# Supplementary Material (ESI) for Catalysis Science & Technology # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Angew.Chem.,Int.Ed. _journal_coden_cambridge 0179 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.M.Castro ;Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; H.Gulyas ;Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; J.Benet-Buchholz ;Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) X-ray Diffraction Unit Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; 'P.W.N.M.van Leuwen' ;Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; ; Z.Freixa ; ;Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; _publ_contact_author ; Jordi Benet-Buchholz Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ) X-ray Diffraction Unit Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; _publ_contact_author_email jbenet@iciq.es _publ_contact_author_fax '+34 977 920 224' _publ_contact_author_phone '+34 977 920 204' _publ_contact_letter ; ? ; _publ_requested_coeditor_name ? #----------------------------------------------------------------------- #3 Publication details _publ_section_title ; Secondary Phosphine Oxides in Rhodium(III) Catalyzed Transfer Hydrogenation of Ketones ; data_zf129_0m _database_code_depnum_ccdc_archive 'CCDC 685489' _ccdc_compound_id 1 _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _ccdc_disorder 1 _ccdc_comments ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H53 Cl4 O5 P5 Rh2' _chemical_formula_weight 1356.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 17.0585(15) _cell_length_b 17.1534(16) _cell_length_c 19.5448(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.797(2) _cell_angle_gamma 90.00 _cell_volume 5718.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9756 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 38.94 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.912941 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112410 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 39.46 _reflns_number_total 32712 _reflns_number_gt 22866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius,2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick,2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick,2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick,2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick,2001)' _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. The hydrogen attached to the atoms O(4) and o(5) are disordered in two positions (ration 65:34). ; _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^)+(0.0433P)^2^+3.0925P] 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 32712 _refine_ls_number_parameters 700 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.212572(6) 0.558929(8) 0.321795(5) 0.01016(2) Uani 1 1 d . . . Cl1 Cl 0.32256(2) 0.61564(3) 0.255578(18) 0.01355(6) Uani 1 1 d . . . P1 P 0.25854(2) 0.58036(3) 0.43151(2) 0.01248(7) Uani 1 1 d . . . O1 O 0.19274(7) 0.61282(9) 0.48083(6) 0.0172(2) Uani 1 1 d . . . H1 H 0.1559(18) 0.598(2) 0.4734(15) 0.036(8) Uiso 1 1 d . . . C1 C 0.29464(9) 0.49301(12) 0.47398(8) 0.0159(3) Uani 1 1 d . . . Rh2 Rh 0.303815(6) 0.492281(8) 0.186600(6) 0.01088(3) Uani 1 1 d . . . Cl2 Cl 0.16553(2) 0.52931(3) 0.206475(18) 0.01345(7) Uani 1 1 d . . . P2 P 0.10451(2) 0.50173(3) 0.37133(2) 0.01219(7) Uani 1 1 d . . . O2 O 0.06767(7) 0.55898(9) 0.42370(6) 0.0155(2) Uani 1 1 d . . . C2 C 0.35991(10) 0.45180(12) 0.45001(9) 0.0185(3) Uani 1 1 d . . . H2A H 0.3886 0.4715 0.4124 0.022 Uiso 1 1 calc R . . Cl3 Cl 0.29174(2) 0.44056(3) 0.298129(18) 0.01362(6) Uani 1 1 d . . . P3 P 0.15166(2) 0.67850(3) 0.31815(2) 0.01230(7) Uani 1 1 d . . . O3 O 0.06894(7) 0.68003(9) 0.35382(7) 0.0176(2) Uani 1 1 d . . . H3 H 0.0654(15) 0.641(2) 0.3801(13) 0.023(7) Uiso 1 1 d . . . C3 C 0.38273(12) 0.38237(14) 0.48096(10) 0.0250(4) Uani 