Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_contact_author_name 'Prof Helmut Werner' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Inorganic Chemistry Universitaet Wuerzburg Am Hubland Wuerzburg D-97074 GERMANY ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_section_title ; HELMUT.WERNER@MAIL.UNI-WUERZBURG.DE ; loop_ _publ_author_name 'Helmut Werner' 'Carsten D. Brandt' 'Thomas Pechmann' data_tp4cb _database_code_depnum_ccdc_archive 'CCDC 178267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H70 Cl4 P2 Rh4' _chemical_formula_weight 1526.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 22.2854(11) _cell_length_b 15.1150(7) _cell_length_c 19.2895(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.8780(10) _cell_angle_gamma 90.00 _cell_volume 6358.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8804 _cell_measurement_theta_min 2.303 _cell_measurement_theta_max 28.246 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldick 2000)' _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 Smart Apex with D8-Goniometer' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60158 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11183 _reflns_number_gt 10525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-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^)+(0.0265P)^2^+4.0856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 11183 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.005 _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 0.083229(8) 0.917474(11) 0.218533(8) 0.02346(5) Uani 1 1 d . . . Rh2 Rh 0.039610(7) 0.954659(10) 0.091590(8) 0.01958(5) Uani 1 1 d . . . Rh3 Rh 0.386688(8) 1.418240(11) 0.294523(9) 0.02460(5) Uani 1 1 d . . . Rh4 Rh 0.452577(7) 1.453846(11) 0.412466(8) 0.02129(5) Uani 1 1 d . . . P1 P 0.03496(3) 1.06197(4) 0.17937(3) 0.02857(13) Uani 1 1 d . . . P2 P 0.44177(3) 1.55656(4) 0.31656(3) 0.02816(13) Uani 1 1 d . . . Cl1 Cl 0.12648(3) 0.85404(4) 0.32610(3) 0.04055(15) Uani 1 1 d . . . Cl2 Cl -0.06411(2) 0.97620(4) 0.01488(3) 0.02888(12) Uani 1 1 d . . . Cl3 Cl 0.32639(3) 1.36621(5) 0.19140(3) 0.04618(16) Uani 1 1 d . . . Cl4 Cl 0.44622(2) 1.56270(4) 0.50765(3) 0.03216(13) Uani 1 1 d . . . C1 C 0.12832(9) 0.92869(14) 0.14013(11) 0.0231(4) Uani 1 1 d . . . C2 C 0.01416(9) 0.85887(14) 0.15517(10) 0.0227(4) Uani 1 1 d . . . C3 C -0.04607(12) 1.08124(17) 0.17539(14) 0.0426(6) Uani 1 1 d . . . H3A H -0.0525 1.1433 0.1866 0.064 Uiso 1 1 calc R . . H3B H -0.0603 1.0430 0.2098 0.064 Uiso 1 1 calc R . . H3C H -0.0692 1.0678 0.1276 0.064 Uiso 1 1 calc R . . C4 C 0.06518(14) 1.09995(19) 0.27044(14) 0.0487(7) Uani 1 1 d . . . H4A H 0.1101 1.0980 0.2802 0.073 Uiso 1 1 calc R . . H4B H 0.0500 1.0613 0.3038 0.073 Uiso 1 1 calc R . . H4C H 0.0516 1.1608 0.2758 0.073 Uiso 1 1 calc R . . C5 C 0.05862(17) 1.15548(17) 0.13229(16) 0.0598(9) Uani 1 1 d . . . H5A H 0.0338 1.1575 0.0841 0.090 Uiso 1 1 calc R . . H5B H 0.1020 1.1491 0.1302 0.090 Uiso 1 1 calc R . . H5C H 0.0529 1.2104 0.1572 0.090 Uiso 1 1 calc R . . C10 C 0.15634(10) 0.84588(14) 0.11693(12) 0.0262(5) Uani 1 1 d . . . C11 C 0.13977(11) 0.81196(15) 0.04874(12) 0.0319(5) Uani 1 1 d . . . H11 H 0.1071 0.8383 0.0158 0.038 Uiso 1 1 calc R . . C12 C 0.17075(13) 0.73946(17) 0.02839(15) 0.0438(7) Uani 1 1 d . . . H12 H 0.1591 0.7167 -0.0183 0.053 Uiso 1 1 calc R . . C13 C 0.21814(13) 0.70081(18) 0.07574(17) 0.0498(7) Uani 1 1 d . . . H13 H 0.2397 0.6521 0.0614 0.060 Uiso 1 1 calc R . . C14 C 0.23423(12) 0.73266(17) 0.14370(17) 0.0501(7) Uani 1 1 d . . . H14 H 0.2663 0.7050 0.1767 0.060 Uiso 1 1 calc R . . C15 C 0.20408(11) 0.80480(16) 0.16446(14) 0.0391(6) Uani 1 1 d . . . H15 H 0.2159 0.8267 0.2115 0.047 Uiso 1 1 calc R . . C20 C 0.17606(10) 1.00065(14) 0.15441(12) 0.0282(5) Uani 1 1 d . . . C21 C 0.20161(12) 1.02785(19) 0.22235(14) 0.0453(7) Uani 1 1 d . . . H21 H 0.1880 1.0022 0.2613 0.054 Uiso 1 1 calc R . . C22 C 0.24714(15) 1.0925(2) 0.23458(19) 0.0663(10) Uani 1 1 d . . . H22 H 0.2643 1.1105 0.2817 0.080 Uiso 1 1 calc R . . C23 C 0.26725(14) 1.1301(2) 0.1787(2) 0.0636(9) Uani 1 1 d . . . H23 H 0.2974 1.1755 0.1869 0.076 Uiso 1 1 calc R . . C24 C 0.24358(13) 1.10198(19) 0.11095(18) 0.0538(8) Uani 1 1 d . . . H24 H 0.2580 1.1272 0.0723 0.065 Uiso 1 1 calc R . . C25 C 0.19889(11) 1.03722(17) 0.09863(14) 0.0395(6) Uani 1 1 d . . . H25 H 0.1835 1.0173 0.0516 0.047 Uiso 1 1 calc R . . C30 C 0.02430(9) 0.77013(14) 0.12485(11) 0.0245(4) Uani 1 1 d . . . C31 C 0.06362(10) 0.70780(15) 0.16355(13) 0.0308(5) Uani 1 1 d . . . H31 H 0.0854 0.7220 0.2099 0.037 Uiso 1 1 calc R . . C32 C 0.07122(12) 0.62558(16) 0.13514(15) 0.0419(6) Uani 1 1 d . . . H32 H 0.0983 0.5839 0.1621 0.050 Uiso 1 1 calc R . . C33 C 0.03977(13) 0.60363(18) 0.06800(17) 0.0500(7) Uani 1 1 d . . . H33 H 0.0450 0.5470 0.0488 0.060 Uiso 1 1 calc R . . C34 C 0.00095(13) 0.66427(18) 0.02930(15) 0.0483(7) Uani 1 1 d . . . H34 H -0.0208 0.6493 -0.0169 0.058 Uiso 1 1 calc R . . C35 C -0.00684(11) 0.74717(16) 0.05679(13) 0.0352(5) Uani 1 1 d . . . H35 H -0.0336 0.7887 0.0291 0.042 Uiso 1 1 calc R . . C40 C -0.04354(10) 0.86377(14) 0.18443(11) 0.0245(4) Uani 1 1 d . . . C41 C -0.04015(11) 0.87276(16) 0.25696(12) 0.0326(5) Uani 1 1 d . . . H41 H -0.0011 0.8756 0.2880 0.039 Uiso 1 1 calc R . . C42 C -0.09279(12) 0.87764(18) 0.28460(13) 0.0396(6) Uani 1 1 d . . . H42 H -0.0895 0.8845 0.3342 0.047 Uiso 1 1 calc R . . C43 C -0.14979(11) 0.87261(18) 0.24046(14) 0.0411(6) Uani 1 1 d . . . H43 H -0.1859 0.8760 0.2594 0.049 Uiso 1 1 calc R . . C44 C -0.15390(11) 0.86263(17) 0.16841(14) 0.0391(6) Uani 1 1 d . . . H44 H -0.1930 0.8592 0.1376 0.047 Uiso 1 1 calc R . . C45 C -0.10150(10) 0.85755(15) 0.14084(12) 0.0309(5) Uani 1 1 d . . . H45 H -0.1051 0.8497 0.0913 0.037 Uiso 1 1 calc R . . C50 C 0.45249(10) 1.26273(14) 0.36392(12) 0.0283(5) Uani 1 1 d . . . C51 C 0.46951(11) 1.23285(16) 0.43338(13) 0.0365(6) Uani 1 1 d . . . H51 H 0.4886 1.2724 0.4695 0.044 Uiso 1 1 calc R . . C52 C 0.45887(13) 1.14593(17) 0.45037(15) 0.0470(7) Uani 1 1 d . . . H52 H 0.4706 1.1266 0.4981 0.056 Uiso 1 1 calc R . . C53 C 0.43149(13) 1.08719(17) 0.39880(16) 0.0455(7) Uani 1 1 d . . . H53 H 0.4241 1.0278 0.4108 0.055 Uiso 1 1 calc R . . C54 C 0.41503(12) 1.11558(16) 0.32977(15) 0.0415(6) Uani 1 1 d . . . H54 H 0.3965 1.0754 0.2939 0.050 Uiso 1 1 calc R . . C55 C 0.42526(11) 1.20201(16) 0.31216(13) 0.0349(5) Uani 1 1 d . . . H55 H 0.4136 1.2205 0.2642 0.042 Uiso 1 1 calc R . . C60 C 0.51356(11) 1.36241(15) 0.30152(13) 0.0323(5) Uani 1 1 d . . . C61 C 0.50084(13) 1.36834(16) 0.22836(14) 0.0422(6) Uani 1 1 d . . . H61 H 0.4595 1.3671 0.2031 0.051 Uiso 1 1 calc R . . C62 C 0.54827(16) 1.37611(18) 0.19122(17) 0.0547(8) Uani 1 1 d . . . H62 H 0.5390 1.3797 0.1410 0.066 Uiso 1 1 calc R . . C63 C 0.60779(16) 1.37860(19) 0.2270(2) 0.0645(10) Uani 1 1 d . . . H63 H 0.6399 1.3868 0.2019 0.077 Uiso 1 1 calc R . . C64 C 0.62121(14) 1.3692(2) 0.2991(2) 0.0658(10) Uani 1 1 d . . . H64 H 0.6628 1.3692 0.3238 0.079 Uiso 1 1 calc R . . C65 C 0.57466(12) 1.3598(2) 0.33648(16) 0.0529(8) Uani 1 1 d . . . H65 H 0.5846 1.3515 0.3864 0.064 Uiso 1 1 calc R . . C70 C 0.34788(9) 1.35134(14) 0.42597(11) 0.0243(4) Uani 1 1 d . . . C71 C 0.36784(11) 1.34784(15) 0.49931(12) 0.0321(5) Uani 1 1 d . . . H71 H 0.3905 1.3960 0.5233 0.039 Uiso 1 1 calc R . . C72 C 0.35514(12) 1.27539(16) 0.53767(13) 0.0376(6) Uani 1 1 d . . . H72 H 0.3698 1.2735 0.5875 0.045 Uiso 1 1 calc R . . C73 C 0.32123(12) 1.20593(16) 0.50357(14) 0.0402(6) Uani 1 1 d . . . H73 H 0.3119 1.1564 0.5297 0.048 Uiso 1 1 calc R . . C74 C 0.30098(12) 1.20918(16) 0.43112(13) 0.0368(6) Uani 1 1 d . . . H74 H 0.2778 1.1612 0.4076 0.044 Uiso 1 1 calc R . . C75 C 0.31367(10) 1.28048(15) 0.39206(12) 0.0287(5) Uani 1 1 d . . . H75 H 0.2992 1.2815 0.3422 0.034 Uiso 1 1 calc R . . C80 C 0.31073(10) 1.50047(14) 0.38228(12) 0.0284(5) Uani 1 1 d . . . C81 C 0.29525(12) 1.53419(17) 0.44371(14) 0.0388(6) Uani 1 1 d . . . H81 H 0.3172 1.5148 0.4887 0.047 Uiso 1 1 calc R . . C82 C 0.24860(13) 1.59522(19) 0.44005(17) 0.0519(7) Uani 1 1 d . . . H82 H 0.2393 1.6181 0.4825 0.062 Uiso 1 1 calc R . . C83 C 0.21562(13) 1.62310(19) 0.37580(18) 0.0552(8) Uani 1 1 d . . . H83 H 0.1839 1.6656 0.3737 0.066 Uiso 1 1 calc R . . C84 C 0.22865(13) 1.58941(19) 0.31454(17) 0.0522(8) Uani 1 1 d . . . H84 H 0.2053 1.6078 0.2700 0.063 Uiso 1 1 calc R . . C85 C 0.27610(11) 1.52819(17) 0.31726(14) 0.0398(6) Uani 1 1 d . . . H85 H 0.2848 1.5053 0.2745 0.048 Uiso 1 1 calc R . . C90 C 0.46270(10) 1.35625(14) 0.34290(11) 0.0258(5) Uani 1 1 d . . . C91 C 0.36010(9) 1.43178(14) 0.38565(11) 0.0232(4) Uani 1 1 d . . . C92 C 0.52152(13) 1.5898(2) 0.33738(16) 0.0590(9) Uani 1 1 d . . . H92A H 0.5265 1.6452 0.3127 0.088 Uiso 1 1 calc R . . H92B H 0.5468 1.5436 0.3221 0.088 Uiso 1 1 calc R . . H92C H 0.5345 1.5987 0.3886 0.088 Uiso 1 1 calc R . . C93 C 0.42768(15) 1.57419(18) 0.22011(13) 0.0483(7) Uani 1 1 d . . . H93A H 0.4395 1.6347 0.2103 0.072 Uiso 1 1 calc R . . H93B H 0.3840 1.5654 0.1998 0.072 Uiso 1 1 calc R . . H93C H 0.4520 1.5320 0.1989 0.072 Uiso 1 1 calc R . . C94 C 0.40158(15) 1.65191(17) 0.34159(17) 0.0535(8) Uani 1 1 d . . . H94A H 0.4071 1.6542 0.3933 0.080 Uiso 1 1 calc R . . H94B H 0.3578 1.6471 0.3204 0.080 Uiso 1 1 calc R . . H94C H 0.4181 1.7060 0.3246 0.080 Uiso 1 1 calc R . . C100 C -0.16620(12) 0.69936(18) -0.00880(14) 0.0451(6) Uani 1 1 d . . . H100 H -0.1678 0.7620 -0.0059 0.054 Uiso 1 1 calc R . . C101 C -0.14834(13) 0.64995(19) 0.05186(15) 0.0503(7) Uani 1 1 d . . . H101 H -0.1380 0.6786 0.0966 0.060 Uiso 1 1 calc R . . C102 C -0.14542(14) 0.55960(19) 0.04799(17) 0.0531(8) Uani 1 1 d . . . H102 H -0.1333 0.5253 0.0898 0.064 Uiso 1 1 calc R . . C103 C -0.16017(14) 0.5190(2) -0.01716(17) 0.0564(8) Uani 1 1 d . . . H103 H -0.1575 0.4565 -0.0204 0.068 Uiso 1 1 calc R . . C104 C -0.17875(14) 0.5682(2) -0.07747(16) 0.0547(8) Uani 1 1 d . . . H104 H -0.1896 0.5395 -0.1221 0.066 Uiso 1 1 calc R . . C105 C -0.18171(12) 0.6584(2) -0.07356(14) 0.0461(7) Uani 1 1 d . . . H105 H -0.1944 0.6925 -0.1154 0.055 Uiso 1 1 calc R . . C106 C 0.28510(14) 0.9015(2) 0.42252(17) 0.0581(8) Uani 1 1 d . . . H106 H 0.2525 0.9136 0.3835 0.070 Uiso 1 1 calc R . . C107 C 0.30341(16) 0.9644(2) 0.47228(18) 0.0618(9) Uani 1 1 d . . . H107 