Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Brian James' _publ_contact_author_address ; Department of Chemistry University of British Columbia Vancouver British Columbia V6T 1Z1 CANADA ; _publ_contact_author_email BRJ@CHEM.UBC.CA _publ_section_title ; Synthesis and X-ray structures of water-soluble tris(hydroxymethyl)phosphine complexes of rhodium(I) ; loop_ _publ_author_name 'Brian James' 'Fabio Lorenzini' "Brian O'Patrick" data_bj439 _database_code_depnum_ccdc_archive 'CCDC 641989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 Cl O3 P Rh' _chemical_formula_weight 370.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P ca21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 12.5827(5) _cell_length_b 18.3977(7) _cell_length_c 11.7294(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2715.27(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4430 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.70 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19471 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.93 _reflns_number_total 6225 _reflns_number_gt 5394 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0338P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 6225 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 C1 C 1.1490(4) 1.0509(2) 0.5354(4) 0.0239(10) Uani 1 1 d . . . H1A H 1.1118 1.0454 0.4615 0.029 Uiso 1 1 calc R . . H1B H 1.1094 1.0868 0.5816 0.029 Uiso 1 1 calc R . . C2 C 1.2381(3) 0.9838(2) 0.7322(4) 0.0208(11) Uani 1 1 d . . . H2A H 1.2472 0.9399 0.7800 0.025 Uiso 1 1 calc R . . H2B H 1.3090 0.9982 0.7033 0.025 Uiso 1 1 calc R . . C3 C 1.0196(3) 0.9630(2) 0.6826(4) 0.0227(10) Uani 1 1 d . . . H3A H 1.0080 1.0110 0.7185 0.027 Uiso 1 1 calc R . . H3B H 0.9628 0.9552 0.6255 0.027 Uiso 1 1 calc R . . C4 C 1.0470(3) 0.8106(2) 0.5270(4) 0.0241(10) Uani 1 1 d . . . H4 H 1.0443 0.8330 0.5999 0.029 Uiso 1 1 calc R . . C5 C 1.0424(3) 0.8553(2) 0.4316(4) 0.0223(10) Uani 1 1 d . . . H5 H 1.0342 0.9060 0.4441 0.027 Uiso 1 1 calc R . . C6 C 1.0493(4) 0.8295(3) 0.3090(4) 0.0276(10) Uani 1 1 d . . . H6A H 1.0626 0.8720 0.2593 0.033 Uiso 1 1 calc R . . H6B H 0.9799 0.8085 0.2868 0.033 Uiso 1 1 calc R . . C7 C 1.1360(4) 0.7728(2) 0.2871(4) 0.0260(11) Uani 1 1 d . . . H7A H 1.1060 0.7237 0.2996 0.031 Uiso 1 1 calc R . . H7B H 1.1585 0.7760 0.2064 0.031 Uiso 1 1 calc R . . C8 C 1.2331(4) 0.7824(2) 0.3634(4) 0.0235(10) Uani 1 1 d . . . H8 H 1.2879 0.8136 0.3365 0.028 Uiso 1 1 calc R . . C9 C 1.2483(4) 0.7501(2) 0.4673(4) 0.0264(11) Uani 1 1 d . . . H9 H 1.3148 0.7588 0.5031 0.032 Uiso 1 1 calc R . . C10 C 1.1712(4) 0.7024(2) 0.5311(4) 0.0316(12) Uani 1 1 d . . . H10A H 1.1919 0.7013 0.6126 0.038 Uiso 1 1 calc R . . H10B H 1.1766 0.6522 0.5012 0.038 Uiso 1 1 calc R . . C11 C 1.0562(4) 0.7274(2) 0.5222(5) 0.0283(11) Uani 1 1 d . . . H11A H 1.0146 0.7059 0.5855 0.034 Uiso 1 1 calc R . . H11B H 1.0255 0.7096 0.4496 0.034 Uiso 1 1 calc R . . C12 C 0.9735(4) 0.7081(3) 0.9243(4) 0.0271(11) Uani 1 1 d . . . H12A H 1.0272 0.7062 0.8627 0.032 Uiso 1 1 calc R . . H12B H 0.9796 0.7562 0.9615 0.032 Uiso 1 1 calc R . . C13 C 0.8379(4) 0.7892(2) 0.7843(4) 0.0249(11) Uani 1 1 d . . . H13A H 0.8784 0.8251 0.8298 0.030 Uiso 1 1 calc R . . H13B H 0.8742 0.7838 0.7099 0.030 Uiso 1 1 calc R . . C14 C 0.7515(4) 0.7212(2) 0.9811(4) 0.0217(11) Uani 1 1 d . . . H14A H 0.6792 0.7318 0.9523 0.026 Uiso 1 1 calc R . . H14B H 0.7470 0.6780 1.0312 0.026 Uiso 1 1 calc R . . C15 C 0.9162(3) 0.5365(2) 0.8177(4) 0.0218(10) Uani 1 1 d . . . H15 H 0.9194 0.5670 0.8830 0.026 Uiso 1 1 calc R . . C16 C 0.9470(3) 0.5671(2) 0.7144(4) 0.0227(10) Uani 1 1 d . . . H16 H 0.9647 0.6173 0.7137 0.027 Uiso 1 1 calc R . . C17 C 0.9543(4) 0.5257(3) 0.6023(4) 0.0270(10) Uani 1 1 d . . . H17A H 0.9763 0.4751 0.6186 0.032 Uiso 1 1 calc R . . H17B H 1.0105 0.5482 0.5549 0.032 Uiso 1 1 calc R . . C18 C 0.8500(4) 0.5240(3) 0.5329(4) 0.0290(11) Uani 1 1 d . . . H18A H 0.8514 0.5641 0.4766 0.035 Uiso 1 1 calc R . . H18B H 0.8468 0.4777 0.4899 0.035 Uiso 1 1 calc R . . C19 C 0.7504(4) 0.5309(2) 0.6043(4) 0.0235(9) Uani 1 1 d . . . H19 H 0.6988 0.5655 0.5810 0.028 Uiso 1 1 calc R . . C20 C 0.7295(4) 0.4912(2) 