# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Janssen (nee Kirleis), Karin' 'Butenschoen, Holger' _publ_contact_author_name 'Dr Holger Butenschoen' _publ_contact_author_email holger.butenschoen@mbox.oci.uni-hannover.de _publ_section_title ; New Cyclopentadienylethylphosphane Chelate Complexes with Unsymmetrical Phoshane Substitution ; # Attachment 'Co-complex-rac-6.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 820401' #TrackingRef 'Co-complex-rac-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 Co P' _chemical_formula_sum 'C19 H26 Co P' _chemical_formula_weight 344.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.070(5) _cell_length_b 11.504(4) _cell_length_c 14.202(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.47(5) _cell_angle_gamma 90.00 _cell_volume 1751.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7430 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details 'MULABS (PLATON)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294 _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 'STOE IPDS' _diffrn_measurement_method Psi-scan _diffrn_reflns_number 24177 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.23 _reflns_number_total 3479 _reflns_number_gt 2070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution SIR-92 _computing_structure_refinement SHELXL-97 _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^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3479 _refine_ls_number_parameters 202 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _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 Co Co 1.04097(3) 0.05063(3) 0.30653(2) 0.03693(10) Uani 1 1 d . . . P P 1.01018(5) 0.22357(6) 0.24654(4) 0.03418(16) Uani 1 1 d . . . C1 C 0.8721(3) 0.0156(2) 0.21183(19) 0.0551(7) Uani 1 1 d . . . C2 C 0.8648(2) -0.0118(3) 0.30810(19) 0.0595(8) Uani 1 1 d . . . H2 H 0.8090 0.0213 0.3417 0.095 Uiso 1 1 calc R . . C3 C 0.9554(3) -0.0966(3) 0.3439(2) 0.0688(9) Uani 1 1 d . . . H3 H 0.9734 -0.1294 0.4073 0.110 Uiso 1 1 calc R . . C4 C 1.0157(3) -0.1254(3) 0.2702(3) 0.0735(10) Uani 1 1 d . . . H4 H 1.0799 -0.1815 0.2753 0.118 Uiso 1 1 calc R . . C5 C 0.9644(3) -0.0571(3) 0.1884(2) 0.0638(7) Uani 1 1 d . . . H5 H 0.9871 -0.0589 0.1282 0.102 Uiso 1 1 calc R . . C6 C 0.8027(3) 0.1115(3) 0.1483(2) 0.0680(9) Uani 1 1 d . . . H6A H 0.7126 0.0993 0.1373 0.109 Uiso 1 1 calc R . . H6B H 0.8233 0.1102 0.0851 0.109 Uiso 1 1 calc R . . C7 C 0.8384(2) 0.2291(3) 0.19724(19) 0.0550(7) Uani 1 1 d . . . H7A H 0.7965 0.2411 0.2496 0.088 Uiso 1 1 calc R . . H7B H 0.8152 0.2923 0.1500 0.088 Uiso 1 1 calc R . . C8 C 1.0684(2) 0.24869(19) 0.13736(15) 0.0353(6) Uani 1 1 d . . . C10 C 1.1764(2) 0.1915(2) 0.13005(16) 0.0461(6) Uani 1 1 d . . . H10 H 1.2181 0.1415 0.1811 0.074 Uiso 1 1 calc R . . C11 C 1.2239(3) 0.2064(3) 0.04955(18) 0.0606(8) Uani 1 1 d . . . H11 H 1.2988 0.1681 0.0463 0.097 Uiso 1 1 calc R . . C12 C 1.1630(3) 0.2765(3) -0.02574(19) 0.0618(8) Uani 1 1 d . . . H12 H 1.1954 0.2865 -0.0812 0.099 Uiso 1 1 calc R . . C13 C 1.0555(3) 0.3319(3) -0.02057(18) 0.0626(8) Uani 1 1 d . . . H13 H 1.0131 0.3801 -0.0727 0.100 Uiso 1 1 calc R . . C14 C 1.0081(2) 0.3182(2) 0.06004(17) 0.0512(7) Uani 1 1 d . . . H14 H 0.9332 0.3570 0.0625 0.082 Uiso 1 1 calc R . . C15 C 1.0500(2) 0.3604(2) 0.31958(17) 0.0424(6) Uani 1 1 d . . . C16 C 0.9892(3) 0.3534(3) 0.40567(19) 0.0672(9) Uani 1 1 d . . . H16A H 0.8983 0.3495 0.3811 0.108 Uiso 1 1 calc R . . H16B H 1.0116 0.4226 0.4466 0.108 Uiso 1 1 calc R . . H16C H 1.0190 0.2837 0.4442 0.108 Uiso 1 1 calc R . . C17 C 1.1929(2) 0.3679(2) 0.35734(18) 0.0538(7) Uani 1 1 d . . . H17A H 1.2239 0.2982 0.3954 0.086 Uiso 1 1 calc R . . H17B H 1.2150 0.4369 0.3986 0.086 Uiso 1 1 calc R . . H17C H 1.2309 0.3734 0.3021 0.086 Uiso 1 1 calc R . . C18 C 1.0032(3) 0.4699(2) 0.26056(19) 0.0627(8) Uani 1 1 d . . . H18A H 0.9123 0.4661 0.2363 0.100 Uiso 1 1 calc R . . H18B H 1.0415 0.4751 0.2055 0.100 Uiso 1 1 calc R . . H18C H 1.0260 0.5386 0.3020 0.100 Uiso 1 1 calc R . . C19 C 1.2260(2) 0.0503(3) 0.36494(18) 0.0537(7) Uani 1 1 d D . . H19A H 1.256(3) -0.0254(13) 0.3580(19) 0.086 Uiso 1 1 d D . . H19B H 1.268(3) 0.1136(18) 0.343(2) 0.086 Uiso 1 1 d D . . C20 C 1.1619(3) 0.0714(3) 0.43673(18) 0.0542(7) Uani 1 1 d D . . H20A H 1.157(3) 0.1477(12) 0.4614(19) 0.087 Uiso 1 1 d D . . H20B H 1.151(3) 0.0073(16) 0.4761(16) 0.087 Uiso 1 1 d 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 Co 0.03669(16) 0.0379(2) 0.03648(16) 0.00502(19) 0.00967(12) -0.00195(19) P 0.0282(3) 0.0375(4) 0.0364(3) 0.0044(3) 0.0072(3) 0.0008(3) C1 0.0461(15) 0.052(2) 0.0598(17) 0.0011(14) 0.0000(13) -0.0216(14) C2 0.0463(16) 0.068(2) 0.0643(17) 0.0138(15) 0.0145(13) -0.0196(15) C3 0.064(2) 0.057(2) 0.086(2) 0.0267(17) 0.0192(18) -0.0148(16) C4 0.080(2) 0.0364(19) 0.107(3) -0.0038(18) 0.028(2) -0.0085(17) C5 0.079(2) 0.0510(18) 0.0592(16) -0.0141(19) 0.0144(14) -0.022(2) C6 0.0433(16) 0.080(2) 0.0674(18) 0.0150(17) -0.0111(14) -0.0188(16) C7 0.0323(13) 0.065(2) 0.0656(17) 0.0148(15) 0.0086(13) 0.0016(13) C8 0.0388(13) 0.0324(15) 0.0314(12) 0.0010(10) 0.0026(10) -0.0048(11) C10 0.0525(15) 0.0457(17) 0.0423(13) 0.0061(12) 0.0159(12) 0.0060(13) C11 0.0767(19) 0.065(2) 0.0496(16) 0.0011(16) 