H 0.2830 1.0200 0.4685 0.074 Uiso 1 1 calc R . . C108 C 0.35071(15) 0.9487(2) 0.52750(18) 0.0624(9) Uani 1 1 d . . . H108 H 0.3634 0.9931 0.5623 0.075 Uiso 1 1 calc R . . C109 C 0.37956(16) 0.8700(3) 0.53293(17) 0.0778(12) Uani 1 1 d . . . H109 H 0.4132 0.8596 0.5711 0.093 Uiso 1 1 calc R . . C110 C 0.3611(2) 0.8053(3) 0.48444(18) 0.0833(13) Uani 1 1 d . . . H110 H 0.3812 0.7495 0.4895 0.100 Uiso 1 1 calc R . . C111 C 0.31330(18) 0.8203(2) 0.42800(17) 0.0671(9) Uani 1 1 d . . . H111 H 0.3001 0.7756 0.3936 0.081 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 0.02581(9) 0.02516(10) 0.01826(9) 0.00009(6) 0.00188(7) 0.00042(7) Rh2 0.02221(9) 0.01848(9) 0.01752(8) 0.00001(6) 0.00289(6) -0.00082(6) Rh3 0.02773(10) 0.02389(10) 0.02108(9) -0.00309(7) 0.00247(7) -0.00358(7) Rh4 0.02171(9) 0.01905(9) 0.02222(9) -0.00405(6) 0.00246(7) -0.00004(6) P1 0.0374(3) 0.0230(3) 0.0259(3) -0.0050(2) 0.0077(2) 0.0011(2) P2 0.0334(3) 0.0239(3) 0.0265(3) 0.0019(2) 0.0049(2) -0.0037(2) Cl1 0.0437(3) 0.0487(4) 0.0253(3) 0.0079(3) -0.0022(2) 0.0061(3) Cl2 0.0240(3) 0.0386(3) 0.0232(3) 0.0076(2) 0.0031(2) -0.0025(2) Cl3 0.0534(4) 0.0486(4) 0.0302(3) -0.0097(3) -0.0063(3) -0.0118(3) Cl4 0.0265(3) 0.0332(3) 0.0332(3) -0.0141(2) -0.0023(2) 0.0068(2) C1 0.0221(11) 0.0240(11) 0.0227(10) 0.0014(8) 0.0034(8) -0.0008(8) C2 0.0240(11) 0.0226(11) 0.0208(10) 0.0037(8) 0.0027(8) -0.0010(8) C3 0.0411(15) 0.0380(15) 0.0469(15) -0.0131(12) 0.0045(12) 0.0129(12) C4 0.0552(17) 0.0454(16) 0.0406(15) -0.0195(12) -0.0016(13) 0.0124(13) C5 0.110(3) 0.0224(14) 0.0593(18) -0.0049(13) 0.0453(18) -0.0033(15) C10 0.0243(11) 0.0220(11) 0.0351(12) -0.0007(9) 0.0123(9) -0.0035(9) C11 0.0394(13) 0.0267(12) 0.0328(12) 0.0002(10) 0.0148(10) -0.0050(10) C12 0.0618(18) 0.0304(14) 0.0479(15) -0.0110(12) 0.0314(14) -0.0098(12) C13 0.0423(15) 0.0291(14) 0.086(2) -0.0078(14) 0.0315(15) 0.0010(12) C14 0.0336(14) 0.0327(15) 0.082(2) -0.0022(14) 0.0081(14) 0.0070(11) C15 0.0293(13) 0.0347(14) 0.0512(15) -0.0044(12) 0.0031(11) 0.0020(10) C20 0.0235(11) 0.0226(11) 0.0371(12) -0.0030(9) 0.0032(9) -0.0017(9) C21 0.0390(15) 0.0537(17) 0.0432(15) -0.0146(13) 0.0086(12) -0.0144(12) C22 0.0541(19) 0.073(2) 0.070(2) -0.0380(18) 0.0088(16) -0.0258(17) C23 0.0465(17) 0.0428(18) 0.100(3) -0.0096(17) 0.0112(18) -0.0243(14) C24 0.0368(15) 0.0455(17) 0.075(2) 0.0194(15) 0.0022(14) -0.0124(13) C25 0.0286(13) 0.0404(15) 0.0466(15) 0.0119(12) 0.0008(11) -0.0056(11) C30 0.0238(11) 0.0209(11) 0.0313(11) 0.0001(9) 0.0114(9) -0.0055(8) C31 0.0315(12) 0.0265(12) 0.0365(13) 0.0045(10) 0.0119(10) -0.0018(10) C32 0.0382(14) 0.0245(13) 0.0656(18) 0.0030(12) 0.0170(13) 0.0027(11) C33 0.0458(16) 0.0288(14) 0.077(2) -0.0187(14) 0.0157(15) -0.0007(12) C34 0.0455(16) 0.0426(16) 0.0539(17) -0.0218(13) 0.0033(13) -0.0044(13) C35 0.0348(13) 0.0316(13) 0.0384(13) -0.0057(10) 0.0053(10) -0.0004(10) C40 0.0258(11) 0.0201(11) 0.0290(11) 0.0041(9) 0.0086(9) 0.0005(9) C41 0.0330(13) 0.0363(13) 0.0301(12) 0.0053(10) 0.0099(10) 0.0049(10) C42 0.0445(15) 0.0456(15) 0.0331(13) 0.0066(11) 0.0184(11) 0.0080(12) C43 0.0341(14) 0.0454(15) 0.0492(15) 0.0094(12) 0.0210(12) 0.0076(11) C44 0.0278(12) 0.0430(15) 0.0468(15) 0.0063(12) 0.0081(11) -0.0016(11) C45 0.0309(12) 0.0324(13) 0.0304(12) 0.0021(10) 0.0084(10) -0.0032(10) C50 0.0251(11) 0.0223(11) 0.0398(13) -0.0060(10) 0.0120(10) 0.0038(9) C51 0.0387(14) 0.0279(13) 0.0410(14) -0.0031(11) 0.0035(11) 0.0041(10) C52 0.0582(17) 0.0336(15) 0.0487(16) 0.0076(12) 0.0100(13) 0.0091(13) C53 0.0544(17) 0.0219(13) 0.0666(19) 0.0003(12) 0.0273(14) 0.0022(11) C54 0.0445(15) 0.0270(13) 0.0577(17) -0.0161(12) 0.0216(13) -0.0061(11) C55 0.0387(13) 0.0307(13) 0.0384(13) -0.0105(10) 0.0149(11) -0.0024(10) C60 0.0355(13) 0.0221(12) 0.0439(14) -0.0100(10) 0.0187(11) -0.0022(10) C61 0.0537(16) 0.0309(14) 0.0480(15) 0.0010(11) 0.0244(13) 0.0039(12) C62 0.084(2) 0.0325(15) 0.0614(19) 0.0070(13) 0.0481(18) 0.0073(15) C63 0.072(2) 0.0347(16) 0.107(3) -0.0139(17) 0.067(2) -0.0062(15) C64 0.0450(17) 0.063(2) 0.098(3) -0.0379(19) 0.0370(18) -0.0077(15) C65 0.0356(15) 0.069(2) 0.0580(18) -0.0322(15) 0.0187(13) -0.0030(14) C70 0.0220(10) 0.0230(11) 0.0299(11) -0.0006(9) 0.0097(9) 0.0031(8) C71 0.0354(13) 0.0281(12) 0.0327(12) -0.0015(10) 0.0066(10) 0.0001(10) C72 0.0508(15) 0.0349(14) 0.0299(12) 0.0055(10) 0.0147(11) 0.0067(12) C73 0.0560(16) 0.0270(13) 0.0450(15) 0.0080(11) 0.0274(13) 0.0034(11) C74 0.0427(14) 0.0258(12) 0.0451(15) -0.0048(11) 0.0163(11) -0.0071(10) C75 0.0274(11) 0.0279(12) 0.0315(12) -0.0012(9) 0.0079(9) -0.0006(9) C80 0.0223(11) 0.0224(11) 0.0407(13) 0.0000(10) 0.0067(9) -0.0015(9) C81 0.0364(14) 0.0363(14) 0.0452(15) -0.0015(11) 0.0122(11) 0.0062(11) C82 0.0448(16) 0.0425(16) 0.073(2) -0.0068(14) 0.0226(15) 0.0105(13) C83 0.0340(15) 0.0371(16) 0.093(2) -0.0024(16) 0.0104(15) 0.0127(12) C84 0.0351(15) 0.0431(16) 0.070(2) 0.0081(15) -0.0083(14) 0.0073(12) C85 0.0345(13) 0.0370(14) 0.0442(15) 0.0008(11) -0.0005(11) 0.0037(11) C90 0.0256(11) 0.0241(11) 0.0271(11) -0.0069(9) 0.0043(9) -0.0004(9) C91 0.0205(10) 0.0242(11) 0.0238(11) -0.0034(8) 0.0021(8) -0.0012(8) C92 0.0424(16) 0.074(2) 0.0545(18) 0.0308(16) -0.0029(13) -0.0246(15) C93 0.075(2) 0.0354(15) 0.0313(14) 0.0069(11) 0.0047(13) -0.0130(14) C94 0.076(2) 0.0224(13) 0.069(2) 0.0009(13) 0.0302(16) 0.0030(13) C100 0.0432(15) 0.0380(15) 0.0496(16) -0.0023(12) -0.0009(12) 0.0036(12) C101 0.0539(17) 0.0466(17) 0.0437(15) -0.0046(13) -0.0054(13) -0.0075(13) C102 0.0532(18) 0.0451(17) 0.0557(18) 0.0062(14) -0.0014(14) -0.0123(14) C103 0.063(2) 0.0365(16) 0.073(2) -0.0075(15) 0.0218(16) -0.0121(14) C104 0.0605(19) 0.060(2) 0.0477(17) -0.0194(15) 0.0207(15) -0.0127(15) C105 0.0401(15) 0.0577(19) 0.0405(15) -0.0009(13) 0.0084(12) -0.0011(13) C106 0.0434(17) 0.071(2) 0.0529(18) 0.0166(16) -0.0055(14) -0.0079(15) C107 0.071(2) 0.0372(17) 0.072(2) 0.0146(15) 0.0028(18) -0.0030(15) C108 0.058(2) 0.065(2) 0.060(2) -0.0059(16) 0.0043(16) -0.0074(17) C109 0.060(2) 0.124(3) 0.0452(18) -0.009(2) 0.0015(15) 0.041(2) C110 0.114(3) 0.084(3) 0.056(2) 0.0026(19) 0.026(2) 0.059(2) C111 0.093(3) 0.062(2) 0.0500(19) -0.0145(16) 0.0232(18) -0.0105(19) _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 1.968(2) . ? Rh1 C1 1.988(2) . ? Rh1 Cl1 2.3088(6) . ? Rh1 P1 2.4826(6) . ? Rh1 Rh2 2.5054(2) . ? Rh2 C1 2.044(2) . ? Rh2 C2 2.051(2) . ? Rh2 P1 2.3625(6) . ? Rh2 Cl2 2.4636(5) 3_575 ? Rh2 Cl2 2.4961(5) . ? Rh3 C91 1.978(2) . ? Rh3 C90 1.992(2) . ? Rh3 Cl3 2.2979(6) . ? Rh3 P2 2.4173(6) . ? Rh3 Rh4 2.4993(2) . ? Rh4 C90 2.038(2) . ? Rh4 C91 2.046(2) . ? Rh4 P2 2.3890(6) . ? Rh4 Cl4 2.4685(6) 3_686 ? Rh4 Cl4 2.4911(5) . ? P1 C3 1.815(3) . ? P1 C5 1.816(3) . ? P1 C4 1.839(2) . ? P2 C92 1.811(3) . ? P2 C94 1.814(3) . ? P2 C93 1.841(3) . ? Cl2 Rh2 2.4636(5) 3_575 ? Cl4 Rh4 2.4685(6) 3_686 ? C1 C20 1.507(3) . ? C1 C10 1.507(3) . ? C2 C30 1.499(3) . ? C2 C40 1.509(3) . ? C10 C11 1.389(3) . ? C10 C15 1.399(3) . ? C11 C12 1.394(3) . ? C12 C13 1.376(4) . ? C13 C14 1.373(4) . ? C14 C15 1.383(4) . ? C20 C21 1.380(3) . ? C20 C25 1.396(3) . ? C21 C22 1.393(4) . ? C22 C23 1.374(5) . ? C23 C24 1.372(4) . ? C24 C25 1.382(4) . ? C30 C31 1.394(3) . ? C30 C35 1.397(3) . ? C31 C32 1.383(3) . ? C32 C33 1.380(4) . ? C33 C34 1.371(4) . ? C34 C35 1.385(4) . ? C40 C45 1.392(3) . ? C40 C41 1.392(3) . ? C41 C42 1.387(3) . ? C42 C43 1.378(4) . ? C43 C44 1.382(4) . ? C44 C45 1.381(3) . ? C50 C51 1.391(3) . ? C50 C55 1.399(3) . ? C50 C90 1.501(3) . ? C51 C52 1.386(4) . ? C52 C53 1.379(4) . ? C53 C54 1.375(4) . ? C54 C55 1.380(4) . ? C60 C61 1.384(4) . ? C60 C65 1.390(4) . ? C60 C90 1.517(3) . ? C61 C62 1.398(4) . ? C62 C63 1.364(5) . ? C63 C64 1.369(5) . ? C64 C65 1.387(4) . ? C70 C71 1.394(3) . ? C70 C75 1.397(3) . ? C70 C91 1.498(3) . ? C71 C72 1.383(3) . ? C72 C73 1.379(4) . ? C73 C74 1.378(4) . ? C74 C75 1.377(3) . ? C80 C85 1.395(3) . ? C80 C81 1.397(3) . ? C80 C91 1.504(3) . ? C81 C82 1.381(4) . ? C82 C83 1.371(4) . ? C83 C84 1.371(4) . ? C84 C85 1.398(4) . ? C100 C105 1.373(4) . ? C100 C101 1.376(4) . ? C101 C102 1.370(4) . ? C102 C103 1.376(4) . ? C103 C104 1.371(4) . ? C104 C105 1.369(4) . ? C106 C107 1.354(4) . ? C106 C111 1.373(5) . ? C107 C108 1.357(4) . ? C108 C109 1.347(5) . ? C109 C110 1.357(5) . ? C110 C111 1.376(5) . ? 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 91.09(8) . . ? C2 Rh1 Cl1 119.98(6) . . ? C1 Rh1 Cl1 122.43(6) . . ? C2 Rh1 P1 88.43(6) . . ? C1 Rh1 P1 87.06(6) . . ? Cl1 Rh1 P1 135.51(2) . . ? C2 Rh1 Rh2 52.95(6) . . ? C1 Rh1 Rh2 52.59(6) . . ? Cl1 Rh1 Rh2 167.894(19) . . ? P1 Rh1 Rh2 56.538(14) . . ? C1 Rh2 C2 87.19(8) . . ? C1 Rh2 P1 89.11(6) . . ? C2 Rh2 P1 89.88(6) . . ? C1 Rh2 Cl2 95.97(6) . 3_575 ? C2 Rh2 Cl2 159.02(6) . 3_575 ? P1 Rh2 Cl2 110.87(2) . 3_575 ? C1 Rh2 Cl2 170.77(6) . . ? C2 Rh2 Cl2 96.33(6) . . ? P1 Rh2 Cl2 99.41(2) . . ? Cl2 Rh2 Cl2 77.733(19) 3_575 . ? C1 Rh2 Rh1 50.58(6) . . ? C2 Rh2 Rh1 49.97(6) . . ? P1 Rh2 Rh1 61.245(16) . . ? Cl2 Rh2 Rh1 143.314(15) 3_575 . ? Cl2 Rh2 Rh1 137.252(14) . . ? C91 Rh3 C90 90.79(9) . . ? C91 Rh3 Cl3 125.17(6) . . ? C90 Rh3 Cl3 122.27(6) . . ? C91 Rh3 P2 89.34(6) . . ? C90 Rh3 P2 88.42(6) . . ? Cl3 Rh3 P2 129.31(2) . . ? C91 Rh3 Rh4 52.84(6) . . ? C90 Rh3 Rh4 52.50(6) . . ? Cl3 Rh3 Rh4 172.29(2) . . ? P2 Rh3 Rh4 58.114(15) . . ? C90 Rh4 C91 87.58(8) . . ? C90 Rh4 P2 88.15(6) . . ? C91 Rh4 P2 88.54(6) . . ? C90 Rh4 Cl4 97.29(6) . 3_686 ? C91 Rh4 Cl4 152.20(6) . 3_686 ? P2 Rh4 Cl4 118.87(2) . 