# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Paul Pringle' _publ_contact_author_email PAUL.PRINGLE@BRIS.AC.UK _publ_section_title ; Stereoelectronic Effects in a Homologous Series of Bidentate Cyclic Phosphines. A Clear Correlation of Hydroformylation Catalyst Activity with Ring Size ; loop_ _publ_author_name 'Paul Pringle' 'Mairi F Haddow' 'Ann J. Middleton' 'A. Orpen' 'Rainer Papp' # Attachment 'all_structures.cif' data_4a_donkeysad _database_code_depnum_ccdc_archive 'CCDC 700268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H22 Cl2 P2 Pt, C H Cl3' _chemical_formula_sum 'C12 H23 Cl5 P2 Pt' _chemical_formula_weight 601.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.165(2) _cell_length_b 12.425(3) _cell_length_c 12.614(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1906.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10091 _cell_measurement_theta_min 2.301 _cell_measurement_theta_max 27.477 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 8.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_process_details 'SADABS V2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 21202 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4334 _reflns_number_gt 4162 _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^)+(0.0240P)^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 0.460(5) _refine_ls_number_reflns 4334 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0463 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.524853(9) 0.228537(9) 0.001290(13) 0.00882(4) Uani 1 1 d . . . P1 P 0.56675(11) 0.33620(9) 0.13521(8) 0.0101(2) Uani 1 1 d . . . P2 P 0.56828(11) 0.34378(9) -0.12532(8) 0.0097(2) Uani 1 1 d . . . Cl1 Cl 0.47993(12) 0.10537(8) -0.13444(7) 0.0155(2) Uani 1 1 d . . . Cl2 Cl 0.49051(11) 0.09336(8) 0.12770(8) 0.0175(3) Uani 1 1 d . . . C1 C 0.4751(4) 0.3317(4) 0.2507(3) 0.0156(10) Uani 1 1 d . . . H1A H 0.4452 0.4040 0.2666 0.019 Uiso 1 1 calc R . . H1B H 0.4131 0.2816 0.2381 0.019 Uiso 1 1 calc R . . C2 C 0.5482(4) 0.2914(4) 0.3419(3) 0.0195(10) Uani 1 1 d . . . H2A H 0.5216 0.3210 0.4100 0.023 Uiso 1 1 calc R . . H2B H 0.5449 0.2119 0.3459 0.023 Uiso 1 1 calc R . . C3 C 0.6656(4) 0.3271(4) 0.3226(3) 0.0225(11) Uani 1 1 d . . . H3A H 0.7164 0.2886 0.3708 0.027 Uiso 1 1 calc R . . H3B H 0.6731 0.4054 0.3352 0.027 Uiso 1 1 calc R . . C4 C 0.6922(4) 0.3002(4) 0.2067(3) 0.0170(10) Uani 1 1 d . . . H4A H 0.7090 0.2227 0.1983 0.020 Uiso 1 1 calc R . . H4B H 0.7555 0.3428 0.1810 0.020 Uiso 1 1 calc R . . C5 C 0.5827(4) 0.4782(3) 0.1082(3) 0.0131(10) Uani 1 1 d . . . H5A H 0.5086 0.5104 0.1013 0.016 Uiso 1 1 calc R . . H5B H 0.6187 0.5121 0.1701 0.016 Uiso 1 1 calc R . . C6 C 0.6482(3) 0.5064(3) 0.0100(3) 0.0167(8) Uani 1 1 d . . . H6A H 0.7169 0.4637 0.0094 0.020 Uiso 1 1 calc R . . H6B H 0.6687 0.5835 0.0129 0.020 Uiso 1 1 calc R . . C7 C 0.5852(4) 0.4852(3) -0.0919(3) 0.0146(10) Uani 1 1 d . . . H7A H 0.6239 0.5213 -0.1510 0.017 Uiso 1 1 calc R . . H7B H 0.5115 0.5183 -0.0857 0.017 Uiso 1 1 calc R . . C8 C 0.6940(4) 0.3085(4) -0.1957(3) 0.0171(10) Uani 1 1 d . . . H8A H 0.7582 0.3464 -0.1651 0.020 Uiso 1 1 calc R . . H8B H 0.7074 0.2300 -0.1929 0.020 Uiso 1 1 calc R . . C9 C 0.6722(4) 0.3456(4) -0.3094(3) 0.0203(11) Uani 1 1 d . . . H9A H 0.6804 0.4246 -0.3150 0.024 Uiso 1 1 calc R . . H9B H 0.7249 0.3112 -0.3588 0.024 Uiso 1 1 calc R . . C10 C 0.5552(5) 0.3123(4) -0.3363(3) 0.0281(13) Uani 1 1 d . . . H10A H 0.5512 0.2333 -0.3463 0.034 Uiso 1 1 calc R . . H10B H 0.5313 0.3475 -0.4029 0.034 Uiso 1 1 calc R . . C11 C 0.4800(4) 0.3471(4) -0.2435(3) 0.0143(9) Uani 1 1 d . . . H11A H 0.4174 0.2968 -0.2356 0.017 Uiso 1 1 calc R . . H11B H 0.4509 0.4205 -0.2555 0.017 Uiso 1 1 calc R . . C12 C 0.2223(3) 0.5029(3) 0.0323(3) 0.0179(9) Uani 1 1 d . . . H12 H 0.1424 0.4841 0.0331 0.021 Uiso 1 1 calc R . . Cl3 Cl 0.26489(9) 0.53493(9) 0.16209(8) 0.0265(2) Uani 1 1 d . . . Cl4 Cl 0.24340(12) 0.61329(10) -0.05168(10) 0.0400(3) Uani 1 1 d . . . Cl5 Cl 0.29767(8) 0.39208(8) -0.01257(9) 0.0233(2) 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 Pt1 0.00986(7) 0.00663(7) 0.00997(6) 0.00026(8) 0.00026(9) 0.00019(4) P1 0.0121(6) 0.0080(5) 0.0101(5) -0.0001(4) 0.0005(4) -0.0009(5) P2 0.0107(5) 0.0093(5) 0.0091(4) -0.0003(4) 0.0004(4) 0.0006(5) Cl1 0.0206(6) 0.0092(4) 0.0168(4) -0.0031(4) -0.0048(4) 0.0009(5) Cl2 0.0254(7) 0.0104(5) 0.0167(5) 0.0044(4) 0.0043(4) -0.0007(5) C1 0.018(2) 0.018(2) 0.0112(17) 0.0002(15) 0.0041(19) 0.003(2) C2 0.025(3) 0.023(2) 0.0099(18) 0.0004(17) 0.0010(18) 0.002(2) C3 0.029(3) 0.022(3) 0.016(2) -0.0011(19) -0.0087(19) 0.006(2) C4 0.015(2) 0.021(2) 0.0149(19) 0.0014(18) -0.0043(18) 0.005(2) C5 0.017(2) 0.009(2) 0.0132(18) -0.0004(16) 0.0009(17) 0.000(2) C6 0.0231(19) 0.0120(16) 0.0151(18) -0.0005(19) -0.0082(19) -0.0058(14) C7 0.020(3) 0.009(2) 0.0139(19) 0.0014(16) 0.0045(18) -0.002(2) C8 0.017(3) 0.013(2) 0.022(2) 0.0054(18) 0.0075(18) 0.001(2) C9 0.031(3) 0.012(2) 0.019(2) 0.0008(18) 0.0138(19) -0.004(2) C10 0.046(4) 0.025(3) 0.014(2) -0.0018(19) 0.003(2) -0.001(3) C11 0.012(2) 0.015(2) 0.0154(18) 0.0036(16) -0.0039(19) -0.004(2) C12 0.013(2) 0.0159(19) 0.025(2) 0.0009(14) 0.0000(14) -0.0008(17) Cl3 0.0240(6) 0.0299(6) 0.0257(5) -0.0094(4) 0.0004(4) 0.0036(5) Cl4 0.0465(8) 0.0267(6) 0.0468(7) 0.0188(5) -0.0095(6) -0.0078(6) Cl5 0.0186(4) 0.0207(4) 0.0308(6) -0.0100(5) 0.0049(5) -0.0007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2089(11) . ? Pt1 P1 2.2142(11) . ? Pt1 Cl2 2.3532(10) . ? Pt1 Cl1 2.3604(10) . ? P1 C5 1.807(4) . ? P1 C4 1.828(4) . ? P1 C1 1.835(4) . ? P2 C7 1.818(4) . ? P2 C8 1.821(5) . ? P2 C11 1.838(4) . ? C1 C2 1.538(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.515(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.535(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.520(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.530(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.521(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.548(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 Cl5 1.748(4) . ? C12 Cl4 1.753(4) . ? C12 Cl3 1.762(4) . ? C12 H12 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 P2 Pt1 P1 96.02(3) . . ? P2 Pt1 Cl2 174.22(4) . . ? P1 Pt1 Cl2 87.43(4) . . ? P2 Pt1 Cl1 87.20(4) . . ? P1 Pt1 Cl1 176.67(4) . . ? Cl2 Pt1 Cl1 89.29(3) . . ? C5 P1 C4 104.0(2) . . ? C5 P1 C1 104.2(2) . . ? C4 P1 C1 96.2(2) . . ? C5 P1 Pt1 118.06(13) . . ? C4 P1 Pt1 114.86(16) . . ? C1 P1 Pt1 116.54(16) . . ? C7 P2 C8 104.5(2) . . ? C7 P2 C11 103.4(2) . . ? C8 P2 C11 95.8(2) . . ? C7 P2 Pt1 119.06(14) . . ? C8 P2 Pt1 113.40(15) . . ? C11 P2 Pt1 117.47(15) . . ? C2 C1 P1 104.6(3) . . ? C2 C1 H1A 110.8 . . ? P1 C1 H1A 110.8 . . ? C2 C1 H1B 110.8 . . ? P1 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C3 C2 C1 109.3(4) . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C2 C3 C4 106.7(4) . . ? C2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 P1 103.9(3) . . ? C3 C4 H4A 111.0 . . ? P1 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? P1 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C6 C5 P1 115.9(3) . . ? C6 C5 H5A 108.3 . . ? P1 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? P1 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 112.7(3) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 P2 114.9(3) . . ? C6 C7 H7A 108.5 . . ? P2 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? P2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 P2 103.9(3) . . ? C9 C8 H8A 111.0 . . ? P2 C8 H8A 111.0 . . ? C9 C8 H8B 111.0 . . ? P2 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? C10 C9 C8 106.8(4) . . ? C10 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? C10 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C9 C10 C11 108.0(4) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 P2 105.2(3) . . ? C10 C11 H11A 110.7 . . ? P2 C11 H11A 110.7 . . ? C10 C11 H11B 110.7 . . ? P2 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? Cl5 C12 Cl4 110.1(2) . . ? Cl5 C12 Cl3 109.0(2) . . ? Cl4 C12 Cl3 110.0(2) . . ? Cl5 C12 H12 109.3 . . ? Cl4 C12 H12 109.3 . . ? Cl3 C12 H12 109.3 . . ? 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 P2 Pt1 P1 C5 15.85(19) . . . . ? Cl2 Pt1 P1 C5 -168.8(2) . . . . ? Cl1 Pt1 P1 C5 -178(13) . . . . ? P2 Pt1 P1 C4 -107.52(18) . . . . ? Cl2 Pt1 P1 C4 67.84(17) . . . . ? Cl1 Pt1 P1 C4 58.4(9) . . . . ? P2 Pt1 P1 C1 141.07(18) . . . . ? Cl2 Pt1 P1 C1 -43.58(17) . . . . ? Cl1 Pt1 P1 C1 -53.0(9) . . . . ? P1 Pt1 P2 C7 -15.5(2) . . . . ? Cl2 Pt1 P2 C7 -142.0(4) . . . . ? Cl1 Pt1 P2 C7 165.3(2) . . . . ? P1 Pt1 P2 C8 108.00(18) . . . . ? Cl2 Pt1 P2 C8 -18.5(5) . . . . ? Cl1 Pt1 P2 C8 -71.19(17) . . . . ? P1 Pt1 P2 C11 -141.59(18) . . . . ? Cl2 Pt1 P2 C11 91.9(5) . . . . ? Cl1 Pt1 P2 C11 39.22(18) . . . . ? C5 P1 C1 C2 -110.9(3) . . . . ? C4 P1 C1 C2 -4.7(4) . . . . ? Pt1 P1 C1 C2 117.1(3) . . . . ? P1 C1 C2 C3 29.8(4) . . . . ? C1 C2 C3 C4 -47.2(5) . . . . ? C2 C3 C4 P1 40.7(4) . . . . ? C5 P1 C4 C3 85.8(3) . . . . ? C1 P1 C4 C3 -20.6(4) . . . . ? Pt1 P1 C4 C3 -143.6(3) . . . . ? C4 P1 C5 C6 84.4(3) . . . . ? C1 P1 C5 C6 -175.3(3) . . . . ? Pt1 P1 C5 C6 -44.2(4) . . . . ? P1 C5 C6 C7 73.7(4) . . . . ? C5 C6 C7 P2 -72.1(4) . . . . ? C8 P2 C7 C6 -85.1(4) . . . . ? C11 P2 C7 C6 175.2(3) . . . . ? Pt1 P2 C7 C6 42.7(4) . . . . ? C7 P2 C8 C9 -83.1(3) . . . . ? C11 P2 C8 C9 22.5(4) . . . . ? Pt1 P2 C8 C9 145.8(3) . . . . ? P2 C8 C9 C10 -42.9(4) . . . . ? C8 C9 C10 C11 47.7(5) . . . . ? C9 C10 C11 P2 -29.0(5) . . . . ? C7 P2 C11 C10 109.8(3) . . . . ? C8 P2 C11 C10 3.4(4) . . . . ? Pt1 P2 C11 C10 -116.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.069 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.158 data_4b_mushs _database_code_depnum_ccdc_archive 'CCDC 700269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H26 Cl2 P2 Pt' _chemical_formula_sum 'C13 H26 Cl2 P2 Pt' _chemical_formula_weight 510.27 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.723(3) _cell_length_b 11.954(3) _cell_length_c 22.007(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3347.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 297 _cell_measurement_theta_min 2.4485 _cell_measurement_theta_max 27.483 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 8.