1 1 d . . . H3A H 0.4272 0.3550 0.4648 0.030 Uiso 1 1 calc R . . Cl4 Cl 0.30850(2) 0.55544(3) 0.082228(19) 0.01594(7) Uani 1 1 d . . . P4 P 0.43327(2) 0.46271(3) 0.17535(2) 0.01380(8) Uani 1 1 d . . . O4 O 0.44947(7) 0.38813(9) 0.13298(7) 0.0195(3) Uani 1 1 d D . . H4 H 0.400(8) 0.365(12) 0.105(8) 0.080 Uiso 0.34(18) 1 d PD A 1 H5 H 0.383(4) 0.370(6) 0.092(5) 0.080 Uiso 0.66(18) 1 d PD A 2 C4 C 0.34064(12) 0.35266(15) 0.53563(11) 0.0281(4) Uani 1 1 d . . . H4A H 0.3549 0.3040 0.5554 0.034 Uiso 1 1 calc R . . P5 P 0.26528(2) 0.38599(3) 0.12564(2) 0.01377(8) Uani 1 1 d . . . O5 O 0.32790(7) 0.35257(9) 0.07736(6) 0.0177(2) Uani 1 1 d D . . C5 C 0.27770(12) 0.39441(16) 0.56110(10) 0.0272(4) Uani 1 1 d . . . H5A H 0.2502 0.3751 0.5995 0.033 Uiso 1 1 calc R . . C6 C 0.25452(10) 0.46423(14) 0.53080(9) 0.0210(4) Uani 1 1 d . . . H6A H 0.2115 0.4925 0.5486 0.025 Uiso 1 1 calc R . . C7 C 0.33559(9) 0.65155(11) 0.44324(8) 0.0144(3) Uani 1 1 d . . . C8 C 0.40440(9) 0.64514(13) 0.40572(8) 0.0177(3) Uani 1 1 d . . . H8A H 0.4107 0.6035 0.3743 0.021 Uiso 1 1 calc R . . C9 C 0.46379(10) 0.70025(14) 0.41464(10) 0.0221(4) Uani 1 1 d . . . H9A H 0.5100 0.6970 0.3882 0.027 Uiso 1 1 calc R . . C10 C 0.45563(11) 0.75973(14) 0.46193(10) 0.0235(4) Uani 1 1 d . . . H10A H 0.4964 0.7970 0.4679 0.028 Uiso 1 1 calc R . . C11 C 0.38802(11) 0.76528(13) 0.50084(10) 0.0225(4) Uani 1 1 d . . . H11A H 0.3832 0.8055 0.5339 0.027 Uiso 1 1 calc R . . C12 C 0.32763(10) 0.71167(12) 0.49107(8) 0.0179(3) Uani 1 1 d . . . H12A H 0.2810 0.7159 0.5169 0.021 Uiso 1 1 calc R . . C13 C 0.11981(9) 0.41172(11) 0.41841(8) 0.0143(3) Uani 1 1 d . . . C14 C 0.16445(10) 0.34907(12) 0.39499(9) 0.0170(3) Uani 1 1 d . . . H14A H 0.1912 0.3530 0.3528 0.020 Uiso 1 1 calc R . . C15 C 0.16963(10) 0.28117(13) 0.43331(9) 0.0194(3) Uani 1 1 d . . . H15A H 0.2005 0.2389 0.4175 0.023 Uiso 1 1 calc R . . C16 C 0.12983(10) 0.27457(13) 0.49488(9) 0.0192(3) Uani 1 1 d . . . H16A H 0.1337 0.2281 0.5211 0.023 Uiso 1 1 calc R . . C17 C 0.08451(10) 0.33636(13) 0.51768(9) 0.0191(3) Uani 1 1 d . . . H17A H 0.0569 0.3317 0.5594 0.023 Uiso 1 1 calc R . . C18 C 0.07924(10) 0.40485(12) 0.48004(8) 0.0171(3) Uani 1 1 d . . . H18A H 0.0482 0.4469 0.4960 0.021 Uiso 1 1 calc R . . C19 C 0.02515(9) 0.47553(12) 0.31268(8) 0.0161(3) Uani 1 1 d . . . C20 C -0.04617(11) 0.51590(14) 0.31734(11) 0.0253(4) Uani 1 1 d . . . H20A H -0.0509 0.5590 0.3475 0.030 Uiso 1 1 calc R . . C21 C -0.11023(12) 0.49201(16) 0.27718(13) 0.0316(5) Uani 1 1 d . . . H21A H -0.1587 0.5190 0.2803 0.038 Uiso 1 1 calc R . . C22 C -0.10384(12) 0.42965(15) 0.23301(11) 0.0280(4) Uani 1 1 d . . . H22A H -0.1474 0.4146 0.2052 0.034 Uiso 1 1 calc R . . C23 C -0.03315(10) 0.38846(14) 0.22910(9) 0.0216(4) Uani 1 1 d . . . H23A H -0.0288 0.3452 0.1990 0.026 Uiso 1 1 calc R . . C24 C 0.03067(10) 0.41126(13) 0.26949(9) 0.0190(3) Uani 1 1 d . . . H24A H 0.0783 0.3828 0.2676 0.023 Uiso 1 1 calc R . . C25 C 0.20285(9) 0.76062(11) 0.35687(8) 0.0140(3) Uani 1 1 d . . . C26 C 0.27552(10) 0.78785(13) 0.33414(9) 0.0184(3) Uani 1 1 d . . . H26A H 0.3028 0.7600 0.2999 0.022 Uiso 1 1 calc R . . C27 C 0.30769(11) 0.85567(13) 0.36171(10) 0.0215(3) Uani 1 1 d . . . H27A H 0.3563 0.8746 0.3454 0.026 Uiso 1 1 calc R . . C28 C 0.26899(11) 0.89600(14) 0.41313(10) 0.0235(4) Uani 1 1 d . . . H28A H 0.2908 0.9427 0.4313 0.028 Uiso 1 1 calc R . . C29 C 0.19862(11) 0.86782(13) 0.43766(10) 0.0220(4) Uani 1 1 d . . . H29A H 0.1731 0.8944 0.4737 0.026 Uiso 1 1 calc R . . C30 C 0.16514(10) 0.80072(12) 0.40972(8) 0.0177(3) Uani 1 1 d . . . H30A H 0.1166 0.7820 0.4265 0.021 Uiso 1 1 calc R . . C31 C 0.12685(10) 0.70967(12) 0.23186(8) 0.0171(3) Uani 1 1 d . . . C32 C 0.05213(12) 0.69031(15) 0.20688(11) 0.0270(4) Uani 1 1 d . . . H32A H 0.0187 0.6581 0.2332 0.032 Uiso 1 1 calc R . . C33 C 0.02671(14) 0.71831(18) 