0.0330(15) 0.0040(17) C12 0.087(2) 0.060(2) 0.0440(15) -0.0029(15) 0.0269(15) -0.0146(18) C13 0.083(2) 0.063(2) 0.0358(14) 0.0149(14) 0.0030(14) -0.0130(17) C14 0.0498(16) 0.0543(19) 0.0457(14) 0.0109(13) 0.0048(12) -0.0025(13) C15 0.0493(15) 0.0371(15) 0.0443(14) -0.0024(12) 0.0182(12) 0.0017(13) C16 0.089(2) 0.060(2) 0.0646(18) -0.0059(15) 0.0435(18) 0.0056(17) C17 0.0588(17) 0.0502(18) 0.0498(15) -0.0071(13) 0.0086(13) -0.0113(14) C18 0.0681(18) 0.0405(19) 0.0814(18) 0.0028(16) 0.0223(15) 0.0043(16) C19 0.0404(14) 0.065(2) 0.0502(14) 0.0045(18) 0.0014(11) 0.0114(16) C20 0.0567(16) 0.060(2) 0.0403(14) 0.0098(14) 0.0024(13) 0.0031(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co C20 2.008(3) . ? Co C19 2.008(3) . ? Co C1 2.052(3) . ? Co C3 2.074(3) . ? Co C2 2.083(3) . ? Co C5 2.088(3) . ? Co C4 2.091(3) . ? Co P 2.1576(9) . ? P C8 1.844(2) . ? P C7 1.856(3) . ? P C15 1.877(3) . ? C1 C5 1.423(4) . ? C1 C2 1.425(3) . ? C1 C6 1.508(4) . ? C2 C3 1.400(4) . ? C2 H2 0.9500 . ? C3 C4 1.414(4) . ? C3 H3 0.9500 . ? C4 C5 1.400(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.527(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C14 1.388(3) . ? C8 C10 1.391(3) . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.375(4) . ? C11 H11 0.9500 . ? C12 C13 1.367(4) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C18 1.529(3) . ? C15 C16 1.538(3) . ? C15 C17 1.541(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.401(4) . ? C19 H19A 0.946(10) . ? C19 H19B 0.957(10) . ? C20 H20A 0.952(10) . ? C20 H20B 0.950(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Co C19 40.85(11) . . ? C20 Co C1 156.29(11) . . ? C19 Co C1 159.80(12) . . ? C20 Co C3 95.92(12) . . ? C19 Co C3 112.11(13) . . ? C1 Co C3 66.91(12) . . ? C20 Co C2 116.19(11) . . ? C19 Co C2 148.80(12) . . ? C1 Co C2 40.30(10) . . ? C3 Co C2 39.37(11) . . ? C20 Co C5 148.67(13) . . ? C19 Co C5 119.88(13) . . ? C1 Co C5 40.20(11) . . ? C3 Co C5 66.50(12) . . ? C2 Co C5 67.09(12) . . ? C20 Co C4 111.08(13) . . ? C19 Co C4 99.20(14) . . ? C1 Co C4 66.69(13) . . ? C3 Co C4 39.69(11) . . ? C2 Co C4 66.46(13) . . ? C5 Co C4 39.15(11) . . ? C20 Co P 104.91(9) . . ? C19 Co P 102.08(10) . . ? C1 Co P 83.91(8) . . ? C3 Co P 144.80(10) . . ? C2 Co P 105.44(9) . . ? C5 Co P 103.74(10) . . ? C4 Co P 142.88(10) . . ? C8 P C7 102.57(12) . . ? C8 P C15 104.49(11) . . ? C7 P C15 104.88(13) . . ? C8 P Co 114.99(8) . . ? C7 P Co 103.08(10) . . ? C15 P Co 124.29(8) . . ? C5 C1 C2 108.1(3) . . ? C5 C1 C6 125.3(3) . . ? C2 C1 C6 126.4(3) . . ? C5 C1 Co 71.25(16) . . ? C2 C1 Co 71.03(15) . . ? C6 C1 Co 119.57(18) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 Co 69.95(16) . . ? C1 C2 Co 68.67(15) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? Co C2 H2 126.6 . . ? C2 C3 C4 108.7(3) . . ? C2 C3 Co 70.68(15) . . ? C4 C3 Co 70.82(16) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? Co C3 H3 124.5 . . ? C5 C4 C3 108.3(3) . . ? C5 C4 Co 70.29(16) . . ? C3 C4 Co 69.49(17) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Co C4 H4 126.0 . . ? C4 C5 C1 107.6(3) . . ? C4 C5 Co 70.56(17) . . ? C1 C5 Co 68.55(15) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Co C5 H5 126.2 . . ? C1 C6 C7 109.9(2) . . ? C1 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? C1 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 P 105.43(19) . . ? C6 C7 H7A 110.7 . . ? P C7 H7A 110.7 . . ? C6 C7 H7B 110.7 . . ? P C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C14 C8 C10 117.8(2) . . ? C14 C8 P 123.75(19) . . ? C10 C8 P 118.43(17) . . ? C11 C10 C8 121.0(2) . . ? C11 C10 H10 119.5 . . ? C8 C10 H10 119.5 . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.8(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C8 120.9(3) . . ? C13 C14 H14 119.5 . . ? C8 C14 H14 119.5 . . ? C18 C15 C16 108.9(2) . . ? C18 C15 C17 108.8(2) . . ? C16 C15 C17 110.0(2) . . ? C18 C15 P 112.79(17) . . ? C16 C15 P 107.86(18) . . ? C17 C15 P 108.53(17) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Co 69.55(16) . . ? C20 C19 H19A 119.4(17) . . ? Co C19 H19A 107.9(19) . . ? C20 C19 H19B 118.6(18) . . ? Co C19 H19B 113.4(18) . . ? H19A C19 H19B 117(2) . . ? C19 C20 Co 69.60(15) . . ? C19 C20 H20A 121.1(18) . . ? Co C20 H20A 111.2(18) . . ? C19 C20 H20B 116.9(17) . . ? Co C20 H20B 107.4(17) . . ? H20A C20 H20B 118(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.244 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.048 # Attachment 'Cr-complex-rac-21.cif' data_II _database_code_depnum_ccdc_archive 'CCDC 820402' #TrackingRef 'Cr-complex-rac-21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H22 Cl2 Cr1 P1' _chemical_formula_weight 380.216 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.428(3) _cell_length_b 16.376(5) _cell_length_c 15.847(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.182(19) _cell_angle_gamma 90.00 _cell_volume 3623.