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_process_details 'sadabs v2.03(bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 20486 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3843 _reflns_number_gt 2963 _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^)+(0.0341P)^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 3843 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Pt1 Pt 0.064687(13) 0.818741(13) 0.290617(9) 0.01731(7) Uani 1 1 d . . . P2 P 0.13235(9) 0.88057(9) 0.20344(6) 0.0165(3) Uani 1 1 d . . . Cl1 Cl -0.04269(9) 0.69746(10) 0.23213(6) 0.0264(3) Uani 1 1 d . . . P1 P 0.15975(9) 0.92761(9) 0.35131(6) 0.0175(3) Uani 1 1 d . . . Cl2 Cl -0.01071(10) 0.73963(11) 0.37963(6) 0.0328(3) Uani 1 1 d . . . C8 C 0.2316(4) 0.9898(4) 0.2056(2) 0.0205(10) Uani 1 1 d . . . H8A H 0.2742 0.9851 0.1680 0.025 Uiso 1 1 calc R . . H8B H 0.1958 1.0633 0.2055 0.025 Uiso 1 1 calc R . . C12 C 0.0754(4) 0.9455(4) 0.0863(2) 0.0276(12) Uani 1 1 d . . . H12A H 0.1329 1.0012 0.0859 0.033 Uiso 1 1 calc R . . H12B H 0.0185 0.9738 0.0597 0.033 Uiso 1 1 calc R . . C1 C 0.2391(4) 0.8429(4) 0.4028(2) 0.0227(11) Uani 1 1 d . . . H1A H 0.1974 0.7773 0.4159 0.027 Uiso 1 1 calc R . . H1B H 0.3014 0.8149 0.3806 0.027 Uiso 1 1 calc R . . C5 C 0.0764(4) 1.0109(4) 0.4012(2) 0.0216(11) Uani 1 1 d . . . H5A H 0.0480 1.0750 0.3779 0.026 Uiso 1 1 calc R . . H5B H 0.0161 0.9646 0.4145 0.026 Uiso 1 1 calc R . . C13 C 0.0334(3) 0.9346(4) 0.1509(2) 0.0203(10) Uani 1 1 d . . . H13A H -0.0280 0.8837 0.1509 0.024 Uiso 1 1 calc R . . H13B H 0.0094 1.0088 0.1653 0.024 Uiso 1 1 calc R . . C3 C 0.1851(4) 0.9608(4) 0.4940(2) 0.0298(12) Uani 1 1 d . . . H3A H 0.2115 0.9910 0.5330 0.036 Uiso 1 1 calc R . . H3B H 0.1317 0.9031 0.5032 0.036 Uiso 1 1 calc R . . C10 C 0.2142(4) 0.7929(4) 0.0945(2) 0.0300(12) Uani 1 1 d . . . H10A H 0.2407 0.7248 0.0740 0.036 Uiso 1 1 calc R . . H10B H 0.2698 0.8506 0.0920 0.036 Uiso 1 1 calc R . . C2 C 0.2762(4) 0.9069(4) 0.4594(2) 0.0273(11) Uani 1 1 d . . . H2A H 0.3137 0.8548 0.4868 0.033 Uiso 1 1 calc R . . H2B H 0.3264 0.9659 0.4469 0.033 Uiso 1 1 calc R . . C9 C 0.1938(4) 0.7657(4) 0.1617(2) 0.0238(11) Uani 1 1 d . . . H9A H 0.2614 0.7467 0.1815 0.029 Uiso 1 1 calc R . . H9B H 0.1478 0.6990 0.1642 0.029 Uiso 1 1 calc R . . C6 C 0.2534(3) 1.0258(4) 0.3184(2) 0.0199(10) Uani 1 1 d . . . H6A H 0.2165 1.0967 0.3094 0.024 Uiso 1 1 calc R . . H6B H 0.3085 1.0421 0.3489 0.024 Uiso 1 1 calc R . . C7 C 0.3061(3) 0.9849(4) 0.2607(2) 0.0211(11) Uani 1 1 d . . . H7A H 0.3300 0.9068 0.2666 0.025 Uiso 1 1 calc R . . H7B H 0.3688 1.0315 0.2524 0.025 Uiso 1 1 calc R . . C4 C 0.1339(4) 1.0554(4) 0.4575(2) 0.0270(11) Uani 1 1 d . . . H4A H 0.1886 1.1093 0.4446 0.032 Uiso 1 1 calc R . . H4B H 0.0833 1.0957 0.4837 0.032 Uiso 1 1 calc R . . C11 C 0.1164(5) 0.8351(4) 0.0605(3) 0.0346(13) Uani 1 1 d . . . H11A H 0.1341 0.8454 0.0170 0.042 Uiso 1 1 calc R . . H11B H 0.0603 0.7779 0.0631 0.042 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 Pt1 0.01559(10) 0.01712(10) 0.01920(12) 0.00126(8) 0.00031(7) -0.00349(7) P2 0.0151(6) 0.0157(5) 0.0187(7) 0.0008(5) 0.0005(5) -0.0008(4) Cl1 0.0258(6) 0.0245(6) 0.0288(7) -0.0026(5) -0.0027(5) -0.0104(5) P1 0.0167(6) 0.0183(6) 0.0175(7) 0.0016(5) -0.0011(5) -0.0018(5) Cl2 0.0347(7) 0.0368(7) 0.0269(8) 0.0059(6) 0.0062(6) -0.0151(6) C8 0.023(2) 0.020(2) 0.019(3) 0.002(2) -0.001(2) -0.0031(18) C12 0.023(3) 0.038(3) 0.022(3) 0.005(2) -0.002(2) 0.001(2) C1 0.019(2) 0.023(2) 0.027(3) 0.008(2) -0.003(2) 0.0010(19) C5 0.022(3) 0.025(2) 0.017(3) 0.002(2) 0.003(2) 0.0033(19) C13 0.015(2) 0.024(2) 0.022(3) 0.001(2) -0.0021(19) 0.0019(18) C3 0.033(3) 0.034(3) 0.022(3) -0.004(2) -0.003(2) -0.008(2) C10 0.033(3) 0.031(3) 0.026(3) -0.008(2) 0.006(2) 0.001(2) C2 0.023(3) 0.037(3) 0.022(3) 0.005(2) -0.007(2) -0.003(2) C9 0.024(3) 0.018(2) 0.029(3) -0.003(2) 0.006(2) 0.003(2) C6 0.014(2) 0.021(2) 0.025(3) 0.001(2) -0.0020(19) -0.0044(18) C7 0.015(2) 0.026(2) 0.022(3) 0.006(2) -0.001(2) -0.0019(19) C4 0.029(3) 0.027(3) 0.024(3) -0.002(2) 0.000(2) 0.001(2) C11 0.039(3) 0.042(3) 0.022(3) -0.005(3) -0.003(3) -0.005(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. ; 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 Pt1 P1 2.2228(12) . yes Pt1 P2 2.2289(13) . yes Pt1 Cl1 2.3716(13) . yes Pt1 Cl2 2.3774(13) . yes P2 C8 1.817(5) . yes P2 C13 1.827(5) . yes P2 C9 1.827(5) . yes P1 C5 1.822(5) . yes P1 C6 1.823(4) . yes P1 C1 1.825(5) . yes C8 C7 1.541(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C12 C13 1.526(7) . ? C12 C11 1.529(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C1 C2 1.535(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C5 C4 1.535(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C3 C2 1.528(7) . ? C3 C4 1.533(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C10 C9 1.536(7) . ? C10 C11 1.538(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C6 C7 1.517(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 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 P1 Pt1 P2 96.48(5) . . yes P1 Pt1 Cl1 175.92(5) . . ? P2 Pt1 Cl1 87.60(5) . . ? P1 Pt1 Cl2 87.55(5) . . ? P2 Pt1 Cl2 175.55(4) . . ? Cl1 Pt1 Cl2 88.37(5) . . ? C8 P2 C13 104.0(2) . . yes C8 P2 C9 104.8(2) . . yes C13 P2 C9 104.0(2) . . yes C8 P2 Pt1 118.99(17) . . ? C13 P2 Pt1 113.29(16) . . ? C9 P2 Pt1 110.39(16) . . ? C5 P1 C6 105.6(2) . . yes C5 P1 C1 104.5(2) . . yes C6 P1 C1 104.0(2) . . yes C5 P1 Pt1 111.41(16) . . ? C6 P1 Pt1 119.60(17) . . ? C1 P1 Pt1 110.48(16) . . ? C7 C8 P2 114.9(3) . . ? C7 C8 H8A 108.6 . . ? P2 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? P2 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? C13 C12 C11 113.1(4) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C2 C1 P1 113.4(3) . . ? C2 C1 H1A 108.9 . . ? P1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C4 C5 P1 113.5(3) . . ? C4 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C12 C13 P2 112.3(3) . . ? C12 C13 H13A 109.1 . . ? P2 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? P2 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C2 C3 C4 111.9(4) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C9 C10 C11 113.7(4) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C3 C2 C1 112.4(4) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C10 C9 P2 113.4(3) . . ? C10 C9 H9A 108.9 . . ? P2 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? P2 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C7 C6 P1 114.5(3) . . ? C7 C6 H6A 108.6 . . ? P1 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? P1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 112.0(4) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C3 C4 C5 111.7(4) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C12 C11 C10 112.2(4) . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11B 109.2 . . ? C10 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.655 _refine_diff_density_min -1.606 _refine_diff_density_rms 0.170 data_4c_ajm193sad _database_code_depnum_ccdc_archive 'CCDC 700270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H30 Cl2 P2 Pt' _chemical_formula_sum 'C15 H30 Cl2 P2 Pt' _chemical_formula_weight 538.32 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 34.324(7) _cell_length_b 6.3850(13) _cell_length_c 12.625(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.05(3) _cell_angle_gamma 90.00 _cell_volume 2765.1(10) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5098 _cell_measurement_theta_min 2.376 _cell_measurement_theta_max 27.498 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 8.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.335706 _exptl_absorpt_correction_T_max 0.620000 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick,2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28297 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12421 _reflns_number_gt 11954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.02 (Bruker, 1999)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.0361P)^2^+4.4274P] 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 -0.001(4) _refine_ls_number_reflns 12421 _refine_ls_number_parameters 625 _refine_ls_number_restraints 175 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.039 _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 Pt1 Pt 0.650905(7) 0.81590(3) 0.533472(13) 0.01782(5) Uani 1 1 d . . . Pt2 Pt 0.318036(6) 0.81625(3) 0.560025(13) 0.01667(5) Uani 1 1 d . . . Pt3 Pt -0.014473(9) 0.22875(4) 0.979454(19) 0.02510(6) Uani 1 1 d . C . P1 P 0.71026(5) 0.7386(2) 0.47933(12) 0.0192(3) Uani 1 1 d . . . P2 P 0.61762(4) 0.6130(2) 0.41809(11) 0.0171(3) Uani 1 1 d . . . P3 P 0.37662(4) 0.7363(2) 0.62983(12) 0.0179(3) Uani 1 1 d . . . P4 P 0.28348(4) 0.6161(2) 0.66675(11) 0.0182(3) Uani 1 1 d . B . P5 P 0.04467(5) 0.3009(3) 0.92156(13) 0.0242(3) Uani 1 1 d D . . P6 P -0.04564(5) 0.4619(3) 0.87517(13) 0.0251(3) Uani 1 1 d . . . Cl1 Cl 0.59023(4) 0.8769(3) 0.61222(12) 0.0263(3) Uani 1 1 d . . . Cl2 Cl 0.68158(5) 1.0535(2) 0.65649(12) 0.0296(3) Uani 1 1 d . . . Cl3 Cl 0.25837(4) 0.8823(2) 0.46500(12) 0.0268(3) Uani 1 1 d . . . Cl4 Cl 0.35040(5) 1.0555(2) 0.44715(12) 0.0279(3) Uani 1 1 d . . . Cl5 Cl -0.07403(6) 0.1388(3) 1.05611(14) 0.0370(4) Uani 1 1 d . . . Cl6 Cl 0.01514(6) -0.0596(3) 1.07270(13) 0.0350(4) Uani 1 1 d . . . C1 C 0.71543(19) 0.5599(10) 0.3667(5) 0.0278(13) Uani 1 1 d . . . H1A H 0.7159 0.6420 0.3021 0.033 Uiso 1 1 calc R . . H1B H 0.7403 0.4881 0.3748 0.033 Uiso 1 1 calc R . . C2 C 0.68307(18) 0.3960(10) 0.3545(5) 0.0243(12) Uani 1 1 d . . . H2A H 0.6910 0.2880 0.3057 0.029 Uiso 1 1 calc R . . H2B H 0.6791 0.3307 0.4226 0.029 Uiso 1 1 calc R . . C3 C 0.64494(17) 0.4932(10) 0.3133(4) 0.0214(12) Uani 1 1 d . . . H3A H 0.6290 0.3857 0.2789 0.026 Uiso 1 1 calc R . . H3B H 0.6506 0.5986 0.2606 0.026 Uiso 1 1 calc R . . C4 C 0.73837(18) 0.9659(10) 0.4400(5) 0.0265(13) Uani 1 1 d . . . H4A H 0.7264 1.0214 0.3751 0.032 Uiso 1 1 calc R . . H4B H 0.7360 1.0725 0.4942 0.032 Uiso 1 1 calc R . . C5 C 0.78190(19) 0.9319(11) 0.4219(6) 0.0343(15) Uani 1 1 d . . . H5A H 0.7852 0.7933 0.3921 0.041 Uiso 1 1 calc R . . H5B H 0.7901 1.0326 0.3697 0.041 Uiso 1 1 calc R . . C6 C 0.8086(2) 0.9519(14) 0.5198(7) 0.046(2) Uani 1 1 d . . . H6A H 0.8349 0.9164 0.5002 0.056 Uiso 1 1 calc R . . H6B H 0.8089 1.0975 0.5418 0.056 Uiso 1 1 calc R . . C7 C 0.7985(3) 0.8188(14) 0.6142(7) 0.053(2) Uani 1 1 d . . . H7A H 0.8222 0.7974 0.6569 0.063 Uiso 1 1 calc R . . H7B H 0.7808 0.8992 0.6567 0.063 Uiso 1 1 calc R . . C8A C 0.7801(2) 0.6066(14) 0.5938(7) 0.048(2) Uani 1 1 d . . . H8A H 0.7895 0.5527 0.5275 0.058 Uiso 1 1 calc R . . H8B H 0.7890 0.5119 0.6496 0.058 Uiso 1 1 calc R . . C9 C 0.73616(19) 0.6035(10) 0.5880(5) 0.0284(13) Uani 1 1 d . . . H9A H 0.7272 0.6620 0.6537 0.034 Uiso 1 1 calc R . . H9B H 0.7280 0.4580 0.5859 0.034 Uiso 1 1 calc R . . C10 C 0.58028(18) 0.7679(10) 0.3473(5) 0.0238(12) Uani 1 1 d . . . H10A H 0.5628 0.8240 0.3990 0.029 Uiso 1 1 calc R . . H10B H 0.5930 0.8859 0.3147 0.029 Uiso 1 1 calc R . . C11 C 0.55568(19) 0.6558(10) 0.2618(5) 0.0262(13) Uani 1 1 d . . . H11A H 0.5453 0.7600 0.2125 0.031 Uiso 1 1 calc R . . H11B H 0.5726 0.5648 0.2227 0.031 Uiso 1 1 calc R . . C12 C 0.52220(19) 0.5266(11) 0.3003(5) 0.0295(14) Uani 1 1 d . . . H12A H 0.5065 0.4826 0.2390 0.035 Uiso 1 1 calc R . . H12B H 0.5061 0.6165 0.3425 0.035 Uiso 1 1 calc R . . C13 C 0.5326(2) 0.3309(11) 0.3663(6) 0.0340(15) Uani 1 1 d . . . H13A H 0.5091 0.2488 0.3738 0.041 Uiso 1 1 calc R . . H13B H 0.5507 0.2466 0.3270 0.041 Uiso 1 1 calc R . . C14 C 0.55068(18) 0.3707(11) 0.4766(5) 0.0267(13) Uani 1 1 d . . . H14A H 0.5430 0.2576 0.5227 0.032 Uiso 1 1 calc R . . H14B H 0.5397 0.4990 0.5038 0.032 Uiso 1 1 calc R . . C15 C 0.59545(16) 0.3894(10) 0.4839(5) 0.0224(12) Uani 1 1 d . . . H15A H 0.6063 0.2625 0.4547 0.027 Uiso 1 1 calc R . . H15B H 0.6034 0.3941 0.5583 0.027 Uiso 1 1 calc R . . C16 C 0.38081(18) 0.5526(10) 0.7415(5) 0.0244(12) Uani 1 1 d . . . H16A H 0.4053 0.4775 0.7371 0.029 Uiso 1 1 calc R . . H16B H 0.3819 0.6325 0.8068 0.029 Uiso 1 1 calc R . . C17 C 0.34778(18) 0.3924(9) 0.7474(5) 0.0247(12) Uani 1 1 d . . . H17A H 0.3441 0.3242 0.6791 0.030 Uiso 1 1 calc R . . H17B H 0.3550 0.2860 0.7993 0.030 Uiso 1 1 calc R . . C18 C 0.30955(17) 0.4954(10) 0.7779(5) 0.0234(12) Uani 1 1 d . . . H18A H 0.3151 0.6010 0.8316 0.028 Uiso 1 1 calc R . . H18B H 0.2930 0.3903 0.8088 0.028 Uiso 1 1 calc R . . C19 C 0.40390(18) 0.6078(10) 0.5264(5) 0.0247(12) Uani 1 1 d . . . H19A H 0.3959 0.4621 0.5235 0.030 Uiso 1 1 calc R . . H19B H 0.3960 0.6707 0.4590 0.030 Uiso 1 1 calc R . . C20 C 0.44841(19) 0.6138(11) 0.5357(6) 0.0320(14) Uani 1 1 d . . . H20A H 0.4589 0.5265 0.4807 0.038 Uiso 1 1 calc R . . H20B H 0.4569 0.5554 0.6036 0.038 Uiso 1 1 calc R . . C21 C 0.4650(2) 0.8370(12) 0.5260(6) 0.0369(16) Uani 1 1 d . . . H21A H 0.4882 0.8299 0.4843 0.044 Uiso 1 1 calc R . . H21B H 0.4460 0.9218 0.4868 0.044 Uiso 1 1 calc R . . C22 C 0.4756(2) 0.9488(12) 0.6295(6) 0.0379(16) Uani 1 1 d . . . H22A H 0.5006 0.8958 0.6560 0.046 Uiso 1 1 calc R . . H22B H 0.4790 1.0966 0.6145 0.046 Uiso 1 1 calc R . . C23 C 0.44651(19) 0.9274(11) 0.7169(5) 0.0320(14) Uani 1 1 d . . . H23A H 0.4533 1.0273 0.7724 0.038 Uiso 1 1 calc R . . H23B H 0.4490 0.7883 0.7473 0.038 Uiso 1 1 calc R . . C24 C 0.40358(17) 0.9626(10) 0.6807(5) 0.0241(12) Uani 1 1 d . . . H24A H 0.4030 1.0694 0.6261 0.029 Uiso 1 1 calc R . . H24B H 0.3898 1.0182 0.7404 0.029 Uiso 1 1 calc R . . C25 C 0.26113(18) 0.3943(11) 0.5969(5) 0.0289(13) Uani 1 1 d DU . . H25A H 0.2687 0.4032 0.5237 0.035 Uiso 1 1 calc R A 1 H25B H 0.2731 0.2685 0.6262 0.035 Uiso 1 1 calc R A 1 C26A C 0.2184(3) 0.3612(19) 0.5951(9) 0.028(2) Uani 0.657(13) 1 d PDU B 1 H26A H 0.2125 0.2408 0.5506 0.034 Uiso 0.657(13) 1 calc PR B 1 H26B H 0.2061 0.4820 0.5616 0.034 Uiso 0.657(13) 1 calc PR B 1 C27A C 0.1999(4) 0.3266(17) 0.7017(9) 0.042(3) Uani 0.657(13) 1 d PD B 1 H27A H 0.2183 0.2501 0.7473 0.050 Uiso 0.657(13) 1 calc PR B 1 H27B H 0.1771 0.2384 0.6904 0.050 Uiso 0.657(13) 1 calc PR B 1 C28A C 0.1874(4) 0.526(2) 0.7608(11) 0.032(3) Uani 0.657(13) 1 d PD B 1 H28A H 0.1715 0.6103 0.7124 0.038 Uiso 0.657(13) 1 calc PR B 1 H28B H 0.1712 0.4843 0.8185 0.038 Uiso 0.657(13) 1 calc PR B 1 C26B C 0.2211(4) 0.320(3) 0.6401(18) 0.027(3) Uani 0.343(13) 1 d PDU B 2 H26C H 0.2127 0.1987 0.5993 0.032 Uiso 0.343(13) 1 calc PR B 2 H26D H 0.2257 0.2744 0.7126 0.032 Uiso 0.343(13) 1 calc PR B 2 C27B C 0.1871(5) 0.476(3) 0.6390(13) 0.026(3) Uani 0.343(13) 1 d PDU B 2 H27C H 0.1632 0.3994 0.6234 0.032 Uiso 0.343(13) 1 calc PR B 2 H27D H 0.1906 0.5744 0.5816 0.032 Uiso 0.343(13) 1 calc PR B 2 C28B C 0.1821(6) 0.602(3) 0.7420(17) 0.028(6) Uani 0.343(13) 1 d PD B 2 H28C H 0.1658 0.5207 0.7881 0.033 Uiso 0.343(13) 1 calc PR B 2 H28D H 0.1682 0.7298 0.7242 0.033 Uiso 0.343(13) 1 calc PR B 2 C29 C 0.2200(2) 0.6606(11) 0.8054(5) 0.0324(15) Uani 1 1 d D . . H29A H 0.2366 0.5728 0.8508 0.039 Uiso 1 1 calc R B 1 H29B H 0.2086 0.7654 0.8504 0.039 Uiso 1 1 calc R B 1 C30 C 0.24639(18) 0.7747(10) 0.7287(5) 0.0243(13) Uani 1 1 d . B . H30A H 0.2594 0.8882 0.7669 0.029 Uiso 1 1 calc R . . H30B H 0.2300 0.8370 0.6730 0.029 Uiso 1 1 calc R . . C31 C 0.05143(19) 0.5444(10) 0.8509(6) 0.0334(15) Uani 1 1 d . C . H31A H 0.0528 0.6572 0.9024 0.040 Uiso 1 1 calc R . . H31B H 0.0764 0.5385 0.8174 0.040 Uiso 1 1 calc R . . C32 C 0.0203(2) 0.6006(11) 0.7663(5) 0.0343(16) Uani 1 1 d . . . H32A H 0.0151 0.4799 0.7213 0.041 Uiso 1 1 calc R C . H32B H 0.0298 0.7128 0.7223 0.041 Uiso 1 1 calc R . . C33 C -0.0175(2) 0.6695(10) 0.8166(5) 0.0290(14) Uani 1 1 d . C . H33A H -0.0337 0.7385 0.7628 0.035 Uiso 1 1 calc R . . H33B H -0.0110 0.7721 0.8711 0.035 Uiso 1 1 calc R . . C40 C -0.0844(2) 0.6057(11) 0.9384(5) 0.0333(15) Uani 1 1 d . C . H40A H -0.0948 0.5178 0.9933 0.040 Uiso 1 1 calc R . . H40B H -0.0731 0.7283 0.9728 0.040 Uiso 1 1 calc R . . C41 C -0.1186(2) 0.6778(11) 0.8636(7) 0.0400(18) Uani 1 1 d . . . H41A H -0.1308 0.7996 0.8945 0.048 Uiso 1 1 calc R C . H41B H -0.1083 0.7203 0.7965 0.048 Uiso 1 1 calc R . . C42 C -0.1494(2) 0.5128(13) 0.8430(6) 0.0420(18) Uani 1 1 d . C . H42A H -0.1739 0.5827 0.8262 0.050 Uiso 1 1 calc R . . H42B H -0.1526 0.4346 0.9080 0.050 Uiso 1 1 calc R . . C43 C -0.1415(2) 0.3566(13) 0.7541(7) 0.0434(18) Uani 1 1 d . . . H43A H -0.1392 0.4345 0.6886 0.052 Uiso 1 1 calc R C . H43B H -0.1641 0.2658 0.7452 0.052 Uiso 1 1 calc R . . C44 C -0.1051(2) 0.2183(11) 0.7697(6) 0.0364(16) Uani 1 1 d . C . H44A H -0.1055 0.1564 0.8399 0.044 Uiso 1 1 calc R . . H44B H -0.1068 0.1048 0.7187 0.044 Uiso 1 1 calc R . . C45 C -0.0664(2) 0.3280(11) 0.7584(5) 0.0328(15) Uani 1 1 d . C . H45A H -0.0695 0.4301 0.7018 0.039 Uiso 1 1 calc R . . H45B H -0.0477 0.2250 0.7360 0.039 Uiso 1 1 calc R . . C34A C 0.0765(4) 0.356(3) 1.0360(12) 0.028(3) Uani 0.571(10) 1 d PU C 3 H34A H 0.0675 0.4820 1.0702 0.034 Uiso 0.571(10) 1 calc PR C 3 H34B H 0.0746 0.2414 1.0863 0.034 Uiso 0.571(10) 1 calc PR C 3 C35A C 0.1195(3) 0.384(2) 1.0084(10) 0.030(2) Uani 0.571(10) 1 d PU C 3 H35A H 0.1205 0.4549 0.9406 0.037 Uiso 0.571(10) 1 calc PR C 3 H35B H 0.1320 0.4743 1.0612 0.037 Uiso 0.571(10) 1 calc PR C 3 C36A C 0.1428(4) 0.182(2) 1.0024(11) 0.037(3) Uani 0.571(10) 1 d PU C 3 H36A H 0.1678 0.2154 0.9727 0.045 Uiso 0.571(10) 1 calc PR C 3 H36B H 0.1480 0.1330 1.0742 0.045 Uiso 0.571(10) 1 calc PR C 3 C37A C 0.1249(4) 0.004(2) 0.9390(11) 0.037(3) Uani 0.571(10) 1 d PU C 3 H37A H 0.1063 -0.0672 0.9827 0.044 Uiso 0.571(10) 1 calc PR C 3 H37B H 0.1453 -0.0959 0.9239 0.044 Uiso 0.571(10) 1 calc PR C 3 C38A C 0.1036(3) 0.066(2) 0.8316(10) 0.031(2) Uani 0.571(10) 1 d PDU C 3 H38A H 0.1145 0.1970 0.8068 0.037 Uiso 0.571(10) 1 calc PR C 3 H38B H 0.1085 -0.0404 0.7791 0.037 Uiso 0.571(10) 1 calc PR C 3 C39A C 0.0598(6) 0.092(4) 0.8413(15) 0.026(4) Uani 0.571(10) 1 d PDU C 3 H39A H 0.0495 -0.0372 0.8695 0.031 Uiso 0.571(10) 1 calc PR C 3 H39B H 0.0482 0.1108 0.7708 0.031 Uiso 0.571(10) 1 calc PR C 3 C34B C 0.0864(5) 0.291(3) 1.0213(15) 0.028(4) Uani 0.429(10) 1 d PDU C 4 H34C H 0.1013 0.4195 1.0142 0.034 Uiso 0.429(10) 1 calc PR C 4 H34D H 0.0756 0.2933 1.0912 0.034 Uiso 0.429(10) 1 calc PR C 4 C35B C 0.1167(5) 0.098(3) 1.0180(14) 0.038(3) Uani 0.429(10) 1 d PU C 4 H35C H 0.1307 0.0902 1.0859 0.046 Uiso 0.429(10) 1 calc PR C 4 H35D H 0.1020 -0.0305 1.0088 0.046 Uiso 0.429(10) 1 calc PR C 4 C36B C 0.1461(5) 0.112(3) 0.9313(16) 0.042(4) Uani 0.429(10) 1 d PU C 4 H36C H 0.1525 0.2581 0.9203 0.050 Uiso 0.429(10) 1 calc PR C 4 H36D H 0.1698 0.0409 0.9553 0.050 Uiso 0.429(10) 1 calc PR C 4 C37B C 0.1325(5) 0.019(3) 0.8268(14) 0.038(3) Uani 0.429(10) 1 d PU C 4 H37C H 0.1244 -0.1242 0.8393 0.046 Uiso 0.429(10) 1 calc PR C 4 H37D H 0.1546 0.0135 0.7812 0.046 Uiso 0.429(10) 1 calc PR C 4 C38B C 0.0996(4) 0.130(2) 0.7679(13) 0.025(3) Uani 0.429(10) 1 d PU C 4 H38C H 0.0973 0.0728 0.6969 0.030 Uiso 0.429(10) 1 calc PR C 4 H38D H 0.1067 0.2768 0.7614 0.030 Uiso 0.429(10) 1 calc PR C 4 C39B C 0.0595(9) 0.118(4) 0.8176(19) 0.024(5) Uani 0.429(10) 1 d PDU C 4 H39C H 0.0571 -0.0220 0.8464 0.029 Uiso 0.429(10) 1 calc PR C 4 H39D H 0.0402 0.1296 0.7599 0.029 Uiso 0.429(10) 1 calc PR C 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02126(11) 0.01751(11) 0.01475(12) -0.00144(8) 0.00131(8) 0.00303(9) Pt2 0.01784(11) 0.01679(11) 0.01535(11) 0.00163(8) 0.00006(8) 0.00218(8) Pt3 0.03520(13) 0.02276(10) 0.01748(10) 0.00078(10) 0.00308(9) -0.00849(10) P1 0.0202(7) 0.0192(7) 0.0183(7) 0.0015(6) -0.0001(6) 0.0033(6) P2 0.0183(7) 0.0172(7) 0.0157(6) 0.0005(5) 0.0008(5) 0.0011(5) P3 0.0183(7) 0.0193(7) 0.0163(7) 0.0002(6) 0.0018(5) 0.0026(6) P4 0.0190(7) 0.0186(7) 0.0173(6) -0.0015(5) 0.0019(5) -0.0002(6) P5 0.0306(9) 0.0223(8) 0.0197(7) 0.0016(6) -0.0029(6) -0.0082(6) P6 0.0313(9) 0.0237(8) 0.0205(7) -0.0026(6) 0.0040(6) -0.0026(7) Cl1 0.0269(7) 0.0291(7) 0.0234(7) -0.0024(6) 0.0070(6) 0.0055(6) Cl2 0.0324(8) 0.0290(8) 0.0269(7) -0.0110(6) -0.0026(6) 0.0016(6) Cl3 0.0247(7) 0.0310(8) 0.0242(7) 0.0006(6) -0.0066(6) 0.0069(6) Cl4 0.0326(8) 0.0264(7) 0.0250(7) 0.0086(6) 0.0042(6) -0.0005(6) Cl5 0.0436(10) 0.0360(9) 0.0321(8) 0.0029(7) 0.0129(7) -0.0108(8) Cl6 0.0508(10) 0.0294(8) 0.0247(7) 0.0067(6) -0.0013(7) -0.0067(7) C1 0.029(3) 0.033(3) 0.022(3) -0.005(3) 0.006(2) 0.008(3) C2 0.028(3) 0.024(3) 0.021(3) -0.004(2) 0.004(2) 0.005(2) C3 0.022(3) 0.025(3) 0.017(3) -0.004(2) 0.000(2) 0.002(2) C4 0.023(3) 0.025(3) 0.032(3) 0.002(3) 0.003(2) 0.003(2) C5 0.023(3) 0.035(4) 0.045(4) 0.007(3) 0.008(3) -0.004(3) C6 0.025(4) 0.047(5) 0.067(5) 0.006(4) -0.002(3) -0.005(3) C7 0.057(6) 0.061(6) 0.039(4) 0.004(4) -0.017(4) -0.016(4) C8A 0.037(4) 0.052(5) 0.055(5) 0.007(4) -0.007(4) 0.008(4) C9 0.036(4) 0.028(3) 0.021(3) 0.005(2) -0.007(3) 0.006(3) C10 0.023(3) 0.024(3) 0.024(3) 0.003(2) -0.002(2) 0.005(2) C11 0.027(3) 0.032(3) 0.019(3) 0.006(2) -0.004(2) 0.003(3) C12 0.025(3) 0.042(4) 0.021(3) 0.001(3) -0.003(2) -0.005(3) C13 0.035(4) 0.035(4) 0.031(3) 0.001(3) -0.007(3) -0.006(3) C14 0.021(3) 0.036(3) 0.024(3) 0.007(3) 0.002(2) -0.005(3) C15 0.016(3) 0.026(3) 0.025(3) 0.009(2) 0.001(2) 0.002(2) C16 0.025(3) 0.028(3) 0.020(3) 0.002(2) -0.004(2) 0.003(2) C17 0.027(3) 0.022(3) 0.026(3) 0.005(2) 0.006(2) 0.004(2) C18 0.021(3) 0.025(3) 0.024(3) 0.005(2) 0.000(2) 0.004(2) C19 0.029(3) 0.023(3) 0.022(3) -0.004(2) 0.002(2) 0.007(2) C20 0.025(3) 0.039(4) 0.032(3) -0.004(3) 0.006(3) 0.005(3) C21 0.023(3) 0.047(4) 0.041(4) -0.001(3) 0.012(3) -0.004(3) C22 0.028(4) 0.035(4) 0.050(4) 0.001(3) 0.001(3) 0.000(3) C23 0.030(3) 0.033(4) 0.033(3) -0.005(3) -0.006(3) -0.005(3) C24 0.024(3) 0.024(3) 0.025(3) -0.006(2) -0.001(2) 0.007(2) C25 0.030(3) 0.030(3) 0.026(3) -0.006(3) 0.004(2) -0.006(3) C26A 0.021(4) 0.033(4) 0.030(5) -0.006(4) -0.008(4) -0.002(3) C27A 0.043(7) 0.038(6) 0.045(7) -0.007(5) 0.008(6) -0.016(5) C28A 0.031(6) 0.027(7) 0.037(7) -0.001(6) 0.011(5) -0.003(6) C26B 0.023(5) 0.030(6) 0.026(6) -0.005(6) -0.005(6) -0.002(5) C27B 0.015(6) 0.036(7) 0.028(6) -0.003(6) -0.007(5) -0.004(5) C28B 0.027(11) 0.013(11) 0.044(13) 0.008(10) 0.005(9) 0.000(9) C29 0.032(4) 0.038(4) 0.028(3) -0.007(3) 0.013(3) 0.001(3) C30 0.021(3) 0.026(3) 0.027(3) -0.005(2) 0.002(2) 0.002(2) C31 0.026(3) 0.025(3) 0.050(4) 0.004(3) 0.011(3) -0.001(3) C32 0.051(4) 0.028(3) 0.024(3) 0.010(3) 0.013(3) 0.000(3) C33 0.038(4) 0.024(3) 0.025(3) 0.006(2) 0.008(3) -0.002(3) C40 0.035(4) 0.034(4) 0.031(3) -0.004(3) 0.007(3) -0.007(3) C41 0.046(5) 0.033(4) 0.042(4) -0.003(3) 0.010(4) 0.006(3) C42 0.033(4) 0.053(5) 0.040(4) 0.013(4) 0.007(3) 0.007(3) C43 0.041(4) 0.047(4) 0.043(4) 0.002(4) 0.004(3) -0.007(4) C44 0.046(4) 0.030(3) 0.033(4) -0.004(3) -0.005(3) -0.006(3) C45 0.038(4) 0.036(4) 0.024(3) -0.007(3) 0.000(3) 0.005(3) C34A 0.025(7) 0.037(8) 0.023(6) -0.011(5) -0.001(5) -0.005(5) C35A 0.021(5) 0.040(6) 0.031(5) 0.004(5) -0.004(4) -0.001(4) C36A 0.023(6) 0.053(7) 0.036(6) 0.009(5) -0.001(5) 0.005(5) C37A 0.025(5) 0.044(6) 0.042(6) 0.002(5) 0.000(5) 0.006(5) C38A 0.021(5) 0.041(6) 0.032(5) -0.001(5) 0.009(4) 0.002(4) C39A 0.028(6) 0.024(7) 0.026(8) 0.004(6) 0.000(6) 0.001(5) C34B 0.025(8) 0.038(9) 0.020(7) -0.015(6) -0.007(6) -0.001(7) C35B 0.036(7) 0.045(7) 0.033(7) 0.007(6) -0.009(6) 0.006(6) C36B 0.025(7) 0.053(8) 0.047(8) 0.000(7) 0.000(6) 0.007(6) C37B 0.031(7) 0.038(7) 0.047(7) -0.005(6) 0.001(6) 0.008(6) C38B 0.017(6) 0.030(6) 0.028(6) -0.004(6) -0.002(5) 0.001(5) C39B 0.029(7) 0.020(8) 0.025(10) 0.000(8) 0.009(7) -0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2275(17) . yes Pt1 P2 2.2330(15) . yes Pt1 Cl1 2.3719(16) . yes Pt1 Cl2 2.3884(16) . yes Pt2 P3 2.2258(16) . yes Pt2 P4 2.2293(15) . yes Pt2 Cl3 2.3740(16) . yes Pt2 Cl4 2.3898(15) . yes Pt3 P5 2.2303(18) . yes Pt3 P6 2.2347(18) . yes Pt3 Cl5 2.3636(18) . yes Pt3 Cl6 2.3921(18) . yes P1 C4 1.821(6) . yes P1 C9 1.825(6) . yes P1 C1 1.837(6) . yes P2 C3 1.818(6) . yes P2 C10 1.827(6) . yes P2 C15 1.831(6) . yes P3 C24 1.821(6) . yes P3 C19 1.829(6) . yes P3 C16 1.835(6) . yes P4 C18 1.810(6) . yes P4 C25 1.823(6) . yes P4 C30 1.825(6) . yes P5 C39A 1.765(19) . yes P5 C31 1.811(7) . yes P5 C34A 1.813(15) . yes P5 C39B 1.842(18) . yes P5 C34B 1.875(15) . yes P6 C33 1.814(6) . yes P6 C40 1.823(7) . yes P6 C45 