0.6996(4) 0.0233(10) Uani 1 1 d . . . H20 H 0.6659 0.5012 0.7403 0.028 Uiso 1 1 calc R . . C21 C 0.8026(3) 0.4314(2) 0.7446(5) 0.0279(10) Uani 1 1 d . . . H21A H 0.8444 0.4111 0.6806 0.033 Uiso 1 1 calc R . . H21B H 0.7589 0.3917 0.7770 0.033 Uiso 1 1 calc R . . C22 C 0.8785(4) 0.4597(2) 0.8360(4) 0.0257(10) Uani 1 1 d . . . H22A H 0.8424 0.4570 0.9109 0.031 Uiso 1 1 calc R . . H22B H 0.9412 0.4273 0.8392 0.031 Uiso 1 1 calc R . . O1 O 1.2540(3) 1.07664(16) 0.5159(4) 0.0233(7) Uani 1 1 d . . . O2 O 1.1953(3) 1.04135(15) 0.8003(3) 0.0234(7) Uani 1 1 d . . . H2 H 1.2124 1.0816 0.7717 0.035 Uiso 1 1 calc R . . O3 O 1.0137(3) 0.9081(2) 0.7669(4) 0.0327(8) Uani 1 1 d . . . O12 O 0.9981(3) 0.65371(18) 1.0057(4) 0.0337(8) Uani 1 1 d . . . O13 O 0.7339(3) 0.81617(15) 0.7656(4) 0.0259(8) Uani 1 1 d . . . O14 O 0.7884(3) 0.78145(18) 1.0455(3) 0.0282(8) Uani 1 1 d . . . P1 P 1.15055(8) 0.96211(6) 0.61062(10) 0.0163(2) Uani 1 1 d . . . P2 P 0.83955(9) 0.70057(6) 0.85943(10) 0.0174(2) Uani 1 1 d . . . Cl1 Cl 1.37770(7) 0.90276(5) 0.51057(11) 0.0243(2) Uani 1 1 d . . . Cl2 Cl 0.61498(7) 0.65309(5) 0.74653(11) 0.0226(2) Uani 1 1 d . . . Rh01 Rh 1.19765(2) 0.863774(15) 0.50283(3) 0.01620(7) Uani 1 1 d . . . Rh2 Rh 0.78917(2) 0.601417(15) 0.75466(3) 0.01548(7) Uani 1 1 d . . . H1 H 1.270(4) 1.063(3) 0.458(5) 0.023(15) Uiso 1 1 d . . . H3 H 1.042(4) 0.919(3) 0.815(4) 0.018(15) Uiso 1 1 d . . . H12 H 0.965(4) 0.664(3) 1.053(4) 0.024(17) Uiso 1 1 d . . . H13 H 0.715(5) 0.798(3) 0.704(6) 0.05(2) Uiso 1 1 d . . . H14 H 0.775(4) 0.817(3) 1.021(5) 0.028(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(2) 0.024(2) 0.023(3) -0.0014(17) -0.0002(18) 0.0005(17) C2 0.021(2) 0.0183(19) 0.024(3) -0.0017(17) -0.0045(18) -0.0021(15) C3 0.020(2) 0.025(2) 0.023(3) -0.0034(18) 0.0023(18) -0.0021(17) C4 0.023(2) 0.022(2) 0.027(3) -0.0036(18) -0.0009(18) -0.0057(17) C5 0.017(2) 0.017(2) 0.033(3) 0.0013(18) -0.0017(18) 0.0023(16) C6 0.027(2) 0.025(2) 0.031(3) 0.002(2) -0.003(2) -0.0002(19) C7 0.032(3) 0.027(2) 0.020(3) -0.0037(18) -0.0019(19) 0.0033(19) C8 0.026(2) 0.020(2) 0.024(3) -0.0058(19) 0.001(2) 0.0058(17) C9 0.028(2) 0.021(2) 0.031(3) -0.0055(18) -0.003(2) 0.0042(19) C10 0.040(3) 0.015(2) 0.039(4) -0.0013(19) -0.006(2) -0.0002(19) C11 0.033(2) 0.022(2) 0.030(3) 0.000(2) 0.005(2) -0.0084(18) C12 0.028(3) 0.027(3) 0.026(3) -0.007(2) -0.001(2) 0.0006(19) C13 0.030(2) 0.019(2) 0.025(3) 0.0002(17) 0.0046(19) -0.0034(18) C14 0.025(2) 0.017(2) 0.024(4) -0.0018(17) 0.001(2) -0.0011(17) C15 0.021(2) 0.021(2) 0.024(3) -0.0058(18) -0.0011(18) 0.0062(17) C16 0.022(2) 0.019(2) 0.028(3) -0.0050(18) 0.0020(18) 0.0010(17) C17 0.030(2) 0.028(2) 0.023(3) -0.002(2) 0.006(2) 0.0041(19) C18 0.037(3) 0.032(2) 0.019(3) -0.0060(19) 0.000(2) 0.007(2) C19 0.030(2) 0.020(2) 0.021(3) 0.0007(19) -0.0095(19) 0.0042(18) C20 0.024(2) 0.016(2) 0.030(3) -0.0079(19) -0.0028(19) -0.0032(17) C21 0.038(3) 0.0149(19) 0.031(3) 0.001(2) -0.003(3) -0.0031(16) C22 0.031(2) 0.021(2) 0.025(3) -0.0020(18) 0.000(2) 0.0045(18) O1 0.0316(16) 0.0197(14) 0.019(2) -0.0018(16) 0.0052(15) -0.0031(14) O2 0.0385(19) 0.0148(14) 0.0170(17) 0.0002(12) -0.0021(13) -0.0043(13) O3 0.0320(18) 0.045(2) 0.021(2) -0.0001(18) 0.0002(19) -0.0174(15) O12 0.0359(18) 0.038(2) 0.027(2) -0.003(2) -0.005(2) 0.0075(14) O13 0.0361(19) 0.0184(14) 0.023(2) 0.0009(16) -0.0017(17) 0.0028(12) O14 0.048(2) 0.0177(17) 0.0193(19) -0.0012(14) -0.0008(14) -0.0001(15) P1 0.0170(5) 0.0138(5) 0.0182(6) -0.0010(4) 0.0012(4) -0.0017(4) P2 0.0186(5) 0.0153(5) 0.0183(6) -0.0018(4) 0.0000(4) -0.0005(4) Cl1 0.0162(4) 0.0323(5) 0.0244(6) -0.0023(5) 0.0018(5) -0.0034(4) Cl2 0.0180(4) 0.0235(5) 0.0264(6) -0.0012(5) -0.0003(5) 0.0010(3) Rh01 0.01686(13) 0.01458(14) 0.01716(17) -0.00162(14) 0.00073(15) -0.00034(12) Rh2 0.01771(13) 0.01337(14) 0.01537(17) -0.00110(14) -0.00046(16) 0.00030(10) _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 C1 O1 1.423(6) . ? C1 P1 1.856(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.432(5) . ? C2 P1 1.845(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.416(6) . ? C3 P1 1.852(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.390(6) . ? C4 C11 1.537(6) . ? C4 