3_686 ? C90 Rh4 Cl4 173.90(6) . . ? C91 Rh4 Cl4 94.98(6) . . ? P2 Rh4 Cl4 97.44(2) . . ? Cl4 Rh4 Cl4 77.89(2) 3_686 . ? C90 Rh4 Rh3 50.85(6) . . ? C91 Rh4 Rh3 50.39(6) . . ? P2 Rh4 Rh3 59.225(15) . . ? Cl4 Rh4 Rh3 146.777(15) 3_686 . ? Cl4 Rh4 Rh3 134.527(15) . . ? C3 P1 C5 104.05(15) . . ? C3 P1 C4 98.96(13) . . ? C5 P1 C4 98.51(14) . . ? C3 P1 Rh2 105.66(8) . . ? C5 P1 Rh2 96.65(9) . . ? C4 P1 Rh2 146.88(9) . . ? C3 P1 Rh1 121.27(9) . . ? C5 P1 Rh1 133.21(11) . . ? C4 P1 Rh1 86.18(9) . . ? Rh2 P1 Rh1 62.217(15) . . ? C92 P2 C94 103.66(16) . . ? C92 P2 C93 98.01(14) . . ? C94 P2 C93 99.38(14) . . ? C92 P2 Rh4 94.06(9) . . ? C94 P2 Rh4 106.67(10) . . ? C93 P2 Rh4 147.73(9) . . ? C92 P2 Rh3 135.96(12) . . ? C94 P2 Rh3 118.25(10) . . ? C93 P2 Rh3 88.44(9) . . ? Rh4 P2 Rh3 62.662(15) . . ? Rh2 Cl2 Rh2 102.267(19) 3_575 . ? Rh4 Cl4 Rh4 102.11(2) 3_686 . ? C20 C1 C10 109.49(17) . . ? C20 C1 Rh1 111.78(14) . . ? C10 C1 Rh1 117.41(14) . . ? C20 C1 Rh2 121.68(15) . . ? C10 C1 Rh2 116.38(14) . . ? Rh1 C1 Rh2 76.83(7) . . ? C30 C2 C40 113.48(17) . . ? C30 C2 Rh1 118.92(14) . . ? C40 C2 Rh1 111.31(14) . . ? C30 C2 Rh2 108.42(13) . . ? C40 C2 Rh2 123.42(14) . . ? Rh1 C2 Rh2 77.08(7) . . ? C11 C10 C15 118.4(2) . . ? C11 C10 C1 122.8(2) . . ? C15 C10 C1 118.7(2) . . ? C10 C11 C12 120.4(2) . . ? C13 C12 C11 120.2(3) . . ? C14 C13 C12 119.9(2) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 C10 120.6(3) . . ? C21 C20 C25 118.0(2) . . ? C21 C20 C1 121.8(2) . . ? C25 C20 C1 120.1(2) . . ? C20 C21 C22 120.9(3) . . ? C23 C22 C21 120.1(3) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C20 120.8(3) . . ? C31 C30 C35 118.1(2) . . ? C31 C30 C2 121.64(19) . . ? C35 C30 C2 120.2(2) . . ? C32 C31 C30 120.7(2) . . ? C33 C32 C31 120.5(2) . . ? C34 C33 C32 119.5(2) . . ? C33 C34 C35 120.7(3) . . ? C34 C35 C30 120.5(2) . . ? C45 C40 C41 117.7(2) . . ? C45 C40 C2 121.82(19) . . ? C41 C40 C2 120.44(19) . . ? C42 C41 C40 121.1(2) . . ? C43 C42 C41 120.3(2) . . ? C42 C43 C44 119.3(2) . . ? C45 C44 C43 120.5(2) . . ? C44 C45 C40 121.1(2) . . ? C51 C50 C55 117.8(2) . . ? C51 C50 C90 122.7(2) . . ? C55 C50 C90 119.5(2) . . ? C52 C51 C50 120.6(2) . . ? C53 C52 C51 120.8(3) . . ? C54 C53 C52 119.2(2) . . ? C53 C54 C55 120.6(2) . . ? C54 C55 C50 121.0(2) . . ? C61 C60 C65 118.1(2) . . ? C61 C60 C90 121.5(2) . . ? C65 C60 C90 120.4(2) . . ? C60 C61 C62 120.7(3) . . ? C63 C62 C61 120.1(3) . . ? C62 C63 C64 119.9(3) . . ? C63 C64 C65 120.6(3) . . ? C64 C65 C60 120.5(3) . . ? C71 C70 C75 118.4(2) . . ? C71 C70 C91 120.23(19) . . ? C75 C70 C91 121.28(19) . . ? C72 C71 C70 121.0(2) . . ? C73 C72 C71 120.0(2) . . ? C74 C73 C72 119.3(2) . . ? C75 C74 C73 121.4(2) . . ? C74 C75 C70 119.8(2) . . ? C85 C80 C81 117.7(2) . . ? C85 C80 C91 120.7(2) . . ? C81 C80 C91 121.4(2) . . ? C82 C81 C80 121.0(3) . . ? C83 C82 C81 120.6(3) . . ? C82 C83 C84 119.7(3) . . ? C83 C84 C85 120.4(3) . . ? C80 C85 C84 120.4(3) . . ? C50 C90 C60 111.80(18) . . ? C50 C90 Rh3 114.07(15) . . ? C60 C90 Rh3 112.34(16) . . ? C50 C90 Rh4 117.41(15) . . ? C60 C90 Rh4 119.86(15) . . ? Rh3 C90 Rh4 76.65(7) . . ? C70 C91 C80 111.91(18) . . ? C70 C91 Rh3 119.81(14) . . ? C80 C91 Rh3 112.52(15) . . ? C70 C91 Rh4 106.40(14) . . ? C80 C91 Rh4 126.01(15) . . ? Rh3 C91 Rh4 76.77(7) . . ? C105 C100 C101 120.2(3) . . ? C102 C101 C100 120.2(3) . . ? C101 C102 C103 119.3(3) . . ? C104 C103 C102 120.5(3) . . ? C105 C104 C103 120.2(3) . . ? C104 C105 C100 119.6(3) . . ? C107 C106 C111 120.5(3) . . ? C106 C107 C108 120.4(3) . . ? C109 C108 C107 119.8(3) . . ? C108 C109 C110 120.7(3) . . ? C109 C110 C111 120.1(3) . . ? C106 C111 C110 118.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Rh1 Rh2 C1 -127.41(11) . . . . ? Cl1 Rh1 Rh2 C1 -69.71(12) . . . . ? P1 Rh1 Rh2 C1 115.35(8) . . . . ? C1 Rh1 Rh2 C2 127.41(11) . . . . ? Cl1 Rh1 Rh2 C2 57.70(12) . . . . ? P1 Rh1 Rh2 C2 -117.24(8) . . . . ? C2 Rh1 Rh2 P1 117.24(8) . . . . ? C1 Rh1 Rh2 P1 -115.35(8) . . . . ? Cl1 Rh1 Rh2 P1 174.94(9) . . . . ? C2 Rh1 Rh2 Cl2 -156.00(8) . . . 3_575 ? C1 Rh1 Rh2 Cl2 -28.59(8) . . . 3_575 ? Cl1 Rh1 Rh2 Cl2 -98.30(9) . . . 3_575 ? P1 Rh1 Rh2 Cl2 86.76(3) . . . 3_575 ? C2 Rh1 Rh2 Cl2 45.84(8) . . . . ? C1 Rh1 Rh2 Cl2 173.25(8) . . . . ? Cl1 Rh1 Rh2 Cl2 103.54(9) . . . . ? P1 Rh1 Rh2 Cl2 -71.40(3) . . . . ? C91 Rh3 Rh4 C90 127.11(11) . . . . ? Cl3 Rh3 Rh4 C90 49.28(17) . . . . ? P2 Rh3 Rh4 C90 -115.87(8) . . . . ? C90 Rh3 Rh4 C91 -127.11(11) . . . . ? Cl3 Rh3 Rh4 C91 -77.83(17) . . . . ? P2 Rh3 Rh4 C91 117.02(8) . . . . ? C91 Rh3 Rh4 P2 -117.02(8) . . . . ? C90 Rh3 Rh4 P2 115.87(8) . . . . ? Cl3 Rh3 Rh4 P2 165.15(15) . . . . ? C91 Rh3 Rh4 Cl4 146.30(8) . . . 3_686 ? C90 Rh3 Rh4 Cl4 19.19(9) . . . 3_686 ? Cl3 Rh3 Rh4 Cl4 68.47(16) . . . 3_686 ? P2 Rh3 Rh4 Cl4 -96.68(4) . . . 3_686 ? C91 Rh3 Rh4 Cl4 -49.00(8) . . . . ? C90 Rh3 Rh4 Cl4 -176.11(8) . . . . ? Cl3 Rh3 Rh4 Cl4 -126.83(15) . . . . ? P2 Rh3 Rh4 Cl4 68.02(3) . . . . ? C1 Rh2 P1 C3 -161.77(11) . . . . ? C2 Rh2 P1 C3 -74.59(11) . . . . ? Cl2 Rh2 P1 C3 102.18(10) 3_575 . . . ? Cl2 Rh2 P1 C3 21.81(10) . . . . ? Rh1 Rh2 P1 C3 -117.49(10) . . . . ? C1 Rh2 P1 C5 91.58(14) . . . . ? C2 Rh2 P1 C5 178.77(13) . . . . ? Cl2 Rh2 P1 C5 -4.47(12) 3_575 . . . ? Cl2 Rh2 P1 C5 -84.83(12) . . . . ? Rh1 Rh2 P1 C5 135.87(12) . . . . ? C1 Rh2 P1 C4 -25.2(2) . . . . ? C2 Rh2 P1 C4 61.9(2) . . . . ? Cl2 Rh2 P1 C4 -121.3(2) 3_575 . . . ? Cl2 Rh2 P1 C4 158.3(2) . . . . ? Rh1 Rh2 P1 C4 19.04(19) . . . . ? C1 Rh2 P1 Rh1 -44.29(6) . . . . ? C2 Rh2 P1 Rh1 42.90(6) . . . . ? Cl2 Rh2 P1 Rh1 -140.332(16) 3_575 . . . ? Cl2 Rh2 P1 Rh1 139.300(16) . . . . ? C2 Rh1 P1 C3 46.90(12) . . . . ? C1 Rh1 P1 C3 138.07(12) . . . . ? Cl1 Rh1 P1 C3 -86.37(10) . . . . ? Rh2 Rh1 P1 C3 92.12(10) . . . . ? C2 Rh1 P1 C5 -116.84(16) . . . . ? C1 Rh1 P1 C5 -25.67(16) . . . . ? Cl1 Rh1 P1 C5 109.89(15) . . . . ? Rh2 Rh1 P1 C5 -71.62(14) . . . . ? C2 Rh1 P1 C4 145.07(12) . . . . ? C1 Rh1 P1 C4 -123.76(12) . . . . ? Cl1 Rh1 P1 C4 11.80(11) . . . . ? Rh2 Rh1 P1 C4 -169.71(11) . . . . ? C2 Rh1 P1 Rh2 -45.22(6) . . . . ? C1 Rh1 P1 Rh2 45.95(6) . . . . ? Cl1 Rh1 P1 Rh2 -178.49(3) . . . . ? C90 Rh4 P2 C92 -96.49(14) . . . . ? C91 Rh4 P2 C92 175.88(14) . . . . ? Cl4 Rh4 P2 C92 0.81(13) 3_686 . . . ? Cl4 Rh4 P2 C92 81.05(12) . . . . ? Rh3 Rh4 P2 C92 -140.77(12) . . . . ? C90 Rh4 P2 C94 157.94(13) . . . . ? C91 Rh4 P2 C94 70.31(13) . . . . ? Cl4 Rh4 P2 C94 -104.75(11) 3_686 . . . ? Cl4 Rh4 P2 C94 -24.52(11) . . . . ? Rh3 Rh4 P2 C94 113.67(11) . . . . ? C90 Rh4 P2 C93 15.5(2) . . . . ? C91 Rh4 P2 C93 -72.2(2) . . . . ? Cl4 Rh4 P2 C93 112.8(2) 3_686 . . . ? Cl4 Rh4 P2 C93 -167.0(2) . . . . ? Rh3 Rh4 P2 C93 -28.8(2) . . . . ? C90 Rh4 P2 Rh3 44.28(6) . . . . ? C91 Rh4 P2 Rh3 -43.35(6) . . . . ? Cl4 Rh4 P2 Rh3 141.582(18) 3_686 . . . ? Cl4 Rh4 P2 Rh3 -138.185(17) . . . . ? C91 Rh3 P2 C92 110.41(16) . . . . ? C90 Rh3 P2 C92 19.60(16) . . . . ? Cl3 Rh3 P2 C92 -112.29(15) . . . . ? Rh4 Rh3 P2 C92 65.17(15) . . . . ? C91 Rh3 P2 C94 -49.86(13) . . . . ? C90 Rh3 P2 C94 -140.66(13) . . . . ? Cl3 Rh3 P2 C94 87.45(12) . . . . ? Rh4 Rh3 P2 C94 -95.10(12) . . . . ? C91 Rh3 P2 C93 -149.67(12) . . . . ? C90 Rh3 P2 C93 119.52(12) . . . . ? Cl3 Rh3 P2 C93 -12.37(11) . . . . ? Rh4 Rh3 P2 C93 165.09(11) . . . . ? C91 Rh3 P2 Rh4 45.24(6) . . . . ? C90 Rh3 P2 Rh4 -45.57(6) . . . . ? Cl3 Rh3 P2 Rh4 -177.45(3) . . . . ? C1 Rh2 Cl2 Rh2 -47.6(4) . . . 3_575 ? C2 Rh2 Cl2 Rh2 -159.60(6) . . . 3_575 ? P1 Rh2 Cl2 Rh2 109.48(2) . . . 3_575 ? Cl2 Rh2 Cl2 Rh2 0.0 3_575 . . 3_575 ? Rh1 Rh2 Cl2 Rh2 166.855(14) . . . 3_575 ? C90 Rh4 Cl4 Rh4 38.2(6) . . . 3_686 ? C91 Rh4 Cl4 Rh4 152.80(6) . . . 3_686 ? P2 Rh4 Cl4 Rh4 -118.03(2) . . . 3_686 ? Cl4 Rh4 Cl4 Rh4 0.0 3_686 . . 3_686 ? Rh3 Rh4 Cl4 Rh4 -171.497(14) . . . 3_686 ? C2 Rh1 C1 C20 158.51(15) . . . . ? Cl1 Rh1 C1 C20 -74.31(15) . . . . ? P1 Rh1 C1 C20 70.15(14) . . . . ? Rh2 Rh1 C1 C20 119.17(16) . . . . ? C2 Rh1 C1 C10 -73.77(16) . . . . ? Cl1 Rh1 C1 C10 53.40(17) . . . . ? P1 Rh1 C1 C10 -162.14(15) . . . . ? Rh2 Rh1 C1 C10 -113.12(17) . . . . ? C2 Rh1 C1 Rh2 39.35(8) . . . . ? Cl1 Rh1 C1 Rh2 166.52(3) . . . . ? P1 Rh1 C1 Rh2 -49.02(5) . . . . ? C2 Rh2 C1 C20 -145.17(18) . . . . ? P1 Rh2 C1 C20 -55.25(17) . . . . ? Cl2 Rh2 C1 C20 55.64(17) 3_575 . . . ? Cl2 Rh2 C1 C20 102.1(4) . . . . ? Rh1 Rh2 C1 C20 -107.66(18) . . . . ? C2 Rh2 C1 C10 76.80(16) . . . . ? P1 Rh2 C1 C10 166.72(15) . . . . ? Cl2 Rh2 C1 C10 -82.39(15) 3_575 . . . ? Cl2 Rh2 C1 C10 -35.9(5) . . . . ? Rh1 Rh2 C1 C10 114.31(17) . . . . ? C2 Rh2 C1 Rh1 -37.51(7) . . . . ? P1 Rh2 C1 Rh1 52.41(5) . . . . ? Cl2 Rh2 C1 Rh1 163.30(4) 3_575 . . . ? Cl2 Rh2 C1 Rh1 -150.2(3) . . . . ? C1 Rh1 C2 C30 64.98(16) . . . . ? Cl1 Rh1 C2 C30 -64.09(17) . . . . ? P1 Rh1 C2 C30 152.01(15) . . . . ? Rh2 Rh1 C2 C30 104.10(17) . . . . ? C1 Rh1 C2 C40 -160.26(15) . . . . ? Cl1 Rh1 C2 C40 70.67(15) . . . . ? P1 Rh1 C2 C40 -73.23(14) . . . . ? Rh2 Rh1 C2 C40 -121.14(16) . . . . ? C1 Rh1 C2 Rh2 -39.12(8) . . . . ? Cl1 Rh1 C2 Rh2 -168.19(3) . . . . ? P1 Rh1 C2 Rh2 47.90(5) . . . . ? C1 Rh2 C2 C30 -78.62(14) . . . . ? P1 Rh2 C2 C30 -167.74(13) . . . . ? Cl2 Rh2 C2 C30 20.7(3) 3_575 . . . ? Cl2 Rh2 C2 C30 92.81(13) . . . . ? Rh1 Rh2 C2 C30 -116.53(16) . . . . ? C1 Rh2 C2 C40 145.08(17) . . . . ? P1 Rh2 C2 C40 55.97(16) . . . . ? Cl2 Rh2 C2 C40 -115.56(19) 3_575 . . . ? Cl2 Rh2 C2 C40 -43.49(17) . . . . ? Rh1 Rh2 C2 C40 107.18(18) . . . . ? C1 Rh2 C2 Rh1 37.90(8) . . . . ? P1 Rh2 C2 Rh1 -51.21(5) . . . . ? Cl2 Rh2 C2 Rh1 137.26(12) 3_575 . . . ? Cl2 Rh2 C2 Rh1 -150.66(5) . . . . ? C20 C1 C10 C11 -112.2(2) . . . . ? Rh1 C1 C10 C11 119.0(2) . . . . ? Rh2 C1 C10 C11 30.7(3) . . . . ? C20 C1 C10 C15 63.2(3) . . . . ? Rh1 C1 C10 C15 -65.6(2) . . . . ? Rh2 C1 C10 C15 -153.90(17) . . . . ? C15 C10 C11 C12 -0.8(3) . . . . ? C1 C10 C11 C12 174.6(2) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C11 C12 C13 C14 1.2(4) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 C10 0.7(4) . . . . ? C11 C10 C15 C14 0.5(4) . . . . ? C1 C10 C15 C14 -175.1(2) . . . . ? C10 C1 C20 C21 -107.3(3) . . . . ? Rh1 C1 C20 C21 24.5(3) . . . . ? Rh2 C1 C20 C21 112.1(2) . . . . ? C10 C1 C20 C25 68.0(3) . . . . ? Rh1 C1 C20 C25 -160.19(18) . . . . ? Rh2 C1 C20 C25 -72.6(3) . . . . ? C25 C20 C21 C22 2.5(4) . . . . ? C1 C20 C21 C22 177.9(3) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C21 C22 C23 C24 -1.9(5) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? C23 C24 C25 C20 1.4(4) . . . . ? C21 C20 C25 C24 -3.2(4) . . . . ? C1 C20 C25 C24 -178.7(2) . . . . ? C40 C2 C30 C31 -98.4(2) . . . . ? Rh1 C2 C30 C31 35.5(3) . . . . ? Rh2 C2 C30 C31 120.57(18) . . . . ? C40 C2 C30 C35 80.3(2) . . . . ? Rh1 C2 C30 C35 -145.86(17) . . . . ? Rh2 C2 C30 C35 -60.7(2) . . . . ? C35 C30 C31 C32 -0.2(3) . . . . ? C2 C30 C31 C32 178.5(2) . . . . ? C30 C31 C32 C33 -0.3(4) . . . . ? C31 C32 C33 C34 0.3(4) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C30 -0.7(4) . . . . ? C31 C30 C35 C34 0.7(3) . . . . ? C2 C30 C35 C34 -178.1(2) . . . . ? C30 C2 C40 C45 -66.5(3) . . . . ? Rh1 C2 C40 C45 156.13(17) . . . . ? Rh2 C2 C40 C45 67.8(3) . . . . ? C30 C2 C40 C41 112.0(2) . . . . ? Rh1 C2 