# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1576 data_COMPOUND5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H34 Cl4 O4 P2 Rh2, 2(C H Cl3)' _chemical_formula_sum 'C42 H36 Cl10 O4 P2 Rh2' _chemical_formula_weight 1226.97 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.398(6) _cell_length_b 13.623(5) _cell_length_c 14.538(5) _cell_angle_alpha 77.40(5) _cell_angle_beta 84.25(5) _cell_angle_gamma 69.69(4) _cell_volume 2427.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Enraf-Nonius CAD4 single crystal diffractometer. ; _diffrn_ambient_temperature 290(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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\Q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6.23 _diffrn_reflns_number 8941 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.98 _reflns_number_total 8538 _reflns_number_gt 6549 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Nonius CAD-4 Diffractometer Control Software. Data collection with profile analysis over all reflections (Lehman and Larsen, 1974 Grant and Gable, 1978) ; _computing_cell_refinement 'CRYSDA (Beurskens et al, 1992)' _computing_data_reduction 'THE REFLEX (local program)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'EUCLID (Spek, 1982)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+3.7821P] 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 8538 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.82778(3) 0.68124(2) 0.20280(2) 0.03243(10) Uani 1 d . . . Rh2 Rh 0.73877(2) 0.70592(2) 0.36501(2) 0.03065(10) Uani 1 d . . . Cl3 Cl 0.73424(9) 0.87823(8) 0.36110(7) 0.0384(2) Uani 1 d . . . Cl4 Cl 0.68234(8) 0.75549(9) 0.10498(7) 0.0401(2) Uani 1 d . . . C5 C 1.0823(4) 0.5619(4) 0.4012(4) 0.0563(14) Uani 1 d . . . H51 H 1.1330 0.5317 0.3548 0.13(3) Uiso 1 calc R . . H52 H 1.0822 0.5069 0.4553 0.150 Uiso 1 calc R . . H53 H 1.1013 0.6164 0.4198 0.13(3) Uiso 1 calc R . . C6 C 0.9729(3) 0.6098(3) 0.3601(3) 0.0384(10) Uani 1 d . . . O7 O 0.9655(2) 0.6033(2) 0.2758(2) 0.0442(7) Uani 1 d . . . O8 O 0.8967(2) 0.6530(2) 0.4110(2) 0.0422(7) Uani 1 d . . . C9 C 0.7591(5) 0.3902(4) 0.3367(5) 0.0696(17) Uani 1 d . . . H91 H 0.7788 0.3601 0.2810 0.13(3) Uiso 1 calc R . . H92 H 0.6865 0.3964 0.3545 0.11(3) Uiso 1 calc R . . H93 H 0.8047 0.3447 0.3871 0.12(3) Uiso 1 calc R . . C10 C 0.7705(4) 0.4998(4) 0.3172(4) 0.0450(11) Uani 1 d . . . O11 O 0.7476(3) 0.5496(2) 0.3837(2) 0.0440(7) Uani 1 d . . . O12 O 0.7989(3) 0.5352(2) 0.2354(2) 0.0499(8) Uani 1 d . . . P13 P 0.56236(8) 0.76181(8) 0.34459(8) 0.0320(2) Uani 1 d . . . C14 C 0.4889(3) 0.8809(3) 0.2604(3) 0.0346(9) Uani 1 d . . . C15 C 0.4828(4) 0.9800(4) 0.2745(4) 0.0493(12) Uani 1 d . . . H15 H 0.5193 0.9850 0.3235 0.054(15) Uiso 1 calc R . . C16 C 0.3684(4) 1.0664(4) 0.1435(4) 0.0563(13) Uani 1 d . . . H16 H 0.3274 1.1285 0.1049 0.063(16) Uiso 1 calc R . . C17 C 0.4225(4) 1.0717(4) 0.2159(4) 0.0566(13) Uani 1 d . . . H17 H 0.4188 1.1380 0.2260 0.067(17) Uiso 1 calc R . . C18 C 0.3754(4) 0.9678(5) 0.1285(4) 0.0642(15) Uani 1 d . . . H18 H 0.3397 0.9634 0.0787 0.076(18) Uiso 1 calc R . . C19 C 0.4349(4) 0.8753(4) 0.1868(3) 0.0477(11) Uani 1 d . . . H19 H 0.4386 0.8092 0.1763 0.046(14) Uiso 1 calc R . . C20 C 0.5086(3) 0.6583(3) 0.3330(3) 0.0386(10) Uani 1 d . . . C21 C 0.5290(4) 0.6172(4) 0.2509(4) 0.0495(12) Uani 1 d . . . H21 H 0.5734 0.6392 0.2037 0.052(14) Uiso 1 calc R . . C22 C 0.4838(5) 0.5443(4) 0.2388(4) 0.0590(14) Uani 1 d . . . H22 H 0.4973 0.5178 0.1834 0.053(15) Uiso 1 calc R . . C23 C 0.4186(5) 0.5103(4) 0.3084(4) 0.0602(14) Uani 1 d . . . H23 H 0.3867 0.4627 0.2991 0.049(14) Uiso 1 calc R . . C24 C 0.4009(4) 0.5469(4) 0.3917(4) 0.0575(14) Uani 1 d . . . H24 H 0.3593 0.5217 0.4397 0.055(15) Uiso 1 calc R . . C25 C 0.4446(4) 0.6212(4) 0.4043(3) 0.0448(11) Uani 1 d . . . H25 H 0.4315 0.6465 0.4603 0.060(16) Uiso 1 calc R . . C26 C 0.4981(4) 0.7980(3) 0.4560(3) 0.0391(10) Uani 1 d . . . C27 C 0.3897(4) 0.8578(4) 0.4610(4) 0.0529(12) Uani 1 d . . . H27 H 0.3508 0.8828 0.4061 0.051(14) Uiso 1 calc R . . C28 C 0.3394(5) 0.8804(5) 0.5445(4) 0.0708(17) Uani 1 d . . . H28 H 0.2673 0.9204 0.5460 0.069(17) Uiso 1 calc R . . C29 C 0.3965(6) 0.8432(5) 0.6271(4) 0.0735(18) Uani 1 d . . . H29 H 0.3629 0.8592 0.6837 0.058(15) Uiso 1 calc R . . C30 C 0.5019(5) 0.7831(4) 0.6251(4) 0.0585(14) Uani 1 d . . . H30 H 0.5397 0.7567 0.6806 0.075(19) Uiso 1 calc R . . C31 C 0.5520(4) 0.7617(4) 0.5408(3) 0.0423(10) Uani 1 d . . . Cl32 Cl 0.68766(8) 0.68484(9) 0.54317(7) 0.0373(2) Uani 1 d . . . P33 P 0.87649(8) 0.82547(8) 0.14518(7) 0.0315(2) Uani 1 d . . . C34 C 1.0058(3) 0.8124(3) 0.1873(3) 0.0374(10) Uani 1 d . . . C35 C 1.0126(4) 0.8284(4) 0.2773(3) 0.0471(11) Uani 1 d . . . H35 H 0.9514 0.8474 0.3151 0.049(14) Uiso 1 calc R . . C36 C 1.1100(4) 0.8160(5) 0.3109(4) 0.0579(14) Uani 1 d . . . H36 H 1.1138 0.8281 0.3708 0.08(2) Uiso 1 calc R . . C37 C 1.2015(4) 0.7859(5) 0.2562(4) 0.0632(15) Uani 1 d . . . H37 H 1.2671 0.7770 0.2791 0.069(17) Uiso 1 calc R . . C38 C 1.1948(4) 0.7692(5) 0.1677(5) 0.0701(17) Uani 1 d . . . H38 H 1.2563 0.7485 0.1307 0.09(2) Uiso 1 calc R . . C39 C 1.0979(4) 0.7828(4) 0.1330(4) 0.0552(13) Uani 1 d . . . H39 H 1.0945 0.7720 0.0726 0.061(16) Uiso 1 calc R . . C40 C 0.7960(3) 0.9662(3) 0.1404(3) 0.0344(9) Uani 1 d . . . C41 C 0.8441(4) 1.0384(4) 0.1503(4) 0.0562(14) Uani 1 d . . . H41 H 0.9148 1.0141 0.1677 