) . . . . ? C7 C2 C3 C4 174.7(4) . . . . ? N1 C2 C3 C13 175.8(4) . . . . ? C7 C2 C3 C13 -6.0(7) . . . . ? C2 C3 C4 C5 2.0(6) . . . . ? C13 C3 C4 C5 -177.3(4) . . . . ? C2 C3 C4 C19 -178.8(4) . . . . ? C13 C3 C4 C19 2.0(6) . . . . ? C3 C4 C5 C6 2.2(6) . . . . ? C19 C4 C5 C6 -177.1(4) . . . . ? C3 C4 C5 C25 -177.7(4) . . . . ? C19 C4 C5 C25 3.1(6) . . . . ? C2 N1 C6 C5 4.0(7) . . . . ? C2 N1 C6 C31 -175.0(4) . . . . ? C4 C5 C6 N1 -5.3(7) . . . . ? C25 C5 C6 N1 174.5(4) . . . . ? C4 C5 C6 C31 173.6(4) . . . . ? C25 C5 C6 C31 -6.6(7) . . . . ? N1 C2 C7 N8 -52.8(6) . . . . ? C3 C2 C7 N8 128.9(5) . . . . ? N1 C2 C7 C12 124.7(5) . . . . ? C3 C2 C7 C12 -53.6(6) . . . . ? C12 C7 N8 C9 0.3(7) . . . . ? C2 C7 N8 C9 177.8(4) . . . . ? C7 N8 C9 C10 0.4(8) . . . . ? N8 C9 C10 C11 -2.1(8) . . . . ? C9 C10 C11 C12 3.1(7) . . . . ? C10 C11 C12 C7 -2.5(7) . . . . ? N8 C7 C12 C11 0.9(7) . . . . ? C2 C7 C12 C11 -176.5(4) . . . . ? C4 C3 C13 C18 116.9(5) . . . . ? C2 C3 C13 C18 -62.4(6) . . . . ? C4 C3 C13 C14 -62.2(6) . . . . ? C2 C3 C13 C14 118.5(5) . . . . ? C18 C13 C14 C15 -0.3(6) . . . . ? C3 C13 C14 C15 178.9(4) . . . . ? C13 C14 C15 C16 -0.9(7) . . . . ? C14 C15 C16 C17 1.4(7) . . . . ? C15 C16 C17 C18 -0.8(7) . . . . ? C16 C17 C18 C13 -0.3(7) . . . . ? C14 C13 C18 C17 0.9(6) . . . . ? C3 C13 C18 C17 -178.3(4) . . . . ? C3 C4 C19 C24 -59.7(6) . . . . ? C5 C4 C19 C24 119.5(4) . . . . ? C3 C4 C19 C20 119.4(5) . . . . ? C5 C4 C19 C20 -61.3(6) . . . . ? C24 C19 C20 C21 -0.3(6) . . . . ? C4 C19 C20 C21 -179.4(4) . . . . ? C19 C20 C21 C22 1.9(7) . . . . ? C20 C21 C22 C23 -2.6(7) . . . . ? C21 C22 C23 C24 1.7(7) . . . . ? C20 C19 C24 C23 -0.7(6) . . . . ? C4 C19 C24 C23 178.4(4) . . . . ? C22 C23 C24 C19 0.0(6) . . . . ? C6 C5 C25 C30 118.7(5) . . . . ? C4 C5 C25 C30 -61.5(6) . . . . ? C6 C5 C25 C26 -63.3(5) . . . . ? C4 C5 C25 C26 116.5(4) . . . . ? C30 C25 C26 C27 0.1(6) . . . . ? C5 C25 C26 C27 -178.0(4) . . . . ? C25 C26 C27 C28 -0.3(6) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? C27 C28 C29 C30 -0.7(7) . . . . ? C26 C25 C30 C29 -0.2(6) . . . . ? C5 C25 C30 C29 177.7(4) . . . . ? C28 C29 C30 C25 0.5(6) . . . . ? N1 C6 C31 C36 126.5(4) . . . . ? C5 C6 C31 C36 -52.5(6) . . . . ? N1 C6 C31 C32 -48.5(6) . . . . ? C5 C6 C31 C32 132.5(5) . . . . ? C36 C31 C32 C33 1.7(7) . . . . ? C6 C31 C32 C33 176.8(4) . . . . ? C31 C32 C33 C34 -1.9(8) . . . . ? C32 C33 C34 C35 1.2(8) . . . . ? C33 C34 C35 C36 -0.2(8) . . . . ? C32 C31 C36 C35 -0.7(7) . . . . ? C6 C31 C36 C35 -175.7(4) . . . . ? C34 C35 C36 C31 0.0(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.248 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.055 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 644545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 Cl2 N3 Rh, 4(C H Cl3)' _chemical_formula_sum 'C40 H30 Cl14 N3 Rh' _chemical_formula_weight 1151.88 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 11.8530(9) _cell_length_b 26.863(2) _cell_length_c 15.1269(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.269(2) _cell_angle_gamma 90.00 _cell_volume 4723.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(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 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8313 _exptl_absorpt_correction_T_max 0.9766 _exptl_absorpt_process_details 'blessing Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36953 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8307 _reflns_number_gt 5842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+7.5896P] 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 8307 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Rh1 Rh 0.80253(4) 0.527125(16) 0.12007(3) 0.02085(13) Uani 1 1 d . . . Cl1 Cl 0.72594(12) 0.46503(5) 0.19997(9) 0.0279(3) Uani 1 1 d . . . N1 N 0.8036(4) 0.57182(15) 0.2228(3) 0.0206(10) Uani 1 1 d . . . C2 C 0.8972(4) 0.57071(19) 0.2899(3) 0.0215(11) Uani 1 1 d . . . Cl2 Cl 0.87851(13) 0.58947(5) 0.04114(9) 0.0315(3) Uani 1 1 d . . . C3 C 0.8968(5) 0.5999(2) 0.3669(3) 0.0234(12) Uani 1 1 d . . . C4 C 0.7950(5) 0.62545(19) 0.3742(3) 0.0224(12) Uani 1 1 d . . . C5 C 0.6968(5) 0.62271(19) 0.3052(4) 0.0234(12) Uani 1 1 d . . . C6 C 0.7062(4) 0.59753(19) 0.2263(3) 0.0223(12) Uani 1 1 d . . . C7 C 0.6191(5) 0.5965(2) 0.1404(3) 0.0249(12) Uani 1 1 d . . . N8 N 0.6359(4) 0.56159(17) 0.0801(3) 0.0262(10) Uani 1 1 d . . . C9 C 0.5622(5) 0.5579(2) 0.0016(4) 0.0320(14) Uani 1 1 d . . . H9A H 0.5756 0.5332 -0.0401 0.038 Uiso 1 1 calc R . . C10 C 0.4677(5) 0.5882(2) -0.0215(4) 0.0338(14) Uani 1 1 d . . . H10A H 0.4142 0.5835 -0.0764 0.041 Uiso 1 1 calc R . . C11 C 0.4529(5) 0.6254(2) 0.0371(4) 0.0346(14) Uani 1 1 d . . . H11A H 0.3907 0.6481 0.0214 0.042 Uiso 1 1 calc R . . C12 C 0.5282(5) 0.6301(2) 0.1193(4) 0.0318(13) Uani 1 1 d . . . H12A H 0.5180 0.6557 0.1604 0.038 Uiso 1 1 calc R . . C13 C 0.5866(5) 0.6447(2) 0.3191(3) 0.0241(12) Uani 1 1 d . . . C14 C 0.4954(5) 0.6130(2) 0.3241(4) 0.0319(13) Uani 1 1 d . . . H14A H 0.5040 0.5781 0.3183 0.038 Uiso 1 1 calc R . . C15 C 0.3903(5) 0.6327(3) 0.3378(4) 0.0368(15) Uani 1 1 d . . . H15A H 0.3281 0.6111 0.3418 0.044 Uiso 1 1 calc R . . C16 C 0.3778(6) 0.6832(3) 0.3452(4) 0.0432(17) Uani 1 1 d . . . H16A H 0.3064 0.6966 0.3534 0.052 Uiso 1 1 calc R . . C17 C 0.4676(6) 0.7142(2) 0.3408(4) 0.0411(16) Uani 1 1 d . . . H17A H 0.4581 0.7491 0.3469 0.049 Uiso 1 1 calc R . . C18 C 0.5709(5) 0.6961(2) 0.3279(4) 0.0321(14) Uani 1 1 d . . . H18A H 0.6323 0.7184 0.3249 0.039 Uiso 1 1 calc R . . C19 C 0.7921(5) 0.6554(2) 0.4575(3) 0.0266(13) Uani 1 1 d . . . C20 C 0.7344(5) 0.6383(2) 0.5220(4) 0.0372(15) Uani 1 1 d . . . H20A H 0.6951 0.6073 0.5131 0.045 Uiso 1 1 calc R . . C21 C 0.7326(6) 0.6654(3) 0.5998(4) 0.0468(18) Uani 1 1 d . . . H21A H 0.6931 0.6529 0.6441 0.056 Uiso 1 1 calc R . . C22 C 0.7884(6) 0.7105(3) 0.6122(4) 0.0484(18) Uani 1 1 d . . . H22A H 0.7859 0.7298 0.6645 0.058 Uiso 1 1 calc R . . C23 C 0.8478(7) 0.7278(3) 0.5487(4) 0.0491(18) Uani 1 1 d . . . H23A H 0.8878 0.7586 0.5581 0.059 Uiso 1 1 calc R . . C24 C 0.8497(5) 0.7006(2) 0.4710(4) 0.0349(14) Uani 1 1 d . . . H24A H 0.8902 0.7129 0.4272 0.042 Uiso 1 1 calc R . . C25 C 0.9963(5) 0.6033(2) 0.4432(3) 0.0226(12) Uani 1 1 d . . . C26 C 1.0000(5) 0.5736(2) 0.5186(4) 0.0312(13) Uani 1 1 d . . . H26A H 0.9406 0.5500 0.5197 0.037 Uiso 1 1 calc R . . C27 C 1.0886(5) 0.5780(3) 0.5916(4) 0.0438(17) Uani 1 1 d . . . H27A H 1.0906 0.5574 0.6429 0.053 Uiso 1 1 calc R . . C28 C 1.1743(6) 0.6121(3) 0.5904(4) 0.0486(18) Uani 1 1 d . . . H28A H 1.2346 0.6157 0.6415 0.058 Uiso 1 1 calc R . . C29 C 1.1735(6) 0.6415(3) 0.5152(4) 0.0456(17) Uani 1 1 d . . . H29A H 1.2337 0.6648 0.5141 0.055 Uiso 1 1 calc R . . C30 C 1.0845(5) 0.6368(2) 0.4418(4) 0.0349(14) Uani 1 1 d . . . H30A H 1.0838 0.6568 0.3898 0.042 Uiso 1 1 calc R . . C31 C 0.9868(5) 0.53583(19) 0.2724(3) 0.0229(12) Uani 1 1 d . . . C32 C 0.9580(4) 0.5089(2) 0.1893(3) 0.0219(12) Uani 1 1 d . . . C33 C 1.0333(5) 0.4737(2) 0.1692(4) 0.0308(13) Uani 1 1 d . . . H33A H 1.0155 0.4565 0.1133 0.037 Uiso 1 1 calc R . . C34 C 1.1341(5) 0.4627(2) 0.2284(4) 0.0368(15) Uani 1 1 d . . . H34A H 1.1842 0.4377 0.2138 0.044 Uiso 1 1 calc R . . C35 C 1.1621(5) 0.4882(2) 0.3092(4) 0.0378(15) Uani 1 1 d . . . H35A H 1.2314 0.4806 0.3502 0.045 Uiso 1 1 calc R . . C36 C 1.0897(5) 0.5245(2) 0.3304(4) 0.0306(13) Uani 1 1 d . . . H36A H 1.1105 0.5421 0.3856 0.037 Uiso 1 1 calc R . . N40 N 0.8015(4) 0.48056(17) 0.0145(3) 0.0265(11) Uani 1 1 d . . . C41 C 0.8010(5) 0.4564(2) -0.0468(4) 0.0257(12) Uani 1 1 d . . . C42 C 0.8019(6) 0.4245(2) -0.1244(4) 0.0361(15) Uani 1 1 d . . . H42A H 0.8816 0.4168 -0.1283 0.054 Uiso 1 1 calc R . . H42B H 0.7642 0.4417 -0.1794 0.054 Uiso 1 1 calc R . . H42C H 0.7606 0.3935 -0.1176 0.054 Uiso 1 1 calc R . . C50 C 0.5745(8) 0.4550(3) 0.3690(6) 0.070(2) Uani 1 1 d . . . H50A H 0.6282 0.4416 0.3314 0.084 Uiso 1 1 calc R . . Cl51 Cl 0.5378(2) 0.40613(11) 0.4323(2) 0.1136(11) Uani 1 1 d . . . Cl52 Cl 0.6480(3) 0.50296(10) 0.4370(2) 0.1032(9) Uani 1 1 d . . . Cl53 Cl 0.4527(2) 0.47725(9) 0.29514(19) 0.0864(8) Uani 1 1 d . . . C60 C 0.6388(5) 0.8535(3) 0.3346(5) 0.0481(18) Uani 1 1 d . . . H60A H 0.6513 0.8902 0.3305 0.058 Uiso 1 1 calc R . . Cl61 Cl 0.60892(18) 0.84011(9) 0.44222(14) 0.0702(6) Uani 1 1 d . . . Cl62 Cl 0.52246(15) 0.83658(8) 0.25046(13) 0.0606(5) Uani 1 1 d . . . Cl63 Cl 0.76467(15) 0.82285(7) 0.32181(13) 0.0520(5) Uani 1 1 d . . . C70 C 0.0549(6) 0.2922(2) 0.8663(4) 0.0476(18) Uani 1 1 d . . . H70A H 0.0817 0.3205 0.9080 0.057 Uiso 1 1 calc R . . Cl71 Cl 0.1522(2) 0.28373(10) 0.79610(17) 0.0938(8) Uani 1 1 d . . . Cl72 Cl -0.0831(2) 0.30708(9) 0.80156(15) 0.0774(7) Uani 1 1 d . . . Cl73 Cl 0.04303(18) 0.23950(8) 0.93030(14) 0.0669(6) Uani 1 1 d . . . C80 C 0.1635(6) 0.8295(3) 0.3960(4) 0.0430(16) Uani 1 1 d . . . H80A H 0.1710 0.8585 0.4380 0.052 Uiso 1 1 calc R . . Cl81 Cl 0.1301(3) 0.77710(9) 0.45293(19) 0.0959(9) Uani 1 1 d . . . Cl82 Cl 0.05375(19) 0.84222(12) 0.30320(15) 0.0931(9) Uani 1 1 d . . . Cl83 Cl 0.29257(15) 0.82222(7) 0.35913(14) 0.0587(5) Uani 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 Rh1 0.0270(2) 0.0207(2) 0.0150(2) -0.00273(18) 0.00451(16) -0.00305(19) Cl1 0.0339(7) 0.0281(8) 0.0216(7) 0.0016(6) 0.0053(6) -0.0075(6) N1 0.029(2) 0.020(2) 0.013(2) -0.0036(18) 0.0041(18) -0.0044(19) C2 0.028(3) 0.024(3) 0.014(3) 0.001(2) 0.005(2) -0.001(2) Cl2 0.0434(8) 0.0261(8) 0.0270(7) 0.0016(6) 0.0120(6) -0.0070(6) C3 0.030(3) 0.024(3) 0.016(3) 0.002(2) 0.004(2) -0.006(2) C4 0.032(3) 0.019(3) 0.018(3) 0.001(2) 0.008(2) -0.004(2) C5 0.029(3) 0.016(3) 0.026(3) 0.001(2) 0.005(2) -0.002(2) C6 0.025(3) 0.023(3) 0.020(3) 0.002(2) 0.007(2) -0.003(2) C7 0.029(3) 0.026(3) 0.020(3) 0.004(2) 0.005(2) -0.002(2) N8 0.033(3) 0.025(3) 0.019(2) 0.001(2) 0.002(2) -0.006(2) C9 0.042(4) 0.026(3) 0.027(3) -0.003(3) 0.003(3) -0.012(3) C10 0.031(3) 0.042(4) 0.022(3) 0.005(3) -0.010(2) -0.007(3) C11 0.032(3) 0.040(4) 0.029(3) 0.006(3) -0.002(3) -0.002(3) C12 0.032(3) 0.032(3) 0.031(3) 0.000(3) 0.006(3) 0.001(3) C13 0.032(3) 0.026(3) 0.013(3) -0.001(2) 0.003(2) 0.001(2) C14 0.036(3) 0.029(3) 0.029(3) -0.001(3) 0.004(3) -0.004(3) C15 0.026(3) 0.055(4) 0.032(3) 0.003(3) 0.012(3) -0.003(3) C16 0.034(4) 0.059(5) 0.038(4) -0.008(3) 0.009(3) 0.015(3) C17 0.043(4) 0.032(4) 0.047(4) -0.008(3) 0.007(3) 0.010(3) C18 0.038(3) 0.028(3) 0.031(3) -0.001(3) 0.008(3) 0.000(3) C19 0.030(3) 0.030(3) 0.018(3) -0.004(2) 0.000(2) 0.004(3) C20 0.044(4) 0.041(4) 0.027(3) -0.008(3) 0.008(3) -0.004(3) C21 0.042(4) 0.072(5) 0.028(4) -0.011(3) 0.010(3) 0.007(4) C22 0.053(4) 0.054(5) 0.036(4) -0.020(3) 0.003(3) 0.017(4) C23 0.069(5) 0.033(4) 0.042(4) -0.017(3) 0.000(4) -0.003(3) C24 0.048(4) 0.033(3) 0.023(3) -0.006(3) 0.005(3) -0.005(3) C25 0.029(3) 0.024(3) 0.015(3) -0.005(2) 0.005(2) 0.004(2) C26 0.036(3) 0.033(3) 0.023(3) 0.000(3) 0.003(3) -0.006(3) C27 0.043(4) 0.062(5) 0.026(3) 0.012(3) 0.005(3) 0.001(3) C28 0.043(4) 0.069(5) 0.029(4) -0.005(3) -0.006(3) 0.001(4) C29 0.036(4) 0.055(4) 0.042(4) -0.005(3) -0.001(3) -0.016(3) C30 0.039(3) 0.040(4) 0.025(3) -0.003(3) 0.004(3) -0.007(3) C31 0.028(3) 0.019(3) 0.021(3) 0.000(2) 0.003(2) -0.005(2) C32 0.023(3) 0.024(3) 0.019(3) 0.002(2) 0.007(2) -0.005(2) C33 0.037(3) 0.029(3) 0.028(3) -0.005(3) 0.010(3) -0.006(3) C34 0.046(4) 0.028(3) 0.040(4) -0.001(3) 0.019(3) 0.010(3) C35 0.031(3) 0.044(4) 0.037(4) 0.005(3) 0.004(3) 0.008(3) C36 0.033(3) 0.035(3) 0.023(3) -0.001(3) 0.005(2) 0.002(3) N40 0.037(3) 0.026(3) 0.018(2) -0.003(2) 0.009(2) -0.003(2) C41 0.030(3) 0.026(3) 0.021(3) -0.002(2) 0.005(2) -0.006(2) C42 0.052(4) 0.037(4) 0.022(3) -0.010(3) 0.013(3) -0.008(3) C50 0.091(7) 0.056(5) 0.069(6) 0.011(4) 0.033(5) 0.020(5) Cl51 0.0928(19) 0.105(2) 0.162(3) 0.056(2) 0.0712(19) 0.0062(16) Cl52 0.115(2) 0.0710(17) 0.107(2) -0.0174(15) -0.0192(17) 0.0157(16) Cl53 0.0603(13) 0.0710(16) 0.125(2) 0.0002(14) 0.0107(14) 0.0008(12) C60 0.038(4) 0.036(4) 0.074(5) -0.004(4) 0.018(4) -0.001(3) Cl61 0.0653(13) 0.0885(16) 0.0625(13) -0.0251(11) 0.0262(10) -0.0276(12) Cl62 0.0422(10) 0.0745(14) 0.0628(12) 0.0149(10) 0.0047(9) -0.0110(9) Cl63 0.0429(10) 0.0506(11) 0.0637(12) 0.0001(9) 0.0131(8) 0.0055(8) C70 0.076(5) 0.036(4) 0.035(4) 0.000(3) 0.022(3) -0.008(4) Cl71 0.109(2) 0.104(2) 0.0878(17) -0.0116(15) 0.0681(16) -0.0249(16) Cl72 0.0966(17) 0.0637(14) 0.0640(14) 0.0040(11) -0.0037(12) 0.0150(12) Cl73 0.0689(13) 0.0678(13) 0.0625(12) 0.0302(11) 0.0092(10) -0.0122(11) C80 0.044(4) 0.046(4) 0.042(4) -0.009(3) 0.015(3) 0.005(3) Cl81 0.129(2) 0.0605(14) 0.117(2) 0.0109(14) 0.0714(18) -0.0043(14) Cl82 0.0523(13) 0.166(3) 0.0598(14) 0.0012(15) 0.0081(10) 0.0368(15) Cl83 0.0403(10) 0.0626(12) 0.0774(13) -0.0168(10) 0.0217(9) 0.0064(9) _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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:16.6(3), B:65.8(2), C:75.8(2), D:81.8(2), E:10.5(3) ; 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 Rh1 N1 1.962(4) . ? Rh1 C32 1.994(5) . ? Rh1 N40 2.027(4) . ? Rh1 N8 2.158(5) . ? Rh1 Cl2 2.3369(14) . ? Rh1 Cl1 2.3445(14) . ? N1 C2 1.350(6) . ? N1 C6 1.355(7) . ? C2 C3 1.405(7) . ? C2 C31 1.478(7) . ? C3 C4 1.412(7) . ? C3 C25 1.483(7) . ? C4 C5 1.406(7) . ? C4 C19 1.500(7) . ? C5 C6 1.395(7) . ? C5 C13 1.486(7) . ? C6 C7 1.494(7) . ? C7 N8 1.349(7) . ? C7 C12 1.393(8) . ? N8 C9 1.334(7) . ? C9 C10 1.374(8) . ? C9 H9A 0.9500 . ? C10 C11 1.369(8) . ? C10 H10A 0.9500 . ? C11 C12 1.388(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.391(8) . ? C13 C18 1.403(8) . ? C14 C15 1.404(8) . ? C14 H14A 0.9500 . ? C15 C16 1.372(9) . ? C15 H15A 0.9500 . ? C16 C17 1.363(9) . ? C16 H16A 0.9500 . ? C17 C18 1.367(8) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.376(8) . ? C19 C24 1.389(8) . ? C20 C21 1.388(8) . ? C20 H20A 0.9500 . ? C21 C22 1.377(10) . ? C21 H21A 0.9500 . ? C22 C23 1.378(10) . ? C22 H22A 0.9500 . ? C23 C24 1.388(8) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.383(8) . ? C25 C26 1.386(7) . ? C26 C27 1.373(8) . ? C26 H26A 0.9500 . ? C27 C28 1.372(9) . ? C27 H27A 0.9500 . ? C28 C29 1.383(9) . ? C28 H28A 0.9500 . ? C29 C30 1.379(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.389(8) . ? C31 C32 1.432(7) . ? C32 C33 1.376(8) . ? C33 C34 1.378(8) . ? C33 H33A 0.9500 . ? C34 C35 1.383(8) . ? C34 H34A 0.9500 . ? C35 C36 1.379(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N40 C41 1.130(7) . ? C41 C42 1.456(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C50 Cl51 1.730(8) . ? C50 Cl53 1.749(9) . ? C50 Cl52 1.768(9) . ? C50 H50A 1.0000 . ? C60 Cl62 1.744(7) . ? C60 Cl63 1.748(7) . ? C60 Cl61 1.769(7) . ? C60 H60A 1.0000 . ? C70 Cl71 1.728(7) . ? C70 Cl73 1.736(7) . ? C70 Cl72 1.780(8) . ? C70 H70A 1.0000 . ? C80 Cl81 1.735(7) . ? C80 Cl83 1.739(6) . ? C80 Cl82 1.751(7) . ? C80 H80A 1.0000 . ? 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 Rh1 C32 82.6(2) . . ? N1 Rh1 N40 179.64(18) . . ? C32 Rh1 N40 97.2(2) . . ? N1 Rh1 N8 79.80(17) . . ? C32 Rh1 N8 162.43(19) . . ? N40 Rh1 N8 100.38(18) . . ? N1 Rh1 Cl2 91.28(13) . . ? C32 Rh1 Cl2 92.02(15) . . ? N40 Rh1 Cl2 89.03(13) . . ? N8 Rh1 Cl2 88.42(12) . . ? N1 Rh1 Cl1 88.31(13) . . ? C32 Rh1 Cl1 88.04(15) . . ? N40 Rh1 Cl1 91.37(13) . . ? N8 Rh1 Cl1 91.39(12) . . ? Cl2 Rh1 Cl1 179.58(5) . . ? C2 N1 C6 124.3(4) . . ? C2 N1 Rh1 117.3(3) . . ? C6 N1 Rh1 118.0(3) . . ? N1 C2 C3 118.4(5) . . ? N1 C2 C31 113.2(4) . . ? C3 C2 C31 128.3(5) . . ? C2 C3 C4 118.5(5) . . ? C2 C3 C25 123.3(5) . . ? C4 C3 C25 118.1(5) . . ? C5 C4 C3 120.8(5) . . ? C5 C4 C19 120.1(5) . . ? C3 C4 C19 119.1(5) . . ? C6 C5 C4 117.9(5) . . ? C6 C5 C13 122.3(5) . . ? C4 C5 C13 119.7(5) . . ? N1 C6 C5 119.5(5) . . ? N1 C6 C7 113.9(4) . . ? C5 C6 C7 126.6(5) . . ? N8 C7 C12 120.4(5) . . ? N8 C7 C6 115.6(5) . . ? C12 C7 C6 124.0(5) . . ? C9 N8 C7 119.7(5) . . ? C9 N8 Rh1 128.4(4) . . ? C7 N8 Rh1 110.9(3) . . ? N8 C9 C10 122.8(6) . . ? N8 C9 H9A 118.6 . . ? C10 C9 H9A 118.6 . . ? C11 C10 C9 118.0(5) . . ? C11 C10 H10A 121.0 . . ? C9 C10 H10A 121.0 . . ? C10 C11 C12 120.3(6) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 118.6(6) . . ? C11 C12 H12A 120.7 . . ? C7 C12 H12A 120.7 . . ? C14 C13 C18 118.6(5) . . ? C14 C13 C5 118.6(5) . . ? C18 C13 C5 122.8(5) . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.1(6) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 121.3(6) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C17 C18 C13 120.1(6) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C20 C19 C24 119.1(5) . . ? C20 C19 C4 120.8(5) . . ? C24 C19 C4 120.1(5) . . ? C19 C20 C21 121.2(6) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C22 C21 C20 119.5(6) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.5(6) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C23 C24 C19 119.8(6) . . ? C23 C24 H24A 120.1 . . ? C19 C24 H24A 120.1 . . ? C30 C25 C26 119.1(5) . . ? C30 C25 C3 121.1(5) . . ? C26 C25 C3 119.8(5) . . ? C27 C26 C25 120.5(6) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 120.5(6) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C29 C30 C25 120.6(6) . . ? C29 C30 H30A 119.7 . . ? C25 C30 H30A 119.7 . . ? C36 C31 C32 118.2(5) . . ? C36 C31 C2 126.8(5) . . ? C32 C31 C2 114.8(5) . . ? C33 C32 C31 119.2(5) . . ? C33 C32 Rh1 128.7(4) . . ? C31 C32 Rh1 112.0(4) . . ? C32 C33 C34 121.4(5) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C33 C34 C35 119.7(5) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 120.2(6) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C31 121.2(5) . . ? C35 C36 H36A 119.4 . . ? C31 C36 H36A 119.4 . . ? C41 N40 Rh1 176.9(4) . . ? N40 C41 C42 178.7(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Cl51 C50 Cl53 110.3(5) . . ? Cl51 C50 Cl52 112.3(5) . . ? Cl53 C50 Cl52 112.0(4) . . ? Cl51 C50 H50A 107.3 . . ? Cl53 C50 H50A 107.3 . . ? Cl52 C50 H50A 107.3 . . ? Cl62 C60 Cl63 111.5(4) . . ? Cl62 C60 Cl61 110.3(4) . . ? Cl63 C60 Cl61 109.6(4) . . ? Cl62 C60 H60A 108.5 . . ? Cl63 C60 H60A 108.5 . . ? Cl61 C60 H60A 108.5 . . ? Cl71 C70 Cl73 111.8(4) . . ? Cl71 C70 Cl72 110.1(4) . . ? Cl73 C70 Cl72 108.9(4) . . ? Cl71 C70 H70A 108.6 . . ? Cl73 C70 H70A 108.6 . . ? Cl72 C70 H70A 108.6 . . ? Cl81 C80 Cl83 111.7(4) . . ? Cl81 C80 Cl82 110.5(4) . . ? Cl83 C80 Cl82 109.1(4) . . ? Cl81 C80 H80A 108.5 . . ? Cl83 C80 H80A 108.5 . . ? Cl82 C80 H80A 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 Rh1 N1 C2 -1.2(4) . . . . ? N40 Rh1 N1 C2 58(29) . . . . ? N8 Rh1 N1 C2 178.8(4) . . . . ? Cl2 Rh1 N1 C2 -93.1(4) . . . . ? Cl1 Rh1 N1 C2 87.0(4) . . . . ? C32 Rh1 N1 C6 -174.2(4) . . . . ? N40 Rh1 N1 C6 -115(28) . . . . ? N8 Rh1 N1 C6 5.8(4) . . . . ? Cl2 Rh1 N1 C6 93.9(4) . . . . ? Cl1 Rh1 N1 C6 -85.9(4) . . . . ? C6 N1 C2 C3 -3.3(7) . . . . ? Rh1 N1 C2 C3 -175.8(4) . . . . ? C6 N1 C2 C31 174.1(4) . . . . ? Rh1 N1 C2 C31 1.6(6) . . . . ? N1 C2 C3 C4 5.7(7) . . . . ? C31 C2 C3 C4 -171.3(5) . . . . ? N1 C2 C3 C25 -177.4(5) . . . . ? C31 C2 C3 C25 5.6(8) . . . . ? C2 C3 C4 C5 -1.4(7) . . . . ? C25 C3 C4 C5 -178.5(5) . . . . ? C2 C3 C4 C19 178.0(5) . . . . ? C25 C3 C4 C19 1.0(7) . . . . ? C3 C4 C5 C6 -5.3(7) . . . . ? C19 C4 C5 C6 175.3(5) . . . . ? C3 C4 C5 C13 172.6(5) . . . . ? C19 C4 C5 C13 -6.9(7) . . . . ? C2 N1 C6 C5 -3.6(8) . . . . ? Rh1 N1 C6 C5 168.8(4) . . . . ? C2 N1 C6 C7 174.8(5) . . . . ? Rh1 N1 C6 C7 -12.7(6) . . . . ? C4 C5 C6 N1 7.8(7) . . . . ? C13 C5 C6 N1 -170.0(5) . . . . ? C4 C5 C6 C7 -170.4(5) . . . . ? C13 C5 C6 C7 11.8(8) . . . . ? N1 C6 C7 N8 15.2(7) . . . . ? C5 C6 C7 N8 -166.5(5) . . . . ? N1 C6 C7 C12 -162.0(5) . . . . ? C5 C6 C7 C12 16.3(9) . . . . ? C12 C7 N8 C9 -2.9(8) . . . . ? C6 C7 N8 C9 179.8(5) . . . . ? C12 C7 N8 Rh1 167.1(4) . . . . ? C6 C7 N8 Rh1 -10.1(5) . . . . ? N1 Rh1 N8 C9 171.8(5) . . . . ? C32 Rh1 N8 C9 171.9(6) . . . . ? N40 Rh1 N8 C9 -8.5(5) . . . . ? Cl2 Rh1 N8 C9 80.2(5) . . . . ? Cl1 Rh1 N8 C9 -100.2(5) . . . . ? N1 Rh1 N8 C7 2.9(3) . . . . ? C32 Rh1 N8 C7 3.0(8) . . . . ? N40 Rh1 N8 C7 -177.5(3) . . . . ? Cl2 Rh1 N8 C7 -88.7(3) . . . . ? Cl1 Rh1 N8 C7 90.9(3) . . . . ? C7 N8 C9 C10 -0.3(8) . . . . ? Rh1 N8 C9 C10 -168.4(4) . . . . ? N8 C9 C10 C11 3.6(9) . . . . ? C9 C10 C11 C12 -3.5(9) . . . . ? C10 C11 C12 C7 0.4(9) . . . . ? N8 C7 C12 C11 2.9(8) . . . . ? C6 C7 C12 C11 179.9(5) . . . . ? C6 C5 C13 C14 65.1(7) . . . . ? C4 C5 C13 C14 -112.7(6) . . . . ? C6 C5 C13 C18 -115.2(6) . . . . ? C4 C5 C13 C18 67.0(7) . . . . ? C18 C13 C14 C15 0.0(8) . . . . ? C5 C13 C14 C15 179.7(5) . . . . ? C13 C14 C15 C16 0.7(9) . . . . ? C14 C15 C16 C17 -1.1(9) . . . . ? C15 C16 C17 C18 0.9(10) . . . . ? C16 C17 C18 C13 -0.2(9) . . . . ? C14 C13 C18 C17 -0.2(8) . . . . ? C5 C13 C18 C17 -179.9(5) . . . . ? C5 C4 C19 C20 74.3(7) . . . . ? C3 C4 C19 C20 -105.1(6) . . . . ? C5 C4 C19 C24 -106.7(6) . . . . ? C3 C4 C19 C24 73.9(7) . . . . ? C24 C19 C20 C21 0.2(9) . . . . ? C4 C19 C20 C21 179.2(6) . . . . ? C19 C20 C21 C22 0.7(10) . . . . ? C20 C21 C22 C23 -1.6(10) . . . . ? C21 C22 C23 C24 1.5(11) . . . . ? C22 C23 C24 C19 -0.6(10) . . . . ? C20 C19 C24 C23 -0.3(9) . . . . ? C4 C19 C24 C23 -179.2(6) . . . . ? C2 C3 C25 C30 85.3(7) . . . . ? C4 C3 C25 C30 -97.8(6) . . . . ? C2 C3 C25 C26 -96.6(6) . . . . ? C4 C3 C25 C26 80.3(7) . . . . ? C30 C25 C26 C27 1.3(9) . . . . ? C3 C25 C26 C27 -176.8(5) . . . . ? C25 C26 C27 C28 0.2(10) . . . . ? C26 C27 C28 C29 -1.5(11) . . . . ? C27 C28 C29 C30 1.1(11) . . . . ? C28 C29 C30 C25 0.4(10) . . . . ? C26 C25 C30 C29 -1.6(9) . . . . ? C3 C25 C30 C29 176.5(6) . . . . ? N1 C2 C31 C36 -176.4(5) . . . . ? C3 C2 C31 C36 0.7(9) . . . . ? N1 C2 C31 C32 -1.2(6) . . . . ? C3 C2 C31 C32 175.9(5) . . . . ? C36 C31 C32 C33 -1.0(8) . . . . ? C2 C31 C32 C33 -176.7(5) . . . . ? C36 C31 C32 Rh1 175.9(4) . . . . ? C2 C31 C32 Rh1 0.3(6) . . . . ? N1 Rh1 C32 C33 177.0(5) . . . . ? N40 Rh1 C32 C33 -2.7(5) . . . . ? N8 Rh1 C32 C33 176.9(5) . . . . ? Cl2 Rh1 C32 C33 -92.0(5) . . . . ? Cl1 Rh1 C32 C33 88.5(5) . . . . ? N1 Rh1 C32 C31 0.4(4) . . . . ? N40 Rh1 C32 C31 -179.2(4) . . . . ? N8 Rh1 C32 C31 0.3(9) . . . . ? Cl2 Rh1 C32 C31 91.5(4) . . . . ? Cl1 Rh1 C32 C31 -88.1(4) . . . . ? C31 C32 C33 C34 2.0(8) . . . . ? Rh1 C32 C33 C34 -174.4(4) . . . . ? C32 C33 C34 C35 -1.4(9) . . . . ? C33 C34 C35 C36 -0.2(9) . . . . ? C34 C35 C36 C31 1.1(9) . . . . ? C32 C31 C36 C35 -0.5(8) . . . . ? C2 C31 C36 C35 174.6(5) . . . . ? N1 Rh1 N40 C41 -173(100) . . . . ? C32 Rh1 N40 C41 -114(9) . . . . ? N8 Rh1 N40 C41 66(9) . . . . ? Cl2 Rh1 N40 C41 -22(9) . . . . ? Cl1 Rh1 N40 C41 158(9) . . . . ? Rh1 N40 C41 C42 145(25) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.063 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.117 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 644546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H29 Cl N4 Rh), 2(F6 P), 4(C H Cl3), C H Cl3' _chemical_formula_sum 'C81 H63 Cl17 F12 N8 P2 Rh2' _chemical_formula_weight 2246.80 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 12.6221(8) _cell_length_b 34.842(2) _cell_length_c 11.6836(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.2170(10) _cell_angle_gamma 90.00 _cell_volume 4821.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8178 _exptl_absorpt_correction_T_max 0.8981 _exptl_absorpt_process_details 'blessing Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41199 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9479 _reflns_number_gt 8315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+15.4517P] 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 9479 _refine_ls_number_parameters 607 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1763 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.24944(3) 0.029122(9) 0.64894(3) 0.02895(13) Uani 1 1 d . . . N1 N 0.3113(3) 0.08142(10) 0.6723(3) 0.0267(7) Uani 1 1 d . . . C2 C 0.2445(4) 0.10948(13) 0.6900(4) 0.0310(9) Uani 1 1 d . . . C3 C 0.2832(4) 0.14769(13) 0.6966(4) 0.0316(9) Uani 1 1 d . . . C4 C 0.3854(4) 0.15500(12) 0.6804(4) 0.0298(9) Uani 1 1 d . . . C5 C 0.4508(4) 0.12507(13) 0.6580(4) 0.0302(9) Uani 1 1 d . . . C6 C 0.4126(4) 0.08746(12) 0.6601(4) 0.0279(9) Uani 1 1 d . . . C7 C 0.4734(4) 0.05136(12) 0.6522(4) 0.0282(9) Uani 1 1 d . . . N8 N 0.4120(3) 0.01842(11) 0.6408(3) 0.0313(8) Uani 1 1 d . . . C9 C 0.4611(4) -0.01590(13) 0.6377(4) 0.0339(10) Uani 1 1 d . . . H9A H 0.4176 -0.0386 0.6309 0.041 Uiso 1 1 calc R . . C10 C 0.5714(4) -0.01914(14) 0.6441(4) 0.0353(10) Uani 1 1 d . . . H10A H 0.6031 -0.0435 0.6391 0.042 Uiso 1 1 calc R . . C11 C 0.6349(4) 0.01362(14) 0.6579(4) 0.0360(10) Uani 1 1 d . . . H11A H 0.7116 0.0120 0.6633 0.043 Uiso 1 1 calc R . . C12 C 0.5870(4) 0.04905(13) 0.6639(4) 0.0342(10) Uani 1 1 d . . . H12A H 0.6315 0.0717 0.6759 0.041 Uiso 1 1 calc R . . C13 C 0.5512(4) 0.13564(13) 0.6257(5) 0.0364(11) Uani 1 1 d . . . C14 C 0.6460(5) 0.15284(15) 0.7119(6) 0.0479(13) Uani 1 1 d . . . H14A H 0.6503 0.1554 0.7943 0.057 Uiso 1 1 calc R . . C15 C 0.7326(6) 0.16594(18) 0.6764(9) 0.071(2) Uani 1 1 d . . . H15A H 0.7963 0.1778 0.7347 0.085 Uiso 1 1 calc R . . C16 C 0.7284(6) 0.1622(2) 0.5585(9) 0.077(2) Uani 1 1 d . . . H16A H 0.7888 0.1716 0.5356 0.092 Uiso 1 1 calc R . . C17 C 0.6371(7) 0.1449(2) 0.4725(7) 0.070(2) Uani 1 1 d . . . H17A H 0.6350 0.1421 0.3909 0.084 Uiso 1 1 calc R . . C18 C 0.5475(5) 0.13138(17) 0.5059(5) 0.0502(13) Uani 1 1 d . . . H18A H 0.4845 0.1194 0.4471 0.060 Uiso 1 1 calc R . . C19 C 0.4254(4) 0.19578(13) 0.6845(5) 0.0344(10) Uani 1 1 d . . . C20 C 0.4813(5) 0.21253(14) 0.7956(5) 0.0440(12) Uani 1 1 d . . . H20A H 0.4943 0.1981 0.8682 0.053 Uiso 1 1 calc R . . C21 C 0.5190(5) 0.25020(16) 0.8032(7) 0.0573(16) Uani 1 1 d . . . H21A H 0.5572 0.2616 0.8804 0.069 Uiso 1 1 calc R . . C22 C 0.5007(6) 0.27086(17) 0.6983(8) 0.0642(18) Uani 1 1 d . . . H22A H 0.5261 0.2967 0.7026 0.077 Uiso 1 1 calc R . . C23 C 0.4456(6) 0.25428(18) 0.5870(7) 0.0618(18) Uani 1 1 d . . . H23A H 0.4334 0.2687 0.5145 0.074 Uiso 1 1 calc R . . C24 C 0.4074(5) 0.21671(16) 0.5792(5) 0.0471(13) Uani 1 1 d . . . H24A H 0.3692 0.2055 0.5019 0.056 Uiso 1 1 calc R . . C25 C 0.2140(4) 0.18047(14) 0.7142(5) 0.0400(11) Uani 1 1 d . . . C26 C 0.1343(5) 0.19789(18) 0.6152(7) 0.0587(16) Uani 1 1 d . . . H26A H 0.1258 0.1900 0.5347 0.070 Uiso 1 1 calc R . . C27 C 0.0672(7) 0.2268(2) 0.6335(9) 0.080(2) Uani 1 1 d . . . H27A H 0.0112 0.2383 0.5657 0.096 Uiso 1 1 calc R . . C28 C 0.0811(7) 0.2387(2) 0.7489(10) 0.083(2) Uani 1 1 d . . . H28A H 0.0343 0.2586 0.7606 0.099 Uiso 1 1 calc R . . C29 C 0.1610(6) 0.22262(19) 0.8483(8) 0.070(2) Uani 1 1 d . . . H29A H 0.1701 0.2313 0.9282 0.084 Uiso 1 1 calc R . . C30 C 0.2287(5) 0.19342(16) 0.8311(6) 0.0478(13) Uani 1 1 d . . . H30A H 0.2852 0.1823 0.8993 0.057 Uiso 1 1 calc R . . C31 C 0.1364(4) 0.09498(14) 0.6972(4) 0.0343(10) Uani 1 1 d . . . C36 C 0.0569(4) 0.11668(16) 0.7275(5) 0.0450(12) Uani 1 1 d . . . H36A H 0.0689 0.1433 0.7439 0.054 Uiso 1 1 calc R . . C35 C -0.0393(5) 0.09923(18) 0.7333(6) 0.0560(15) Uani 1 1 d . . . H35A H -0.0920 0.1137 0.7571 0.067 Uiso 1 1 calc R . . C34 C -0.0593(5) 0.06079(18) 0.7049(6) 0.0547(15) Uani 1 1 d . . . H34A H -0.1272 0.0492 0.7057 0.066 Uiso 1 1 calc R . . C33 C 0.0192(4) 0.03931(15) 0.6755(5) 0.0416(12) Uani 1 1 d . . . H33A H 0.0056 0.0128 0.6571 0.050 Uiso 1 1 calc R . . C32 C 0.1162(4) 0.05573(13) 0.6724(4) 0.0309(9) Uani 1 1 d . . . Cl1 Cl 0.17543(10) 0.04151(3) 0.44182(10) 0.0362(3) Uani 1 1 d . . . N40 N 0.1841(3) -0.02444(11) 0.6239(4) 0.0344(9) Uani 1 1 d . . . C41 C 0.1477(5) -0.05441(15) 0.6184(5) 0.0420(12) Uani 1 1 d . . . C42 C 0.0996(5) -0.09293(15) 0.6106(6) 0.0566(16) Uani 1 1 d . . . H42A H 0.0218 -0.0911 0.6096 0.085 Uiso 1 1 calc R . . H42B H 0.1448 -0.1081 0.6813 0.085 Uiso 1 1 calc R . . H42C H 0.1000 -0.1054 0.5356 0.085 Uiso 1 1 calc R . . N50 N 0.3092(3) 0.01908(11) 0.8299(4) 0.0313(8) Uani 1 1 d . . . C51 C 0.3351(5) 0.01396(16) 0.9292(5) 0.0426(12) Uani 1 1 d . . . C52 C 0.3695(7) 0.0077(2) 1.0594(6) 0.074(2) Uani 1 1 d . . . H52A H 0.4270 0.0267 1.1020 0.111 Uiso 1 1 calc R . . H52B H 0.4008 -0.0182 1.0790 0.111 Uiso 1 1 calc R . . H52C H 0.3039 0.0105 1.0855 0.111 Uiso 1 1 calc R . . P1 P 0.55318(16) 0.10684(5) 0.07194(16) 0.0588(4) Uani 1 1 d . . . F1 F 0.475(2) 0.0854(5) -0.0354(10) 0.137(8) Uani 0.67(3) 1 d P A 1 F2 F 0.4765(15) 0.1448(4) 0.0427(12) 0.115(5) Uani 0.67(3) 1 d P A 1 F3 F 0.6371(18) 0.0727(4) 0.1186(13) 0.140(8) Uani 0.67(3) 1 d P A 1 F4 F 0.4923(5) 0.0952(2) 0.1650(6) 0.122(2) Uani 1 1 d . A . F5 F 0.6391(12) 0.1321(5) 0.1819(8) 0.096(4) Uani 0.67(3) 1 d P A 1 F6 F 0.6133(6) 0.1215(2) -0.0171(6) 0.139(2) Uani 1 1 d . A . F1A F 0.428(2) 0.1020(11) -0.021(3) 0.127(11) Uani 0.33(3) 1 d P A 2 F2A F 0.538(3) 0.1470(6) 0.066(4) 0.191(18) Uani 0.33(3) 1 d P A 2 F3A F 0.567(3) 0.0634(6) 0.065(5) 0.180(17) Uani 0.33(3) 1 d P A 2 F5A F 0.6674(16) 0.1097(9) 0.166(2) 0.101(9) Uani 0.33(3) 1 d P A 2 C60 C 0.8028(9) 0.1894(4) 0.1373(12) 0.151(6) Uani 1 1 d . . . H60A H 0.7376 0.1711 0.1107 0.181 Uiso 1 1 calc R . . Cl61 Cl 0.8324(4) 0.20100(14) 0.2942(4) 0.1782(18) Uani 1 1 d . . . Cl62 Cl 0.7684(3) 0.22795(16) 0.0566(6) 0.264(4) Uani 1 1 d . . . Cl63 Cl 0.9217(4) 0.16561(11) 0.1404(6) 0.188(2) Uani 1 1 d . . . C70 C 0.2609(7) 0.1376(3) 0.1719(7) 0.084(2) Uani 1 1 d D . . H70A H 0.3412 0.1342 0.1773 0.101 Uiso 1 1 calc R . . Cl71 Cl 0.23771(18) 0.11084(7) 0.2886(2) 0.0888(7) Uani 1 1 d D . . Cl72 Cl 0.2367(3) 0.18651(8) 0.1918(3) 0.1172(9) Uani 1 1 d D . . Cl73 Cl 0.1733(3) 0.12184(10) 0.0312(2) 0.1309(12) Uani 1 1 d D . . C80 C 0.9650(19) 0.0352(6) -0.001(2) 0.23(2) Uani 0.50 1 d PD . 1 H80A H 1.0027 0.0476 -0.0496 0.275 Uiso 0.50 1 d PR . 1 Cl81 Cl 0.8513(8) 0.0634(3) -0.0131(10) 0.181(4) Uani 0.50 1 d PD B 1 Cl82 Cl 0.9383(9) -0.0110(3) -0.0584(9) 0.169(3) Uani 0.50 1 d PD . 1 Cl83 Cl 1.0581(13) 0.0349(4) 0.1404(8) 0.249(7) Uani 0.50 1 d PD . 1 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 Rh1 0.0333(2) 0.02455(19) 0.02439(19) -0.00072(13) 0.00419(14) -0.00434(14) N1 0.0276(18) 0.0253(18) 0.0243(18) 0.0007(14) 0.0050(14) -0.0005(14) C2 0.031(2) 0.032(2) 0.026(2) -0.0016(18) 0.0054(18) -0.0010(18) C3 0.034(2) 0.029(2) 0.028(2) 0.0013(18) 0.0063(18) 0.0016(18) C4 0.036(2) 0.025(2) 0.026(2) 0.0009(17) 0.0067(18) -0.0003(17) C5 0.033(2) 0.028(2) 0.026(2) 0.0002(17) 0.0062(18) -0.0005(18) C6 0.031(2) 0.027(2) 0.022(2) 0.0002(16) 0.0056(17) -0.0005(17) C7 0.038(2) 0.021(2) 0.025(2) -0.0016(16) 0.0089(18) -0.0027(17) N8 0.039(2) 0.0265(19) 0.0254(18) -0.0011(15) 0.0068(16) 0.0013(16) C9 0.047(3) 0.026(2) 0.025(2) -0.0002(17) 0.008(2) 0.0009(19) C10 0.044(3) 0.032(2) 0.026(2) -0.0025(18) 0.007(2) 0.009(2) C11 0.037(2) 0.038(3) 0.031(2) -0.001(2) 0.009(2) 0.004(2) C12 0.038(2) 0.029(2) 0.034(2) -0.0012(19) 0.010(2) -0.0031(19) C13 0.038(3) 0.025(2) 0.049(3) 0.006(2) 0.019(2) 0.0018(19) C14 0.041(3) 0.034(3) 0.070(4) -0.009(2) 0.019(3) -0.003(2) C15 0.045(3) 0.044(3) 0.128(7) -0.008(4) 0.036(4) -0.008(3) C16 0.062(4) 0.056(4) 0.134(8) 0.027(4) 0.062(5) 0.005(3) C17 0.082(5) 0.070(4) 0.078(5) 0.033(4) 0.056(4) 0.024(4) C18 0.057(3) 0.050(3) 0.048(3) 0.012(3) 0.023(3) 0.008(3) C19 0.033(2) 0.029(2) 0.043(3) 0.004(2) 0.014(2) 0.0006(19) C20 0.051(3) 0.027(2) 0.052(3) 0.000(2) 0.015(3) -0.002(2) C21 0.060(4) 0.032(3) 0.077(4) -0.009(3) 0.020(3) -0.009(3) C22 0.064(4) 0.027(3) 0.106(6) 0.005(3) 0.036(4) -0.007(3) C23 0.073(4) 0.042(3) 0.078(5) 0.032(3) 0.035(4) 0.009(3) C24 0.054(3) 0.039(3) 0.046(3) 0.013(2) 0.015(3) 0.006(2) C25 0.039(3) 0.028(2) 0.054(3) 0.001(2) 0.017(2) 0.001(2) C26 0.056(4) 0.051(4) 0.069(4) 0.017(3) 0.021(3) 0.017(3) C27 0.073(5) 0.063(4) 0.102(6) 0.023(4) 0.027(4) 0.034(4) C28 0.076(5) 0.049(4) 0.131(8) 0.002(4) 0.046(5) 0.026(4) C29 0.078(5) 0.045(4) 0.097(6) -0.019(4) 0.045(4) -0.002(3) C30 0.045(3) 0.038(3) 0.062(4) -0.010(3) 0.019(3) -0.002(2) C31 0.034(2) 0.032(2) 0.033(2) -0.0041(19) 0.0057(19) -0.0032(19) C36 0.038(3) 0.037(3) 0.059(3) -0.008(2) 0.014(2) -0.003(2) C35 0.040(3) 0.050(3) 0.080(4) -0.005(3) 0.024(3) -0.001(2) C34 0.032(3) 0.058(4) 0.074(4) -0.005(3) 0.018(3) -0.014(2) C33 0.038(3) 0.036(3) 0.043(3) 0.000(2) 0.005(2) -0.008(2) C32 0.032(2) 0.033(2) 0.022(2) 0.0027(17) 0.0025(17) -0.0032(18) Cl1 0.0416(6) 0.0360(6) 0.0257(5) 0.0014(4) 0.0048(5) -0.0016(5) N40 0.040(2) 0.027(2) 0.030(2) 0.0017(15) 0.0050(17) -0.0031(17) C41 0.045(3) 0.035(3) 0.038(3) 0.000(2) 0.003(2) -0.001(2) C42 0.053(3) 0.028(3) 0.073(4) 0.004(3) 0.003(3) -0.010(2) N50 0.037(2) 0.0275(19) 0.029(2) -0.0026(15) 0.0109(16) -0.0055(15) C51 0.044(3) 0.046(3) 0.033(3) 0.001(2) 0.008(2) -0.006(2) C52 0.086(5) 0.094(6) 0.034(3) 0.012(3) 0.008(3) -0.009(4) P1 0.0707(11) 0.0385(8) 0.0528(9) 0.0032(7) 0.0032(8) -0.0030(7) F1 0.205(19) 0.106(11) 0.059(5) -0.015(6) -0.007(8) -0.096(12) F2 0.114(10) 0.088(7) 0.129(9) 0.036(6) 0.023(7) 0.042(7) F3 0.172(15) 0.099(11) 0.129(10) 0.031(8) 0.027(9) 0.075(11) F4 0.114(4) 0.151(6) 0.104(4) 0.018(4) 0.042(4) -0.015(4) F5 0.115(8) 0.090(9) 0.071(5) -0.017(5) 0.014(5) -0.038(7) F6 0.151(6) 0.174(7) 0.103(4) 0.015(4) 0.059(4) -0.028(5) F1A 0.082(12) 0.13(2) 0.13(2) 0.000(16) -0.007(11) 0.011(13) F2A 0.11(2) 0.035(9) 0.38(5) -0.042(16) 0.02(3) 0.004(11) F3A 0.11(2) 0.041(9) 0.33(5) -0.013(16) 0.00(2) 0.017(11) F5A 0.064(10) 0.093(19) 0.107(14) 0.005(13) -0.020(9) -0.017(11) C60 0.078(7) 0.165(12) 0.157(11) 0.052(9) -0.025(7) -0.067(8) Cl61 0.174(4) 0.187(4) 0.187(4) -0.033(3) 0.077(3) -0.081(3) Cl62 0.108(3) 0.224(5) 0.353(7) 0.177(5) -0.056(3) -0.052(3) Cl63 0.171(4) 0.099(2) 0.336(7) -0.017(3) 0.141(4) -0.029(2) C70 0.074(5) 0.092(6) 0.082(5) 0.027(5) 0.022(4) -0.019(4) Cl71 0.0770(12) 0.0970(15) 0.0914(14) 0.0456(12) 0.0280(11) 0.0099(11) Cl72 0.131(2) 0.0800(15) 0.136(2) 0.0329(15) 0.0403(18) -0.0144(14) Cl73 0.156(3) 0.128(2) 0.0835(16) 0.0286(15) 0.0100(16) -0.051(2) C80 0.16(3) 0.11(2) 0.27(4) 0.02(2) -0.12(3) 0.024(19) Cl81 0.178(7) 0.162(7) 0.249(10) -0.074(7) 0.133(8) -0.061(6) Cl82 0.222(10) 0.136(7) 0.141(7) -0.015(5) 0.052(7) -0.023(6) Cl83 0.367(18) 0.224(12) 0.105(6) 0.026(6) 0.016(8) -0.137(12) _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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:12.2(2), B:69.9(2), C:83.5(2), D:89.6(2), E:8.3(2) ; 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 Rh1 N1 1.964(4) . ? Rh1 N50 2.015(4) . ? Rh1 N40 2.020(4) . ? Rh1 C32 2.020(5) . ? Rh1 N8 2.119(4) . ? Rh1 Cl1 2.3136(11) . ? N1 C6 1.351(6) . ? N1 C2 1.353(6) . ? C2 C3 1.411(6) . ? C2 C31 1.484(7) . ? C3 C4 1.390(7) . ? C3 C25 1.495(7) . ? C4 C5 1.409(6) . ? C4 C19 1.503(6) . ? C5 C6 1.400(6) . ? C5 C13 1.488(7) . ? C6 C7 1.493(6) . ? C7 N8 1.366(6) . ? C7 C12 1.395(7) . ? N8 C9 1.353(6) . ? C9 C10 1.373(7) . ? C9 H9A 0.9500 . ? C10 C11 1.372(7) . ? C10 H10A 0.9500 . ? C11 C12 1.387(7) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.392(8) . ? C13 C14 1.405(8) . ? C14 C15 1.374(9) . ? C14 H14A 0.9500 . ? C15 C16 1.366(12) . ? C15 H15A 0.9500 . ? C16 C17 1.380(12) . ? C16 H16A 0.9500 . ? C17 C18 1.398(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.375(7) . ? C19 C24 1.379(7) . ? C20 C21 1.388(7) . ? C20 H20A 0.9500 . ? C21 C22 1.370(10) . ? C21 H21A 0.9500 . ? C22 C23 1.372(10) . ? C22 H22A 0.9500 . ? C23 C24 1.387(8) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.384(8) . ? C25 C30 1.388(8) . ? C26 C27 1.379(9) . ? C26 H26A 0.9500 . ? C27 C28 1.363(12) . ? C27 H27A 0.9500 . ? C28 C29 1.367(12) . ? C28 H28A 0.9500 . ? C29 C30 1.387(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.396(7) . ? C31 C32 1.403(6) . ? C36 C35 1.381(8) . ? C36 H36A 0.9500 . ? C35 C34 1.382(9) . ? C35 H35A 0.9500 . ? C34 C33 1.377(8) . ? C34 H34A 0.9500 . ? C33 C32 1.363(7) . ? C33 H33A 0.9500 . ? N40 C41 1.134(6) . ? C41 C42 1.462(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N50 C51 1.106(6) . ? C51 C52 1.447(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? P1 F2A 1.41(2) . ? P1 F5A 1.484(16) . ? P1 F1 1.501(9) . ? P1 F3A 1.53(2) . ? P1 F3 1.561(10) . ? P1 F6 1.570(6) . ? P1 F4 1.585(6) . ? P1 F1A 1.59(3) . ? P1 F2 1.606(11) . ? P1 F5 1.624(9) . ? C60 Cl62 1.613(13) . ? C60 Cl63 1.704(16) . ? C60 Cl61 1.786(15) . ? C60 H60A 1.0000 . ? C70 Cl73 1.724(9) . ? C70 Cl71 1.758(7) . ? C70 Cl72 1.761(10) . ? C70 H70A 1.0000 . ? C80 Cl82 1.448(19) 3_755 ? C80 Cl83 1.665(18) . ? C80 Cl81 1.704(18) . ? C80 Cl82 1.732(17) . ? C80 H80A 0.9600 . ? Cl82 Cl83 1.280(15) 3_755 ? Cl82 C80 1.448(19) 3_755 ? Cl82 Cl82 1.847(19) 3_755 ? Cl83 Cl82 1.280(15) 3_755 ? 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 Rh1 N50 91.63(15) . . ? N1 Rh1 N40 179.39(16) . . ? N50 Rh1 N40 88.71(15) . . ? N1 Rh1 C32 82.25(17) . . ? N50 Rh1 C32 87.95(16) . . ? N40 Rh1 C32 97.26(18) . . ? N1 Rh1 N8 79.92(15) . . ? N50 Rh1 N8 89.98(15) . . ? N40 Rh1 N8 100.59(16) . . ? C32 Rh1 N8 161.98(17) . . ? N1 Rh1 Cl1 88.28(11) . . ? N50 Rh1 Cl1 178.08(12) . . ? N40 Rh1 Cl1 91.37(11) . . ? C32 Rh1 Cl1 90.13(12) . . ? N8 Rh1 Cl1 91.89(10) . . ? C6 N1 C2 124.5(4) . . ? C6 N1 Rh1 118.4(3) . . ? C2 N1 Rh1 116.9(3) . . ? N1 C2 C3 117.9(4) . . ? N1 C2 C31 113.4(4) . . ? C3 C2 C31 128.7(4) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 C25 119.5(4) . . ? C2 C3 C25 121.4(4) . . ? C3 C4 C5 121.4(4) . . ? C3 C4 C19 119.1(4) . . ? C5 C4 C19 119.6(4) . . ? C6 C5 C4 117.5(4) . . ? C6 C5 C13 124.4(4) . . ? C4 C5 C13 118.0(4) . . ? N1 C6 C5 119.5(4) . . ? N1 C6 C7 113.6(4) . . ? C5 C6 C7 126.9(4) . . ? N8 C7 C12 119.4(4) . . ? N8 C7 C6 115.3(4) . . ? C12 C7 C6 125.2(4) . . ? C9 N8 C7 119.7(4) . . ? C9 N8 Rh1 128.0(3) . . ? C7 N8 Rh1 111.9(3) . . ? N8 C9 C10 122.4(4) . . ? N8 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C11 C10 C9 118.6(4) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 119.8(4) . . ? C11 C12 H12A 120.1 . . ? C7 C12 H12A 120.1 . . ? C18 C13 C14 119.4(5) . . ? C18 C13 C5 119.6(5) . . ? C14 C13 C5 120.8(5) . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C16 C15 C14 121.0(7) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 120.5(6) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C16 C17 C18 119.8(7) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C13 C18 C17 119.7(6) . . ? C13 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C20 C19 C24 119.3(5) . . ? C20 C19 C4 119.2(4) . . ? C24 C19 C4 121.4(5) . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C22 C21 C20 119.5(6) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 120.0(5) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.7(6) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C19 C24 C23 119.6(6) . . ? C19 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C26 C25 C30 119.4(5) . . ? C26 C25 C3 120.7(5) . . ? C30 C25 C3 119.9(5) . . ? C27 C26 C25 119.9(7) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C28 C27 C26 120.0(7) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 121.3(7) . . ? C27 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C28 C29 C30 119.2(7) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C29 C30 C25 120.1(6) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C36 C31 C32 119.0(5) . . ? C36 C31 C2 125.8(4) . . ? C32 C31 C2 115.2(4) . . ? C35 C36 C31 119.7(5) . . ? C35 C36 H36A 120.1 . . ? C31 C36 H36A 120.1 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C32 C33 C34 120.6(5) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C33 C32 C31 120.3(5) . . ? C33 C32 Rh1 127.5(4) . . ? C31 C32 Rh1 112.0(3) . . ? C41 N40 Rh1 175.0(4) . . ? N40 C41 C42 179.5(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C51 N50 Rh1 175.5(4) . . ? N50 C51 C52 179.3(7) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? F2A P1 F5A 92.8(14) . . ? F2A P1 F1 114.4(15) . . ? F5A P1 F1 147.5(12) . . ? F2A P1 F3A 174(3) . . ? F5A P1 F3A 90.1(13) . . ? F1 P1 F3A 61.4(14) . . ? F2A P1 F3 146.8(14) . . ? F5A P1 F3 54.9(11) . . ? F1 P1 F3 94.8(9) . . ? F3A P1 F3 35.4(9) . . ? F2A P1 F6 74.2(18) . . ? F5A P1 F6 84.3(10) . . ? F1 P1 F6 86.5(7) . . ? F3A P1 F6 101.4(17) . . ? F3 P1 F6 93.1(7) . . ? F2A P1 F4 101.7(18) . . ? F5A P1 F4 94.9(11) . . ? F1 P1 F4 96.3(7) . . ? F3A P1 F4 82.8(16) . . ? F3 P1 F4 89.8(7) . . ? F6 P1 F4 175.8(4) . . ? F2A P1 F1A 89.3(15) . . ? F5A P1 F1A 175.7(16) . . ? F1 P1 F1A 32.9(10) . . ? F3A P1 F1A 88.1(13) . . ? F3 P1 F1A 123.5(12) . . ? F6 P1 F1A 99.9(14) . . ? F4 P1 F1A 81.0(14) . . ? F2A P1 F2 27.3(12) . . ? F5A P1 F2 117.5(12) . . ? F1 P1 F2 93.3(8) . . ? F3A P1 F2 151.4(11) . . ? F3 P1 F2 171.7(7) . . ? F6 P1 F2 89.1(6) . . ? F4 P1 F2 87.5(6) . . ? F1A P1 F2 63.8(12) . . ? F2A P1 F5 62.8(14) . . ? F5A P1 F5 33.4(10) . . ? F1 P1 F5 176.3(6) . . ? F3A P1 F5 121.2(14) . . ? F3 P1 F5 87.2(7) . . ? F6 P1 F5 90.3(5) . . ? F4 P1 F5 86.9(5) . . ? F1A P1 F5 146.6(12) . . ? F2 P1 F5 84.8(6) . . ? Cl62 C60 Cl63 118.4(9) . . ? Cl62 C60 Cl61 109.2(10) . . ? Cl63 C60 Cl61 102.6(6) . . ? Cl62 C60 H60A 108.8 . . ? Cl63 C60 H60A 108.8 . . ? Cl61 C60 H60A 108.8 . . ? Cl73 C70 Cl71 110.3(4) . . ? Cl73 C70 Cl72 110.5(5) . . ? Cl71 C70 Cl72 109.1(5) . . ? Cl73 C70 H70A 109.0 . . ? Cl71 C70 H70A 109.0 . . ? Cl72 C70 H70A 109.0 . . ? Cl82 C80 Cl83 47.9(8) 3_755 . ? Cl82 C80 Cl81 157(2) 3_755 . ? Cl83 C80 Cl81 111.8(16) . . ? Cl82 C80 Cl82 70.4(11) 3_755 . ? Cl83 C80 Cl82 110.7(13) . . ? Cl81 C80 Cl82 117.3(14) . . ? Cl82 C80 H80A 92.2 3_755 . ? Cl83 C80 H80A 105.4 . . ? Cl81 C80 H80A 105.5 . . ? Cl82 C80 H80A 105.1 . . ? Cl83 Cl82 C80 75.0(11) 3_755 3_755 ? Cl83 Cl82 C80 147.2(14) 3_755 . ? C80 Cl82 C80 109.6(11) 3_755 . ? Cl83 Cl82 Cl82 125.8(13) 3_755 3_755 ? C80 Cl82 Cl82 62.0(9) 3_755 3_755 ? C80 Cl82 Cl82 47.6(7) . 3_755 ? Cl82 Cl83 C80 57.1(9) 3_755 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N50 Rh1 N1 C6 96.6(3) . . . . ? N40 Rh1 N1 C6 -140(15) . . . . ? C32 Rh1 N1 C6 -175.7(3) . . . . ? N8 Rh1 N1 C6 6.9(3) . . . . ? Cl1 Rh1 N1 C6 -85.4(3) . . . . ? N50 Rh1 N1 C2 -88.7(3) . . . . ? N40 Rh1 N1 C2 35(15) . . . . ? C32 Rh1 N1 C2 -1.0(3) . . . . ? N8 Rh1 N1 C2 -178.4(3) . . . . ? Cl1 Rh1 N1 C2 89.4(3) . . . . ? C6 N1 C2 C3 -0.3(6) . . . . ? Rh1 N1 C2 C3 -174.7(3) . . . . ? C6 N1 C2 C31 178.5(4) . . . . ? Rh1 N1 C2 C31 4.1(5) . . . . ? N1 C2 C3 C4 2.3(6) . . . . ? C31 C2 C3 C4 -176.2(4) . . . . ? N1 C2 C3 C25 179.2(4) . . . . ? C31 C2 C3 C25 0.6(8) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C25 C3 C4 C5 -177.1(4) . . . . ? C2 C3 C4 C19 178.6(4) . . . . ? C25 C3 C4 C19 1.7(7) . . . . ? C3 C4 C5 C6 -3.9(6) . . . . ? C19 C4 C5 C6 177.4(4) . . . . ? C3 C4 C5 C13 172.2(4) . . . . ? C19 C4 C5 C13 -6.6(6) . . . . ? C2 N1 C6 C5 -3.9(6) . . . . ? Rh1 N1 C6 C5 170.4(3) . . . . ? C2 N1 C6 C7 175.1(4) . . . . ? Rh1 N1 C6 C7 -10.6(5) . . . . ? C4 C5 C6 N1 5.8(6) . . . . ? C13 C5 C6 N1 -169.9(4) . . . . ? C4 C5 C6 C7 -173.0(4) . . . . ? C13 C5 C6 C7 11.3(7) . . . . ? N1 C6 C7 N8 9.1(5) . . . . ? C5 C6 C7 N8 -172.1(4) . . . . ? N1 C6 C7 C12 -166.4(4) . . . . ? C5 C6 C7 C12 12.4(7) . . . . ? C12 C7 N8 C9 -1.7(6) . . . . ? C6 C7 N8 C9 -177.5(4) . . . . ? C12 C7 N8 Rh1 172.2(3) . . . . ? C6 C7 N8 Rh1 -3.6(5) . . . . ? N1 Rh1 N8 C9 171.8(4) . . . . ? N50 Rh1 N8 C9 80.2(4) . . . . ? N40 Rh1 N8 C9 -8.5(4) . . . . ? C32 Rh1 N8 C9 163.5(5) . . . . ? Cl1 Rh1 N8 C9 -100.3(4) . . . . ? N1 Rh1 N8 C7 -1.4(3) . . . . ? N50 Rh1 N8 C7 -93.0(3) . . . . ? N40 Rh1 N8 C7 178.3(3) . . . . ? C32 Rh1 N8 C7 -9.7(7) . . . . ? Cl1 Rh1 N8 C7 86.5(3) . . . . ? C7 N8 C9 C10 -0.9(7) . . . . ? Rh1 N8 C9 C10 -173.6(3) . . . . ? N8 C9 C10 C11 2.0(7) . . . . ? C9 C10 C11 C12 -0.6(7) . . . . ? C10 C11 C12 C7 -1.9(7) . . . . ? N8 C7 C12 C11 3.1(7) . . . . ? C6 C7 C12 C11 178.4(4) . . . . ? C6 C5 C13 C18 69.4(6) . . . . ? C4 C5 C13 C18 -106.3(5) . . . . ? C6 C5 C13 C14 -116.0(5) . . . . ? C4 C5 C13 C14 68.3(6) . . . . ? C18 C13 C14 C15 1.4(8) . . . . ? C5 C13 C14 C15 -173.2(5) . . . . ? C13 C14 C15 C16 -0.6(9) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C15 C16 C17 C18 0.7(11) . . . . ? C14 C13 C18 C17 -1.2(8) . . . . ? C5 C13 C18 C17 173.5(5) . . . . ? C16 C17 C18 C13 0.1(9) . . . . ? C3 C4 C19 C20 83.2(6) . . . . ? C5 C4 C19 C20 -98.0(6) . . . . ? C3 C4 C19 C24 -96.9(6) . . . . ? C5 C4 C19 C24 81.8(6) . . . . ? C24 C19 C20 C21 0.5(8) . . . . ? C4 C19 C20 C21 -179.6(5) . . . . ? C19 C20 C21 C22 -0.3(9) . . . . ? C20 C21 C22 C23 -0.1(10) . . . . ? C21 C22 C23 C24 0.3(10) . . . . ? C20 C19 C24 C23 -0.2(8) . . . . ? C4 C19 C24 C23 179.9(5) . . . . ? C22 C23 C24 C19 -0.2(9) . . . . ? C4 C3 C25 C26 89.6(6) . . . . ? C2 C3 C25 C26 -87.2(6) . . . . ? C4 C3 C25 C30 -91.0(6) . . . . ? C2 C3 C25 C30 92.1(6) . . . . ? C30 C25 C26 C27 -2.7(9) . . . . ? C3 C25 C26 C27 176.6(6) . . . . ? C25 C26 C27 C28 1.5(12) . . . . ? C26 C27 C28 C29 0.1(13) . . . . ? C27 C28 C29 C30 -0.4(12) . . . . ? C28 C29 C30 C25 -0.9(10) . . . . ? C26 C25 C30 C29 2.4(9) . . . . ? C3 C25 C30 C29 -176.9(5) . . . . ? N1 C2 C31 C36 172.9(5) . . . . ? C3 C2 C31 C36 -8.5(8) . . . . ? N1 C2 C31 C32 -6.2(6) . . . . ? C3 C2 C31 C32 172.4(4) . . . . ? C32 C31 C36 C35 0.5(8) . . . . ? C2 C31 C36 C35 -178.6(5) . . . . ? C31 C36 C35 C34 -2.5(10) . . . . ? C36 C35 C34 C33 2.7(10) . . . . ? C35 C34 C33 C32 -0.9(9) . . . . ? C34 C33 C32 C31 -1.2(8) . . . . ? C34 C33 C32 Rh1 173.2(4) . . . . ? C36 C31 C32 C33 1.4(7) . . . . ? C2 C31 C32 C33 -179.5(4) . . . . ? C36 C31 C32 Rh1 -173.8(4) . . . . ? C2 C31 C32 Rh1 5.3(5) . . . . ? N1 Rh1 C32 C33 -177.3(4) . . . . ? N50 Rh1 C32 C33 -85.3(4) . . . . ? N40 Rh1 C32 C33 3.1(4) . . . . ? N8 Rh1 C32 C33 -169.0(4) . . . . ? Cl1 Rh1 C32 C33 94.5(4) . . . . ? N1 Rh1 C32 C31 -2.5(3) . . . . ? N50 Rh1 C32 C31 89.4(3) . . . . ? N40 Rh1 C32 C31 177.9(3) . . . . ? N8 Rh1 C32 C31 5.8(7) . . . . ? Cl1 Rh1 C32 C31 -90.7(3) . . . . ? N1 Rh1 N40 C41 -101(15) . . . . ? N50 Rh1 N40 C41 22(5) . . . . ? C32 Rh1 N40 C41 -65(5) . . . . ? N8 Rh1 N40 C41 112(5) . . . . ? Cl1 Rh1 N40 C41 -156(5) . . . . ? Rh1 N40 C41 C42 105(72) . . . . ? N1 Rh1 N50 C51 102(5) . . . . ? N40 Rh1 N50 C51 -78(5) . . . . ? C32 Rh1 N50 C51 20(5) . . . . ? N8 Rh1 N50 C51 -178(100) . . . . ? Cl1 Rh1 N50 C51 15(8) . . . . ? Rh1 N50 C51 C52 -95(100) . . . . ? Cl82 C80 Cl82 Cl83 -93(2) 3_755 . . 3_755 ? Cl83 C80 Cl82 Cl83 -119(2) . . . 3_755 ? Cl81 C80 Cl82 Cl83 111(3) . . . 3_755 ? Cl82 C80 Cl82 C80 0.0 3_755 . . 3_755 ? Cl83 C80 Cl82 C80 -26.4(11) . . . 3_755 ? Cl81 C80 Cl82 C80 -156(3) . . . 3_755 ? Cl83 C80 Cl82 Cl82 -26.4(11) . . . 3_755 ? Cl81 C80 Cl82 Cl82 -156(3) . . . 3_755 ? Cl81 C80 Cl83 Cl82 167(2) . . . 3_755 ? Cl82 C80 Cl83 Cl82 34.4(14) . . . 3_755 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.330 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.110 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 644547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H46 Cl4 N4 Rh2, 6(C H Cl3)' _chemical_formula_sum 'C74 H52 Cl22 N4 Rh2' _chemical_formula_weight 1982.92 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2841(12) _cell_length_b 20.2395(13) _cell_length_c 21.0781(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.6660(10) _cell_angle_gamma 90.00 _cell_volume 7985.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6080 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.10 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6987 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details 'blessing Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33833 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7853 _reflns_number_gt 6103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+22.9653P] 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 7853 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Rh1 Rh 0.57268(2) 0.051403(18) 0.044642(19) 0.01744(11) Uani 1 1 d . . . Cl1 Cl 0.58695(7) 0.14541(6) 0.11187(6) 0.0256(3) Uani 1 1 d . . . Cl2 Cl 0.44811(6) 0.04664(6) 0.02214(6) 0.0221(3) Uani 1 1 d . . . N1 N 0.67403(19) 0.04543(19) 0.0609(2) 0.0176(8) Uani 1 1 d . . . C2 C 0.6969(2) 0.0792(2) 0.0176(2) 0.0189(10) Uani 1 1 d . . . C3 C 0.7693(3) 0.0745(2) 0.0275(2) 0.0186(10) Uani 1 1 d . . . C4 C 0.8130(3) 0.0301(2) 0.0769(2) 0.0203(10) Uani 1 1 d . . . C5 C 0.7850(3) -0.0089(2) 0.1162(2) 0.0204(10) Uani 1 1 d . . . C6 C 0.7153(3) 0.0031(2) 0.1101(2) 0.0211(11) Uani 1 1 d . . . C31 C 0.6383(3) 0.1156(2) -0.0366(2) 0.0194(10) Uani 1 1 d . . . C32 C 0.5704(3) 0.1090(2) -0.0335(2) 0.0187(10) Uani 1 1 d . . . C33 C 0.5129(3) 0.1420(2) -0.0807(3) 0.0245(11) Uani 1 1 d . . . H33A H 0.4672 0.1383 -0.0782 0.029 Uiso 1 1 calc R . . C34 C 0.5207(3) 0.1810(2) -0.1321(3) 0.0288(12) Uani 1 1 d . . . H34A H 0.4810 0.2044 -0.1636 0.035 Uiso 1 1 calc R . . C35 C 0.5866(3) 0.1852(3) -0.1367(3) 0.0269(12) Uani 1 1 d . . . H35A H 0.5916 0.2103 -0.1727 0.032 Uiso 1 1 calc R . . C36 C 0.6451(3) 0.1535(2) -0.0898(3) 0.0239(11) Uani 1 1 d . . . H36A H 0.6902 0.1571 -0.0933 0.029 Uiso 1 1 calc R . . C7 C 0.6790(3) -0.0243(2) 0.1544(3) 0.0225(11) Uani 1 1 d . . . N8 N 0.6093(2) -0.0073(2) 0.1355(2) 0.0223(9) Uani 1 1 d . . . C9 C 0.5726(3) -0.0242(3) 0.1738(3) 0.0271(12) Uani 1 1 d . . . H9A H 0.5242 -0.0106 0.1598 0.032 Uiso 1 1 calc R . . C10 C 0.6034(3) -0.0613(3) 0.2333(3) 0.0314(13) Uani 1 1 d . . . H10A H 0.5767 -0.0730 0.2601 0.038 Uiso 1 1 calc R . . C11 C 0.6734(3) -0.0805(3) 0.2526(3) 0.0377(14) Uani 1 1 d . . . H11A H 0.6953 -0.1069 0.2925 0.045 Uiso 1 1 calc R . . C12 C 0.7118(3) -0.0615(3) 0.2142(3) 0.0337(13) Uani 1 1 d . . . H12A H 0.7606 -0.0738 0.2283 0.040 Uiso 1 1 calc R . . C13 C 0.8290(3) -0.0635(2) 0.1599(3) 0.0217(11) Uani 1 1 d . . . C18 C 0.8872(3) -0.0519(3) 0.2212(3) 0.0257(11) Uani 1 1 d . . . H18A H 0.9019 -0.0080 0.2357 0.031 Uiso 1 1 calc R . . C17 C 0.9231(3) -0.1051(3) 0.2608(3) 0.0348(14) Uani 1 1 d . . . H17A H 0.9621 -0.0973 0.3031 0.042 Uiso 1 1 calc R . . C16 C 0.9037(3) -0.1688(3) 0.2400(3) 0.0374(15) Uani 1 1 d . . . H16A H 0.9291 -0.2047 0.2676 0.045 Uiso 1 1 calc R . . C15 C 0.8473(3) -0.1805(3) 0.1790(3) 0.0380(14) Uani 1 1 d . . . H15A H 0.8336 -0.2246 0.1644 0.046 Uiso 1 1 calc R . . C14 C 0.8103(3) -0.1280(3) 0.1386(3) 0.0329(13) Uani 1 1 d . . . H14A H 0.7718 -0.1364 0.0961 0.039 Uiso 1 1 calc R . . C19 C 0.8902(3) 0.0246(2) 0.0883(3) 0.0231(11) Uani 1 1 d . . . C24 C 0.9374(3) 0.0729(3) 0.1263(3) 0.0292(12) Uani 1 1 d . . . H24A H 0.9205 0.1082 0.1458 0.035 Uiso 1 1 calc R . . C23 C 1.0090(3) 0.0703(3) 0.1361(3) 0.0338(13) Uani 1 1 d . . . H23A H 1.0412 0.1034 0.1624 0.041 Uiso 1 1 calc R . . C22 C 1.0333(3) 0.0195(3) 0.1075(3) 0.0365(14) Uani 1 1 d . . . H22A H 1.0822 0.0178 0.1138 0.044 Uiso 1 1 calc R . . C21 C 0.9874(3) -0.0288(3) 0.0702(3) 0.0353(14) Uani 1 1 d . . . H21A H 1.0047 -0.0635 0.0505 0.042 Uiso 1 1 calc R . . C20 C 0.9157(3) -0.0273(3) 0.0608(3) 0.0291(12) Uani 1 1 d . . . H20A H 0.8843 -0.0615 0.0358 0.035 Uiso 1 1 calc R . . C25 C 0.8013(2) 0.1138(2) -0.0140(2) 0.0208(10) Uani 1 1 d . . . C26 C 0.8153(3) 0.0835(3) -0.0668(3) 0.0237(11) Uani 1 1 d . . . H26A H 0.8056 0.0378 -0.0760 0.028 Uiso 1 1 calc R . . C27 C 0.8436(3) 0.1201(3) -0.1062(3) 0.0287(12) Uani 1 1 d . . . H27A H 0.8529 0.0995 -0.1424 0.034 Uiso 1 1 calc R . . C28 C 0.8582(3) 0.1864(3) -0.0927(3) 0.0310(13) Uani 1 1 d . . . H28A H 0.8765 0.2117 -0.1202 0.037 Uiso 1 1 calc R . . C29 C 0.8462(3) 0.2158(3) -0.0390(3) 0.0307(13) Uani 1 1 d . . . H29A H 0.8579 0.2611 -0.0288 0.037 Uiso 1 1 calc R . . C30 C 0.8175(3) 0.1804(2) -0.0004(3) 0.0269(12) Uani 1 1 d . . . H30A H 0.8087 0.2014 0.0358 0.032 Uiso 1 1 calc R . . C50 C 0.3516(4) 0.1145(3) 0.1198(4) 0.0499(17) Uani 1 1 d . . . H50A H 0.3857 0.1252 0.0974 0.060 Uiso 1 1 calc R . . Cl51 Cl 0.33539(14) 0.02932(9) 0.11267(12) 0.0774(7) Uani 1 1 d . . . Cl52 Cl 0.39100(11) 0.13697(9) 0.20665(10) 0.0641(5) Uani 1 1 d . . . Cl53 Cl 0.27193(11) 0.15895(12) 0.07748(10) 0.0721(6) Uani 1 1 d . . . C54 C 0.7352(3) 0.3277(3) 0.7679(3) 0.0396(15) Uani 1 1 d . . . H54A H 0.7885 0.3266 0.7908 0.048 Uiso 1 1 calc R . . Cl55 Cl 0.70798(16) 0.25933(11) 0.71497(12) 0.0932(8) Uani 1 1 d . . . Cl56 Cl 0.70024(13) 0.32505(11) 0.83123(11) 0.0753(6) Uani 1 1 d . . . Cl57 Cl 0.71067(12) 0.40084(10) 0.72109(12) 0.0738(6) Uani 1 1 d . . . C59 C 0.0564(3) 0.2488(3) 0.9910(3) 0.0412(15) Uani 1 1 d . . . H59A H 0.0160 0.2808 0.9799 0.049 Uiso 1 1 calc R . . Cl60 Cl 0.04333(10) 0.18480(9) 1.04066(9) 0.0563(5) Uani 1 1 d . . . Cl61 Cl 0.13721(9) 0.29046(8) 1.03758(10) 0.0529(4) Uani 1 1 d . . . Cl62 Cl 0.05786(12) 0.21797(10) 0.91375(10) 0.0667(5) Uani 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 Rh1 0.01345(19) 0.02097(19) 0.0181(2) 0.00202(16) 0.00629(15) -0.00064(16) Cl1 0.0267(7) 0.0255(6) 0.0242(6) -0.0017(5) 0.0094(5) -0.0019(5) Cl2 0.0166(6) 0.0249(6) 0.0258(6) -0.0011(5) 0.0093(5) -0.0001(5) N1 0.0083(18) 0.026(2) 0.020(2) 0.0019(17) 0.0065(16) -0.0017(16) C2 0.019(3) 0.021(2) 0.015(2) -0.0043(19) 0.005(2) 0.001(2) C3 0.019(3) 0.022(2) 0.014(2) -0.0030(19) 0.006(2) -0.0048(19) C4 0.019(3) 0.023(2) 0.021(3) -0.006(2) 0.009(2) -0.0042(19) C5 0.020(3) 0.024(2) 0.020(3) -0.004(2) 0.009(2) -0.003(2) C6 0.019(3) 0.025(2) 0.017(3) -0.005(2) 0.005(2) -0.002(2) C31 0.021(3) 0.019(2) 0.018(2) -0.0036(19) 0.006(2) -0.0012(19) C32 0.020(3) 0.020(2) 0.016(2) 0.0018(19) 0.006(2) 0.000(2) C33 0.021(3) 0.025(2) 0.026(3) -0.001(2) 0.008(2) -0.003(2) C34 0.031(3) 0.028(3) 0.021(3) 0.006(2) 0.003(2) 0.005(2) C35 0.031(3) 0.030(3) 0.019(3) 0.004(2) 0.010(2) 0.002(2) C36 0.025(3) 0.026(3) 0.024(3) -0.002(2) 0.013(2) -0.002(2) C7 0.018(3) 0.026(2) 0.020(3) 0.003(2) 0.004(2) -0.003(2) N8 0.019(2) 0.026(2) 0.023(2) 0.0019(18) 0.0092(19) -0.0012(17) C9 0.019(3) 0.035(3) 0.028(3) 0.001(2) 0.010(2) -0.003(2) C10 0.029(3) 0.041(3) 0.031(3) 0.006(2) 0.019(3) -0.004(2) C11 0.030(3) 0.050(3) 0.034(3) 0.021(3) 0.013(3) 0.004(3) C12 0.026(3) 0.046(3) 0.029(3) 0.014(3) 0.011(3) 0.002(3) C13 0.019(3) 0.027(3) 0.022(3) 0.005(2) 0.011(2) 0.005(2) C18 0.019(3) 0.035(3) 0.025(3) 0.003(2) 0.011(2) 0.002(2) C17 0.024(3) 0.058(4) 0.023(3) 0.007(3) 0.010(2) 0.010(3) C16 0.036(4) 0.041(3) 0.042(4) 0.018(3) 0.023(3) 0.021(3) C15 0.047(4) 0.029(3) 0.044(4) 0.004(3) 0.023(3) 0.004(3) C14 0.033(3) 0.036(3) 0.027(3) 0.002(2) 0.009(3) -0.001(2) C19 0.017(3) 0.029(3) 0.024(3) 0.004(2) 0.008(2) 0.001(2) C24 0.027(3) 0.031(3) 0.032(3) -0.002(2) 0.013(3) 0.000(2) C23 0.019(3) 0.037(3) 0.041(3) 0.001(3) 0.006(3) -0.008(2) C22 0.019(3) 0.048(3) 0.043(4) 0.010(3) 0.013(3) 0.002(3) C21 0.028(3) 0.046(3) 0.036(3) 0.004(3) 0.016(3) 0.012(3) C20 0.026(3) 0.033(3) 0.029(3) 0.000(2) 0.011(2) 0.000(2) C25 0.012(2) 0.031(3) 0.018(3) 0.004(2) 0.003(2) 0.004(2) C26 0.020(3) 0.027(3) 0.026(3) -0.002(2) 0.010(2) 0.000(2) C27 0.027(3) 0.040(3) 0.024(3) 0.002(2) 0.014(2) 0.008(2) C28 0.027(3) 0.041(3) 0.032(3) 0.009(3) 0.018(3) -0.003(2) C29 0.032(3) 0.028(3) 0.034(3) 0.000(2) 0.014(3) -0.006(2) C30 0.028(3) 0.032(3) 0.024(3) -0.003(2) 0.014(2) -0.005(2) C50 0.064(5) 0.043(4) 0.054(4) -0.011(3) 0.037(4) -0.009(3) Cl51 0.127(2) 0.0482(10) 0.0906(15) -0.0294(10) 0.0792(15) -0.0393(11) Cl52 0.0657(12) 0.0546(10) 0.0548(11) -0.0143(9) 0.0043(9) 0.0093(9) Cl53 0.0605(13) 0.1044(16) 0.0463(11) -0.0033(11) 0.0150(10) 0.0042(11) C54 0.033(3) 0.051(4) 0.032(3) -0.010(3) 0.009(3) 0.001(3) Cl55 0.141(2) 0.0742(14) 0.0781(16) -0.0377(12) 0.0578(16) -0.0085(14) Cl56 0.0963(17) 0.0899(15) 0.0619(13) -0.0185(11) 0.0552(13) -0.0101(12) Cl57 0.0748(14) 0.0676(12) 0.0774(14) 0.0172(11) 0.0276(12) 0.0121(11) C59 0.039(4) 0.044(3) 0.043(4) -0.003(3) 0.018(3) 0.005(3) Cl60 0.0631(12) 0.0532(10) 0.0534(11) 0.0036(8) 0.0234(9) -0.0112(9) Cl61 0.0391(9) 0.0484(9) 0.0661(12) 0.0064(8) 0.0146(9) -0.0014(7) Cl62 0.0873(15) 0.0730(13) 0.0513(11) -0.0077(9) 0.0396(11) 0.0063(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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:11.1(3), B:C:71.4(2), D:80.2(2), E:74.8(2), 6.3(3) ; 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 Rh1 N1 1.953(4) . ? Rh1 C32 2.005(5) . ? Rh1 N8 2.130(4) . ? Rh1 Cl1 2.3230(13) . ? Rh1 Cl2 2.3747(12) 5_655 ? Rh1 Cl2 2.3866(12) . ? Cl2 Rh1 2.3747(12) 5_655 ? N1 C6 1.357(6) . ? N1 C2 1.358(6) . ? C2 C3 1.406(7) . ? C2 C31 1.487(6) . ? C3 C4 1.403(7) . ? C3 C25 1.501(7) . ? C4 C5 1.412(7) . ? C4 C19 1.495(7) . ? C5 C6 1.389(7) . ? C5 C13 1.495(7) . ? C6 C7 1.501(7) . ? C31 C36 1.407(7) . ? C31 C32 1.411(7) . ? C32 C33 1.379(7) . ? C33 C34 1.397(7) . ? C33 H33A 0.9500 . ? C34 C35 1.379(7) . ? C34 H34A 0.9500 . ? C35 C36 1.377(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C7 N8 1.357(6) . ? C7 C12 1.398(7) . ? N8 C9 1.335(6) . ? C9 C10 1.387(7) . ? C9 H9A 0.9500 . ? C10 C11 1.375(8) . ? C10 H10A 0.9500 . ? C11 C12 1.377(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.384(7) . ? C13 C18 1.394(7) . ? C18 C17 1.385(7) . ? C18 H18A 0.9500 . ? C17 C16 1.370(8) . ? C17 H17A 0.9500 . ? C16 C15 1.372(9) . ? C16 H16A 0.9500 . ? C15 C14 1.387(8) . ? C15 H15A 0.9500 . ? C14 H14A 0.9500 . ? C19 C24 1.387(7) . ? C19 C20 1.391(7) . ? C24 C23 1.388(7) . ? C24 H24A 0.9500 . ? C23 C22 1.374(8) . ? C23 H23A 0.9500 . ? C22 C21 1.370(8) . ? C22 H22A 0.9500 . ? C21 C20 1.391(7) . ? C21 H21A 0.9500 . ? C20 H20A 0.9500 . ? C25 C30 1.391(7) . ? C25 C26 1.393(7) . ? C26 C27 1.390(7) . ? C26 H26A 0.9500 . ? C27 C28 1.379(8) . ? C27 H27A 0.9500 . ? C28 C29 1.380(8) . ? C28 H28A 0.9500 . ? C29 C30 1.371(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C50 Cl51 1.750(6) . ? C50 Cl52 1.752(7) . ? C50 Cl53 1.762(7) . ? C50 H50A 1.0000 . ? C54 Cl55 1.729(6) . ? C54 Cl56 1.738(6) . ? C54 Cl57 1.741(7) . ? C54 H54A 1.0000 . ? C59 Cl60 1.749(6) . ? C59 Cl62 1.754(6) . ? C59 Cl61 1.767(6) . ? C59 H59A 1.0000 . ? 