0.14343(12) 0.0368(6) Uani 1 1 d . . . H33A H -0.0245 0.7059 0.1270 0.044 Uiso 1 1 calc R . . C34 C 0.07539(16) 0.7639(2) 0.10433(11) 0.0406(7) Uani 1 1 d . . . H34A H 0.0578 0.7826 0.0610 0.049 Uiso 1 1 calc R . . C35 C 0.15021(16) 0.7827(2) 0.12838(11) 0.0408(7) Uani 1 1 d . . . H35A H 0.1837 0.8142 0.1015 0.049 Uiso 1 1 calc R . . C36 C 0.17598(12) 0.75519(17) 0.19201(10) 0.0289(5) Uani 1 1 d . . . H36A H 0.2273 0.7676 0.2082 0.035 Uiso 1 1 calc R . . C37 C 0.48639(9) 0.44453(13) 0.25541(9) 0.0182(3) Uani 1 1 d . . . C38 C 0.50538(11) 0.50475(15) 0.30038(10) 0.0247(4) Uani 1 1 d . . . H38A H 0.4881 0.5563 0.2908 0.030 Uiso 1 1 calc R . . C39 C 0.54972(13) 0.48989(18) 0.35949(11) 0.0331(5) Uani 1 1 d . . . H39A H 0.5620 0.5311 0.3902 0.040 Uiso 1 1 calc R . . C40 C 0.57572(14) 0.4152(2) 0.37329(12) 0.0374(6) Uani 1 1 d . . . H40A H 0.6055 0.4051 0.4137 0.045 Uiso 1 1 calc R . . C41 C 0.55842(14) 0.35504(18) 0.32815(14) 0.0391(6) Uani 1 1 d . . . H41A H 0.5772 0.3039 0.3373 0.047 Uiso 1 1 calc R . . C42 C 0.51337(12) 0.36954(15) 0.26920(12) 0.0281(4) Uani 1 1 d . . . H42A H 0.5012 0.3282 0.2385 0.034 Uiso 1 1 calc R . . C43 C 0.49139(9) 0.53900(12) 0.13560(8) 0.0151(3) Uani 1 1 d . . . C44 C 0.54069(9) 0.51521(13) 0.08273(8) 0.0168(3) Uani 1 1 d . . . H44A H 0.5407 0.4623 0.0683 0.020 Uiso 1 1 calc R . . C45 C 0.58965(10) 0.56919(13) 0.05139(9) 0.0193(3) Uani 1 1 d . . . H45A H 0.6223 0.5531 0.0150 0.023 Uiso 1 1 calc R . . C46 C 0.59106(10) 0.64593(14) 0.07293(9) 0.0206(4) Uani 1 1 d . . . H46A H 0.6258 0.6821 0.0524 0.025 Uiso 1 1 calc R . . C47 C 0.54139(10) 0.67024(14) 0.12486(10) 0.0221(4) Uani 1 1 d . . . H47A H 0.5417 0.7231 0.1393 0.027 Uiso 1 1 calc R . . C48 C 0.49124(10) 0.61677(13) 0.15565(10) 0.0208(3) Uani 1 1 d . . . H48A H 0.4568 0.6336 0.1905 0.025 Uiso 1 1 calc R . . C49 C 0.18168(10) 0.40553(12) 0.06969(8) 0.0173(3) Uani 1 1 d . . . C50 C 0.19581(11) 0.41264(13) -0.00035(9) 0.0210(3) Uani 1 1 d . . . H50A H 0.2481 0.4113 -0.0164 0.025 Uiso 1 1 calc R . . C51 C 0.13349(13) 0.42173(15) -0.04680(10) 0.0274(4) Uani 1 1 d . . . H51A H 0.1436 0.4279 -0.0942 0.033 Uiso 1 1 calc R . . C52 C 0.05692(13) 0.42179(16) -0.02381(12) 0.0313(5) Uani 1 1 d . . . H52A H 0.0145 0.4256 -0.0557 0.038 Uiso 1 1 calc R . . C53 C 0.04220(12) 0.41621(16) 0.04588(11) 0.0283(4) Uani 1 1 d . . . H53A H -0.0102 0.4165 0.0616 0.034 Uiso 1 1 calc R . . C54 C 0.10450(10) 0.41021(14) 0.09262(10) 0.0217(4) Uani 1 1 d . . . H54A H 0.0944 0.4093 0.1403 0.026 Uiso 1 1 calc R . . C55 C 0.23995(11) 0.30453(13) 0.18100(9) 0.0187(3) Uani 1 1 d . . . C56 C 0.30237(14) 0.27268(16) 0.21883(12) 0.0324(5) Uani 1 1 d . . . H56A H 0.3526 0.2963 0.2164 0.039 Uiso 1 1 calc R . . C57 C 0.29282(19) 0.20786(19) 0.25960(14) 0.0434(7) Uani 1 1 d . . . H57A H 0.3363 0.1872 0.2845 0.052 Uiso 1 1 calc R . . C58 C 0.2205(2) 0.17313(19) 0.26427(12) 0.0443(7) Uani 1 1 d . . . H58A H 0.2136 0.1289 0.2928 0.053 Uiso 1 1 calc R . . C59 C 0.15791(17) 0.20307(19) 0.22711(14) 0.0409(6) Uani 1 1 d . . . H59A H 0.1079 0.1791 0.2303 0.049 Uiso 1 1 calc R . . C60 C 0.16709(12) 0.26791(15) 0.18503(12) 0.0274(4) Uani 1 1 d . . . H60A H 0.1238 0.2872 0.1591 0.033 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 0.00861(4) 0.01122(6) 0.01065(4) -0.00108(4) 0.00011(3) 0.00021(4) Cl1 0.01189(12) 0.01404(19) 0.01475(13) -0.00227(13) 0.00168(10) -0.00157(12) P1 0.01145(14) 0.0145(2) 0.01145(14) -0.00092(14) -0.00075(11) -0.00004(14) O1 0.0144(5) 0.0218(8) 0.0155(5) -0.0048(5) 0.0004(4) -0.0011(5) C1 0.0164(6) 0.0154(8) 0.0158(6) 0.0003(6) -0.0035(5) -0.0015(6) Rh2 0.01025(4) 0.01165(6) 0.01077(4) -0.00084(4) 0.00094(3) -0.00055(4) Cl2 0.01124(12) 0.01612(19) 0.01296(13) -0.00231(12) -0.00081(10) -0.00005(12) P2 0.01022(14) 0.0127(2) 0.01369(15) -0.00045(14) 0.00082(11) -0.00038(13) O2 0.0130(4) 0.0155(7) 0.0180(5) -0.0026(4) 