data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Mueller, Christian' 'Broeckx, Leen' 'Lutz, Martin' 'Vogt, Dieter' _publ_contact_author_name 'Mueller, Christian' _publ_contact_author_email c.mueller@tue.nl _publ_section_title ; C-H Activation of 2,4,6-Triphenylphosphinine: Unprecedented Formation of Cyclometalated [(P^C)Ir(III)] and [(P^C)Rh(III)] Complexes ; # Attachment '- deposit.cif' data_l0094a _database_code_depnum_ccdc_archive 'CCDC 798976' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H31 Cl Ir P' _chemical_formula_sum 'C33 H31 Cl Ir P' _chemical_formula_weight 686.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.1991(8) _cell_length_b 14.1332(15) _cell_length_c 25.829(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2628.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9915 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.42 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 5.264 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3433 _exptl_absorpt_correction_T_max 0.8571 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31203 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6014 _reflns_number_gt 5582 _reflns_threshold_expression I>2\s(I) _computing_data_collection ApexII _computing_cell_refinement Saint _computing_data_reduction 'Saint, Sadabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0331P)^2^+0.3335P] 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 -0.016(6) _refine_ls_number_reflns 6014 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Ir1 Ir 0.57057(2) 0.397679(12) 0.610293(6) 0.01581(5) Uani 1 1 d . . . Cl1 Cl 0.81916(16) 0.42964(8) 0.55150(5) 0.0258(3) Uani 1 1 d . . . P1 P 0.72830(16) 0.35043(8) 0.68042(4) 0.0168(2) Uani 1 1 d . . . C1 C 0.7604(6) 0.2504(3) 0.71758(17) 0.0180(9) Uani 1 1 d . . . C2 C 0.7837(6) 0.2599(3) 0.77158(17) 0.0200(9) Uani 1 1 d . . . H2 H 0.7970 0.2029 0.7907 0.024 Uiso 1 1 calc R . . C3 C 0.7891(6) 0.3435(3) 0.79975(17) 0.0187(9) Uani 1 1 d . . . C4 C 0.7794(7) 0.4322(3) 0.77518(18) 0.0219(10) Uani 1 1 d . . . H4 H 0.7954 0.4871 0.7959 0.026 Uiso 1 1 calc R . . C5 C 0.7479(6) 0.4446(3) 0.72250(17) 0.0165(9) Uani 1 1 d . . . C6 C 0.7127(6) 0.5340(3) 0.69465(17) 0.0181(9) Uani 1 1 d . . . C7 C 0.6357(7) 0.5266(3) 0.64434(18) 0.0197(10) Uani 1 1 d . . . C8 C 0.6016(6) 0.6106(3) 0.61780(17) 0.0226(9) Uani 1 1 d . . . H8 H 0.5536 0.6078 0.5836 0.027 Uiso 1 1 calc R . . C9 C 0.6360(7) 0.6985(4) 0.64015(19) 0.0246(10) Uani 1 1 d . . . H9 H 0.6081 0.7548 0.6217 0.030 Uiso 1 1 calc R . . C10 C 0.7111(7) 0.7034(3) 0.68944(18) 0.0264(11) Uani 1 1 d . . . H10 H 0.7333 0.7634 0.7049 0.032 Uiso 1 1 calc R . . C11 C 0.7534(7) 0.6222(3) 0.71608(18) 0.0248(11) Uani 1 1 d . . . H11 H 0.8106 0.6260 0.7492 0.030 Uiso 1 1 calc R . . C12 C 0.7681(6) 0.1557(3) 0.69341(17) 0.0185(9) Uani 1 1 d . . . C13 C 0.6836(6) 0.0777(3) 0.71670(19) 0.0225(10) Uani 1 1 d . . . H13 H 0.6181 0.0859 0.7483 0.027 Uiso 1 1 calc R . . C14 C 0.6934(7) -0.0112(4) 0.69469(19) 0.0272(11) Uani 1 1 d . . . H14 H 0.6344 -0.0632 0.7112 0.033 Uiso 1 1 calc R . . C15 C 0.7893(7) -0.0250(3) 0.6484(2) 0.0278(11) Uani 1 1 d . . . H15 H 0.7956 -0.0862 0.6333 0.033 Uiso 1 1 calc R . . C16 C 0.8746(6) 0.0505(4) 0.62492(19) 0.0260(11) Uani 1 1 d . . . H16 H 0.9422 0.0415 0.5937 0.031 Uiso 1 1 calc R . . C17 C 0.8620(7) 0.1403(3) 0.64683(18) 0.0225(10) Uani 1 1 d . . . H17 H 0.9187 0.1923 0.6297 0.027 Uiso 1 1 calc R . . C18 C 0.7996(7) 0.3381(3) 0.85715(18) 0.0225(10) Uani 1 1 d . . . C19 C 0.8947(6) 0.2659(4) 0.88195(19) 0.0273(11) Uani 1 1 d . . . H19 H 0.9577 0.2195 0.8620 0.033 Uiso 1 1 calc R . . C20 C 0.8992(8) 0.2605(4) 0.9360(2) 0.0346(13) Uani 1 1 d . . . H20 H 0.9658 0.2109 0.9525 0.042 Uiso 1 1 calc R . . C21 C 0.8069(9) 0.3270(5) 0.9651(2) 0.0435(16) Uani 1 1 d . . . H21 H 0.8090 0.3229 1.0018 0.052 Uiso 1 1 calc R . . C22 C 0.7120(8) 0.3991(4) 0.94149(19) 0.0381(13) Uani 1 1 d . . . H22 H 0.6491 0.4451 0.9618 0.046 Uiso 1 1 calc R . . C23 C 0.7079(7) 0.4048(4) 0.88781(19) 0.0300(10) Uani 1 1 d . . . H23 H 0.6415 0.4549 0.8717 0.036 Uiso 1 1 calc R . . C24 C 0.3095(6) 0.3321(3) 0.63250(18) 0.0215(10) Uani 1 1 d . . . C25 C 0.3803(6) 0.2737(3) 0.59062(18) 0.0208(10) Uani 1 1 d . . . C26 C 0.3949(6) 0.3313(3) 0.54636(18) 0.0206(10) Uani 1 1 d . . . C27 C 0.3309(6) 0.4256(3) 0.55888(18) 0.0185(10) Uani 1 1 d . . . C28 C 0.2725(6) 0.4249(3) 0.6122(2) 0.0240(10) Uani 1 1 d . . . C29 C 0.2613(7) 0.2986(4) 0.68561(18) 0.0287(11) Uani 1 1 d . . . H29A H 0.2549 0.3528 0.7092 0.043 Uiso 1 1 calc R . . H29B H 0.3566 0.2543 0.6977 0.043 Uiso 1 1 calc R . . H29C H 0.1406 0.2666 0.6848 0.043 Uiso 1 1 calc R . . C30 C 0.4116(8) 0.1685(3) 0.59354(19) 0.0279(11) Uani 1 1 d . . . H30A H 0.2927 0.1355 0.5896 0.042 Uiso 1 1 calc R . . H30B H 0.4665 0.1524 0.6271 0.042 Uiso 1 1 calc R . . H30C H 0.4961 0.1490 0.5658 0.042 Uiso 1 1 calc R . . C31 C 0.4642(7) 0.3028(4) 0.49413(18) 