C40 C41 -25.3(2) . . . . ? Rh2 C2 C40 C41 -113.6(2) . . . . ? C45 C40 C41 C42 -1.6(3) . . . . ? C2 C40 C41 C42 179.8(2) . . . . ? C40 C41 C42 C43 0.8(4) . . . . ? C41 C42 C43 C44 0.0(4) . . . . ? C42 C43 C44 C45 0.1(4) . . . . ? C43 C44 C45 C40 -1.1(4) . . . . ? C41 C40 C45 C44 1.8(3) . . . . ? C2 C40 C45 C44 -179.7(2) . . . . ? C55 C50 C51 C52 -0.9(4) . . . . ? C90 C50 C51 C52 179.7(2) . . . . ? C50 C51 C52 C53 0.3(4) . . . . ? C51 C52 C53 C54 0.4(4) . . . . ? C52 C53 C54 C55 -0.5(4) . . . . ? C53 C54 C55 C50 0.0(4) . . . . ? C51 C50 C55 C54 0.7(3) . . . . ? C90 C50 C55 C54 -179.8(2) . . . . ? C65 C60 C61 C62 -3.3(4) . . . . ? C90 C60 C61 C62 178.5(2) . . . . ? C60 C61 C62 C63 -0.5(4) . . . . ? C61 C62 C63 C64 3.1(4) . . . . ? C62 C63 C64 C65 -1.9(5) . . . . ? C63 C64 C65 C60 -1.9(5) . . . . ? C61 C60 C65 C64 4.5(4) . . . . ? C90 C60 C65 C64 -177.2(3) . . . . ? C75 C70 C71 C72 1.2(3) . . . . ? C91 C70 C71 C72 177.8(2) . . . . ? C70 C71 C72 C73 -1.3(4) . . . . ? C71 C72 C73 C74 0.8(4) . . . . ? C72 C73 C74 C75 -0.3(4) . . . . ? C73 C74 C75 C70 0.2(4) . . . . ? C71 C70 C75 C74 -0.6(3) . . . . ? C91 C70 C75 C74 -177.2(2) . . . . ? C85 C80 C81 C82 -2.2(4) . . . . ? C91 C80 C81 C82 -178.0(2) . . . . ? C80 C81 C82 C83 1.1(4) . . . . ? C81 C82 C83 C84 0.7(4) . . . . ? C82 C83 C84 C85 -1.3(4) . . . . ? C81 C80 C85 C84 1.6(4) . . . . ? C91 C80 C85 C84 177.4(2) . . . . ? C83 C84 C85 C80 0.1(4) . . . . ? C51 C50 C90 C60 108.0(2) . . . . ? C55 C50 C90 C60 -71.5(3) . . . . ? C51 C50 C90 Rh3 -123.2(2) . . . . ? C55 C50 C90 Rh3 57.3(2) . . . . ? C51 C50 C90 Rh4 -36.3(3) . . . . ? C55 C50 C90 Rh4 144.30(18) . . . . ? C61 C60 C90 C50 99.6(3) . . . . ? C65 C60 C90 C50 -78.6(3) . . . . ? C61 C60 C90 Rh3 -30.1(3) . . . . ? C65 C60 C90 Rh3 151.6(2) . . . . ? C61 C60 C90 Rh4 -117.2(2) . . . . ? C65 C60 C90 Rh4 64.6(3) . . . . ? C91 Rh3 C90 C50 74.87(16) . . . . ? Cl3 Rh3 C90 C50 -58.76(17) . . . . ? P2 Rh3 C90 C50 164.18(15) . . . . ? Rh4 Rh3 C90 C50 114.34(17) . . . . ? C91 Rh3 C90 C60 -156.58(15) . . . . ? Cl3 Rh3 C90 C60 69.79(16) . . . . ? P2 Rh3 C90 C60 -67.26(14) . . . . ? Rh4 Rh3 C90 C60 -117.11(17) . . . . ? C91 Rh3 C90 Rh4 -39.47(8) . . . . ? Cl3 Rh3 C90 Rh4 -173.10(3) . . . . ? P2 Rh3 C90 Rh4 49.84(5) . . . . ? C91 Rh4 C90 C50 -72.50(17) . . . . ? P2 Rh4 C90 C50 -161.11(16) . . . . ? Cl4 Rh4 C90 C50 80.02(16) 3_686 . . . ? Cl4 Rh4 C90 C50 42.5(7) . . . . ? Rh3 Rh4 C90 C50 -110.44(18) . . . . ? C91 Rh4 C90 C60 146.26(18) . . . . ? P2 Rh4 C90 C60 57.64(17) . . . . ? Cl4 Rh4 C90 C60 -61.23(17) 3_686 . . . ? Cl4 Rh4 C90 C60 -98.8(6) . . . . ? Rh3 Rh4 C90 C60 108.31(19) . . . . ? C91 Rh4 C90 Rh3 37.94(8) . . . . ? P2 Rh4 C90 Rh3 -50.67(5) . . . . ? Cl4 Rh4 C90 Rh3 -169.54(5) 3_686 . . . ? Cl4 Rh4 C90 Rh3 152.9(5) . . . . ? C71 C70 C91 C80 -87.1(2) . . . . ? C75 C70 C91 C80 89.4(2) . . . . ? C71 C70 C91 Rh3 137.92(18) . . . . ? C75 C70 C91 Rh3 -45.6(3) . . . . ? C71 C70 C91 Rh4 54.0(2) . . . . ? C75 C70 C91 Rh4 -129.46(18) . . . . ? C85 C80 C91 C70 -119.6(2) . . . . ? C81 C80 C91 C70 56.1(3) . . . . ? C85 C80 C91 Rh3 18.7(3) . . . . ? C81 C80 C91 Rh3 -165.59(18) . . . . ? C85 C80 C91 Rh4 108.5(2) . . . . ? C81 C80 C91 Rh4 -75.9(3) . . . . ? C90 Rh3 C91 C70 -62.26(17) . . . . ? Cl3 Rh3 C91 C70 69.26(17) . . . . ? P2 Rh3 C91 C70 -150.67(15) . . . . ? Rh4 Rh3 C91 C70 -101.51(17) . . . . ? C90 Rh3 C91 C80 163.06(15) . . . . ? Cl3 Rh3 C91 C80 -65.42(16) . . . . ? P2 Rh3 C91 C80 74.65(14) . . . . ? Rh4 Rh3 C91 C80 123.80(17) . . . . ? C90 Rh3 C91 Rh4 39.25(8) . . . . ? Cl3 Rh3 C91 Rh4 170.77(3) . . . . ? P2 Rh3 C91 Rh4 -49.15(5) . . . . ? C90 Rh4 C91 C70 79.35(14) . . . . ? P2 Rh4 C91 C70 167.56(13) . . . . ? Cl4 Rh4 C91 C70 -21.7(2) 3_686 . . . ? Cl4 Rh4 C91 C70 -95.10(13) . . . . ? Rh3 Rh4 C91 C70 117.59(15) . . . . ? C90 Rh4 C91 C80 -146.64(19) . . . . ? P2 Rh4 C91 C80 -58.43(18) . . . . ? Cl4 Rh4 C91 C80 112.27(18) 3_686 . . . ? Cl4 Rh4 C91 C80 38.91(18) . . . . ? Rh3 Rh4 C91 C80 -108.4(2) . . . . ? C90 Rh4 C91 Rh3 -38.24(8) . . . . ? P2 Rh4 C91 Rh3 49.96(5) . . . . ? Cl4 Rh4 C91 Rh3 -139.33(9) 3_686 . . . ? Cl4 Rh4 C91 Rh3 147.31(5) . . . . ? C105 C100 C101 C102 0.5(5) . . . . ? C100 C101 C102 C103 0.4(5) . . . . ? C101 C102 C103 C104 -1.3(5) . . . . ? C102 C103 C104 C105 1.2(5) . . . . ? C103 C104 C105 C100 -0.3(5) . . . . ? C101 C100 C105 C104 -0.6(4) . . . . ? C111 C106 C107 C108 1.3(5) . . . . ? C106 C107 C108 C109 -0.1(6) . . . . ? C107 C108 C109 C110 -1.3(6) . . . . ? C108 C109 C110 C111 1.5(6) . . . . ? C107 C106 C111 C110 -1.1(5) . . . . ? C109 C110 C111 C106 -0.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.472 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.069 data_tp5neu _database_code_depnum_ccdc_archive 'CCDC 229310' _publ_section_exptl_prep ; Crystals were grown by adding of excessive trimethylsilylchlorid to a saturated solution of [Rh2(acac)2(CPh2)2(AsMe3)]in benzene within 5 hours. ; _publ_section_exptl_refinement ; The asymmetric unit contains two molecules of benzene and two half molecules of the tetranuclear compound. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H70 As2 Cl4 Rh4' _chemical_formula_weight 1614.54 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' As As 0.0499 2.0058 '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 22.4012(13) _cell_length_b 15.2521(9) _cell_length_c 19.4838(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.535(10) _cell_angle_gamma 90.00 _cell_volume 6498.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8282 _cell_measurement_theta_min 2.292 _cell_measurement_theta_max 28.146 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.66 _exptl_crystal_size_min 0.63 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 2.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _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 Smart apex with D8-Goniometer' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35365 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10588 _reflns_number_gt 9823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-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^)+(0.0280P)^2^+3.5946P] 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 10588 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.46517(11) 0.14734(14) 0.34690(11) 0.0308(5) Uani 1 1 d . . . C2 C 0.45556(11) 0.23949(14) 0.37010(12) 0.0334(5) Uani 1 1 d . . . C3 C 0.47346(14) 0.26685(17) 0.43915(14) 0.0490(7) Uani 1 1 d . . . H3 H 0.4931 0.2268 0.4742 0.059 Uiso 1 1 calc R . . C4 C 0.46292(16) 0.35297(19) 0.45770(17) 0.0633(9) Uani 1 1 d . . . H4 H 0.4751 0.3706 0.5055 0.076 Uiso 1 1 calc R . . C5 C 0.43563(15) 0.41190(17) 0.40867(18) 0.0593(9) Uani 1 1 d . . . H5 H 0.4290 0.4704 0.4219 0.071 Uiso 1 1 calc R . . C6 C 0.41762(14) 0.38616(17) 0.33950(17) 0.0539(8) Uani 1 1 d . . . H6 H 0.3985 0.4271 0.3049 0.065 Uiso 1 1 calc R . . C7 C 0.42726(12) 0.30086(16) 0.32028(14) 0.0426(6) Uani 1 1 d . . . H7 H 0.4144 0.2837 0.2725 0.051 Uiso 1 1 calc R . . C8 C 0.51732(12) 0.14024(14) 0.30865(13) 0.0373(6) Uani 1 1 d . . . C9 C 0.57792(13) 0.14862(19) 0.34570(16) 0.0527(7) Uani 1 1 d . . . H9 H 0.5866 0.1625 0.3944 0.063 Uiso 1 1 calc R . . C10 C 0.62574(15) 0.1366(2) 0.3110(2) 0.0702(10) Uani 1 1 d . . . H10 H 0.6669 0.1396 0.3369 0.084 Uiso 1 1 calc R . . C11 C 0.61404(19) 0.1203(2) 0.2400(2) 0.0735(11) Uani 1 1 d . . . H11 H 0.6469 0.1115 0.2171 0.088 Uiso 1 1 calc R . . C12 C 0.55499(19) 0.11694(18) 0.20248(18) 0.0653(10) Uani 1 1 d . . . H12 H 0.5469 0.1078 0.1531 0.078 Uiso 1 1 calc R . . C13 C 0.50627(14) 0.12683(16) 0.23637(14) 0.0480(7) Uani 1 1 d . . . H13 H 0.4654 0.1244 0.2098 0.058 Uiso 1 1 calc R . . C14 C 0.36068(11) 0.07002(14) 0.38380(11) 0.0294(5) Uani 1 1 d . . . C15 C 0.34646(10) 0.14936(14) 0.42348(12) 0.0306(5) Uani 1 1 d . . . C16 C 0.31134(11) 0.21828(15) 0.38915(13) 0.0383(6) Uani 1 1 d . . . H16 H 0.2969 0.2167 0.3396 0.046 Uiso 1 1 calc R . . C17 C 0.29743(13) 0.28917(17) 0.42735(15) 0.0491(7) Uani 1 1 d . . . H17 H 0.2734 0.3358 0.4036 0.059 Uiso 1 1 calc R . . C18 C 0.31804(14) 0.29295(16) 0.49946(15) 0.0494(7) Uani 1 1 d . . . H18 H 0.3083 0.3420 0.5250 0.059 Uiso 1 1 calc R . . C19 C 0.35259(13) 0.22563(17) 0.53406(14) 0.0475(7) Uani 1 1 d . . . H19 H 0.3671 0.2282 0.5836 0.057 Uiso 1 1 calc R . . C20 C 0.36634(12) 0.15384(16) 0.49667(13) 0.0426(6) Uani 1 1 d . . . H20 H 0.3896 0.1069 0.5211 0.051 Uiso 1 1 calc R . . C21 C 0.31224(11) -0.00010(15) 0.37724(14) 0.0374(6) Uani 1 1 d . . . C22 C 0.28178(13) -0.03089(18) 0.31142(16) 0.0517(7) Uani 1 1 d . . . H22 H 0.2924 -0.0089 0.2700 0.062 Uiso 1 1 calc R . . C23 C 0.23575(15) -0.0938(2) 0.3062(2) 0.0678(10) Uani 1 1 d . . . H23 H 0.2152 -0.1140 0.2611 0.081 Uiso 1 1 calc R . . C24 C 0.21987(15) -0.1267(2) 0.3649(2) 0.0721(10) Uani 1 1 d . . . H24 H 0.1891 -0.1704 0.3608 0.087 Uiso 1 1 calc R . . C25 C 0.24880(15) -0.0961(2) 0.4303(2) 0.0658(9) Uani 1 1 d . . . H25 H 0.2375 -0.1185 0.4713 0.079 Uiso 1 1 calc R . . C26 C 0.29420(12) -0.03308(17) 0.43675(16) 0.0475(7) Uani 1 1 d . . . H26 H 0.3133 -0.0119 0.4821 0.057 Uiso 1 1 calc R . . C27 C 0.53196(14) -0.0841(2) 0.33160(15) 0.0580(8) Uani 1 1 d . . . H27A H 0.5504 -0.0821 0.3820 0.087 Uiso 1 1 calc R . . H27B H 0.5521 -0.0411 0.3069 0.087 Uiso 1 1 calc R . . H27C H 0.5370 -0.1429 0.3134 0.087 Uiso 1 1 calc R . . C28 C 0.42329(15) -0.08007(18) 0.21503(14) 0.0536(8) Uani 1 1 d . . . H28A H 0.4358 -0.1398 0.2059 0.080 Uiso 1 1 calc R . . H28B H 0.4441 -0.0380 0.1903 0.080 Uiso 1 1 calc R . . H28C H 0.3789 -0.0742 0.1983 0.080 Uiso 1 1 calc R . . C29 C 0.41020(17) -0.16042(16) 0.34915(17) 0.0645(9) Uani 1 1 d . . . H29A H 0.4051 -0.2058 0.3127 0.097 Uiso 1 1 calc R . . H29B H 0.3703 -0.1459 0.3590 0.097 Uiso 1 1 calc R . . H29C H 0.4374 -0.1821 0.3921 0.097 Uiso 1 1 calc R . . C31 C 0.01569(10) 0.64287(14) 0.15320(11) 0.0289(5) Uani 1 1 d . . . C32 C 0.02518(10) 0.73158(14) 0.12333(12) 0.0306(5) Uani 1 1 d . . . C33 C -0.00595(12) 0.75510(17) 0.05613(14) 0.0430(6) Uani 1 1 d . . . H33 H -0.0329 0.7142 0.0285 0.052 Uiso 1 1 calc R . . C34 C 0.00179(14) 0.83743(19) 0.02883(17) 0.0583(8) Uani 1 1 d . . . H34 H -0.0200 0.8527 -0.0171 0.070 Uiso 1 1 calc R . . C35 C 0.04113(14) 0.89704(18) 0.06833(19) 0.0592(8) Uani 1 1 d . . . H35 H 0.0466 0.9532 0.0496 0.071 