0.0044(4) -0.0001(4) C2 0.0186(7) 0.0173(9) 0.0196(7) 0.0023(6) -0.0043(5) 0.0016(6) Cl3 0.01401(13) 0.01405(18) 0.01285(13) 0.00067(12) 0.00153(10) 0.00145(12) P3 0.01072(14) 0.0121(2) 0.01402(15) -0.00068(14) -0.00046(11) 0.00105(13) O3 0.0134(5) 0.0160(7) 0.0234(6) 0.0004(5) 0.0042(4) 0.0021(4) C3 0.0239(8) 0.0220(11) 0.0287(8) 0.0018(8) -0.0082(6) 0.0030(7) Cl4 0.01778(15) 0.0168(2) 0.01327(13) 0.00204(13) 0.00063(11) -0.00197(14) P4 0.01117(15) 0.0146(2) 0.01572(16) -0.00022(15) 0.00174(12) 0.00007(14) O4 0.0156(5) 0.0174(7) 0.0257(6) -0.0048(5) 0.0030(4) 0.0016(5) C4 0.0286(9) 0.0216(11) 0.0338(10) 0.0098(8) -0.0141(7) -0.0033(8) P5 0.01417(15) 0.0135(2) 0.01364(15) -0.00230(14) 0.00154(12) -0.00211(14) O5 0.0182(5) 0.0161(7) 0.0188(5) -0.0056(5) 0.0037(4) -0.0009(5) C5 0.0248(8) 0.0308(13) 0.0257(8) 0.0118(8) -0.0071(6) -0.0078(8) C6 0.0187(7) 0.0253(11) 0.0188(7) 0.0051(7) -0.0035(5) -0.0051(7) C7 0.0143(6) 0.0139(8) 0.0149(6) -0.0003(5) -0.0032(4) -0.0002(5) C8 0.0141(6) 0.0215(10) 0.0175(6) -0.0008(6) -0.0021(5) -0.0007(6) C9 0.0152(6) 0.0263(11) 0.0248(8) 0.0019(7) -0.0043(5) -0.0045(7) C10 0.0215(7) 0.0210(10) 0.0276(8) 0.0035(7) -0.0085(6) -0.0075(7) C11 0.0269(8) 0.0168(10) 0.0236(8) -0.0027(7) -0.0076(6) -0.0015(7) C12 0.0204(7) 0.0157(9) 0.0175(6) -0.0020(6) -0.0031(5) 0.0003(6) C13 0.0126(5) 0.0144(8) 0.0159(6) 0.0012(5) 0.0012(4) -0.0003(5) C14 0.0178(6) 0.0143(8) 0.0188(6) 0.0003(6) 0.0037(5) -0.0004(6) C15 0.0200(7) 0.0152(9) 0.0231(7) 0.0022(6) 0.0050(6) 0.0025(6) C16 0.0207(7) 0.0160(9) 0.0210(7) 0.0048(6) 0.0025(5) 0.0009(6) C17 0.0189(7) 0.0201(10) 0.0185(7) 0.0041(6) 0.0045(5) 0.0004(6) C18 0.0160(6) 0.0169(9) 0.0186(6) 0.0012(6) 0.0034(5) 0.0006(6) C19 0.0137(6) 0.0161(9) 0.0183(6) 0.0008(6) -0.0026(5) -0.0025(5) C20 0.0171(7) 0.0219(11) 0.0368(10) -0.0073(8) -0.0076(7) 0.0020(7) C21 0.0187(8) 0.0275(13) 0.0481(12) -0.0073(10) -0.0132(8) 0.0024(8) C22 0.0220(8) 0.0258(12) 0.0359(10) -0.0010(9) -0.0124(7) -0.0049(7) C23 0.0203(7) 0.0228(11) 0.0216(7) -0.0025(7) -0.0016(6) -0.0069(7) C24 0.0154(6) 0.0211(10) 0.0204(7) -0.0034(6) 0.0012(5) -0.0021(6) C25 0.0158(6) 0.0112(8) 0.0149(6) -0.0005(5) -0.0020(4) 0.0006(5) C26 0.0168(6) 0.0163(9) 0.0220(7) -0.0014(6) -0.0001(5) -0.0012(6) C27 0.0196(7) 0.0172(10) 0.0276(8) -0.0019(7) -0.0023(6) -0.0035(6) C28 0.0249(8) 0.0183(10) 0.0271(8) -0.0048(7) -0.0059(6) -0.0018(7) C29 0.0252(8) 0.0185(10) 0.0223(7) -0.0068(7) -0.0024(6) 0.0021(7) C30 0.0194(7) 0.0166(9) 0.0171(6) -0.0024(6) -0.0007(5) 0.0020(6) C31 0.0175(6) 0.0182(9) 0.0155(6) -0.0010(6) -0.0036(5) 0.0048(6) C32 0.0241(8) 0.0281(12) 0.0286(9) -0.0008(8) -0.0111(7) 0.0016(8) C33 0.0365(11) 0.0411(17) 0.0321(10) -0.0070(10) -0.0203(9) 0.0123(11) C34 0.0514(14) 0.0497(19) 0.0202(8) 0.0001(10) -0.0113(9) 0.0254(13) C35 0.0444(13) 0.057(2) 0.0209(9) 0.0129(10) 0.0030(8) 0.0167(13) C36 0.0260(8) 0.0408(15) 0.0199(7) 0.0079(8) 0.0012(6) 0.0058(9) C37 0.0126(6) 0.0223(10) 0.0197(6) 0.0036(6) 0.0000(5) -0.0018(6) C38 0.0209(7) 0.0319(13) 0.0211(7) -0.0024(7) -0.0030(6) 0.0051(7) C39 0.0269(9) 0.0456(17) 0.0265(9) -0.0026(9) -0.0091(7) 0.0004(10) C40 0.0289(10) 0.0475(18) 0.0354(11) 0.0143(11) -0.0142(8) -0.0057(10) C41 0.0335(11) 0.0310(15) 0.0523(14) 0.0209(12) -0.0188(10) -0.0071(10) C42 0.0255(8) 0.0202(11) 0.0384(10) 0.0094(9) -0.0104(7) -0.0046(7) C43 0.0115(5) 0.0171(9) 0.0169(6) 0.0008(6) 0.0019(4) 0.0002(5) C44 0.0138(6) 0.0205(9) 0.0163(6) -0.0004(6) 0.0026(5) 0.0001(6) C45 0.0158(6) 0.0247(11) 0.0174(6) 0.0017(6) 0.0039(5) -0.0007(6) C46 0.0144(6) 0.0246(11) 0.0228(7) 0.0063(7) 0.0023(5) -0.0017(6) C47 0.0180(7) 0.0188(10) 0.0298(8) -0.0001(7) 0.0060(6) -0.0014(6) C48 0.0169(6) 0.0194(10) 0.0262(8) -0.0022(7) 0.0078(6) -0.0018(6) C49 0.0182(6) 0.0162(9) 0.0176(6) -0.0049(6) -0.0017(5) -0.0012(6) C50 0.0251(8) 0.0184(10) 