0.0276(11) Uani 1 1 d . . . H31A H 0.5162 0.2388 0.4959 0.041 Uiso 1 1 calc R . . H31B H 0.5606 0.3471 0.4828 0.041 Uiso 1 1 calc R . . H31C H 0.3611 0.3037 0.4694 0.041 Uiso 1 1 calc R . . C32 C 0.3065(7) 0.5044(4) 0.52079(19) 0.0281(11) Uani 1 1 d . . . H32A H 0.4222 0.5135 0.5014 0.042 Uiso 1 1 calc R . . H32B H 0.2752 0.5628 0.5393 0.042 Uiso 1 1 calc R . . H32C H 0.2061 0.4884 0.4967 0.042 Uiso 1 1 calc R . . C33 C 0.1774(7) 0.5052(4) 0.63899(19) 0.0262(11) Uani 1 1 d . . . H33A H 0.0443 0.5037 0.6310 0.039 Uiso 1 1 calc R . . H33B H 0.2303 0.5652 0.6270 0.039 Uiso 1 1 calc R . . H33C H 0.1952 0.4994 0.6765 0.039 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 Ir1 0.01756(7) 0.01749(8) 0.01237(8) -0.00035(7) -0.00076(7) -0.00072(7) Cl1 0.0243(6) 0.0324(6) 0.0207(6) -0.0020(5) 0.0052(5) -0.0052(5) P1 0.0201(5) 0.0170(5) 0.0132(6) -0.0008(4) -0.0022(4) 0.0000(5) C1 0.020(2) 0.021(2) 0.013(2) -0.0003(17) 0.0012(17) 0.0031(18) C2 0.024(2) 0.023(2) 0.013(2) 0.0040(17) -0.0012(18) 0.001(2) C3 0.020(2) 0.026(2) 0.011(2) -0.0021(18) -0.0010(18) -0.004(2) C4 0.026(2) 0.024(2) 0.016(2) -0.0048(18) -0.0011(19) -0.001(2) C5 0.017(2) 0.018(2) 0.015(2) -0.0005(17) 0.0008(17) -0.0018(17) C6 0.017(2) 0.023(2) 0.014(2) -0.0019(18) 0.0042(18) -0.0019(19) C7 0.019(2) 0.024(2) 0.017(2) -0.0036(19) 0.0025(18) 0.0009(19) C8 0.022(2) 0.025(2) 0.021(2) -0.001(2) -0.0012(17) -0.003(2) C9 0.029(2) 0.018(2) 0.026(3) 0.004(2) 0.001(2) 0.002(2) C10 0.036(3) 0.020(2) 0.023(3) -0.009(2) 0.009(2) -0.005(2) C11 0.032(3) 0.026(3) 0.016(2) -0.0020(19) 0.002(2) -0.004(2) C12 0.016(2) 0.026(2) 0.014(2) 0.0001(17) -0.0044(17) 0.0050(19) C13 0.022(2) 0.025(2) 0.020(2) 0.0052(18) -0.0003(19) 0.0020(19) C14 0.030(3) 0.024(2) 0.028(3) 0.007(2) -0.004(2) -0.001(2) C15 0.031(3) 0.018(2) 0.034(3) -0.007(2) -0.007(2) 0.007(2) C16 0.024(2) 0.033(3) 0.021(3) -0.004(2) 0.0005(18) 0.006(2) C17 0.026(2) 0.027(2) 0.015(2) 0.0004(19) 0.0004(19) -0.003(2) C18 0.025(2) 0.028(2) 0.015(2) -0.0029(19) -0.0011(19) -0.010(2) C19 0.025(2) 0.032(3) 0.024(3) 0.003(2) -0.001(2) -0.006(2) C20 0.041(3) 0.040(3) 0.023(3) 0.008(2) -0.012(2) -0.013(3) C21 0.058(4) 0.062(4) 0.010(3) -0.002(3) 0.003(3) -0.026(3) C22 0.055(3) 0.041(3) 0.018(2) -0.015(3) 0.005(2) -0.009(3) C23 0.038(2) 0.031(2) 0.021(2) -0.004(3) 0.000(2) -0.007(2) C24 0.017(2) 0.028(3) 0.019(2) 0.0032(19) -0.0053(18) -0.006(2) C25 0.024(2) 0.019(2) 0.020(2) 0.0057(18) -0.0047(18) -0.0039(18) C26 0.018(2) 0.028(2) 0.015(2) -0.0024(18) -0.0054(18) -0.0042(19) C27 0.015(2) 0.026(2) 0.015(2) -0.0045(17) -0.0023(17) 0.0021(18) C28 0.019(2) 0.031(2) 0.022(2) -0.004(2) 0.000(2) -0.0056(18) C29 0.026(2) 0.041(3) 0.019(2) 0.008(2) 0.001(2) -0.007(2) C30 0.032(3) 0.020(2) 0.032(3) 0.0009(18) -0.010(2) -0.001(2) C31 0.031(3) 0.032(3) 0.019(2) -0.008(2) -0.002(2) 0.003(2) C32 0.031(3) 0.032(3) 0.022(3) 0.003(2) -0.007(2) 0.002(2) C33 0.024(3) 0.030(3) 0.025(3) -0.008(2) 0.002(2) 0.007(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 Ir1 C7 2.076(5) . ? Ir1 C24 2.173(5) . ? Ir1 C28 2.181(5) . ? Ir1 C27 2.213(4) . ? Ir1 P1 2.2396(12) . ? Ir1 C25 2.281(4) . ? Ir1 C26 2.282(4) . ? Ir1 Cl1 2.3902(12) . ? P1 C5 1.724(4) . ? P1 C1 1.724(5) . ? C1 C2 1.411(6) . ? C1 C12 1.479(6) . ? C2 C3 1.389(6) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 C18 1.486(6) . ? C4 C5 1.391(6) . ? C4 H4 0.9500 . ? C5 C6 1.476(6) . ? C6 C11 1.395(6) . ? C6 C7 1.417(6) . ? C7 C8 1.393(6) . ? C8 C9 1.392(7) . ? C8 H8 0.9500 . ? C9 C10 1.385(7) . ? C9 H9 0.9500 . ? C10 C11 1.373(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.395(6) . ? C12 C17 1.397(6) . ? C13 C14 1.380(7) . ? C13 H13 0.9500 . ? C14 C15 1.394(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(7) . ? C15 H15 0.9500 . ? C16 C17 1.391(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.386(7) . ? C18 C23 1.397(7) . ? C19 C20 1.398(7) . ? C19 H19 0.9500 . ? C20 C21 1.375(8) . ? C20 H20 0.9500 . ? C21 C22 1.370(9) . ? C21 H21 0.9500 . ? C22 C23 1.389(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C28 1.438(7) . ? C24 C25 1.452(7) . ? C24 C29 1.492(6) . ? C25 C26 1.407(6) . ? C25 C30 1.507(6) . ? C26 C27 1.447(6) . ? C26 C31 1.493(6) . ? C27 C28 1.440(7) . ? C27 C32 1.496(6) . ? C28 C33 1.495(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ir1 C24 117.26(18) . . ? C7 Ir1 C28 93.32(18) . . ? C24 Ir1 C28 38.57(17) . . ? C7 Ir1 C27 105.90(18) . . ? C24 Ir1 C27 63.90(17) . . ? C28 Ir1 C27 38.26(18) . . ? C7 Ir1 P1 78.72(14) . . ? C24 Ir1 P1 95.62(13) . . ? C28 Ir1 P1 122.22(15) . . ? C27 Ir1 P1 159.05(12) . . ? C7 Ir1 C25 154.65(18) . . ? C24 Ir1 C25 37.97(17) . . ? C28 Ir1 C25 63.24(17) . . ? C27 Ir1 C25 62.29(16) . . ? P1 Ir1 C25 104.81(12) . . ? C7 Ir1 C26 142.43(17) . . ? C24 Ir1 C26 62.36(17) . . ? C28 Ir1 C26 62.86(17) . . ? C27 Ir1 C26 37.53(16) . . ? P1 Ir1 C26 138.04(12) . . ? C25 Ir1 C26 35.91(16) . . ? C7 Ir1 Cl1 86.23(13) . . ? C24 Ir1 Cl1 153.64(13) . . ? C28 Ir1 Cl1 135.88(14) . . ? C27 Ir1 Cl1 99.72(12) . . ? P1 Ir1 Cl1 100.98(4) . . ? C25 Ir1 Cl1 116.95(12) . . ? C26 Ir1 Cl1 91.88(12) . . ? C5 P1 C1 105.7(2) . . ? C5 P1 Ir1 108.75(15) . . ? C1 P1 Ir1 139.71(16) . . ? C2 C1 C12 119.9(4) . . ? C2 C1 P1 119.3(3) . . ? C12 C1 P1 120.8(3) . . ? C3 C2 C1 127.0(4) . . ? C3 C2 H2 116.5 . . ? C1 C2 H2 116.5 . . ? C2 C3 C4 121.4(4) . . ? C2 C3 C18 118.7(4) . . ? C4 C3 C18 119.9(4) . . ? C5 C4 C3 124.2(4) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? C4 C5 C6 127.8(4) . . ? C4 C5 P1 122.2(3) . . ? C6 C5 P1 109.9(3) . . ? C11 C6 C7 120.9(4) . . ? C11 C6 C5 122.4(4) . . ? C7 C6 C5 116.8(4) . . ? C8 C7 C6 117.2(4) . . ? C8 C7 Ir1 120.0(3) . . ? C6 C7 Ir1 122.8(4) . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C6 120.1(4) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? C13 C12 C17 117.3(4) . . ? C13 C12 C1 121.1(4) . . ? C17 C12 C1 121.5(4) . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.4(4) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 121.6(4) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? C19 C18 C23 117.9(4) . . ? C19 C18 C3 121.6(4) . . ? C23 C18 C3 120.5(5) . . ? C18 C19 C20 120.9(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.8(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 121.1(5) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C28 C24 C25 108.2(4) . . ? C28 C24 C29 125.5(5) . . ? C25 C24 C29 125.9(4) . . ? C28 C24 Ir1 71.0(3) . . ? C25 C24 Ir1 75.0(3) . . ? C29 C24 Ir1 125.4(3) . . ? C26 C25 C24 107.7(4) . . ? C26 C25 C30 126.9(4) . . ? C24 C25 C30 125.1(4) . . ? C26 C25 Ir1 72.1(3) . . ? C24 C25 Ir1 67.0(3) . . ? C30 C25 Ir1 131.1(3) . . ? C25 C26 C27 109.1(4) . . ? C25 C26 C31 127.1(4) . . ? C27 C26 C31 123.8(4) . . ? C25 C26 Ir1 72.0(3) . . ? C27 C26 Ir1 68.6(2) . . ? C31 C26 Ir1 125.4(3) . . ? C28 C27 C26 107.5(4) . . ? C28 C27 C32 126.8(4) . . ? C26 C27 C32 125.2(4) . . ? C28 C27 Ir1 69.7(3) . . ? C26 C27 Ir1 73.8(2) . . ? C32 C27 Ir1 128.2(3) . . ? C24 C28 C27 107.5(4) . . ? C24 C28 C33 127.5(5) . . ? C27 C28 C33 124.8(4) . . ? C24 C28 Ir1 70.4(3) . . ? C27 C28 Ir1 72.1(3) . . ? C33 C28 Ir1 126.5(3) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Ir1 P1 C5 14.3(2) . . . . ? C24 Ir1 P1 C5 -102.4(2) . . . . ? C28 Ir1 P1 C5 -72.5(2) . . . . ? C27 Ir1 P1 C5 -90.8(4) . . . . ? C25 Ir1 P1 C5 -139.9(2) . . . . ? C26 Ir1 P1 C5 -156.4(2) . . . . ? Cl1 Ir1 P1 C5 98.17(16) . . . . ? C7 Ir1 P1 C1 161.7(3) . . . . ? C24 Ir1 P1 C1 44.9(3) . . . . ? C28 Ir1 P1 C1 74.9(3) . . . . ? C27 Ir1 P1 C1 56.6(4) . . . . ? C25 Ir1 P1 C1 7.5(3) . . . . ? C26 Ir1 P1 C1 -9.1(3) . . . . ? Cl1 Ir1 P1 C1 -114.5(2) . . . . ? C5 P1 C1 C2 3.6(4) . . . . ? Ir1 P1 C1 C2 -144.4(3) . . . . ? C5 P1 C1 C12 -175.0(4) . . . . ? Ir1 P1 C1 C12 37.1(5) . . . . ? C12 C1 C2 C3 176.7(5) . . . . ? P1 C1 C2 C3 -1.9(7) . . . . ? C1 C2 C3 C4 -3.0(8) . . . . ? C1 C2 C3 C18 175.1(4) . . . . ? C2 C3 C4 C5 5.8(8) . . . . ? C18 C3 C4 C5 -172.3(4) . . . . ? C3 C4 C5 C6 171.7(5) . . . . ? C3 C4 C5 P1 -3.3(7) . . . . ? C1 P1 C5 C4 -1.2(4) . . . . ? Ir1 P1 C5 C4 157.5(3) . . . . ? C1 P1 C5 C6 -177.1(3) . . . . ? Ir1 P1 C5 C6 -18.3(3) . . . . ? C4 C5 C6 C11 17.1(7) . . . . ? P1 C5 C6 C11 -167.4(4) . . . . ? C4 C5 C6 C7 -163.4(4) . . . . ? P1 C5 C6 C7 12.2(5) . . . . ? C11 C6 C7 C8 -0.6(7) . . . . ? C5 C6 C7 C8 179.9(4) . . . . ? C11 C6 C7 Ir1 -179.7(3) . . . . ? C5 C6 C7 Ir1 0.7(6) . . . . ? C24 Ir1 C7 C8 -98.4(4) . . . . ? C28 Ir1 C7 C8 -66.7(4) . . . . ? C27 Ir1 C7 C8 -30.0(4) . . . . ? P1 Ir1 C7 C8 171.1(4) . . . . ? C25 Ir1 C7 C8 -88.1(5) . . . . ? C26 Ir1 C7 C8 -19.1(5) . . . . ? Cl1 Ir1 C7 C8 69.1(3) . . . . ? C24 Ir1 C7 C6 80.7(4) . . . . ? C28 Ir1 C7 C6 112.4(4) . . . . ? C27 Ir1 C7 C6 149.1(4) . . . . ? P1 Ir1 C7 C6 -9.8(4) . . . . ? C25 Ir1 C7 C6 91.0(5) . . . . ? C26 Ir1 C7 C6 160.0(3) . . . . ? Cl1 Ir1 C7 C6 -111.8(4) . . . . ? C6 C7 C8 C9 -1.9(6) . . . . ? Ir1 C7 C8 C9 177.2(4) . . . . ? C7 C8 C9 C10 1.9(7) . . . . ? C8 C9 C10 C11 0.7(7) . . . . ? C9 C10 C11 C6 -3.1(7) . . . . ? C7 C6 C11 C10 3.1(7) . . . . ? C5 C6 C11 C10 -177.4(5) . . . . ? C2 C1 C12 C13 41.3(6) . . . . ? P1 C1 C12 C13 -140.1(4) . . . . ? C2 C1 C12 C17 -137.9(5) . . . . ? P1 C1 C12 C17 40.7(6) . . . . ? C17 C12 C13 C14 0.3(7) . . . . ? C1 C12 C13 C14 -178.9(4) . . . . ? C12 C13 C14 C15 0.2(7) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C14 C15 C16 C17 -1.2(7) . . . . ? C15 C16 C17 C12 1.8(7) . . . . ? C13 C12 C17 C16 -1.3(7) . . . . ? C1 C12 C17 C16 177.9(4) . . . . ? C2 C3 C18 C19 33.6(7) . . . . ? C4 C3 C18 C19 -148.3(5) . . . . ? C2 C3 C18 C23 -144.3(5) . . . . ? C4 C3 C18 C23 33.8(7) . . . . ? C23 C18 C19 C20 -0.3(7) . . . . ? C3 C18 C19 C20 -178.3(5) . . . . ? C18 C19 C20 C21 0.6(8) . . . . ? C19 C20 C21 C22 -0.6(8) . . . . ? C20 C21 C22 C23 0.4(9) . . . . ? C21 C22 C23 C18 -0.2(8) . . . . ? C19 C18 C23 C22 0.1(7) . . . . ? C3 C18 C23 C22 