Uiso 1 1 calc R . . C36 C 0.07229(13) 0.87493(17) 0.13477(17) 0.0513(7) Uani 1 1 d . . . H36 H 0.0994 0.9161 0.1619 0.062 Uiso 1 1 calc R . . C37 C 0.06459(11) 0.79298(15) 0.16270(14) 0.0384(6) Uani 1 1 d . . . H37 H 0.0862 0.7786 0.2088 0.046 Uiso 1 1 calc R . . C38 C -0.04165(11) 0.63547(14) 0.18199(12) 0.0305(5) Uani 1 1 d . . . C39 C -0.09991(11) 0.64423(16) 0.13874(13) 0.0385(6) Uani 1 1 d . . . H39 H -0.1039 0.6560 0.0901 0.046 Uiso 1 1 calc R . . C40 C -0.15198(12) 0.63604(18) 0.16591(15) 0.0485(7) Uani 1 1 d . . . H40 H -0.1912 0.6403 0.1355 0.058 Uiso 1 1 calc R . . C41 C -0.14713(13) 0.62162(18) 0.23710(16) 0.0505(7) Uani 1 1 d . . . H41 H -0.1829 0.6166 0.2556 0.061 Uiso 1 1 calc R . . C42 C -0.09003(13) 0.61456(17) 0.28086(14) 0.0458(7) Uani 1 1 d . . . H42 H -0.0865 0.6048 0.3297 0.055 Uiso 1 1 calc R . . C43 C -0.03761(12) 0.62165(16) 0.25404(13) 0.0386(6) Uani 1 1 d . . . H43 H 0.0014 0.6171 0.2849 0.046 Uiso 1 1 calc R . . C44 C 0.12951(10) 0.57324(14) 0.13608(11) 0.0280(5) Uani 1 1 d . . . C45 C 0.15614(11) 0.65469(14) 0.11092(13) 0.0348(5) Uani 1 1 d . . . C46 C 0.20457(13) 0.69729(17) 0.15617(18) 0.0540(7) Uani 1 1 d . . . H46 H 0.2175 0.6771 0.2032 0.065 Uiso 1 1 calc R . . C47 C 0.23374(15) 0.7676(2) 0.1341(2) 0.0725(10) Uani 1 1 d . . . H47 H 0.2662 0.7958 0.1659 0.087 Uiso 1 1 calc R . . C48 C 0.21625(17) 0.7973(2) 0.0665(3) 0.0769(12) Uani 1 1 d . . . H48 H 0.2373 0.8450 0.0511 0.092 Uiso 1 1 calc R . . C49 C 0.16806(17) 0.75814(19) 0.02047(19) 0.0653(10) Uani 1 1 d . . . H49 H 0.1554 0.7797 -0.0262 0.078 Uiso 1 1 calc R . . C50 C 0.13775(13) 0.68610(16) 0.04286(14) 0.0456(7) Uani 1 1 d . . . H50 H 0.1046 0.6590 0.0112 0.055 Uiso 1 1 calc R . . C51 C 0.17689(11) 0.50174(14) 0.15019(12) 0.0331(5) Uani 1 1 d . . . C52 C 0.20054(13) 0.47096(19) 0.21778(15) 0.0501(7) Uani 1 1 d . . . H52 H 0.1856 0.4939 0.2562 0.060 Uiso 1 1 calc R . . C53 C 0.24591(16) 0.4069(2) 0.22978(19) 0.0709(10) Uani 1 1 d . . . H53 H 0.2621 0.3870 0.2763 0.085 Uiso 1 1 calc R . . C54 C 0.26746(15) 0.3722(2) 0.1747(2) 0.0691(10) Uani 1 1 d . . . H54 H 0.2973 0.3270 0.1828 0.083 Uiso 1 1 calc R . . C55 C 0.24556(13) 0.40335(19) 0.10771(18) 0.0563(8) Uani 1 1 d . . . H55 H 0.2610 0.3802 0.0697 0.068 Uiso 1 1 calc R . . C56 C 0.20129(12) 0.46808(17) 0.09527(14) 0.0417(6) Uani 1 1 d . . . H56 H 0.1873 0.4900 0.0489 0.050 Uiso 1 1 calc R . . C57 C -0.04991(13) 0.41203(18) 0.16942(15) 0.0504(7) Uani 1 1 d . . . H57A H -0.0709 0.4209 0.1203 0.076 Uiso 1 1 calc R . . H57B H -0.0673 0.4515 0.1996 0.076 Uiso 1 1 calc R . . H57C H -0.0552 0.3511 0.1829 0.076 Uiso 1 1 calc R . . C58 C 0.06494(14) 0.40094(19) 0.27873(14) 0.0520(7) Uani 1 1 d . . . H58A H 0.0507 0.3413 0.2847 0.078 Uiso 1 1 calc R . . H58B H 0.0484 0.4411 0.3092 0.078 Uiso 1 1 calc R . . H58C H 0.1097 0.4024 0.2914 0.078 Uiso 1 1 calc R . . C59 C 0.06695(17) 0.33675(16) 0.13644(16) 0.0630(9) Uani 1 1 d . . . H59A H 0.0613 0.2833 0.1622 0.094 Uiso 1 1 calc R . . H59B H 0.1105 0.3447 0.1374 0.094 Uiso 1 1 calc R . . H59C H 0.0443 0.3316 0.0876 0.094 Uiso 1 1 calc R . . C60 C 0.18277(14) 0.3391(2) 0.58011(16) 0.0571(8) Uani 1 1 d . . . H60 H 0.1949 0.3044 0.6212 0.069 Uiso 1 1 calc R . . C61 C 0.18199(17) 0.4295(2) 0.58469(19) 0.0714(10) Uani 1 1 d . . . H61 H 0.1941 0.4573 0.6292 0.086 Uiso 1 1 calc R . . C62 C 0.16378(16) 0.4790(2) 0.5250(2) 0.0724(10) Uani 1 1 d . . . H62 H 0.1627 0.5411 0.5285 0.087 Uiso 1 1 calc R . . C63 C 0.14715(16) 0.4401(2) 0.4603(2) 0.0672(9) Uani 1 1 d . . . H63 H 0.1349 0.4747 0.4191 0.081 Uiso 1 1 calc R . . C64 C 0.14839(15) 0.3499(2) 0.45592(17) 0.0623(8) Uani 1 1 d . . . H64 H 0.1372 0.3220 0.4114 0.075 Uiso 1 1 calc R . . C65 C 0.16582(13) 0.3006(2) 0.51572(16) 0.0557(8) Uani 1 1 d . . . H65 H 0.1661 0.2384 0.5122 0.067 Uiso 1 1 calc R . . C70 C 0.31333(18) 0.6740(2) 0.42072(18) 0.0744(10) Uani 1 1 d . . . H70 H 0.3011 0.7166 0.3849 0.089 Uiso 1 1 calc R . . C71 C 0.3576(2) 0.6925(3) 0.47864(19) 0.0978(15) Uani 1 1 d . . . H71 H 0.3766 0.7485 0.4832 0.117 Uiso 1 1 calc R . . C72 C 0.37504(19) 0.6313(3) 0.53019(19) 0.0931(14) Uani 1 1 d . . . H72 H 0.4065 0.6450 0.5700 0.112 Uiso 1 1 calc R . . C73 C 0.34807(17) 0.5513(2) 0.52534(19) 0.0698(9) Uani 1 1 d . . . H73 H 0.3599 0.5090 0.5615 0.084 Uiso 1 1 calc R . . C74 C 0.30366(18) 0.5331(2) 0.4675(2) 0.0779(11) Uani 1 1 d . . . H74 H 0.2841 0.4775 0.4636 0.094 Uiso 1 1 calc R . . C75 C 0.28681(16) 0.5932(2) 0.4152(2) 0.0713(10) Uani 1 1 d . . . H75 H 0.2564 0.5787 0.3746 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.33211(4) 0.14009(5) 0.19059(4) 0.0600(2) Uani 1 1 d . . . Cl2 Cl 0.55617(3) 0.05699(4) 0.49138(3) 0.03587(13) Uani 1 1 d . . . Cl3 Cl 0.13027(3) 0.64675(5) 0.32378(3) 0.04972(17) Uani 1 1 d . . . Cl4 Cl -0.06374(3) 0.52967(4) 0.01265(3) 0.03405(13) Uani 1 1 d . . . As1 As 0.445430(13) -0.056562(15) 0.316699(12) 0.03462(7) Uani 1 1 d . . . As2 As 0.036837(12) 0.437056(15) 0.180168(12) 0.03278(6) Uani 1 1 d . . . Rh1 Rh 0.389241(9) 0.088692(11) 0.295462(9) 0.03112(5) Uani 1 1 d . . . Rh2 Rh 0.452924(8) 0.050059(10) 0.414977(8) 0.02472(5) Uani 1 1 d . . . Rh3 Rh 0.086958(8) 0.587263(11) 0.215323(9) 0.02865(5) Uani 1 1 d . . . Rh4 Rh 0.040138(8) 0.548841(10) 0.088936(8) 0.02375(5) 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 C1 0.0355(14) 0.0278(11) 0.0279(12) 0.0051(9) 0.0045(10) -0.0010(10) C2 0.0355(14) 0.0270(11) 0.0410(13) 0.0045(10) 0.0153(11) -0.0041(10) C3 0.0630(19) 0.0339(14) 0.0468(16) -0.0016(11) 0.0050(14) -0.0036(13) C4 0.089(3) 0.0420(16) 0.061(2) -0.0135(14) 0.0213(18) -0.0124(16) C5 0.078(2) 0.0274(13) 0.084(2) -0.0033(14) 0.0436(19) -0.0054(14) C6 0.0583(19) 0.0308(13) 0.080(2) 0.0163(14) 0.0307(17) 0.0094(12) C7 0.0493(17) 0.0339(13) 0.0479(15) 0.0088(11) 0.0180(13) 0.0000(11) C8 0.0461(17) 0.0265(11) 0.0435(14) 0.0101(10) 0.0189(12) 0.0026(10) C9 0.0466(18) 0.0544(17) 0.0612(18) 0.0226(14) 0.0205(15) -0.0008(13) C10 0.051(2) 0.064(2) 0.105(3) 0.035(2) 0.036(2) 0.0042(16) C11 0.086(3) 0.0458(17) 0.110(3) 0.0214(18) 0.067(3) 0.0128(17) C12 0.106(3) 0.0381(15) 0.069(2) 0.0006(14) 0.056(2) -0.0017(17) C13 0.068(2) 0.0361(13) 0.0464(16) -0.0002(11) 0.0264(14) -0.0035(13) C14 0.0292(13) 0.0278(11) 0.0285(12) 0.0031(9) 0.0004(10) 0.0007(9) C15 0.0265(13) 0.0287(11) 0.0377(13) -0.0006(9) 0.0096(10) -0.0043(9) C16 0.0372(15) 0.0358(13) 0.0430(14) 0.0042(11) 0.0114(11) 0.0040(11) C17 0.0591(19) 0.0334(13) 0.0596(18) 0.0055(12) 0.0236(15) 0.0104(12) C18 0.070(2) 0.0330(13) 0.0559(17) -0.0065(12) 0.0364(15) -0.0039(13) C19 0.0587(18) 0.0479(15) 0.0393(14) -0.0080(12) 0.0183(13) -0.0043(13) C20 0.0472(16) 0.0398(13) 0.0409(14) -0.0006(11) 0.0097(12) 0.0037(12) C21 0.0297(14) 0.0277(11) 0.0526(15) 0.0002(11) 0.0043(11) 0.0005(10) C22 0.0428(17) 0.0451(15) 0.0600(18) -0.0064(13) -0.0050(14) -0.0063(13) C23 0.046(2) 0.0535(18) 0.091(3) -0.0159(18) -0.0129(18) -0.0094(15) C24 0.0427(19) 0.0454(17) 0.124(3) -0.002(2) 0.010(2) -0.0160(14) C25 0.052(2) 0.0500(17) 0.101(3) 0.0083(17) 0.0289(19) -0.0121(15) C26 0.0385(16) 0.0405(14) 0.0638(18) 0.0025(13) 0.0121(14) -0.0052(12) C27 0.058(2) 0.0648(19) 0.0471(17) -0.0152(14) 0.0022(14) 0.0256(15) C28 0.076(2) 0.0451(15) 0.0357(15) -0.0109(12) 0.0034(14) 0.0109(14) C29 0.110(3) 0.0235(13) 0.067(2) -0.0036(13) 0.0344(19) -0.0041(15) C31 0.0323(13) 0.0288(11) 0.0251(11) -0.0037(9) 0.0054(10) 0.0018(9) C32 0.0326(14) 0.0262(11) 0.0356(12) -0.0008(9) 0.0134(10) 0.0066(10) C33 0.0456(16) 0.0360(13) 0.0459(15) 0.0043(11) 0.0072(12) 0.0014(11) C34 0.058(2) 0.0489(17) 0.0653(19) 0.0256(15) 0.0083(16) 0.0053(15) C35 0.053(2) 0.0352(15) 0.091(2) 0.0200(15) 0.0204(18) 0.0015(13) C36 0.0450(17) 0.0315(13) 0.079(2) -0.0032(13) 0.0169(15) -0.0042(12) C37 0.0368(15) 0.0326(12) 0.0477(15) -0.0061(11) 0.0130(12) 0.0027(11) C38 0.0336(14) 0.0261(11) 0.0335(12) -0.0054(9) 0.0110(10) -0.0003(9) C39 0.0358(15) 0.0427(13) 0.0373(14) -0.0057(11) 0.0088(11) 0.0060(11) C40 0.0317(16) 0.0564(16) 0.0583(18) -0.0130(13) 0.0115(13) 0.0030(12) C41 0.0441(18) 0.0548(16) 0.0603(18) -0.0121(14) 0.0280(15) -0.0080(13) C42 0.0557(19) 0.0464(15) 0.0411(15) -0.0062(12) 0.0237(14) -0.0061(13) C43 0.0404(16) 0.0397(13) 0.0376(14) -0.0045(11) 0.0128(12) -0.0016(11) C44 0.0271(13) 0.0292(11) 0.0269(11) -0.0012(9) 0.0042(9) 0.0021(9) C45 0.0320(14) 0.0274(11) 0.0500(15) 0.0026(10) 0.0198(11) 0.0057(10) C46 0.0373(17) 0.0406(15) 0.082(2) 0.0015(14) 0.0085(15) -0.0023(12) C47 0.0424(19) 0.0411(17) 0.134(3) 0.0046(19) 0.020(2) -0.0064(14) C48 0.061(2) 0.0342(16) 0.153(4) 0.015(2) 0.061(3) 0.0026(15) C49 0.093(3) 0.0411(16) 0.079(2) 0.0211(15) 0.057(2) 0.0219(17) C50 0.0598(18) 0.0350(13) 0.0486(16) 0.0068(11) 0.0264(14) 0.0100(12) C51 0.0274(13) 0.0294(11) 0.0407(13) 0.0008(10) 0.0033(10) 0.0018(10) C52 0.0453(17) 0.0577(17) 0.0467(16) 0.0141(13) 0.0089(13) 0.0156(14) C53 0.061(2) 0.075(2) 0.071(2) 0.0327(18) 0.0023(18) 0.0244(18) C54 0.053(2) 0.0513(18) 0.099(3) 0.0082(18) 0.0077(19) 0.0266(15) C55 0.0429(18) 0.0495(16) 0.074(2) -0.0122(15) 0.0083(15) 0.0145(13) C56 0.0336(15) 0.0418(14) 0.0474(15) -0.0039(11) 0.0036(12) 0.0056(11) C57 0.0522(18) 0.0490(16) 0.0467(16) 0.0103(12) 0.0037(13) -0.0171(13) C58 0.0593(19) 0.0559(17) 0.0380(15) 0.0190(13) 0.0045(13) -0.0104(14) C59 0.110(3) 0.0267(13) 0.0618(19) 0.0078(12) 0.0400(19) 0.0092(15) C60 0.0484(19) 0.071(2) 0.0520(18) -0.0037(15) 0.0113(14) -0.0047(15) C61 0.076(3) 0.077(2) 0.068(2) -0.0261(19) 0.032(2) -0.0212(19) C62 0.077(3) 0.0452(17) 0.101(3) -0.0094(18) 0.033(2) -0.0152(17) C63 0.066(2) 0.0537(19) 0.076(2) 0.0085(17) 0.0013(18) -0.0152(16) C64 0.063(2) 0.0571(18) 0.0580(19) -0.0039(15) -0.0052(16) -0.0094(15) C65 0.0489(18) 0.0498(16) 0.0612(19) -0.0028(14) -0.0039(14) 0.0021(14) C70 0.097(3) 0.070(2) 0.056(2) 0.0089(17) 0.018(2) 0.000(2) C71 0.144(4) 0.095(3) 0.054(2) 0.000(2) 0.020(2) -0.071(3) C72 0.089(3) 0.136(4) 0.048(2) 0.009(2) 0.0024(19) -0.056(3) C73 0.074(3) 0.066(2) 0.065(2) 0.0014(17) 0.0074(19) 0.0059(18) C74 0.086(3) 0.0415(17) 0.094(3) -0.0165(18) -0.007(2) 0.0071(17) C75 0.054(2) 0.069(2) 0.078(2) -0.0160(18) -0.0143(18) 0.0099(17) Cl1 0.0762(5) 0.0564(4) 0.0364(4) 0.0092(3) -0.0122(3) 0.0177(4) Cl2 0.0311(3) 0.0381(3) 0.0348(3) 0.0132(2) -0.0009(2) -0.0069(2) Cl3 0.0544(4) 0.0585(4) 0.0307(3) -0.0120(3) -0.0029(3) -0.0074(3) Cl4 