1.827(7) . yes C1 C2 1.529(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.523(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.535(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.518(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.514(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8A 1.512(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8A C9 1.508(10) . ? C8A H8A 0.9700 . ? C8A H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.525(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.509(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.537(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.525(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.541(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.530(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.529(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.529(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.542(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.522(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.521(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.543(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26A 1.480(10) . ? C25 C26B 1.569(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26A C27A 1.525(13) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C27A C28A 1.543(13) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29 1.505(12) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C26B C27B 1.531(16) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B C28B 1.543(17) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29 1.550(17) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29 C30 1.533(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.527(10) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.528(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C40 C41 1.551(11) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.508(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.533(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.537(11) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.513(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C34A C35A 1.541(18) . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C35A C36A 1.519(18) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C36A C37A 1.51(2) . ? C36A H36A 0.9700 . ? C36A H36B 0.9700 . ? C37A C38A 1.568(18) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C38A C39A 1.521(18) . ? C38A H38A 0.9700 . ? C38A H38B 0.9700 . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C34B C35B 1.61(2) . ? C34B H34C 0.9700 . ? C34B H34D 0.9700 . ? C35B C36B 1.52(3) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36B C37B 1.50(3) . ? C36B H36C 0.9700 . ? C36B H36D 0.9700 . ? C37B C38B 1.51(2) . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38B C39B 1.54(3) . ? C38B H38C 0.9700 . ? C38B H38D 0.9700 . ? C39B H39C 0.9700 . ? C39B H39D 0.9700 . ? 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 P1 Pt1 P2 97.09(6) . . yes P1 Pt1 Cl1 172.54(6) . . ? P2 Pt1 Cl1 86.12(6) . . ? P1 Pt1 Cl2 87.34(6) . . ? P2 Pt1 Cl2 174.87(5) . . ? Cl1 Pt1 Cl2 89.79(6) . . ? P3 Pt2 P4 97.00(6) . . yes P3 Pt2 Cl3 172.61(6) . . ? P4 Pt2 Cl3 86.52(6) . . ? P3 Pt2 Cl4 87.14(6) . . ? P4 Pt2 Cl4 174.57(5) . . ? Cl3 Pt2 Cl4 89.77(6) . . ? P5 Pt3 P6 95.24(6) . . yes P5 Pt3 Cl5 174.33(6) . . ? P6 Pt3 Cl5 90.02(7) . . ? P5 Pt3 Cl6 86.83(6) . . ? P6 Pt3 Cl6 171.38(6) . . ? Cl5 Pt3 Cl6 88.27(7) . . ? C4 P1 C9 109.5(3) . . yes C4 P1 C1 102.6(3) . . yes C9 P1 C1 103.3(3) . . yes C4 P1 Pt1 114.0(2) . . ? C9 P1 Pt1 107.5(2) . . ? C1 P1 Pt1 119.3(2) . . ? C3 P2 C10 104.1(3) . . yes C3 P2 C15 103.6(3) . . yes C10 P2 C15 110.4(3) . . yes C3 P2 Pt1 117.0(2) . . ? C10 P2 Pt1 109.8(2) . . ? C15 P2 Pt1 111.6(2) . . ? C24 P3 C19 110.0(3) . . yes C24 P3 C16 102.2(3) . . yes C19 P3 C16 103.5(3) . . yes C24 P3 Pt2 113.5(2) . . ? C19 P3 Pt2 107.4(2) . . ? C16 P3 Pt2 119.7(2) . . ? C18 P4 C25 103.4(3) . . yes C18 P4 C30 103.7(3) . . yes C25 P4 C30 110.5(3) . . yes C18 P4 Pt2 117.0(2) . . ? C25 P4 Pt2 112.1(2) . . ? C30 P4 Pt2 109.6(2) . . ? C39A P5 C31 108.7(8) . . yes C39A P5 C34A 114.9(8) . . yes C31 P5 C34A 98.2(6) . . yes C31 P5 C39B 98.6(10) . . yes C31 P5 C34B 104.5(8) . . yes C39B P5 C34B 103.5(11) . . yes C39A P5 Pt3 108.8(8) . . ? C31 P5 Pt3 118.2(2) . . ? C34A P5 Pt3 107.9(5) . . ? C39B P5 Pt3 112.4(10) . . ? C34B P5 Pt3 117.1(7) . . ? C33 P6 C40 102.6(3) . . yes C33 P6 C45 102.2(3) . . yes C40 P6 C45 108.6(3) . . yes C33 P6 Pt3 118.4(2) . . ? C40 P6 Pt3 114.8(2) . . ? C45 P6 Pt3 109.2(2) . . ? C2 C1 P1 114.4(4) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 111.6(5) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 P2 112.5(4) . . ? C2 C3 H3A 109.1 . . ? P2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? P2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 P1 117.1(4) . . ? C5 C4 H4A 108.0 . . ? P1 C4 H4A 108.0 . . ? C5 C4 H4B 108.0 . . ? P1 C4 H4B 108.0 . . ? H4A C4 H4B 107.3 . . ? C6 C5 C4 115.5(6) . . ? C6 C5 H5A 108.4 . . ? C4 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C4 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 116.4(6) . . ? C7 C6 H6A 108.2 . . ? C5 C6 H6A 108.2 . . ? C7 C6 H6B 108.2 . . ? C5 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C8A C7 C6 118.3(7) . . ? C8A C7 H7A 107.7 . . ? C6 C7 H7A 107.7 . . ? C8A C7 H7B 107.7 . . ? C6 C7 H7B 107.7 . . ? H7A C7 H7B 107.1 . . ? C9 C8A C7 115.5(7) . . ? C9 C8A H8A 108.4 . . ? C7 C8A H8A 108.4 . . ? C9 C8A H8B 108.4 . . ? C7 C8A H8B 108.4 . . ? H8A C8A H8B 107.5 . . ? C8A C9 P1 119.3(5) . . ? C8A C9 H9A 107.5 . . ? P1 C9 H9A 107.5 . . ? C8A C9 H9B 107.5 . . ? P1 C9 H9B 107.5 . . ? H9A C9 H9B 107.0 . . ? C11 C10 P2 117.0(4) . . ? C11 C10 H10A 108.1 . . ? P2 C10 H10A 108.1 . . ? C11 C10 H10B 108.1 . . ? P2 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C12 C11 C10 115.9(5) . . ? C12 C11 H11A 108.3 . . ? C10 C11 H11A 108.3 . . ? C12 C11 H11B 108.3 . . ? C10 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C11 C12 C13 117.0(6) . . ? C11 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? C11 C12 H12B 108.0 . . ? C13 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C12 116.0(6) . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 116.1(5) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 P2 117.6(4) . . ? C14 C15 H15A 107.9 . . ? P2 C15 H15A 107.9 . . ? C14 C15 H15B 107.9 . . ? P2 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? C17 C16 P3 115.3(4) . . ? C17 C16 H16A 108.5 . . ? P3 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? P3 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C16 111.6(5) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 P4 113.1(4) . . ? C17 C18 H18A 109.0 . . ? P4 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? P4 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C20 C19 P3 118.0(4) . . ? C20 C19 H19A 107.8 . . ? P3 C19 H19A 107.8 . . ? C20 C19 H19B 107.8 . . ? P3 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? C19 C20 C21 112.8(6) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 116.3(6) . . ? C22 C21 H21A 108.2 . . ? C20 C21 H21A 108.2 . . ? C22 C21 H21B 108.2 . . ? C20 C21 H21B 108.2 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C21 115.9(6) . . ? C23 C22 H22A 108.3 . . ? C21 C22 H22A 108.3 . . ? C23 C22 H22B 108.3 . . ? C21 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 C24 114.7(6) . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23B 108.6 . . ? C24 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C23 C24 P3 117.2(4) . . ? C23 C24 H24A 108.0 . . ? P3 C24 H24A 108.0 . . ? C23 C24 H24B 108.0 . . ? P3 C24 H24B 108.0 . . ? H24A C24 H24B 107.2 . . ? C26A C25 P4 121.2(6) . . ? C26B C25 P4 115.1(9) . . ? C26A C25 H25A 107.0 . . ? C26B C25 H25A 128.0 . . ? P4 C25 H25A 107.0 . . ? C26A C25 H25B 107.0 . . ? C26B C25 H25B 89.0 . . ? P4 C25 H25B 107.0 . . ? H25A C25 H25B 106.8 . . ? C25 C26A C27A 116.9(9) . . ? C25 C26A H26A 108.1 . . ? C27A C26A H26A 108.1 . . ? C25 C26A H26B 108.1 . . ? C27A C26A H26B 108.1 . . ? H26A C26A H26B 107.3 . . ? C26A C27A C28A 116.0(10) . . ? C26A C27A H27A 108.3 . . ? C28A C27A H27A 108.3 . . ? C26A C27A H27B 108.3 . . ? C28A C27A H27B 108.3 . . ? H27A C27A H27B 107.4 . . ? C29 C28A C27A 115.9(10) . . ? C29 C28A H28A 108.3 . . ? C27A C28A H28A 108.3 . . ? C29 C28A H28B 108.3 . . ? C27A C28A H28B 108.3 . . ? H28A C28A H28B 107.4 . . ? C27B C26B C25 118.6(14) . . ? C27B C26B H26C 107.7 . . ? C25 C26B H26C 107.7 . . ? C27B C26B H26D 107.7 . . ? C25 C26B H26D 107.7 . . ? H26C C26B H26D 107.1 . . ? C26B C27B C28B 116.0(15) . . ? C26B C27B H27C 108.3 . . ? C28B C27B H27C 108.3 . . ? C26B C27B H27D 108.3 . . ? C28B C27B H27D 108.3 . . ? H27C C27B H27D 107.4 . . ? C27B C28B C29 116.3(15) . . ? C27B C28B H28C 108.2 . . ? C29 C28B H28C 108.2 . . ? C27B C28B H28D 108.2 . . ? C29 C28B H28D 108.2 . . ? H28C C28B H28D 107.4 . . ? C28A C29 C30 118.9(7) . . ? C30 C29 C28B 107.1(10) . . ? C28A C29 H29A 107.6 . . ? C30 C29 H29A 107.6 . . ? C28B C29 H29A 128.8 . . ? C28A C29 H29B 107.6 . . ? C30 C29 H29B 107.6 . . ? C28B C29 H29B 96.9 . . ? H29A C29 H29B 107.0 . . ? C29 C30 P4 116.3(5) . . ? C29 C30 H30A 108.2 . . ? P4 C30 H30A 108.2 . . ? C29 C30 H30B 108.2 . . ? P4 C30 H30B 108.2 . . ? H30A C30 H30B 107.4 . . ? C32 C31 P5 116.6(5) . . ? C32 C31 H31A 108.2 . . ? P5 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? P5 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? C31 C32 C33 111.1(5) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C32 C33 P6 115.6(4) . . ? C32 C33 H33A 108.4 . . ? P6 C33 H33A 108.4 . . ? C32 C33 H33B 108.4 . . ? P6 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? C41 C40 P6 115.6(5) . . ? C41 C40 H40A 108.4 . . ? P6 C40 H40A 108.4 . . ? C41 C40 H40B 108.4 . . ? P6 C40 H40B 108.4 . . ? H40A C40 H40B 107.4 . . ? C42 C41 C40 114.1(6) . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 116.1(6) . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C42 C43 C44 116.3(7) . . ? C42 C43 H43A 108.2 . . ? C44 C43 H43A 108.2 . . ? C42 C43 H43B 108.2 . . ? C44 C43 H43B 108.2 . . ? H43A C43 H43B 107.4 . . ? C45 C44 C43 115.7(6) . . ? C45 C44 H44A 108.3 . . ? C43 C44 H44A 108.3 . . ? C45 C44 H44B 108.3 . . ? C43 C44 H44B 108.3 . . ? H44A C44 H44B 107.4 . . ? C44 C45 P6 117.3(5) . . ? C44 C45 H45A 108.0 . . ? P6 C45 H45A 108.0 . . ? C44 C45 H45B 108.0 . . ? P6 C45 H45B 108.0 . . ? H45A C45 H45B 107.2 . . ? C35A C34A P5 113.4(10) . . ? C35A C34A H34A 108.9 . . ? P5 C34A H34A 108.9 . . ? C35A C34A H34B 108.9 . . ? P5 C34A H34B 108.9 . . ? H34A C34A H34B 107.7 . . ? C36A C35A C34A 115.0(11) . . ? C36A C35A H35A 108.5 . . ? C34A C35A H35A 108.5 . . ? C36A C35A H35B 108.5 . . ? C34A C35A H35B 108.5 . . ? H35A C35A H35B 107.5 . . ? C37A C36A C35A 117.4(11) . . ? C37A C36A H36A 107.9 . . ? C35A C36A H36A 107.9 . . ? C37A C36A H36B 107.9 . . ? C35A C36A H36B 107.9 . . ? H36A C36A H36B 107.2 . . ? C36A C37A C38A 115.7(11) . . ? C36A C37A H37A 108.4 . . ? C38A C37A H37A 108.4 . . ? C36A C37A H37B 108.4 . . ? C38A C37A H37B 108.4 . . ? H37A C37A H37B 107.4 . . ? C39A C38A C37A 112.9(12) . . ? C39A C38A H38A 109.0 . . ? C37A C38A H38A 109.0 . . ? C39A C38A H38B 109.0 . . ? C37A C38A H38B 109.0 . . ? H38A C38A H38B 107.8 . . ? C38A C39A P5 116.1(15) . . ? C38A C39A H39A 108.3 . . ? P5 C39A H39A 108.3 . . ? C38A C39A H39B 108.3 . . ? P5 C39A H39B 108.3 . . ? H39A C39A H39B 107.4 . . ? C35B C34B P5 119.0(12) . . ? C35B C34B H34C 107.6 . . ? P5 C34B H34C 107.6 . . ? C35B C34B H34D 107.6 . . ? P5 C34B H34D 107.6 . . ? H34C C34B H34D 107.0 . . ? C36B C35B C34B 114.8(16) . . ? C36B C35B H35C 108.6 . . ? C34B C35B H35C 108.6 . . ? C36B C35B H35D 108.6 . . ? C34B C35B H35D 108.6 . . ? H35C C35B H35D 107.5 . . ? C37B C36B C35B 114.6(16) . . ? C37B C36B H36C 108.6 . . ? C35B C36B H36C 108.6 . . ? C37B C36B H36D 108.6 . . ? C35B C36B H36D 108.6 . . ? H36C C36B H36D 107.6 . . ? C36B C37B C38B 116.7(14) . . ? C36B C37B H37C 108.1 . . ? C38B C37B H37C 108.1 . . ? C36B C37B H37D 108.1 . . ? C38B C37B H37D 108.1 . . ? H37C C37B H37D 107.3 . . ? C37B C38B C39B 116.2(18) . . ? C37B C38B H38C 108.2 . . ? C39B C38B H38C 108.2 . . ? C37B C38B H38D 108.2 . . ? C39B C38B H38D 108.2 . . ? H38C C38B H38D 107.4 . . ? C38B C39B P5 122.2(19) . . ? C38B C39B H39C 106.8 . . ? P5 C39B H39C 106.8 . . ? C38B C39B H39D 106.8 . . ? P5 C39B H39D 106.8 . . ? H39C C39B H39D 106.6 . . ? 