178.1(5) . . . . ? C7 Ir1 C24 C28 57.2(3) . . . . ? C27 Ir1 C24 C28 -38.0(3) . . . . ? P1 Ir1 C24 C28 137.4(3) . . . . ? C25 Ir1 C24 C28 -115.7(4) . . . . ? C26 Ir1 C24 C28 -80.2(3) . . . . ? Cl1 Ir1 C24 C28 -93.6(4) . . . . ? C7 Ir1 C24 C25 172.9(3) . . . . ? C28 Ir1 C24 C25 115.7(4) . . . . ? C27 Ir1 C24 C25 77.7(3) . . . . ? P1 Ir1 C24 C25 -107.0(2) . . . . ? C26 Ir1 C24 C25 35.4(2) . . . . ? Cl1 Ir1 C24 C25 22.1(4) . . . . ? C7 Ir1 C24 C29 -63.4(5) . . . . ? C28 Ir1 C24 C29 -120.6(6) . . . . ? C27 Ir1 C24 C29 -158.6(5) . . . . ? P1 Ir1 C24 C29 16.7(4) . . . . ? C25 Ir1 C24 C29 123.7(5) . . . . ? C26 Ir1 C24 C29 159.1(5) . . . . ? Cl1 Ir1 C24 C29 145.8(3) . . . . ? C28 C24 C25 C26 2.8(5) . . . . ? C29 C24 C25 C26 175.9(4) . . . . ? Ir1 C24 C25 C26 -60.9(3) . . . . ? C28 C24 C25 C30 -171.2(4) . . . . ? C29 C24 C25 C30 1.9(7) . . . . ? Ir1 C24 C25 C30 125.1(5) . . . . ? C28 C24 C25 Ir1 63.8(3) . . . . ? C29 C24 C25 Ir1 -123.1(5) . . . . ? C7 Ir1 C25 C26 104.0(5) . . . . ? C24 Ir1 C25 C26 118.9(4) . . . . ? C28 Ir1 C25 C26 79.9(3) . . . . ? C27 Ir1 C25 C26 36.7(3) . . . . ? P1 Ir1 C25 C26 -161.1(2) . . . . ? Cl1 Ir1 C25 C26 -50.3(3) . . . . ? C7 Ir1 C25 C24 -15.0(5) . . . . ? C28 Ir1 C25 C24 -39.0(3) . . . . ? C27 Ir1 C25 C24 -82.3(3) . . . . ? P1 Ir1 C25 C24 80.0(3) . . . . ? C26 Ir1 C25 C24 -118.9(4) . . . . ? Cl1 Ir1 C25 C24 -169.2(2) . . . . ? C7 Ir1 C25 C30 -132.3(5) . . . . ? C24 Ir1 C25 C30 -117.3(5) . . . . ? C28 Ir1 C25 C30 -156.4(5) . . . . ? C27 Ir1 C25 C30 160.4(5) . . . . ? P1 Ir1 C25 C30 -37.4(5) . . . . ? C26 Ir1 C25 C30 123.7(6) . . . . ? Cl1 Ir1 C25 C30 73.4(4) . . . . ? C24 C25 C26 C27 -1.1(5) . . . . ? C30 C25 C26 C27 172.8(4) . . . . ? Ir1 C25 C26 C27 -58.8(3) . . . . ? C24 C25 C26 C31 178.9(4) . . . . ? C30 C25 C26 C31 -7.2(7) . . . . ? Ir1 C25 C26 C31 121.2(4) . . . . ? C24 C25 C26 Ir1 57.7(3) . . . . ? C30 C25 C26 Ir1 -128.4(5) . . . . ? C7 Ir1 C26 C25 -137.1(3) . . . . ? C24 Ir1 C26 C25 -37.4(3) . . . . ? C28 Ir1 C26 C25 -81.1(3) . . . . ? C27 Ir1 C26 C25 -119.7(4) . . . . ? P1 Ir1 C26 C25 27.9(3) . . . . ? Cl1 Ir1 C26 C25 136.7(3) . . . . ? C7 Ir1 C26 C27 -17.3(4) . . . . ? C24 Ir1 C26 C27 82.3(3) . . . . ? C28 Ir1 C26 C27 38.6(3) . . . . ? P1 Ir1 C26 C27 147.7(2) . . . . ? C25 Ir1 C26 C27 119.7(4) . . . . ? Cl1 Ir1 C26 C27 -103.6(2) . . . . ? C7 Ir1 C26 C31 99.8(5) . . . . ? C24 Ir1 C26 C31 -160.6(5) . . . . ? C28 Ir1 C26 C31 155.7(5) . . . . ? C27 Ir1 C26 C31 117.1(5) . . . . ? P1 Ir1 C26 C31 -95.2(4) . . . . ? C25 Ir1 C26 C31 -123.2(5) . . . . ? Cl1 Ir1 C26 C31 13.5(4) . . . . ? C25 C26 C27 C28 -1.0(5) . . . . ? C31 C26 C27 C28 178.9(4) . . . . ? Ir1 C26 C27 C28 -61.9(3) . . . . ? C25 C26 C27 C32 -173.4(4) . . . . ? C31 C26 C27 C32 6.6(7) . . . . ? Ir1 C26 C27 C32 125.7(5) . . . . ? C25 C26 C27 Ir1 60.9(3) . . . . ? C31 C26 C27 Ir1 -119.2(4) . . . . ? C7 Ir1 C27 C28 -74.7(3) . . . . ? C24 Ir1 C27 C28 38.3(3) . . . . ? P1 Ir1 C27 C28 25.4(5) . . . . ? C25 Ir1 C27 C28 81.1(3) . . . . ? C26 Ir1 C27 C28 116.2(4) . . . . ? Cl1 Ir1 C27 C28 -163.5(2) . . . . ? C7 Ir1 C27 C26 169.1(3) . . . . ? C24 Ir1 C27 C26 -77.9(3) . . . . ? C28 Ir1 C27 C26 -116.2(4) . . . . ? P1 Ir1 C27 C26 -90.8(4) . . . . ? C25 Ir1 C27 C26 -35.1(2) . . . . ? Cl1 Ir1 C27 C26 80.3(2) . . . . ? C7 Ir1 C27 C32 46.8(4) . . . . ? C24 Ir1 C27 C32 159.8(5) . . . . ? C28 Ir1 C27 C32 121.5(5) . . . . ? P1 Ir1 C27 C32 146.9(3) . . . . ? C25 Ir1 C27 C32 -157.5(5) . . . . ? C26 Ir1 C27 C32 -122.3(5) . . . . ? Cl1 Ir1 C27 C32 -42.0(4) . . . . ? C25 C24 C28 C27 -3.5(5) . . . . ? C29 C24 C28 C27 -176.6(4) . . . . ? Ir1 C24 C28 C27 62.9(3) . . . . ? C25 C24 C28 C33 172.0(4) . . . . ? C29 C24 C28 C33 -1.1(7) . . . . ? Ir1 C24 C28 C33 -121.5(5) . . . . ? C25 C24 C28 Ir1 -66.4(3) . . . . ? C29 C24 C28 Ir1 120.5(5) . . . . ? C26 C27 C28 C24 2.8(5) . . . . ? C32 C27 C28 C24 174.9(4) . . . . ? Ir1 C27 C28 C24 -61.9(3) . . . . ? C26 C27 C28 C33 -172.9(4) . . . . ? C32 C27 C28 C33 -0.7(7) . . . . ? Ir1 C27 C28 C33 122.5(4) . . . . ? C26 C27 C28 Ir1 64.7(3) . . . . ? C32 C27 C28 Ir1 -123.2(5) . . . . ? C7 Ir1 C28 C24 -131.5(3) . . . . ? C27 Ir1 C28 C24 116.8(4) . . . . ? P1 Ir1 C28 C24 -52.8(3) . . . . ? C25 Ir1 C28 C24 38.4(3) . . . . ? C26 Ir1 C28 C24 78.9(3) . . . . ? Cl1 Ir1 C28 C24 140.5(2) . . . . ? C7 Ir1 C28 C27 111.7(3) . . . . ? C24 Ir1 C28 C27 -116.8(4) . . . . ? P1 Ir1 C28 C27 -169.6(2) . . . . ? C25 Ir1 C28 C27 -78.4(3) . . . . ? C26 Ir1 C28 C27 -37.9(3) . . . . ? Cl1 Ir1 C28 C27 23.7(3) . . . . ? C7 Ir1 C28 C33 -8.8(5) . . . . ? C24 Ir1 C28 C33 122.8(6) . . . . ? C27 Ir1 C28 C33 -120.5(5) . . . . ? P1 Ir1 C28 C33 70.0(5) . . . . ? C25 Ir1 C28 C33 161.1(5) . . . . ? C26 Ir1 C28 C33 -158.4(5) . . . . ? Cl1 Ir1 C28 C33 -96.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.982 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.121 #===END data_l0121a _database_code_depnum_ccdc_archive 'CCDC 798977' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H31 Cl P Rh' _chemical_formula_sum 'C33 H31 Cl P Rh' _chemical_formula_weight 596.