Rh01 2.152(4) . ? C4 H4 0.9500 . ? C5 C6 1.517(6) . ? C5 Rh01 2.131(4) . ? C5 H5 0.9500 . ? C6 C7 1.530(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.525(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.369(6) . ? C8 Rh01 2.261(4) . ? C8 H8 0.9500 . ? C9 C10 1.508(7) . ? C9 Rh01 2.225(4) . ? C9 H9 0.9500 . ? C10 C11 1.522(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.418(6) . ? C12 P2 1.854(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O13 1.417(6) . ? C13 P2 1.854(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O14 1.419(5) . ? C14 P2 1.846(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.391(6) . ? C15 C22 1.506(6) . ? C15 Rh2 2.128(4) . ? C15 H15 0.9500 . ? C16 C17 1.522(6) . ? C16 Rh2 2.137(4) . ? C16 H16 0.9500 . ? C17 C18 1.545(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.513(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.360(7) . ? C19 Rh2 2.243(5) . ? C19 H19 0.9500 . ? C20 C21 1.528(6) . ? C20 Rh2 2.257(4) . ? C20 H20 0.9500 . ? C21 C22 1.528(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O1 H1 0.76(5) . ? O2 H2 0.8400 . ? O3 H3 0.69(5) . ? O12 H12 0.71(5) . ? O13 H13 0.82(6) . ? O14 H14 0.73(5) . ? P1 Rh01 2.2854(11) . ? P2 Rh2 2.2890(11) . ? Cl1 Rh01 2.3781(10) . ? Cl2 Rh2 2.3910(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 O1 C1 P1 111.1(3) . . ? O1 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? O1 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? O2 C2 P1 111.5(3) . . ? O2 C2 H2A 109.3 . . ? P1 C2 H2A 109.3 . . ? O2 C2 H2B 109.3 . . ? P1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O3 C3 P1 111.1(3) . . ? O3 C3 H3A 109.4 . . ? P1 C3 H3A 109.4 . . ? O3 C3 H3B 109.4 . . ? P1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C11 124.3(4) . . ? C5 C4 Rh01 70.3(3) . . ? C11 C4 Rh01 112.5(3) . . ? C5 C4 H4 117.9 . . ? C11 C4 H4 117.9 . . ? Rh01 C4 H4 87.3 . . ? C4 C5 C6 125.2(4) . . ? C4 C5 Rh01 71.9(3) . . ? C6 C5 Rh01 110.0(3) . . ? C4 C5 H5 117.4 . . ? C6 C5 H5 117.4 . . ? Rh01 C5 H5 88.1 . . ? C5 C6 C7 114.4(4) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C6 113.2(4) . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 125.7(4) . . ? C9 C8 Rh01 70.8(3) . . ? C7 C8 Rh01 110.1(3) . . ? C9 C8 H8 117.2 . . ? C7 C8 H8 117.2 . . ? Rh01 C8 H8 89.1 . . ? C8 C9 C10 127.3(5) . . ? C8 C9 Rh01 73.7(3) . . ? C10 C9 Rh01 105.7(3) . . ? C8 C9 H9 116.4 . . ? C10 C9 H9 116.4 . . ? Rh01 C9 H9 90.7 . . ? C9 C10 C11 113.7(4) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C4 111.7(4) . . ? C10 C11 H11A 109.3 . . ? C4 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C4 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? O12 C12 P2 115.0(3) . . ? O12 C12 H12A 108.5 . . ? P2 C12 H12A 108.5 . . ? O12 C12 H12B 108.5 . . ? P2 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? O13 C13 P2 113.1(3) . . ? O13 C13 H13A 109.0 . . ? P2 C13 H13A 109.0 . . ? O13 C13 H13B 109.0 . . ? P2 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O14 C14 P2 112.1(3) . . ? O14 C14 H14A 109.2 . . ? P2 C14 H14A 109.2 . . ? O14 C14 H14B 109.2 . . ? P2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C22 126.2(4) . . ? C16 C15 Rh2 71.3(3) . . ? C22 C15 Rh2 109.8(3) . . ? C16 C15 H15 116.9 . . ? C22 C15 H15 116.9 . . ? Rh2 C15 H15 88.8 . . ? C15 C16 C17 124.6(4) . . ? C15 C16 Rh2 70.6(3) . . ? C17 C16 Rh2 113.3(3) . . ? C15 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? Rh2 C16 H16 86.1 . . ? C16 C17 C18 114.5(4) . . ? C16 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? C16 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C17 114.2(4) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 124.8(4) . . ? C20 C19 Rh2 73.0(3) . . ? C18 C19 Rh2 107.7(3) . . ? C20 C19 H19 117.6 . . ? C18 C19 H19 117.6 . . ? Rh2 C19 H19 89.3 . . ? C19 C20 C21 123.6(4) . . ? C19 C20 Rh2 71.8(3) . . ? C21 C20 Rh2 110.3(3) . . ? C19 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? Rh2 C20 H20 87.9 . . ? C20 C21 C22 111.9(3) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C15 C22 C21 114.7(4) . . ? C15 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C15 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C1 