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 Rh1 C32 82.55(17) . . ? N1 Rh1 N8 80.14(15) . . ? C32 Rh1 N8 162.47(17) . . ? N1 Rh1 Cl1 93.91(12) . . ? C32 Rh1 Cl1 89.02(14) . . ? N8 Rh1 Cl1 89.41(11) . . ? N1 Rh1 Cl2 89.25(12) . 5_655 ? C32 Rh1 Cl2 93.23(13) . 5_655 ? N8 Rh1 Cl2 89.31(11) . 5_655 ? Cl1 Rh1 Cl2 176.34(5) . 5_655 ? N1 Rh1 Cl2 174.01(12) . . ? C32 Rh1 Cl2 99.93(14) . . ? N8 Rh1 Cl2 97.57(11) . . ? Cl1 Rh1 Cl2 91.60(4) . . ? Cl2 Rh1 Cl2 85.18(4) 5_655 . ? Rh1 Cl2 Rh1 94.83(4) 5_655 . ? C6 N1 C2 124.2(4) . . ? C6 N1 Rh1 118.1(3) . . ? C2 N1 Rh1 117.4(3) . . ? N1 C2 C3 118.3(4) . . ? N1 C2 C31 112.8(4) . . ? C3 C2 C31 128.8(4) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C25 118.8(4) . . ? C2 C3 C25 122.7(4) . . ? C3 C4 C5 120.8(4) . . ? C3 C4 C19 119.3(4) . . ? C5 C4 C19 119.9(4) . . ? C6 C5 C4 118.2(5) . . ? C6 C5 C13 122.1(4) . . ? C4 C5 C13 119.6(4) . . ? N1 C6 C5 119.2(4) . . ? N1 C6 C7 113.7(4) . . ? C5 C6 C7 127.1(4) . . ? C36 C31 C32 119.0(4) . . ? C36 C31 C2 126.0(4) . . ? C32 C31 C2 115.1(4) . . ? C33 C32 C31 119.4(4) . . ? C33 C32 Rh1 128.3(4) . . ? C31 C32 Rh1 112.2(3) . . ? C32 C33 C34 120.9(5) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 119.6(5) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C36 C35 C34 120.6(5) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C31 120.4(5) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? N8 C7 C12 118.8(5) . . ? N8 C7 C6 115.5(4) . . ? C12 C7 C6 125.6(5) . . ? C9 N8 C7 121.2(4) . . ? C9 N8 Rh1 127.2(3) . . ? C7 N8 Rh1 111.6(3) . . ? N8 C9 C10 121.6(5) . . ? N8 C9 H9A 119.2 . . ? C10 C9 H9A 119.2 . . ? C11 C10 C9 118.3(5) . . ? C11 C10 H10A 120.9 . . ? C9 C10 H10A 120.9 . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C7 120.0(5) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? C14 C13 C18 119.2(5) . . ? C14 C13 C5 118.3(5) . . ? C18 C13 C5 122.5(4) . . ? C17 C18 C13 119.2(5) . . ? C17 C18 H18A 120.4 . . ? C13 C18 H18A 120.4 . . ? C16 C17 C18 121.3(5) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C15 C14 120.1(5) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C13 C14 C15 120.5(5) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C24 C19 C20 119.3(5) . . ? C24 C19 C4 119.2(4) . . ? C20 C19 C4 121.6(5) . . ? C19 C24 C23 120.5(5) . . ? C19 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C21 C20 120.6(5) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C30 C25 C26 119.1(5) . . ? C30 C25 C3 120.9(4) . . ? C26 C25 C3 120.0(4) . . ? C27 C26 C25 120.0(5) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.0(5) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 119.8(5) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 120.6(5) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C25 120.3(5) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? Cl51 C50 Cl52 109.9(4) . . ? Cl51 C50 Cl53 110.8(4) . . ? Cl52 C50 Cl53 110.9(4) . . ? Cl51 C50 H50A 108.4 . . ? Cl52 C50 H50A 108.4 . . ? Cl53 C50 H50A 108.4 . . ? Cl55 C54 Cl56 110.3(4) . . ? Cl55 C54 Cl57 111.4(3) . . ? Cl56 C54 Cl57 110.4(3) . . ? Cl55 C54 H54A 108.2 . . ? Cl56 C54 H54A 108.2 . . ? Cl57 C54 H54A 108.2 . . ? Cl60 C59 Cl62 110.7(3) . . ? Cl60 C59 Cl61 110.0(3) . . ? Cl62 C59 Cl61 110.0(3) . . ? Cl60 C59 H59A 108.7 . . ? Cl62 C59 H59A 108.7 . . ? Cl61 C59 H59A 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Cl2 Rh1 -21.5(11) . . . 5_655 ? C32 Rh1 Cl2 Rh1 92.44(14) . . . 5_655 ? N8 Rh1 Cl2 Rh1 -88.67(12) . . . 5_655 ? Cl1 Rh1 Cl2 Rh1 -178.28(5) . . . 5_655 ? Cl2 Rh1 Cl2 Rh1 0.0 5_655 . . 5_655 ? C32 Rh1 N1 C6 -173.4(4) . . . . ? N8 Rh1 N1 C6 9.4(3) . . . . ? Cl1 Rh1 N1 C6 98.1(3) . . . . ? Cl2 Rh1 N1 C6 -80.1(3) 5_655 . . . ? Cl2 Rh1 N1 C6 -58.6(13) . . . . ? C32 Rh1 N1 C2 0.3(3) . . . . ? N8 Rh1 N1 C2 -176.9(4) . . . . ? Cl1 Rh1 N1 C2 -88.2(3) . . . . ? Cl2 Rh1 N1 C2 93.7(3) 5_655 . . . ? Cl2 Rh1 N1 C2 115.2(11) . . . . ? C6 N1 C2 C3 -5.3(7) . . . . ? Rh1 N1 C2 C3 -178.6(3) . . . . ? C6 N1 C2 C31 172.9(4) . . . . ? Rh1 N1 C2 C31 -0.4(5) . . . . ? N1 C2 C3 C4 6.3(6) . . . . ? C31 C2 C3 C4 -171.6(4) . . . . ? N1 C2 C3 C25 -175.3(4) . . . . ? C31 C2 C3 C25 6.9(7) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C25 C3 C4 C5 -178.8(4) . . . . ? C2 C3 C4 C19 -179.7(4) . . . . ? C25 C3 C4 C19 1.7(7) . . . . ? C3 C4 C5 C6 -7.0(7) . . . . ? C19 C4 C5 C6 172.5(4) . . . . ? C3 C4 C5 C13 169.8(4) . . . . ? C19 C4 C5 C13 -10.7(7) . . . . ? C2 N1 C6 C5 -2.1(7) . . . . ? Rh1 N1 C6 C5 171.2(3) . . . . ? C2 N1 C6 C7 175.9(4) . . . . ? Rh1 N1 C6 C7 -10.8(5) . . . . ? C4 C5 C6 N1 8.1(7) . . . . ? C13 C5 C6 N1 -168.6(4) . . . . ? C4 C5 C6 C7 -169.6(5) . . . . ? C13 C5 C6 C7 13.7(8) . . . . ? N1 C2 C31 C36 -178.2(4) . . . . ? C3 C2 C31 C36 -0.3(8) . . . . ? N1 C2 C31 C32 0.3(6) . . . . ? C3 C2 C31 C32 178.3(4) . . . . ? C36 C31 C32 C33 -2.8(7) . . . . ? C2 C31 C32 C33 178.6(4) . . . . ? C36 C31 C32 Rh1 178.6(3) . . . . ? C2 C31 C32 Rh1 0.0(5) . . . . ? N1 Rh1 C32 C33 -178.6(5) . . . . ? N8 Rh1 C32 C33 -169.5(5) . . . . ? Cl1 Rh1 C32 C33 -84.5(4) . . . . ? Cl2 Rh1 C32 C33 92.6(4) 5_655 . . . ? Cl2 Rh1 C32 C33 6.9(5) . . . . ? N1 Rh1 C32 C31 -0.2(3) . . . . ? N8 Rh1 C32 C31 9.0(8) . . . . ? Cl1 Rh1 C32 C31 93.9(3) . . . . ? Cl2 Rh1 C32 C31 -89.0(3) 5_655 . . . ? Cl2 Rh1 C32 C31 -174.6(3) . . . . ? C31 C32 C33 C34 1.0(7) . . . . ? Rh1 C32 C33 C34 179.4(4) . . . . ? C32 C33 C34 C35 1.6(8) . . . . ? C33 C34 C35 C36 -2.4(8) . . . . ? C34 C35 C36 C31 0.6(8) . . . . ? C32 C31 C36 C35 2.0(7) . . . . ? C2 C31 C36 C35 -179.5(4) . . . . ? N1 C6 C7 N8 5.1(6) . . . . ? C5 C6 C7 N8 -177.1(5) . . . . ? N1 C6 C7 C12 -170.8(5) . . . . ? C5 C6 C7 C12 7.0(8) . . . . ? C12 C7 N8 C9 1.4(7) . . . . ? C6 C7 N8 C9 -174.8(4) . . . . ? C12 C7 N8 Rh1 178.4(4) . . . . ? C6 C7 N8 Rh1 2.2(5) . . . . ? N1 Rh1 N8 C9 170.7(4) . . . . ? C32 Rh1 N8 C9 161.5(5) . . . . ? Cl1 Rh1 N8 C9 76.7(4) . . . . ? Cl2 Rh1 N8 C9 -99.9(4) 5_655 . . . ? Cl2 Rh1 N8 C9 -14.9(4) . . . . ? N1 Rh1 N8 C7 -6.0(3) . . . . ? C32 Rh1 N8 C7 -15.2(8) . . . . ? Cl1 Rh1 N8 C7 -100.1(3) . . . . ? Cl2 Rh1 N8 C7 83.4(3) 5_655 . . . ? Cl2 Rh1 N8 C7 168.4(3) . . . . ? C7 N8 C9 C10 -1.6(8) . . . . ? Rh1 N8 C9 C10 -178.0(4) . . . . ? N8 C9 C10 C11 -0.1(8) . . . . ? C9 C10 C11 C12 1.8(9) . . . . ? C10 C11 C12 C7 -1.9(9) . . . . ? N8 C7 C12 C11 0.3(8) . . . . ? C6 C7 C12 C11 176.1(5) . . . . ? C6 C5 C13 C14 69.6(7) . . . . ? C4 C5 C13 C14 -107.0(6) . . . . ? C6 C5 C13 C18 -109.5(6) . . . . ? C4 C5 C13 C18 73.9(6) . . . . ? C14 C13 C18 C17 -2.5(7) . . . . ? C5 C13 C18 C17 176.6(5) . . . . ? C13 C18 C17 C16 1.5(8) . . . . ? C18 C17 C16 C15 -0.3(9) . . . . ? C17 C16 C15 C14 0.0(9) . . . . ? C18 C13 C14 C15 2.3(8) . . . . ? C5 C13 C14 C15 -176.9(5) . . . . ? C16 C15 C14 C13 -1.0(9) . . . . ? C3 C4 C19 C24 77.6(6) . . . . ? C5 C4 C19 C24 -101.9(6) . . . . ? C3 C4 C19 C20 -101.5(6) . . . . ? C5 C4 C19 C20 79.1(6) . . . . ? C20 C19 C24 C23 0.9(8) . . . . ? C4 C19 C24 C23 -178.1(5) . . . . ? C19 C24 C23 C22 0.4(8) . . . . ? C24 C23 C22 C21 -0.7(9) . . . . ? C23 C22 C21 C20 -0.3(9) . . . . ? C22 C21 C20 C19 1.6(8) . . . . ? C24 C19 C20 C21 -1.8(8) . . . . ? C4 C19 C20 C21 177.2(5) . . . . ? C4 C3 C25 C30 -104.6(5) . . . . ? C2 C3 C25 C30 77.0(6) . . . . ? C4 C3 C25 C26 75.3(6) . . . . ? C2 C3 C25 C26 -103.2(6) . . . . ? C30 C25 C26 C27 -1.4(7) . . . . ? C3 C25 C26 C27 178.7(5) . . . . ? C25 C26 C27 C28 0.3(8) . . . . ? C26 C27 C28 C29 1.5(8) . . . . ? C27 C28 C29 C30 -2.2(8) . . . . ? C28 C29 C30 C25 1.2(8) . . . . ? C26 C25 C30 C29 0.7(8) . . . . ? C3 C25 C30 C29 -179.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.291 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.120 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 644548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H48 Cl2 N4 Rh, F6 P, C H2 Cl2' _chemical_formula_sum 'C69 H50 Cl4 F6 N4 P Rh' _chemical_formula_weight 1324.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.1740(12) _cell_length_b 16.0642(8) _cell_length_c 31.4753(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.9429(11) _cell_angle_gamma 90.00 _cell_volume 11809.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5392 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8325 _exptl_absorpt_correction_T_max 0.9354 _exptl_absorpt_process_details 'blessing Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50481 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11586 _reflns_number_gt 8309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+47.0434P] 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 11586 _refine_ls_number_parameters 767 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.030 _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 Rh1 Rh 1.0000 0.24833(3) 0.7500 0.01890(12) Uani 1 2 d S . . Rh2 Rh 1.0000 0.74493(3) 0.7500 0.02408(13) Uani 1 2 d S . . N1 N 0.96723(12) 0.33501(19) 0.70055(10) 0.0204(7) Uani 1 1 d . . . C2 C 0.99252(16) 0.3277(3) 0.66641(12) 0.0241(8) Uani 1 1 d . . . C3 C 0.96581(17) 0.3596(3) 0.62492(13) 0.0306(9) Uani 1 1 d . . . C4 C 0.91266(18) 0.4000(3) 0.61883(14) 0.0337(10) Uani 1 1 d . . . C5 C 0.88977(17) 0.4132(3) 0.65456(13) 0.0283(9) Uani 1 1 d . . . C6 C 0.91912(16) 0.3807(2) 0.69593(13) 0.0244(8) Uani 1 1 d . . . C7 C 1.04893(16) 0.2843(2) 0.67794(12) 0.0222(8) Uani 1 1 d . . . N8 N 1.06115(13) 0.24418(19) 0.71681(10) 0.0216(7) Uani 1 1 d . . . C9 C 1.10812(16) 0.1970(2) 0.72937(14) 0.0252(8) Uani 1 1 d . . . H37A H 1.1155 0.1691 0.7569 0.030 Uiso 1 1 calc R . . C10 C 1.14621(16) 0.1874(2) 0.70385(14) 0.0275(9) Uani 1 1 d . . . H13A H 1.1777 0.1502 0.7123 0.033 Uiso 1 1 calc R . . C11 C 1.13717(17) 0.2335(3) 0.66577(14) 0.0282(9) Uani 1 1 d . . . H65A H 1.1640 0.2314 0.6485 0.034 Uiso 1 1 calc R . . C12 C 1.08866(16) 0.2830(3) 0.65277(13) 0.0266(9) Uani 1 1 d . . . H25A H 1.0826 0.3158 0.6269 0.032 Uiso 1 1 calc R . . C13 C 0.99063(18) 0.3510(3) 0.58584(13) 0.0386(11) Uani 1 1 d . . . C14 C 0.9885(2) 0.2762(4) 0.56449(15) 0.0482(13) Uani 1 1 d . . . H70A H 0.9707 0.2295 0.5740 0.058 Uiso 1 1 calc R . . C15 C 1.0123(2) 0.2686(5) 0.52887(18) 0.068(2) Uani 1 1 d . . . H54A H 1.0106 0.2170 0.5138 0.081 Uiso 1 1 calc R . . C16 C 1.0388(3) 0.3373(6) 0.51542(18) 0.075(2) Uani 1 1 d . . . H62A H 1.0559 0.3321 0.4916 0.090 Uiso 1 1 calc R . . C17 C 1.0401(3) 0.4110(5) 0.5361(2) 0.0672(19) Uani 1 1 d . . . H53A H 1.0581 0.4575 0.5265 0.081 Uiso 1 1 calc R . . C18 C 1.0157(2) 0.4195(4) 0.57097(17) 0.0529(14) Uani 1 1 d . . . H60A H 1.0159 0.4721 0.5848 0.064 Uiso 1 1 calc R . . C19 C 0.8803(2) 0.4290(4) 0.57379(17) 0.0594(17) Uani 1 1 d . . . C20 C 0.8528(3) 0.3692(5) 0.54321(18) 0.076(2) Uani 1 1 d U . . H20A H 0.8588 0.3120 0.5508 0.091 Uiso 1 1 calc R . . C21 C 0.8169(3) 0.3893(7) 0.5022(2) 0.091(2) Uani 1 1 d U . . H21A H 0.7963 0.3488 0.4823 0.109 Uiso 1 1 calc R . . C22 C 0.8143(4) 0.4698(7) 0.4935(3) 0.096(3) Uani 1 1 d U . . H22B H 0.7915 0.4846 0.4652 0.115 Uiso 1 1 calc R . . C23 C 0.8394(3) 0.5347(6) 0.5191(3) 0.088(2) Uani 1 1 d U . . H23A H 0.8344 0.5908 0.5093 0.106 Uiso 1 1 calc R . . C24 C 0.8752(3) 0.5116(5) 0.5636(2) 0.083(2) Uani 1 1 d U . . H24A H 0.8937 0.5528 0.5840 0.099 Uiso 1 1 calc R . . C25 C 0.83307(17) 0.4557(3) 0.64832(13) 0.0266(9) Uani 1 1 d . . . C26 C 0.78404(18) 0.4156(3) 0.62455(13) 0.0288(9) Uani 1 1 d . . . H35A H 0.7868 0.3620 0.6125 0.035 Uiso 1 1 calc R . . C27 C 0.73105(18) 0.4534(3) 0.61832(14) 0.0327(10) Uani 1 1 d . . . H39A H 0.6976 0.4252 0.6023 0.039 Uiso 1 1 calc R . . C28 C 0.72654(18) 0.5315(3) 0.63518(15) 0.0370(10) Uani 1 1 d . . . H61A H 0.6902 0.5577 0.6305 0.044 Uiso 1 1 calc R . . C29 C 0.77509(19) 0.5709(3) 0.65871(17) 0.0406(11) Uani 1 1 d . . . H72A H 0.7722 0.6247 0.6705 0.049 Uiso 1 1 calc R . . C30 C 0.82847(18) 0.5336(3) 0.66565(15) 0.0344(10) Uani 1 1 d . . . H52A H 0.8617 0.5615 0.6822 0.041 Uiso 1 1 calc R . . C31 C 0.89675(16) 0.4019(2) 0.73478(12) 0.0224(8) Uani 1 1 d . . . C32 C 0.84337(17) 0.3746(2) 0.73778(13) 0.0264(9) Uani 1 1 d . . . H26A H 0.8224 0.3359 0.7169 0.032 Uiso 1 1 calc R . . C33 C 0.82063(18) 0.4038(3) 0.77116(14) 0.0311(10) Uani 1 1 d . . . H57A H 0.7840 0.3851 0.7730 0.037 Uiso 1 1 calc R . . C34 C 0.8507(2) 0.4595(3) 0.80154(14) 0.0349(10) Uani 1 1 d . . . H45A H 0.8348 0.4793 0.8243 0.042 Uiso 1 1 calc R . . C35 C 0.9041(2) 0.4870(2) 0.79915(14) 0.0320(10) Uani 1 1 d . . . H66A H 0.9251 0.5250 0.8204 0.038 Uiso 1 1 calc R . . C36 C 0.92663(17) 0.4587(2) 0.76560(13) 0.0257(8) Uani 1 1 d . . . H48A H 0.9629 0.4783 0.7636 0.031 Uiso 1 1 calc R . . N37 N 0.96690(13) 0.83163(19) 0.70100(10) 0.0219(7) Uani 1 1 d . . . C38 C 0.90850(16) 0.8231(2) 0.68506(13) 0.0256(8) Uani 1 1 d . . . C39 C 0.87968(17) 0.8553(3) 0.64417(13) 0.0277(9) Uani 1 1 d . . . C40 C 0.91051(17) 0.9030(3) 0.62053(13) 0.0299(9) Uani 1 1 d . . . C41 C 0.96958(17) 0.9148(3) 0.63817(13) 0.0271(9) Uani 1 1 d . . . C42 C 0.99631(17) 0.8794(3) 0.67919(13) 0.0262(9) Uani 1 1 d . . . C43 C 0.88050(16) 0.7793(2) 0.71572(13) 0.0249(8) Uani 1 1 d . . . N44 N 0.91649(13) 0.74056(19) 0.74971(12) 0.0257(7) Uani 1 1 d . . . C45 C 0.89645(18) 0.6961(3) 0.77847(15) 0.0323(10) Uani 1 1 d . . . H84A H 0.9228 0.6676 0.8015 0.039 Uiso 1 1 calc R . . C46 C 0.83861(18) 0.6904(3) 0.77572(16) 0.0340(10) Uani 1 1 d . . . H63A H 0.8250 0.6568 0.7957 0.041 Uiso 1 1 calc R . . C47 C 0.80158(18) 0.7346(3) 0.74335(15) 0.0313(10) Uani 1 1 d . . . H64A H 0.7618 0.7346 0.7418 0.038 Uiso 1 1 calc R . . C48 C 0.82193(17) 0.7794(3) 0.71287(14) 0.0300(9) Uani 1 1 d . . . H49A H 0.7962 0.8098 0.6903 0.036 Uiso 1 1 calc R . . C49 C 0.81801(17) 0.8366(3) 0.62288(14) 0.0316(9) Uani 1 1 d . . . C50 C 0.8038(2) 0.7580(3) 0.60607(17) 0.0471(12) Uani 1 1 d . . . H73A H 0.8323 0.7163 0.6089 0.057 Uiso 1 1 calc R . . C51 C 0.7466(3) 0.7406(4) 0.5848(2) 0.0663(18) Uani 1 1 d . . . H87A H 0.7367 0.6865 0.5731 0.080 Uiso 1 1 calc R . . C52 C 0.7052(2) 0.7992(5) 0.58046(19) 0.0669(19) Uani 1 1 d . . . H68A H 0.6667 0.7864 0.5657 0.080 Uiso 1 1 calc R . . C53 C 0.7194(2) 0.8771(4) 0.59752(18) 0.0548(15) Uani 1 1 d . . . H90A H 0.6903 0.9179 0.5950 0.066 Uiso 1 1 calc R . . C54 C 0.77600(18) 0.8971(3) 0.61856(15) 0.0384(11) Uani 1 1 d . . . H56A H 0.7856 0.9516 0.6298 0.046 Uiso 1 1 calc R . . C55 C 0.88067(18) 0.9473(4) 0.57888(14) 0.0400(12) Uani 1 1 d . . . C56 C 0.8550(2) 0.9053(4) 0.54055(17) 0.0596(16) Uani 1 1 d . . . H82A H 0.8561 0.8462 0.5396 0.072 Uiso 1 1 calc R . . C57 C 0.8270(2) 0.9515(5) 0.50252(17) 0.0624(18) Uani 1 1 d . . . H89A H 0.8088 0.9234 0.4761 0.075 Uiso 1 1 calc R . . C58 C 0.8262(3) 1.0370(5) 0.5042(2) 0.0731(19) Uani 1 1 d . . . H91A H 0.8078 1.0676 0.4787 0.088 Uiso 1 1 calc R . . C59 C 0.8512(2) 1.0780(4) 0.54155(19) 0.0615(16) Uani 1 1 d . . . H59A H 0.8501 1.1371 0.5423 0.074 Uiso 1 1 calc R . . C60 C 0.8787(2) 1.0338(4) 0.57892(17) 0.0466(12) Uani 1 1 d . . . H74A H 0.8965 1.0632 0.6051 0.056 Uiso 1 1 calc R . . C61 C 1.00368(16) 0.9589(3) 0.61167(13) 0.0274(9) Uani 1 1 d . . . C62 C 1.01214(18) 0.9201(3) 0.57451(14) 0.0350(10) Uani 1 1 d . . . H58A H 0.9968 0.8661 0.5668 0.042 Uiso 1 1 calc R . . C63 C 1.0427(2) 0.9593(3) 0.54847(15) 0.0426(12) Uani 1 1 d . . . H22A H 1.0482 0.9323 0.5230 0.051 Uiso 1 1 calc R . . C64 C 1.0650(2) 1.0375(3) 0.55981(16) 0.0425(11) Uani 1 1 d . . . H36A H 1.0861 1.0647 0.5422 0.051 Uiso 1 1 calc R . . C65 C 1.0566(2) 1.0759(3) 0.59645(16) 0.0421(11) Uani 1 1 d . . . H86A H 1.0718 1.1301 0.6040 0.051 Uiso 1 1 calc R . . C66 C 1.02649(18) 1.0374(3) 0.62274(14) 0.0350(10) Uani 1 1 d . . . H43A H 1.0215 1.0646 0.6483 0.042 Uiso 1 1 calc R . . C67 C 1.05763(16) 0.9005(2) 0.69894(13) 0.0253(8) Uani 1 1 d . . . C68 C 1.10059(18) 0.8743(3) 0.68035(15) 0.0325(10) Uani 1 1 d . . . H33A H 1.0920 0.8359 0.6566 0.039 Uiso 1 1 calc R . . C69 C 1.15633(19) 0.9035(3) 0.69615(17) 0.0405(12) Uani 1 1 d . . . H75A H 1.1857 0.8844 0.6835 0.049 Uiso 1 1 calc R . . C70 C 1.16879(18) 0.9601(3) 0.73017(17) 0.0421(12) Uani 1 1 d . . . H67A H 1.2067 0.9810 0.7404 0.050 Uiso 1 1 calc R . . C71 C 1.12709(19) 0.9867(3) 0.74947(16) 0.0366(11) Uani 1 1 d . . . H38A H 1.1362 1.0247 0.7734 0.044 Uiso 1 1 calc R . . C72 C 1.07105(17) 0.9575(3) 0.73363(14) 0.0289(9) Uani 1 1 d . . . H27A H 1.0419 0.9765 0.7465 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.95876(4) 0.14569(6) 0.69949(3) 0.0279(2) Uani 1 1 d . . . Cl2 Cl 1.02797(4) 0.64275(7) 0.80449(4) 0.0363(3) Uani 1 1 d . . . P1 P 0.76967(5) 0.15865(8) 0.64857(4) 0.0360(3) Uani 1 1 d . . . F1 F 0.82056(13) 0.2249(2) 0.65944(13) 0.0664(9) Uani 1 1 d . . . F2 F 0.76273(16) 0.1737(3) 0.59801(10) 0.0818(12) Uani 1 1 d . . . F3 F 0.72388(14) 0.2297(2) 0.64814(12) 0.0676(10) Uani 1 1 d . . . F4 F 0.71925(14) 0.0929(2) 0.63842(14) 0.0794(11) Uani 1 1 d . . . F5 F 0.77714(14) 0.1451(3) 0.69977(10) 0.0742(11) Uani 1 1 d . . . F6 F 0.81578(12) 0.08731(19) 0.64996(11) 0.0548(8) Uani 1 1 d . . . C80 C 0.6027(3) 0.1704(4) 0.5679(2) 0.0693(18) Uani 1 1 d . . . H55A H 0.6388 0.1438 0.5843 0.083 Uiso 1 1 calc R . . H55B H 0.5879 0.1388 0.5403 0.083 Uiso 1 1 calc R . . Cl81 Cl 0.61656(8) 0.27310(12) 0.55532(7) 0.0814(5) Uani 1 1 d . . . Cl82 Cl 0.55188(9) 0.16542(13) 0.59984(6) 0.0859(6) Uani 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 Rh1 0.0143(2) 0.0231(2) 0.0190(2) 0.000 0.00372(15) 0.000 Rh2 0.0153(2) 0.0225(2) 0.0345(3) 0.000 0.00673(18) 0.000 N1 0.0161(15) 0.0247(17) 