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 P2 Pt1 P1 C4 123.3(2) . . . . ? Cl2 Pt1 P1 C4 -54.1(2) . . . . ? P2 Pt1 P1 C9 -115.2(2) . . . . ? Cl2 Pt1 P1 C9 67.4(2) . . . . ? P2 Pt1 P1 C1 1.8(3) . . . . ? Cl2 Pt1 P1 C1 -175.6(3) . . . . ? P1 Pt1 P2 C3 -8.7(2) . . . . ? Cl1 Pt1 P2 C3 178.0(2) . . . . ? P1 Pt1 P2 C10 -127.0(2) . . . . ? Cl1 Pt1 P2 C10 59.8(2) . . . . ? P1 Pt1 P2 C15 110.3(2) . . . . ? Cl1 Pt1 P2 C15 -62.9(2) . . . . ? P4 Pt2 P3 C24 -120.9(2) . . . . ? Cl4 Pt2 P3 C24 55.6(2) . . . . ? P4 Pt2 P3 C19 117.4(2) . . . . ? Cl4 Pt2 P3 C19 -66.2(2) . . . . ? P4 Pt2 P3 C16 -0.1(2) . . . . ? Cl4 Pt2 P3 C16 176.4(2) . . . . ? P3 Pt2 P4 C18 8.5(2) . . . . ? Cl3 Pt2 P4 C18 -178.0(2) . . . . ? P3 Pt2 P4 C25 -110.8(2) . . . . ? Cl3 Pt2 P4 C25 62.7(2) . . . . ? P3 Pt2 P4 C30 126.1(2) . . . . ? Cl3 Pt2 P4 C30 -60.4(2) . . . . ? P6 Pt3 P5 C39A -107.3(7) . . . . ? Cl6 Pt3 P5 C39A 64.3(7) . . . . ? P6 Pt3 P5 C31 17.2(3) . . . . ? Cl6 Pt3 P5 C31 -171.2(3) . . . . ? P6 Pt3 P5 C34A 127.4(6) . . . . ? Cl6 Pt3 P5 C34A -61.0(6) . . . . ? P6 Pt3 P5 C39B -96.6(10) . . . . ? Cl6 Pt3 P5 C39B 75.0(10) . . . . ? P6 Pt3 P5 C34B 143.7(7) . . . . ? Cl6 Pt3 P5 C34B -44.7(7) . . . . ? P5 Pt3 P6 C33 -18.0(3) . . . . ? Cl5 Pt3 P6 C33 159.9(3) . . . . ? P5 Pt3 P6 C40 -139.5(3) . . . . ? Cl5 Pt3 P6 C40 38.3(3) . . . . ? P5 Pt3 P6 C45 98.3(3) . . . . ? Cl5 Pt3 P6 C45 -83.8(3) . . . . ? C4 P1 C1 C2 -156.9(5) . . . . ? C9 P1 C1 C2 89.3(5) . . . . ? Pt1 P1 C1 C2 -29.8(5) . . . . ? P1 C1 C2 C3 73.1(6) . . . . ? C1 C2 C3 P2 -82.6(5) . . . . ? C10 P2 C3 C2 167.2(4) . . . . ? C15 P2 C3 C2 -77.4(5) . . . . ? Pt1 P2 C3 C2 45.9(5) . . . . ? C9 P1 C4 C5 48.4(6) . . . . ? C1 P1 C4 C5 -60.8(6) . . . . ? Pt1 P1 C4 C5 168.8(4) . . . . ? P1 C4 C5 C6 -87.1(7) . . . . ? C4 C5 C6 C7 53.5(10) . . . . ? C5 C6 C7 C8A 33.1(12) . . . . ? C6 C7 C8A C9 -91.7(10) . . . . ? C7 C8A C9 P1 66.2(9) . . . . ? C4 P1 C9 C8A -31.7(7) . . . . ? C1 P1 C9 C8A 77.0(6) . . . . ? Pt1 P1 C9 C8A -156.0(5) . . . . ? C3 P2 C10 C11 51.7(5) . . . . ? C15 P2 C10 C11 -58.9(6) . . . . ? Pt1 P2 C10 C11 177.7(4) . . . . ? P2 C10 C11 C12 81.2(7) . . . . ? C10 C11 C12 C13 -67.0(8) . . . . ? C11 C12 C13 C14 69.1(8) . . . . ? C12 C13 C14 C15 -89.2(8) . . . . ? C13 C14 C15 P2 65.8(7) . . . . ? C3 P2 C15 C14 -114.3(5) . . . . ? C10 P2 C15 C14 -3.4(6) . . . . ? Pt1 P2 C15 C14 119.0(4) . . . . ? C24 P3 C16 C17 153.5(5) . . . . ? C19 P3 C16 C17 -92.3(5) . . . . ? Pt2 P3 C16 C17 27.1(5) . . . . ? P3 C16 C17 C18 -70.3(6) . . . . ? C16 C17 C18 P4 81.9(6) . . . . ? C25 P4 C18 C17 77.3(5) . . . . ? C30 P4 C18 C17 -167.3(4) . . . . ? Pt2 P4 C18 C17 -46.5(5) . . . . ? C24 P3 C19 C20 32.3(6) . . . . ? C16 P3 C19 C20 -76.3(5) . . . . ? Pt2 P3 C19 C20 156.2(4) . . . . ? P3 C19 C20 C21 -65.3(7) . . . . ? C19 C20 C21 C22 97.9(7) . . . . ? C20 C21 C22 C23 -43.1(9) . . . . ? C21 C22 C23 C24 -46.2(9) . . . . ? C22 C23 C24 P3 87.4(7) . . . . ? C19 P3 C24 C23 -51.8(6) . . . . ? C16 P3 C24 C23 57.7(5) . . . . ? Pt2 P3 C24 C23 -172.0(4) . . . . ? C18 P4 C25 C26A 110.5(7) . . . . ? C30 P4 C25 C26A 0.1(8) . . . . ? Pt2 P4 C25 C26A -122.5(7) . . . . ? C18 P4 C25 C26B 84.7(10) . . . . ? C30 P4 C25 C26B -25.8(10) . . . . ? Pt2 P4 C25 C26B -148.4(9) . . . . ? C26B C25 C26A C27A 20(2) . . . . ? P4 C25 C26A C27A -61.3(12) . . . . ? C25 C26A C27A C28A 87.7(13) . . . . ? C26A C27A C28A C29 -70.3(15) . . . . ? C26A C25 C26B C27B -50.6(19) . . . . ? P4 C25 C26B C27B 60.2(19) . . . . ? C25 C26B C27B C28B -94(2) . . . . ? C26B C27B C28B C29 34(2) . . . . ? C27A C28A C29 C30 67.3(13) . . . . ? C27A C28A C29 C28B 128(4) . . . . ? C27B C28B C29 C28A -73(3) . . . . ? C27B C28B C29 C30 54.1(19) . . . . ? C28A C29 C30 P4 -77.4(9) . . . . ? C28B C29 C30 P4 -96.7(10) . . . . ? C18 P4 C30 C29 -54.1(5) . . . . ? C25 P4 C30 C29 56.2(6) . . . . ? Pt2 P4 C30 C29 -179.7(4) . . . . ? C39A P5 C31 C32 79.5(9) . . . . ? C34A P5 C31 C32 -160.6(7) . . . . ? C39B P5 C31 C32 76.1(11) . . . . ? C34B P5 C31 C32 -177.5(8) . . . . ? Pt3 P5 C31 C32 -45.1(6) . . . . ? P5 C31 C32 C33 73.0(7) . . . . ? C31 C32 C33 P6 -73.3(7) . . . . ? C40 P6 C33 C32 173.9(5) . . . . ? C45 P6 C33 C32 -73.6(6) . . . . ? Pt3 P6 C33 C32 46.4(6) . . . . ? C33 P6 C40 C41 79.8(6) . . . . ? C45 P6 C40 C41 -27.9(6) . . . . ? Pt3 P6 C40 C41 -150.4(5) . . . . ? P6 C40 C41 C42 84.0(7) . . . . ? C40 C41 C42 C43 -84.6(9) . . . . ? C41 C42 C43 C44 62.1(9) . . . . ? C42 C43 C44 C45 -72.3(9) . . . . ? C43 C44 C45 P6 84.8(7) . . . . ? C33 P6 C45 C44 -151.4(6) . . . . ? C40 P6 C45 C44 -43.4(6) . . . . ? Pt3 P6 C45 C44 82.4(6) . . . . ? C39A P5 C34A C35A 52.0(14) . . . . ? C31 P5 C34A C35A -63.2(11) . . . . ? C39B P5 C34A C35A 42.1(17) . . . . ? C34B P5 C34A C35A 49(3) . . . . ? Pt3 P5 C34A C35A 173.5(9) . . . . ? P5 C34A C35A C36A -85.3(13) . . . . ? C34A C35A C36A C37A 47.9(16) . . . . ? C35A C36A C37A C38A 41.2(16) . . . . ? C36A C37A C38A C39A -96.4(15) . . . . ? C37A C38A C39A P5 66.0(17) . . . . ? C31 P5 C39A C38A 74.1(14) . . . . ? C34A P5 C39A C38A -34.8(17) . . . . ? C39B P5 C39A C38A 93(9) . . . . ? C34B P5 C39A C38A -34.0(16) . . . . ? Pt3 P5 C39A C38A -155.9(12) . . . . ? C39A P5 C34B C35B -8.8(18) . . . . ? C31 P5 C34B C35B -120.3(15) . . . . ? C34A P5 C34B C35B 169(5) . . . . ? C39B P5 C34B C35B -18(2) . . . . ? Pt3 P5 C34B C35B 106.7(15) . . . . ? P5 C34B C35B C36B 77(2) . . . . ? C34B C35B C36B C37B -88(2) . . . . ? C35B C36B C37B C38B 68(2) . . . . ? C36B C37B C38B C39B -69(2) . . . . ? C37B C38B C39B P5 85(2) . . . . ? C39A P5 C39B C38B -105(9) . . . . ? C31 P5 C39B C38B 57(2) . . . . ? C34A P5 C39B C38B -48(3) . . . . ? C34B P5 C39B C38B -50(2) . . . . ? Pt3 P5 C39B C38B -177.7(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.763 _refine_diff_density_min -1.574 _refine_diff_density_rms 0.129 data_5a_toads _database_code_depnum_ccdc_archive 'CCDC 700271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 Cl2 O2 P4 Rh2' _chemical_formula_sum 'C24 H44 Cl2 O2 P4 Rh2' _chemical_formula_weight 765.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 '-P 2ybc' 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 11.7519(7) _cell_length_b 11.9472(7) _cell_length_c 22.4102(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.1220(10) _cell_angle_gamma 90.00 _cell_volume 3145.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5531 _cell_measurement_theta_min 2.431 _cell_measurement_theta_max 27.427 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'sadabs v2.03(bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 20348 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7198 _reflns_number_gt 4995 _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^)+(0.0285P)^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 7198 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 Rh2 Rh 0.18230(2) 0.81891(2) 0.090638(12) 0.01916(8) Uani 1 1 d . . . Rh1 Rh 0.34042(2) 0.82990(2) 0.328834(12) 0.01884(8) Uani 1 1 d . . . P1 P 0.52604(7) 0.82060(7) 0.29602(4) 0.0200(2) Uani 1 1 d . . . P4 P 0.15505(7) 0.85717(7) 0.35728(4) 0.01775(19) Uani 1 1 d . . . P3 P 0.00114(7) 0.85863(7) 0.12245(4) 0.0193(2) Uani 1 1 d . . . P2 P 0.36622(8) 0.79561(8) 0.05943(4) 0.0218(2) Uani 1 1 d . . . Cl1 Cl 0.36535(8) 1.02458(7) 0.34507(5) 0.0326(2) Uani 1 1 d . . . Cl2 Cl 0.20933(8) 1.01475(8) 0.07966(4) 0.0331(2) Uani 1 1 d . . . C8 C 0.4282(3) 0.6574(3) 0.04437(18) 0.0328(9) Uani 1 1 d . . . H8A H 0.4805 0.6352 0.0775 0.039 Uiso 1 1 calc R . . H8B H 0.3673 0.6004 0.0406 0.039 Uiso 1 1 calc R . . C15 C -0.1043(3) 0.7465(3) 0.13442(17) 0.0270(8) Uani 1 1 d . . . H15A H -0.0691 0.6720 0.1292 0.032 Uiso 1 1 calc R . . H15B H -0.1352 0.7512 0.1751 0.032 Uiso 1 1 calc R . . C1 C 0.6072(3) 0.6891(3) 0.29482(17) 0.0269(8) Uani 1 1 d . . . H1A H 0.5844 0.6392 0.3278 0.032 Uiso 1 1 calc R . . H1B H 0.5950 0.6494 0.2564 0.032 Uiso 1 1 calc R . . C16 C 0.0039(3) 0.9386(3) 0.19239(15) 0.0245(8) Uani 1 1 d . . . H16A H 0.0415 1.0116 0.1858 0.029 Uiso 1 1 calc R . . H16B H -0.0751 0.9534 0.2048 0.029 Uiso 1 1 calc R . . C19 C 0.1316(3) 0.9256(3) 0.42936(15) 0.0227(8) Uani 1 1 d . . . H19A H 0.1975 0.9132 0.4568 0.027 Uiso 1 1 calc R . . H19B H 0.1208 1.0071 0.4239 0.027 Uiso 1 1 calc R . . C12 C -0.0919(3) 0.9374(3) 0.07065(16) 0.0227(8) Uani 1 1 d . . . H12A H -0.0913 1.0180 0.0809 0.027 Uiso 1 1 calc R . . H12B H -0.0663 0.9285 0.0291 0.027 Uiso 1 1 calc R . . C22 C 0.0595(3) 0.7388(3) 0.37304(16) 0.0233(8) Uani 1 1 d . . . H22A H -0.0101 0.7430 0.3475 0.028 Uiso 1 1 calc R . . H22B H 0.0982 0.6668 0.3653 0.028 Uiso 1 1 calc R . . C18 C 0.0753(3) 0.9388(3) 0.30095(15) 0.0223(8) Uani 1 1 d . . . H18A H -0.0022 0.9542 0.3154 0.027 Uiso 1 1 calc R . . H18B H 0.1139 1.0115 0.2947 0.027 Uiso 1 1 calc R . . C7 C 0.4666(3) 0.8614(3) 0.11212(15) 0.0249(8) Uani 1 1 d . . . H7A H 0.5452 0.8489 0.0985 0.030 Uiso 1 1 calc R . . H7B H 0.4528 0.9431 0.1128 0.030 Uiso 1 1 calc R . . C5 C 0.5363(3) 0.8733(3) 0.21953(16) 0.0256(8) Uani 1 1 d . . . H5A H 0.5194 0.9545 0.2194 0.031 Uiso 1 1 calc R . . H5B H 0.6154 0.8636 0.2061 0.031 Uiso 1 1 calc R . . C6 C 0.4554(3) 0.8147(3) 0.17517(16) 0.0271(8) Uani 1 1 d . . . H6A H 0.4723 0.7335 0.1749 0.033 Uiso 1 1 calc R . . H6B H 0.3760 0.8245 0.1883 0.033 Uiso 1 1 calc R . . C20 C 0.0240(3) 0.8719(3) 0.45436(16) 0.0274(8) Uani 1 1 d . . . H20A H 0.0218 0.8821 0.4982 0.033 Uiso 1 1 calc R . . H20B H -0.0449 0.9065 0.4362 0.033 Uiso 1 1 calc R . . C24 C 0.1653(3) 0.6705(3) 0.10423(18) 0.0307(9) Uani 1 1 d . . . C23 C 0.3153(3) 0.6833(3) 0.31428(19) 0.0351(10) Uani 1 1 d . . . C11 C 0.4046(3) 0.8523(3) -0.01365(17) 0.0333(9) Uani 1 1 d . . . H11A H 0.3418 0.8411 -0.0432 0.040 Uiso 1 1 calc R . . H11B H 0.4215 0.9333 -0.0107 0.040 Uiso 1 1 calc R . . C21 C 0.0294(3) 0.7483(3) 0.43884(16) 0.0292(9) Uani 1 1 d . . . H21A H -0.0450 0.7123 0.4459 0.035 Uiso 1 1 calc R . . H21B H 0.0880 0.7106 0.4640 0.035 Uiso 1 1 calc R . . C14 C -0.1981(3) 0.7657(3) 0.0876(2) 0.0456(12) Uani 1 1 d . . . H14A H -0.1783 0.7281 0.0499 0.055 Uiso 1 1 calc R . . H14B H -0.2707 0.7341 0.1016 0.055 Uiso 1 1 calc R . . C4 C 0.6383(3) 0.8998(3) 0.33697(17) 0.0284(9) Uani 1 1 d . . . H4A H 0.6663 0.9623 0.3122 0.034 Uiso 1 1 calc R . . H4B H 0.6082 0.9309 0.3745 0.034 Uiso 1 1 calc R . . C13 C -0.2104(3) 0.8888(3) 0.07755(19) 0.0380(10) Uani 1 1 d . . . H13A H -0.2484 0.9240 0.1118 0.046 Uiso 1 1 calc R . . H13B H -0.2571 0.9031 0.0411 0.046 Uiso 1 1 calc R . . C3 C 0.7345(3) 0.8163(3) 0.35055(19) 0.0397(10) Uani 1 1 d . . . H3A H 0.8089 0.8553 0.3506 0.048 Uiso 1 1 calc R . . H3B H 0.7242 0.7825 0.3904 0.048 Uiso 1 1 