O1 H1 107(4) . . ? C2 O2 H2 109.5 . . ? C3 O3 H3 110(4) . . ? C12 O12 H12 102(4) . . ? C13 O13 H13 105(4) . . ? C14 O14 H14 114(5) . . ? C2 P1 C3 100.2(2) . . ? C2 P1 C1 100.6(2) . . ? C3 P1 C1 101.5(2) . . ? C2 P1 Rh01 116.33(14) . . ? C3 P1 Rh01 119.32(15) . . ? C1 P1 Rh01 115.85(15) . . ? C14 P2 C13 100.4(2) . . ? C14 P2 C12 102.3(2) . . ? C13 P2 C12 98.0(2) . . ? C14 P2 Rh2 114.38(14) . . ? C13 P2 Rh2 116.27(16) . . ? C12 P2 Rh2 122.12(15) . . ? C5 Rh01 C4 37.86(16) . . ? C5 Rh01 C9 96.89(17) . . ? C4 Rh01 C9 81.36(17) . . ? C5 Rh01 C8 81.29(17) . . ? C4 Rh01 C8 88.17(17) . . ? C9 Rh01 C8 35.52(16) . . ? C5 Rh01 P1 92.14(12) . . ? C4 Rh01 P1 93.37(12) . . ? C9 Rh01 P1 157.19(12) . . ? C8 Rh01 P1 167.21(12) . . ? C5 Rh01 Cl1 155.59(12) . . ? C4 Rh01 Cl1 166.25(13) . . ? C9 Rh01 Cl1 91.02(13) . . ? C8 Rh01 Cl1 92.24(13) . . ? P1 Rh01 Cl1 89.27(4) . . ? C15 Rh2 C16 38.07(16) . . ? C15 Rh2 C19 96.41(16) . . ? C16 Rh2 C19 81.77(17) . . ? C15 Rh2 C20 81.10(17) . . ? C16 Rh2 C20 88.86(17) . . ? C19 Rh2 C20 35.18(17) . . ? C15 Rh2 P2 93.01(12) . . ? C16 Rh2 P2 95.57(12) . . ? C19 Rh2 P2 160.62(12) . . ? C20 Rh2 P2 164.13(13) . . ? C15 Rh2 Cl2 157.76(12) . . ? C16 Rh2 Cl2 163.87(13) . . ? C19 Rh2 Cl2 89.98(12) . . ? C20 Rh2 Cl2 92.34(12) . . ? P2 Rh2 Cl2 87.61(4) . . ? 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 C4 C5 C6 -2.2(7) . . . . ? Rh01 C4 C5 C6 102.1(4) . . . . ? C11 C4 C5 Rh01 -104.3(4) . . . . ? C4 C5 C6 C7 -44.0(6) . . . . ? Rh01 C5 C6 C7 37.5(5) . . . . ? C5 C6 C7 C8 -32.1(6) . . . . ? C6 C7 C8 C9 91.2(5) . . . . ? C6 C7 C8 Rh01 11.0(5) . . . . ? C7 C8 C9 C10 -3.9(7) . . . . ? Rh01 C8 C9 C10 97.5(5) . . . . ? C7 C8 C9 Rh01 -101.4(4) . . . . ? C8 C9 C10 C11 -38.8(6) . . . . ? Rh01 C9 C10 C11 42.4(5) . . . . ? C9 C10 C11 C4 -38.9(6) . . . . ? C5 C4 C11 C10 94.9(5) . . . . ? Rh01 C4 C11 C10 14.1(5) . . . . ? C22 C15 C16 C17 -4.1(7) . . . . ? Rh2 C15 C16 C17 -105.4(4) . . . . ? C22 C15 C16 Rh2 101.3(4) . . . . ? C15 C16 C17 C18 88.4(6) . . . . ? Rh2 C16 C17 C18 6.6(5) . . . . ? C16 C17 C18 C19 -26.8(6) . . . . ? C17 C18 C19 C20 -49.1(6) . . . . ? C17 C18 C19 Rh2 32.1(5) . . . . ? C18 C19 C20 C21 -2.7(7) . . . . ? Rh2 C19 C20 C21 -102.8(4) . . . . ? C18 C19 C20 Rh2 100.1(4) . . . . ? C19 C20 C21 C22 94.8(5) . . . . ? Rh2 C20 C21 C22 13.7(5) . . . . ? C16 C15 C22 C21 -41.8(6) . . . . ? Rh2 C15 C22 C21 39.1(5) . . . . ? C20 C21 C22 C15 -35.0(6) . . . . ? O2 C2 P1 C3 -43.9(3) . . . . ? O2 C2 P1 C1 60.0(3) . . . . ? O2 C2 P1 Rh01 -174.0(2) . . . . ? O3 C3 P1 C2 -62.9(3) . . . . ? O3 C3 P1 C1 -166.1(3) . . . . ? O3 C3 P1 Rh01 65.3(3) . . . . ? O1 C1 P1 C2 51.7(4) . . . . ? O1 C1 P1 C3 154.5(3) . . . . ? O1 C1 P1 Rh01 -74.6(3) . . . . ? O14 C14 P2 C13 -56.9(4) . . . . ? O14 C14 P2 C12 43.7(3) . . . . ? O14 C14 P2 Rh2 177.8(2) . . . . ? O13 C13 P2 C14 -50.4(4) . . . . ? O13 C13 P2 C12 -154.5(3) . . . . ? O13 C13 P2 Rh2 73.6(4) . . . . ? O12 C12 P2 C14 67.8(4) . . . . ? O12 C12 P2 C13 170.3(3) . . . . ? O12 C12 P2 Rh2 -61.6(4) . . . . ? C6 C5 Rh01 C4 -121.7(4) . . . . ? C4 C5 Rh01 C9 66.3(3) . . . . ? C6 C5 Rh01 C9 -55.4(3) . . . . ? C4 C5 Rh01 C8 98.3(3) . . . . ? C6 C5 Rh01 C8 -23.4(3) . . . . ? C4 C5 Rh01 P1 -92.7(2) . . . . ? C6 C5 Rh01 P1 145.6(3) . . . . ? C4 C5 Rh01 Cl1 174.3(2) . . . . ? C6 C5 Rh01 Cl1 52.6(5) . . . . ? C11 C4 Rh01 C5 119.9(4) . . . . ? C5 C4 Rh01 C9 -113.2(3) . . . . ? C11 C4 Rh01 C9 6.8(3) . . . . ? C5 C4 Rh01 C8 -78.1(3) . . . . ? C11 C4 Rh01 C8 41.8(3) . . . . ? C5 C4 Rh01 P1 89.2(2) . . . . ? C11 C4 Rh01 P1 -150.9(3) . . . . ? C5 C4 Rh01 Cl1 -170.1(4) . . . . ? C11 C4 Rh01 Cl1 -50.2(7) . . . . ? C8 C9 Rh01 C5 64.4(3) . . . . ? C10 C9 Rh01 C5 -60.5(3) . . . . ? C8 C9 Rh01 C4 99.1(3) . . . . ? C10 C9 Rh01 C4 -25.9(3) . . . . ? C10 C9 Rh01 C8 -125.0(5) . . . . ? C8 C9 Rh01 P1 177.0(3) . . . . ? C10 C9 Rh01 P1 52.1(5) . . . . ? C8 C9 Rh01 Cl1 -92.4(3) . . . . ? C10 C9 Rh01 Cl1 142.6(3) . . . . ? C9 C8 Rh01 C5 -115.1(3) . . . . ? C7 C8 Rh01 C5 7.0(3) . . . . ? C9 C8 Rh01 C4 -77.6(3) . . . . ? C7 C8 Rh01 C4 44.4(3) . . . . ? C7 C8 Rh01 C9 122.0(5) . . . . ? C9 C8 Rh01 P1 -174.8(4) . . . . ? C7 C8 Rh01 P1 -52.8(8) . . . . ? C9 C8 Rh01 Cl1 88.6(3) . . . . ? C7 