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 7.33421(12) _cell_length_b 16.3287(4) _cell_length_c 22.9799(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.867(1) _cell_angle_gamma 90.00 _cell_volume 2719.14(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 46565 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6694 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49748 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6249 _reflns_number_gt 5694 _reflns_threshold_expression I>2\s(I) _computing_data_collection Apex _computing_cell_refinement Peakref _computing_data_reduction 'Eval15, Sadabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0275P)^2^+1.7007P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6249 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.661361(15) 0.201389(7) 0.228568(5) 0.02121(4) Uani 1 1 d . . . Cl1 Cl 0.95641(5) 0.13662(2) 0.25145(2) 0.03424(10) Uani 1 1 d . . . P1 P 0.72433(5) 0.28456(2) 0.158121(18) 0.02258(8) Uani 1 1 d . . . C1 C 0.7193(2) 0.29211(9) 0.08334(7) 0.0252(3) Uani 1 1 d . . . C2 C 0.7452(2) 0.36826(10) 0.05838(7) 0.0273(3) Uani 1 1 d . . . H2 H 0.7375 0.3698 0.0167 0.033 Uiso 1 1 calc R . . C3 C 0.7812(2) 0.44269(9) 0.08810(7) 0.0260(3) Uani 1 1 d . . . C4 C 0.8020(2) 0.44703(9) 0.14991(7) 0.0252(3) Uani 1 1 d . . . H4 H 0.8317 0.4986 0.1681 0.030 Uiso 1 1 calc R . . C5 C 0.7817(2) 0.38032(9) 0.18580(7) 0.0227(3) Uani 1 1 d . . . C6 C 0.8114(2) 0.37689(9) 0.25055(7) 0.0231(3) Uani 1 1 d . . . C7 C 0.8872(2) 0.44228(10) 0.28551(8) 0.0313(3) Uani 1 1 d . . . H7 H 0.9098 0.4930 0.2676 0.038 Uiso 1 1 calc R . . C8 C 0.9292(3) 0.43357(11) 0.34578(8) 0.0362(4) Uani 1 1 d . . . H8 H 0.9803 0.4782 0.3693 0.043 Uiso 1 1 calc R . . C9 C 0.8968(3) 0.35975(11) 0.37197(8) 0.0357(4) Uani 1 1 d . . . H9 H 0.9273 0.3535 0.4134 0.043 Uiso 1 1 calc R . . C10 C 0.8198(2) 0.29470(10) 0.33767(7) 0.0295(3) Uani 1 1 d . . . H10 H 0.7983 0.2444 0.3563 0.035 Uiso 1 1 calc R . . C11 C 0.7733(2) 0.30133(9) 0.27666(7) 0.0230(3) Uani 1 1 d . . . C12 C 0.6916(2) 0.21693(10) 0.04672(7) 0.0283(3) Uani 1 1 d . . . C13 C 0.7861(3) 0.14535(11) 0.06487(8) 0.0369(4) Uani 1 1 d . . . H13 H 0.8700 0.1447 0.1008 0.044 Uiso 1 1 calc R . . C14 C 0.7589(3) 0.07493(12) 0.03105(9) 0.0476(5) Uani 1 1 d . . . H14 H 0.8250 0.0264 0.0436 0.057 Uiso 1 1 calc R . . C15 C 0.6364(4) 0.07509(12) -0.02075(9) 0.0504(5) Uani 1 1 d . . . H15 H 0.6186 0.0268 -0.0440 0.061 Uiso 1 1 calc R . . C16 C 0.5397(3) 0.14498(13) -0.03891(8) 0.0472(5) Uani 1 1 d . . . H16 H 0.4532 0.1445 -0.0742 0.057 Uiso 1 1 calc R . . C17 C 0.5681(3) 0.21643(11) -0.00588(8) 0.0368(4) Uani 1 1 d . . . H17 H 0.5032 0.2650 -0.0191 0.044 Uiso 1 1 calc R . . C18 C 0.8014(2) 0.51840(10) 0.05307(7) 0.0271(3) Uani 1 1 d . . . C19 C 0.8959(3) 0.58682(10) 0.07810(8) 0.0343(4) Uani 1 1 d . . . H19 H 0.9478 0.5860 0.1186 0.041 Uiso 1 1 calc R . . C20 C 0.9153(3) 0.65626(12) 0.04474(9) 0.0411(4) Uani 1 1 d . . . H20 H 0.9803 0.7023 0.0627 0.049 Uiso 1 1 calc R . . C21 C 0.8414(3) 0.65925(11) -0.01416(8) 0.0373(4) Uani 1 1 d . . . H21 H 0.8564 0.7067 -0.0368 0.045 Uiso 1 1 calc R . . C22 C 0.7453(3) 0.59246(12) -0.03982(8) 0.0389(4) Uani 1 1 d . . . H22 H 0.6933 0.5940 -0.0803 0.047 Uiso 1 1 calc R . . C23 C 0.7245(3) 0.52318(11) -0.00657(8) 0.0353(4) Uani 1 1 d . . . H23 H 0.6565 0.4779 -0.0246 0.042 Uiso 1 1 calc R . . C24 C 0.3648(2) 0.20920(9) 0.21673(7) 0.0258(3) Uani 1 1 d . . . C25 C 0.4053(2) 0.14024(10) 0.18121(8) 0.0282(3) Uani 1 1 d . . . C26 C 0.5038(2) 0.08249(10) 0.21828(9) 0.0353(4) Uani 1 1 d . . . C27 C 0.5170(2) 0.11250(12) 0.27830(8) 0.0385(4) Uani 1 1 d . . . C28 C 0.4227(2) 0.18863(12) 0.27696(8) 0.0325(4) Uani 1 1 d . . . C29 C 0.2491(3) 0.28212(11) 0.19557(10) 0.0406(4) Uani 1 1 d . . . H29A H 0.1196 0.2707 0.1984 0.061 Uiso 1 1 calc R . . H29B H 0.2612 0.2936 0.1545 0.061 Uiso 1 1 calc R . . H29C H 0.2910 0.3298 0.2200 0.061 Uiso 1 1 calc R . . C30 C 0.3438(3) 0.13313(14) 0.11599(8) 0.0429(5) Uani 1 1 d . . . H30A H 0.4323 0.0995 0.0986 0.064 Uiso 1 1 calc R . . H30B H 0.3373 0.1878 0.0982 0.064 Uiso 1 1 calc R . . H30C H 0.2217 0.1074 0.1085 0.064 Uiso 1 1 calc R . . C31 C 0.5784(3) 0.00238(12) 0.19982(13) 0.0583(7) Uani 1 1 d . . . H31A H 0.4954 -0.0421 0.2073 0.087 Uiso 1 1 calc R . . H31B H 0.7011 -0.0072 0.2224 0.087 Uiso 1 1 calc R . . H31C H 0.5872 0.0043 0.1577 0.087 Uiso 1 1 calc R . . C32 C 0.6042(3) 0.06583(17) 0.33155(12) 0.0683(8) Uani 1 1 d . . . H32A H 0.6212 0.1023 0.3659 0.102 Uiso 1 1 calc R . . H32B H 0.7243 0.0446 0.3249 0.102 Uiso 1 1 calc R . . H32C H 0.5241 0.0201 0.3387 0.102 Uiso 1 1 calc R . . C33 C 0.3803(3) 0.23771(18) 0.32788(9) 0.0558(6) Uani 1 1 d . . . H33A H 0.4079 0.2955 0.3218 0.084 Uiso 1 1 calc R . . H33B H 0.4558 0.2181 0.3641 0.084 Uiso 1 1 calc R . . H33C H 0.2494 0.2317 0.3312 