0.0193(7) -0.0013(6) -0.0016(6) -0.0018(7) C51 0.0377(10) 0.0220(11) 0.0221(8) -0.0027(7) -0.0088(7) 0.0037(8) C52 0.0325(10) 0.0260(12) 0.0350(10) -0.0074(9) -0.0165(8) 0.0092(9) C53 0.0200(8) 0.0276(12) 0.0370(10) -0.0112(9) -0.0083(7) 0.0059(7) C54 0.0173(7) 0.0223(10) 0.0255(8) -0.0090(7) -0.0017(6) 0.0007(6) C55 0.0228(7) 0.0162(9) 0.0172(6) -0.0019(6) 0.0030(5) -0.0058(6) C56 0.0375(11) 0.0228(12) 0.0364(11) 0.0087(9) -0.0133(9) -0.0096(9) C57 0.0640(17) 0.0269(15) 0.0389(12) 0.0111(11) -0.0208(12) -0.0115(13) C58 0.080(2) 0.0267(15) 0.0261(10) 0.0056(9) 0.0059(11) -0.0184(14) C59 0.0464(14) 0.0287(15) 0.0481(14) 0.0019(11) 0.0210(11) -0.0143(11) C60 0.0260(8) 0.0212(11) 0.0353(10) -0.0022(8) 0.0101(7) -0.0056(8) _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 P3 2.2999(5) . ? Rh1 P1 2.3025(4) . ? Rh1 P2 2.3124(5) . ? Rh1 Cl2 2.4355(4) . ? Rh1 Cl3 2.4855(5) . ? Rh1 Cl1 2.4918(4) . ? Cl1 Rh2 2.5270(5) . ? P1 O1 1.5903(13) . ? P1 C7 1.8063(18) . ? P1 C1 1.8164(19) . ? C1 C6 1.402(2) . ? C1 C2 1.405(3) . ? Rh2 P5 2.2703(5) . ? Rh2 P4 2.2795(5) . ? Rh2 Cl4 2.3121(4) . ? Rh2 Cl3 2.3650(4) . ? Rh2 Cl2 2.4788(4) . ? P2 O2 1.5572(13) . ? P2 C13 1.8143(19) . ? P2 C19 1.8182(16) . ? C2 C3 1.389(3) . ? P3 O3 1.5828(13) . ? P3 C31 1.8138(17) . ? P3 C25 1.8168(18) . ? C3 C4 1.392(3) . ? P4 O4 1.5507(16) . ? P4 C43 1.8222(19) . ? P4 C37 1.8241(17) . ? C4 C5 1.389(4) . ? P5 O5 1.5454(13) . ? P5 C49 1.8162(17) . ? P5 C55 1.823(2) . ? C5 C6 1.391(3) . ? C7 C8 1.397(2) . ? C7 C12 1.400(3) . ? C8 C9 1.395(3) . ? C9 C10 1.385(3) . ? C10 C11 1.393(3) . ? C11 C12 1.392(3) . ? C13 C14 1.398(3) . ? C13 C18 1.402(2) . ? C14 C15 1.387(3) . ? C15 C16 1.394(2) . ? C16 C17 1.389(3) . ? C17 C18 1.388(3) . ? C19 C24 1.392(3) . ? C19 C20 1.404(3) . ? C20 C21 1.398(3) . ? C21 C22 1.380(3) . ? C22 C23 1.401(3) . ? C23 C24 1.392(2) . ? C25 C26 1.403(2) . ? C25 C30 1.405(2) . ? C26 C27 1.392(3) . ? C27 C28 1.394(3) . ? C28 C29 1.386(3) . ? C29 C30 1.393(3) . ? C31 C36 1.392(3) . ? C31 C32 1.399(3) . ? C32 C33 1.393(3) . ? C33 C34 1.380(4) . ? C34 C35 1.392(4) . ? C35 C36 1.395(3) . ? C37 C42 1.391(3) . ? C37 C38 1.392(3) . ? C38 C39 1.396(3) . ? C39 C40 1.381(4) . ? C40 C41 1.387(4) . ? C41 C42 1.398(3) . ? C43 C48 1.390(3) . ? C43 C44 1.402(2) . ? C44 C45 1.394(3) . ? C45 C46 1.382(3) . ? C46 C47 1.395(3) . ? C47 C48 1.396(3) . ? C49 C50 1.399(2) . ? C49 C54 1.399(2) . ? C50 C51 1.397(3) . ? C51 C52 1.387(3) . ? C52 C53 1.392(3) . ? C53 C54 1.396(3) . ? C55 C60 1.396(3) . ? C55 C56 1.399(3) . ? C56 C57 1.379(4) . ? C57 C58 1.374(4) . ? C58 C59 1.382(5) . ? C59 C60 1.393(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 P3 Rh1 P1 91.966(16) . . ? P3 Rh1 P2 91.658(17) . . ? P1 Rh1 P2 86.615(16) . . ? P3 Rh1 Cl2 90.829(15) . . ? P1 Rh1 Cl2 177.107(18) . . ? P2 Rh1 Cl2 92.561(15) . . ? P3 Rh1 Cl3 165.733(14) . . ? P1 Rh1 Cl3 97.173(15) . . ? P2 Rh1 Cl3 99.770(17) . . ? Cl2 Rh1 Cl3 80.227(14) . . ? P3 Rh1 Cl1 88.787(16) . . ? P1 Rh1 Cl1 99.918(15) . . ? P2 Rh1 Cl1 173.435(14) . . ? Cl2 Rh1 Cl1 80.883(14) . . ? Cl3 Rh1 Cl1 78.887(15) . . ? Rh1 Cl1 Rh2 81.927(14) . . ? O1 P1 C7 101.82(8) . . ? O1 P1 C1 104.44(8) . . ? C7 P1 C1 104.96(8) . . ? O1 P1 Rh1 112.73(5) . . ? C7 P1 Rh1 117.64(5) . . ? C1 P1 Rh1 113.75(6) . . ? C6 C1 C2 119.00(18) . . ? C6 C1 P1 119.09(15) . . ? C2 C1 P1 121.87(13) . . ? P5 Rh2 P4 92.549(17) . . ? P5 Rh2 Cl4 85.791(17) . . ? P4 Rh2 Cl4 88.495(16) . . ? P5 Rh2 Cl3 98.869(17) . . ? P4 Rh2 Cl3 95.873(15) . . ? Cl4 Rh2 Cl3 173.438(17) . . ? P5 Rh2 Cl2 91.079(15) . . ? P4 Rh2 Cl2 175.934(15) . . ? Cl4 Rh2 Cl2 93.604(14) . . ? Cl3 Rh2 Cl2 81.745(13) . . ? P5 Rh2 Cl1 170.425(14) . . ? P4 Rh2 Cl1 97.022(16) . . ? Cl4 Rh2 Cl1 94.166(16) . . ? Cl3 Rh2 Cl1 80.467(16) . . ? Cl2 Rh2 Cl1 79.364(13) . . ? Rh1 Cl2 Rh2 84.059(12) . . ? O2 P2 C13 105.06(8) . . ? O2 P2 C19 105.45(8) . . ? C13 