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 297 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5.01 _cell_measurement_theta_max 24.33 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_ambient_temperature 297 _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 'STOE IPDS' _diffrn_measurement_method psi-scan _diffrn_reflns_number 50517 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.14 _reflns_number_total 7080 _reflns_number_gt 3591 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0023P)^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 7080 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _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 Cr1 Cr 0.14228(4) 0.29353(3) 0.34675(3) 0.03984(14) Uani 1 1 d . . . Cl1 Cl 0.16080(7) 0.17565(5) 0.42848(5) 0.0631(3) Uani 1 1 d . . . Cl2 Cl 0.03352(7) 0.35576(6) 0.38838(5) 0.0626(3) Uani 1 1 d . . . P1 P 0.03737(6) 0.24242(5) 0.19020(5) 0.0384(2) Uani 1 1 d . . . C1 C 0.2303(2) 0.3117(2) 0.2662(2) 0.0481(9) Uani 1 1 d . . . C2 C 0.2892(2) 0.2832(2) 0.3547(2) 0.0563(10) Uani 1 1 d . . . H2 H 0.3221 0.2338 0.3675 0.068 Uiso 1 1 calc R . . C3 C 0.2917(3) 0.3394(2) 0.4212(2) 0.0678(11) Uani 1 1 d . . . H3 H 0.3267 0.3340 0.4853 0.081 Uiso 1 1 calc R . . C4 C 0.2339(3) 0.4042(2) 0.3764(3) 0.0674(11) Uani 1 1 d . . . H4 H 0.2224 0.4502 0.4046 0.081 Uiso 1 1 calc R . . C5 C 0.1954(3) 0.3884(2) 0.2799(2) 0.0528(9) Uani 1 1 d . . . H5 H 0.1541 0.4224 0.2331 0.063 Uiso 1 1 calc R . . C6 C 0.1289(3) 0.2028(2) 0.1564(2) 0.0522(9) Uani 1 1 d . . . H6A H 0.1587 0.1540 0.1930 0.063 Uiso 1 1 calc R . . H6B H 0.0999 0.1880 0.0902 0.063 Uiso 1 1 calc R . . C8 C -0.0621(2) 0.38837(19) 0.1362(2) 0.0456(9) Uani 1 1 d . . . H8 H -0.0604 0.3878 0.1956 0.055 Uiso 1 1 calc R . . C9 C -0.0207(2) 0.32455(18) 0.10867(18) 0.0397(8) Uani 1 1 d . . . C10 C -0.1055(2) 0.4520(2) 0.0774(2) 0.0542(9) Uani 1 1 d . . . H10 H -0.1331 0.4942 0.0967 0.065 Uiso 1 1 calc R . . C11 C -0.1079(3) 0.4532(2) -0.0102(2) 0.0625(11) Uani 1 1 d . . . H11 H -0.1365 0.4968 -0.0500 0.075 Uiso 1 1 calc R . . C12 C -0.0689(3) 0.3911(3) -0.0392(2) 0.0693(11) Uani 1 1 d . . . H12 H -0.0718 0.3921 -0.0991 0.083 Uiso 1 1 calc R . . C13 C -0.0250(3) 0.3266(2) 0.0194(2) 0.0566(10) Uani 1 1 d . . . H13 H 0.0017 0.2844 -0.0009 0.068 Uiso 1 1 calc R . . C14 C 0.2041(3) 0.2692(2) 0.1746(2) 0.0620(10) Uani 1 1 d . . . H14A H 0.2618 0.2447 0.1740 0.074 Uiso 1 1 calc R . . H14B H 0.1796 0.3096 0.1242 0.074 Uiso 1 1 calc R . . C15 C -0.0551(3) 0.1616(2) 0.1655(2) 0.0517(10) Uani 1 1 d . . . C16 C -0.0104(3) 0.0856(2) 0.2171(3) 0.0856(14) Uani 1 1 d . . . H16A H 0.0350 0.0641 0.1942 0.103 Uiso 1 1 calc R . . H16B H -0.0603 0.0448 0.2072 0.103 Uiso 1 1 calc R . . H16C H 0.0236 0.0976 0.2838 0.103 Uiso 1 1 calc R . . C17 C -0.1263(3) 0.1927(3) 0.2020(3) 0.0887(14) Uani 1 1 d . . . H17A H -0.1569 0.2427 0.1687 0.106 Uiso 1 1 calc R . . H17B H -0.0923 0.2043 0.2689 0.106 Uiso 1 1 calc R . . H17C H -0.1752 0.1510 0.1919 0.106 Uiso 1 1 calc R . . C18 C -0.1081(3) 0.1450(3) 0.0625(2) 0.1104(19) Uani 1 1 d . . . H18A H -0.1375 0.1957 0.0300 0.133 Uiso 1 1 calc R . . H18B H -0.1581 0.1042 0.0520 0.133 Uiso 1 1 calc R . . H18C H -0.0632 0.1244 0.0387 0.133 Uiso 1 1 calc R . . Cr2 Cr -0.48945(4) 0.44533(3) -0.19149(3) 0.03675(13) Uani 1 1 d . . . Cl3 Cl -0.56654(7) 0.35630(5) -0.31097(5) 0.0555(3) Uani 1 1 d . . . Cl4 Cl -0.56344(7) 0.40719(5) -0.10007(5) 0.0577(3) Uani 1 1 d . . . P2 P -0.57873(6) 0.57249(5) -0.25267(5) 0.0358(2) Uani 1 1 d . . . C20 C -0.3739(2) 0.53984(19) -0.14390(19) 0.0424(8) Uani 1 1 d . . . C21 C -0.3660(2) 0.4919(2) -0.2149(2) 0.0548(10) Uani 1 1 d . . . H21 H -0.3734 0.5104 -0.2731 0.066 Uiso 1 1 calc R . . C22 C -0.3416(3) 0.4091(2) -0.0931(2) 0.0623(11) Uani 1 1 d . . . H22 H -0.3295 0.3627 -0.0560 0.075 Uiso 1 1 calc R . . C23 C -0.3455(3) 0.4135(2) -0.1823(3) 0.0640(11) Uani 1 1 d . . . H23 H -0.3356 0.3699 -0.2148 0.077 Uiso 1 1 calc R . . C25 C -0.5017(3) 0.64325(18) -0.16376(18) 0.0483(9) Uani 1 1 d . . . H25A H -0.5213 0.6996 -0.1833 0.058 Uiso 1 1 calc R . . H25B H -0.5067 0.6335 -0.1050 0.058 Uiso 1 1 calc R . . C26 C -0.3995(3) 0.62972(19) -0.1506(2) 0.0572(10) Uani 1 1 d . . . H26A H -0.3911 0.6540 -0.2031 0.069 Uiso 1 1 calc R . . H26B H -0.3556 0.6574 -0.0935 0.069 Uiso 1 1 calc R . . C27 C -0.5503(3) 0.68301(18) -0.3760(2) 0.0471(9) Uani 1 1 d . . . H27 H -0.5346 0.7218 -0.3289 0.057 Uiso 1 1 calc R . . C28 C -0.5750(2) 0.60467(17) -0.36184(17) 0.0355(8) Uani 1 1 d . . . C29 C -0.5715(3) 0.6479(2) -0.5292(2) 0.0600(11) Uani 1 1 d . . . H29 H -0.5709 0.6628 -0.5856 0.072 Uiso 1 1 calc R . . C30 C -0.5952(3) 0.5697(2) -0.5165(2) 0.0622(11) Uani 1 1 d . . . H30 H -0.6101 0.5313 -0.5638 0.075 Uiso 1 1 calc R . . C31 C -0.5489(3) 0.7039(2) -0.4598(2) 0.0553(10) Uani 1 1 d . . . H31 H -0.5324 0.7567 -0.4688 0.066 Uiso 1 1 calc R . . C32 C -0.5968(2) 0.54855(19) -0.43284(19) 0.0485(9) Uani 1 1 d . . . H32 H -0.6128 0.4955 -0.4242 0.058 Uiso 1 1 calc R . . C33 C -0.7037(3) 0.5919(2) -0.2697(2) 0.0527(9) Uani 1 1 d . . . C34 C -0.3595(2) 0.4877(2) -0.0699(2) 0.0505(9) Uani 1 1 d . . . H34 H -0.3614 0.5027 -0.0141 0.061 Uiso 1 1 calc R . . C35 C -0.7384(3) 0.6749(2) -0.3112(2) 0.0680(11) Uani 1 1 d . . . H35A H -0.6981 0.7172 -0.2687 0.082 Uiso 1 1 calc R . . H35B H -0.8049 0.6824 -0.3206 0.082 Uiso 1 1 calc R . . H35C H -0.7346 0.6793 -0.3712 0.082 Uiso 1 1 calc R . . C36 C -0.7672(3) 0.5268(2) -0.3351(3) 0.0877(14) Uani 1 1 d . . . H36A H -0.7451 0.4727 -0.3082 0.105 Uiso 1 1 calc R . . H36B H -0.7642 0.5308 -0.3955 