0.084 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 Rh1 0.02037(7) 0.01582(6) 0.02681(7) 0.00164(4) 0.00165(5) -0.00202(4) Cl1 0.02448(18) 0.02073(18) 0.0557(3) 0.00173(16) 0.00040(17) 0.00225(14) P1 0.02502(19) 0.01718(17) 0.02551(19) -0.00020(14) 0.00384(15) -0.00180(14) C1 0.0263(7) 0.0218(7) 0.0279(8) -0.0016(6) 0.0053(6) -0.0008(6) C2 0.0303(8) 0.0254(8) 0.0270(8) 0.0008(6) 0.0066(6) -0.0013(6) C3 0.0255(7) 0.0213(7) 0.0314(8) 0.0033(6) 0.0054(6) 0.0002(6) C4 0.0264(7) 0.0178(7) 0.0315(8) 0.0002(6) 0.0049(6) -0.0001(6) C5 0.0223(7) 0.0178(7) 0.0282(7) -0.0009(6) 0.0047(6) 0.0002(5) C6 0.0224(7) 0.0193(7) 0.0276(7) -0.0012(6) 0.0039(6) 0.0004(5) C7 0.0382(9) 0.0201(7) 0.0360(9) -0.0030(6) 0.0066(7) -0.0057(7) C8 0.0436(10) 0.0286(8) 0.0350(9) -0.0083(7) 0.0021(8) -0.0081(7) C9 0.0412(10) 0.0369(9) 0.0272(8) -0.0023(7) -0.0008(7) -0.0046(8) C10 0.0321(8) 0.0264(8) 0.0292(8) 0.0023(6) 0.0022(7) -0.0040(6) C11 0.0214(7) 0.0198(7) 0.0278(7) -0.0009(5) 0.0032(6) -0.0009(5) C12 0.0348(9) 0.0240(7) 0.0276(8) -0.0021(6) 0.0093(7) -0.0040(6) C13 0.0448(10) 0.0283(9) 0.0370(9) -0.0048(7) 0.0046(8) 0.0025(7) C14 0.0695(14) 0.0266(9) 0.0470(11) -0.0060(8) 0.0102(10) 0.0047(9) C15 0.0883(17) 0.0294(9) 0.0354(10) -0.0106(8) 0.0149(10) -0.0105(10) C16 0.0746(15) 0.0402(11) 0.0253(8) -0.0037(8) 0.0029(9) -0.0140(10) C17 0.0529(11) 0.0309(9) 0.0262(8) 0.0005(7) 0.0052(8) -0.0054(8) C18 0.0284(8) 0.0214(7) 0.0319(8) 0.0041(6) 0.0057(6) 0.0005(6) C19 0.0412(9) 0.0274(8) 0.0319(8) 0.0072(7) -0.0020(7) -0.0046(7) C20 0.0506(11) 0.0277(9) 0.0420(10) 0.0067(8) -0.0020(8) -0.0097(8) C21 0.0432(10) 0.0290(9) 0.0396(9) 0.0131(7) 0.0056(8) -0.0009(7) C22 0.0488(11) 0.0368(10) 0.0301(9) 0.0078(7) 0.0024(8) -0.0017(8) C23 0.0447(10) 0.0287(8) 0.0316(8) 0.0029(7) 0.0031(7) -0.0054(7) C24 0.0205(7) 0.0245(7) 0.0323(8) 0.0001(6) 0.0038(6) -0.0033(6) C25 0.0222(7) 0.0247(8) 0.0370(9) -0.0044(6) 0.0023(6) -0.0065(6) C26 0.0238(8) 0.0208(8) 0.0602(12) 0.0027(7) 0.0026(7) -0.0066(6) C27 0.0254(8) 0.0420(10) 0.0456(10) 0.0219(8) -0.0029(7) -0.0129(7) C28 0.0237(8) 0.0434(10) 0.0306(8) -0.0015(7) 0.0046(6) -0.0125(7) C29 0.0283(9) 0.0320(9) 0.0609(12) 0.0043(9) 0.0047(8) 0.0039(7) C30 0.0363(10) 0.0540(12) 0.0368(10) -0.0130(9) 0.0009(8) -0.0123(9) C31 0.0358(10) 0.0202(9) 0.116(2) -0.0027(11) 0.0033(12) -0.0029(8) C32 0.0432(12) 0.0790(18) 0.0754(16) 0.0538(14) -0.0141(11) -0.0231(12) C33 0.0432(11) 0.0912(18) 0.0362(10) -0.0221(11) 0.0159(9) -0.0236(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C11 2.0687(15) . ? Rh1 C24 2.1536(16) . ? Rh1 C27 2.2150(16) . ? Rh1 P1 2.2156(4) . ? Rh1 C28 2.2236(16) . ? Rh1 C26 2.2531(16) . ? Rh1 C25 2.2533(15) . ? Rh1 Cl1 2.3931(4) . ? P1 C5 1.7160(15) . ? P1 C1 1.7176(17) . ? C1 C2 1.394(2) . ? C1 C12 1.485(2) . ? C2 C3 1.399(2) . ? C2 H2 0.9500 . ? C3 C4 1.407(2) . ? C3 C18 1.495(2) . ? C4 C5 1.388(2) . ? C4 H4 0.9500 . ? C5 C6 1.471(2) . ? C6 C7 1.399(2) . ? C6 C11 1.418(2) . ? C7 C8 1.379(2) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(2) . ? C9 H9 0.9500 . ? C10 C11 1.395(2) . ? C10 H10 0.9500 . ? C12 C13 1.390(2) . ? C12 C17 1.394(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.376(3) . ? C14 H14 0.9500 . ? C15 C16 1.374(3) . ? C15 H15 0.9500 . ? C16 C17 1.390(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.391(2) . ? C18 C23 1.402(2) . ? C19 C20 1.388(2) . ? C19 H19 0.9500 . ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C28 1.424(2) . ? C24 C25 1.448(2) . ? C24 C29 1.499(2) . ? C25 C26 1.395(2) . ? C25 C30 1.502(2) . ? C26 C27 1.453(3) . ? C26 C31 1.504(3) . ? C27 C28 1.421(3) . ? C27 C32 1.499(3) . ? C28 C33 1.490(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 C24 109.32(6) . . ? C11 Rh1 C27 115.04(7) . . ? C24 Rh1 C27 63.28(6) . . ? C11 Rh1 P1 78.26(4) . . ? C24 Rh1 P1 101.04(4) . . ? C27 Rh1 P1 161.56(5) . . ? C11 Rh1 C28 94.88(6) . . ? C24 Rh1 C28 37.93(6) . . ? C27 Rh1 C28 37.33(7) . . ? P1 Rh1 C28 133.77(5) . . ? C11 Rh1 C26 152.97(7) . . ? C24 Rh1 C26 63.01(6) . . ? C27 Rh1 C26 37.94(7) . . ? P1 Rh1 C26 127.79(5) . . ? C28 Rh1 C26 62.69(7) . . ? C11 Rh1 C25 147.17(6) . . ? C24 Rh1 C25 38.28(6) . . ? C27 Rh1 C25 61.96(6) . . ? P1 Rh1 C25 99.83(5) . . ? C28 Rh1 C25 62.51(6) . . ? C26 Rh1 C25 36.08(6) . . ? C11 Rh1 Cl1 87.71(4) . . ? C24 Rh1 Cl1 156.25(4) . . ? C27 Rh1 Cl1 94.87(5) . . ? P1 Rh1 Cl1 98.521(15) . . ? C28 Rh1 Cl1 127.12(5) . . ? C26 Rh1 Cl1 94.24(5) . . ? C25 Rh1 Cl1 124.63(4) . . ? C5 P1 C1 105.76(7) . . ? C5 P1 Rh1 110.77(5) . . ? C1 P1 Rh1 143.17(5) . . ? C2 C1 C12 121.30(14) . . ? C2 C1 P1 119.50(12) . . ? C12 C1 P1 119.19(11) . . ? C1 C2 C3 126.95(15) . . ? C1 C2 H2 116.5 . . ? C3 C2 H2 116.5 . . ? C2 C3 C4 121.30(14) . . ? C2 C3 C18 118.85(14) . . ? C4 C3 C18 119.84(14) . . ? C5 C4 C3 123.75(14) . . ? C5 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? C4 C5 C6 128.18(14) . . ? C4 C5 P1 122.51(12) . . ? C6 C5 P1 109.25(11) . . ? C7 