0.0196(16) -0.0009(13) 0.0032(12) 0.0007(12) C2 0.0190(19) 0.032(2) 0.0210(19) 0.0003(16) 0.0052(15) -0.0014(16) C3 0.026(2) 0.039(2) 0.027(2) 0.0067(18) 0.0075(17) 0.0057(18) C4 0.028(2) 0.048(3) 0.025(2) 0.0103(19) 0.0074(18) 0.0087(19) C5 0.026(2) 0.032(2) 0.027(2) 0.0072(17) 0.0073(17) 0.0041(17) C6 0.0185(19) 0.028(2) 0.027(2) 0.0018(16) 0.0063(16) -0.0002(16) C7 0.0184(19) 0.026(2) 0.0204(19) -0.0027(15) 0.0020(15) -0.0023(15) N8 0.0172(15) 0.0224(16) 0.0254(17) -0.0031(13) 0.0060(13) -0.0012(13) C9 0.0193(19) 0.024(2) 0.032(2) -0.0012(16) 0.0056(16) -0.0021(15) C10 0.0184(19) 0.025(2) 0.039(2) -0.0032(18) 0.0082(17) 0.0003(16) C11 0.023(2) 0.035(2) 0.029(2) -0.0043(18) 0.0122(17) -0.0022(17) C12 0.022(2) 0.035(2) 0.024(2) 0.0002(17) 0.0076(16) -0.0032(17) C13 0.028(2) 0.067(3) 0.021(2) 0.011(2) 0.0061(17) 0.017(2) C14 0.030(2) 0.081(4) 0.030(2) -0.011(3) 0.000(2) 0.004(2) C15 0.038(3) 0.131(6) 0.031(3) -0.025(3) 0.003(2) 0.017(3) C16 0.045(3) 0.157(8) 0.027(3) 0.019(4) 0.017(2) 0.028(4) C17 0.057(4) 0.102(5) 0.052(4) 0.038(4) 0.032(3) 0.031(4) C18 0.050(3) 0.071(4) 0.044(3) 0.026(3) 0.024(3) 0.025(3) C19 0.039(3) 0.106(5) 0.039(3) 0.032(3) 0.021(2) 0.038(3) C20 0.053(3) 0.141(6) 0.029(3) -0.001(3) 0.001(2) 0.041(4) C21 0.072(4) 0.146(7) 0.054(4) 0.004(4) 0.015(3) 0.024(5) C22 0.082(5) 0.133(6) 0.090(5) 0.038(5) 0.054(4) 0.020(5) C23 0.059(4) 0.117(6) 0.100(5) 0.054(5) 0.043(4) 0.023(4) C24 0.057(4) 0.114(5) 0.088(4) 0.067(4) 0.039(3) 0.034(4) C25 0.024(2) 0.030(2) 0.028(2) 0.0072(17) 0.0094(17) 0.0039(17) C26 0.035(2) 0.028(2) 0.023(2) 0.0024(17) 0.0065(18) 0.0016(18) C27 0.024(2) 0.044(3) 0.029(2) 0.0047(19) 0.0043(17) -0.0021(19) C28 0.023(2) 0.043(3) 0.043(3) 0.005(2) 0.0059(19) 0.0075(19) C29 0.036(3) 0.027(2) 0.056(3) -0.001(2) 0.007(2) 0.0077(19) C30 0.024(2) 0.033(2) 0.042(3) 0.005(2) 0.0018(19) -0.0011(18) C31 0.0195(19) 0.0224(19) 0.024(2) 0.0040(15) 0.0034(15) 0.0067(15) C32 0.023(2) 0.023(2) 0.032(2) 0.0042(17) 0.0063(17) 0.0000(16) C33 0.026(2) 0.032(2) 0.039(2) 0.0088(19) 0.0146(19) 0.0082(17) C34 0.046(3) 0.030(2) 0.036(2) 0.0035(19) 0.022(2) 0.010(2) C35 0.043(3) 0.023(2) 0.031(2) 0.0005(17) 0.0107(19) 0.0007(18) C36 0.024(2) 0.025(2) 0.029(2) 0.0016(17) 0.0082(17) 0.0003(16) N37 0.0167(15) 0.0211(16) 0.0283(18) -0.0040(13) 0.0065(13) -0.0020(12) C38 0.0190(19) 0.025(2) 0.033(2) -0.0046(17) 0.0071(16) -0.0002(16) C39 0.023(2) 0.030(2) 0.031(2) -0.0041(18) 0.0068(17) -0.0024(17) C40 0.026(2) 0.040(2) 0.022(2) -0.0052(18) 0.0043(17) -0.0046(18) C41 0.025(2) 0.032(2) 0.024(2) -0.0052(17) 0.0059(17) -0.0021(17) C42 0.023(2) 0.029(2) 0.028(2) -0.0074(17) 0.0083(17) 0.0009(16) C43 0.0200(19) 0.0223(19) 0.033(2) -0.0038(17) 0.0078(17) -0.0027(16) N44 0.0173(16) 0.0223(17) 0.038(2) 0.0001(14) 0.0077(14) -0.0005(13) C45 0.023(2) 0.029(2) 0.046(3) 0.0071(19) 0.0104(19) -0.0018(17) C46 0.029(2) 0.028(2) 0.049(3) 0.003(2) 0.016(2) -0.0021(18) C47 0.020(2) 0.028(2) 0.047(3) -0.0014(19) 0.0111(19) -0.0023(17) C48 0.020(2) 0.032(2) 0.038(2) -0.0006(19) 0.0059(18) -0.0003(17) C49 0.022(2) 0.042(3) 0.029(2) 0.0021(19) 0.0029(17) -0.0067(18) C50 0.042(3) 0.048(3) 0.046(3) -0.001(2) 0.001(2) -0.011(2) C51 0.059(4) 0.070(4) 0.058(4) 0.000(3) -0.007(3) -0.040(3) C52 0.029(3) 0.100(5) 0.059(4) 0.036(4) -0.011(3) -0.025(3) C53 0.023(2) 0.081(4) 0.057(3) 0.035(3) 0.004(2) -0.001(3) C54 0.026(2) 0.047(3) 0.043(3) 0.016(2) 0.012(2) -0.001(2) C55 0.024(2) 0.077(4) 0.021(2) 0.001(2) 0.0087(17) -0.008(2) C56 0.045(3) 0.098(5) 0.038(3) -0.009(3) 0.014(2) -0.020(3) C57 0.043(3) 0.116(6) 0.026(3) -0.003(3) 0.004(2) -0.021(3) C58 0.050(4) 0.114(6) 0.055(4) 0.023(4) 0.013(3) 0.007(4) C59 0.054(3) 0.079(4) 0.053(4) 0.019(3) 0.015(3) 0.013(3) C60 0.036(3) 0.061(3) 0.044(3) 0.016(3) 0.012(2) 0.008(2) C61 0.021(2) 0.037(2) 0.025(2) 0.0007(18) 0.0065(16) 0.0013(17) C62 0.033(2) 0.038(2) 0.035(2) -0.003(2) 0.0118(19) -0.0085(19) C63 0.047(3) 0.057(3) 0.029(2) 0.001(2) 0.019(2) 0.000(2) C64 0.040(3) 0.052(3) 0.039(3) 0.007(2) 0.017(2) -0.010(2) C65 0.047(3) 0.037(3) 0.045(3) 0.000(2) 0.015(2) -0.012(2) C66 0.035(2) 0.041(3) 0.031(2) -0.004(2) 0.0115(19) -0.003(2) C67 0.020(2) 0.029(2) 0.026(2) 0.0026(16) 0.0058(16) -0.0041(16) C68 0.028(2) 0.035(2) 0.037(2) 0.0060(19) 0.0122(19) 0.0021(18) C69 0.025(2) 0.043(3) 0.059(3) 0.019(2) 0.022(2) 0.006(2) C70 0.020(2) 0.033(2) 0.067(3) 0.014(2) -0.002(2) -0.0034(18) C71 0.030(2) 0.023(2) 0.047(3) 0.0055(19) -0.006(2) -0.0024(18) C72 0.022(2) 0.029(2) 0.035(2) 0.0024(18) 0.0046(17) 0.0009(17) Cl1 0.0232(5) 0.0311(5) 0.0300(5) -0.0072(4) 0.0080(4) -0.0061(4) Cl2 0.0234(5) 0.0304(6) 0.0546(7) 0.0120(5) 0.0091(5) 0.0038(4) P1 0.0305(6) 0.0430(7) 0.0330(6) -0.0008(5) 0.0054(5) 0.0013(5) F1 0.0453(18) 0.0487(18) 0.101(3) -0.0043(18) 0.0119(18) -0.0032(15) F2 0.073(2) 0.135(4) 0.0348(18) 0.006(2) 0.0105(16) 0.011(2) F3 0.0517(19) 0.070(2) 0.084(2) 0.0152(19) 0.0228(18) 0.0269(17) F4 0.0435(19) 0.070(2) 0.116(3) 0.009(2) 0.0035(19) -0.0182(17) F5 0.0527(19) 0.132(3) 0.0396(17) 0.0091(19) 0.0143(15) 0.031(2) F6 0.0465(17) 0.0493(18) 0.072(2) -0.0033(15) 0.0221(16) 0.0064(14) C80 0.066(4) 0.077(5) 0.056(4) -0.005(3) 0.001(3) 0.012(3) Cl81 0.0696(11) 0.0709(11) 0.0915(13) 0.0054(9) -0.0015(9) 0.0015(9) Cl82 0.1047(14) 0.0933(13) 0.0514(9) -0.0029(9) 0.0050(9) -0.0058(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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:15.7(2), B:74.3(2), C:73.6(2), D:71.4(2), E:67.8(2) A:15.6(2), B:73.0(2), C:66.4(2), D:72.0(2), E:70.5(2) ; 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 Rh1 N8 2.019(3) . ? Rh1 N8 2.019(3) 2_756 ? Rh1 N1 2.086(3) 2_756 ? Rh1 N1 2.086(3) . ? Rh1 Cl1 2.3287(10) . ? Rh1 Cl1 2.3287(10) 2_756 ? Rh2 N44 2.018(3) . ? Rh2 N44 2.018(3) 2_756 ? Rh2 N37 2.079(3) 2_756 ? Rh2 N37 2.079(3) . ? Rh2 Cl2 2.3441(11) 2_756 ? Rh2 Cl2 2.3442(11) . ? N1 C6 1.351(5) . ? N1 C2 1.372(5) . ? C2 C3 1.396(5) . ? C2 C7 1.491(5) . ? C3 C4 1.407(6) . ? C3 C13 1.507(6) . ? C4 C5 1.392(6) . ? C4 C19 1.506(6) . ? C5 C6 1.413(5) . ? C5 C25 1.498(5) . ? C6 C31 1.498(5) . ? C7 N8 1.347(5) . ? C7 C12 1.394(5) . ? N8 C9 1.337(5) . ? C9 C10 1.378(6) . ? C9 H37A 0.9500 . ? C10 C11 1.377(6) . ? C10 H13A 0.9500 . ? C11 C12 1.388(6) . ? C11 H65A 0.9500 . ? C12 H25A 0.9500 . ? C13 C14 1.372(7) . ? C13 C18 1.393(7) . ? C14 C15 1.392(7) . ? C14 H70A 0.9500 . ? C15 C16 1.396(10) . ? C15 H54A 0.9500 . ? C16 C17 1.346(10) . ? C16 H62A 0.9500 . ? C17 C18 1.383(7) . ? C17 H53A 0.9500 . ? C18 H60A 0.9500 . ? C19 C24 1.363(9) . ? C19 C20 1.402(10) . ? C20 C21 1.396(8) . ? C20 H20A 0.9500 . ? C21 C22 1.319(12) . ? C21 H21A 0.9500 . ? C22 C23 1.361(12) . ? C22 H22B 0.9500 . ? C23 C24 1.491(10) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.381(6) . ? C25 C26 1.387(6) . ? C26 C27 1.385(6) . ? C26 H35A 0.9500 . ? C27 C28 1.378(7) . ? C27 H39A 0.9500 . ? C28 C29 1.371(6) . ? C28 H61A 0.9500 . ? C29 C30 1.388(6) . ? C29 H72A 0.9500 . ? C30 H52A 0.9500 . ? C31 C32 1.389(5) . ? C31 C36 1.391(5) . ? C32 C33 1.387(6) . ? C32 H26A 0.9500 . ? C33 C34 1.373(6) . ? C33 H57A 0.9500 . ? C34 C35 1.385(6) . ? C34 H45A 0.9500 . ? C35 C36 1.384(6) . ? C35 H66A 0.9500 . ? C36 H48A 0.9500 . ? N37 C42 1.348(5) . ? N37 C38 1.378(5) . ? C38 C39 1.395(6) . ? C38 C43 1.490(5) . ? C39 C40 1.408(6) . ? C39 C49 1.499(5) . ? C40 C41 1.405(6) . ? C40 C55 1.503(6) . ? C41 C42 1.407(6) . ? C41 C61 1.494(6) . ? C42 C67 1.491(5) . ? C43 N44 1.345(5) . ? C43 C48 1.395(5) . ? N44 C45 1.338(5) . ? C45 C46 1.382(6) . ? C45 H84A 0.9500 . ? C46 C47 1.368(6) . ? C46 H63A 0.9500 . ? C47 C48 1.387(6) . ? C47 H64A 0.9500 . ? C48 H49A 0.9500 . ? C49 C50 1.378(7) . ? C49 C54 1.386(6) . ? C50 C51 1.399(7) . ? C50 H73A 0.9500 . ? C51 C52 1.356(9) . ? C51 H87A 0.9500 . ? C52 C53 1.369(9) . ? C52 H68A 0.9500 . ? C53 C54 1.396(7) . ? C53 H90A 0.9500 . ? C54 H56A 0.9500 . ? C55 C56 1.382(7) . ? C55 C60 1.390(8) . ? C56 C57 1.423(8) . ? C56 H82A 0.9500 . ? C57 C58 1.375(10) . ? C57 H89A 0.9500 . ? C58 C59 1.347(9) . ? C58 H91A 0.9500 . ? C59 C60 1.389(7) . ? C59 H59A 0.9500 . ? C60 H74A 0.9500 . ? C61 C66 1.384(6) . ? C61 C62 1.386(6) . ? C62 C63 1.388(6) . ? C62 H58A 0.9500 . ? C63 C64 1.377(7) . ? C63 H22A 0.9500 . ? C64 C65 1.369(7) . ? C64 H36A 0.9500 . ? C65 C66 1.382(6) . ? C65 H86A 0.9500 . ? C66 H43A 0.9500 . ? C67 C68 1.383(6) . ? C67 C72 1.397(6) . ? C68 C69 1.392(6) . ? C68 H33A 0.9500 . ? C69 C70 1.378(7) . ? C69 H75A 0.9500 . ? C70 C71 1.372(7) . ? C70 H67A 0.9500 . ? C71 C72 1.398(6) . ? C71 H38A 0.9500 . ? C72 H27A 0.9500 . ? P1 F2 1.575(3) . ? P1 F4 1.582(3) . ? P1 F3 1.587(3) . ? P1 F5 1.590(3) . ? P1 F6 1.591(3) . ? P1 F1 1.595(3) . ? C80 Cl81 1.750(7) . ? C80 Cl82 1.778(7) . ? C80 H55A 0.9900 . ? C80 H55B 0.9900 . ? 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 N8 Rh1 N8 176.21(17) . 2_756 ? N8 Rh1 N1 102.72(12) . 2_756 ? N8 Rh1 N1 79.86(12) 2_756 2_756 ? N8 Rh1 N1 79.86(12) . . ? N8 Rh1 N1 102.72(12) 2_756 . ? N1 Rh1 N1 96.27(17) 2_756 . ? N8 Rh1 Cl1 82.24(9) . . ? N8 Rh1 Cl1 95.06(9) 2_756 . ? N1 Rh1 Cl1 174.39(9) 2_756 . ? N1 Rh1 Cl1 87.13(9) . . ? N8 Rh1 Cl1 95.06(9) . 2_756 ? N8 Rh1 Cl1 82.24(9) 2_756 2_756 ? N1 Rh1 Cl1 87.13(9) 2_756 2_756 ? N1 Rh1 Cl1 174.39(9) . 2_756 ? Cl1 Rh1 Cl1 89.85(5) . 2_756 ? N44 Rh2 N44 176.01(18) . 2_756 ? N44 Rh2 N37 102.70(12) . 2_756 ? N44 Rh2 N37 80.02(13) 2_756 2_756 ? N44 Rh2 N37 80.02(13) . . ? N44 Rh2 N37 102.70(12) 2_756 . ? N37 Rh2 N37 95.88(17) 2_756 . ? N44 Rh2 Cl2 82.70(10) . 2_756 ? N44 Rh2 Cl2 94.50(10) 2_756 2_756 ? N37 Rh2 Cl2 174.32(9) 2_756 2_756 ? N37 Rh2 Cl2 86.74(9) . 2_756 ? N44 Rh2 Cl2 94.50(10) . . ? N44 Rh2 Cl2 82.69(10) 2_756 . ? N37 Rh2 Cl2 86.74(9) 2_756 . ? N37 Rh2 Cl2 174.32(9) . . ? Cl2 Rh2 Cl2 91.11(6) 2_756 . ? C6 N1 C2 120.5(3) . . ? C6 N1 Rh1 126.4(3) . . ? C2 N1 Rh1 111.6(2) . . ? N1 C2 C3 120.6(3) . . ? N1 C2 C7 114.4(3) . . ? C3 C2 C7 124.9(3) . . ? C2 C3 C4 118.8(4) . . ? C2 C3 C13 123.0(4) . . ? C4 C3 C13 118.2(4) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 C19 119.7(4) . . ? C3 C4 C19 120.3(4) . . ? C4 C5 C6 118.6(4) . . ? C4 C5 C25 120.3(4) . . ? C6 C5 C25 121.0(4) . . ? N1 C6 C5 120.9(4) . . ? N1 C6 C31 121.2(3) . . ? C5 C6 C31 117.9(3) . . ? N8 C7 C12 119.1(3) . . ? N8 C7 C2 114.7(3) . . ? C12 C7 C2 126.1(4) . . ? C9 N8 C7 120.7(3) . . ? C9 N8 Rh1 123.0(3) . . ? C7 N8 Rh1 115.8(2) . . ? N8 C9 C10 122.3(4) . . ? N8 C9 H37A 118.8 . . ? C10 C9 H37A 118.8 . . ? C11 C10 C9 117.9(4) . . ? C11 C10 H13A 121.1 . . ? C9 C10 H13A 121.1 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H65A 120.1 . . ? C12 C11 H65A 120.1 . . ? C11 C12 C7 119.6(4) . . ? C11 C12 H25A 120.2 . . ? C7 C12 H25A 120.2 . . ? C14 C13 C18 119.5(5) . . ? C14 C13 C3 120.5(5) . . ? C18 C13 C3 120.1(5) . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H70A 120.0 . . ? C15 C14 H70A 120.0 . . ? C14 C15 C16 119.5(6) . . ? C14 C15 H54A 120.2 . . ? C16 C15 H54A 120.3 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H62A 119.8 . . ? C15 C16 H62A 119.8 . . ? C16 C17 C18 120.5(6) . . ? C16 C17 H53A 119.7 . . ? C18 C17 H53A 119.7 . . ? C17 C18 C13 120.1(6) . . ? C17 C18 H60A 120.0 . . ? C13 C18 H60A 120.0 . . ? C24 C19 C20 120.5(6) . . ? C24 C19 C4 121.2(6) . . ? C20 C19 C4 118.2(6) . . ? C21 C20 C19 123.2(8) . . ? C21 C20 H20A 118.4 . . ? C19 C20 H20A 118.4 . . ? C22 C21 C20 113.8(9) . . ? C22 C21 H21A 123.1 . . ? C20 C21 H21A 123.1 . . ? C21 C22 C23 129.8(9) . . ? C21 C22 H22B 115.1 . . ? C23 C22 H22B 115.1 . . ? C22 C23 C24 115.2(8) . . ? C22 C23 H23A 122.4 . . ? C24 C23 H23A 122.4 . . ? C19 C24 C23 117.3(8) . . ? C19 C24 H24A 121.3 . . ? C23 C24 H24A 121.3 . . ? C30 C25 C26 119.3(4) . . ? C30 C25 C5 121.7(4) . . ? C26 C25 C5 119.0(4) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H35A 119.9 . . ? C25 C26 H35A 119.9 . . ? C28 C27 C26 120.5(4) . . ? C28 C27 H39A 119.8 . . ? C26 C27 H39A 119.8 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 H61A 120.4 . . ? C27 C28 H61A 120.4 . . ? C28 C29 C30 121.2(4) . . ? C28 C29 H72A 119.4 . . ? C30 C29 H72A 119.4 . . ? C25 C30 C29 119.7(4) . . ? C25 C30 H52A 120.2 . . ? C29 C30 H52A 120.2 . . ? C32 C31 C36 119.0(4) . . ? C32 C31 C6 121.4(3) . . ? C36 C31 C6 119.1(3) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H26A 119.9 . . ? C31 C32 H26A 119.9 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H57A 119.8 . . ? C32 C33 H57A 119.8 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H45A 119.9 . . ? C35 C34 H45A 119.9 . . ? C36 C35 C34 119.5(4) . . ? C36 C35 H66A 120.2 . . ? C34 C35 H66A 120.2 . . ? C35 C36 C31 120.8(4) . . ? C35 C36 H48A 119.6 . . ? C31 C36 H48A 119.6 . . ? C42 N37 C38 119.8(3) . . ? C42 N37 Rh2 127.3(3) . . ? C38 N37 Rh2 111.4(3) . . ? N37 C38 C39 121.3(4) . . ? N37 C38 C43 113.9(3) . . ? C39 C38 C43 124.8(3) . . ? C38 C39 C40 118.9(4) . . ? C38 C39 C49 122.8(4) . . ? C40 C39 C49 118.3(4) . . ? C41 C40 C39 119.2(4) . . ? C41 C40 C55 119.4(4) . . ? C39 C40 C55 121.2(4) . . ? C40 C41 C42 119.2(4) . . ? C40 C41 C61 119.6(4) . . ? C42 C41 C61 121.0(4) . . ? N37 C42 C41 121.3(4) . . ? N37 C42 C67 121.0(4) . . ? C41 C42 C67 117.6(4) . . ? N44 C43 C48 119.3(4) . . ? N44 C43 C38 115.1(3) . . ? C48 C43 C38 125.5(4) . . ? C45 N44 C43 120.8(3) . . ? C45 N44 Rh2 123.5(3) . . ? C43 N44 Rh2 115.4(3) . . ? N44 C45 C46 122.0(4) . . ? N44 C45 H84A 119.0 . . ? C46 C45 H84A 119.0 . . ? C47 C46 C45 118.0(4) . . ? C47 C46 H63A 121.0 . . ? C45 C46 H63A 121.0 . . ? C46 C47 C48 120.2(4) . . ? C46 C47 H64A 119.9 . . ? C48 C47 H64A 119.9 . . ? C47 C48 C43 119.3(4) . . ? C47 C48 H49A 120.3 . . ? C43 C48 H49A 120.3 . . ? C50 C49 C54 120.0(4) . . ? C50 C49 C39 118.4(4) . . ? C54 C49 C39 121.5(4) . . ? C49 C50 C51 119.0(5) . . ? C49 C50 H73A 120.5 . . ? C51 C50 H73A 120.5 . . ? C52 C51 C50 121.5(6) . . ? C52 C51 H87A 119.3 . . ? C50 C51 H87A 119.3 . . ? C51 C52 C53 119.4(5) . . ? C51 C52 H68A 120.3 . . ? C53 C52 H68A 120.3 . . ? C52 C53 C54 120.8(5) . . ? C52 C53 H90A 119.6 . . ? C54 C53 H90A 119.6 . . ? C49 C54 C53 119.2(5) . . ? C49 C54 H56A 120.4 . . ? C53 C54 H56A 120.4 . . ? C56 C55 C60 118.8(5) . . ? C56 C55 C40 122.5(5) . . ? C60 C55 C40 118.8(4) . . ? C55 C56 C57 119.2(6) . . ? C55 C56 H82A 120.4 . . ? C57 C56 H82A 120.4 . . ? C58 C57 C56 119.8(6) . . ? C58 C57 H89A 120.1 . . ? C56 C57 H89A 120.1 . . ? C59 C58 C57 121.0(6) . . ? C59 C58 H91A 119.5 . . ? C57 C58 H91A 119.5 . . ? C58 C59 C60 119.8(7) . . ? C58 C59 H59A 120.1 . . ? C60 C59 H59A 120.1 . . ? C59 C60 C55 121.3(6) . . ? C59 C60 H74A 119.3 . . ? C55 C60 H74A 119.3 . . ? C66 C61 C62 119.1(4) . . ? C66 C61 C41 122.2(4) . . ? C62 C61 C41 118.7(4) . . ? C61 C62 C63 120.8(4) . . ? C61 C62 H58A 119.6 . . ? C63 C62 H58A 119.6 . . ? C64 C63 C62 119.5(4) . . ? C64 C63 H22A 120.2 . . ? C62 C63 H22A 120.2 . . ? C65 C64 C63 119.8(4) . . ? C65 C64 H36A 120.1 . . ? C63 C64 H36A 120.1 . . ? C64 C65 C66 121.2(5) . . ? C64 C65 H86A 119.4 . . ? C66 C65 H86A 119.4 . . ? C65 C66 C61 119.7(4) . . ? C65 C66 H43A 120.2 . . ? C61 C66 H43A 120.2 . . ? C68 C67 C72 118.8(4) . . ? C68 C67 C42 121.9(4) . . ? C72 C67 C42 118.7(4) . . ? C67 C68 C69 120.6(4) . . ? C67 C68 H33A 119.7 . . ? C69 C68 H33A 119.7 . . ? C70 C69 C68 119.9(4) . . ? C70 C69 H75A 120.1 . . ? C68 C69 H75A 120.1 . . ? C71 C70 C69 120.7(4) . . ? C71 C70 H67A 119.6 . . ? C69 C70 H67A 119.6 . . ? C70 C71 C72 119.5(4) . . ? C70 C71 H38A 120.3 . . ? C72 C71 H38A 120.3 . . ? C67 C72 C71 120.5(4) . . ? C67 C72 H27A 119.8 . . ? C71 C72 H27A 119.8 . . ? F2 P1 F4 91.3(2) . . ? F2 P1 F3 89.4(2) . . ? F4 P1 F3 88.8(2) . . ? F2 P1 F5 179.0(3) . . ? F4 P1 F5 89.6(2) . . ? F3 P1 F5 90.22(19) . . ? F2 P1 F6 91.7(2) . . ? F4 P1 F6 91.29(19) . . ? F3 P1 F6 178.94(19) . . ? F5 P1 F6 88.73(18) . . ? F2 P1 F1 89.4(2) . . ? F4 P1 F1 179.3(2) . . ? F3 P1 F1 91.14(19) . . ? F5 P1 F1 89.7(2) . . ? F6 P1 F1 88.76(17) . . ? Cl81 C80 Cl82 111.8(4) . . ? Cl81 C80 H55A 109.3 . . ? Cl82 C80 H55A 109.3 . . ? Cl81 C80 H55B 109.3 . . ? Cl82 C80 H55B 109.3 . . ? H55A C80 H55B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Rh1 N1 C6 -177.6(3) . . . . ? N8 Rh1 N1 C6 5.2(3) 2_756 . . . ? N1 Rh1 N1 C6 -75.8(3) 2_756 . . . ? Cl1 Rh1 N1 C6 99.7(3) . . . . ? Cl1 Rh1 N1 C6 157.1(7) 2_756 . . . ? N8 Rh1 N1 C2 16.6(2) . . . . ? N8 Rh1 N1 C2 -160.5(2) 2_756 . . . ? N1 Rh1 N1 C2 118.5(3) 2_756 . . . ? Cl1 Rh1 N1 C2 -66.0(2) . . . . ? Cl1 Rh1 N1 C2 -8.6(11) 2_756 . . . ? C6 N1 C2 C3 -7.1(6) . . . . ? Rh1 N1 C2 C3 159.6(3) . . . . ? C6 N1 C2 C7 172.9(3) . . . . ? Rh1 N1 C2 C7 -20.4(4) . . . . ? N1 C2 C3 C4 0.5(6) . . . . ? C7 C2 C3 C4 -179.4(4) . . . . ? N1 C2 C3 C13 -178.0(4) . . . . ? C7 C2 C3 C13 2.1(7) . . . . ? C2 C3 C4 C5 5.0(7) . . . . ? C13 C3 C4 C5 -176.5(4) . . . . ? C2 C3 C4 C19 -175.1(5) . . . . ? C13 C3 C4 C19 3.5(7) . . . . ? C3 C4 C5 C6 -4.0(7) . . . . ? C19 C4 C5 C6 176.0(5) . . . . ? C3 C4 C5 C25 -179.7(4) . . . . ? C19 C4 C5 C25 0.4(7) . . . . ? C2 N1 C6 C5 8.1(6) . . . . ? Rh1 N1 C6 C5 -156.5(3) . . . . ? C2 N1 C6 C31 -169.0(3) . . . . ? Rh1 N1 C6 C31 26.4(5) . . . . ? C4 C5 C6 N1 -2.5(6) . . . . ? C25 C5 C6 N1 173.2(4) . . . . ? C4 C5 C6 C31 174.7(4) . . . . ? C25 C5 C6 C31 -9.7(6) . . . . ? N1 C2 C7 N8 12.9(5) . . . . ? C3 C2 C7 N8 -167.2(4) . . . . ? N1 C2 C7 C12 -166.3(4) . . . . ? C3 C2 C7 C12 13.6(7) . . . . ? C12 C7 N8 C9 -6.3(5) . . . . ? C2 C7 N8 C9 174.3(3) . . . . ? C12 C7 N8 Rh1 -178.9(3) . . . . ? C2 C7 N8 Rh1 1.8(4) . . . . ? N8 Rh1 N8 C9 -49.1(3) 2_756 . . . ? N1 Rh1 N8 C9 83.5(3) 2_756 . . . ? N1 Rh1 N8 C9 177.7(3) . . . . ? Cl1 Rh1 N8 C9 -93.8(3) . . . . ? Cl1 Rh1 N8 C9 -4.7(3) 2_756 . . . ? N8 Rh1 N8 C7 123.3(3) 2_756 . . . ? N1 Rh1 N8 C7 -104.1(3) 2_756 . . . ? N1 Rh1 N8 C7 -9.9(3) . . . . ? Cl1 Rh1 N8 C7 78.5(3) . . . . ? Cl1 Rh1 N8 C7 167.7(3) 2_756 . . . ? C7 N8 C9 C10 0.5(6) . . . . ? Rh1 N8 C9 C10 172.5(3) . . . . ? N8 C9 C10 C11 5.0(6) . . . . ? C9 C10 C11 C12 -4.4(6) . . . . ? C10 C11 C12 C7 -1.3(6) . . . . ? N8 C7 C12 C11 6.7(6) . . . . ? C2 C7 C12 C11 -174.0(4) . . . . ? C2 C3 C13 C14 74.8(6) . . . . ? C4 C3 C13 C14 -103.7(5) . . . . ? C2 C3 C13 C18 -105.6(5) . . . . ? C4 C3 C13 C18 75.9(6) . . . . ? C18 C13 C14 C15 1.4(7) . . . . ? C3 C13 C14 C15 -179.0(4) . . . . ? C13 C14 C15 C16 0.6(8) . . . . ? C14 C15 C16 C17 -1.5(9) . . . . ? C15 C16 C17 C18 0.4(9) . . . . ? C16 C17 C18 C13 1.7(8) . . . . ? C14 C13 C18 C17 -2.5(7) . . . . ? C3 C13 C18 C17 177.8(4) . . . . ? C5 C4 C19 C24 70.7(7) . . . . ? C3 C4 C19 C24 -109.3(6) . . . . ? C5 C4 C19 C20 -105.8(6) . . . . ? C3 C4 C19 C20 74.3(6) . . . . ? C24 C19 C20 C21 -3.1(9) . . . . ? C4 C19 C20 C21 173.3(5) . . . . ? C19 C20 C21 C22 4.3(10) . . . . ? C20 C21 C22 C23 -2.7(12) . . . . ? C21 C22 C23 C24 0.0(12) . . . . ? C20 C19 C24 C23 0.1(8) . . . . ? C4 C19 C24 C23 -176.3(5) . . . . ? C22 C23 C24 