C8 Rh01 Cl1 -149.4(3) . . . . ? C2 P1 Rh01 C5 161.6(2) . . . . ? C3 P1 Rh01 C5 41.3(2) . . . . ? C1 P1 Rh01 C5 -80.5(2) . . . . ? C2 P1 Rh01 C4 123.7(2) . . . . ? C3 P1 Rh01 C4 3.4(2) . . . . ? C1 P1 Rh01 C4 -118.4(2) . . . . ? C2 P1 Rh01 C9 48.1(4) . . . . ? C3 P1 Rh01 C9 -72.2(4) . . . . ? C1 P1 Rh01 C9 166.0(4) . . . . ? C2 P1 Rh01 C8 -139.7(6) . . . . ? C3 P1 Rh01 C8 100.0(6) . . . . ? C1 P1 Rh01 C8 -21.8(6) . . . . ? C2 P1 Rh01 Cl1 -42.79(17) . . . . ? C3 P1 Rh01 Cl1 -163.10(18) . . . . ? C1 P1 Rh01 Cl1 75.09(17) . . . . ? C22 C15 Rh2 C16 -122.8(4) . . . . ? C16 C15 Rh2 C19 67.8(3) . . . . ? C22 C15 Rh2 C19 -54.9(3) . . . . ? C16 C15 Rh2 C20 99.6(3) . . . . ? C22 C15 Rh2 C20 -23.2(3) . . . . ? C16 C15 Rh2 P2 -95.2(2) . . . . ? C22 C15 Rh2 P2 142.0(3) . . . . ? C16 C15 Rh2 Cl2 173.7(3) . . . . ? C22 C15 Rh2 Cl2 51.0(5) . . . . ? C17 C16 Rh2 C15 120.3(4) . . . . ? C15 C16 Rh2 C19 -111.6(3) . . . . ? C17 C16 Rh2 C19 8.7(3) . . . . ? C15 C16 Rh2 C20 -77.0(3) . . . . ? C17 C16 Rh2 C20 43.3(3) . . . . ? C15 C16 Rh2 P2 87.8(2) . . . . ? C17 C16 Rh2 P2 -152.0(3) . . . . ? C15 C16 Rh2 Cl2 -171.5(3) . . . . ? C17 C16 Rh2 Cl2 -51.2(6) . . . . ? C20 C19 Rh2 C15 64.6(3) . . . . ? C18 C19 Rh2 C15 -57.4(3) . . . . ? C20 C19 Rh2 C16 99.8(3) . . . . ? C18 C19 Rh2 C16 -22.1(3) . . . . ? C18 C19 Rh2 C20 -121.9(4) . . . . ? C20 C19 Rh2 P2 -176.8(3) . . . . ? C18 C19 Rh2 P2 61.3(5) . . . . ? C20 C19 Rh2 Cl2 -94.1(3) . . . . ? C18 C19 Rh2 Cl2 144.0(3) . . . . ? C19 C20 Rh2 C15 -114.7(3) . . . . ? C21 C20 Rh2 C15 5.2(3) . . . . ? C19 C20 Rh2 C16 -77.3(3) . . . . ? C21 C20 Rh2 C16 42.7(4) . . . . ? C21 C20 Rh2 C19 120.0(5) . . . . ? C19 C20 Rh2 P2 176.2(3) . . . . ? C21 C20 Rh2 P2 -63.9(6) . . . . ? C19 C20 Rh2 Cl2 86.6(3) . . . . ? C21 C20 Rh2 Cl2 -153.4(3) . . . . ? C14 P2 Rh2 C15 -107.7(2) . . . . ? C13 P2 Rh2 C15 136.0(2) . . . . ? C12 P2 Rh2 C15 16.4(2) . . . . ? C14 P2 Rh2 C16 -145.8(2) . . . . ? C13 P2 Rh2 C16 97.9(2) . . . . ? C12 P2 Rh2 C16 -21.7(2) . . . . ? C14 P2 Rh2 C19 133.2(4) . . . . ? C13 P2 Rh2 C19 16.9(4) . . . . ? C12 P2 Rh2 C19 -102.7(4) . . . . ? C14 P2 Rh2 C20 -40.1(5) . . . . ? C13 P2 Rh2 C20 -156.4(5) . . . . ? C12 P2 Rh2 C20 84.0(5) . . . . ? C14 P2 Rh2 Cl2 50.08(17) . . . . ? C13 P2 Rh2 Cl2 -66.27(18) . . . . ? C12 P2 Rh2 Cl2 174.17(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.031 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.105 # Attachment 'bj441_June8.cif' data_bj441 _database_code_depnum_ccdc_archive 'CCDC 641990' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H18 Cl O7 P2 Rh' _chemical_formula_weight 414.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.1225(7) _cell_length_b 7.6560(10) _cell_length_c 15.582(2) _cell_angle_alpha 90.676(5) _cell_angle_beta 91.539(5) _cell_angle_gamma 98.235(5) _cell_volume 722.51(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2801 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 22.59 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.423 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5050 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 22.77 _reflns_number_total 5050 _reflns_number_gt 4645 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0874P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 5050 _refine_ls_number_parameters 308 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _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 C1 C 0.760(2) 0.491(2) 0.7876(13) 0.037(5) Uiso 1 1 d . . . H1A H 0.6752 0.5876 0.7729 0.044 Uiso 1 1 calc R . . H1B H 0.7928 0.4334 0.7331 0.044 Uiso 1 1 calc R . . C2 C 1.114(2) 0.3877(18) 0.8853(11) 0.022(4) Uani 1 1 d . . . H2A H 0.9974 0.3219 0.9202 0.026 Uiso 1 1 calc R . . H2B H 1.1509 0.3083 0.8390 0.026 Uiso 1 1 calc R . . C3 C 0.920(2) 0.6827(17) 0.9377(9) 0.019(4) Uani 1 1 d . . . H3A H 0.8051 0.5980 0.9646 0.023 Uiso 1 1 calc R . . H3B H 1.0447 0.7124 0.9794 0.023 Uiso 1 1 calc R . . C4 C 1.553(3) 0.7942(19) 0.5580(10) 0.033(4) Uani 1 1 d . . . H4A H 1.4109 0.7558 0.5269 0.040 Uiso 1 1 calc R . . H4B H 1.6454 0.8780 0.5214 0.040 Uiso 1 1 calc R . . C5 C 1.393(2) 1.1015(19) 0.6212(12) 0.032(5) Uani 1 1 d . . . H5A H 1.2414 1.0652 0.5972 