C6 C11 120.50(15) . . ? C7 C6 C5 122.39(14) . . ? C11 C6 C5 116.93(13) . . ? C8 C7 C6 120.38(15) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 119.98(16) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.07(16) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 121.71(15) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 117.33(14) . . ? C10 C11 Rh1 119.41(11) . . ? C6 C11 Rh1 123.23(11) . . ? C13 C12 C17 118.85(16) . . ? C13 C12 C1 120.47(15) . . ? C17 C12 C1 120.68(15) . . ? C14 C13 C12 120.53(18) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.13(19) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.11(18) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.32(19) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.05(18) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 C23 117.34(15) . . ? C19 C18 C3 121.72(15) . . ? C23 C18 C3 120.94(15) . . ? C20 C19 C18 120.96(16) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.84(17) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.26(16) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 120.09(17) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 121.49(17) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C28 C24 C25 107.95(14) . . ? C28 C24 C29 124.87(16) . . ? C25 C24 C29 126.15(16) . . ? C28 C24 Rh1 73.70(9) . . ? C25 C24 Rh1 74.58(9) . . ? C29 C24 Rh1 126.73(11) . . ? C26 C25 C24 108.25(15) . . ? C26 C25 C30 127.21(17) . . ? C24 C25 C30 124.51(16) . . ? C26 C25 Rh1 71.95(9) . . ? C24 C25 Rh1 67.13(8) . . ? C30 C25 Rh1 128.04(12) . . ? C25 C26 C27 107.71(16) . . ? C25 C26 C31 126.3(2) . . ? C27 C26 C31 125.96(19) . . ? C25 C26 Rh1 71.97(9) . . ? C27 C26 Rh1 69.61(9) . . ? C31 C26 Rh1 125.19(12) . . ? C28 C27 C26 108.28(15) . . ? C28 C27 C32 127.4(2) . . ? C26 C27 C32 124.1(2) . . ? C28 C27 Rh1 71.66(9) . . ? C26 C27 Rh1 72.45(9) . . ? C32 C27 Rh1 125.23(13) . . ? C27 C28 C24 107.38(15) . . ? C27 C28 C33 127.84(19) . . ? C24 C28 C33 124.71(19) . . ? C27 C28 Rh1 71.00(10) . . ? C24 C28 Rh1 68.37(9) . . ? C33 C28 Rh1 128.16(13) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Rh1 P1 C5 -10.79(7) . . . . ? C24 Rh1 P1 C5 96.90(7) . . . . ? C27 Rh1 P1 C5 127.24(19) . . . . ? C28 Rh1 P1 C5 74.70(8) . . . . ? C26 Rh1 P1 C5 161.19(8) . . . . ? C25 Rh1 P1 C5 135.83(7) . . . . ? Cl1 Rh1 P1 C5 -96.64(6) . . . . ? C11 Rh1 P1 C1 177.02(11) . . . . ? C24 Rh1 P1 C1 -75.30(11) . . . . ? C27 Rh1 P1 C1 -45.0(2) . . . . ? C28 Rh1 P1 C1 -97.50(11) . . . . ? C26 Rh1 P1 C1 -11.01(11) . . . . ? C25 Rh1 P1 C1 -36.37(11) . . . . ? Cl1 Rh1 P1 C1 91.17(10) . . . . ? C5 P1 C1 C2 -4.67(15) . . . . ? Rh1 P1 C1 C2 167.75(9) . . . . ? C5 P1 C1 C12 174.01(13) . . . . ? Rh1 P1 C1 C12 -13.58(19) . . . . ? C12 C1 C2 C3 -176.75(16) . . . . ? P1 C1 C2 C3 1.9(2) . . . . ? C1 C2 C3 C4 2.3(3) . . . . ? C1 C2 C3 C18 -178.90(15) . . . . ? C2 C3 C4 C5 -2.7(2) . . . . ? C18 C3 C4 C5 178.54(14) . . . . ? C3 C4 C5 C6 175.84(15) . . . . ? C3 C4 C5 P1 -1.2(2) . . . . ? C1 P1 C5 C4 4.45(15) . . . . ? Rh1 P1 C5 C4 -170.70(11) . . . . ? C1 P1 C5 C6 -173.09(10) . . . . ? Rh1 P1 C5 C6 11.77(12) . . . . ? C4 C5 C6 C7 -7.4(2) . . . . ? P1 C5 C6 C7 169.92(13) . . . . ? C4 C5 C6 C11 177.43(15) . . . . ? P1 C5 C6 C11 -5.22(17) . . . . ? C11 C6 C7 C8 1.3(3) . . . . ? C5 C6 C7 C8 -173.67(16) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 0.1(3) . . . . ? C9 C10 C11 C6 1.3(2) . . . . ? C9 C10 C11 Rh1 179.46(14) . . . . ? C7 C6 C11 C10 -2.0(2) . . . . ? C5 C6 C11 C10 173.24(14) . . . . ? C7 C6 C11 Rh1 179.95(12) . . . . ? C5 C6 C11 Rh1 -4.81(19) . . . . ? C24 Rh1 C11 C10 93.82(13) . . . . ? C27 Rh1 C11 C10 25.05(15) . . . . ? P1 Rh1 C11 C10 -168.45(13) . . . . ? C28 Rh1 C11 C10 57.81(14) . . . . ? C26 Rh1 C11 C10 25.6(2) . . . . ? C25 Rh1 C11 C10 101.57(16) . . . . ? Cl1 Rh1 C11 C10 -69.26(13) . . . . ? C24 Rh1 C11 C6 -88.16(13) . . . . ? C27 Rh1 C11 C6 -156.93(12) . . . . ? P1 Rh1 C11 C6 9.57(12) . . . . ? C28 Rh1 C11 C6 -124.17(13) . . . . ? C26 Rh1 C11 C6 -156.38(13) . . . . ? C25 Rh1 C11 C6 -80.41(17) . . . . ? Cl1 Rh1 C11 C6 108.76(12) . . . . ? C2 C1 C12 C13 134.56(18) . . . . ? P1 C1 C12 C13 -44.1(2) . . . . ? C2 C1 C12 C17 -46.6(2) . . . . ? P1 C1 C12 C17 134.77(15) . . . . ? C17 C12 C13 C14 0.5(3) . . . . ? C1 C12 C13 C14 179.32(17) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C14 C15 C16 C17 1.5(3) . . . . ? C15 C16 C17 C12 -1.6(3) . . . . ? C13 C12 C17 C16 0.6(3) . . . . ? C1 C12 C17 C16 -178.24(17) . . . . ? C2 C3 C18 C19 -157.86(16) . . . . ? C4 C3 C18 C19 21.0(2) . . . . ? C2 C3 C18 C23 22.5(2) . . . . ? C4 C3 C18 C23 -158.72(16) . . . . ? C23 C18 C19 C20 -1.1(3) . . . . ? C3 C18 C19 C20 179.19(17) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? C21 C22 C23 C18 -0.9(3) . . . . ? C19 C18 C23 C22 1.6(3) . . . . ? C3 C18 C23 C22 -178.74(17) . . . . ? C11 Rh1 C24 C28 -72.35(11) . . . . ? C27 Rh1 C24 C28 36.66(11) . . . . ? P1 Rh1 C24 C28 -153.65(9) . . . . ? C26 Rh1 C24 C28 79.39(11) . . . . ? C25 Rh1 C24 C28 114.44(14) . . . . ? Cl1 Rh1 C24 C28 61.43(16) . . . . ? C11 Rh1 C24 C25 173.22(9) . . . . ? C27 Rh1 C24 C25 -77.78(11) . . . . ? P1 Rh1 C24 C25 91.92(9) . . . . ? C28 Rh1 C24 C25 -114.44(14) . . . . ? C26 Rh1 C24 C25 -35.05(10) . . . . ? Cl1 Rh1 C24 C25 -53.01(16) . . . . ? C11 Rh1 C24 C29 49.32(17) . . . . ? C27 Rh1 C24 C29 158.32(18) . . . . ? P1 Rh1 C24 C29 -31.98(16) . . . . ? C28 Rh1 C24 C29 121.7(2) . . . . ? C26 Rh1 C24 C29 -158.94(18) . . . . ? C25 Rh1 C24 C29 -123.9(2) . . . . ? Cl1 Rh1 C24 C29 -176.91(11) . . . . ? C28 C24 C25 C26 -6.26(18) . . . . ? C29 C24 C25 C26 -175.01(16) . . . . ? Rh1 C24 C25 C26 60.45(11) . . . . ? C28 C24 C25 C30 171.85(15) . . . . ? C29 C24 C25 C30 3.1(3) . . . . ? Rh1 C24 C25 C30 -121.44(16) . . . . ? C28 C24 C25 Rh1 -66.71(11) . . . . ? C29 C24 C25 Rh1 124.53(16) . . . . ? C11 Rh1 C25 C26 -131.53(13) . . . . ? C24 Rh1 C25 C26 -119.67(15) . . . . ? C27 Rh1 C25 C26 -38.15(11) . . . . ? P1 Rh1 C25 C26 144.92(10) . . . . ? C28 Rh1 C25 C26 -80.55(12) . . . . ? Cl1 Rh1 C25 C26 37.32(12) . . . . ? C11 Rh1 C25 C24 -11.86(16) . . . . ? C27 Rh1 C25 C24 81.52(11) . . . . ? P1 Rh1 C25 C24 -95.41(9) . . . . ? C28 Rh1 C25 C24 39.11(10) . . . . ? C26 Rh1 C25 C24 119.67(15) . . . . ? Cl1 Rh1 C25 C24 156.98(8) . . . . ? C11 Rh1 C25 C30 104.93(18) . . . . ? C24 Rh1 C25 C30 116.8(2) . . . . ? C27 Rh1 C25 C30 -161.70(19) . . . . ? P1 Rh1 C25 C30 21.37(16) . . . . ? C28 Rh1 C25 C30 155.90(18) . . . . ? C26 Rh1 C25 C30 -123.5(2) . . . . ? Cl1 Rh1 C25 C30 -86.23(16) . . . . ? C24 C25 C26 C27 3.29(18) . . . . ? C30 C25 C26 C27 -174.75(16) . . . . ? Rh1 C25 C26 C27 60.76(11) . . . . ? C24 C25 C26 C31 -178.32(16) . . . . ? C30 C25 C26 C31 3.6(3) . . . . ? Rh1 C25 C26 C31 -120.85(18) . . . . ? C24 C25 C26 Rh1 -57.46(11) . . . . ? C30 C25 C26 Rh1 124.49(17) . . . . ? C11 Rh1 C26 C25 116.72(15) . . . . ? C24 Rh1 C26 C25 37.17(10) . . . . ? C27 Rh1 C26 C25 117.53(15) . . . . ? P1 Rh1 C26 C25 -45.77(12) . . . . ? C28 Rh1 C26 C25 80.01(11) . . . . ? Cl1 Rh1 C26 C25 -149.99(10) . . . . ? C11 Rh1 C26 C27 -0.81(19) . . . . ? C24 Rh1 C26 C27 -80.36(11) . . . . ? P1 Rh1 C26 C27 -163.30(8) . . . . ? C28 Rh1 C26 C27 -37.52(10) . . . . ? C25 Rh1 C26 C27 -117.53(15) . . . . ? Cl1 Rh1 C26 C27 92.48(10) . . . . ? C11 Rh1 C26 C31 -121.1(2) . . . . ? C24 Rh1 C26 C31 159.3(2) . . . . ? C27 Rh1 C26 C31 -120.3(2) . . . . ? P1 Rh1 C26 C31 76.4(2) . . . . ? C28 Rh1 C26 C31 -157.8(2) . . . . ? C25 Rh1 C26 C31 122.2(2) . . . . ? Cl1 Rh1 C26 C31 -27.82(19) . . . . ? C25 C26 C27 C28 0.86(18) . . . . ? C31 C26 C27 C28 -177.53(16) . . . . ? Rh1 C26 C27 C28 63.13(11) . . . . ? C25 C26 C27 C32 176.63(16) . . . . ? C31 C26 C27 C32 -1.8(3) . . . . ? Rh1 C26 C27 C32 -121.10(17) . . . . ? C25 C26 C27 Rh1 -62.27(11) . . . . ? C31 C26 C27 Rh1 119.33(17) . . . . ? C11 Rh1 C27 C28 62.76(11) . . . . ? C24 Rh1 C27 C28 -37.24(10) . . . . ? P1 Rh1 C27 C28 -71.0(2) . . . . ? C26 Rh1 C27 C28 -116.83(14) . . . . ? C25 Rh1 C27 C28 -80.56(10) . . . . ? Cl1 Rh1 C27 C28 152.51(9) . . . . ? C11 Rh1 C27 C26 179.59(9) . . . . ? C24 Rh1 C27 C26 79.59(10) . . . . ? P1 Rh1 C27 C26 45.9(2) . . . . ? C28 Rh1 C27 C26 116.83(14) . . . . ? C25 Rh1 C27 C26 36.27(9) . . . . ? Cl1 Rh1 C27 C26 -90.66(9) . . . . ? C11 Rh1 C27 C32 -60.6(2) . . . . ? C24 Rh1 C27 C32 -160.6(2) . . . . ? P1 Rh1 C27 C32 165.70(17) . . . . ? C28 Rh1 C27 C32 -123.3(3) . . . . ? C26 Rh1 C27 C32 119.8(3) . . . . ? C25 Rh1 C27 C32 156.1(2) . . . . ? Cl1 Rh1 C27 C32 29.2(2) . . . . ? C26 C27 C28 C24 -4.72(18) . . . . ? C32 C27 C28 C24 179.70(17) . . . . ? Rh1 C27 C28 C24 58.92(11) . . . . ? C26 C27 C28 C33 172.30(17) . . . . ? C32 C27 C28 C33 -3.3(3) . . . . ? Rh1 C27 C28 C33 -124.06(18) . . . . ? C26 C27 C28 Rh1 -63.64(11) . . . . ? C32 C27 C28 Rh1 120.77(18) . . . . ? C25 C24 C28 C27 6.71(17) . . . . ? C29 C24 C28 C27 175.64(15) . . . . ? Rh1 C24 C28 C27 -60.60(11) . . . . ? C25 C24 C28 C33 -170.42(16) . . . . ? C29 C24 C28 C33 -1.5(3) . . . . ? Rh1 C24 C28 C33 122.27(17) . . . . ? C25 C24 C28 Rh1 67.30(11) . . . . ? C29 C24 C28 Rh1 -123.76(16) . . . . ? C11 Rh1 C28 C27 -126.05(11) . . . . ? C24 Rh1 C28 C27 118.44(15) . . . . ? P1 Rh1 C28 C27 155.55(9) . . . . ? C26 Rh1 C28 C27 38.13(10) . . . . ? C25 Rh1 C28 C27 78.96(11) . . . . ? Cl1 Rh1 C28 C27 -35.23(12) . . . . ? C11 Rh1 C28 C24 115.51(10) . . . . ? C27 Rh1 C28 C24 -118.44(15) . . . . ? P1 Rh1 C28 C24 37.11(12) . . . . ? C26 Rh1 C28 C24 -80.31(10) . . . . ? C25 Rh1 C28 C24 -39.48(9) . . . . ? Cl1 Rh1 C28 C24 -153.67(8) . . . . ? C11 Rh1 C28 C33 -2.4(2) . . . . ? C24 Rh1 C28 C33 -117.9(2) . . . . ? C27 Rh1 C28 C33 123.7(2) . . . . ? P1 Rh1 C28 C33 -80.8(2) . . . . ? C26 Rh1 C28 C33 161.8(2) . . . . ? C25 Rh1 C28 C33 -157.4(2) . . . . ? Cl1 Rh1 C28 C33 88.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.468 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.055 #===END