C19 1.4(9) . . . . ? C4 C5 C25 C30 -112.6(5) . . . . ? C6 C5 C25 C30 71.9(5) . . . . ? C4 C5 C25 C26 67.5(5) . . . . ? C6 C5 C25 C26 -108.0(5) . . . . ? C30 C25 C26 C27 0.0(6) . . . . ? C5 C25 C26 C27 179.9(4) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C26 C27 C28 C29 -0.9(7) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? C26 C25 C30 C29 -0.6(6) . . . . ? C5 C25 C30 C29 179.5(4) . . . . ? C28 C29 C30 C25 0.5(7) . . . . ? N1 C6 C31 C32 -117.8(4) . . . . ? C5 C6 C31 C32 65.0(5) . . . . ? N1 C6 C31 C36 70.6(5) . . . . ? C5 C6 C31 C36 -106.6(4) . . . . ? C36 C31 C32 C33 -0.1(6) . . . . ? C6 C31 C32 C33 -171.7(4) . . . . ? C31 C32 C33 C34 -0.2(6) . . . . ? C32 C33 C34 C35 -0.1(6) . . . . ? C33 C34 C35 C36 0.8(6) . . . . ? C34 C35 C36 C31 -1.2(6) . . . . ? C32 C31 C36 C35 0.9(6) . . . . ? C6 C31 C36 C35 172.6(4) . . . . ? N44 Rh2 N37 C42 175.9(3) . . . . ? N44 Rh2 N37 C42 -7.1(3) 2_756 . . . ? N37 Rh2 N37 C42 74.0(3) 2_756 . . . ? Cl2 Rh2 N37 C42 -101.0(3) 2_756 . . . ? Cl2 Rh2 N37 C42 -168.8(7) . . . . ? N44 Rh2 N37 C38 -18.0(3) . . . . ? N44 Rh2 N37 C38 159.0(3) 2_756 . . . ? N37 Rh2 N37 C38 -119.9(3) 2_756 . . . ? Cl2 Rh2 N37 C38 65.1(2) 2_756 . . . ? Cl2 Rh2 N37 C38 -2.7(11) . . . . ? C42 N37 C38 C39 7.2(6) . . . . ? Rh2 N37 C38 C39 -160.1(3) . . . . ? C42 N37 C38 C43 -171.3(3) . . . . ? Rh2 N37 C38 C43 21.4(4) . . . . ? N37 C38 C39 C40 -5.1(6) . . . . ? C43 C38 C39 C40 173.3(4) . . . . ? N37 C38 C39 C49 170.8(4) . . . . ? C43 C38 C39 C49 -10.9(6) . . . . ? C38 C39 C40 C41 1.8(6) . . . . ? C49 C39 C40 C41 -174.3(4) . . . . ? C38 C39 C40 C55 -173.0(4) . . . . ? C49 C39 C40 C55 11.0(6) . . . . ? C39 C40 C41 C42 -0.7(6) . . . . ? C55 C40 C41 C42 174.2(4) . . . . ? C39 C40 C41 C61 174.7(4) . . . . ? C55 C40 C41 C61 -10.5(6) . . . . ? C38 N37 C42 C41 -6.0(6) . . . . ? Rh2 N37 C42 C41 159.1(3) . . . . ? C38 N37 C42 C67 170.5(3) . . . . ? Rh2 N37 C42 C67 -24.4(5) . . . . ? C40 C41 C42 N37 2.8(6) . . . . ? C61 C41 C42 N37 -172.5(4) . . . . ? C40 C41 C42 C67 -173.8(4) . . . . ? C61 C41 C42 C67 10.9(6) . . . . ? N37 C38 C43 N44 -12.7(5) . . . . ? C39 C38 C43 N44 168.9(4) . . . . ? N37 C38 C43 C48 164.0(4) . . . . ? C39 C38 C43 C48 -14.5(6) . . . . ? C48 C43 N44 C45 6.0(6) . . . . ? C38 C43 N44 C45 -177.1(4) . . . . ? C48 C43 N44 Rh2 180.0(3) . . . . ? C38 C43 N44 Rh2 -3.2(4) . . . . ? N44 Rh2 N44 C45 51.9(3) 2_756 . . . ? N37 Rh2 N44 C45 -80.9(3) 2_756 . . . ? N37 Rh2 N44 C45 -174.8(4) . . . . ? Cl2 Rh2 N44 C45 97.3(3) 2_756 . . . ? Cl2 Rh2 N44 C45 6.7(3) . . . . ? N44 Rh2 N44 C43 -121.9(3) 2_756 . . . ? N37 Rh2 N44 C43 105.3(3) 2_756 . . . ? N37 Rh2 N44 C43 11.4(3) . . . . ? Cl2 Rh2 N44 C43 -76.5(3) 2_756 . . . ? Cl2 Rh2 N44 C43 -167.1(3) . . . . ? C43 N44 C45 C46 -2.5(6) . . . . ? Rh2 N44 C45 C46 -176.0(3) . . . . ? N44 C45 C46 C47 -2.5(7) . . . . ? C45 C46 C47 C48 3.8(7) . . . . ? C46 C47 C48 C43 -0.4(6) . . . . ? N44 C43 C48 C47 -4.6(6) . . . . ? C38 C43 C48 C47 178.9(4) . . . . ? C38 C39 C49 C50 -72.1(6) . . . . ? C40 C39 C49 C50 103.8(5) . . . . ? C38 C39 C49 C54 110.1(5) . . . . ? C40 C39 C49 C54 -74.0(6) . . . . ? C54 C49 C50 C51 -0.1(7) . . . . ? C39 C49 C50 C51 -177.9(5) . . . . ? C49 C50 C51 C52 -0.1(9) . . . . ? C50 C51 C52 C53 -0.5(9) . . . . ? C51 C52 C53 C54 1.2(9) . . . . ? C50 C49 C54 C53 0.7(7) . . . . ? C39 C49 C54 C53 178.5(4) . . . . ? C52 C53 C54 C49 -1.3(7) . . . . ? C41 C40 C55 C56 116.6(5) . . . . ? C39 C40 C55 C56 -68.7(6) . . . . ? C41 C40 C55 C60 -63.6(6) . . . . ? C39 C40 C55 C60 111.2(5) . . . . ? C60 C55 C56 C57 -0.6(7) . . . . ? C40 C55 C56 C57 179.3(4) . . . . ? C55 C56 C57 C58 0.7(8) . . . . ? C56 C57 C58 C59 -0.7(9) . . . . ? C57 C58 C59 C60 0.6(9) . . . . ? C58 C59 C60 C55 -0.5(8) . . . . ? C56 C55 C60 C59 0.6(7) . . . . ? C40 C55 C60 C59 -179.3(4) . . . . ? C40 C41 C61 C66 110.5(5) . . . . ? C42 C41 C61 C66 -74.3(5) . . . . ? C40 C41 C61 C62 -68.8(5) . . . . ? C42 C41 C61 C62 106.4(5) . . . . ? C66 C61 C62 C63 -0.4(7) . . . . ? C41 C61 C62 C63 178.9(4) . . . . ? C61 C62 C63 C64 0.2(7) . . . . ? C62 C63 C64 C65 -0.3(8) . . . . ? C63 C64 C65 C66 0.6(8) . . . . ? C64 C65 C66 C61 -0.8(7) . . . . ? C62 C61 C66 C65 0.7(7) . . . . ? C41 C61 C66 C65 -178.6(4) . . . . ? N37 C42 C67 C68 116.2(4) . . . . ? C41 C42 C67 C68 -67.2(5) . . . . ? N37 C42 C67 C72 -72.5(5) . . . . ? C41 C42 C67 C72 104.1(4) . . . . ? C72 C67 C68 C69 0.6(6) . . . . ? C42 C67 C68 C69 171.8(4) . . . . ? C67 C68 C69 C70 -1.0(7) . . . . ? C68 C69 C70 C71 1.6(7) . . . . ? C69 C70 C71 C72 -1.6(7) . . . . ? C68 C67 C72 C71 -0.6(6) . . . . ? C42 C67 C72 C71 -172.1(4) . . . . ? C70 C71 C72 C67 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.566 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.101 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 644549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H46 N4 Rh, F6 P, 3(C H Cl3), O' _chemical_formula_sum 'C71 H49 Cl9 F6 N4 O P Rh' _chemical_formula_weight 1541.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall -P2ybc 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 24.611(8) _cell_length_b 13.238(4) _cell_length_c 21.081(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.501(7) _cell_angle_gamma 90.00 _cell_volume 6866(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8694 _exptl_absorpt_correction_T_max 0.9797 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35046 _diffrn_reflns_av_R_equivalents 0.2245 _diffrn_reflns_av_sigmaI/netI 0.2771 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12083 _reflns_number_gt 4974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12083 _refine_ls_number_parameters 839 _refine_ls_number_restraints 1164 _refine_ls_R_factor_all 0.2754 _refine_ls_R_factor_gt 0.1414 _refine_ls_wR_factor_ref 0.3471 _refine_ls_wR_factor_gt 0.3003 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.300 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.72585(5) 0.13148(9) 0.87966(6) 0.0222(3) Uani 1 1 d U . . N1 N 0.6977(4) 0.0279(8) 0.8194(5) 0.019(3) Uani 1 1 d U A . C2 C 0.6423(6) 0.0150(10) 0.8148(7) 0.023(3) Uani 1 1 d U . . C3 C 0.6230(6) -0.0727(10) 0.7819(7) 0.026(4) Uani 1 1 d U A . C4 C 0.6587(5) -0.1345(11) 0.7509(7) 0.025(3) Uani 1 1 d U . . C5 C 0.7157(6) -0.1153(10) 0.7544(7) 0.022(3) Uani 1 1 d U A . C6 C 0.7335(5) -0.0331(10) 0.7912(7) 0.021(3) Uani 1 1 d U . . C7 C 0.6108(5) 0.0949(10) 0.8470(7) 0.020(3) Uani 1 1 d U A . N8 N 0.6405(5) 0.1539(8) 0.8872(6) 0.024(3) Uani 1 1 d U A . C9 C 0.6168(6) 0.2223(11) 0.9224(8) 0.039(4) Uani 1 1 d U . . H9A H 0.6377 0.2570 0.9540 0.046 Uiso 1 1 calc R A . C10 C 0.5626(7) 0.2445(12) 0.9145(8) 0.041(4) Uani 1 1 d U A . H10A H 0.5463 0.2961 0.9389 0.050 Uiso 1 1 calc R . . C11 C 0.5317(7) 0.1892(12) 0.8696(8) 0.047(5) Uani 1 1 d U . . H11A H 0.4946 0.2054 0.8614 0.057 Uiso 1 1 calc R A . C12 C 0.5556(6) 0.1119(10) 0.8377(7) 0.029(4) Uani 1 1 d U A . H12A H 0.5347 0.0704 0.8095 0.035 Uiso 1 1 calc R . . C13 C 0.5621(6) -0.0970(10) 0.7780(7) 0.025(3) Uani 1 1 d U . . C14 C 0.5395(6) -0.1497(11) 0.8253(8) 0.039(4) Uani 1 1 d U A . H14A H 0.5606 -0.1672 0.8621 0.047 Uiso 1 1 calc R . . C15 C 0.4850(7) -0.1785(13) 0.8201(10) 0.054(5) Uani 1 1 d U . . H15A H 0.4685 -0.2136 0.8539 0.065 Uiso 1 1 calc R A . C16 C 0.4554(7) -0.1557(12) 0.7655(9) 0.050(5) Uani 1 1 d U A . H16A H 0.4191 -0.1794 0.7605 0.060 Uiso 1 1 calc R . . C17 C 0.4771(7) -0.1012(13) 0.7202(9) 0.055(5) Uani 1 1 d U . . H17A H 0.4547 -0.0812 0.6850 0.066 Uiso 1 1 calc R A . C18 C 0.5330(6) -0.0708(12) 0.7217(8) 0.041(4) Uani 1 1 d U A . H18A H 0.5492 -0.0360 0.6876 0.049 Uiso 1 1 calc R . . C19 C 0.6388(5) -0.2301(10) 0.7227(7) 0.022(3) Uani 1 1 d U A . C20 C 0.6272(6) -0.3136(11) 0.7586(8) 0.035(4) Uani 1 1 d U . . H20A H 0.6324 -0.3081 0.8033 0.042 Uiso 1 1 calc R A . C21 C 0.6089(6) -0.4042(12) 0.7351(8) 0.041(4) Uani 1 1 d U A . H21A H 0.6003 -0.4594 0.7618 0.049 Uiso 1 1 calc R . . C22 C 0.6037(6) -0.4099(12) 0.6691(8) 0.036(4) Uani 1 1 d U . . H22A H 0.5926 -0.4724 0.6509 0.044 Uiso 1 1 calc R A . C23 C 0.6136(6) -0.3313(12) 0.6291(8) 0.040(4) Uani 1 1 d U A . H23A H 0.6081 -0.3381 0.5845 0.048 Uiso 1 1 calc R . . C24 C 0.6324(6) -0.2388(12) 0.6564(7) 0.032(4) Uani 1 1 d U . . H24A H 0.6405 -0.1830 0.6299 0.038 Uiso 1 1 calc R A . C25 C 0.7523(5) -0.1831(10) 0.7219(7) 0.024(3) Uani 1 1 d U . . C26 C 0.7663(6) -0.1643(11) 0.6595(8) 0.033(4) Uani 1 1 d U A . H26A H 0.7512 -0.1078 0.6376 0.039 Uiso 1 1 calc R . . C27 C 0.8015(7) -0.2265(13) 0.6297(9) 0.046(5) Uani 1 1 d U . . H27A H 0.8097 -0.2141 0.5867 0.056 Uiso 1 1 calc R A . C28 C 0.8257(7) -0.3081(13) 0.6612(8) 0.044(4) Uani 1 1 d U A . H28A H 0.8523 -0.3484 0.6414 0.053 Uiso 1 1 calc R . . C29 C 0.8098(7) -0.3285(13) 0.7219(9) 0.047(5) Uani 1 1 d U . . H29A H 0.8241 -0.3856 0.7439 0.056 Uiso 1 1 calc R A . C30 C 0.7746(6) -0.2682(11) 0.7494(8) 0.033(4) Uani 1 1 d U A . H30A H 0.7640 -0.2849 0.7911 0.040 Uiso 1 1 calc R . . C31 C 0.7911(6) -0.0018(11) 0.8075(7) 0.026(4) Uani 1 1 d U A . C32 C 0.7968(6) 0.0784(11) 0.8498(7) 0.029(4) Uani 1 1 d U A . C33 C 0.8499(6) 0.1081(11) 0.8697(7) 0.031(4) Uani 1 1 d U . . H33A H 0.8542 0.1606 0.9002 0.037 Uiso 1 1 calc R A . C34 C 0.8953(7) 0.0625(13) 0.8459(8) 0.044(4) Uani 1 1 d U A . H34A H 0.9305 0.0840 0.8596 0.053 Uiso 1 1 calc R . . C35 C 0.8898(8) -0.0139(15) 0.8024(10) 0.065(5) Uani 1 1 d U . . H35A H 0.9210 -0.0461 0.7861 0.078 Uiso 1 1 calc R A . C36 C 0.8372(7) -0.0443(13) 0.7818(8) 0.048(5) Uani 1 1 d U A . H36A H 0.8332 -0.0947 0.7500 0.057 Uiso 1 1 calc R . . N37 N 0.7597(4) 0.2325(8) 0.9400(5) 0.022(3) Uani 1 1 d U A . C38 C 0.7742(6) 0.1968(11) 0.9981(7) 0.026(4) Uani 1 1 d U . . C39 C 0.8116(5) 0.2533(9) 1.0346(6) 0.013(3) Uani 1 1 d U A . C40 C 0.8265(5) 0.3457(9) 1.0121(6) 0.016(3) Uani 1 1 d U . . C41 C 0.8060(5) 0.3887(10) 0.9550(7) 0.023(3) Uani 1 1 d U A . C42 C 0.7727(5) 0.3235(10) 0.9174(7) 0.020(3) Uani 1 1 d U . . C43 C 0.7543(6) 0.0946(10) 1.0101(7) 0.023(3) Uani 1 1 d U A . N44 N 0.7307(6) 0.0404(10) 0.9574(7) 0.028(4) Uani 0.19(10) 1 d PU A 1 C44 C 0.7307(6) 0.0404(10) 0.9574(7) 0.028(4) Uani 0.81(10) 1 d PU A 2 C45 C 0.7141(6) -0.0567(11) 0.9663(8) 0.030(4) Uani 1 1 d U . . H45A H 0.7017 -0.0938 0.9301 0.036 Uiso 1 1 calc R A 1 C46 C 0.7140(6) -0.1037(12) 1.0231(8) 0.039(4) Uani 1 1 d U A . H46A H 0.7025 -0.1718 1.0271 0.046 Uiso 1 1 calc R . . C47 C 0.7314(6) -0.0480(12) 1.0750(8) 0.040(4) Uani 1 1 d U . . H47A H 0.7295 -0.0771 1.1161 0.048 Uiso 1 1 calc R A . C48 C 0.7515(6) 0.0483(11) 1.0692(8) 0.031(4) Uani 1 1 d U A . H48A H 0.7637 0.0838 1.1061 0.038 Uiso 1 1 calc R . . C49 C 0.8356(6) 0.2115(11) 1.0959(7) 0.028(4) Uani 1 1 d U . . C50 C 0.8212(6) 0.2515(12) 1.1550(7) 0.035(4) Uani 1 1 d U A . H50A H 0.7970 0.3072 1.1568 0.041 Uiso 1 1 calc R . . C51 C 0.8423(7) 0.2096(13) 1.2100(8) 0.044(4) Uani 1 1 d U . . H51A H 0.8329 0.2364 1.2500 0.053 Uiso 1 1 calc R A . C52 C 0.8772(7) 0.1285(15) 1.2066(9) 0.055(5) Uani 1 1 d U A . H52A H 0.8909 0.0989 1.2448 0.066 Uiso 1 1 calc R . . C53 C 0.8930(7) 0.0882(13) 1.1478(9) 0.053(5) Uani 1 1 d U . . H53A H 0.9175 0.0329 1.1463 0.064 Uiso 1 1 calc R A . C54 C 0.8717(6) 0.1312(12) 1.0920(8) 0.039(4) Uani 1 1 d U A . H54A H 0.8819 0.1059 1.0518 0.047 Uiso 1 1 calc R . . C55 C 0.8725(6) 0.4043(10) 1.0467(7) 0.025(3) Uani 1 1 d U A . C56 C 0.8624(7) 0.4753(12) 1.0905(8) 0.042(4) Uani 1 1 d U . . H56A H 0.8261 0.4910 1.1012 0.050 Uiso 1 1 calc R A . C57 C 0.9077(8) 0.5276(14) 1.1209(9) 0.061(5) Uani 1 1 d U A . H57A H 0.9012 0.5798 1.1507 0.073 Uiso 1 1 calc R . . C58 C 0.9595(8) 0.5020(14) 1.1069(9) 0.060(5) Uani 1 1 d U . . H58A H 0.9894 0.5336 1.1283 0.072 Uiso 1 1 calc R A . C59 C 0.9679(8) 0.4328(14) 1.0632(9) 0.058(5) Uani 1 1 d U A . H59A H 1.0042 0.4179 1.0522 0.069 Uiso 1 1 calc R . . C60 C 0.9257(6) 0.3809(12) 1.0325(8) 0.043(4) Uani 1 1 d U . . H60A H 0.9332 0.3300 1.0022 0.052 Uiso 1 1 calc R A . C61 C 0.8222(6) 0.4916(11) 0.9352(7) 0.030(4) Uani 1 1 d U . . C62 C 0.8636(6) 0.5115(11) 0.8985(7) 0.029(4) Uani 1 1 d U A . H62A H 0.8862 0.4572 0.8860 0.035 Uiso 1 1 calc R . . C63 C 0.8753(7) 0.6044(13) 0.8783(8) 0.049(5) Uani 1 1 d U . . H63A H 0.9054 0.6148 0.8518 0.059 Uiso 1 1 calc R A . C64 C 0.8444(8) 0.6834(14) 0.8954(8) 0.051(5) Uani 1 1 d U A . H64A H 0.8530 0.7489 0.8802 0.061 Uiso 1 1 calc R . . C65 C 0.8008(8) 0.6717(14) 0.9344(9) 0.056(5) Uani 1 1 d U . . H65A H 0.7798 0.7283 0.9464 0.067 Uiso 1 1 calc R A . C66 C 0.7878(7) 0.5725(12) 0.9564(8) 0.040(4) Uani 1 1 d U A . H66A H 0.7583 0.5606 0.9835 0.047 Uiso 1 1 calc R . . C67 C 0.7493(5) 0.3465(11) 0.8529(7) 0.025(3) Uani 1 1 d U A . C68 C 0.7286(5) 0.2613(9) 0.8234(6) 0.027(4) Uani 0.19(10) 1 d PU A 1 N68 N 0.7286(5) 0.2613(9) 0.8234(6) 0.027(4) Uani 0.81(10) 1 d PU A 2 C69 C 0.7050(6) 0.2727(12) 0.7622(7) 0.031(4) Uani 1 1 d U . . H69A H 0.6893 0.2152 0.7421 0.037 Uiso 1 1 calc R A 1 C70 C 0.7037(6) 0.3615(12) 0.7310(7) 0.030(4) Uani 1 1 d U A . H70A H 0.6895 0.3657 0.6887 0.037 Uiso 1 1 calc R . . C71 C 0.7240(6) 0.4473(12) 0.7623(8) 0.038(4) Uani 1 1 d U . . H71A H 0.7214 0.5115 0.7423 0.045 Uiso 1 1 calc R A . C72 C 0.7479(6) 0.4390(11) 0.8231(7) 0.027(4) Uani 1 1 d U A . H72A H 0.7631 0.4967 0.8436 0.032 Uiso 1 1 calc R . . P1 P 0.65719(19) 0.1094(3) 0.6000(2) 0.0413(12) Uani 1 1 d U . . F1 F 0.7080(5) 0.0853(9) 0.6420(6) 0.089(4) Uani 1 1 d U . . F2 F 0.6885(6) 0.0984(11) 0.5378(7) 0.119(5) Uani 1 1 d U . . F3 F 0.6409(6) -0.0038(9) 0.5982(7) 0.110(5) Uani 1 1 d U . . F4 F 0.6732(5) 0.2228(9) 0.6021(6) 0.095(4) Uani 1 1 d U . . F5 F 0.6242(6) 0.1293(11) 0.6606(6) 0.115(5) Uani 1 1 d U . . F6 F 0.6060(4) 0.1336(9) 0.5541(5) 0.083(4) Uani 1 1 d U . . C80 C 0.9866(9) 0.1982(15) 0.7481(10) 0.074(6) Uani 1 1 d U . . H80A H 0.9484 0.1775 0.7369 0.089 Uiso 1 1 calc R . . Cl81 Cl 0.9839(4) 0.2781(6) 0.8134(4) 0.146(3) Uani 1 1 d U . . Cl82 Cl 1.0114(3) 0.2661(6) 0.6824(5) 0.150(3) Uani 1 1 d U . . Cl83 Cl 1.0228(2) 0.0910(4) 0.7620(3) 0.0788(18) Uani 1 1 d U . . C84 C 0.5979(8) 0.9255(14) 0.4599(9) 0.066(6) Uani 1 1 d DU . . H84A H 0.5999 0.9620 0.5014 0.079 Uiso 1 1 calc R . . Cl85 Cl 0.6241(3) 0.8094(4) 0.4687(3) 0.104(2) Uani 1 1 d DU . . Cl86 Cl 0.5289(2) 0.9186(5) 0.4320(3) 0.090(2) Uani 1 1 d DU . . Cl87 Cl 0.6343(2) 0.9951(4) 0.4015(2) 0.0609(14) Uani 1 1 d DU . . C88 C 0.0639(9) 0.3542(17) 0.4778(12) 0.28(2) Uani 1 1 d DU . . H88A H 0.0511 0.3911 0.4388 0.340 Uiso 1 1 calc R . . Cl89 Cl 0.0669(4) 0.2309(7) 0.4631(5) 0.190(4) Uani 1 1 d DU . . Cl90 Cl 0.0177(5) 0.3747(10) 0.5405(7) 0.274(7) Uani 1 1 d DU . . Cl91 Cl 0.1289(2) 0.4037(4) 0.5049(3) 0.0830(18) Uani 1 1 d DU . . O100 O 0.5307(5) -0.0855(11) 0.9868(5) 0.076(4) Uani 1 1 d U . . 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 Rh1 0.0139(5) 0.0277(6) 0.0242(7) -0.0035(7) -0.0118(5) -0.0026(6) N1 0.020(3) 0.020(3) 0.019(3) -0.001(2) -0.002(2) -0.002(2) C2 0.020(6) 0.023(6) 0.024(7) -0.003(6) -0.012(6) -0.005(5) C3 0.025(6) 0.026(6) 0.028(7) 0.003(6) -0.011(6) -0.003(5) C4 0.024(6) 0.027(6) 0.022(6) -0.002(6) -0.006(5) -0.001(6) C5 0.023(6) 0.024(6) 0.019(6) -0.004(6) -0.004(5) -0.010(5) C6 0.018(6) 0.029(6) 0.017(7) 0.005(6) 0.006(6) 0.007(5) C7 0.015(6) 0.020(6) 0.026(7) 0.000(5) 0.001(6) -0.006(5) N8 0.023(6) 0.021(6) 0.028(6) -0.008(5) -0.009(5) -0.005(5) C9 0.038(7) 0.036(7) 0.041(8) -0.013(6) -0.016(7) -0.007(6) C10 0.039(7) 0.037(7) 0.048(8) -0.013(7) -0.008(7) 0.010(6) C11 0.033(7) 0.051(8) 0.057(8) -0.007(7) -0.010(7) 0.002(6) C12 0.022(6) 0.031(7) 0.034(7) -0.008(6) -0.005(6) -0.003(5) C13 0.020(6) 0.026(6) 0.029(7) -0.004(6) -0.011(6) -0.006(5) C14 0.023(7) 0.042(7) 0.051(8) 0.002(7) -0.005(6) 0.000(6) C15 0.044(8) 0.050(8) 0.069(9) 0.001(7) 0.014(7) -0.004(7) C16 0.036(8) 0.051(8) 0.063(9) -0.006(7) -0.008(7) -0.008(7) C17 0.045(8) 0.061(8) 0.058(9) -0.017(7) -0.018(7) 0.007(7) C18 0.033(7) 0.050(7) 0.040(8) -0.010(7) -0.010(7) 0.007(6) C19 0.018(6) 0.027(6) 0.022(7) -0.009(6) 0.002(6) 0.000(5) C20 0.031(7) 0.038(7) 0.034(7) 0.004(6) -0.012(6) 0.000(6) C21 0.039(7) 0.037(7) 0.047(8) 0.005(7) -0.005(7) -0.007(6) C22 0.033(7) 0.030(7) 0.046(8) -0.013(6) -0.003(7) -0.002(6) C23 0.036(7) 0.047(7) 0.037(8) -0.010(7) -0.001(6) -0.007(6) C24 0.027(7) 0.040(7) 0.029(7) -0.001(6) 0.004(6) -0.004(6) C25 0.015(6) 0.026(6) 0.031(7) -0.003(6) -0.004(6) -0.002(5) C26 0.029(7) 0.033(7) 0.036(7) -0.002(6) -0.005(6) -0.002(6) C27 0.048(8) 0.049(8) 0.042(8) 0.001(7) 0.002(7) -0.002(7) C28 0.039(7) 0.047(8) 0.047(8) -0.002(7) 0.002(7) 0.007(6) C29 0.043(8) 0.051(8) 0.047(8) 0.003(7) 0.003(7) 0.003(7) C30 0.032(7) 0.037(7) 0.031(7) -0.002(6) -0.002(6) 0.003(6) C31 0.026(6) 0.030(7) 0.023(7) 0.000(6) 0.002(6) -0.001(6) C32 0.017(6) 0.035(7) 0.035(7) 0.003(6) -0.010(6) 0.002(6) C33 0.028(7) 0.034(7) 0.031(7) 0.002(6) -0.008(6) -0.005(6) C34 0.033(7) 0.055(8) 0.046(8) -0.014(7) 0.006(7) -0.005(6) C35 0.049(8) 0.071(9) 0.075(9) -0.013(8) 0.001(8) -0.001(7) C36 0.037(7) 0.058(8) 0.048(8) -0.013(7) -0.007(7) -0.006(7) N37 0.017(5) 0.028(6) 0.021(6) 0.001(5) -0.007(5) 0.000(5) C38 0.024(6) 0.027(6) 0.027(7) -0.002(6) 0.003(6) 0.004(5) C39 0.012(3) 0.014(3) 0.014(4) -0.001(2) -0.002(2) 0.000(2) C40 0.012(6) 0.020(6) 0.017(6) -0.003(5) -0.009(5) 0.002(5) C41 0.017(6) 0.023(6) 0.028(7) -0.003(6) -0.002(6) 0.009(5) C42 0.015(6) 0.023(6) 0.021(7) -0.004(6) -0.009(5) -0.006(5) C43 0.022(6) 0.027(6) 0.020(7) 0.005(6) -0.002(6) -0.001(5) N44 0.028(6) 0.030(6) 0.026(6) 0.000(5) 0.000(5) 0.001(5) C44 0.028(6) 0.030(6) 0.026(6) 0.000(5) 0.000(5) 0.001(5) C45 0.024(7) 0.031(7) 0.035(7) -0.002(6) -0.004(6) -0.001(6) C46 0.040(7) 0.032(7) 0.044(8) -0.002(6) -0.005(7) -0.001(6) C47 0.040(7) 0.044(7) 0.036(8) 0.007(7) -0.005(7) 0.001(6) C48 0.022(6) 0.037(7) 0.035(7) 0.011(6) -0.015(6) -0.004(6) C49 0.022(6) 0.033(7) 0.028(7) 0.001(6) -0.004(6) -0.005(6) C50 0.025(7) 0.044(7) 0.034(8) 0.004(6) -0.003(6) -0.004(6) C51 0.047(8) 0.057(8) 0.029(8) 0.003(7) 0.002(7) -0.007(7) C52 0.052(8) 0.066(8) 0.045(8) 0.008(7) -0.015(7) -0.010(7) C53 0.053(8) 0.048(8) 0.058(9) 0.005(7) -0.010(7) 0.002(7) C54 0.045(7) 0.036(7) 0.036(7) 0.005(7) -0.005(6) -0.003(6) C55 0.023(6) 0.028(6) 0.024(7) -0.007(6) -0.013(6) 0.002(5) C56 0.027(7) 0.048(7) 0.050(8) -0.005(7) -0.013(7) -0.006(6) C57 0.063(9) 0.059(8) 0.061(9) -0.019(7) -0.006(8) -0.005(7) C58 0.049(8) 0.061(8) 0.069(9) -0.014(7) -0.016(7) 0.000(7) C59 0.041(8) 0.062(8) 0.069(9) -0.015(7) -0.015(7) 0.002(7) C60 0.034(7) 0.043(7) 0.052(8) -0.017(7) -0.010(7) 0.005(6) C61 0.028(7) 0.032(7) 0.031(7) -0.001(6) -0.018(6) -0.004(6) C62 0.029(7) 0.030(7) 0.028(7) 0.003(6) -0.006(6) -0.007(6) C63 0.047(8) 0.056(8) 0.045(8) 0.004(7) -0.010(7) -0.007(7) C64 0.059(8) 0.047(8) 0.045(8) 0.004(7) -0.018(7) -0.018(7) C65 0.060(8) 0.051(8) 0.054(9) -0.012(7) -0.020(7) 0.004(7) C66 0.038(7) 0.042(7) 0.037(8) -0.004(7) -0.016(7) -0.006(6) C67 0.012(6) 0.032(7) 0.031(7) -0.005(6) -0.005(5) -0.003(5) C68 0.019(5) 0.031(6) 0.031(6) -0.006(5) -0.003(5) -0.007(4) N68 0.019(5) 0.031(6) 0.031(6) -0.006(5) -0.003(5) -0.007(4) C69 0.024(7) 0.037(7) 0.030(7) -0.006(6) -0.012(6) 0.002(6) C70 0.029(7) 0.038(7) 0.024(7) -0.003(6) -0.012(6) 0.001(6) C71 0.041(7) 0.034(7) 0.037(8) 0.008(6) -0.002(7) 0.007(6) C72 0.022(7) 0.030(7) 0.027(7) -0.003(6) -0.005(6) -0.005(5) P1 0.041(3) 0.046(3) 0.036(3) 0.004(2) -0.017(2) -0.006(2) F1 0.079(7) 0.089(7) 0.095(7) -0.005(6) -0.050(6) 0.012(6) F2 0.103(8) 0.154(9) 0.099(8) -0.020(7) 0.000(7) -0.005(7) F3 0.133(8) 0.078(7) 0.115(8) 0.016(7) -0.044(7) -0.017(6) F4 0.112(8) 0.077(7) 0.095(7) 0.004(6) -0.034(7) -0.017(6) F5 0.102(8) 0.153(9) 0.089(8) -0.021(7) 0.012(7) -0.014(7) F6 0.061(6) 0.103(7) 0.084(7) 0.008(6) -0.032(6) 0.003(6) C80 0.067(9) 0.071(9) 0.085(10) -0.006(8) 0.009(8) -0.001(8) Cl81 0.159(6) 0.113(5) 0.163(6) -0.055(5) -0.063(5) -0.002(5) Cl82 0.124(6) 0.117(5) 0.213(7) 0.049(5) 0.056(5) 0.050(5) Cl83 0.040(3) 0.076(3) 0.119(5) 0.013(3) -0.020(3) 0.008(2) C84 0.076(10) 0.062(9) 0.058(9) -0.002(8) -0.013(8) -0.002(8) Cl85 0.135(5) 0.074(4) 0.101(5) 0.023(4) -0.044(4) 0.000(4) Cl86 0.067(4) 0.106(4) 0.095(4) -0.015(4) -0.014(3) -0.015(3) Cl87 0.057(3) 0.066(3) 0.059(3) 0.003(3) -0.018(3) -0.002(2) C88 0.28(2) 0.27(2) 0.30(2) -0.001(10) 0.034(10) -0.001(10) Cl89 0.159(7) 0.216(8) 0.197(8) -0.041(7) 0.019(6) -0.032(6) Cl90 0.242(10) 0.284(10) 0.298(10) -0.052(8) 0.048(8) -0.026(8) Cl91 0.094(4) 0.067(3) 0.088(4) 0.009(3) -0.009(4) -0.008(3) O100 0.080(7) 0.134(8) 0.013(6) 0.012(6) 0.002(6) 0.059(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. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:17.1(7), B:81.7(4), C:80.3(5), D:89.7(5), E:8.4(8) A:18.3(6), B:68.5(4), C:88.3(5), D:87.2(4), E:14.6(7) ; 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 Rh1 N1 1.982(11) . ? Rh1 C32 1.999(15) . ? Rh1 N37 2.011(11) . ? Rh1 N44 2.035(14) . ? Rh1 C68 2.090(12) . ? Rh1 N8 2.132(11) . ? N1 C6 1.347(16) . ? N1 C2 1.374(17) . ? C2 C3 1.427(18) . ? C2 C7 1.485(18) . ? C3 C4 1.377(19) . ? C3 C13 1.533(19) . ? C4 C5 1.427(18) . ? C4 C19 1.476(18) . ? C5 C6 1.401(18) . ? C5 C25 1.455(18) . ? C6 C31 1.508(19) . ? C7 N8 1.352(16) . ? C7 C12 1.386(18) . ? N8 C9 1.316(17) . ? C9 C10 1.37(2) . ? C9 H9A 0.9500 . ? C10 C11 1.41(2) . ? C10 H10A 0.9500 . ? C11 C12 1.37(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.35(2) . ? C13 C18 1.41(2) . ? C14 C15 1.40(2) . ? C14 H14A 0.9500 . ? C15 C16 1.38(2) . ? C15 H15A 0.9500 . ? C16 C17 1.32(2) . ? C16 H16A 0.9500 . ? C17 C18 1.43(2) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.373(19) . ? C19 C24 1.407(19) . ? C20 C21 1.37(2) . ? C20 H20A 0.9500 . ? C21 C22 1.39(2) . ? C21 H21A 0.9500 . ? C22 C23 1.36(2) . ? C22 H22A 0.9500 . ? C23 C24 1.43(2) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.376(19) . ? C25 C26 1.39(2) . ? C26 C27 1.36(2) . ? C26 H26A 0.9500 . ? C27 C28 1.39(2) . ? C27 H27A 0.9500 . ? C28 C29 1.37(2) . ? C28 H28A 0.9500 . ? C29 C30 1.32(2) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.392(19) . ? C31 C36 1.39(2) . ? C32 C33 1.417(19) . ? C33 C34 1.38(2) . ? C33 H33A 0.9500 . ? C34 C35 1.37(2) . ? C34 H34A 0.9500 . ? C35 C36 1.41(2) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N37 C42 1.337(16) . ? N37 C38 1.353(17) . ? C38 C39 1.400(18) . ? C38 C43 1.464(18) . ? C39 C40 1.365(17) . ? C39 C49 1.512(18) . ? C40 C41 1.414(18) . ? C40 C55 1.540(18) . ? C41 C42 1.417(18) . ? C41 C61 1.483(19) . ? C42 C67 1.494(19) . ? C43 C48 1.392(19) . ? C43 N44 1.433(19) . ? N44 C45 1.365(19) . ? C45 C46 1.35(2) . ? C45 H45A 0.9500 . ? C46 C47 1.38(2) . ? C46 H46A 0.9500 . ? C47 C48 1.37(2) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C54 1.39(2) . ? C49 C50 1.41(2) . ? C50 C51 1.37(2) . ? C50 H50A 0.9500 . ? C51 C52 1.38(2) . ? C51 H51A 0.9500 . ? C52 C53 1.41(2) . ? C52 H52A 0.9500 . ? C53 C54 1.40(2) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.34(2) . ? C55 C60 1.39(2) . ? C56 C57 1.45(2) . ? C56 H56A 0.9500 . ? C57 C58 1.36(2) . ? C57 H57A 0.9500 . ? C58 C59 1.32(2) . ? C58 H58A 0.9500 . ? C59 C60 1.39(2) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C62 1.32(2) . ? C61 C66 1.44(2) . ? C62 C63 1.34(2) . ? C62 H62A 0.9500 . ? C63 C64 1.35(2) . ? C63 H63A 0.9500 . ? C64 C65 1.38(2) . ? C64 H64A 0.9500 . ? C65 C66 1.43(2) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C68 1.379(17) . ? C67 C72 1.375(19) . ? C68 C69 1.408(18) . ? C69 C70 1.347(19) . ? C69 H69A 0.9500 . ? C70 C71 1.40(2) . ? C70 H70A 0.9500 . ? C71 C72 1.40(2) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? P1 F2 1.546(14) . ? P1 F1 1.545(11) . ? P1 F4 1.551(12) . ? P1 F3 1.551(12) . ? P1 F5 1.554(13) . ? P1 F6 1.602(11) . ? C80 Cl83 1.70(2) . ? C80 Cl81 1.74(2) . ? C80 Cl82 1.77(2) . ? C80 H80A 1.0000 . ? C84 Cl85 1.675(18) . ? C84 Cl86 1.785(19) . ? C84 Cl87 1.795(19) . ? C84 H84A 1.0000 . ? C88 Cl89 1.66(2) . ? C88 Cl90 1.79(2) . ? C88 Cl91 1.81(2) . ? C88 H88A 1.0000 . ? 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 Rh1 C32 81.3(5) . . ? N1 Rh1 N37 176.0(5) . . ? C32 Rh1 N37 94.7(5) . . ? N1 Rh1 N44 96.8(5) . . ? C32 Rh1 N44 90.7(6) . . ? N37 Rh1 N44 82.6(5) . . ? N1 Rh1 C68 102.7(5) . . ? C32 Rh1 C68 93.9(5) . . ? N37 Rh1 C68 78.0(5) . . ? N44 Rh1 C68 160.4(5) . . ? N1 Rh1 N8 79.3(4) . . ? C32 Rh1 N8 160.5(5) . . ? N37 Rh1 N8 104.7(4) . . ? N44 Rh1 N8 93.4(5) . . ? C68 Rh1 N8 88.5(4) . . ? C6 N1 C2 123.7(12) . . ? C6 N1 Rh1 118.4(9) . . ? C2 N1 Rh1 117.5(9) . . ? N1 C2 C3 116.9(13) . . ? N1 C2 C7 114.0(11) . . ? C3 C2 C7 129.1(13) . . ? C4 C3 C2 120.4(13) . . ? C4 C3 C13 119.0(12) . . ? C2 C3 C13 120.6(13) . . ? C3 C4 C5 120.6(13) . . ? C3 C4 C19 119.5(12) . . ? C5 C4 C19 119.2(12) . . ? C6 C5 C4 117.4(13) . . ? C6 C5 C25 123.4(12) . . ? C4 C5 C25 119.1(12) . . ? N1 C6 C5 120.8(13) . . ? N1 C6 C31 111.0(12) . . ? C5 C6 C31 128.2(13) . . ? N8 C7 C12 120.4(13) . . ? N8 C7 C2 114.8(12) . . ? C12 C7 C2 124.8(13) . . ? C9 N8 C7 120.8(12) . . ? C9 N8 Rh1 126.1(10) . . ? C7 N8 Rh1 112.9(9) . . ? N8 C9 C10 121.5(15) . . ? N8 C9 H9A 119.2 . . ? C10 C9 H9A 119.2 . . ? C9 C10 C11 118.5(15) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 119.3(15) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C7 119.0(14) . . ? C11 C12 H12A 120.5 . . ? C7 C12 H12A 120.5 . . ? C14 C13 C18 122.6(14) . . ? C14 C13 C3 119.4(13) . . ? C18 C13 C3 117.8(14) . . ? C13 C14 C15 119.8(17) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 119.4(18) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C17 C16 C15 120.5(17) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 122.9(18) . . ? C16 C17 H17A 118.5 . . ? C18 C17 H17A 118.5 . . ? C13 C18 C17 114.5(16) . . ? C13 C18 H18A 122.8 . . ? C17 C18 H18A 122.8 . . ? C20 C19 C24 117.5(14) . . ? C20 C19 C4 122.6(13) . . ? C24 C19 C4 119.8(13) . . ? C21 C20 C19 125.2(16) . . ? C21 C20 H20A 117.4 . . ? C19 C20 H20A 117.4 . . ? C20 C21 C22 115.4(15) . . ? C20 C21 H21A 122.3 . . ? C22 C21 H21A 122.3 . . ? C21 C22 C23 124.2(15) . . ? C21 C22 H22A 117.9 . . ? C23 C22 H22A 117.9 . . ? C22 C23 C24 117.8(15) . . ? C22 C23 H23A 121.1 . . ? C24 C23 H23A 121.1 . . ? C19 C24 C23 119.9(15) . . ? C19 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C30 C25 C26 116.1(14) . . ? C30 C25 C5 123.5(14) . . ? C26 C25 C5 120.4(13) . . ? C27 C26 C25 120.3(15) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 121.2(17) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 117.9(17) . . ? C29 C28 H28A 121.1 . . ? C27 C28 H28A 121.1 . . ? C30 C29 C28 119.7(17) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C25 124.6(16) . . ? C29 C30 H30A 117.7 . . ? C25 C30 H30A 117.7 . . ? C32 C31 C36 119.4(14) . . ? C32 C31 C6 115.7(13) . . ? C36 C31 C6 124.9(14) . . ? C31 C32 C33 118.5(14) . . ? C31 C32 Rh1 113.4(10) . . ? C33 C32 Rh1 127.9(12) . . ? C34 C33 C32 121.4(15) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C33 C34 C35 120.0(17) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 119.3(18) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? C35 C36 C31 121.1(17) . . ? C35 C36 H36A 119.4 . . ? C31 C36 H36A 119.4 . . ? C42 N37 C38 125.3(12) . . ? C42 N37 Rh1 118.2(9) . . ? C38 N37 Rh1 115.8(9) . . ? N37 C38 C39 117.7(13) . . ? N37 C38 C43 113.5(13) . . ? C39 C38 C43 128.1(13) . . ? C40 C39 C38 117.8(12) . . ? C40 C39 C49 121.5(12) . . ? C38 C39 C49 120.7(12) . . ? C39 C40 C41 124.2(12) . . ? C39 C40 C55 119.2(12) . . ? C41 C40 C55 116.3(11) . . ? C40 C41 C42 114.9(12) . . ? C40 C41 C61 121.1(12) . . ? C42 C41 C61 123.9(13) . . ? N37 C42 C41 119.3(13) . . ? N37 C42 C67 114.7(12) . . ? C41 C42 C67 126.0(12) . . ? C48 C43 N44 116.4(13) . . ? C48 C43 C38 125.9(14) . . ? N44 C43 C38 117.3(13) . . ? C45 N44 C43 118.8(14) . . ? C45 N44 Rh1 131.1(12) . . ? C43 N44 Rh1 110.0(9) . . ? N44 C45 C46 124.3(16) . . ? N44 C45 H45A 117.8 . . ? C46 C45 H45A 117.8 . . ? C45 C46 C47 116.8(15) . . ? C45 C46 H46A 121.6 . . ? C47 C46 H46A 121.6 . . ? C48 C47 C46 122.0(16) . . ? C48 C47 H47A 119.0 . . ? C46 C47 H47A 119.0 . . ? C47 C48 C43 121.0(15) . . ? C47 C48 H48A 119.5 . . ? C43 C48 H48A 119.5 . . ? C54 C49 C50 121.1(15) . . ? C54 C49 C39 117.8(13) . . ? C50 C49 C39 121.0(13) . . ? C51 C50 C49 119.8(15) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C50 C51 C52 119.5(17) . . ? C50 C51 H51A 120.3 . . ? C52 C51 H51A 120.3 . . ? C51 C52 C53 121.8(17) . . ? C51 C52 H52A 119.1 . . ? C53 C52 H52A 119.1 . . ? C54 C53 C52 118.7(17) . . ? C54 C53 H53A 120.7 . . ? C52 C53 H53A 120.7 . . ? C49 C54 C53 119.2(16) . . ? C49 C54 H54A 120.4 . . ? C53 C54 H54A 120.4 . . ? C56 C55 C60 119.8(14) . . ? C56 C55 C40 122.1(13) . . ? C60 C55 C40 118.1(13) . . ? C55 C56 C57 119.0(16) . . ? C55 C56 H56A 120.5 . . ? C57 C56 H56A 120.5 . . ? C58 C57 C56 120.0(18) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C59 C58 C57 119.3(19) . . ? C59 C58 H58A 120.3 . . ? C57 C58 H58A 120.3 . . ? C58 C59 C60 122.6(19) . . ? C58 C59 H59A 118.7 . . ? C60 C59 H59A 118.7 . . ? C55 C60 C59 119.1(16) . . ? C55 C60 H60A 120.4 . . ? C59 C60 H60A 120.4 . . ? C62 C61 C66 120.1(15) . . ? C62 C61 C41 124.4(14) . . ? C66 C61 C41 115.5(14) . . ? C61 C62 C63 123.0(16) . . ? C61 C62 H62A 118.5 . . ? C63 C62 H62A 118.5 . . ? C64 C63 C62 120.2(18) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C63 C64 C65 121.7(18) . . ? C63 C64 H64A 119.1 . . ? C65 C64 H64A 119.1 . . ? C64 C65 C66 118.8(17) . . ? C64 C65 H65A 120.6 . . ? C66 C65 H65A 120.6 . . ? C65 C66 C61 116.2(16) . . ? C65 C66 H66A 121.9 . . ? C61 C66 H66A 121.9 . . ? C68 C67 C72 121.2(14) . . ? C68 C67 C42 111.9(12) . . ? C72 C67 C42 126.9(13) . . ? C67 C68 C69 117.6(13) . . ? C67 C68 Rh1 115.7(10) . . ? C69 C68 Rh1 126.1(10) . . ? C70 C69 C68 123.1(14) . . ? C70 C69 H69A 118.5 . . ? C68 C69 H69A 118.5 . . ? C69 C70 C71 118.2(14) . . ? C69 C70 H70A 120.9 . . ? C71 C70 H70A 120.9 . . ? C72 C71 C70 120.3(15) . . ? C72 C71 H71A 119.9 . . ? C70 C71 H71A 119.9 . . ? C67 C72 C71 119.5(14) . . ? C67 C72 H72A 120.3 . . ? C71 C72 H72A 120.3 . . ? F2 P1 F1 92.9(8) . . ? F2 P1 F4 89.1(8) . . ? F1 P1 F4 89.0(7) . . ? F2 P1 F3 91.2(8) . . ? F1 P1 F3 91.1(7) . . ? F4 P1 F3 179.7(10) . . ? F2 P1 F5 175.3(9) . . ? F1 P1 F5 89.9(8) . . ? F4 P1 F5 87.2(8) . . ? F3 P1 F5 92.5(8) . . ? F2 P1 F6 84.7(7) . . ? F1 P1 F6 177.6(8) . . ? F4 P1 F6 91.1(7) . . ? F3 P1 F6 88.8(7) . . ? F5 P1 F6 92.5(7) . . ? Cl83 C80 Cl81 113.7(13) . . ? Cl83 C80 Cl82 111.6(12) . . ? Cl81 C80 Cl82 109.3(12) . . ? Cl83 C80 H80A 107.3 . . ? Cl81 C80 H80A 107.3 . . ? Cl82 C80 H80A 107.3 . . ? Cl85 C84 Cl86 110.5(10) . . ? Cl85 C84 Cl87 110.4(11) . . ? Cl86 C84 Cl87 106.8(10) . . ? Cl85 C84 H84A 109.7 . . ? Cl86 C84 H84A 109.7 . . ? Cl87 C84 H84A 109.7 . . ? Cl89 C88 Cl90 108.6(13) . . ? Cl89 C88 Cl91 111.8(13) . . ? Cl90 C88 Cl91 106.7(12) . . ? Cl89 C88 H88A 109.9 . . ? Cl90 C88 H88A 109.9 . . ? Cl91 C88 H88A 109.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 Rh1 N1 C6 5.0(10) . . . . ? N37 Rh1 N1 C6 -4(7) . . . . ? N44 Rh1 N1 C6 -84.6(10) . . . . ? C68 Rh1 N1 C6 97.1(10) . . . . ? N8 Rh1 N1 C6 -176.9(10) . . . . ? C32 Rh1 N1 C2 177.4(11) . . . . ? N37 Rh1 N1 C2 169(6) . . . . ? N44 Rh1 N1 C2 87.8(10) . . . . ? C68 Rh1 N1 C2 -90.4(10) . . . . ? N8 Rh1 N1 C2 -4.5(10) . . . . ? C6 N1 C2 C3 5(2) . . . . ? Rh1 N1 C2 C3 -167.2(10) . . . . ? C6 N1 C2 C7 -176.8(12) . . . . ? Rh1 N1 C2 C7 11.2(15) . . . . ? N1 C2 C3 C4 -7(2) . . . . ? C7 C2 C3 C4 175.2(14) . . . . ? N1 C2 C3 C13 176.1(13) . . . . ? C7 C2 C3 C13 -2(2) . . . . ? C2 C3 C4 C5 4(2) . . . . ? C13 C3 C4 C5 -178.9(13) . . . . ? C2 C3 C4 C19 173.9(13) . . . . ? C13 C3 C4 C19 -9(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C19 C4 C5 C6 -168.9(13) . . . . ? C3 C4 C5 C25 179.0(13) . . . . ? C19 C4 C5 C25 9(2) . . . . ? C2 N1 C6 C5 0(2) . . . . ? Rh1 N1 C6 C5 172.1(10) . . . . ? C2 N1 C6 C31 -177.6(12) . . . . ? Rh1 N1 C6 C31 -5.6(15) . . . . ? C4 C5 C6 N1 -3(2) . . . . ? C25 C5 C6 N1 179.0(13) . . . . ? C4 C5 C6 C31 174.1(14) . . . . ? C25 C5 C6 C31 -4(2) . . . . ? N1 C2 C7 N8 -14.2(18) . . . . ? C3 C2 C7 N8 164.0(14) . . . . ? N1 C2 C7 C12 164.9(13) . . . . ? C3 C2 C7 C12 -17(2) . . . . ? C12 C7 N8 C9 6(2) . . . . ? C2 C7 N8 C9 -174.6(13) . . . . ? C12 C7 N8 Rh1 -168.8(11) . . . . ? C2 C7 N8 Rh1 10.4(15) . . . . ? N1 Rh1 N8 C9 -178.3(13) . . . . ? C32 Rh1 N8 C9 -172.6(16) . . . . ? N37 Rh1 N8 C9 2.2(13) . . . . ? N44 Rh1 N8 C9 85.4(13) . . . . ? C68 Rh1 N8 C9 -75.0(13) . . . . ? N1 Rh1 N8 C7 -3.6(9) . . . . ? C32 Rh1 N8 C7 2(2) . . . . ? N37 Rh1 N8 C7 176.9(9) . . . . ? N44 Rh1 N8 C7 -99.9(10) . . . . ? C68 Rh1 N8 C7 99.7(10) . . . . ? C7 N8 C9 C10 -8(2) . . . . ? Rh1 N8 C9 C10 166.6(12) . . . . ? N8 C9 C10 C11 3(3) . . . . ? C9 C10 C11 C12 3(3) . . . . ? C10 C11 C12 C7 -5(2) . . . . ? N8 C7 C12 C11 0(2) . . . . ? C2 C7 C12 C11 -178.9(14) . . . . ? C4 C3 C13 C14 96.5(18) . . . . ? C2 C3 C13 C14 -86.2(18) . . . . ? C4 C3 C13 C18 -77.8(18) . . . . ? C2 C3 C13 C18 99.5(17) . . . . ? C18 C13 C14 C15 -1(2) . . . . ? C3 C13 C14 C15 -175.4(14) . . . . ? C13 C14 C15 C16 2(3) . . . . ? C14 C15 C16 C17 -5(3) . . . . ? C15 C16 C17 C18 6(3) . . . . ? C14 C13 C18 C17 2(2) . . . . ? C3 C13 C18 C17 176.6(13) . . . . ? C16 C17 C18 C13 -5(2) . . . . ? C3 C4 C19 C20 -74.7(19) . . . . ? C5 C4 C19 C20 95.5(17) . . . . ? C3 C4 C19 C24 106.8(16) . . . . ? C5 C4 C19 C24 -83.0(18) . . . . ? C24 C19 C20 C21 -1(2) . . . . ? C4 C19 C20 C21 -179.8(15) . . . . ? C19 C20 C21 C22 2(2) . . . . ? C20 C21 C22 C23 -3(2) . . . . ? C21 C22 C23 C24 2(2) . . . . ? C20 C19 C24 C23 1(2) . . . . ? C4 C19 C24 C23 179.5(13) . . . . ? C22 C23 C24 C19 -2(2) . . . . ? C6 C5 C25 C30 88.6(19) . . . . ? C4 C5 C25 C30 -89.1(18) . . . . ? C6 C5 C25 C26 -91.9(18) . . . . ? C4 C5 C25 C26 90.4(17) . . . . ? C30 C25 C26 C27 -2(2) . . . . ? C5 C25 C26 C27 178.5(14) . . . . ? C25 C26 C27 C28 -2(2) . . . . ? C26 C27 C28 C29 5(3) . . . . ? C27 C28 C29 C30 -3(3) . . . . ? C28 C29 C30 C25 -1(3) . . . . ? C26 C25 C30 C29 4(2) . . . . ? C5 C25 C30 C29 -176.8(15) . . . . ? N1 C6 C31 C32 3.0(18) . . . . ? C5 C6 C31 C32 -174.6(14) . . . . ? N1 C6 C31 C36 -174.5(14) . . . . ? C5 C6 C31 C36 8(2) . . . . ? C36 C31 C32 C33 -6(2) . . . . ? C6 C31 C32 C33 176.7(13) . . . . ? C36 C31 C32 Rh1 178.5(12) . . . . ? C6 C31 C32 Rh1 0.9(17) . . . . ? N1 Rh1 C32 C31 -3.0(11) . . . . ? N37 Rh1 C32 C31 176.4(11) . . . . ? N44 Rh1 C32 C31 93.8(11) . . . . ? C68 Rh1 C32 C31 -105.3(11) . . . . ? N8 Rh1 C32 C31 -9(2) . . . . ? N1 Rh1 C32 C33 -178.3(14) . . . . ? N37 Rh1 C32 C33 1.1(14) . . . . ? N44 Rh1 C32 C33 -81.5(14) . . . . ? C68 Rh1 C32 C33 79.4(14) . . . . ? N8 Rh1 C32 C33 176.1(12) . . . . ? C31 C32 C33 C34 3(2) . . . . ? Rh1 C32 C33 C34 178.2(12) . . . . ? C32 C33 C34 C35 -1(3) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C34 C35 C36 C31 -3(3) . . . . ? C32 C31 C36 C35 6(3) . . . . ? C6 C31 C36 C35 -176.6(16) . . . . ? N1 Rh1 N37 C42 95(7) . . . . ? C32 Rh1 N37 C42 86.5(11) . . . . ? N44 Rh1 N37 C42 176.6(10) . . . . ? C68 Rh1 N37 C42 -6.6(10) . . . . ? N8 Rh1 N37 C42 -91.8(10) . . . . ? N1 Rh1 N37 C38 -76(7) . . . . ? C32 Rh1 N37 C38 -84.6(10) . . . . ? N44 Rh1 N37 C38 5.5(10) . . . . ? C68 Rh1 N37 C38 -177.6(10) . . . . ? N8 Rh1 N37 C38 97.1(10) . . . . ? C42 N37 C38 C39 -9(2) . . . . ? Rh1 N37 C38 C39 161.5(10) . . . . ? C42 N37 C38 C43 -180.0(12) . . . . ? Rh1 N37 C38 C43 -9.6(15) . . . . ? N37 C38 C39 C40 6.7(19) . . . . ? C43 C38 C39 C40 176.4(13) . . . . ? N37 C38 C39 C49 -171.4(12) . . . . ? C43 C38 C39 C49 -2(2) . . . . ? C38 C39 C40 C41 1.3(19) . . . . ? C49 C39 C40 C41 179.4(12) . . . . ? C38 C39 C40 C55 -172.7(12) . . . . ? C49 C39 C40 C55 5.5(19) . . . . ? C39 C40 C41 C42 -7.3(19) . . . . ? C55 C40 C41 C42 166.7(12) . . . . ? C39 C40 C41 C61 177.0(13) . . . . ? C55 C40 C41 C61 -8.9(19) . . . . ? C38 N37 C42 C41 2(2) . . . . ? Rh1 N37 C42 C41 -167.7(10) . . . . ? C38 N37 C42 C67 -177.1(12) . . . . ? Rh1 N37 C42 C67 12.8(15) . . . . ? C40 C41 C42 N37 5.5(19) . . . . ? C61 C41 C42 N37 -179.0(13) . . . . ? C40 C41 C42 C67 -175.1(12) . . . . ? C61 C41 C42 C67 0(2) . . . . ? N37 C38 C43 C48 -163.7(14) . . . . ? C39 C38 C43 C48 26(2) . . . . ? N37 C38 C43 N44 9.8(18) . . . . ? C39 C38 C43 N44 -160.2(14) . . . . ? C48 C43 N44 C45 -9(2) . . . . ? C38 C43 N44 C45 177.0(13) . . . . ? C48 C43 N44 Rh1 169.0(10) . . . . ? C38 C43 N44 Rh1 -5.2(15) . . . . ? N1 Rh1 N44 C45 -6.6(14) . . . . ? C32 Rh1 N44 C45 -87.9(14) . . . . ? N37 Rh1 N44 C45 177.5(14) . . . . ? C68 Rh1 N44 C45 168.3(13) . . . . ? N8 Rh1 N44 C45 73.1(14) . . . . ? N1 Rh1 N44 C43 176.0(10) . . . . ? C32 Rh1 N44 C43 94.7(10) . . . . ? N37 Rh1 N44 C43 0.0(10) . . . . ? C68 Rh1 N44 C43 -9(2) . . . . ? N8 Rh1 N44 C43 -104.4(10) . . . . ? C43 N44 C45 C46 6(2) . . . . ? Rh1 N44 C45 C46 -171.4(12) . . . . ? N44 C45 C46 C47 1(2) . . . . ? C45 C46 C47 C48 -4(2) . . . . ? C46 C47 C48 C43 1(2) . . . . ? N44 C43 C48 C47 6(2) . . . . ? C38 C43 C48 C47 179.2(14) . . . . ? C40 C39 C49 C54 -108.7(15) . . . . ? C38 C39 C49 C54 69.4(18) . . . . ? C40 C39 C49 C50 72.3(18) . . . . ? C38 C39 C49 C50 -109.7(16) . . . . ? C54 C49 C50 C51 -1(2) . . . . ? C39 C49 C50 C51 177.8(14) . . . . ? C49 C50 C51 C52 0(2) . . . . ? C50 C51 C52 C53 1(3) . . . . ? C51 C52 C53 C54 -1(3) . . . . ? C50 C49 C54 C53 2(2) . . . . ? C39 C49 C54 C53 -177.4(14) . . . . ? C52 C53 C54 C49 0(2) . . . . ? C39 C40 C55 C56 -95.7(17) . . . . ? C41 C40 C55 C56 90.0(17) . . . . ? C39 C40 C55 C60 83.3(18) . . . . ? C41 C40 C55 C60 -91.1(16) . . . . ? C60 C55 C56 C57 1(2) . . . . ? C40 C55 C56 C57 -179.8(14) . . . . ? C55 C56 C57 C58 -2(3) . . . . ? C56 C57 C58 C59 3(3) . . . . ? C57 C58 C59 C60 -3(3) . . . . ? C56 C55 C60 C59 -1(3) . . . . ? C40 C55 C60 C59 180.0(15) . . . . ? C58 C59 C60 C55 2(3) . . . . ? C40 C41 C61 C62 91.8(18) . . . . ? C42 C41 C61 C62 -83.5(19) . . . . ? C40 C41 C61 C66 -90.8(16) . . . . ? C42 C41 C61 C66 94.0(17) . . . . ? C66 C61 C62 C63 -2(2) . . . . ? C41 C61 C62 C63 175.8(15) . . . . ? C61 C62 C63 C64 0(3) . . . . ? C62 C63 C64 C65 1(3) . . . . ? C63 C64 C65 C66 -1(3) . . . . ? C64 C65 C66 C61 0(2) . . . . ? C62 C61 C66 C65 1(2) . . . . ? C41 C61 C66 C65 -176.1(14) . . . . ? N37 C42 C67 C68 -13.3(17) . . . . ? C41 C42 C67 C68 167.3(13) . . . . ? N37 C42 C67 C72 167.8(14) . . . . ? C41 C42 C67 C72 -12(2) . . . . ? C72 C67 C68 C69 -1(2) . . . . ? C42 C67 C68 C69 179.8(11) . . . . ? C72 C67 C68 Rh1 -173.1(10) . . . . ? C42 C67 C68 Rh1 7.9(14) . . . . ? N1 Rh1 C68 C67 -177.3(10) . . . . ? C32 Rh1 C68 C67 -95.4(11) . . . . ? N37 Rh1 C68 C67 -1.4(10) . . . . ? N44 Rh1 C68 C67 8(2) . . . . ? N8 Rh1 C68 C67 104.0(10) . . . . ? N1 Rh1 C68 C69 11.6(12) . . . . ? C32 Rh1 C68 C69 93.6(12) . . . . ? N37 Rh1 C68 C69 -172.5(12) . . . . ? N44 Rh1 C68 C69 -163.1(14) . . . . ? N8 Rh1 C68 C69 -67.1(11) . . . . ? C67 C68 C69 C70 2(2) . . . . ? Rh1 C68 C69 C70 173.4(11) . . . . ? C68 C69 C70 C71 -4(2) . . . . ? C69 C70 C71 C72 4(2) . . . . ? C68 C67 C72 C71 1(2) . . . . ? C42 C67 C72 C71 -179.7(13) . . . . ? C70 C71 C72 C67 -3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.482 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.204 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 644550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 N2 O2 Pd, C H4 O' _chemical_formula_sum 'C37 H30 N2 O3 Pd' _chemical_formula_weight 657.03 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' Pd Pd -0.9988 1.0072 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2973(6) _cell_length_b 12.3281(7) _cell_length_c 12.8367(8) _cell_angle_alpha 94.3690(10) _cell_angle_beta 103.5000(10) _cell_angle_gamma 109.5570(10) _cell_volume 1471.80(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5300 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.58 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_T_max 0.8039 _exptl_absorpt_process_details 'blessing Acta Cryst. 