calc R . . C2 C 0.7318(3) 0.7251(3) 0.30267(18) 0.0360(10) Uani 1 1 d . . . H2A H 0.7794 0.6607 0.3154 0.043 Uiso 1 1 calc R . . H2B H 0.7611 0.7545 0.2646 0.043 Uiso 1 1 calc R . . C10 C 0.5101(3) 0.7869(4) -0.03152(18) 0.0419(11) Uani 1 1 d . . . H10A H 0.5208 0.7924 -0.0751 0.050 Uiso 1 1 calc R . . H10B H 0.5785 0.8177 -0.0110 0.050 Uiso 1 1 calc R . . O1 O 0.1543(2) 0.5787(2) 0.11327(16) 0.0546(9) Uani 1 1 d . . . C17 C 0.0673(3) 0.8752(3) 0.24188(16) 0.0267(8) Uani 1 1 d . . . H17A H 0.1452 0.8583 0.2285 0.032 Uiso 1 1 calc R . . H17B H 0.0282 0.8030 0.2486 0.032 Uiso 1 1 calc R . . O2 O 0.2955(3) 0.5917(2) 0.30368(17) 0.0669(11) Uani 1 1 d . . . C9 C 0.4929(4) 0.6663(4) -0.0137(2) 0.0499(12) Uani 1 1 d . . . H9A H 0.5679 0.6293 -0.0088 0.060 Uiso 1 1 calc R . . H9B H 0.4499 0.6269 -0.0458 0.060 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 Rh2 0.01728(15) 0.02155(15) 0.01866(16) 0.00024(11) 0.00029(11) 0.00022(11) Rh1 0.01705(15) 0.02137(15) 0.01811(16) -0.00069(11) 0.00083(11) 0.00025(11) P1 0.0168(5) 0.0264(5) 0.0168(5) -0.0015(4) 0.0003(4) -0.0004(4) P4 0.0182(5) 0.0197(5) 0.0154(5) -0.0011(4) 0.0008(4) 0.0000(4) P3 0.0182(5) 0.0216(5) 0.0180(5) 0.0012(4) 0.0005(4) 0.0006(4) P2 0.0191(5) 0.0308(5) 0.0155(5) 0.0005(4) 0.0004(4) 0.0013(4) Cl1 0.0309(5) 0.0238(5) 0.0431(6) -0.0032(4) 0.0047(4) -0.0036(4) Cl2 0.0332(5) 0.0268(5) 0.0394(6) 0.0046(4) 0.0016(4) -0.0020(4) C8 0.029(2) 0.039(2) 0.031(2) -0.0052(18) -0.0007(17) 0.0077(17) C15 0.027(2) 0.026(2) 0.029(2) 0.0035(16) 0.0064(16) -0.0037(16) C1 0.026(2) 0.030(2) 0.026(2) 0.0000(16) 0.0032(16) 0.0079(16) C16 0.025(2) 0.027(2) 0.021(2) 0.0001(15) -0.0021(16) 0.0051(15) C19 0.025(2) 0.0228(18) 0.020(2) -0.0016(15) 0.0000(15) 0.0024(15) C12 0.026(2) 0.0212(18) 0.021(2) 0.0040(15) -0.0031(16) 0.0028(15) C22 0.0238(19) 0.0217(19) 0.024(2) 0.0036(15) 0.0015(16) -0.0012(15) C18 0.025(2) 0.0220(18) 0.020(2) -0.0012(15) 0.0010(15) 0.0023(15) C7 0.0206(19) 0.035(2) 0.019(2) 0.0013(16) -0.0025(15) -0.0027(16) C5 0.023(2) 0.030(2) 0.024(2) 0.0013(16) 0.0011(16) -0.0057(16) C6 0.022(2) 0.039(2) 0.020(2) -0.0005(17) -0.0044(15) -0.0026(16) C20 0.032(2) 0.032(2) 0.019(2) -0.0027(16) 0.0077(16) 0.0064(17) C24 0.019(2) 0.034(2) 0.039(3) -0.0010(19) 0.0021(17) 0.0035(17) C23 0.023(2) 0.032(2) 0.050(3) -0.009(2) 0.0104(18) -0.0002(17) C11 0.028(2) 0.051(3) 0.022(2) 0.0024(18) 0.0019(17) -0.0067(18) C21 0.029(2) 0.035(2) 0.024(2) 0.0029(17) 0.0062(16) -0.0047(17) C14 0.027(2) 0.044(3) 0.066(3) 0.010(2) -0.009(2) -0.0075(19) C4 0.020(2) 0.041(2) 0.024(2) -0.0031(17) -0.0043(16) -0.0036(16) C13 0.022(2) 0.050(3) 0.041(3) 0.016(2) -0.0056(19) -0.0034(19) C3 0.023(2) 0.055(3) 0.041(3) 0.004(2) -0.0083(18) 0.0009(19) C2 0.023(2) 0.047(3) 0.038(3) 0.003(2) 0.0070(18) 0.0096(18) C10 0.031(2) 0.071(3) 0.025(2) -0.007(2) 0.0085(18) 0.001(2) O1 0.045(2) 0.0328(18) 0.086(3) 0.0105(17) 0.0007(17) -0.0019(15) C17 0.032(2) 0.026(2) 0.023(2) -0.0009(16) 0.0000(17) 0.0049(16) O2 0.053(2) 0.0283(18) 0.120(3) -0.0230(18) 0.025(2) -0.0053(15) C9 0.056(3) 0.057(3) 0.038(3) -0.008(2) 0.018(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh2 C24 1.811(4) . yes Rh2 P2 2.3017(9) . yes Rh2 P3 2.3077(9) . yes Rh2 Cl2 2.3746(9) . yes Rh1 C23 1.805(4) . yes Rh1 P4 2.3049(9) . yes Rh1 P1 2.3183(9) . yes Rh1 Cl1 2.3714(9) . yes P1 C5 1.833(4) . yes P1 C1 1.839(3) . yes P1 C4 1.852(3) . yes P4 C19 1.836(3) . yes P4 C18 1.838(3) . yes P4 C22 1.844(3) . yes P3 C16 1.835(3) . yes P3 C12 1.838(3) . yes P3 C15 1.847(3) . yes P2 C7 1.831(3) . yes P2 C11 1.836(4) . yes P2 C8 1.839(4) . yes C8 C9 1.524(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C15 C14 1.524(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C1 C2 1.533(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C16 C17 1.525(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C19 C20 1.534(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C12 C13 1.520(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C22 C21 1.527(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C18 C17 1.528(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C7 C6 1.527(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C5 C6 1.532(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C20 C21 1.518(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C24 O1 1.123(4) . ? C23 O2 1.143(4) . ? C11 C10 1.526(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C14 C13 1.495(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C4 C3 1.534(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C3 C2 1.529(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C10 C9 1.510(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 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 C24 Rh2 P2 92.30(12) . . ? C24 Rh2 P3 92.51(11) . . ? P2 Rh2 P3 175.05(3) . . ? C24 Rh2 Cl2 176.07(13) . . ? P2 Rh2 Cl2 87.67(3) . . ? P3 Rh2 Cl2 87.45(3) . . ? C23 Rh1 P4 92.02(11) . . ? C23 Rh1 P1 92.73(12) . . ? P4 Rh1 P1 174.16(3) . . ? C23 Rh1 Cl1 177.20(13) . . ? P4 Rh1 Cl1 86.19(3) . . ? P1 Rh1 Cl1 88.94(3) . . ? C5 P1 C1 103.68(17) . . yes C5 P1 C4 103.21(17) . . yes C1 P1 C4 94.56(16) . . yes C5 P1 Rh1 111.08(12) . . ? C1 P1 Rh1 122.49(12) . . ? C4 P1 Rh1 118.94(12) . . ? C19 P4 C18 106.55(16) . . yes C19 P4 C22 94.05(16) . . yes C18 P4 C22 103.57(16) . . yes C19 P4 Rh1 117.71(12) . . ? C18 P4 Rh1 110.91(12) . . ? C22 P4 Rh1 121.79(12) . . ? C16 P3 C12 105.84(16) . . yes C16 P3 C15 104.71(17) . . yes C12 P3 C15 94.05(16) . . yes C16 P3 Rh2 111.72(12) . . ? C12 P3 Rh2 116.82(12) . . ? C15 P3 Rh2 121.40(12) . . ? C7 P2 C11 104.51(17) . . yes C7 P2 C8 104.57(18) . . yes C11 P2 C8 93.59(18) . . yes C7 P2 Rh2 110.45(12) . . ? C11 P2 Rh2 118.34(12) . . ? C8 P2 Rh2 122.82(13) . . ? C9 C8 P2 107.5(3) . . ? C9 C8 H8A 110.2 . . ? P2 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? P2 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C14 C15 P3 105.6(3) . . ? C14 C15 H15A 110.6 . . ? P3 C15 H15A 110.6 . . ? C14 C15 H15B 110.6 . . ? P3 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? C2 C1 P1 104.7(2) . . ? C2 C1 H1A 110.8 . . ? P1 C1 H1A 110.8 . . ? C2 C1 H1B 110.8 . . ? P1 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C17 C16 P3 111.3(2) . . ? C17 C16 H16A 109.4 . . ? P3 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? P3 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C20 C19 P4 105.9(2) . . ? C20 C19 H19A 110.6 . . ? P4 C19 H19A 110.6 . . ? C20 C19 H19B 110.6 . . ? P4 C19 H19B 110.6 . . ? H19A C19 H19B 108.7 . . ? C13 C12 P3 106.0(2) . . ? C13 C12 H12A 110.5 . . ? P3 C12 H12A 110.5 . . ? C13 C12 H12B 110.5 . . ? P3 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C21 C22 P4 106.3(2) . . ? C21 C22 H22A 110.5 . . ? P4 C22 H22A 110.5 . . ? C21 C22 H22B 110.5 . . ? P4 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C17 C18 P4 110.7(2) . . ? C17 C18 H18A 109.5 . . ? P4 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? P4 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C6 C7 P2 111.9(2) . . ? C6 C7 H7A 109.2 . . ? P2 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? P2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C6 C5 P1 113.5(2) . . ? C6 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 111.7(3) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C21 C20 C19 106.5(3) . . ? C21 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? C21 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O1 C24 Rh2 179.2(4) . . ? O2 C23 Rh1 177.1(4) . . ? C10 C11 P2 105.1(3) . . ? C10 C11 H11A 110.7 . . ? P2 C11 H11A 110.7 . . ? C10 C11 H11B 110.7 . . ? P2 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C20 C21 C22 107.8(3) . . ? C20 C21 H21A 110.2 . . ? C22 C21 H21A 110.2 . . ? C20 C21 H21B 110.2 . . ? C22 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? C13 C14 C15 108.6(3) . . ? C13 C14 H14A 110.0 . . ? C15 C14 H14A 110.0 . . ? C13 C14 H14B 110.0 . . ? C15 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C3 C4 P1 106.3(2) . . ? C3 C4 H4A 110.5 . . ? P1 C4 H4A 110.5 . . ? C3 C4 H4B 110.5 . . ? P1 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C14 C13 C12 107.8(3) . . ? C14 C13 H13A 110.2 . . ? C12 C13 H13A 110.2 . . ? C14 C13 H13B 110.2 . . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C2 C3 C4 108.6(3) . . ? C2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? C3 C2 C1 106.7(3) . . ? C3 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? C3 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? C9 C10 C11 107.8(3) . . ? C9 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? C9 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C16 C17 C18 113.8(3) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C10 C9 C8 111.3(3) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.117 data_5c_ajm199sad _database_code_depnum_ccdc_archive 'CCDC 700272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H60 Cl2 O2 P4 Rh2' _chemical_formula_sum 'C32 H60 Cl2 O2 P4 Rh2' _chemical_formula_weight 877.40 _chemical_absolute_configuration ad 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0204(18) _cell_length_b 11.9691(16) _cell_length_c 28.877(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3809.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5098 _cell_measurement_theta_min 2.323 _cell_measurement_theta_max 23.685 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731683 _exptl_absorpt_correction_T_max 0.980000 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25010 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8754 _reflns_number_gt 5884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.02 (Bruker, 1999)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.0438P)^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 -0.01(4) _refine_ls_number_reflns 8754 _refine_ls_number_parameters 456 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.992 _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 0.16582(4) 0.98200(4) 0.159888(15) 0.02354(12) Uani 1 1 d . A . Rh2 Rh 0.04920(4) 0.98878(4) -0.034026(16) 0.02772(13) Uani 1 1 d . . . P1 P 0.35651(14) 1.04940(14) 0.14046(5) 0.0245(4) Uani 1 1 d . . . P2 P 0.24614(15) 1.04097(14) -0.05100(5) 0.0253(4) Uani 1 1 d . A . P3 P -0.02412(15) 0.90471(14) 0.17219(6) 0.0236(4) Uani 1 1 d . . . Cl1 Cl 0.07522(19) 1.14161(17) 0.12490(7) 0.0512(5) Uani 1 1 d . . . Cl2 Cl 0.0974(2) 0.80209(16) -0.05513(11) 0.0785(9) Uani 1 1 d . A . O1 O 0.2747(6) 0.7952(6) 0.2037(3) 0.066(2) Uani 1 1 d . A . O2 O -0.0088(5) 1.2212(5) -0.0097(2) 0.0578(16) Uani 1 1 d . . . C1 C 0.4034(5) 1.0146(6) 0.08128(18) 0.0300(15) Uani 1 1 d . . . H1A H 0.4787 1.0562 0.0741 0.036 Uiso 1 1 calc R . . H1B H 0.4230 0.9339 0.0800 0.036 Uiso 1 1 calc R . . C2 C 0.3085(5) 1.0405(5) 0.04350(19) 0.0274(15) Uani 1 1 d . A . H2A H 0.2318 1.0015 0.0510 0.033 Uiso 1 1 calc R . . H2B H 0.2919 1.1218 0.0432 0.033 Uiso 1 1 calc R . . C3 C 0.3520(5) 1.0041(5) -0.00436(18) 0.0266(13) Uani 1 1 d . . . H3A H 0.3639 0.9221 -0.0043 0.032 Uiso 1 1 calc R A . H3B H 0.4315 1.0393 -0.0107 0.032 Uiso 1 1 calc R . . C4 C 0.3766(6) 1.2009(5) 0.1444(2) 0.0345(17) Uani 1 1 d . . . H4A H 0.4637 1.2180 0.1398 0.041 Uiso 1 1 calc R . . H4B H 0.3314 1.2361 0.1186 0.041 Uiso 1 1 calc R . . C5 C 0.3357(7) 1.2551(6) 0.1896(2) 0.0443(19) Uani 1 1 d . . . H5A H 0.2476 1.2703 0.1874 0.053 Uiso 1 1 calc R . . H5B H 0.3774 1.3280 0.1926 0.053 Uiso 1 1 calc R . . C6 C 0.3596(8) 1.1858(8) 0.2346(3) 0.067(3) Uani 1 1 d . . . H6A H 0.3449 1.2355 0.2614 