0.0296(3) 0.0440(3) 0.0273(3) -0.0085(2) 0.0035(2) 0.0057(2) As1 0.04821(17) 0.02613(12) 0.02860(13) -0.00222(9) 0.00632(11) 0.00449(10) As2 0.04385(16) 0.02729(12) 0.02742(12) 0.00474(9) 0.00824(11) -0.00115(10) Rh1 0.03814(12) 0.02780(9) 0.02455(10) 0.00237(7) 0.00049(8) 0.00395(8) Rh2 0.02770(11) 0.02148(9) 0.02347(9) 0.00275(6) 0.00225(7) -0.00053(7) Rh3 0.03190(12) 0.03040(9) 0.02211(9) -0.00166(7) 0.00243(7) 0.00029(7) Rh4 0.02722(11) 0.02314(9) 0.02026(9) 0.00029(6) 0.00376(7) 0.00219(7) _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 C2 1.506(3) . ? C1 C8 1.520(3) . ? C1 Rh1 1.989(2) . ? C1 Rh2 2.048(2) . ? C2 C3 1.382(4) . ? C2 C7 1.398(3) . ? C3 C4 1.396(4) . ? C4 C5 1.357(5) . ? C5 C6 1.377(4) . ? C6 C7 1.384(4) . ? C8 C13 1.391(4) . ? C8 C9 1.398(4) . ? C9 C10 1.397(4) . ? C10 C11 1.373(5) . ? C11 C12 1.367(5) . ? C12 C13 1.401(4) . ? C14 C15 1.507(3) . ? C14 C21 1.509(3) . ? C14 Rh1 1.983(2) . ? C14 Rh2 2.046(2) . ? C15 C16 1.394(3) . ? C15 C20 1.400(3) . ? C16 C17 1.386(3) . ? C17 C18 1.382(4) . ? C18 C19 1.372(4) . ? C19 C20 1.386(3) . ? C21 C22 1.397(4) . ? C21 C26 1.402(4) . ? C22 C23 1.396(4) . ? C23 C24 1.366(5) . ? C24 C25 1.379(5) . ? C25 C26 1.385(4) . ? C27 As1 1.943(3) . ? C28 As1 1.968(3) . ? C29 As1 1.936(3) . ? C31 C32 1.506(3) . ? C31 C38 1.513(3) . ? C31 Rh3 1.973(2) . ? C31 Rh4 2.055(2) . ? C32 C33 1.390(3) . ? C32 C37 1.397(3) . ? C33 C34 1.389(4) . ? C34 C35 1.379(4) . ? C35 C36 1.373(4) . ? C36 C37 1.389(4) . ? C38 C39 1.398(3) . ? C38 C43 1.403(3) . ? C39 C40 1.387(4) . ? C40 C41 1.385(4) . ? C41 C42 1.379(4) . ? C42 C43 1.389(4) . ? C44 C51 1.505(3) . ? C44 C45 1.506(3) . ? C44 Rh3 1.994(2) . ? C44 Rh4 2.047(2) . ? C45 C50 1.386(3) . ? C45 C46 1.400(4) . ? C46 C47 1.373(4) . ? C47 C48 1.367(5) . ? C48 C49 1.380(5) . ? C49 C50 1.410(4) . ? C51 C52 1.390(3) . ? C51 C56 1.400(3) . ? C52 C53 1.393(4) . ? C53 C54 1.375(5) . ? C54 C55 1.375(5) . ? C55 C56 1.383(4) . ? C57 As2 1.946(3) . ? C58 As2 1.965(3) . ? C59 As2 1.942(3) . ? C60 C65 1.363(4) . ? C60 C61 1.382(5) . ? C61 C62 1.373(5) . ? C62 C63 1.370(5) . ? C63 C64 1.379(4) . ? C64 C65 1.371(4) . ? C70 C71 1.361(5) . ? C70 C75 1.363(5) . ? C71 C72 1.364(5) . ? C72 C73 1.356(5) . ? C73 C74 1.360(5) . ? C74 C75 1.362(5) . ? Cl1 Rh1 2.3006(7) . ? Cl2 Rh2 2.4662(7) . ? Cl2 Rh2 2.4895(6) 3_656 ? Cl3 Rh3 2.3108(6) . ? Cl4 Rh4 2.4669(6) 3_565 ? Cl4 Rh4 2.4917(6) . ? As1 Rh2 2.4899(3) . ? As1 Rh1 2.5372(3) . ? As2 Rh4 2.4757(3) . ? As2 Rh3 2.5777(3) . ? Rh1 Rh2 2.5225(3) . ? Rh2 Cl2 2.4895(6) 3_656 ? Rh3 Rh4 2.5271(3) . ? Rh4 Cl4 2.4669(6) 3_565 ? 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 C1 C8 112.88(18) . . ? C2 C1 Rh1 114.11(16) . . ? C8 C1 Rh1 112.65(16) . . ? C2 C1 Rh2 115.70(15) . . ? C8 C1 Rh2 119.42(15) . . ? Rh1 C1 Rh2 77.32(8) . . ? C3 C2 C7 117.8(2) . . ? C3 C2 C1 122.9(2) . . ? C7 C2 C1 119.3(2) . . ? C2 C3 C4 120.4(3) . . ? C5 C4 C3 121.1(3) . . ? C4 C5 C6 119.5(3) . . ? C5 C6 C7 120.2(3) . . ? C6 C7 C2 121.0(3) . . ? C13 C8 C9 118.4(2) . . ? C13 C8 C1 121.3(2) . . ? C9 C8 C1 120.3(2) . . ? C10 C9 C8 119.9(3) . . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 119.8(3) . . ? C11 C12 C13 120.4(3) . . ? C8 C13 C12 120.5(3) . . ? C15 C14 C21 112.60(19) . . ? C15 C14 Rh1 118.30(15) . . ? C21 C14 Rh1 112.95(16) . . ? C15 C14 Rh2 106.23(15) . . ? C21 C14 Rh2 125.52(15) . . ? Rh1 C14 Rh2 77.51(8) . . ? C16 C15 C20 118.3(2) . . ? C16 C15 C14 121.3(2) . . ? C20 C15 C14 120.4(2) . . ? C17 C16 C15 120.0(2) . . ? C18 C17 C16 121.0(2) . . ? C19 C18 C17 119.8(2) . . ? C18 C19 C20 119.9(3) . . ? C19 C20 C15 121.0(2) . . ? C22 C21 C26 117.9(2) . . ? C22 C21 C14 121.0(2) . . ? C26 C21 C14 121.0(2) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 120.9(3) . . ? C23 C24 C25 119.6(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C21 120.8(3) . . ? C32 C31 C38 114.36(18) . . ? C32 C31 Rh3 117.39(16) . . ? C38 C31 Rh3 112.30(15) . . ? C32 C31 Rh4 108.24(14) . . ? C38 C31 Rh4 122.25(15) . . ? Rh3 C31 Rh4 77.68(8) . . ? C33 C32 C37 118.2(2) . . ? C33 C32 C31 120.8(2) . . ? C37 C32 C31 121.0(2) . . ? C34 C33 C32 121.0(3) . . ? C35 C34 C33 120.0(3) . . ? C36 C35 C34 119.8(3) . . ? C35 C36 C37 120.6(3) . . ? C36 C37 C32 120.4(3) . . ? C39 C38 C43 117.8(2) . . ? C39 C38 C31 121.7(2) . . ? C43 C38 C31 120.4(2) . . ? C40 C39 C38 120.9(2) . . ? C41 C40 C39 120.4(3) . . ? C42 C41 C40 119.5(3) . . ? C41 C42 C43 120.5(3) . . ? C42 C43 C38 120.8(2) . . ? C51 C44 C45 110.11(19) . . ? C51 C44 Rh3 111.90(15) . . ? C45 C44 Rh3 116.96(15) . . ? C51 C44 Rh4 122.17(15) . . ? C45 C44 Rh4 114.96(15) . . ? Rh3 C44 Rh4 77.39(8) . . ? C50 C45 C46 118.1(2) . . ? C50 C45 C44 122.7(2) . . ? C46 C45 C44 119.0(2) . . ? C47 C46 C45 121.4(3) . . ? C48 C47 C46 120.3(3) . . ? C47 C48 C49 120.1(3) . . ? C48 C49 C50 119.9(3) . . ? C45 C50 C49 120.2(3) . . ? C52 C51 C56 117.9(2) . . ? C52 C51 C44 121.8(2) . . ? C56 C51 C44 120.2(2) . . ? C51 C52 C53 120.7(3) . . ? C54 C53 C52 120.4(3) . . ? C55 C54 C53 119.7(3) . . ? C54 C55 C56 120.5(3) . . ? C55 C56 C51 120.8(3) . . ? C65 C60 C61 119.0(3) . . ? C62 C61 C60 120.0(3) . . ? C63 C62 C61 120.9(3) . . ? C62 C63 C64 118.9(3) . . ? C65 C64 C63 120.1(3) . . ? C60 C65 C64 121.1(3) . . ? C71 C70 C75 118.7(3) . . ? C70 C71 C72 120.7(3) . . ? C73 C72 C71 120.8(4) . . ? C72 C73 C74 118.4(3) . . ? C73 C74 C75 121.1(3) . . ? C74 C75 C70 120.3(3) . . ? Rh2 Cl2 Rh2 101.48(2) . 3_656 ? Rh4 Cl4 Rh4 101.57(2) 3_565 . ? C29 As1 C27 103.80(15) . . ? C29 As1 C28 98.52(13) . . ? C27 As1 C28 97.84(13) . . ? C29 As1 Rh2 104.32(9) . . ? C27 As1 Rh2 97.33(8) . . ? C28 As1 Rh2 148.58(8) . . ? C29 As1 Rh1 123.00(10) . . ? C27 As1 Rh1 131.05(10) . . ? C28 As1 Rh1 89.27(8) . . ? Rh2 As1 Rh1 60.225(9) . . ? C59 As2 C57 103.42(14) . . ? C59 As2 C58 98.04(13) . . ? C57 As2 C58 98.67(12) . . ? C59 As2 Rh4 99.22(8) . . ? C57 As2 Rh4 104.03(8) . . ? C58 As2 Rh4 147.29(8) . . ? C59 As2 Rh3 130.09(10) . . ? C57 As2 Rh3 124.75(9) . . ? C58 As2 Rh3 87.75(8) . . ? Rh4 As2 Rh3 59.970(9) . . ? C14 Rh1 C1 91.66(9) . . ? C14 Rh1 Cl1 126.72(7) . . ? C1 Rh1 Cl1 122.97(6) . . ? C14 Rh1 Rh2 52.37(7) . . ? C1 Rh1 Rh2 52.38(6) . . ? Cl1 Rh1 Rh2 173.55(2) . . ? C14 Rh1 As1 88.58(6) . . ? C1 Rh1 As1 88.33(6) . . ? Cl1 Rh1 As1 127.09(2) . . ? Rh2 Rh1 As1 58.958(8) . . ? C14 Rh2 C1 88.19(9) . . ? C14 Rh2 Cl2 158.01(6) . . ? C1 Rh2 Cl2 96.89(7) . . ? C14 Rh2 Cl2 94.43(6) . 3_656 ? C1 Rh2 Cl2 173.52(6) . 3_656 ? Cl2 Rh2 Cl2 78.52(2) . 3_656 ? C14 Rh2 As1 88.49(6) . . ? C1 Rh2 As1 88.35(6) . . ? Cl2 Rh2 As1 112.956(18) . . ? Cl2 Rh2 As1 97.628(17) 3_656 . ? C14 Rh2 Rh1 50.12(6) . . ? C1 Rh2 Rh1 50.30(6) . . ? Cl2 Rh2 Rh1 144.647(17) . . ? Cl2 Rh2 Rh1 135.230(16) 3_656 . ? As1 Rh2 Rh1 60.817(9) . . ? C31 Rh3 C44 91.73(9) . . ? C31 Rh3 Cl3 121.02(6) . . ? C44 Rh3 Cl3 125.01(7) . . ? C31 Rh3 Rh4 52.60(6) . . ? C44 Rh3 Rh4 52.25(6) . . ? Cl3 Rh3 Rh4 170.13(2) . . ? C31 Rh3 As2 88.36(6) . . ? C44 Rh3 As2 87.29(6) . . ? Cl3 Rh3 As2 131.62(2) . . ? Rh4 Rh3 As2 58.011(8) . . ? C44 Rh4 C31 87.92(9) . . ? C44 Rh4 Cl4 95.11(6) . 3_565 ? C31 Rh4 Cl4 163.66(6) . 3_565 ? C44 Rh4 As2 88.95(6) . . ? C31 Rh4 As2 89.41(6) . . ? Cl4 Rh4 As2 106.665(17) 3_565 . ? C44 Rh4 Cl4 169.94(6) . . ? C31 Rh4 Cl4 96.17(6) . . ? Cl4 Rh4 Cl4 78.43(2) 3_565 . ? As2 Rh4 Cl4 100.250(17) . . ? C44 Rh4 Rh3 50.37(6) . . ? C31 Rh4 Rh3 49.72(6) . . ? Cl4 Rh4 Rh3 141.124(16) 3_565 . ? As2 Rh4 Rh3 62.018(8) . . ? Cl4 Rh4 Rh3 138.145(16) . . ? 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 C8 C1 C2 C3 -104.7(3) . . . . ? Rh1 C1 C2 C3 125.0(2) . . . . ? Rh2 C1 C2 C3 38.0(3) . . . . ? C8 C1 C2 C7 75.4(3) . . . . ? Rh1 C1 C2 C7 -54.9(3) . . . . ? Rh2 C1 C2 C7 -141.92(19) . . . . ? C7 C2 C3 C4 0.4(4) . . . . ? C1 C2 C3 C4 -179.5(3) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C2 -0.4(4) . . . . ? C3 C2 C7 C6 0.1(4) . . . . ? C1 C2 C7 C6 -180.0(2) . . . . ? C2 C1 C8 C13 -107.2(3) . . . . ? Rh1 C1 C8 C13 23.8(3) . . . . ? Rh2 C1 C8 C13 111.6(2) . . . . ? C2 C1 C8 C9 71.7(3) . . . . ? Rh1 C1 C8 C9 -157.28(19) . . . . ? Rh2 C1 C8 C9 -69.4(3) . . . . ? C13 C8 C9 C10 -5.1(4) . . . . ? C1 C8 C9 C10 176.0(2) . . . . ? C8 C9 C10 C11 2.9(4) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C10 C11 C12 C13 -2.3(5) . . . . ? C9 C8 C13 C12 3.6(4) . . . . ? C1 C8 C13 C12 -177.4(2) . . . . ? C11 C12 C13 C8 0.0(4) . . . . ? C21 C14 C15 C16 -88.1(3) . . . . ? Rh1 C14 C15 C16 46.7(3) . . . . ? Rh2 C14 C15 C16 131.0(2) . . . . ? C21 C14 C15 C20 89.3(3) . . . . ? Rh1 C14 C15 C20 -136.0(2) . . . . ? Rh2 C14 C15 C20 -51.6(2) . . . . ? C20 C15 C16 C17 0.6(4) . . . . ? C14 C15 C16 C17 178.0(2) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C18 C19 C20 C15 1.2(4) . . . . ? C16 C15 C20 C19 -1.3(4) . . . . ? C14 C15 C20 C19 -178.7(2) . . . . ? C15 C14 C21 C22 122.7(3) . . . . ? Rh1 C14 C21 C22 -14.5(3) . . . . ? Rh2 C14 C21 C22 -105.3(2) . . . . ? C15 C14 C21 C26 -54.0(3) . . . . ? Rh1 C14 C21 C26 168.82(19) . . . . ? Rh2 C14 C21 C26 78.0(3) . . . . ? C26 C21 C22 C23 -1.2(4) . . . . ? C14 C21 C22 C23 -178.0(3) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C25 1.4(5) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? C24 C25 C26 C21 -0.9(5) . . . . ? C22 C21 C26 C25 1.9(4) . . . . ? C14 C21 C26 C25 178.6(2) . . . . ? C38 C31 C32 C33 -80.0(3) . . . . ? Rh3 C31 C32 C33 145.24(19) . . . . ? Rh4 C31 C32 C33 60.0(2) . . . . ? C38 C31 C32 C37 98.8(3) . . . . ? Rh3 C31 C32 C37 -35.9(3) . . . . ? Rh4 C31 C32 C37 -121.15(19) . . . . ? C37 C32 C33 C34 -0.1(4) . . . . ? C31 C32 C33 C34 178.8(2) . . . . ? C32 C33 C34 C35 0.4(4) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? C35 C36 C37 C32 0.4(4) . . . . ? C33 C32 C37 C36 -0.3(4) . . . . ? C31 C32 C37 C36 -179.2(2) . . . . ? C32 C31 C38 C39 63.6(3) . . . . ? Rh3 C31 C38 C39 -159.38(18) . . . . ? Rh4 C31 C38 C39 -70.2(3) . . . . ? C32 C31 C38 C43 -114.8(2) . . . . ? Rh3 C31 C38 C43 22.3(3) . . . . ? Rh4 C31 C38 C43 111.5(2) . . . . ? C43 C38 C39 C40 -2.5(3) . . . . ? C31 C38 C39 C40 179.1(2) . . . . ? C38 C39 C40 C41 2.0(4) . . . . ? C39 C40 C41 C42 -0.6(4) . . . . ? C40 C41 C42 C43 -0.1(4) . . . . ? C41 C42 C43 C38 -0.5(4) . . . . ? C39 C38 C43 C42 1.7(3) . . . . ? C31 C38 C43 C42 -179.8(2) . . . . ? C51 C44 C45 C50 111.6(2) . . . . ? Rh3 C44 C45 C50 -119.2(2) . . . . ? Rh4 