1995(A51) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13720 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6708 _reflns_number_gt 6204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.9507P] 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 6708 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Pd1 Pd 0.395748(18) 0.708296(14) 0.361339(13) 0.02165(7) Uani 1 1 d . . . N1 N 0.3388(2) 0.59788(17) 0.45952(15) 0.0213(4) Uani 1 1 d . A . C2 C 0.2392(2) 0.4900(2) 0.41635(18) 0.0223(4) Uani 1 1 d . . . C3 C 0.1884(2) 0.4141(2) 0.48601(18) 0.0222(4) Uani 1 1 d . A . C4 C 0.2439(2) 0.4527(2) 0.59882(18) 0.0219(4) Uani 1 1 d . . . C5 C 0.3487(2) 0.5648(2) 0.64138(18) 0.0226(4) Uani 1 1 d . A . C6 C 0.3974(2) 0.6366(2) 0.56816(18) 0.0216(4) Uani 1 1 d . . . C7 C 0.2542(3) 0.5643(2) 0.24774(18) 0.0283(5) Uani 0.47(2) 1 d P A 1 N7 N 0.2542(3) 0.5643(2) 0.24774(18) 0.0283(5) Uani 0.53(2) 1 d P A 2 C8 C 0.2210(3) 0.5531(3) 0.1370(2) 0.0346(6) Uani 1 1 d . . . H8A H 0.2595 0.6193 0.1050 0.042 Uiso 1 1 calc R A 1 C9 C 0.1335(3) 0.4488(3) 0.0706(2) 0.0389(6) Uani 1 1 d . A . H9A H 0.1113 0.4435 -0.0061 0.047 Uiso 1 1 calc R . . C10 C 0.0783(4) 0.3520(3) 0.1165(2) 0.0466(7) Uani 1 1 d . . . H10A H 0.0197 0.2790 0.0715 0.056 Uiso 1 1 calc R A . C11 C 0.1090(3) 0.3620(3) 0.2290(2) 0.0400(6) Uani 1 1 d . A . H11A H 0.0700 0.2960 0.2610 0.048 Uiso 1 1 calc R . . C12 C 0.1966(3) 0.4683(2) 0.29463(19) 0.0263(5) Uani 1 1 d . A . N13 N 0.5162(2) 0.8139(2) 0.5044(2) 0.0278(5) Uani 0.47(2) 1 d P A 1 C13 C 0.5162(2) 0.8139(2) 0.5044(2) 0.0278(5) Uani 0.53(2) 1 d P A 2 C14 C 0.5068(2) 0.7572(2) 0.59370(19) 0.0242(4) Uani 1 1 d . A . C15 C 0.5986(3) 0.8141(2) 0.6962(2) 0.0303(5) Uani 1 1 d . . . H15A H 0.5957 0.7750 0.7571 0.036 Uiso 1 1 calc R A . C16 C 0.6948(3) 0.9287(2) 0.7090(2) 0.0344(6) Uani 1 1 d . A . H16A H 0.7589 0.9671 0.7783 0.041 Uiso 1 1 calc R . . C17 C 0.6962(3) 0.9856(2) 0.6209(2) 0.0336(6) Uani 1 1 d . . . H17A H 0.7572 1.0650 0.6301 0.040 Uiso 1 1 calc R A . C18 C 0.6089(3) 0.9272(2) 0.5192(2) 0.0305(5) Uani 1 1 d . A . H18A H 0.6131 0.9662 0.4584 0.037 Uiso 1 1 calc R B 1 C19 C 0.0733(2) 0.2953(2) 0.44716(18) 0.0228(4) Uani 1 1 d . . . C20 C -0.0693(3) 0.2823(2) 0.4308(2) 0.0298(5) Uani 1 1 d . A . H20A H -0.0940 0.3489 0.4428 0.036 Uiso 1 1 calc R . . C21 C -0.1764(3) 0.1719(2) 0.3968(2) 0.0347(6) Uani 1 1 d . . . H21A H -0.2740 0.1634 0.3860 0.042 Uiso 1 1 calc R A . C22 C -0.1410(3) 0.0746(2) 0.3787(2) 0.0325(5) Uani 1 1 d . A . H22A H -0.2142 -0.0005 0.3542 0.039 Uiso 1 1 calc R . . C23 C 0.0013(3) 0.0872(2) 0.3965(2) 0.0325(5) Uani 1 1 d . . . H23A H 0.0260 0.0204 0.3851 0.039 Uiso 1 1 calc R A . C24 C 0.1085(3) 0.1971(2) 0.4310(2) 0.0296(5) Uani 1 1 d . A . H24A H 0.2062 0.2052 0.4436 0.036 Uiso 1 1 calc R . . C25 C 0.1880(2) 0.3737(2) 0.67382(18) 0.0226(4) Uani 1 1 d . A . C26 C 0.0681(3) 0.3740(2) 0.7051(2) 0.0301(5) Uani 1 1 d . . . H26A H 0.0235 0.4273 0.6812 0.036 Uiso 1 1 calc R A . C27 C 0.0121(3) 0.2969(2) 0.7715(2) 0.0338(5) Uani 1 1 d . A . H27A H -0.0709 0.2967 0.7918 0.041 Uiso 1 1 calc R . . C28 C 0.0786(3) 0.2206(2) 0.8075(2) 0.0330(5) Uani 1 1 d . . . H28A H 0.0416 0.1683 0.8532 0.040 Uiso 1 1 calc R A . C29 C 0.1992(3) 0.2202(2) 0.7770(2) 0.0334(5) Uani 1 1 d . A . H29A H 0.2444 0.1675 0.8017 0.040 Uiso 1 1 calc R . . C30 C 0.2541(3) 0.2964(2) 0.7103(2) 0.0299(5) Uani 1 1 d . . . H30A H 0.3366 0.2959 0.6895 0.036 Uiso 1 1 calc R A . C31 C 0.3958(3) 0.6050(2) 0.76185(18) 0.0241(4) Uani 1 1 d . . . C32 C 0.5077(3) 0.5819(2) 0.8287(2) 0.0312(5) Uani 1 1 d . A . H32A H 0.5554 0.5394 0.7979 0.037 Uiso 1 1 calc R . . C33 C 0.5498(3) 0.6207(3) 0.9400(2) 0.0365(6) Uani 1 1 d . . . H33A H 0.6266 0.6051 0.9851 0.044 Uiso 1 1 calc R A . C34 C 0.4805(3) 0.6817(3) 0.9855(2) 0.0372(6) Uani 1 1 d . A . H34A H 0.5101 0.7089 1.0616 0.045 Uiso 1 1 calc R . . C35 C 0.3675(3) 0.7034(3) 0.9197(2) 0.0389(6) Uani 1 1 d . . . H35A H 0.3185 0.7442 0.9510 0.047 Uiso 1 1 calc R A . C36 C 0.3258(3) 0.6654(2) 0.8082(2) 0.0316(5) Uani 1 1 d . A . H36A H 0.2488 0.6810 0.7634 0.038 Uiso 1 1 calc R . . C40 C 0.4148(3) 0.8642(2) 0.1941(2) 0.0284(5) Uani 1 1 d . . . C41 C 0.5064(3) 0.9627(2) 0.1494(2) 0.0365(6) Uani 1 1 d . A . H41A H 0.4449 0.9838 0.0903 0.055 Uiso 1 1 calc R . . H41B H 0.5746 0.9376 0.1217 0.055 Uiso 1 1 calc R . . H41C H 0.5590 1.0306 0.2073 0.055 Uiso 1 1 calc R . . O42 O 0.2836(2) 0.82197(17) 0.15361(16) 0.0363(4) Uani 1 1 d . A . O43 O 0.4836(2) 0.83008(16) 0.27290(15) 0.0325(4) Uani 1 1 d . A . O50 O 0.1153(3) 0.9168(2) 0.0294(2) 0.0599(6) Uani 1 1 d . . . H50 H 0.1762 0.8892 0.0589 0.090 Uiso 1 1 calc R . . C51 C 0.1581(6) 0.9731(6) -0.0495(5) 0.105(2) Uani 1 1 d . . . H51A H 0.2062 1.0569 -0.0212 0.157 Uiso 1 1 calc R . . H51B H 0.0745 0.9604 -0.1109 0.157 Uiso 1 1 calc R . . H51C H 0.2247 0.9430 -0.0739 0.157 Uiso 1 1 calc R . . 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 Pd1 0.02608(10) 0.02001(10) 0.02326(10) 0.00975(7) 0.01246(7) 0.00876(7) N1 0.0251(9) 0.0205(9) 0.0229(9) 0.0086(7) 0.0122(7) 0.0091(8) C2 0.0257(11) 0.0205(11) 0.0232(10) 0.0062(8) 0.0100(8) 0.0088(9) C3 0.0246(11) 0.0201(11) 0.0256(11) 0.0069(8) 0.0115(9) 0.0090(9) C4 0.0229(10) 0.0221(11) 0.0255(11) 0.0097(9) 0.0120(9) 0.0094(9) C5 0.0250(11) 0.0240(11) 0.0229(10) 0.0077(8) 0.0111(8) 0.0104(9) C6 0.0223(10) 0.0209(10) 0.0247(10) 0.0066(8) 0.0108(8) 0.0082(8) C7 0.0400(13) 0.0318(12) 0.0242(10) 0.0112(9) 0.0155(9) 0.0208(10) N7 0.0400(13) 0.0318(12) 0.0242(10) 0.0112(9) 0.0155(9) 0.0208(10) C8 0.0526(16) 0.0385(15) 0.0249(12) 0.0130(10) 0.0155(11) 0.0269(13) C9 0.0525(17) 0.0453(16) 0.0237(12) 0.0088(11) 0.0107(11) 0.0231(14) C10 0.0583(19) 0.0421(17) 0.0272(13) 0.0014(12) 0.0096(13) 0.0056(14) C11 0.0495(17) 0.0341(14) 0.0274(13) 0.0061(11) 0.0135(12) 0.0017(12) C12 0.0321(12) 0.0273(12) 0.0235(11) 0.0086(9) 0.0125(9) 0.0118(10) N13 0.0252(11) 0.0247(11) 0.0380(12) 0.0129(9) 0.0138(9) 0.0096(9) C13 0.0252(11) 0.0247(11) 0.0380(12) 0.0129(9) 0.0138(9) 0.0096(9) C14 0.0251(11) 0.0214(11) 0.0305(11) 0.0075(9) 0.0146(9) 0.0087(9) C15 0.0345(13) 0.0256(12) 0.0291(12) 0.0049(10) 0.0138(10) 0.0053(10) C16 0.0370(14) 0.0254(13) 0.0377(14) -0.0010(10) 0.0142(11) 0.0062(11) C17 0.0326(13) 0.0189(11) 0.0519(16) 0.0071(11) 0.0187(12) 0.0075(10) C18 0.0287(12) 0.0222(12) 0.0467(14) 0.0144(10) 0.0176(11) 0.0103(10) C19 0.0267(11) 0.0205(11) 0.0231(10) 0.0085(8) 0.0106(9) 0.0075(9) C20 0.0286(12) 0.0249(12) 0.0389(13) 0.0076(10) 0.0120(10) 0.0111(10) C21 0.0249(12) 0.0327(14) 0.0460(15) 0.0074(11) 0.0121(11) 0.0083(10) C22 0.0317(13) 0.0244(12) 0.0387(13) 0.0067(10) 0.0136(11) 0.0039(10) C23 0.0352(13) 0.0211(12) 0.0434(14) 0.0073(10) 0.0138(11) 0.0107(10) C24 0.0261(12) 0.0259(12) 0.0393(13) 0.0069(10) 0.0123(10) 0.0098(10) C25 0.0259(11) 0.0203(11) 0.0224(10) 0.0073(8) 0.0101(8) 0.0061(9) C26 0.0331(12) 0.0291(12) 0.0371(13) 0.0167(10) 0.0185(10) 0.0144(10) C27 0.0355(13) 0.0354(14) 0.0370(13) 0.0136(11) 0.0225(11) 0.0108(11) C28 0.0443(15) 0.0257(12) 0.0282(12) 0.0118(10) 0.0159(11) 0.0062(11) C29 0.0432(14) 0.0267(12) 0.0350(13) 0.0156(10) 0.0128(11) 0.0150(11) C30 0.0329(13) 0.0294(13) 0.0351(13) 0.0143(10) 0.0159(10) 0.0147(10) C31 0.0289(11) 0.0224(11) 0.0213(10) 0.0086(8) 0.0108(9) 0.0059(9) C32 0.0356(13) 0.0328(13) 0.0304(12) 0.0091(10) 0.0118(10) 0.0163(11) C33 0.0416(15) 0.0402(15) 0.0289(12) 0.0120(11) 0.0061(11) 0.0173(12) C34 0.0477(16) 0.0419(15) 0.0215(11) 0.0058(10) 0.0098(11) 0.0152(13) C35 0.0488(16) 0.0474(17) 0.0277(13) 0.0042(11) 0.0146(12) 0.0242(14) C36 0.0355(13) 0.0371(14) 0.0274(12) 0.0081(10) 0.0108(10) 0.0178(11) C40 0.0384(13) 0.0240(12) 0.0298(12) 0.0107(9) 0.0190(10) 0.0123(10) C41 0.0419(15) 0.0320(14) 0.0396(14) 0.0182(11) 0.0190(12) 0.0105(12) O42 0.0357(10) 0.0344(10) 0.0422(10) 0.0188(8) 0.0162(8) 0.0107(8) O43 0.0356(10) 0.0300(9) 0.0360(9) 0.0175(8) 0.0168(8) 0.0098(8) O50 0.0602(16) 0.0617(16) 0.0573(15) 0.0193(12) 0.0147(12) 0.0206(13) C51 0.084(3) 0.138(5) 0.130(5) 0.105(4) 0.052(3) 0.055(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. The tilt angles made between the central 'NC5' ring and the peripheral aromatic rings. These are given a letter code, with the 'A' ring being the pyridyl, and the remaining rings numbered in a clockwise fashion (see text for details). Values were calculated using SHELXL. An approximate (isotropic) treatment of cell esds is used for estimating esds. A:7.6(1), B:89.4(1), C:88.9(1), D:86.4(1), E:10.4(1) ; 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 Pd1 N1 1.9641(18) . ? Pd1 N13 2.024(2) . ? Pd1 O43 2.0472(17) . ? Pd1 C7 2.070(2) . ? N1 C2 1.355(3) . ? N1 C6 1.360(3) . ? C2 C3 1.402(3) . ? C2 C12 1.498(3) . ? C3 C4 1.406(3) . ? C3 C19 1.500(3) . ? C4 C5 1.408(3) . ? C4 C25 1.495(3) . ? C5 C6 1.403(3) . ? C5 C31 1.498(3) . ? C6 C14 1.489(3) . ? C7 C8 1.366(3) . ? C7 C12 1.385(3) . ? C8 C9 1.375(4) . ? C8 H8A 0.9500 . ? C9 C10 1.379(4) . ? C9 H9A 0.9500 . ? C10 C11 1.391(4) . ? C10 H10A 0.9500 . ? C11 C12 1.388(4) . ? C11 H11A 0.9500 . ? N13 C18 1.371(3) . ? N13 C14 1.393(3) . ? C14 C15 1.397(4) . ? C15 C16 1.399(4) . ? C15 H15A 0.9500 . ? C16 C17 1.376(4) . ? C16 H16A 0.9500 . ? C17 C18 1.381(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.385(3) . ? C19 C24 1.389(3) . ? C20 C21 1.393(4) . ? C20 H20A 0.9500 . ? C21 C22 1.385(4) . ? C21 H21A 0.9500 . ? C22 C23 1.382(4) . ? C22 H22A 0.9500 . ? C23 C24 1.389(4) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.386(3) . ? C25 C30 1.394(3) . ? C26 C27 1.395(3) . ? C26 H26A 0.9500 . ? C27 C28 1.385(4) . ? C27 H27A 0.9500 . ? C28 C29 1.388(4) . ? C28 H28A 0.9500 . ? C29 C30 1.389(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.386(3) . ? C31 C32 1.393(3) . ? C32 C33 1.389(4) . ? C32 H32A 0.9500 . ? C33 C34 1.380(4) . ? C33 H33A 0.9500 . ? C34 C35 1.386(4) . ? C34 H34A 0.9500 . ? C35 C36 1.388(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C40 C41 1.512(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O42 C40 1.235(3) . ? O43 C40 1.277(3) . ? O50 C51 1.346(5) . ? O50 H50 0.8400 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 Pd1 N13 81.51(9) . . ? N1 Pd1 O43 171.99(7) . . ? N13 Pd1 O43 92.51(8) . . ? N1 Pd1 C7 80.52(8) . . ? N13 Pd1 C7 162.03(9) . . ? O43 Pd1 C7 105.38(8) . . ? C2 N1 C6 123.64(19) . . ? C2 N1 Pd1 118.77(15) . . ? C6 N1 Pd1 117.52(15) . . ? N1 C2 C3 119.2(2) . . ? N1 C2 C12 112.69(19) . . ? C3 C2 C12 128.1(2) . . ? C40 O43 Pd1 126.23(17) . . ? C2 C3 C4 118.5(2) . . ? C2 C3 C19 123.7(2) . . ? C4 C3 C19 117.71(19) . . ? C3 C4 C5 121.0(2) . . ? C3 C4 C25 119.0(2) . . ? C5 C4 C25 120.0(2) . . ? C6 C5 C4 118.2(2) . . ? C6 C5 C31 122.9(2) . . ? C4 C5 C31 118.8(2) . . ? N1 C6 C5 119.3(2) . . ? N1 C6 C14 112.77(19) . . ? C5 C6 C14 127.9(2) . . ? C8 C7 C12 119.2(2) . . ? C8 C7 Pd1 127.9(2) . . ? C12 C7 Pd1 112.78(16) . . ? C7 C8 C9 121.9(3) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C7 C12 C11 119.8(2) . . ? C7 C12 C2 115.0(2) . . ? C11 C12 C2 125.2(2) . . ? C18 N13 C14 119.7(2) . . ? C18 N13 Pd1 127.20(19) . . ? C14 N13 Pd1 112.97(17) . . ? N13 C14 C15 119.4(2) . . ? N13 C14 C6 114.7(2) . . ? C15 C14 C6 125.9(2) . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? N13 C18 C17 121.2(2) . . ? N13 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C20 C19 C24 119.4(2) . . ? C20 C19 C3 119.9(2) . . ? C24 C19 C3 120.6(2) . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C19 C24 C23 120.2(2) . . ? C19 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C30 119.5(2) . . ? C26 C25 C4 120.6(2) . . ? C30 C25 C4 119.9(2) . . ? C25 C26 C27 120.7(2) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 119.5(2) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 120.2(2) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C28 C29 C30 120.2(2) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C25 120.0(2) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C36 C31 C32 119.1(2) . . ? C36 C31 C5 119.5(2) . . ? C32 C31 C5 121.4(2) . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 119.8(2) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C31 C36 C35 120.5(2) . . ? C31 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? O42 C40 O43 124.9(2) . . ? O42 C40 C41 120.0(2) . . ? O43 C40 C41 115.1(2) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C51 O50 H50 109.5 . . ? O50 C51 H51A 109.5 . . ? O50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 Pd1 N1 C2 177.58(18) . . . . ? O43 Pd1 N1 C2 -140.4(5) . . . . ? C7 Pd1 N1 C2 -2.44(17) . . . . ? N13 Pd1 N1 C6 0.58(16) . . . . ? O43 Pd1 N1 C6 42.6(6) . . . . ? C7 Pd1 N1 C6 -179.44(17) . . . . ? C6 N1 C2 C3 2.4(3) . . . . ? Pd1 N1 C2 C3 -174.38(15) . . . . ? C6 N1 C2 C12 -177.95(19) . . . . ? Pd1 N1 C2 C12 5.2(2) . . . . ? N1 Pd1 O43 C40 -171.9(5) . . . . ? N13 Pd1 O43 C40 -130.4(2) . . . . ? C7 Pd1 O43 C40 51.3(2) . . . . ? N1 C2 C3 C4 -0.5(3) . . . . ? C12 C2 C3 C4 179.9(2) . . . . ? N1 C2 C3 C19 176.8(2) . . . . ? C12 C2 C3 C19 -2.7(4) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C19 C3 C4 C5 -177.8(2) . . . . ? C2 C3 C4 C25 178.5(2) . . . . ? C19 C3 C4 C25 1.0(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C25 C4 C5 C6 -179.4(2) . . . . ? C3 C4 C5 C31 175.3(2) . . . . ? C25 C4 C5 C31 -3.5(3) . . . . ? C2 N1 C6 C5 -3.4(3) . . . . ? Pd1 N1 C6 C5 173.48(16) . . . . ? C2 N1 C6 C14 178.50(19) . . . . ? Pd1 N1 C6 C14 -4.7(2) . . . . ? C4 C5 C6 N1 2.4(3) . . . . ? C31 C5 C6 N1 -173.4(2) . . . . ? C4 C5 C6 C14 -179.8(2) . . . . ? C31 C5 C6 C14 4.4(4) . . . . ? N1 Pd1 C7 C8 -176.8(2) . . . . ? N13 Pd1 C7 C8 -176.7(2) . . . . ? O43 Pd1 C7 C8 -2.4(2) . . . . ? N1 Pd1 C7 C12 -1.15(17) . . . . ? N13 Pd1 C7 C12 -1.1(4) . . . . ? O43 Pd1 C7 C12 173.30(16) . . . . ? C12 C7 C8 C9 -0.9(4) . . . . ? Pd1 C7 C8 C9 174.5(2) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C11 1.6(5) . . . . ? C9 C10 C11 C12 -1.1(5) . . . . ? C8 C7 C12 C11 1.4(4) . . . . ? Pd1 C7 C12 C11 -174.7(2) . . . . ? C8 C7 C12 C2 -179.7(2) . . . . ? Pd1 C7 C12 C2 4.2(3) . . . . ? C10 C11 C12 C7 -0.5(4) . . . . ? C10 C11 C12 C2 -179.1(3) . . . . ? N1 C2 C12 C7 -6.1(3) . . . . ? C3 C2 C12 C7 173.5(2) . . . . ? N1 C2 C12 C11 172.7(3) . . . . ? C3 C2 C12 C11 -7.8(4) . . . . ? N1 Pd1 N13 C18 179.0(2) . . . . ? O43 Pd1 N13 C18 4.3(2) . . . . ? C7 Pd1 N13 C18 178.9(2) . . . . ? N1 Pd1 N13 C14 3.92(16) . . . . ? O43 Pd1 N13 C14 -170.73(16) . . . . ? C7 Pd1 N13 C14 3.8(4) . . . . ? C18 N13 C14 C15 -4.1(3) . . . . ? Pd1 N13 C14 C15 171.33(18) . . . . ? C18 N13 C14 C6 177.1(2) . . . . ? Pd1 N13 C14 C6 -7.4(2) . . . . ? N1 C6 C14 N13 7.9(3) . . . . ? C5 C6 C14 N13 -170.0(2) . . . . ? N1 C6 C14 C15 -170.7(2) . . . . ? C5 C6 C14 C15 11.3(4) . . . . ? N13 C14 C15 C16 2.6(4) . . . . ? C6 C14 C15 C16 -178.8(2) . . . . ? C14 C15 C16 C17 1.4(4) . . . . ? C15 C16 C17 C18 -3.9(4) . . . . ? C14 N13 C18 C17 1.7(4) . . . . ? Pd1 N13 C18 C17 -173.04(18) . . . . ? C16 C17 C18 N13 2.3(4) . . . . ? C2 C3 C19 C20 -89.2(3) . . . . ? C4 C3 C19 C20 88.2(3) . . . . ? C2 C3 C19 C24 93.1(3) . . . . ? C4 C3 C19 C24 -89.5(3) . . . . ? C24 C19 C20 C21 -1.0(4) . . . . ? C3 C19 C20 C21 -178.7(2) . . . . ? C19 C20 C21 C22 -0.3(4) . . . . ? C20 C21 C22 C23 1.2(4) . . . . ? C21 C22 C23 C24 -0.8(4) . . . . ? C20 C19 C24 C23 1.4(4) . . . . ? C3 C19 C24 C23 179.1(2) . . . . ? C22 C23 C24 C19 -0.4(4) . . . . ? C3 C4 C25 C26 -87.8(3) . . . . ? C5 C4 C25 C26 91.1(3) . . . . ? C3 C4 C25 C30 90.3(3) . . . . ? C5 C4 C25 C30 -90.8(3) . . . . ? C30 C25 C26 C27 -0.8(4) . . . . ? C4 C25 C26 C27 177.3(2) . . . . ? C25 C26 C27 C28 0.9(4) . . . . ? C26 C27 C28 C29 -0.6(4) . . . . ? C27 C28 C29 C30 0.1(4) . . . . ? C28 C29 C30 C25 0.0(4) . . . . ? C26 C25 C30 C29 0.3(4) . . . . ? C4 C25 C30 C29 -177.8(2) . . . . ? C6 C5 C31 C36 84.7(3) . . . . ? C4 C5 C31 C36 -91.1(3) . . . . ? C6 C5 C31 C32 -96.0(3) . . . . ? C4 C5 C31 C32 88.2(3) . . . . ? C36 C31 C32 C33 -1.0(4) . . . . ? C5 C31 C32 C33 179.7(2) . . . . ? C31 C32 C33 C34 0.4(4) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? C33 C34 C35 C36 -1.1(5) . . . . ? C32 C31 C36 C35 0.6(4) . . . . ? C5 C31 C36 C35 179.9(2) . . . . ? C34 C35 C36 C31 0.5(4) . . . . ? Pd1 O43 C40 O42 -5.8(4) . . . . ? Pd1 O43 C40 C41 175.00(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O50 H50 O42 0.84 1.88 2.696(3) 164.1 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.171 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.095 #===END