0.063(16) Uiso 1 calc R . . C42 C 0.7867(5) 1.1472(4) 0.1343(5) 0.0656(16) Uani 1 d . . . H42 H 0.8187 1.1952 0.1425 0.09(2) Uiso 1 calc R . . C43 C 0.6849(4) 1.1834(4) 0.1069(4) 0.0583(14) Uani 1 d . . . H43 H 0.6474 1.2563 0.0945 0.070(17) Uiso 1 calc R . . C44 C 0.6371(4) 1.1125(4) 0.0973(4) 0.0573(14) Uani 1 d . . . H44 H 0.5669 1.1378 0.0783 0.062(16) Uiso 1 calc R . . C45 C 0.6912(4) 1.0043(4) 0.1153(3) 0.0446(11) Uani 1 d . . . H45 H 0.6569 0.9570 0.1104 0.046(13) Uiso 1 calc R . . C46 C 0.9039(3) 0.8245(3) 0.0188(3) 0.0373(10) Uani 1 d . . . C47 C 0.8949(4) 0.9181(4) -0.0484(3) 0.0448(11) Uani 1 d . . . H47 H 0.8728 0.9835 -0.0294 0.042(13) Uiso 1 calc R . . C48 C 0.9183(4) 0.9142(5) -0.1422(4) 0.0577(14) Uani 1 d . . . H48 H 0.9114 0.9771 -0.1859 0.070(17) Uiso 1 calc R . . C49 C 0.9520(5) 0.8183(5) -0.1721(4) 0.0631(15) Uani 1 d . . . H49 H 0.9683 0.8166 -0.2356 0.071(18) Uiso 1 calc R . . C50 C 0.9614(4) 0.7260(5) -0.1086(4) 0.0558(13) Uani 1 d . . . H50 H 0.9842 0.6611 -0.1285 0.075(19) Uiso 1 calc R . . C51 C 0.9372(4) 0.7293(4) -0.0150(3) 0.0447(11) Uani 1 d . . . Cl52 Cl 0.94609(9) 0.60813(8) 0.06440(8) 0.0446(3) Uani 1 d . . . C53 C 0.8860(5) 0.8010(5) 0.5711(4) 0.0682(16) Uani 1 d . . . H531 H 0.8616 0.7922 0.5130 0.11(3) Uiso 1 calc R . . Cl54 Cl 0.77615(14) 0.86704(15) 0.63487(13) 0.0861(5) Uani 1 d . . . Cl55 Cl 0.95174(15) 0.67399(14) 0.63797(14) 0.0891(5) Uani 1 d . . . Cl56 Cl 0.9719(2) 0.8744(2) 0.54134(16) 0.1196(8) Uani 1 d . . . C57 C 0.2934(5) 0.4319(5) 0.0369(6) 0.082(2) Uani 1 d . . . H571 H 0.2766 0.3911 -0.0035 0.11(3) Uiso 1 calc R . . Cl58 Cl 0.42950(18) 0.3865(3) 0.0480(3) 0.1687(15) Uani 1 d . . . Cl59 Cl 0.2319(3) 0.4086(3) 0.1454(2) 0.1646(13) Uani 1 d . . . Cl60 Cl 0.2463(3) 0.56285(19) -0.0147(2) 0.1494(11) Uani 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 Rh1 0.03400(18) 0.03010(17) 0.03259(18) -0.00666(13) 0.00030(14) -0.01001(14) Rh2 0.02936(17) 0.03235(17) 0.03013(18) -0.00360(13) -0.00288(13) -0.01116(13) Cl3 0.0429(6) 0.0366(5) 0.0390(6) -0.0085(4) -0.0022(5) -0.0166(5) Cl4 0.0391(6) 0.0462(6) 0.0378(6) -0.0082(5) -0.0037(4) -0.0171(5) C5 0.040(3) 0.055(3) 0.061(3) 0.009(3) -0.013(3) -0.008(2) C6 0.035(2) 0.030(2) 0.045(3) 0.0041(19) -0.005(2) -0.0106(18) O7 0.0390(17) 0.0411(17) 0.0435(19) -0.0029(14) -0.0037(14) -0.0047(14) O8 0.0302(16) 0.0526(18) 0.0401(17) -0.0055(14) -0.0069(14) -0.0097(14) C9 0.081(4) 0.037(3) 0.092(5) -0.010(3) 0.004(4) -0.025(3) C10 0.043(3) 0.036(2) 0.053(3) -0.004(2) -0.001(2) -0.013(2) O11 0.0483(18) 0.0346(16) 0.0466(19) -0.0019(14) -0.0019(15) -0.0144(14) O12 0.063(2) 0.0364(17) 0.056(2) -0.0131(15) 0.0054(17) -0.0221(16) P13 0.0300(5) 0.0347(5) 