C44 C45 C50 -31.1(3) . . . . ? C51 C44 C45 C46 -63.6(3) . . . . ? Rh3 C44 C45 C46 65.6(3) . . . . ? Rh4 C44 C45 C46 153.66(19) . . . . ? C50 C45 C46 C47 -0.7(4) . . . . ? C44 C45 C46 C47 174.7(2) . . . . ? C45 C46 C47 C48 -0.6(5) . . . . ? C46 C47 C48 C49 1.7(5) . . . . ? C47 C48 C49 C50 -1.4(5) . . . . ? C46 C45 C50 C49 0.9(4) . . . . ? C44 C45 C50 C49 -174.3(2) . . . . ? C48 C49 C50 C45 0.1(4) . . . . ? C45 C44 C51 C52 112.8(3) . . . . ? Rh3 C44 C51 C52 -19.1(3) . . . . ? Rh4 C44 C51 C52 -107.6(2) . . . . ? C45 C44 C51 C56 -63.1(3) . . . . ? Rh3 C44 C51 C56 165.01(18) . . . . ? Rh4 C44 C51 C56 76.5(3) . . . . ? C56 C51 C52 C53 -1.7(4) . . . . ? C44 C51 C52 C53 -177.7(3) . . . . ? C51 C52 C53 C54 -0.9(5) . . . . ? C52 C53 C54 C55 2.3(5) . . . . ? C53 C54 C55 C56 -1.2(5) . . . . ? C54 C55 C56 C51 -1.5(4) . . . . ? C52 C51 C56 C55 2.9(4) . . . . ? C44 C51 C56 C55 179.0(2) . . . . ? C65 C60 C61 C62 0.6(5) . . . . ? C60 C61 C62 C63 -1.0(5) . . . . ? C61 C62 C63 C64 0.6(6) . . . . ? C62 C63 C64 C65 0.3(5) . . . . ? C61 C60 C65 C64 0.3(5) . . . . ? C63 C64 C65 C60 -0.7(5) . . . . ? C75 C70 C71 C72 -0.1(7) . . . . ? C70 C71 C72 C73 -0.9(7) . . . . ? C71 C72 C73 C74 0.7(7) . . . . ? C72 C73 C74 C75 0.6(6) . . . . ? C73 C74 C75 C70 -1.6(6) . . . . ? C71 C70 C75 C74 1.4(6) . . . . ? C15 C14 Rh1 C1 64.39(18) . . . . ? C21 C14 Rh1 C1 -161.03(16) . . . . ? Rh2 C14 Rh1 C1 -37.50(8) . . . . ? C15 C14 Rh1 Cl1 -70.10(19) . . . . ? C21 C14 Rh1 Cl1 64.48(17) . . . . ? Rh2 C14 Rh1 Cl1 -171.99(3) . . . . ? C15 C14 Rh1 Rh2 101.88(18) . . . . ? C21 C14 Rh1 Rh2 -123.53(18) . . . . ? C15 C14 Rh1 As1 152.67(17) . . . . ? C21 C14 Rh1 As1 -72.74(15) . . . . ? Rh2 C14 Rh1 As1 50.79(5) . . . . ? C2 C1 Rh1 C14 -75.24(16) . . . . ? C8 C1 Rh1 C14 154.34(16) . . . . ? Rh2 C1 Rh1 C14 37.49(8) . . . . ? C2 C1 Rh1 Cl1 61.80(17) . . . . ? C8 C1 Rh1 Cl1 -68.63(16) . . . . ? Rh2 C1 Rh1 Cl1 174.52(3) . . . . ? C2 C1 Rh1 Rh2 -112.72(17) . . . . ? C8 C1 Rh1 Rh2 116.85(17) . . . . ? C2 C1 Rh1 As1 -163.76(15) . . . . ? C8 C1 Rh1 As1 65.81(14) . . . . ? Rh2 C1 Rh1 As1 -51.04(5) . . . . ? C29 As1 Rh1 C14 42.44(13) . . . . ? C27 As1 Rh1 C14 -118.10(13) . . . . ? C28 As1 Rh1 C14 142.13(12) . . . . ? Rh2 As1 Rh1 C14 -45.74(7) . . . . ? C29 As1 Rh1 C1 134.14(13) . . . . ? C27 As1 Rh1 C1 -26.39(13) . . . . ? C28 As1 Rh1 C1 -126.17(12) . . . . ? Rh2 As1 Rh1 C1 45.96(6) . . . . ? C29 As1 Rh1 Cl1 -94.52(12) . . . . ? C27 As1 Rh1 Cl1 104.94(12) . . . . ? C28 As1 Rh1 Cl1 5.17(10) . . . . ? Rh2 As1 Rh1 Cl1 177.29(3) . . . . ? C29 As1 Rh1 Rh2 88.18(12) . . . . ? C27 As1 Rh1 Rh2 -72.35(12) . . . . ? C28 As1 Rh1 Rh2 -172.13(10) . . . . ? C15 C14 Rh2 C1 -79.93(15) . . . . ? C21 C14 Rh2 C1 145.7(2) . . . . ? Rh1 C14 Rh2 C1 36.25(8) . . . . ? C15 C14 Rh2 Cl2 24.1(3) . . . . ? C21 C14 Rh2 Cl2 -110.3(2) . . . . ? Rh1 C14 Rh2 Cl2 140.28(12) . . . . ? C15 C14 Rh2 Cl2 94.13(14) . . . 3_656 ? C21 C14 Rh2 Cl2 -40.3(2) . . . 3_656 ? Rh1 C14 Rh2 Cl2 -149.68(5) . . . 3_656 ? C15 C14 Rh2 As1 -168.33(14) . . . . ? C21 C14 Rh2 As1 57.28(19) . . . . ? Rh1 C14 Rh2 As1 -52.15(5) . . . . ? C15 C14 Rh2 Rh1 -116.18(16) . . . . ? C21 C14 Rh2 Rh1 109.4(2) . . . . ? C2 C1 Rh2 C14 74.74(18) . . . . ? C8 C1 Rh2 C14 -145.18(19) . . . . ? Rh1 C1 Rh2 C14 -36.14(8) . . . . ? C2 C1 Rh2 Cl2 -83.79(17) . . . . ? C8 C1 Rh2 Cl2 56.28(18) . . . . ? Rh1 C1 Rh2 Cl2 165.33(5) . . . . ? C2 C1 Rh2 Cl2 -39.3(7) . . . 3_656 ? C8 C1 Rh2 Cl2 100.8(6) . . . 3_656 ? Rh1 C1 Rh2 Cl2 -150.1(6) . . . 3_656 ? C2 C1 Rh2 As1 163.29(17) . . . . ? C8 C1 Rh2 As1 -56.64(18) . . . . ? Rh1 C1 Rh2 As1 52.40(5) . . . . ? C2 C1 Rh2 Rh1 110.88(19) . . . . ? C8 C1 Rh2 Rh1 -109.0(2) . . . . ? Rh2 Cl2 Rh2 C14 72.99(17) 3_656 . . . ? Rh2 Cl2 Rh2 C1 175.37(7) 3_656 . . . ? Rh2 Cl2 Rh2 Cl2 0.0 3_656 . . 3_656 ? Rh2 Cl2 Rh2 As1 -93.50(2) 3_656 . . . ? Rh2 Cl2 Rh2 Rh1 -164.951(17) 3_656 . . . ? C29 As1 Rh2 C14 -76.16(13) . . . . ? C27 As1 Rh2 C14 177.51(12) . . . . ? C28 As1 Rh2 C14 59.2(2) . . . . ? Rh1 As1 Rh2 C14 43.95(6) . . . . ? C29 As1 Rh2 C1 -164.39(13) . . . . ? C27 As1 Rh2 C1 89.28(12) . . . . ? C28 As1 Rh2 C1 -29.1(2) . . . . ? Rh1 As1 Rh2 C1 -44.29(7) . . . . ? C29 As1 Rh2 Cl2 98.82(11) . . . . ? C27 As1 Rh2 Cl2 -7.51(10) . . . . ? C28 As1 Rh2 Cl2 -125.84(19) . . . . ? Rh1 As1 Rh2 Cl2 -141.075(17) . . . . ? C29 As1 Rh2 Cl2 18.11(11) . . . 3_656 ? C27 As1 Rh2 Cl2 -88.22(10) . . . 3_656 ? C28 As1 Rh2 Cl2 153.44(19) . . . 3_656 ? Rh1 As1 Rh2 Cl2 138.212(16) . . . 3_656 ? C29 As1 Rh2 Rh1 -120.11(11) . . . . ? C27 As1 Rh2 Rh1 133.56(10) . . . . ? C28 As1 Rh2 Rh1 15.23(19) . . . . ? C1 Rh1 Rh2 C14 129.81(11) . . . . ? Cl1 Rh1 Rh2 C14 84.3(2) . . . . ? As1 Rh1 Rh2 C14 -115.30(8) . . . . ? C14 Rh1 Rh2 C1 -129.81(11) . . . . ? Cl1 Rh1 Rh2 C1 -45.5(2) . . . . ? As1 Rh1 Rh2 C1 114.89(8) . . . . ? C14 Rh1 Rh2 Cl2 -155.57(8) . . . . ? C1 Rh1 Rh2 Cl2 -25.75(9) . . . . ? Cl1 Rh1 Rh2 Cl2 -71.3(2) . . . . ? As1 Rh1 Rh2 Cl2 89.13(3) . . . . ? C14 Rh1 Rh2 Cl2 45.61(8) . . . 3_656 ? C1 Rh1 Rh2 Cl2 175.43(9) . . . 3_656 ? Cl1 Rh1 Rh2 Cl2 129.9(2) . . . 3_656 ? As1 Rh1 Rh2 Cl2 -69.69(2) . . . 3_656 ? C14 Rh1 Rh2 As1 115.30(8) . . . . ? C1 Rh1 Rh2 As1 -114.89(8) . . . . ? Cl1 Rh1 Rh2 As1 -160.4(2) . . . . ? C32 C31 Rh3 C44 -66.92(16) . . . . ? C38 C31 Rh3 C44 157.47(15) . . . . ? Rh4 C31 Rh3 C44 37.42(8) . . . . ? C32 C31 Rh3 Cl3 66.55(17) . . . . ? C38 C31 Rh3 Cl3 -69.06(16) . . . . ? Rh4 C31 Rh3 Cl3 170.89(3) . . . . ? C32 C31 Rh3 Rh4 -104.34(17) . . . . ? C38 C31 Rh3 Rh4 120.05(17) . . . . ? C32 C31 Rh3 As2 -154.16(15) . . . . ? C38 C31 Rh3 As2 70.23(14) . . . . ? Rh4 C31 Rh3 As2 -49.82(5) . . . . ? C51 C44 Rh3 C31 -157.51(16) . . . . ? C45 C44 Rh3 C31 74.17(18) . . . . ? Rh4 C44 Rh3 C31 -37.63(8) . . . . ? C51 C44 Rh3 Cl3 71.90(17) . . . . ? C45 C44 Rh3 Cl3 -56.43(19) . . . . ? Rh4 C44 Rh3 Cl3 -168.22(3) . . . . ? C51 C44 Rh3 Rh4 -119.88(17) . . . . ? C45 C44 Rh3 Rh4 111.79(19) . . . . ? C51 C44 Rh3 As2 -69.23(15) . . . . ? C45 C44 Rh3 As2 162.44(17) . . . . ? Rh4 C44 Rh3 As2 50.64(5) . . . . ? C59 As2 Rh3 C31 121.52(14) . . . . ? C57 As2 Rh3 C31 -40.86(12) . . . . ? C58 As2 Rh3 C31 -139.86(11) . . . . ? Rh4 As2 Rh3 C31 45.69(6) . . . . ? C59 As2 Rh3 C44 29.71(14) . . . . ? C57 As2 Rh3 C44 -132.67(12) . . . . ? C58 As2 Rh3 C44 128.33(11) . . . . ? Rh4 As2 Rh3 C44 -46.12(6) . . . . ? C59 As2 Rh3 Cl3 -106.86(12) . . . . ? C57 As2 Rh3 Cl3 90.75(10) . . . . ? C58 As2 Rh3 Cl3 -8.24(10) . . . . ? Rh4 As2 Rh3 Cl3 177.30(3) . . . . ? C59 As2 Rh3 Rh4 75.83(12) . . . . ? C57 As2 Rh3 Rh4 -86.55(10) . . . . ? C58 As2 Rh3 Rh4 174.45(9) . . . . ? C51 C44 Rh4 C31 144.01(18) . . . . ? C45 C44 Rh4 C31 -78.19(16) . . . . ? Rh3 C44 Rh4 C31 35.90(8) . . . . ? C51 C44 Rh4 Cl4 -52.08(18) . . . 3_565 ? C45 C44 Rh4 Cl4 85.72(15) . . . 3_565 ? Rh3 C44 Rh4 Cl4 -160.18(5) . . . 3_565 ? C51 C44 Rh4 As2 54.56(17) . . . . ? C45 C44 Rh4 As2 -167.64(15) . . . . ? Rh3 C44 Rh4 As2 -53.54(5) . . . . ? C51 C44 Rh4 Cl4 -101.7(4) . . . . ? C45 C44 Rh4 Cl4 36.1(5) . . . . ? Rh3 C44 Rh4 Cl4 150.2(3) . . . . ? C51 C44 Rh4 Rh3 108.11(19) . . . . ? C45 C44 Rh4 Rh3 -114.09(17) . . . . ? C32 C31 Rh4 C44 78.78(16) . . . . ? C38 C31 Rh4 C44 -145.04(18) . . . . ? Rh3 C31 Rh4 C44 -36.30(8) . . . . ? C32 C31 Rh4 Cl4 -22.4(3) . . . 3_565 ? C38 C31 Rh4 Cl4 113.8(2) . . . 3_565 ? Rh3 C31 Rh4 Cl4 -137.45(19) . . . 3_565 ? C32 C31 Rh4 As2 167.75(15) . . . . ? C38 C31 Rh4 As2 -56.07(17) . . . . ? Rh3 C31 Rh4 As2 52.68(5) . . . . ? C32 C31 Rh4 Cl4 -92.00(15) . . . . ? C38 C31 Rh4 Cl4 44.18(18) . . . . ? Rh3 C31 Rh4 Cl4 152.92(5) . . . . ? C32 C31 Rh4 Rh3 115.07(17) . . . . ? C38 C31 Rh4 Rh3 -108.75(19) . . . . ? C59 As2 Rh4 C44 -86.74(13) . . . . ? C57 As2 Rh4 C44 166.82(11) . . . . ? C58 As2 Rh4 C44 34.24(19) . . . . ? Rh3 As2 Rh4 C44 44.54(6) . . . . ? C59 As2 Rh4 C31 -174.68(13) . . . . ? C57 As2 Rh4 C31 78.89(11) . . . . ? C58 As2 Rh4 C31 -53.69(19) . . . . ? Rh3 As2 Rh4 C31 -43.39(6) . . . . ? C59 As2 Rh4 Cl4 8.28(11) . . . 3_565 ? C57 As2 Rh4 Cl4 -98.15(9) . . . 3_565 ? C58 As2 Rh4 Cl4 129.27(18) . . . 3_565 ? Rh3 As2 Rh4 Cl4 139.567(17) . . . 3_565 ? C59 As2 Rh4 Cl4 89.16(11) . . . . ? C57 As2 Rh4 Cl4 -17.27(9) . . . . ? C58 As2 Rh4 Cl4 -149.86(18) . . . . ? Rh3 As2 Rh4 Cl4 -139.556(16) . . . . ? C59 As2 Rh4 Rh3 -131.28(11) . . . . ? C57 As2 Rh4 Rh3 122.28(9) . . . . ? C58 As2 Rh4 Rh3 -10.30(18) . . . . ? Rh4 Cl4 Rh4 C44 50.8(4) 3_565 . . . ? Rh4 Cl4 Rh4 C31 164.39(6) 3_565 . . . ? Rh4 Cl4 Rh4 Cl4 0.0 3_565 . . 3_565 ? Rh4 Cl4 Rh4 As2 -105.098(19) 3_565 . . . ? Rh4 Cl4 Rh4 Rh3 -164.252(14) 3_565 . . . ? C31 Rh3 Rh4 C44 129.81(11) . . . . ? Cl3 Rh3 Rh4 C44 77.43(14) . . . . ? As2 Rh3 Rh4 C44 -114.41(8) . . . . ? C44 Rh3 Rh4 C31 -129.81(11) . . . . ? Cl3 Rh3 Rh4 C31 -52.38(14) . . . . ? As2 Rh3 Rh4 C31 115.78(8) . . . . ? C31 Rh3 Rh4 Cl4 162.36(9) . . . 3_565 ? C44 Rh3 Rh4 Cl4 32.55(8) . . . 3_565 ? Cl3 Rh3 Rh4 Cl4 109.98(12) . . . 3_565 ? As2 Rh3 Rh4 Cl4 -81.86(3) . . . 3_565 ? C31 Rh3 Rh4 As2 -115.78(8) . . . . ? C44 Rh3 Rh4 As2 114.41(8) . . . . ? Cl3 Rh3 Rh4 As2 -168.16(12) . . . . ? C31 Rh3 Rh4 Cl4 -42.71(8) . . . . ? C44 Rh3 Rh4 Cl4 -172.52(8) . . . . ? Cl3 Rh3 Rh4 Cl4 -95.08(12) . . . . ? As2 Rh3 Rh4 Cl4 73.08(2) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.664 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.069 data_tp7neu _database_code_depnum_ccdc_archive 'CCDC 229311' _publ_section_abstract ; The dinuclear complex [Rh2I2(µ-CPh2)2(µ-PMe3)] was prepared from the Rh2(acac)2 counterpart and Me3SiI and shown crystallographically to contain the PMe3 ligand in a truly symmetrical bridging position; a new synthetic route to migrate more bulky phosphines such as PPh3 and PiPr3 from a terminal into a bridging site is also described. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H33 I2 O0.67 P Rh2' _chemical_formula_weight 906.83 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' Rh Rh -1.1178 0.9187 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 22.9416(17) _cell_length_b 22.9416(17) _cell_length_c 31.230(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14235(2) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9283 _cell_measurement_theta_min 2.431 _cell_measurement_theta_max 24.492 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7836 _exptl_absorpt_coefficient_mu 3.