0.105 Uiso 1 1 calc R . . H36C H -0.8335 0.5349 -0.3439 0.105 Uiso 1 1 calc R . . C37 C -0.7085(3) 0.5855(3) -0.1754(3) 0.0996(17) Uani 1 1 d . . . H37A H -0.6676 0.6276 -0.1332 0.120 Uiso 1 1 calc R . . H37B H -0.6862 0.5314 -0.1484 0.120 Uiso 1 1 calc R . . H37C H -0.7747 0.5935 -0.1841 0.120 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 Cr1 0.0402(4) 0.0421(3) 0.0352(3) -0.0036(2) 0.0140(2) -0.0022(3) Cl1 0.0780(8) 0.0550(5) 0.0515(5) 0.0100(4) 0.0231(5) 0.0008(5) Cl2 0.0746(8) 0.0713(6) 0.0541(5) -0.0003(5) 0.0389(5) 0.0151(5) P1 0.0375(6) 0.0429(5) 0.0355(4) -0.0041(4) 0.0163(4) -0.0002(4) C1 0.035(2) 0.056(2) 0.057(2) 0.0035(17) 0.0233(17) -0.0027(17) C2 0.030(2) 0.062(2) 0.073(2) 0.002(2) 0.0185(19) 0.0040(18) C3 0.045(3) 0.083(3) 0.054(2) -0.005(2) 0.0010(19) -0.012(2) C4 0.062(3) 0.054(2) 0.077(3) -0.015(2) 0.021(2) -0.024(2) C5 0.046(3) 0.048(2) 0.067(2) 0.0065(18) 0.0272(19) -0.0059(18) C6 0.056(3) 0.059(2) 0.0467(18) -0.0087(17) 0.0265(17) 0.009(2) C8 0.042(2) 0.052(2) 0.0379(17) -0.0013(16) 0.0130(16) 0.0011(18) C9 0.039(2) 0.0466(18) 0.0331(16) -0.0034(14) 0.0144(15) -0.0046(16) C10 0.050(3) 0.051(2) 0.057(2) 0.0007(18) 0.0177(18) 0.0049(18) C11 0.051(3) 0.063(2) 0.064(2) 0.021(2) 0.0150(19) 0.001(2) C12 0.073(3) 0.087(3) 0.051(2) 0.013(2) 0.030(2) 0.006(3) C13 0.058(3) 0.066(2) 0.052(2) 0.0032(18) 0.0299(19) 0.007(2) C14 0.051(3) 0.083(3) 0.067(2) -0.004(2) 0.039(2) 0.002(2) C15 0.052(3) 0.053(2) 0.0448(19) -0.0043(17) 0.0158(18) -0.0124(19) C16 0.087(4) 0.052(2) 0.109(3) -0.008(2) 0.034(3) -0.019(2) C17 0.068(3) 0.093(3) 0.117(3) 0.007(3) 0.051(3) -0.023(3) C18 0.134(5) 0.119(4) 0.061(2) -0.022(3) 0.025(3) -0.077(3) Cr2 0.0397(3) 0.0335(3) 0.0368(3) -0.0001(2) 0.0160(2) -0.0005(2) Cl3 0.0730(7) 0.0388(4) 0.0482(4) -0.0088(4) 0.0195(5) -0.0049(4) Cl4 0.0755(7) 0.0502(5) 0.0621(5) 0.0106(4) 0.0436(5) -0.0005(5) P2 0.0430(6) 0.0342(4) 0.0332(4) 0.0022(3) 0.0191(4) -0.0001(4) C20 0.038(2) 0.051(2) 0.0342(17) -0.0053(15) 0.0112(15) -0.0109(16) C21 0.041(2) 0.078(3) 0.051(2) -0.006(2) 0.0251(18) -0.012(2) C22 0.045(3) 0.057(2) 0.066(2) 0.010(2) 0.006(2) 0.0080(19) C23 0.044(3) 0.069(3) 0.080(3) -0.020(2) 0.027(2) 0.007(2) C25 0.072(3) 0.0335(17) 0.0381(17) -0.0047(14) 0.0217(18) 0.0007(18) C26 0.065(3) 0.050(2) 0.0436(19) -0.0077(16) 0.0099(19) -0.020(2) C27 0.067(3) 0.0364(18) 0.0395(17) -0.0034(14) 0.0236(17) -0.0088(17) C28 0.039(2) 0.0370(17) 0.0301(15) -0.0023(13) 0.0147(14) -0.0036(15) C29 0.071(3) 0.074(3) 0.0396(18) 0.0086(19) 0.0282(19) -0.009(2) C30 0.088(3) 0.063(3) 0.0382(18) -0.0065(17) 0.0289(19) -0.007(2) C31 0.075(3) 0.045(2) 0.050(2) 0.0090(18) 0.0311(19) -0.010(2) C32 0.059(3) 0.0447(19) 0.0428(18) 0.0033(16) 0.0223(17) -0.0117(18) C33 0.053(3) 0.055(2) 0.060(2) 0.0180(18) 0.0345(19) 0.0160(19) C34 0.045(2) 0.059(2) 0.0347(18) -0.0012(17) 0.0045(16) 0.0006(19) C35 0.067(3) 0.071(3) 0.073(2) 0.015(2) 0.036(2) 0.024(2) C36 0.045(3) 0.073(3) 0.146(4) 0.023(3) 0.042(3) 0.001(2) C37 0.105(4) 0.132(4) 0.100(3) 0.057(3) 0.080(3) 0.063(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 Cr1 C2 2.223(4) . ? Cr1 C4 2.223(3) . ? Cr1 C5 2.224(3) . ? Cr1 C3 2.226(4) . ? Cr1 C1 2.245(3) . ? Cr1 Cl1 2.2739(10) . ? Cr1 Cl2 2.2871(11) . ? Cr1 P1 2.4613(11) . ? P1 C9 1.815(3) . ? P1 C6 1.829(3) . ? P1 C15 1.861(3) . ? C1 C2 1.388(4) . ? C1 C5 1.419(4) . ? C1 C14 1.502(4) . ? C2 C3 1.387(5) . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C3 H3 0.9300 . ? C4 C5 1.410(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C14 1.526(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C8 C10 1.367(4) . ? C8 C9 1.388(4) . ? C8 H8 0.9300 . ? C9 C13 1.388(4) . ? C10 C11 1.374(5) . ? C10 H10 0.9300 . ? C11 C12 1.357(5) . ? C11 H11 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.489(5) . ? C15 C18 1.507(4) . ? C15 C17 1.530(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Cr2 C34 2.220(3) . ? Cr2 C21 2.224(3) . ? Cr2 C23 2.225(4) . ? Cr2 C22 2.227(3) . ? Cr2 C20 2.235(3) . ? Cr2 Cl4 2.2801(10) . ? Cr2 Cl3 2.2823(10) . ? Cr2 P2 2.4571(11) . ? P2 C25 1.821(3) . ? P2 C28 1.833(3) . ? P2 C33 1.857(4) . ? C20 C34 1.390(4) . ? C20 C21 1.419(4) . ? C20 C26 1.516(4) . ? C21 C23 1.370(5) . ? C21 H21 0.9300 . ? C22 C23 1.391(5) . ? C22 C34 1.398(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.517(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C31 1.380(4) . ? C27 C28 1.383(4) . ? C27 H27 0.9300 . ? C28 C32 1.379(4) . ? C29 C31 1.358(4) . ? C29 C30 1.370(4) . ? C29 H29 0.9300 . ? C30 C32 1.381(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C35 1.506(4) . ? C33 C36 1.520(5) . ? C33 C37 1.532(4) . ? C34 H34 0.9300 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 C2 Cr1 C4 60.55(14) . . ? C2 Cr1 C5 60.41(13) . . ? C4 Cr1 C5 36.96(12) . . ? C2 Cr1 C3 36.33(12) . . ? C4 Cr1 C3 35.98(13) . . ? C5 Cr1 C3 60.56(13) . . ? C2 Cr1 C1 36.19(11) . . ? C4 Cr1 C1 61.81(13) . . ? C5 Cr1 C1 37.02(11) . . ? C3 Cr1 C1 61.04(13) . . ? C2 Cr1 Cl1 91.45(10) . . ? C4 Cr1 Cl1 131.11(11) . . ? C5 Cr1 Cl1 151.86(10) . . ? C3 Cr1 Cl1 97.68(11) . . ? C1 Cr1 Cl1 118.47(9) . . ? C2 Cr1 Cl2 150.85(10) . . ? C4 Cr1 Cl2 93.13(12) . . ? C5 Cr1 Cl2 106.90(10) . . ? C3 Cr1 Cl2 114.74(11) . . ? C1 Cr1 Cl2 