P2 C19 102.12(8) . . ? O2 P2 Rh1 109.82(5) . . ? C13 P2 Rh1 117.62(5) . . ? C19 P2 Rh1 115.58(6) . . ? C3 C2 C1 120.32(18) . . ? Rh2 Cl3 Rh1 85.390(15) . . ? O3 P3 C31 101.93(8) . . ? O3 P3 C25 103.29(8) . . ? C31 P3 C25 105.27(9) . . ? O3 P3 Rh1 113.97(6) . . ? C31 P3 Rh1 113.03(6) . . ? C25 P3 Rh1 117.66(6) . . ? C2 C3 C4 120.2(2) . . ? O4 P4 C43 105.23(8) . . ? O4 P4 C37 103.12(9) . . ? C43 P4 C37 102.81(8) . . ? O4 P4 Rh2 114.53(5) . . ? C43 P4 Rh2 114.51(6) . . ? C37 P4 Rh2 115.19(6) . . ? C5 C4 C3 119.7(2) . . ? O5 P5 C49 104.15(8) . . ? O5 P5 C55 104.46(9) . . ? C49 P5 C55 107.95(9) . . ? O5 P5 Rh2 114.88(6) . . ? C49 P5 Rh2 112.77(7) . . ? C55 P5 Rh2 111.93(6) . . ? C4 C5 C6 120.54(19) . . ? C5 C6 C1 120.08(19) . . ? C8 C7 C12 119.90(16) . . ? C8 C7 P1 119.70(14) . . ? C12 C7 P1 120.37(13) . . ? C9 C8 C7 119.69(18) . . ? C10 C9 C8 120.20(18) . . ? C9 C10 C11 120.41(18) . . ? C12 C11 C10 119.77(19) . . ? C11 C12 C7 119.99(17) . . ? C14 C13 C18 119.61(17) . . ? C14 C13 P2 124.29(12) . . ? C18 C13 P2 115.97(14) . . ? C15 C14 C13 119.99(16) . . ? C14 C15 C16 120.40(18) . . ? C17 C16 C15 119.65(18) . . ? C18 C17 C16 120.53(16) . . ? C17 C18 C13 119.81(18) . . ? C24 C19 C20 119.72(16) . . ? C24 C19 P2 121.46(13) . . ? C20 C19 P2 118.40(15) . . ? C21 C20 C19 119.4(2) . . ? C22 C21 C20 120.7(2) . . ? C21 C22 C23 120.05(17) . . ? C24 C23 C22 119.6(2) . . ? C23 C24 C19 120.49(18) . . ? C26 C25 C30 119.05(17) . . ? C26 C25 P3 123.23(13) . . ? C30 C25 P3 117.63(13) . . ? C27 C26 C25 120.08(17) . . ? C26 C27 C28 120.40(18) . . ? C29 C28 C27 119.8(2) . . ? C28 C29 C30 120.33(18) . . ? C29 C30 C25 120.23(17) . . ? C36 C31 C32 119.40(17) . . ? C36 C31 P3 123.45(14) . . ? C32 C31 P3 117.02(15) . . ? C33 C32 C31 120.0(2) . . ? C34 C33 C32 120.4(2) . . ? C33 C34 C35 120.0(2) . . ? C34 C35 C36 119.9(3) . . ? C31 C36 C35 120.2(2) . . ? C42 C37 C38 119.38(18) . . ? C42 C37 P4 118.89(16) . . ? C38 C37 P4 121.56(17) . . ? C37 C38 C39 120.4(2) . . ? C40 C39 C38 120.0(2) . . ? C39 C40 C41 120.1(2) . . ? C40 C41 C42 120.1(3) . . ? C37 C42 C41 120.0(2) . . ? C48 C43 C44 119.37(17) . . ? C48 C43 P4 124.46(12) . . ? C44 C43 P4 116.14(15) . . ? C45 C44 C43 119.97(19) . . ? C46 C45 C44 120.43(16) . . ? C45 C46 C47 119.89(18) . . ? C46 C47 C48 119.9(2) . . ? C43 C48 C47 120.35(17) . . ? C50 C49 C54 118.97(16) . . ? C50 C49 P5 117.44(13) . . ? C54 C49 P5 123.52(14) . . ? C51 C50 C49 120.38(18) . . ? C52 C51 C50 120.06(19) . . ? C51 C52 C53 120.03(18) . . ? C52 C53 C54 120.0(2) . . ? C53 C54 C49 120.39(18) . . ? C60 C55 C56 117.8(2) . . ? C60 C55 P5 126.66(16) . . ? C56 C55 P5 115.35(15) . . ? C57 C56 C55 121.7(2) . . ? C58 C57 C56 120.1(3) . . ? C57 C58 C59 119.5(3) . . ? C58 C59 C60 120.9(2) . . ? C59 C60 C55 120.0(2) . . ? 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 P3 Rh1 Cl1 Rh2 -132.878(13) . . . . ? P1 Rh1 Cl1 Rh2 135.338(15) . . . . ? P2 Rh1 Cl1 Rh2 -38.91(15) . . . . ? Cl2 Rh1 Cl1 Rh2 -41.843(13) . . . . ? Cl3 Rh1 Cl1 Rh2 39.896(12) . . . . ? P3 Rh1 P1 O1 46.97(7) . . . . ? P2 Rh1 P1 O1 -44.58(7) . . . . ? Cl2 Rh1 P1 O1 -118.1(3) . . . . ? Cl3 Rh1 P1 O1 -144.01(7) . . . . ? Cl1 Rh1 P1 O1 136.08(7) . . . . ? P3 Rh1 P1 C7 -71.07(7) . . . . ? P2 Rh1 P1 C7 -162.62(7) . . . . ? Cl2 Rh1 P1 C7 123.9(3) . . . . ? Cl3 Rh1 P1 C7 97.95(7) . . . . ? Cl1 Rh1 P1 C7 18.04(7) . . . . ? P3 Rh1 P1 C1 165.64(6) . . . . ? P2 Rh1 P1 C1 74.09(6) . . . . ? Cl2 Rh1 P1 C1 0.6(3) . . . . ? Cl3 Rh1 P1 C1 -25.34(6) . . . . ? Cl1 Rh1 P1 C1 -105.25(6) . . . . ? O1 P1 C1 C6 9.58(16) . . . . ? C7 P1 C1 C6 116.31(15) . . . . ? Rh1 P1 C1 C6 -113.73(14) . . . . ? O1 P1 C1 C2 -172.82(14) . . . . ? C7 P1 C1 C2 -66.09(16) . . . . ? Rh1 P1 C1 C2 63.87(15) . . . . ? Rh1 Cl1 Rh2 P5 44.69(10) . . . . ? Rh1 Cl1 Rh2 P4 -136.929(15) . . . . ? Rh1 Cl1 Rh2 Cl4 134.077(13) . . . . ? Rh1 Cl1 Rh2 Cl3 -42.119(12) . . . . ? Rh1 