0.039 Uiso 1 1 calc R . . H5B H 1.3817 1.1812 0.6710 0.039 Uiso 1 1 calc R . . C6 C 1.783(2) 0.9976(18) 0.7015(12) 0.029(4) Uani 1 1 d . . . H6A H 1.8769 0.9028 0.6996 0.035 Uiso 1 1 calc R . . H6B H 1.8465 1.0913 0.6624 0.035 Uiso 1 1 calc R . . C7 C 1.319(2) 0.920(2) 0.8372(12) 0.028(4) Uani 1 1 d . . . C8 C 0.353(2) 1.1588(17) 1.0810(10) 0.023(4) Uani 1 1 d . . . H8A H 0.4657 1.1730 1.0363 0.028 Uiso 1 1 calc R . . H8B H 0.2237 1.0779 1.0579 0.028 Uiso 1 1 calc R . . C9 C 0.554(2) 0.8609(19) 1.1246(11) 0.024(4) Uani 1 1 d . . . H9A H 0.5790 0.7747 1.1693 0.029 Uiso 1 1 calc R . . H9B H 0.4358 0.8043 1.0844 0.029 Uiso 1 1 calc R . . C10 C 0.213(2) 0.9747(17) 1.2307(11) 0.019(4) Uiso 1 1 d . . . H10A H 0.2537 0.9270 1.2868 0.022 Uiso 1 1 calc R . . H10B H 0.1279 1.0728 1.2421 0.022 Uiso 1 1 calc R . . C11 C 1.056(2) 1.2907(19) 1.4536(12) 0.035(5) Uani 1 1 d . . . H11A H 1.1596 1.3770 1.4880 0.042 Uiso 1 1 calc R . . H11B H 0.9217 1.2589 1.4873 0.042 Uiso 1 1 calc R . . C12 C 0.874(2) 1.5949(19) 1.3923(11) 0.025(4) Uiso 1 1 d . . . H12A H 0.8574 1.6725 1.3429 0.030 Uiso 1 1 calc R . . H12B H 0.7262 1.5603 1.4161 0.030 Uiso 1 1 calc R . . C13 C 1.258(2) 1.4848(16) 1.3182(9) 0.019(3) Uiso 1 1 d . . . H13A H 1.3207 1.5838 1.3570 0.023 Uiso 1 1 calc R . . H13B H 1.3554 1.3924 1.3224 0.023 Uiso 1 1 calc R . . C14 C 0.775(2) 1.3955(18) 1.1802(11) 0.022(4) Uiso 1 1 d . . . O1 O 0.6207(14) 0.3631(12) 0.8364(8) 0.034(3) Uani 1 1 d . . . H1 H 0.6974 0.3214 0.8744 0.051 Uiso 1 1 calc R . . O2 O 1.3074(15) 0.4485(13) 0.9385(7) 0.032(3) Uani 1 1 d . . . H2 H 1.4208 0.4291 0.9130 0.048 Uiso 1 1 calc R . . O3 O 0.8306(18) 0.8395(13) 0.9138(7) 0.030(3) Uani 1 1 d . . . H3 H 0.7900 0.8886 0.9579 0.045 Uiso 1 1 calc R . . O4 O 1.6643(16) 0.6416(12) 0.5744(7) 0.031(3) Uani 1 1 d . . . H4 H 1.5902 0.5740 0.6083 0.047 Uiso 1 1 calc R . . O5 O 1.5217(14) 1.1979(12) 0.5575(7) 0.031(3) Uani 1 1 d . . . H5 H 1.4472 1.1958 0.5114 0.046 Uiso 1 1 calc R . . O6 O 1.7940(14) 1.0659(12) 0.7822(8) 0.032(3) Uani 1 1 d . . . H6 H 1.6673 1.0521 0.8027 0.047 Uiso 1 1 calc R . . O7 O 1.3495(17) 1.0197(13) 0.8868(8) 0.035(3) Uani 1 1 d . . . O8 O 0.2888(15) 1.3244(12) 1.0997(7) 0.026(3) Uani 1 1 d . . . H8 H 0.2721 1.3778 1.0538 0.039 Uiso 1 1 calc R . . O9 O 0.7507(14) 0.9107(11) 1.0796(7) 0.025(3) Uani 1 1 d . . . H9 H 0.7537 1.0141 1.0618 0.037 Uiso 1 1 calc R . . O10 O 0.0748(13) 0.8380(10) 1.1822(6) 0.018(2) Uani 1 1 d . . . H10 H 0.0734 0.8648 1.1301 0.027 Uiso 1 1 calc R . . O11 O 1.1560(17) 1.1363(12) 1.4389(9) 0.039(3) Uani 1 1 d . . . H11 H 1.1048 1.0867 1.3928 0.058 Uiso 1 1 calc R . . O12 O 1.0137(13) 1.6909(12) 1.4560(7) 0.029(3) Uani 1 1 d . . . H12 H 1.1301 1.7386 1.4336 0.044 Uiso 1 1 calc R . . O13 O 1.2555(14) 1.5447(12) 1.2340(6) 0.017(2) Uiso 1 1 d . . . H13 H 1.1691 1.6202 1.2296 0.025 Uiso 1 1 calc R . . O14 O 0.8021(18) 1.4956(14) 1.1263(8) 0.041(3) Uani 1 1 d . . . P1 P 1.0149(6) 0.5844(5) 0.8388(3) 0.0170(9) Uani 1 1 d . . . P2 P 1.5015(6) 0.9055(5) 0.6592(3) 0.0189(10) Uani 1 1 d . . . P3 P 0.4657(6) 1.0613(4) 1.1756(3) 0.0136(9) Uani 1 1 d . . . P4 P 0.9806(6) 1.3941(5) 1.3538(3) 0.0184(10) Uani 1 1 d . . . Cl1 Cl 1.1974(6) 0.5052(5) 0.6545(3) 0.0299(10) Uani 1 1 d . . . Cl2 Cl 0.6750(6) 0.9977(5) 1.3608(3) 0.0296(11) Uani 1 1 d . . . Rh1 Rh 1.26486(14) 0.74507(12) 0.75264(7) 0.0157(3) Uani 1 1 d . . . Rh2 Rh 0.72965(13) 1.22858(11) 1.26067(7) 0.0148(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.025(10) 0.014(8) 0.028(12) -0.004(7) -0.013(7) 0.013(8) C3 0.032(9) 0.017(8) 0.009(9) 0.003(6) -0.007(6) 0.004(7) C4 0.070(12) 0.026(9) 0.008(11) -0.001(7) 0.010(8) 0.017(9) C5 0.016(9) 0.030(9) 0.053(12) 0.016(8) 0.010(8) 0.010(7) C6 0.017(8) 0.020(8) 0.053(13) 0.016(8) 0.007(7) 0.009(6) C7 0.008(8) 0.050(11) 0.031(11) 0.025(9) 0.003(7) 0.015(7) C8 0.027(9) 0.021(8) 0.021(11) 0.006(7) 0.005(7) 0.002(7) C9 0.009(9) 0.033(10) 0.033(12) -0.005(8) 0.006(7) 0.011(7) C11 0.017(9) 0.032(9) 0.056(15) -0.005(8) -0.011(8) 0.010(7) O1 0.018(6) 0.023(5) 0.059(10) 0.020(5) 0.004(5) -0.006(5) O2 0.023(6) 0.034(6) 0.040(8) 0.012(5) -0.006(5) 0.010(5) O3 0.051(7) 0.029(6) 0.017(7) -0.002(5) 0.002(5) 0.024(5) O4 0.049(7) 