0.081 Uiso 1 1 calc R . . H6B H 0.2980 1.1256 0.2360 0.081 Uiso 1 1 calc R . . C7 C 0.4801(8) 1.1337(8) 0.2410(3) 0.066(3) Uani 1 1 d . . . H7A H 0.5013 1.1368 0.2743 0.080 Uiso 1 1 calc R . . H7B H 0.5409 1.1787 0.2240 0.080 Uiso 1 1 calc R . . C8 C 0.4897(6) 1.0131(7) 0.2249(2) 0.0452(19) Uani 1 1 d . . . H8A H 0.4211 0.9703 0.2381 0.054 Uiso 1 1 calc R . . H8B H 0.5656 0.9807 0.2373 0.054 Uiso 1 1 calc R . . C9 C 0.4891(5) 0.9981(7) 0.1724(2) 0.0378(17) Uani 1 1 d . . . H9A H 0.4978 0.9173 0.1657 0.045 Uiso 1 1 calc R . . H9B H 0.5618 1.0359 0.1598 0.045 Uiso 1 1 calc R . . C10 C 0.2805(6) 1.1881(5) -0.0599(2) 0.0313(16) Uani 1 1 d . . . H10A H 0.2633 1.2285 -0.0308 0.038 Uiso 1 1 calc R A . H10B H 0.3686 1.1952 -0.0660 0.038 Uiso 1 1 calc R . . C11 C 0.2120(6) 1.2462(6) -0.0992(2) 0.0419(19) Uani 1 1 d . A . H11A H 0.1248 1.2482 -0.0910 0.050 Uiso 1 1 calc R . . H11B H 0.2406 1.3244 -0.1011 0.050 Uiso 1 1 calc R . . C12 C 0.2247(8) 1.1933(7) -0.1465(3) 0.056(2) Uani 1 1 d . . . H12A H 0.3121 1.1807 -0.1526 0.067 Uiso 1 1 calc R A . H12B H 0.1948 1.2469 -0.1699 0.067 Uiso 1 1 calc R . . C13 C 0.1582(8) 1.0833(7) -0.1531(2) 0.057(2) Uani 1 1 d . A . H13A H 0.1253 1.0816 -0.1850 0.068 Uiso 1 1 calc R . . H13B H 0.0882 1.0820 -0.1316 0.068 Uiso 1 1 calc R . . C14 C 0.2322(7) 0.9764(8) -0.1454(2) 0.058(2) Uani 1 1 d . . . H14A H 0.2833 0.9635 -0.1731 0.069 Uiso 1 1 calc R A . H14B H 0.1753 0.9127 -0.1429 0.069 Uiso 1 1 calc R . . C15 C 0.3155(6) 0.9773(7) -0.1018(2) 0.0454(19) Uani 1 1 d . A . H15A H 0.3910 1.0183 -0.1093 0.054 Uiso 1 1 calc R . . H15B H 0.3382 0.8994 -0.0942 0.054 Uiso 1 1 calc R . . C16A C -0.0677(7) 0.8141(7) 0.1247(2) 0.048(2) Uani 0.444(11) 1 d P A 1 H16A H -0.0316 0.7404 0.1320 0.058 Uiso 0.444(11) 1 calc PR A 1 H16B H -0.1566 0.8044 0.1277 0.058 Uiso 0.444(11) 1 calc PR A 1 C17A C -0.0463(16) 0.8310(16) 0.0768(6) 0.030(4) Uani 0.444(11) 1 d P A 1 H17A H -0.0522 0.7595 0.0597 0.036 Uiso 0.444(11) 1 calc PR A 1 H17B H 0.0353 0.8632 0.0716 0.036 Uiso 0.444(11) 1 calc PR A 1 C18A C -0.1459(15) 0.9131(12) 0.0606(5) 0.026(4) Uani 0.444(11) 1 d P A 1 H18A H -0.1338 0.9855 0.0766 0.031 Uiso 0.444(11) 1 calc PR A 1 H18B H -0.2259 0.8835 0.0702 0.031 Uiso 0.444(11) 1 calc PR A 1 C16B C -0.0677(7) 0.8141(7) 0.1247(2) 0.048(2) Uani 0.556(11) 1 d P A 2 H16C H -0.0079 0.7531 0.1207 0.058 Uiso 0.556(11) 1 calc PR A 2 H16D H -0.1485 0.7807 0.1305 0.058 Uiso 0.556(11) 1 calc PR A 2 C17B C -0.0713(13) 0.8963(13) 0.0774(4) 0.030(3) Uani 0.556(11) 1 d P A 2 H17C H -0.1256 0.9608 0.0829 0.036 Uiso 0.556(11) 1 calc PR A 2 H17D H 0.0111 0.9252 0.0708 0.036 Uiso 0.556(11) 1 calc PR A 2 C18B C -0.1169(11) 0.8296(9) 0.0363(4) 0.030(3) Uani 0.556(11) 1 d P A 2 H18C H -0.1968 0.7969 0.0440 0.035 Uiso 0.556(11) 1 calc PR A 2 H18D H -0.0600 0.7673 0.0302 0.035 Uiso 0.556(11) 1 calc PR A 2 C19 C -0.1571(5) 0.9958(6) 0.1788(2) 0.0363(16) Uani 1 1 d . A . H19A H -0.1650 1.0414 0.1503 0.044 Uiso 1 1 calc R . . H19B H -0.2302 0.9479 0.1808 0.044 Uiso 1 1 calc R . . C20 C -0.1574(7) 1.0743(6) 0.2200(2) 0.0411(18) Uani 1 1 d . . . H20A H -0.0895 1.1276 0.2161 0.049 Uiso 1 1 calc R A . H20B H -0.2336 1.1180 0.2191 0.049 Uiso 1 1 calc R . . C21 C -0.1465(6) 1.0219(6) 0.2672(2) 0.0421(17) Uani 1 1 d . A . H21A H -0.2051 0.9595 0.2696 0.051 Uiso 1 1 calc R . . H21B H -0.1686 1.0781 0.2909 0.051 Uiso 1 1 calc R . . C22 C -0.0185(6) 0.9776(6) 0.2776(2) 0.0451(19) Uani 1 1 d . . . H22A H 0.0403 1.0217 0.2592 0.054 Uiso 1 1 calc R A . H22B H -0.0007 0.9918 0.3107 0.054 Uiso 1 1 calc R . . C23 C 0.0043(6) 0.8536(6) 0.2679(2) 0.0381(18) Uani 1 1 d . A . H23A H 0.0927 0.8398 0.2695 0.046 Uiso 1 1 calc R . . H23B H -0.0344 0.8093 0.2928 0.046 Uiso 1 1 calc R . . C24 C -0.0419(6) 0.8109(5) 0.2216(2) 0.0334(16) Uani 1 1 d . A . H24A H -0.1292 0.7931 0.2249 0.040 Uiso 1 1 calc R . . H24B H 0.0008 0.7402 0.2145 0.040 Uiso 1 1 calc R . . C32 C 0.0136(6) 1.1310(6) -0.0180(3) 0.0354(17) Uani 1 1 d . A . P4A P -0.1484(10) 0.9381(9) -0.0032(3) 0.0249(17) Uani 0.444(11) 1 d P A 1 C25A C -0.2118(16) 0.8134(14) -0.0293(7) 0.038(5) Uani 0.444(11) 1 d PU A 1 H25A H -0.1561 0.7505 -0.0227 0.045 Uiso 0.444(11) 1 calc PR A 1 H25B H -0.2895 0.7969 -0.0136 0.045 Uiso 0.444(11) 1 calc PR A 1 C26A C -0.236(2) 0.8153(16) -0.0817(8) 0.040(5) Uani 0.444(11) 1 d PU A 1 H26A H -0.2679 0.7417 -0.0913 0.048 Uiso 0.444(11) 1 calc PR A 1 H26B H -0.1577 0.8271 -0.0981 0.048 Uiso 0.444(11) 1 calc PR A 1 C27A C -0.3290(18) 0.9105(13) -0.0970(6) 0.048(5) Uani 0.444(11) 1 d PU A 1 H27A H -0.3602 0.8914 -0.1282 0.057 Uiso 0.444(11) 1 calc PR A 1 H27B H -0.3988 0.9087 -0.0754 0.057 Uiso 0.444(11) 1 calc PR A 1 C28A C -0.283(3) 1.024(2) -0.0985(8) 0.050(7) Uani 0.444(11) 1 d PU A 1 H28A H -0.3223 1.0629 -0.1246 0.060 Uiso 0.444(11) 1 calc PR A 1 H28B H -0.1950 1.0206 -0.1050 0.060 Uiso 0.444(11) 1 calc PR A 1 C29A C -0.302(5) 1.090(3) -0.0563(10) 0.038(7) Uani 0.444(11) 1 d PU A 1 H29A H -0.3876 1.1143 -0.0557 0.046 Uiso 0.444(11) 1 calc PR A 1 H29B H -0.2515 1.1584 -0.0589 0.046 Uiso 0.444(11) 1 calc PR A 1 C30A C -0.273(5) 1.035(4) -0.0089(12) 0.028(4) Uani 0.444(11) 1 d PU A 1 H30A H -0.3475 0.9961 0.0014 0.033 Uiso 0.444(11) 1 calc PR A 1 H30B H -0.2588 1.0967 0.0135 0.033 Uiso 0.444(11) 1 calc PR A 1 P4B P -0.1319(8) 0.9145(7) -0.0166(3) 0.0240(14) Uani 0.556(11) 1 d PU A 2 C25B C -0.2042(16) 0.8213(15) -0.0579(6) 0.043(4) Uani 0.556(11) 1 d PU A 2 H25C H -0.1622 0.7483 -0.0566 0.051 Uiso 0.556(11) 1 calc PR A 2 H25D H -0.2890 0.8090 -0.0478 0.051 Uiso 0.556(11) 1 calc PR A 2 C26B C -0.2062(14) 0.8602(14) -0.1081(5) 0.049(4) Uani 0.556(11) 1 d PU A 2 H26C H -0.1281 0.8397 -0.1228 0.059 Uiso 0.556(11) 1 calc PR A 2 H26D H -0.2713 0.8195 -0.1247 0.059 Uiso 0.556(11) 1 calc PR A 2 C27B C -0.2258(14) 0.9812(15) -0.1142(5) 0.055(4) Uani 0.556(11) 1 d PU A 2 H27C H -0.2389 0.9956 -0.1476 0.066 Uiso 0.556(11) 1 calc PR A 2 H27D H -0.1500 1.0201 -0.1053 0.066 Uiso 0.556(11) 1 calc PR A 2 C28B C -0.331(2) 1.036(2) -0.0873(7) 0.061(6) Uani 0.556(11) 1 d PU A 2 H28C H -0.3700 1.0925 -0.1073 0.074 Uiso 0.556(11) 1 calc PR A 2 H28D H -0.3929 0.9777 -0.0805 0.074 Uiso 0.556(11) 1 calc PR A 2 C29B C -0.293(3) 1.091(2) -0.0419(8) 0.028(5) Uani 0.556(11) 1 d PU A 2 H29C H -0.3606 1.1398 -0.0315 0.033 Uiso 0.556(11) 1 calc PR A 2 H29D H -0.2226 1.1396 -0.0482 0.033 Uiso 0.556(11) 1 calc PR A 2 C30B C -0.260(4) 1.010(3) -0.0010(9) 0.028(4) Uani 0.556(11) 1 d PU A 2 H30C H -0.3317 0.9653 0.0074 0.033 Uiso 0.556(11) 1 calc PR A 2 H30D H -0.2364 1.0551 0.0264 0.033 Uiso 0.556(11) 1 calc PR A 2 C31 C 0.2398(7) 0.8531(8) 0.1882(3) 0.041(2) 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 0.0201(2) 0.0272(3) 0.0234(2) 0.0045(2) -0.00056(19) 0.0001(2) Rh2 0.0244(3) 0.0247(3) 0.0340(3) 0.0021(2) -0.0083(2) -0.0030(2) P1 0.0200(9) 0.0314(10) 0.0222(8) 0.0030(7) -0.0007(7) -0.0012(7) P2 0.0233(8) 0.0317(10) 0.0208(8) -0.0047(7) -0.0005(7) 0.0053(7) P3 0.0195(9) 0.0286(9) 0.0228(9) 0.0035(7) -0.0005(7) -0.0002(7) Cl1 0.0443(12) 0.0579(12) 0.0514(12) 0.0091(10) 0.0076(9) -0.0015(10) Cl2 0.0468(13) 0.0291(11) 0.160(3) -0.0133(13) -0.0330(15) 0.0100(9) O1 0.046(4) 0.066(5) 0.085(6) 0.006(4) 0.019(4) -0.009(4) O2 0.042(3) 0.052(4) 0.080(4) -0.027(3) 0.017(3) -0.008(3) C1 0.029(3) 0.039(4) 0.023(3) 0.004(3) 0.001(2) 0.000(3) C2 0.028(4) 0.031(4) 0.024(3) -0.002(3) -0.002(3) 0.002(3) C3 0.028(3) 0.022(3) 0.029(3) -0.001(3) -0.005(2) 0.010(3) C4 0.029(4) 0.038(4) 0.036(4) -0.004(3) 0.005(3) -0.008(3) C5 0.041(5) 0.048(5) 0.044(5) -0.019(4) 0.001(4) -0.004(4) C6 0.055(6) 0.107(8) 0.041(5) -0.033(5) 0.003(4) 0.001(6) C7 0.053(6) 0.118(8) 0.028(5) -0.004(5) -0.010(4) -0.017(6) C8 0.035(4) 0.071(6) 0.030(4) 0.020(5) -0.007(3) -0.007(4) C9 0.028(3) 0.054(5) 0.031(3) 0.009(4) -0.008(3) -0.004(4) C10 0.027(4) 0.040(4) 0.027(4) 0.006(3) 0.004(3) -0.006(3) C11 0.036(4) 0.060(5) 0.029(4) 0.011(4) -0.001(3) -0.010(4) C12 0.050(5) 0.085(7) 0.033(5) 0.021(4) 0.006(4) 0.004(5) C13 0.052(5) 0.094(7) 0.023(4) -0.004(4) -0.008(4) 0.019(5) C14 0.056(5) 0.091(7) 0.026(4) -0.018(4) -0.007(3) 0.013(5) C15 0.040(4) 0.069(5) 0.027(3) -0.012(4) 0.000(3) 0.017(4) C16A 0.030(4) 0.081(6) 0.034(4) -0.011(4) 0.001(3) -0.016(4) C17A 0.021(9) 0.033(10) 0.037(10) -0.001(8) -0.001(7) 0.008(8) C18A 0.025(9) 0.024(8) 0.030(9) -0.002(7) 0.002(7) 0.002(7) C16B 0.030(4) 0.081(6) 0.034(4) -0.011(4) 0.001(3) -0.016(4) C17B 0.026(8) 0.041(9) 0.024(7) 0.007(7) -0.009(6) 0.010(7) C18B 0.038(7) 0.027(7) 0.024(7) 0.003(6) 0.002(5) -0.013(5) C19 0.027(3) 0.054(5) 0.028(3) 0.017(4) 0.000(3) 0.006(4) C20 0.039(4) 0.034(4) 0.050(5) 0.011(3) 0.008(4) 0.007(4) C21 0.048(4) 0.043(4) 0.036(4) -0.009(4) 0.004(3) 0.004(4) C22 0.051(5) 0.054(5) 0.031(4) -0.011(4) -0.008(3) -0.006(4) C23 0.033(4) 0.058(5) 0.024(4) 0.013(4) 0.001(3) 0.005(4) C24 0.026(4) 0.037(4) 0.037(4) 0.007(3) 0.002(3) -0.002(3) C32 0.016(3) 0.045(5) 0.045(5) 0.002(4) 0.009(3) -0.007(3) P4A 0.019(3) 0.028(4) 0.028(5) 0.003(3) 0.002(3) -0.007(3) C25A 0.033(10) 0.032(9) 0.049(11) -0.004(9) -0.017(9) 0.006(7) C26A 0.050(13) 0.029(9) 0.041(11) -0.016(9) 0.003(11) -0.013(7) C27A 0.055(12) 0.053(9) 0.035(10) 0.006(7) -0.015(9) -0.016(8) C28A 0.09(2) 0.038(10) 0.023(9) 0.016(9) 0.022(11) -0.004(11) C29A 0.034(17) 0.051(12) 0.029(15) 0.008(9) 0.001(14) 0.007(11) C30A 0.024(8) 0.034(14) 0.025(8) 0.001(7) 0.000(7) -0.001(7) P4B 0.019(3) 0.031(3) 0.023(4) 0.000(2) -0.003(2) -0.004(2) C25B 0.044(10) 0.048(9) 0.035(10) -0.009(6) -0.008(9) 0.000(7) C26B 0.048(10) 0.068(9) 0.033(7) -0.006(7) -0.021(7) -0.015(7) C27B 0.055(10) 0.083(9) 0.027(7) -0.002(7) -0.018(6) 0.008(9) C28B 0.069(15) 0.081(13) 0.034(11) -0.020(9) -0.021(9) 0.010(10) C29B 0.015(8) 0.033(8) 0.036(13) -0.004(9) -0.014(11) 0.007(6) C30B 0.024(8) 0.034(14) 0.025(8) 0.001(7) 0.000(7) -0.001(7) C31 0.018(4) 0.073(7) 0.030(5) 0.000(4) 0.001(3) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C31 1.927(9) . yes Rh1 P3 2.3160(17) . yes Rh1 P1 2.3200(17) . yes Rh1 Cl1 2.381(2) . yes Rh2 C32 1.807(8) . yes Rh2 P4B 2.242(9) . yes Rh2 P2 2.3111(18) . yes Rh2 Cl2 2.376(2) . yes Rh2 P4A 2.429(10) . yes P1 C4 1.830(6) . yes P1 C9 1.833(6) . yes P1 C1 1.833(6) . yes P2 C10 1.819(6) . yes P2 C15 1.822(6) . yes P2 C3 1.836(5) . yes P3 C16A 1.813(7) . yes P3 C24 1.826(6) . yes P3 C19 1.837(6) . yes O1 C31 0.910(9) . ? O2 C32 1.133(8) . ? C1 C2 1.543(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.526(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.525(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.566(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.478(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.526(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.529(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.513(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.519(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.533(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.559(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16A C17A 1.419(17) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A C18A 1.55(2) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A P4A 1.868(18) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C17B C18B 1.516(18) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B P4B 1.840(14) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19 C20 1.516(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.505(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.537(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.531(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.518(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? P4A