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _exptl_special_details ; The asymmetric unit contains half a molecule. Additionally two third of a solvent molecule is found. ; _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 Smart Apex with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53403 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.14 _reflns_number_total 2818 _reflns_number_gt 2780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-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^)+(0.0187P)^2^+592.5870P] 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 2818 _refine_ls_number_parameters 188 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.337 _refine_ls_restrained_S_all 1.336 _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 0.3730(4) 0.3594(4) 0.3803(3) 0.031(2) Uani 1 1 d . . . C2 C 0.3827(4) 0.4290(4) 0.3768(3) 0.0290(19) Uani 1 1 d . . . C3 C 0.4416(5) 0.4845(5) 0.3929(3) 0.040(2) Uani 1 1 d . . . H3 H 0.4748 0.4770 0.4057 0.048 Uiso 1 1 calc R . . C4 C 0.4529(5) 0.5493(5) 0.3906(3) 0.041(2) Uani 1 1 d . . . H4 H 0.4930 0.5856 0.4021 0.049 Uiso 1 1 calc R . . C5 C 0.4054(5) 0.5611(5) 0.3716(4) 0.046(3) Uani 1 1 d . . . H5 H 0.4127 0.6055 0.3689 0.056 Uiso 1 1 calc R . . C6 C 0.3471(6) 0.5068(5) 0.3567(4) 0.055(3) Uani 1 1 d . . . H6 H 0.3135 0.5145 0.3447 0.066 Uiso 1 1 calc R . . C7 C 0.3352(5) 0.4416(5) 0.3583(4) 0.043(2) Uani 1 1 d . . . H7 H 0.2948 0.4056 0.3468 0.052 Uiso 1 1 calc R . . C8 C 0.4069(4) 0.3439(4) 0.3450(3) 0.033(2) Uani 1 1 d . . . C9 C 0.3738(5) 0.3181(5) 0.3059(3) 0.040(2) Uani 1 1 d . . . H9 H 0.3303 0.3125 0.3015 0.048 Uiso 1 1 calc R . . C10 C 0.4035(6) 0.3006(5) 0.2735(4) 0.049(3) Uani 1 1 d . . . H10 H 0.3802 0.2831 0.2473 0.058 Uiso 1 1 calc R . . C11 C 0.4663(6) 0.3085(5) 0.2792(4) 0.048(3) Uani 1 1 d . . . H11 H 0.4862 0.2955 0.2573 0.057 Uiso 1 1 calc R . . C12 C 0.5006(6) 0.3353(6) 0.3168(4) 0.049(3) Uani 1 1 d . . . H12 H 0.5446 0.3419 0.3204 0.059 Uiso 1 1 calc R . . C13 C 0.4715(5) 0.3529(5) 0.3496(4) 0.044(2) Uani 1 1 d . . . H13 H 0.4958 0.3713 0.3754 0.052 Uiso 1 1 calc R . . C14 C 0.3348(13) 0.1827(12) 0.4656(7) 0.047(5) Uani 0.50 1 d P . . H14A H 0.3410 0.1439 0.4609 0.070 Uiso 0.50 1 calc PR . . H14B H 0.2922 0.1682 0.4806 0.070 Uiso 0.50 1 calc PR . . H14C H 0.3721 0.2165 0.4828 0.070 Uiso 0.50 1 calc PR . . C15 C 0.2413(13) 0.1349(11) 0.3975(8) 0.055(6) Uani 0.50 1 d P . . H15A H 0.2440 0.0937 0.3993 0.083 Uiso 0.50 1 calc PR . . H15B H 0.2316 0.1415 0.3679 0.083 Uiso 0.50 1 calc PR . . H15C H 0.2053 0.1310 0.4163 0.083 Uiso 0.50 1 calc PR . . C16 C 0.3788(15) 0.2029(12) 0.3807(7) 0.052(6) Uani 0.50 1 d P . . H16A H 0.3715 0.1573 0.3847 0.078 Uiso 0.50 1 calc PR . . H16B H 0.4267 0.2357 0.3846 0.078 Uiso 0.50 1 calc PR . . H16C H 0.3650 0.2071 0.3517 0.078 Uiso 0.50 1 calc PR . . I1 I 0.49132(4) 0.39739(4) 0.48737(3) 0.0566(3) Uani 1 1 d . . . P P 0.3333 0.21742(17) 0.4167 0.0552(12) Uani 1 2 d S . . Rh1 Rh 0.38501(3) 0.33315(4) 0.43961(2) 0.0310(2) Uani 1 1 d . . . C20 C 0.6667 0.3333 0.2481 0.151(18) Uani 1 3 d SD . . C21 C 0.6060 0.2734 0.2696 0.159(15) Uani 0.67 1 d PDU . . H21A H 0.6115 0.2773 0.3007 0.239 Uiso 0.67 1 calc PR . . H21B H 0.6030 0.2313 0.2600 0.239 Uiso 0.67 1 calc PR . . H21C H 0.5646 0.2734 0.2616 0.239 Uiso 0.67 1 calc PR . . O O 0.629(3) 0.289(2) 0.2171(11) 0.23(3) Uani 0.33 1 d PDU . . 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 0.022(4) 0.030(5) 0.035(5) 0.006(4) -0.001(4) 0.009(4) C2 0.027(4) 0.031(5) 0.028(5) 0.009(4) 0.008(4) 0.013(4) C3 0.035(5) 0.036(5) 0.045(6) -0.002(5) -0.012(5) 0.014(4) C4 0.036(5) 0.031(5) 0.037(6) 0.002(4) 0.005(4) 0.004(4) C5 0.046(6) 0.032(5) 0.059(7) 0.011(5) 0.016(5) 0.018(5) C6 0.041(6) 0.041(6) 0.088(9) 0.013(6) -0.006(6) 0.024(5) C7 0.026(5) 0.039(6) 0.058(7) 0.005(5) 0.003(5) 0.012(4) C8 0.028(5) 0.022(4) 0.044(6) 0.005(4) 0.000(4) 0.010(4) C9 0.040(6) 0.039(5) 0.042(6) 0.010(5) 0.004(5) 0.021(5) C10 0.069(8) 0.039(6) 0.038(6) -0.001(5) 0.003(6) 0.027(6) C11 0.065(7) 0.035(6) 0.045(6) 0.001(5) 0.017(6) 0.027(5) C12 0.044(6) 0.053(7) 0.051(7) -0.002(6) 0.007(5) 0.025(5) C13 0.037(5) 0.040(6) 0.049(7) -0.002(5) 0.002(5) 0.016(5) C14 0.061(15) 0.045(13) 0.040(13) -0.001(10) -0.012(12) 0.032(12) C15 0.072(16) 0.033(11) 0.064(16) 0.000(11) -0.007(13) 0.028(11) C16 0.084(19) 0.048(14) 0.042(14) 0.002(11) 0.013(13) 0.046(14) I1 0.0365(4) 0.0505(5) 0.0701(6) 0.0087(4) -0.0203(4) 0.0123(3) P 0.096(4) 0.0420(14) 0.045(2) 0.0142(12) 0.028(2) 0.0482(18) Rh1 0.0259(4) 0.0312(4) 0.0371(4) 0.0013(3) -0.0017(3) 0.0151(3) C20 0.19(3) 0.19(3) 0.06(2) 0.000 0.000 0.097(14) C21 0.16(2) 0.18(2) 0.18(2) 0.024(16) -0.001(16) 0.111(17) O 0.22(4) 0.22(4) 0.24(4) -0.018(19) -0.02(2) 0.11(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 C1 C8 1.492(13) . ? C1 C2 1.503(12) . ? C1 Rh1 2.004(9) 12 ? C1 Rh1 2.008(9) . ? C2 C7 1.384(13) . ? C2 C3 1.407(13) . ? C3 C4 1.377(14) . ? C4 C5 1.382(15) . ? C5 C6 1.375(16) . ? C6 C7 1.380(15) . ? C8 C13 1.398(13) . ? C8 C9 1.404(14) . ? C9 C10 1.385(15) . ? C10 C11 1.372(16) . ? C11 C12 1.375(16) . ? C12 C13 1.387(15) . ? C14 P 1.73(2) . ? C15 P 2.10(2) . ? C16 P 1.68(2) . ? I1 Rh1 2.5981(10) . ? P C16 1.68(2) 12 ? P C14 1.73(2) 12 ? P C15 2.10(2) 12 ? P Rh1 2.413(3) . ? P Rh1 2.413(3) 12 ? Rh1 C1 2.004(9) 12 ? Rh1 Rh1 2.5042(14) 12 ? C20 O 1.36(4) 2_655 ? C20 O 1.36(4) . ? C20 O 1.36(4) 3_665 ? C20 C21 1.5382 2_655 ? C20 C21 1.5382 . ? C20 C21 1.53823(10) 3_665 ? O O 1.66(6) 2_655 ? O O 1.66(6) 3_665 ? 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 C8 C1 C2 112.4(7) . . ? C8 C1 Rh1 112.3(6) . 12 ? C2 C1 Rh1 119.8(6) . 12 ? C8 C1 Rh1 116.4(6) . . ? C2 C1 Rh1 114.7(6) . . ? Rh1 C1 Rh1 77.2(3) 12 . ? C7 C2 C3 117.5(9) . . ? C7 C2 C1 122.5(9) . . ? C3 C2 C1 120.0(8) . . ? C4 C3 C2 122.4(9) . . ? C3 C4 C5 119.5(10) . . ? C6 C5 C4 118.2(10) . . ? C5 C6 C7 123.1(10) . . ? C6 C7 C2 119.3(10) . . ? C13 C8 C9 117.5(9) . . ? C13 C8 C1 122.0(9) . . ? C9 C8 C1 120.5(8) . . ? C10 C9 C8 121.2(10) . . ? C11 C10 C9 120.2(11) . . ? C10 C11 C12 119.8(10) . . ? C11 C12 C13 120.7(11) . . ? C12 C13 C8 120.6(10) . . ? C16 P C16 118.6(16) 12 . ? C16 P C14 34.7(11) 12 . ? C16 P C14 110.0(11) . . ? C16 P C14 110.0(11) 12 12 ? C16 P C14 34.7(11) . 12 ? C14 P C14 124.0(15) . 12 ? C16 P C15 61.2(11) 12 . ? C16 P C15 94.3(12) . . ? C14 P C15 94.6(11) . . ? C14 P C15 63.0(11) 12 . ? C16 P C15 94.3(12) 12 12 ? C16 P C15 61.2(11) . 12 ? C14 P C15 63.0(11) . 12 ? C14 P C15 94.6(11) 12 12 ? C15 P C15 133.0(13) . 12 ? C16 P Rh1 117.8(8) 12 . ? C16 P Rh1 113.9(9) . . ? C14 P Rh1 97.6(8) . . ? C14 P Rh1 132.1(8) 12 . ? C15 P Rh1 142.8(7) . . ? C15 P Rh1 83.4(6) 12 . ? C16 P Rh1 113.9(9) 12 12 ? C16 P Rh1 117.8(8) . 12 ? C14 P Rh1 132.1(8) . 12 ? C14 P Rh1 97.6(8) 12 12 ? C15 P Rh1 83.4(6) . 12 ? C15 P Rh1 142.8(7) 12 12 ? Rh1 P Rh1 62.53(10) . 12 ? C1 Rh1 C1 87.1(4) 12 . ? C1 Rh1 P 89.6(3) 12 . ? C1 Rh1 P 89.5(3) . . ? C1 Rh1 Rh1 51.5(3) 12 12 ? C1 Rh1 Rh1 51.3(2) . 12 ? P Rh1 Rh1 58.74(5) . 12 ? C1 Rh1 I1 125.5(3) 12 . ? C1 Rh1 I1 126.1(2) . . ? P Rh1 I1 126.88(6) . . ? Rh1 Rh1 I1 174.37(2) 12 . ? O C20 O 75.0(17) 2_655 . ? O C20 O 75.0(17) 2_655 3_665 ? O C20 O 75.0(17) . 3_665 ? O C20 C21 71.6(10) 2_655 2_655 ? O C20 C21 123(4) . 2_655 ? O C20 C21 135(4) 3_665 2_655 ? O C20 C21 135(4) 2_655 . ? O C20 C21 71.6(10) . . ? O C20 C21 123(4) 3_665 . ? C21 C20 C21 102.372(3) 2_655 . ? O C20 C21 123(4) 2_655 3_665 ? O C20 C21 135(4) . 3_665 ? O C20 C21 71.6(10) 3_665 3_665 ? C21 C20 C21 102.372(3) 2_655 3_665 ? C21 C20 C21 102.372(3) . 3_665 ? C20 O O 52.5(8) . 2_655 ? C20 O O 52.5(8) . 3_665 ? O O O 60.000(11) 2_655 3_665 ? 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 C8 C1 C2 C7 96.9(10) . . . . ? Rh1 C1 C2 C7 -38.2(12) 12 . . . ? Rh1 C1 C2 C7 -127.2(9) . . . . ? C8 C1 C2 C3 -83.5(11) . . . . ? Rh1 C1 C2 C3 141.4(8) 12 . . . ? Rh1 C1 C2 C3 52.4(10) . . . . ? C7 C2 C3 C4 -0.1(15) . . . . ? C1 C2 C3 C4 -179.7(9) . . . . ? C2 C3 C4 C5 -0.7(16) . . . . ? C3 C4 C5 C6 2.0(16) . . . . ? C4 C5 C6 C7 -2.7(19) . . . . ? C5 C6 C7 C2 2.0(19) . . . . ? C3 C2 C7 C6 -0.5(15) . . . . ? C1 C2 C7 C6 179.1(10) . . . . ? C2 C1 C8 C13 94.9(11) . . . . ? Rh1 C1 C8 C13 -126.6(8) 12 . . . ? Rh1 C1 C8 C13 -40.2(11) . . . . ? C2 C1 C8 C9 -86.6(10) . . . . ? Rh1 C1 C8 C9 51.9(10) 12 . . . ? Rh1 C1 C8 C9 138.3(7) . . . . ? C13 C8 C9 C10 1.6(14) . . . . ? C1 C8 C9 C10 -177.0(9) . . . . ? C8 C9 C10 C11 -0.1(16) . . . . ? C9 C10 C11 C12 -1.5(17) . . . . ? C10 C11 C12 C13 1.7(17) . . . . ? C11 C12 C13 C8 -0.2(17) . . . . ? C9 C8 C13 C12 -1.4(15) . . . . ? C1 C8 C13 C12 177.2(9) . . . . ? C8 C1 Rh1 C1 -149.5(6) . . . 12 ? C2 C1 Rh1 C1 76.5(6) . . . 12 ? Rh1 C1 Rh1 C1 -40.7(4) 12 . . 12 ? C8 C1 Rh1 P -59.9(6) . . . . ? C2 C1 Rh1 P 166.0(6) . . . . ? Rh1 C1 Rh1 P 48.9(2) 12 . . . ? C8 C1 Rh1 Rh1 -108.8(7) . . . 12 ? C2 C1 Rh1 Rh1 117.1(7) . . . 12 ? C8 C1 Rh1 I1 77.6(7) . . . . ? C2 C1 Rh1 I1 -56.5(7) . . . . ? Rh1 C1 Rh1 I1 -173.68(5) 12 . . . ? C16 P Rh1 C1 -60.5(11) 12 . . 12 ? C16 P Rh1 C1 153.8(10) . . . 12 ? C14 P Rh1 C1 -90.3(9) . . . 12 ? C14 P Rh1 C1 117.9(12) 12 . . 12 ? C15 P Rh1 C1 17.6(12) . . . 12 ? C15 P Rh1 C1 -151.8(8) 12 . . 12 ? Rh1 P Rh1 C1 43.6(3) 12 . . 12 ? C16 P Rh1 C1 -147.5(11) 12 . . . ? C16 P Rh1 C1 66.7(10) . . . . ? C14 P Rh1 C1 -177.4(9) . . . . ? C14 P Rh1 C1 30.9(12) 12 . . . ? C15 P Rh1 C1 -69.4(12) . . . . ? C15 P Rh1 C1 121.1(8) 12 . . . ? Rh1 P Rh1 C1 -43.5(3) 12 . . . ? C16 P Rh1 Rh1 -104.0(11) 12 . . 12 ? C16 P Rh1 Rh1 110.2(10) . . . 12 ? C14 P Rh1 Rh1 -133.9(9) . . . 12 ? C14 P Rh1 Rh1 74.4(11) 12 . . 12 ? C15 P Rh1 Rh1 -25.9(11) . . . 12 ? C15 P Rh1 Rh1 164.6(7) 12 . . 12 ? C16 P Rh1 I1 75.6(11) 12 . . . ? C16 P Rh1 I1 -70.2(10) . . . . ? C14 P Rh1 I1 45.7(9) . . . . ? C14 P Rh1 I1 -106.0(11) 12 . . . ? C15 P Rh1 I1 153.7(11) . . . . ? C15 P Rh1 I1 -15.8(7) 12 . . . ? Rh1 P Rh1 I1 179.61(7) 12 . . . ? O C20 O O 78.1(10) 3_665 . . 2_655 ? C21 C20 O O -56(4) 2_655 . . 2_655 ? C21 C20 O O -149(5) . . . 2_655 ? C21 C20 O O 122(4) 3_665 . . 2_655 ? O C20 O O -78.1(10) 2_655 . . 3_665 ? C21 C20 O O -134(4) 2_655 . . 3_665 ? C21 C20 O O 133(5) . . . 3_665 ? C21 C20 O O 44(4) 3_665 . . 3_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.526 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.153