143.20(9) . . ? Cl1 Cr1 Cl2 98.27(4) . . ? C2 Cr1 P1 104.38(10) . . ? C4 Cr1 P1 125.21(10) . . ? C5 Cr1 P1 88.55(9) . . ? C3 Cr1 P1 137.49(11) . . ? C1 Cr1 P1 76.65(9) . . ? Cl1 Cr1 P1 98.91(4) . . ? Cl2 Cr1 P1 101.18(4) . . ? C9 P1 C6 105.26(15) . . ? C9 P1 C15 105.96(15) . . ? C6 P1 C15 107.75(17) . . ? C9 P1 Cr1 112.28(10) . . ? C6 P1 Cr1 99.03(11) . . ? C15 P1 Cr1 124.75(10) . . ? C2 C1 C5 105.7(3) . . ? C2 C1 C14 127.8(3) . . ? C5 C1 C14 126.5(3) . . ? C2 C1 Cr1 71.03(19) . . ? C5 C1 Cr1 70.69(19) . . ? C14 C1 Cr1 120.6(2) . . ? C3 C2 C1 109.9(3) . . ? C3 C2 Cr1 72.0(2) . . ? C1 C2 Cr1 72.79(19) . . ? C3 C2 H2 125.1 . . ? C1 C2 H2 125.1 . . ? Cr1 C2 H2 121.8 . . ? C4 C3 C2 108.5(3) . . ? C4 C3 Cr1 71.9(2) . . ? C2 C3 Cr1 71.69(19) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? Cr1 C3 H3 122.4 . . ? C3 C4 C5 107.4(3) . . ? C3 C4 Cr1 72.1(2) . . ? C5 C4 Cr1 71.57(19) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Cr1 C4 H4 121.7 . . ? C4 C5 C1 108.5(3) . . ? C4 C5 Cr1 71.5(2) . . ? C1 C5 Cr1 72.29(19) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Cr1 C5 H5 122.1 . . ? C14 C6 P1 108.2(2) . . ? C14 C6 H6A 110.1 . . ? P1 C6 H6A 110.1 . . ? C14 C6 H6B 110.1 . . ? P1 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C10 C8 C9 121.1(3) . . ? C10 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C13 C9 C8 118.2(3) . . ? C13 C9 P1 122.6(3) . . ? C8 C9 P1 119.2(2) . . ? C8 C10 C11 119.6(3) . . ? C8 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C9 120.1(3) . . ? C12 C13 H13 119.9 . . ? C9 C13 H13 119.9 . . ? C1 C14 C6 112.5(3) . . ? C1 C14 H14A 109.1 . . ? C6 C14 H14A 109.1 . . ? C1 C14 H14B 109.1 . . ? C6 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C18 110.7(3) . . ? C16 C15 C17 108.1(3) . . ? C18 C15 C17 108.9(3) . . ? C16 C15 P1 110.2(3) . . ? C18 C15 P1 111.7(2) . . ? C17 C15 P1 107.1(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C34 Cr2 C21 61.07(13) . . ? C34 Cr2 C23 60.55(13) . . ? C21 Cr2 C23 35.87(12) . . ? C34 Cr2 C22 36.64(11) . . ? C21 Cr2 C22 60.90(14) . . ? C23 Cr2 C22 36.41(12) . . ? C34 Cr2 C20 36.35(10) . . ? C21 Cr2 C20 37.10(11) . . ? C23 Cr2 C20 60.62(13) . . ? C22 Cr2 C20 61.05(12) . . ? C34 Cr2 Cl4 92.61(10) . . ? C21 Cr2 Cl4 153.57(9) . . ? C23 Cr2 Cl4 130.53(12) . . ? C22 Cr2 Cl4 97.05(11) . . ? C20 Cr2 Cl4 121.20(8) . . ? C34 Cr2 Cl3 151.56(10) . . ? C21 Cr2 Cl3 105.18(9) . . ? C23 Cr2 Cl3 93.34(10) . . ? C22 Cr2 Cl3 115.33(10) . . ? C20 Cr2 Cl3 141.39(9) . . ? Cl4 Cr2 Cl3 97.30(4) . . ? C34 Cr2 P2 103.01(9) . . ? C21 Cr2 P2 91.10(10) . . ? C23 Cr2 P2 126.91(11) . . ? C22 Cr2 P2 137.48(10) . . ? C20 Cr2 P2 77.23(9) . . ? Cl4 Cr2 P2 97.74(4) . . ? Cl3 Cr2 P2 101.97(4) . . ? C25 P2 C28 105.97(14) . . ? C25 P2 C33 107.37(17) . . ? C28 P2 C33 105.16(14) . . ? C25 P2 Cr2 99.34(11) . . ? C28 P2 Cr2 112.24(10) . . ? C33 P2 Cr2 125.15(11) . . ? C34 C20 C21 107.0(3) . . ? C34 C20 C26 126.8(3) . . ? C21 C20 C26 126.1(3) . . ? C34 C20 Cr2 71.23(18) . . ? C21 C20 Cr2 71.04(18) . . ? C26 C20 Cr2 120.2(2) . . ? C23 C21 C20 107.6(3) . . ? C23 C21 Cr2 72.1(2) . . ? C20 C21 Cr2 71.87(19) . . ? C23 C21 H21 126.2 . . ? C20 C21 H21 126.2 . . ? Cr2 C21 H21 121.6 . . ? C23 C22 C34 107.0(3) . . ? C23 C22 Cr2 71.7(2) . . ? C34 C22 Cr2 71.43(19) . . ? C23 C22 H22 126.5 . . ? C34 C22 H22 126.5 . . ? Cr2 C22 H22 122.1 . . ? C21 C23 C22 109.6(3) . . ? C21 C23 Cr2 72.1(2) . . ? C22 C23 Cr2 71.9(2) . . ? C21 C23 H23 125.2 . . ? C22 C23 H23 125.2 . . ? Cr2 C23 H23 122.5 . . ? C26 C25 P2 108.2(2) . . ? C26 C25 H25A 110.1 . . ? P2 C25 H25A 110.1 . . ? C26 C25 H25B 110.1 . . ? P2 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? C20 C26 C25 112.1(3) . . ? C20 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C20 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C31 C27 C28 120.2(3) . . ? C31 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C32 C28 C27 118.3(3) . . ? C32 C28 P2 118.9(2) . . ? C27 C28 P2 122.7(2) . . ? C31 C29 C30 120.3(3) . . ? C31 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C32 119.3(3) . . ? C29 C30 H30 120.3 . . ? C32 C30 H30 120.3 . . ? C29 C31 C27 120.6(3) . . ? C29 C31 H31 119.7 . . ? C27 C31 H31 119.7 . . ? C28 C32 C30 121.2(3) . . ? C28 C32 H32 119.4 . . ? C30 C32 H32 119.4 . . ? C35 C33 C36 109.2(3) . . ? C35 C33 C37 109.4(3) . . ? C36 C33 C37 109.4(3) . . ? C35 C33 P2 111.9(3) . . ? C36 C33 P2 107.9(2) . . ? C37 C33 P2 109.0(3) . . ? C20 C34 C22 108.8(3) . . ? C20 C34 Cr2 72.42(17) . . ? C22 C34 Cr2 71.93(19) . . ? C20 C34 H34 125.6 . . ? C22 C34 H34 125.6 . . ? Cr2 C34 H34 121.7 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.366 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.054 # Attachment 'Rh-complex-rac-14.cif' data_I _database_code_depnum_ccdc_archive 'CCDC 820403' #TrackingRef 'Rh-complex-rac-14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H25 I1 P1 Rh1' _chemical_formula_weight 502.16 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' I I -0.4742 1.8119 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 21.093(9) _cell_length_b 16.109(5) _cell_length_c 21.823(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7415(4) _cell_formula_units_Z 16 _cell_measurement_temperature 297 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 24.55 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 2.