0.029(6) 0.020(8) 0.005(5) 0.021(5) 0.016(6) O5 0.032(6) 0.034(6) 0.024(7) 0.016(5) -0.007(5) -0.005(5) O6 0.010(5) 0.027(6) 0.057(9) 0.003(6) 0.009(5) 0.000(5) O7 0.027(7) 0.032(7) 0.044(9) -0.025(6) 0.006(6) -0.006(5) O8 0.025(6) 0.033(6) 0.027(8) 0.006(5) 0.007(5) 0.024(5) O9 0.025(6) 0.016(5) 0.036(8) -0.002(5) 0.005(5) 0.009(4) O10 0.020(5) 0.019(5) 0.015(6) 0.003(4) -0.003(4) 0.000(4) O11 0.042(7) 0.023(6) 0.052(10) -0.003(5) -0.026(6) 0.008(6) O12 0.013(6) 0.035(6) 0.038(8) -0.016(5) -0.004(5) 0.003(5) O14 0.037(7) 0.028(6) 0.054(10) 0.006(6) -0.011(6) -0.003(6) P1 0.017(2) 0.014(2) 0.020(3) 0.0044(17) 0.0021(17) 0.0045(18) P2 0.015(2) 0.022(2) 0.019(3) 0.0087(18) 0.0005(17) 0.0015(19) P3 0.011(2) 0.012(2) 0.019(3) -0.0001(16) 0.0015(16) 0.0049(17) P4 0.016(2) 0.018(2) 0.021(3) 0.0023(18) -0.0008(17) 0.0016(18) Cl1 0.032(2) 0.027(2) 0.031(3) -0.0099(18) 0.0093(19) 0.0019(19) Cl2 0.030(2) 0.027(2) 0.029(3) 0.0134(18) -0.0045(18) -0.0033(19) Rh1 0.0179(8) 0.0147(7) 0.0152(9) 0.0003(5) 0.0008(5) 0.0046(6) Rh2 0.0127(7) 0.0127(6) 0.0191(10) 0.0011(5) -0.0014(5) 0.0020(5) _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 C1 O1 1.438(17) . ? C1 P1 1.787(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.446(16) . ? C2 P1 1.849(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.437(16) . ? C3 P1 1.851(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.456(17) . ? C4 P2 1.839(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O5 1.431(17) . ? C5 P2 1.825(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O6 1.353(19) . ? C6 P2 1.865(14) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O7 1.071(19) . ? C7 Rh1 1.86(2) . ? C8 O8 1.410(16) . ? C8 P3 1.823(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O9 1.419(15) . ? C9 P3 1.873(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O10 1.441(16) . ? C10 P3 1.834(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O11 1.426(17) . ? C11 P4 1.830(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.419(18) . ? C12 P4 1.853(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O13 1.395(16) . ? C13 P4 1.844(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O14 1.143(18) . ? C14 Rh2 1.799(15) . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ? O3 H3 0.8400 . ? O4 H4 0.8400 . ? O5 H5 0.8400 . ? O6 H6 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? O11 H11 0.8400 . ? O12 H12 0.8400 . ? O13 H13 0.8400 . ? P1 Rh1 2.295(4) . ? P2 Rh1 2.318(4) . ? P3 Rh2 2.294(4) . ? P4 Rh2 2.314(4) . ? Cl1 Rh1 2.359(4) . ? Cl2 Rh2 2.365(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 P1 116.1(13) . . ? O1 C1 H1A 108.3 . . ? P1 C1 H1A 108.3 . . ? O1 C1 H1B 108.3 . . ? P1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? O2 C2 P1 107.6(8) . . ? O2 C2 H2A 110.2 . . ? P1 C2 H2A 110.2 . . ? O2 C2 H2B 110.2 . . ? P1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O3 C3 P1 107.6(9) . . ? O3 C3 H3A 110.2 . . ? P1 C3 H3A 110.2 . . ? O3 C3 H3B 110.2 . . ? P1 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O4 C4 P2 110.8(10) . . ? O4 C4 H4A 109.5 . . ? P2 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? O5 C5 P2 114.6(10) . . ? O5 C5 H5A 108.6 . . ? P2 C5 H5A 108.6 . . ? O5 C5 H5B 108.6 . . ? P2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? O6 C6 P2 116.0(10) . . ? O6 C6 H6A 108.3 . . ? P2 C6 H6A 108.3 . . ? O6 C6 H6B 108.3 . . ? P2 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? O7 C7 Rh1 178.9(15) . . ? O8 C8 P3 112.1(11) . . ? O8 C8 H8A 109.2 . . ? P3 C8 H8A 109.2 . . ? O8 C8 H8B 109.2 . . ? P3 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O9 C9 P3 109.4(9) . . ? O9 C9 H9A 109.8 . . ? P3 C9 H9A 109.8 . . ? O9 C9 H9B 109.8 . . ? P3 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O10 C10 P3 113.0(11) . . ? O10 C10 H10A 109.0 . . ? P3 C10 H10A 109.0 . . ? O10 C10 H10B 109.0 . . ? P3 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O11 C11 P4 112.7(12) . . ? O11 C11 H11A 109.0 . . ? P4 C11 H11A 109.0 . . ? O11 C11 H11B 109.0 . . ? P4 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O12 C12 P4 113.1(10) . . ? O12 C12 H12A 109.0 . . ? P4 C12 H12A 109.0 . . ? O12 C12 H12B 109.0 . . ? P4 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O13 C13 P4 112.5(9) . . ? O13 C13 H13A 109.1 . . ? P4 C13 H13A 109.1 . . ? O13 C13 H13B 109.1 . . ? P4 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? O14 C14 Rh2 176.8(14) . . ? C1 O1 H1 109.5 . . ? C2 O2 H2 109.5 . . ? C3 O3 H3 109.5 . . ? C4 O4 H4 109.5 . . ? C5 O5 H5 109.5 . . ? C6 O6 H6 109.5 . . ? C8 O8 H8 109.5 . . ? C9 O9 H9 109.5 . . ? C10 O10 H10 109.5 . . ? C11 O11 H11 109.5 . . ? C12 O12 H12 109.5 . . ? C13 O13 H13 109.5 . . ? C1 P1 C2 101.9(7) . . ? C1 P1 C3 101.8(8) . . ? C2 P1 C3 99.3(7) . . ? C1 P1 Rh1 116.0(6) . . ? C2 P1 Rh1 113.9(5) . . ? C3 P1 Rh1 121.1(4) . . ? C5 P2 C4 102.2(8) . . ? C5 P2 C6 102.7(7) . . ? C4 P2 C6 104.0(8) . . ? C5 P2 Rh1 111.9(5) . . ? C4 P2 Rh1 116.6(5) . . ? C6 P2 Rh1 117.5(5) . . ? C8 P3 C10 101.4(7) . . ? C8 P3 C9 99.6(7) . . ? C10 P3 C9 103.9(6) . . ? C8 P3 Rh2 119.5(4) . . ? C10 P3 Rh2 114.7(5) . . ? C9 P3 Rh2 115.4(5) . . ? C11 P4 C13 99.6(6) . . ? C11 P4 C12 103.0(7) . . ? C13 P4 C12 102.0(6) . . ? C11 P4 Rh2 117.6(5) . . ? C13 P4 Rh2 120.7(5) . . ? C12 P4 Rh2 111.4(5) . . ? C7 Rh1 P1 90.0(5) . . ? C7 Rh1 P2 92.1(5) . . ? P1 Rh1 P2 176.63(19) . . ? C7 Rh1 Cl1 175.2(5) . . ? P1 Rh1 Cl1 86.60(14) . . ? P2 Rh1 Cl1 91.46(14) . . ? C14 Rh2 P3 91.7(5) . . ? C14 Rh2 P4 91.0(5) . . ? P3 Rh2 P4 176.27(14) . . ? C14 Rh2 Cl2 176.8(5) . . ? P3 Rh2 Cl2 86.64(13) . . ? P4 Rh2 Cl2 90.88(14) . . ? 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 O1 C1 P1 C2 44.3(14) . . . . ? O1 C1 P1 C3 -58.0(13) . . . . ? O1 C1 P1 Rh1 168.5(9) . . . . ? O2 C2 P1 C1 -172.7(11) . . . . ? O2 C2 P1 C3 -68.4(11) . . . . ? O2 C2 P1 Rh1 61.7(11) . . . . ? O3 C3 P1 C1 -74.5(10) . . . . ? O3 C3 P1 C2 -178.8(9) . . . . ? O3 C3 P1 Rh1 55.9(10) . . . . ? O5 C5 P2 C4 -49.3(14) . . . . ? O5 C5 P2 C6 58.3(14) . . . . ? O5 C5 P2 Rh1 -174.8(10) . . . . ? O4 C4 P2 C5 173.8(9) . . . . ? O4 C4 P2 C6 67.2(11) . . . . ? O4 C4 P2 Rh1 -63.9(11) . . . . ? O6 C6 P2 C5 82.8(12) . . . . ? O6 C6 P2 C4 -171.0(10) . . . . ? O6 C6 P2 Rh1 -40.5(12) . . . . ? O8 C8 P3 C10 78.6(10) . . . . ? O8 C8 P3 C9 -175.0(9) . . . . ? O8 C8 P3 Rh2 -48.6(11) . . . . ? O10 C10 P3 C8 63.8(11) . . . . ? O10 C10 P3 C9 -39.2(12) . . . . ? O10 C10 P3 Rh2 -166.0(8) . . . . ? O9 C9 P3 C8 75.9(11) . . . . ? O9 C9 P3 C10 -179.8(10) . . . . ? O9 C9 P3 Rh2 -53.3(11) . . . . ? O11 C11 P4 C13 -71.5(10) . . . . ? O11 C11 P4 C12 -176.4(9) . . . . ? O11 C11 P4 Rh2 60.7(11) . . . . ? O13 C13 P4 C11 168.8(10) . . . . ? O13 C13 P4 C12 -85.6(11) . . . . ? O13 C13 P4 Rh2 38.5(11) . . . . ? O12 C12 P4 C11 47.2(12) . . . . ? O12 C12 P4 C13 -55.8(12) . . . . ? O12 C12 P4 Rh2 174.2(9) . . . . ? O7 C7 Rh1 P1 19(79) . . . . ? O7 C7 Rh1 P2 -164(79) . . . . ? O7 C7 Rh1 Cl1 -26(84) . . . . ? C1 P1 Rh1 C7 135.1(8) . . . . ? C2 P1 Rh1 C7 -107.1(7) . . . . ? C3 P1 Rh1 C7 11.1(7) . . . . ? C1 P1 Rh1 P2 7(3) . . . . ? C2 P1 Rh1 P2 124(3) . . . . ? C3 P1 Rh1 P2 -117(3) . . . . ? C1 P1 Rh1 Cl1 -48.3(7) . . . . ? C2 P1 Rh1 Cl1 69.5(5) . . . . ? C3 P1 Rh1 Cl1 -172.3(6) . . . . ? C5 P2 Rh1 C7 -69.0(8) . . . . ? C4 P2 Rh1 C7 174.0(8) . . . . ? C6 P2 Rh1 C7 49.5(7) . . . . ? C5 P2 Rh1 P1 59(3) . . . . ? C4 P2 Rh1 P1 -58(3) . . . . ? C6 P2 Rh1 P1 178(3) . . . . ? C5 P2 Rh1 Cl1 114.3(7) . . . . ? C4 P2 Rh1 Cl1 -2.8(6) . . . . ? C6 P2 Rh1 Cl1 -127.3(6) . . . . ? O14 C14 Rh2 P3 -37(25) . . . . ? O14 C14 Rh2 P4 146(25) . . . . ? O14 C14 Rh2 Cl2 20(33) . . . . ? C8 P3 Rh2 C14 -13.4(7) . . . . ? C10 P3 Rh2 C14 -134.1(7) . . . . ? C9 P3 Rh2 C14 105.2(7) . . . . ? C8 P3 Rh2 P4 121(2) . . . . ? C10 P3 Rh2 P4 0(3) . . . . ? C9 P3 Rh2 P4 -120(2) . . . . ? C8 P3 Rh2 Cl2 169.2(6) . . . . ? C10 P3 Rh2 Cl2 48.6(5) . . . . ? C9 P3 Rh2 Cl2 -72.1(5) . . . . ? C11 P4 Rh2 C14 -172.2(7) . . . . ? C13 P4 Rh2 C14 -50.3(7) . . . . ? C12 P4 Rh2 C14 69.2(7) . . . . ? C11 P4 Rh2 P3 53(3) . . . . ? C13 P4 Rh2 P3 175(2) . . . . ? C12 P4 Rh2 P3 -65(3) . . . . ? C11 P4 Rh2 Cl2 5.2(6) . . . . ? C13 P4 Rh2 Cl2 127.2(5) . . . . ? C12 P4 Rh2 Cl2 -113.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 22.77 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.890 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.127