C30A 1.81(3) . yes P4A C25A 1.812(18) . yes C25A C26A 1.53(2) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A C27A 1.60(3) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27A C28A 1.45(3) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A C29A 1.47(3) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C29A C30A 1.55(3) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? P4B C25B 1.816(18) . ? P4B C30B 1.87(3) . ? C25B C26B 1.52(2) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C26B C27B 1.48(2) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27B C28B 1.54(2) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B C29B 1.53(2) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B C30B 1.57(2) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B H30C 0.9900 . ? C30B H30D 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 C31 Rh1 P3 89.9(2) . . ? C31 Rh1 P1 89.9(2) . . ? P3 Rh1 P1 174.13(6) . . ? C31 Rh1 Cl1 179.7(3) . . ? P3 Rh1 Cl1 90.38(7) . . ? P1 Rh1 Cl1 89.90(7) . . ? C32 Rh2 P4B 97.1(3) . . ? C32 Rh2 P2 90.2(2) . . ? P4B Rh2 P2 172.2(2) . . ? C32 Rh2 Cl2 179.6(2) . . ? P4B Rh2 Cl2 83.3(2) . . ? P2 Rh2 Cl2 89.41(7) . . ? C32 Rh2 P4A 87.0(3) . . ? P4B Rh2 P4A 11.7(3) . . ? P2 Rh2 P4A 170.8(2) . . ? Cl2 Rh2 P4A 93.4(2) . . ? C4 P1 C9 101.8(4) . . yes C4 P1 C1 104.4(3) . . yes C9 P1 C1 99.7(3) . . yes C4 P1 Rh1 116.1(2) . . ? C9 P1 Rh1 118.9(2) . . ? C1 P1 Rh1 113.7(2) . . ? C10 P2 C15 101.7(4) . . yes C10 P2 C3 101.8(3) . . yes C15 P2 C3 102.9(3) . . yes C10 P2 Rh2 119.2(2) . . ? C15 P2 Rh2 116.9(3) . . ? C3 P2 Rh2 112.1(2) . . ? C16A P3 C24 101.2(3) . . yes C16A P3 C19 102.8(3) . . yes C24 P3 C19 101.5(3) . . yes C16A P3 Rh1 111.3(2) . . ? C24 P3 Rh1 117.5(2) . . ? C19 P3 Rh1 120.0(2) . . ? C2 C1 P1 115.0(4) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C1 111.7(5) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C2 C3 P2 113.3(4) . . ? C2 C3 H3A 108.9 . . ? P2 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? P2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 P1 116.0(5) . . ? C5 C4 H4A 108.3 . . ? P1 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? P1 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 115.9(6) . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5B 108.3 . . ? C6 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 118.5(7) . . ? C7 C6 H6A 107.7 . . ? C5 C6 H6A 107.7 . . ? C7 C6 H6B 107.7 . . ? C5 C6 H6B 107.7 . . ? H6A C6 H6B 107.1 . . ? C6 C7 C8 115.1(7) . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C9 114.6(6) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 P1 117.6(5) . . ? C8 C9 H9A 107.9 . . ? P1 C9 H9A 107.9 . . ? C8 C9 H9B 107.9 . . ? P1 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C11 C10 P2 116.2(5) . . ? C11 C10 H10A 108.2 . . ? P2 C10 H10A 108.2 . . ? C11 C10 H10B 108.2 . . ? P2 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C10 115.7(6) . . ? C12 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? C11 C12 C13 115.5(6) . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C12 C13 C14 116.6(7) . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C15 115.1(6) . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14B 108.5 . . ? C15 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 P2 114.0(5) . . ? C14 C15 H15A 108.8 . . ? P2 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? P2 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17A C16A P3 127.5(9) . . ? C17A C16A H16A 105.4 . . ? P3 C16A H16A 105.4 . . ? C17A C16A H16B 105.4 . . ? P3 C16A H16B 105.4 . . ? H16A C16A H16B 106.0 . . ? C16A C17A C18A 105.5(13) . . ? C16A C17A H17A 110.6 . . ? C18A C17A H17A 110.6 . . ? C16A C17A H17B 110.6 . . ? C18A C17A H17B 110.6 . . ? H17A C17A H17B 108.8 . . ? C17A C18A P4A 114.2(10) . . ? C17A C18A H18A 108.7 . . ? P4A C18A H18A 108.7 . . ? C17A C18A H18B 108.7 . . ? P4A C18A H18B 108.7 . . ? H18A C18A H18B 107.6 . . ? C18B C17B H17C 109.8 . . ? C18B C17B H17D 109.8 . . ? H17C C17B H17D 108.2 . . ? C17B C18B P4B 112.9(9) . . ? C17B C18B H18C 109.0 . . ? P4B C18B H18C 109.0 . . ? C17B C18B H18D 109.0 . . ? P4B C18B H18D 109.0 . . ? H18C C18B H18D 107.8 . . ? C20 C19 P3 116.8(4) . . ? C20 C19 H19A 108.1 . . ? P3 C19 H19A 108.1 . . ? C20 C19 H19B 108.1 . . ? P3 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? C21 C20 C19 117.0(6) . . ? C21 C20 H20A 108.1 . . ? C19 C20 H20A 108.1 . . ? C21 C20 H20B 108.1 . . ? C19 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 C21 C22 113.2(6) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 116.6(6) . . ? C23 C22 H22A 108.1 . . ? C21 C22 H22A 108.1 . . ? C23 C22 H22B 108.1 . . ? C21 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C24 C23 C22 115.7(5) . . ? C24 C23 H23A 108.4 . . ? C22 C23 H23A 108.4 . . ? C24 C23 H23B 108.4 . . ? C22 C23 H23B 108.4 . . ? H23A C23 H23B 107.4 . . ? C23 C24 P3 116.4(5) . . ? C23 C24 H24A 108.2 . . ? P3 C24 H24A 108.2 . . ? C23 C24 H24B 108.2 . . ? P3 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? O2 C32 Rh2 177.5(7) . . ? C30A P4A C25A 101.5(19) . . yes C30A P4A C18A 101.7(13) . . yes C25A P4A C18A 106.5(10) . . yes C30A P4A Rh2 119.2(18) . . ? C25A P4A Rh2 113.5(7) . . ? C18A P4A Rh2 112.9(7) . . ? C26A C25A P4A 117.6(13) . . ? C26A C25A H25A 107.9 . . ? P4A C25A H25A 107.9 . . ? C26A C25A H25B 107.9 . . ? P4A C25A H25B 107.9 . . ? H25A C25A H25B 107.2 . . ? C25A C26A C27A 113.1(16) . . ? C25A C26A H26A 109.0 . . ? C27A C26A H26A 109.0 . . ? C25A C26A H26B 109.0 . . ? C27A C26A H26B 109.0 . . ? H26A C26A H26B 107.8 . . ? C28A C27A C26A 116.8(18) . . ? C28A C27A H27A 108.1 . . ? C26A C27A H27A 108.1 . . ? C28A C27A H27B 108.1 . . ? C26A C27A H27B 108.1 . . ? H27A C27A H27B 107.3 . . ? C27A C28A C29A 116(2) . . ? C27A C28A H28A 108.4 . . ? C29A C28A H28A 108.4 . . ? C27A C28A H28B 108.4 . . ? C29A C28A H28B 108.4 . . ? H28A C28A H28B 107.4 . . ? C28A C29A C30A 118(3) . . ? C28A C29A H29A 107.7 . . ? C30A C29A H29A 107.7 . . ? C28A C29A H29B 107.7 . . ? C30A C29A H29B 107.7 . . ? H29A C29A H29B 107.1 . . ? C29A C30A P4A 120(3) . . ? C29A C30A H30A 107.2 . . ? P4A C30A H30A 107.2 . . ? C29A C30A H30B 107.2 . . ? P4A C30A H30B 107.2 . . ? H30A C30A H30B 106.9 . . ? C25B P4B C18B 104.2(8) . . yes C25B P4B C30B 101.8(14) . . yes C18B P4B C30B 101.9(10) . . yes C25B P4B Rh2 119.1(6) . . ? C18B P4B Rh2 109.0(5) . . ? C30B P4B Rh2 118.7(14) . . ? C26B C25B P4B 116.4(12) . . ? C26B C25B H25C 108.2 . . ? P4B C25B H25C 108.2 . . ? C26B C25B H25D 108.2 . . ? P4B C25B H25D 108.2 . . ? H25C C25B H25D 107.3 . . ? C27B C26B C25B 114.5(13) . . ? C27B C26B H26C 108.6 . . ? C25B C26B H26C 108.6 . . ? C27B C26B H26D 108.6 . . ? C25B C26B H26D 108.6 . . ? H26C C26B H26D 107.6 . . ? C26B C27B C28B 117.7(16) . . ? C26B C27B H27C 107.9 . . ? C28B C27B H27C 107.9 . . ? C26B C27B H27D 107.9 . . ? C28B C27B H27D 107.9 . . ? H27C C27B H27D 107.2 . . ? C29B C28B C27B 114(2) . . ? C29B C28B H28C 108.7 . . ? C27B C28B H28C 108.7 . . ? C29B C28B H28D 108.7 . . ? C27B C28B H28D 108.7 . . ? H28C C28B H28D 107.6 . . ? C28B C29B C30B 116(2) . . ? C28B C29B H29C 108.2 . . ? C30B C29B H29C 108.2 . . ? C28B C29B H29D 108.2 . . ? C30B C29B H29D 108.2 . . ? H29C C29B H29D 107.4 . . ? C29B C30B P4B 112(2) . . ? C29B C30B H30C 109.2 . . ? P4B C30B H30C 109.2 . . ? C29B C30B H30D 109.2 . . ? P4B C30B H30D 109.2 . . ? H30C C30B H30D 107.9 . . ? O1 C31 Rh1 175.5(11) . . ? 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 C31 Rh1 P1 C4 -142.9(4) . . . . ? Cl1 Rh1 P1 C4 37.0(3) . . . . ? C31 Rh1 P1 C9 -20.9(4) . . . . ? Cl1 Rh1 P1 C9 159.1(3) . . . . ? C31 Rh1 P1 C1 96.0(4) . . . . ? Cl1 Rh1 P1 C1 -84.1(2) . . . . ? C32 Rh2 P2 C10 -17.7(3) . . . . ? Cl2 Rh2 P2 C10 162.4(3) . . . . ? C32 Rh2 P2 C15 -140.6(4) . . . . ? Cl2 Rh2 P2 C15 39.4(3) . . . . ? C32 Rh2 P2 C3 101.0(3) . . . . ? Cl2 Rh2 P2 C3 -79.0(2) . . . . ? C31 Rh1 P3 C16A -87.2(4) . . . . ? Cl1 Rh1 P3 C16A 92.8(3) . . . . ? C31 Rh1 P3 C24 28.8(4) . . . . ? Cl1 Rh1 P3 C24 -151.2(3) . . . . ? C31 Rh1 P3 C19 152.8(3) . . . . ? Cl1 Rh1 P3 C19 -27.1(2) . . . . ? C4 P1 C1 C2 -78.3(5) . . . . ? C9 P1 C1 C2 176.8(5) . . . . ? Rh1 P1 C1 C2 49.2(6) . . . . ? P1 C1 C2 C3 -177.3(4) . . . . ? C1 C2 C3 P2 -176.5(4) . . . . ? C10 P2 C3 C2 79.5(5) . . . . ? C15 P2 C3 C2 -175.4(5) . . . . ? Rh2 P2 C3 C2 -49.0(5) . . . . ? C9 P1 C4 C5 -80.8(6) . . . . ? C1 P1 C4 C5 175.9(5) . . . . ? Rh1 P1 C4 C5 49.9(6) . . . . ? P1 C4 C5 C6 37.2(9) . . . . ? C4 C5 C6 C7 46.2(11) . . . . ? C5 C6 C7 C8 -94.1(9) . . . . ? C6 C7 C8 C9 72.0(9) . . . . ? C7 C8 C9 P1 -59.2(8) . . . . ? C4 P1 C9 C8 71.6(6) . . . . ? C1 P1 C9 C8 178.7(6) . . . . ? Rh1 P1 C9 C8 -57.3(7) . . . . ? C15 P2 C10 C11 70.8(5) . . . . ? C3 P2 C10 C11 176.9(5) . . . . ? Rh2 P2 C10 C11 -59.3(6) . . . . ? P2 C10 C11 C12 -56.2(8) . . . . ? C10 C11 C12 C13 72.1(9) . . . . ? C11 C12 C13 C14 -95.4(8) . . . . ? C12 C13 C14 C15 44.1(10) . . . . ? C13 C14 C15 P2 40.5(9) . . . . ? C10 P2 C15 C14 -85.7(7) . . . . ? C3 P2 C15 C14 169.2(6) . . . . ? Rh2 P2 C15 C14 45.9(7) . . . . ? C24 P3 C16A C17A -164.3(11) . . . . ? C19 P3 C16A C17A 91.0(11) . . . . ? Rh1 P3 C16A C17A -38.7(12) . . . . ? P3 C16A C17A C18A -80.5(13) . . . . ? C16A C17A C18A P4A -173.9(10) . . . . ? C16A P3 C19 C20 172.8(5) . . . . ? C24 P3 C19 C20 68.4(6) . . . . ? Rh1 P3 C19 C20 -63.1(5) . . . . ? P3 C19 C20 C21 -58.0(8) . . . . ? C19 C20 C21 C22 72.9(8) . . . . ? C20 C21 C22 C23 -95.1(8) . . . . ? C21 C22 C23 C24 46.2(8) . . . . ? C22 C23 C24 P3 39.0(8) . . . . ? C16A P3 C24 C23 171.6(5) . . . . ? C19 P3 C24 C23 -82.7(6) . . . . ? Rh1 P3 C24 C23 50.3(6) . . . . ? C17A C18A P4A C30A 180(2) . . . . ? C17A C18A P4A C25A 74.0(14) . . . . ? C17A C18A P4A Rh2 -51.2(13) . . . . ? C32 Rh2 P4A C30A 34.0(17) . . . . ? P4B Rh2 P4A C30A -116(3) . . . . ? Cl2 Rh2 P4A C30A -146.1(17) . . . . ? C32 Rh2 P4A C25A 153.5(8) . . . . ? P4B Rh2 P4A C25A 4(2) . . . . ? Cl2 Rh2 P4A C25A -26.6(8) . . . . ? C32 Rh2 P4A C18A -85.2(7) . . . . ? P4B Rh2 P4A C18A 125(3) . . . . ? Cl2 Rh2 P4A C18A 94.8(6) . . . . ? C30A P4A C25A C26A 68(2) . . . . ? C18A P4A C25A C26A 174.4(14) . . . . ? Rh2 P4A C25A C26A -60.8(16) . . . . ? P4A C25A C26A C27A -60(2) . . . . ? C25A C26A C27A C28A 76(2) . . . . ? C26A C27A C28A C29A -94(3) . . . . ? C27A C28A C29A C30A 45(5) . . . . ? C28A C29A C30A P4A 35(6) . . . . ? C25A P4A C30A C29A -76(4) . . . . ? C18A P4A C30A C29A 174(4) . . . . ? Rh2 P4A C30A C29A 49(5) . . . . ? C17B C18B P4B C25B -173.3(10) . . . . ? C17B C18B P4B C30B -67.7(18) . . . . ? C17B C18B P4B Rh2 58.6(11) . . . . ? C32 Rh2 P4B C25B 133.0(8) . . . . ? Cl2 Rh2 P4B C25B -47.1(8) . . . . ? P4A Rh2 P4B C25B 164(3) . . . . ? C32 Rh2 P4B C18B -107.8(5) . . . . ? Cl2 Rh2 P4B C18B 72.1(5) . . . . ? P4A Rh2 P4B C18B -77(2) . . . . ? C32 Rh2 P4B C30B 8.1(11) . . . . ? Cl2 Rh2 P4B C30B -171.9(10) . . . . ? P4A Rh2 P4B C30B 39(2) . . . . ? C18B P4B C25B C26B -168.2(12) . . . . ? C30B P4B C25B C26B 86.1(17) . . . . ? Rh2 P4B C25B C26B -46.6(15) . . . . ? P4B C25B C26B C27B -37.7(18) . . . . ? C25B C26B C27B C28B -49(2) . . . . ? C26B C27B C28B C29B 97(2) . . . . ? C27B C28B C29B C30B -73(4) . . . . ? C28B C29B C30B P4B 59(4) . . . . ? C25B P4B C30B C29B -71(3) . . . . ? C18B P4B C30B C29B -178(2) . . . . ? Rh2 P4B C30B C29B 62(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.617 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.146