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7499 _exptl_absorpt_correction_T_max 0.8520 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_ambient_temperature 297 _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 'STOE IPDS' _diffrn_measurement_method psi-scan _diffrn_reflns_number 102298 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.15 _reflns_number_total 7303 _reflns_number_gt 4923 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0481P)^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 7303 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 0.034186(18) 0.34139(3) 0.195816(19) 0.03602(11) Uani 1 1 d . . . I1 I 0.04231(2) 0.19525(3) 0.13707(2) 0.06854(15) Uani 1 1 d . . . P1 P -0.04436(5) 0.31535(7) 0.26455(6) 0.0304(3) Uani 1 1 d . . . C1 C -0.0103(3) 0.4623(3) 0.1896(3) 0.0563(17) Uani 1 1 d . . . C2 C 0.0537(3) 0.4709(3) 0.2097(3) 0.0552(16) Uani 1 1 d . . . H2 H 0.0667 0.4895 0.2481 0.066 Uiso 1 1 calc R . . C3 C 0.0931(3) 0.4467(5) 0.1619(4) 0.075(2) Uani 1 1 d . . . H3 H 0.1372 0.4473 0.1630 0.090 Uiso 1 1 calc R . . C4 C 0.0581(4) 0.4224(5) 0.1144(4) 0.080(2) Uani 1 1 d . . . H4 H 0.0741 0.4018 0.0778 0.097 Uiso 1 1 calc R . . C5 C -0.0056(4) 0.4323(4) 0.1276(4) 0.073(2) Uani 1 1 d . . . H5 H -0.0393 0.4215 0.1013 0.088 Uiso 1 1 calc R . . C6 C -0.0688(3) 0.4764(4) 0.2268(4) 0.0672(19) Uani 1 1 d . . . H6A H -0.1062 0.4642 0.2018 0.081 Uiso 1 1 calc R . . H6B H -0.0709 0.5349 0.2390 0.081 Uiso 1 1 calc R . . C7 C -0.0698(3) 0.4228(3) 0.2832(3) 0.0500(14) Uani 1 1 d . . . H7A H -0.1127 0.4217 0.3003 0.060 Uiso 1 1 calc R . . H7B H -0.0413 0.4463 0.3141 0.060 Uiso 1 1 calc R . . C8 C -0.0242(2) 0.2698(3) 0.3380(2) 0.0352(11) Uani 1 1 d . . . C9 C 0.0107(3) 0.1959(3) 0.3386(3) 0.0509(14) Uani 1 1 d . . . H9 H 0.0203 0.1696 0.3018 0.061 Uiso 1 1 calc R . . C10 C 0.0313(3) 0.1611(4) 0.3936(3) 0.0675(19) Uani 1 1 d . . . H10 H 0.0547 0.1122 0.3937 0.081 Uiso 1 1 calc R . . C11 C 0.0165(4) 0.1998(5) 0.4474(3) 0.075(2) Uani 1 1 d . . . H11 H 0.0310 0.1775 0.4841 0.090 Uiso 1 1 calc R . . C12 C -0.0189(3) 0.2704(5) 0.4485(3) 0.0643(18) Uani 1 1 d . . . H12 H -0.0294 0.2950 0.4857 0.077 Uiso 1 1 calc R . . C13 C -0.0393(3) 0.3051(4) 0.3944(3) 0.0516(14) Uani 1 1 d . . . H13 H -0.0636 0.3532 0.3955 0.062 Uiso 1 1 calc R . . C14 C -0.1186(2) 0.2591(3) 0.2397(2) 0.0349(11) Uani 1 1 d . . . C15 C -0.1070(2) 0.1653(3) 0.2419(3) 0.0466(14) Uani 1 1 d . . . H15A H -0.0965 0.1488 0.2839 0.056 Uiso 1 1 calc R . . H15B H -0.0718 0.1510 0.2146 0.056 Uiso 1 1 calc R . . H15C H -0.1454 0.1360 0.2287 0.056 Uiso 1 1 calc R . . C16 C -0.1355(3) 0.2837(4) 0.1739(3) 0.0519(15) Uani 1 1 d . . . H16A H -0.1432 0.3436 0.1720 0.062 Uiso 1 1 calc R . . H16B H -0.1737 0.2538 0.1611 0.062 Uiso 1 1 calc R . . H16C H -0.1003 0.2693 0.1466 0.062 Uiso 1 1 calc R . . C17 C -0.1741(2) 0.2816(4) 0.2832(3) 0.0515(15) Uani 1 1 d . . . H17A H -0.1817 0.3416 0.2816 0.062 Uiso 1 1 calc R . . H17B H -0.1632 0.2654 0.3252 0.062 Uiso 1 1 calc R . . H17C H -0.2124 0.2521 0.2703 0.062 Uiso 1 1 calc R . . C18 C 0.1128(3) 0.2937(4) 0.2497(3) 0.069(2) Uani 1 1 d . . . H18A H 0.1124 0.2329 0.2488 0.082 Uiso 1 1 calc R . . H18B H 0.1087 0.3128 0.2922 0.082 Uiso 1 1 calc R . . H18C H 0.1529 0.3140 0.2326 0.082 Uiso 1 1 calc R . . Rh2 Rh 0.225534(17) 0.55160(2) 0.021813(18) 0.03226(10) Uani 1 1 d . . . I2 I 0.25005(2) 0.40636(3) 0.07686(2) 0.06082(13) Uani 1 1 d . . . P2 P 0.29106(6) 0.54185(8) -0.06034(6) 0.0324(3) Uani 1 1 d . . . C31 C 0.1914(3) 0.6773(4) 0.0169(3) 0.0605(17) Uani 1 1 d . . . H31 H 0.1695 0.6956 -0.0175 0.073 Uiso 1 1 calc R . . C32 C 0.2128(3) 0.6229(4) 0.1102(3) 0.0569(16) Uani 1 1 d . . . H32 H 0.2083 0.5976 0.1482 0.068 Uiso 1 1 calc R . . C33 C 0.1636(3) 0.6424(4) 0.0709(3) 0.0599(17) Uani 1 1 d . . . H33 H 0.1206 0.6344 0.0782 0.072 Uiso 1 1 calc R . . C34 C 0.2713(3) 0.6475(4) 0.0833(3) 0.0531(15) Uani 1 1 d . . . H34 H 0.3112 0.6432 0.1013 0.064 Uiso 1 1 calc R . . C35 C 0.2583(3) 0.6792(3) 0.0249(3) 0.0509(15) Uani 1 1 d . . . C36 C 0.3064(3) 0.7050(4) -0.0219(3) 0.0644(18) Uani 1 1 d . . . H36A H 0.3491 0.6983 -0.0049 0.077 Uiso 1 1 calc R . . H36B H 0.3004 0.7638 -0.0319 0.077 Uiso 1 1 calc R . . C37 C 0.3003(3) 0.6535(3) -0.0797(3) 0.0528(15) Uani 1 1 d . . . H37A H 0.3381 0.6611 -0.1052 0.063 Uiso 1 1 calc R . . H37B H 0.2634 0.6723 -0.1032 0.063 Uiso 1 1 calc R . . C44 C 0.3737(2) 0.4973(4) -0.0519(3) 0.0459(13) Uani 1 1 d . . . C45 C 0.3697(3) 0.4031(4) -0.0543(3) 0.0602(17) Uani 1 1 d . . . H45A H 0.3517 0.3859 -0.0937 0.072 Uiso 1 1 calc R . . H45B H 0.3426 0.3832 -0.0209 0.072 Uiso 1 1 calc R . . H45C H 0.4123 0.3794 -0.0498 0.072 Uiso 1 1 calc R . . C46 C 0.4160(3) 0.5270(5) -0.1053(3) 0.072(2) Uani 1 1 d . . . H46A H 0.4191 0.5877 -0.1044 0.087 Uiso 1 1 calc R . . H46B H 0.3972 0.5094 -0.1443 0.087 Uiso 1 1 calc R . . H46C H 0.4584 0.5028 -0.1012 0.087 Uiso 1 1 calc R . . C47 C 0.4017(3) 0.5250(5) 0.0089(3) 0.0647(19) Uani 1 1 d . . . H47A H 0.4044 0.5857 0.0098 0.078 Uiso 1 1 calc R . . H47B H 0.4443 0.5014 0.0136 0.078 Uiso 1 1 calc R . . H47C H 0.3746 0.5058 0.0425 0.078 Uiso 1 1 calc R . . C48 C 0.2623(2) 