Cl1 Rh2 Cl2 41.185(12) . . . . ? P3 Rh1 Cl2 Rh2 131.246(15) . . . . ? P1 Rh1 Cl2 Rh2 -63.7(3) . . . . ? P2 Rh1 Cl2 Rh2 -137.057(16) . . . . ? Cl3 Rh1 Cl2 Rh2 -37.579(13) . . . . ? Cl1 Rh1 Cl2 Rh2 42.608(14) . . . . ? P5 Rh2 Cl2 Rh1 138.465(16) . . . . ? P4 Rh2 Cl2 Rh1 -14.7(3) . . . . ? Cl4 Rh2 Cl2 Rh1 -135.684(16) . . . . ? Cl3 Rh2 Cl2 Rh1 39.660(15) . . . . ? Cl1 Rh2 Cl2 Rh1 -42.117(13) . . . . ? P3 Rh1 P2 O2 -38.29(5) . . . . ? P1 Rh1 P2 O2 53.59(5) . . . . ? Cl2 Rh1 P2 O2 -129.19(5) . . . . ? Cl3 Rh1 P2 O2 150.29(5) . . . . ? Cl1 Rh1 P2 O2 -132.09(14) . . . . ? P3 Rh1 P2 C13 -158.30(6) . . . . ? P1 Rh1 P2 C13 -66.43(6) . . . . ? Cl2 Rh1 P2 C13 110.80(6) . . . . ? Cl3 Rh1 P2 C13 30.28(6) . . . . ? Cl1 Rh1 P2 C13 107.90(15) . . . . ? P3 Rh1 P2 C19 80.83(7) . . . . ? P1 Rh1 P2 C19 172.70(8) . . . . ? Cl2 Rh1 P2 C19 -10.07(8) . . . . ? Cl3 Rh1 P2 C19 -90.59(7) . . . . ? Cl1 Rh1 P2 C19 -12.97(18) . . . . ? C6 C1 C2 C3 1.9(3) . . . . ? P1 C1 C2 C3 -175.66(15) . . . . ? P5 Rh2 Cl3 Rh1 -128.419(15) . . . . ? P4 Rh2 Cl3 Rh1 138.066(16) . . . . ? Cl4 Rh2 Cl3 Rh1 6.53(13) . . . . ? Cl2 Rh2 Cl3 Rh1 -38.613(13) . . . . ? Cl1 Rh2 Cl3 Rh1 41.904(12) . . . . ? P3 Rh1 Cl3 Rh2 -12.21(6) . . . . ? P1 Rh1 Cl3 Rh2 -141.654(15) . . . . ? P2 Rh1 Cl3 Rh2 130.566(13) . . . . ? Cl2 Rh1 Cl3 Rh2 39.629(13) . . . . ? Cl1 Rh1 Cl3 Rh2 -42.900(12) . . . . ? P1 Rh1 P3 O3 -81.65(6) . . . . ? P2 Rh1 P3 O3 5.02(6) . . . . ? Cl2 Rh1 P3 O3 97.60(6) . . . . ? Cl3 Rh1 P3 O3 148.41(7) . . . . ? Cl1 Rh1 P3 O3 178.47(6) . . . . ? P1 Rh1 P3 C31 162.58(7) . . . . ? P2 Rh1 P3 C31 -110.75(7) . . . . ? Cl2 Rh1 P3 C31 -18.17(7) . . . . ? Cl3 Rh1 P3 C31 32.64(9) . . . . ? Cl1 Rh1 P3 C31 62.69(7) . . . . ? P1 Rh1 P3 C25 39.49(6) . . . . ? P2 Rh1 P3 C25 126.16(6) . . . . ? Cl2 Rh1 P3 C25 -141.25(6) . . . . ? Cl3 Rh1 P3 C25 -90.45(8) . . . . ? Cl1 Rh1 P3 C25 -60.39(6) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? P5 Rh2 P4 O4 0.91(7) . . . . ? Cl4 Rh2 P4 O4 -84.81(7) . . . . ? Cl3 Rh2 P4 O4 100.10(7) . . . . ? Cl2 Rh2 P4 O4 154.0(2) . . . . ? Cl1 Rh2 P4 O4 -178.82(6) . . . . ? P5 Rh2 P4 C43 122.61(6) . . . . ? Cl4 Rh2 P4 C43 36.89(6) . . . . ? Cl3 Rh2 P4 C43 -138.20(6) . . . . ? Cl2 Rh2 P4 C43 -84.3(3) . . . . ? Cl1 Rh2 P4 C43 -57.12(6) . . . . ? P5 Rh2 P4 C37 -118.46(8) . . . . ? Cl4 Rh2 P4 C37 155.82(8) . . . . ? Cl3 Rh2 P4 C37 -19.27(8) . . . . ? Cl2 Rh2 P4 C37 34.7(3) . . . . ? Cl1 Rh2 P4 C37 61.81(8) . . . . ? C2 C3 C4 C5 -2.8(3) . . . . ? P4 Rh2 P5 O5 -22.21(7) . . . . ? Cl4 Rh2 P5 O5 66.09(6) . . . . ? Cl3 Rh2 P5 O5 -118.56(6) . . . . ? Cl2 Rh2 P5 O5 159.62(6) . . . . ? Cl1 Rh2 P5 O5 156.18(10) . . . . ? P4 Rh2 P5 C49 -141.35(6) . . . . ? Cl4 Rh2 P5 C49 -53.05(6) . . . . ? Cl3 Rh2 P5 C49 122.30(6) . . . . ? Cl2 Rh2 P5 C49 40.49(6) . . . . ? Cl1 Rh2 P5 C49 37.04(12) . . . . ? P4 Rh2 P5 C55 96.69(7) . . . . ? Cl4 Rh2 P5 C55 -175.01(7) . . . . ? Cl3 Rh2 P5 C55 0.34(7) . . . . ? Cl2 Rh2 P5 C55 -81.47(7) . . . . ? Cl1 Rh2 P5 C55 -84.91(12) . . . . ? C3 C4 C5 C6 2.4(3) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C2 C1 C6 C5 -2.3(3) . . . . ? P1 C1 C6 C5 175.37(15) . . . . ? O1 P1 C7 C8 -177.61(14) . . . . ? C1 P1 C7 C8 73.74(15) . . . . ? Rh1 P1 C7 C8 -53.88(15) . . . . ? O1 P1 C7 C12 4.23(16) . . . . ? C1 P1 C7 C12 -104.42(15) . . . . ? Rh1 P1 C7 C12 127.95(13) . . . . ? C12 C7 C8 C9 -2.0(3) . . . . ? P1 C7 C8 C9 179.81(14) . . . . ? C7 C8 C9 C10 1.9(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C9 C10 C11 C12 -1.4(3) . . . . ? C10 C11 C12 C7 1.2(3) . . . . ? C8 C7 C12 C11 0.4(3) . . . . ? P1 C7 C12 C11 178.60(14) . . . . ? O2 P2 C13 C14 -167.98(14) . . . . ? C19 P2 C13 C14 82.14(15) . . . . ? Rh1 P2 C13 C14 -45.50(16) . . . . ? O2 P2 C13 C18 16.17(14) . . . . ? C19 P2 C13 C18 -93.70(14) . . . . ? Rh1 P2 C13 C18 138.65(11) . . . . ? C18 C13 C14 C15 -1.2(3) . . . . ? P2 C13 