0.4950(3) -0.1310(2) 0.0358(11) Uani 1 1 d . . . C49 C 0.2658(2) 0.5323(4) -0.1877(2) 0.0438(13) Uani 1 1 d . . . H49 H 0.2848 0.5842 -0.1912 0.053 Uiso 1 1 calc R . . C50 C 0.2343(3) 0.4160(3) -0.1277(3) 0.0455(13) Uani 1 1 d . . . H50 H 0.2317 0.3892 -0.0900 0.055 Uiso 1 1 calc R . . C51 C 0.2414(3) 0.4935(4) -0.2400(3) 0.0541(16) Uani 1 1 d . . . H51 H 0.2435 0.5198 -0.2779 0.065 Uiso 1 1 calc R . . C52 C 0.2106(3) 0.3777(4) -0.1789(3) 0.0550(15) Uani 1 1 d . . . H52 H 0.1919 0.3255 -0.1760 0.066 Uiso 1 1 calc R . . C53 C 0.21463(16) 0.4172(3) -0.23488(16) 0.0585(17) Uani 1 1 d . . . H53 H 0.1988 0.3912 -0.2697 0.070 Uiso 1 1 calc R . . C54 C 0.13774(16) 0.4951(3) -0.02407(16) 0.0323(11) Uani 1 1 d R . . H54A H 0.1428 0.4348 -0.0270 0.039 Uiso 1 1 calc R . . H54B H 0.1328 0.5185 -0.0653 0.039 Uiso 1 1 calc R . . H54C H 0.1000 0.5079 0.0004 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 Rh1 0.03463(19) 0.0393(2) 0.0341(2) -0.00400(18) 0.00225(16) -0.00534(17) I1 0.0604(2) 0.0712(3) 0.0741(3) -0.0364(2) 0.0147(2) -0.0031(2) P1 0.0343(6) 0.0238(6) 0.0332(7) -0.0016(5) 0.0024(5) 0.0008(5) C1 0.057(3) 0.034(3) 0.078(5) 0.023(3) 0.015(3) 0.001(3) C2 0.063(4) 0.038(3) 0.065(4) -0.003(3) 0.000(3) -0.016(3) C3 0.057(4) 0.076(5) 0.091(6) 0.012(4) 0.014(4) -0.026(4) C4 0.093(6) 0.087(6) 0.061(5) 0.023(4) 0.023(4) -0.011(5) C5 0.092(5) 0.058(4) 0.069(5) 0.022(4) -0.033(4) -0.005(4) C6 0.068(4) 0.036(3) 0.098(6) 0.011(3) 0.004(4) 0.010(3) C7 0.059(3) 0.033(3) 0.058(4) -0.008(3) 0.011(3) 0.004(2) C8 0.040(3) 0.033(3) 0.032(3) -0.001(2) 0.000(2) -0.005(2) C9 0.069(4) 0.039(3) 0.045(4) -0.002(3) -0.005(3) 0.010(3) C10 0.084(5) 0.057(4) 0.061(5) 0.019(4) -0.021(4) 0.009(3) C11 0.093(5) 0.092(6) 0.039(4) 0.016(4) -0.016(4) -0.014(5) C12 0.088(5) 0.072(5) 0.033(4) -0.004(3) -0.001(3) -0.005(4) C13 0.066(4) 0.049(3) 0.040(3) -0.007(3) 0.005(3) -0.006(3) C14 0.033(2) 0.030(3) 0.042(3) 0.000(2) 0.000(2) -0.001(2) C15 0.045(3) 0.033(3) 0.062(4) -0.004(3) 0.003(3) -0.003(2) C16 0.050(3) 0.054(4) 0.052(4) 0.003(3) -0.016(3) -0.006(3) C17 0.040(3) 0.046(3) 0.069(4) 0.001(3) 0.011(3) -0.001(2) C18 0.068(4) 0.066(4) 0.071(5) 0.028(4) -0.051(4) -0.028(3) Rh2 0.03288(18) 0.0348(2) 0.0291(2) -0.00032(17) 0.00077(16) 0.00596(16) I2 0.0817(3) 0.0476(2) 0.0532(3) 0.0127(2) 0.0154(2) 0.0117(2) P2 0.0357(6) 0.0305(7) 0.0308(7) 0.0012(5) 0.0016(5) 0.0002(5) C31 0.081(4) 0.042(3) 0.059(4) -0.003(3) -0.001(3) 0.027(3) C32 0.075(4) 0.056(4) 0.040(4) -0.012(3) 0.010(3) 0.014(3) C33 0.055(3) 0.062(4) 0.063(4) -0.011(3) 0.009(3) 0.022(3) C34 0.069(4) 0.043(3) 0.047(4) -0.018(3) -0.003(3) 0.003(3) C35 0.066(4) 0.030(3) 0.056(4) -0.012(3) 0.005(3) 0.007(3) C36 0.094(5) 0.031(3) 0.068(5) -0.002(3) 0.009(4) -0.008(3) C37 0.067(4) 0.037(3) 0.054(4) 0.012(3) 0.009(3) -0.006(3) C44 0.036(3) 0.059(4) 0.043(3) -0.003(3) 0.003(2) 0.005(3) C45 0.060(4) 0.059(4) 0.062(4) 0.000(3) 0.006(3) 0.023(3) C46 0.039(3) 0.111(6) 0.067(5) 0.014(4) 0.013(3) -0.004(3) C47 0.043(3) 0.090(5) 0.061(4) -0.009(4) -0.011(3) 0.004(3) C48 0.031(2) 0.041(3) 0.036(3) 0.000(2) 0.004(2) 0.006(2) C49 0.046(3) 0.049(3) 0.037(3) 0.006(3) 0.005(2) 0.010(2) C50 0.054(3) 0.043(3) 0.039(3) -0.003(3) 0.002(2) -0.002(3) C51 0.053(3) 0.076(4) 0.033(3) 0.003(3) 0.001(3) 0.023(3) C52 0.053(3) 0.054(4) 0.059(4) -0.015(3) 0.000(3) -0.007(3) C53 0.050(3) 0.082(5) 0.044(4) -0.020(4) -0.008(3) 0.012(3) C54 0.040(2) 0.053(3) 0.004(2) -0.006(2) -0.0017(18) -0.010(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 Rh1 C2 2.148(5) . ? Rh1 C1 2.167(6) . ? Rh1 C18 2.174(5) . ? Rh1 C3 2.228(6) . ? Rh1 C5 2.250(6) . ? Rh1 C4 2.261(7) . ? Rh1 P1 2.2739(14) . ? Rh1 I1 2.6859(9) . ? P1 C8 1.814(5) . ? P1 C7 1.857(5) . ? P1 C14 1.889(5) . ? C1 C2 1.427(9) . ? C1 C5 1.438(10) . ? C1 C6 1.495(9) . ? C2 C3 1.390(10) . ? C2 H2 0.9300 . ? C3 C4 1.331(11) . ? C3 H3 0.9300 . ? C4 C5 1.384(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.503(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.393(8) . ? C8 C9 1.399(7) . ? C9 C10 1.395(8) . ? C9 H9 0.9300 . ? C10 C11 1.365(10) . ? C10 H10 0.9300 . ? C11 C12 1.361(10) . ? C11 H11 0.9300 . ? C12 C13 1.374(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C16 1.530(8) . ? C14 C15 1.532(7) . ? C14 C17 1.550(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Rh2 C31 2.152(6) . ? Rh2 C35 2.170(6) . ? Rh2 C33 2.235(6) . ? Rh2 C32 2.260(6) . ? Rh2 C34 2.262(6) . ? Rh2 P2 2.2692(14) . ? Rh2 C54 2.294(4) . ? Rh2 I2 2.6804(9) . ? P2 C48 1.821(5) . ? P2 C37 1.858(6) . ? P2 C44 1.895(5) . ? C31 C35 1.422(9) . ? C31 C33 1.432(9) . ? C31 H31 0.9300 . ? C32 C33 1.382(9) . ? C32 C34 1.424(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.400(9) . ? C34 H34 0.9300 . ? C35 C36 1.500(9) . ? C36 C37 1.515(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C44 C47 1.519(8) . ? C44 C45 1.520(8) . ? C44 C46 1.543(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.376(7) . ? C48 C50 1.406(7) . ? C49 C51 1.400(8) . ? C49 H49 0.9300 . ? C50 C52 1.371(8) . ? C50 H50 0.9300 . ? C51 C53 1.357(8) . ? C51 H51 0.9300 . ? C52 C53 1.381(8) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 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 C2 Rh1 C1 38.6(2) . . ? C2 Rh1 C18 96.9(2) . . ? C1 Rh1 C18 133.0(3) . . ? C2 Rh1 C3 37.0(3) . . ? C1 Rh1 C3 62.4(3) . . ? C18 Rh1 C3 91.3(3) . . ? C2 Rh1 C5 62.1(3) . . ? C1 Rh1 C5 38.0(3) . . ? C18 Rh1 C5 150.8(3) . . ? C3 Rh1 C5 59.6(3) . . ? C2 Rh1 C4 60.5(3) . . ? C1 Rh1 C4 61.8(3) . . ? C18 Rh1 C4 117.3(3) . . ? C3 Rh1 C4 34.5(3) . . ? C5 Rh1 C4 35.7(3) . . ? C2 Rh1 P1 103.02(18) . . ? C1 Rh1 P1 83.78(16) . . ? C18 Rh1 P1 97.7(2) . . ? C3 Rh1 P1 139.9(2) . . ? C5 Rh1 P1 106.5(2) . . ? C4 Rh1 P1 141.9(2) . . ? C2 Rh1 I1 155.03(18) . . ? C1 Rh1 I1 141.8(2) . . ? C18 Rh1 I1 84.26(19) . . ? C3 Rh1 I1 118.2(2) . . ? C5 Rh1 I1 106.2(2) . . ? C4 Rh1 I1 96.7(2) . . ? P1 Rh1 I1 101.52(4) . . ? C8 P1 C7 104.6(3) . . ? C8 P1 C14 104.7(2) . . ? C7 P1 C14 105.7(2) . . ? C8 P1 Rh1 119.14(16) . . ? C7 P1 Rh1 100.53(19) . . ? C14 P1 Rh1 120.21(17) . . ? C2 C1 C5 104.9(6) . . ? C2 C1 C6 126.7(7) . . ? C5 C1 C6 128.2(7) . . ? C2 C1 Rh1 70.0(3) . . ? C5 C1 Rh1 74.2(4) . . ? C6 C1 Rh1 117.4(4) . . ? C3 C2 C1 107.9(6) . . ? C3 C2 Rh1 74.6(4) . . ? C1 C2 Rh1 71.4(3) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Rh1 C2 H2 119.7 . . ? C4 C3 C2 109.6(7) . . ? C4 C3 Rh1 74.1(4) . . ? C2 C3 Rh1 68.4(3) . . ? C4 C3 H3 125.2 . . ? C2 C3 H3 125.2 . . ? Rh1 C3 H3 123.9 . . ? C3 C4 C5 110.0(7) . . ? C3 C4 Rh1 71.4(4) . . ? C5 C4 Rh1 71.7(4) . . ? C3 C4 H4 125.0 . . ? C5 C4 H4 125.0 . . ? Rh1 C4 H4 123.5 . . ? C4 C5 C1 107.5(6) . . ? C4 C5 Rh1 72.5(4) . . ? C1 C5 Rh1 67.9(3) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Rh1 C5 H5 124.9 . . ? C1 C6 C7 111.6(5) . . ? C1 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C1 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C6 C7 P1 110.7(4) . . ? C6 C7 H7A 109.5 . . ? P1 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C13 C8 C9 117.4(5) . . ? C13 C8 P1 124.2(4) . . ? C9 C8 P1 118.4(4) . . ? C10 C9 C8 120.9(6) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.0(7) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 121.5(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C8 121.4(6) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? C16 C14 C15 108.8(5) . . ? C16 C14 C17 109.8(4) . . ? C15 C14 C17 109.4(4) . . ? C16 C14 P1 109.8(3) . . ? C15 C14 P1 109.4(3) . . ? C17 C14 P1 109.7(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Rh1 C18 H18A 109.5 . . ? Rh1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Rh1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C31 Rh2 C35 38.4(2) . . ? C31 Rh2 C33 38.0(2) . . ? C35 Rh2 C33 63.3(2) . . ? C31 Rh2 C32 61.6(3) . . ? C35 Rh2 C32 62.0(2) . . ? C33 Rh2 C32 35.8(2) . . ? C31 Rh2 C34 62.0(2) . . ? C35 Rh2 C34 36.7(2) . . ? C33 Rh2 C34 61.2(2) . . ? C32 Rh2 C34 36.7(2) . . ? C31 Rh2 P2 103.26(19) . . ? C35 Rh2 P2 84.04(16) . . ? C33 Rh2 P2 141.28(19) . . ? C32 Rh2 P2 141.41(18) . . ? C34 Rh2 P2 104.81(17) . . ? C31 Rh2 C54 94.7(2) . . ? C35 Rh2 C54 130.31(19) . . ? C33 Rh2 C54 89.8(2) . . ? C32 Rh2 C54 118.56(19) . . ? C34 Rh2 C54 151.00(18) . . ? P2 Rh2 C54 96.85(10) . . ? C31 Rh2 I2 155.28(19) . . ? C35 Rh2 I2 138.72(17) . . ? C33 Rh2 I2 117.98(18) . . ? C32 Rh2 I2 94.81(17) . . ? C34 Rh2 I2 104.34(16) . . ? P2 Rh2 I2 100.15(4) . . ? C54 Rh2 I2 90.29(11) . . ? C48 P2 C37 104.1(3) . . ? C48 P2 C44 103.4(2) . . ? C37 P2 C44 107.0(3) . . ? C48 P2 Rh2 119.67(15) . . ? C37 P2 Rh2 100.2(2) . . ? C44 P2 Rh2 120.67(18) . . ? C35 C31 C33 108.2(6) . . ? C35 C31 Rh2 71.5(3) . . ? C33 C31 Rh2 74.1(3) . . ? C35 C31 H31 125.9 . . ? C33 C31 H31 125.9 . . ? Rh2 C31 H31 120.3 . . ? C33 C32 C34 109.4(6) . . ? C33 C32 Rh2 71.1(4) . . ? C34 C32 Rh2 71.7(3) . . ? C33 C32 H32 125.3 . . ? C34 C32 H32 125.3 . . ? Rh2 C32 H32 123.5 . . ? C32 C33 C31 107.0(6) . . ? C32 C33 Rh2 73.1(3) . . ? C31 C33 Rh2 67.8(3) . . ? C32 C33 H33 126.5 . . ? C31 C33 H33 126.5 . . ? Rh2 C33 H33 124.1 . . ? C35 C34 C32 107.8(6) . . ? C35 C34 Rh2 68.0(3) . . ? C32 C34 Rh2 71.6(3) . . ? C35 C34 H34 126.1 . . ? C32 C34 H34 126.1 . . ? Rh2 C34 H34 125.9 . . ? C34 C35 C31 107.4(6) . . ? C34 C35 C36 126.1(6) . . ? C31 C35 C36 126.4(6) . . ? C34 C35 Rh2 75.2(3) . . ? C31 C35 Rh2 70.1(3) . . ? C36 C35 Rh2 117.2(4) . . ? C35 C36 C37 110.9(5) . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.0 . . ? C36 C37 P2 110.5(4) . . ? C36 C37 H37A 109.6 . . ? P2 C37 H37A 109.6 . . ? C36 C37 H37B 109.6 . . ? P2 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C47 C44 C45 110.2(5) . . ? C47 C44 C46 110.1(5) . . ? C45 C44 C46 108.4(5) . . ? C47 C44 P2 109.3(4) . . ? C45 C44 P2 108.9(4) . . ? C46 C44 P2 109.9(4) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C50 117.7(5) . . ? C49 C48 P2 124.2(4) . . ? C50 C48 P2 118.1(4) . . ? C48 C49 C51 121.2(6) . . ? C48 C49 H49 119.4 . . ? C51 C49 H49 119.4 . . ? C52 C50 C48 121.3(6) . . ? C52 C50 H50 119.4 . . ? C48 C50 H50 119.4 . . ? C53 C51 C49 119.4(5) . . ? C53 C51 H51 120.3 . . ? C49 C51 H51 120.3 . . ? C50 C52 C53 119.4(5) . . ? C50 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C51 C53 C52 121.1(4) . . ? C51 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? Rh2 C54 H54A 109.5 . . ? Rh2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Rh2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.195 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.115