C14 C15 -176.93(14) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? C14 C15 C16 C17 0.3(3) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C16 C17 C18 C13 0.2(3) . . . . ? C14 C13 C18 C17 0.8(2) . . . . ? P2 C13 C18 C17 176.86(14) . . . . ? O2 P2 C19 C24 -163.91(15) . . . . ? C13 P2 C19 C24 -54.33(17) . . . . ? Rh1 P2 C19 C24 74.60(17) . . . . ? O2 P2 C19 C20 8.57(19) . . . . ? C13 P2 C19 C20 118.14(17) . . . . ? Rh1 P2 C19 C20 -112.92(16) . . . . ? C24 C19 C20 C21 -1.5(3) . . . . ? P2 C19 C20 C21 -174.13(19) . . . . ? C19 C20 C21 C22 -0.3(4) . . . . ? C20 C21 C22 C23 1.4(4) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C22 C23 C24 C19 -1.2(3) . . . . ? C20 C19 C24 C23 2.3(3) . . . . ? P2 C19 C24 C23 174.68(15) . . . . ? O3 P3 C25 C26 -171.53(15) . . . . ? C31 P3 C25 C26 -64.99(16) . . . . ? Rh1 P3 C25 C26 61.95(16) . . . . ? O3 P3 C25 C30 5.02(16) . . . . ? C31 P3 C25 C30 111.56(14) . . . . ? Rh1 P3 C25 C30 -121.51(13) . . . . ? C30 C25 C26 C27 -2.9(3) . . . . ? P3 C25 C26 C27 173.65(15) . . . . ? C25 C26 C27 C28 1.5(3) . . . . ? C26 C27 C28 C29 0.9(3) . . . . ? C27 C28 C29 C30 -2.0(3) . . . . ? C28 C29 C30 C25 0.6(3) . . . . ? C26 C25 C30 C29 1.8(3) . . . . ? P3 C25 C30 C29 -174.90(14) . . . . ? O3 P3 C31 C36 145.26(19) . . . . ? C25 P3 C31 C36 37.7(2) . . . . ? Rh1 P3 C31 C36 -92.0(2) . . . . ? O3 P3 C31 C32 -30.63(19) . . . . ? C25 P3 C31 C32 -138.16(17) . . . . ? Rh1 P3 C31 C32 92.13(17) . . . . ? C36 C31 C32 C33 -1.7(3) . . . . ? P3 C31 C32 C33 174.33(19) . . . . ? C31 C32 C33 C34 1.2(4) . . . . ? C32 C33 C34 C35 -0.4(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C32 C31 C36 C35 1.4(4) . . . . ? P3 C31 C36 C35 -174.4(2) . . . . ? C34 C35 C36 C31 -0.6(4) . . . . ? O4 P4 C37 C42 -13.27(17) . . . . ? C43 P4 C37 C42 -122.52(16) . . . . ? Rh2 P4 C37 C42 112.23(15) . . . . ? O4 P4 C37 C38 161.98(15) . . . . ? C43 P4 C37 C38 52.73(17) . . . . ? Rh2 P4 C37 C38 -72.52(16) . . . . ? C42 C37 C38 C39 -1.3(3) . . . . ? P4 C37 C38 C39 -176.52(16) . . . . ? C37 C38 C39 C40 0.7(3) . . . . ? C38 C39 C40 C41 0.6(4) . . . . ? C39 C40 C41 C42 -1.2(4) . . . . ? C38 C37 C42 C41 0.7(3) . . . . ? P4 C37 C42 C41 176.03(18) . . . . ? C40 C41 C42 C37 0.6(4) . . . . ? O4 P4 C43 C48 176.78(15) . . . . ? C37 P4 C43 C48 -75.56(17) . . . . ? Rh2 P4 C43 C48 50.13(16) . . . . ? O4 P4 C43 C44 -5.19(14) . . . . ? C37 P4 C43 C44 102.47(14) . . . . ? Rh2 P4 C43 C44 -131.84(11) . . . . ? C48 C43 C44 C45 0.8(2) . . . . ? P4 C43 C44 C45 -177.34(13) . . . . ? C43 C44 C45 C46 1.2(3) . . . . ? C44 C45 C46 C47 -2.1(3) . . . . ? C45 C46 C47 C48 1.0(3) . . . . ? C44 C43 C48 C47 -1.9(3) . . . . ? P4 C43 C48 C47 176.07(14) . . . . ? C46 C47 C48 C43 1.0(3) . . . . ? O5 P5 C49 C50 -20.13(19) . . . . ? C55 P5 C49 C50 -130.76(17) . . . . ? Rh2 P5 C49 C50 105.07(16) . . . . ? O5 P5 C49 C54 156.89(18) . . . . ? C55 P5 C49 C54 46.3(2) . . . . ? Rh2 P5 C49 C54 -77.91(19) . . . . ? C54 C49 C50 C51 -2.1(3) . . . . ? P5 C49 C50 C51 175.11(18) . . . . ? C49 C50 C51 C52 -1.6(4) . . . . ? C50 C51 C52 C53 2.8(4) . . . . ? C51 C52 C53 C54 -0.3(4) . . . . ? C52 C53 C54 C49 -3.5(4) . . . . ? C50 C49 C54 C53 4.6(3) . . . . ? P5 C49 C54 C53 -172.39(19) . . . . ? O5 P5 C55 C60 -116.13(19) . . . . ? C49 P5 C55 C60 -5.7(2) . . . . ? Rh2 P5 C55 C60 118.97(18) . . . . ? O5 P5 C55 C56 58.55(18) . . . . ? C49 P5 C55 C56 168.98(17) . . . . ? Rh2 P5 C55 C56 -66.35(18) . . . . ? C60 C55 C56 C57 -0.8(4) . . . . ? P5 C55 C56 C57 -176.0(2) . . . . ? C55 C56 C57 C58 -0.5(5) . . . . ? C56 C57 C58 C59 0.9(5) . . . . ? C57 C58 C59 C60 0.0(5) . . . . ? C58 C59 C60 C55 -1.3(4) . . . . ? C56 C55 C60 C59 1.6(3) . . . . ? P5 C55 C60 C59 176.20(19) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 39.46 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.842 _refine_diff_density_min -1.977 _refine_diff_density_rms 0.147