0.0328(6) -0.0071(4) -0.0026(4) -0.0119(4) C14 0.027(2) 0.038(2) 0.035(2) -0.0045(17) 0.0003(17) -0.0088(17) C15 0.046(3) 0.047(3) 0.052(3) -0.007(2) -0.014(2) -0.010(2) C16 0.051(3) 0.051(3) 0.052(3) 0.007(2) -0.013(2) -0.005(2) C17 0.052(3) 0.041(3) 0.068(4) -0.001(2) -0.007(3) -0.009(2) C18 0.055(3) 0.082(4) 0.046(3) -0.006(3) -0.018(3) -0.011(3) C19 0.042(3) 0.052(3) 0.046(3) -0.013(2) -0.007(2) -0.009(2) C20 0.035(2) 0.040(2) 0.044(3) -0.0054(19) -0.0050(19) -0.0162(19) C21 0.052(3) 0.051(3) 0.054(3) -0.017(2) 0.007(2) -0.026(2) C22 0.074(4) 0.059(3) 0.058(3) -0.023(3) 0.002(3) -0.035(3) C23 0.067(4) 0.051(3) 0.076(4) -0.007(3) -0.014(3) -0.037(3) C24 0.064(3) 0.058(3) 0.059(3) 0.000(3) -0.004(3) -0.037(3) C25 0.048(3) 0.047(3) 0.044(3) -0.003(2) -0.005(2) -0.024(2) C26 0.041(2) 0.038(2) 0.039(2) -0.0110(19) 0.0046(19) -0.0131(19) C27 0.047(3) 0.052(3) 0.052(3) -0.011(2) 0.004(2) -0.008(2) C28 0.063(4) 0.067(4) 0.066(4) -0.020(3) 0.024(3) -0.003(3) C29 0.098(5) 0.063(4) 0.050(3) -0.024(3) 0.030(3) -0.017(3) C30 0.080(4) 0.056(3) 0.039(3) -0.015(2) 0.003(3) -0.020(3) C31 0.053(3) 0.041(2) 0.038(2) -0.0118(19) 0.006(2) -0.020(2) Cl32 0.0348(5) 0.0485(6) 0.0286(5) 0.0011(4) -0.0051(4) -0.0181(5) P33 0.0285(5) 0.0327(5) 0.0321(6) -0.0056(4) -0.0008(4) -0.0091(4) C34 0.032(2) 0.036(2) 0.044(2) -0.0034(18) -0.0073(19) -0.0114(18) C35 0.046(3) 0.058(3) 0.040(3) -0.003(2) -0.005(2) -0.023(2) C36 0.060(3) 0.073(4) 0.048(3) 0.000(3) -0.015(3) -0.035(3) C37 0.043(3) 0.077(4) 0.070(4) 0.002(3) -0.019(3) -0.025(3) C38 0.030(3) 0.095(5) 0.081(4) -0.025(4) 0.001(3) -0.013(3) C39 0.033(2) 0.076(4) 0.059(3) -0.025(3) -0.002(2) -0.013(2) C40 0.039(2) 0.031(2) 0.031(2) -0.0038(16) 0.0025(18) -0.0109(18) C41 0.044(3) 0.042(3) 0.083(4) -0.005(3) -0.012(3) -0.016(2) C42 0.059(3) 0.039(3) 0.102(5) -0.014(3) -0.007(3) -0.020(3) C43 0.056(3) 0.035(3) 0.071(4) -0.003(2) 0.001(3) -0.005(2) C44 0.040(3) 0.046(3) 0.076(4) -0.005(3) -0.006(3) -0.005(2) C45 0.037(2) 0.040(2) 0.055(3) -0.006(2) -0.004(2) -0.012(2) C46 0.033(2) 0.044(2) 0.034(2) -0.0062(19) 0.0007(18) -0.0145(19) C47 0.038(2) 0.050(3) 0.044(3) -0.001(2) -0.001(2) -0.017(2) C48 0.053(3) 0.082(4) 0.038(3) 0.007(3) -0.004(2) -0.033(3) C49 0.067(4) 0.099(5) 0.033(3) -0.011(3) 0.004(2) -0.042(3) C50 0.054(3) 0.077(4) 0.045(3) -0.027(3) 0.008(2) -0.026(3) C51 0.039(2) 0.057(3) 0.039(3) -0.012(2) 0.003(2) -0.017(2) Cl52 0.0551(7) 0.0346(5) 0.0398(6) -0.0160(4) 0.0126(5) -0.0083(5) C53 0.069(4) 0.083(4) 0.057(3) -0.026(3) -0.007(3) -0.021(3) Cl54 0.0708(10) 0.0905(12) 0.0882(12) -0.0338(10) -0.0068(9) -0.0048(9) Cl55 0.0931(12) 0.0753(10) 0.0939(12) -0.0347(9) -0.0257(10) -0.0046(9) Cl56 0.138(2) 0.159(2) 0.0980(15) -0.0314(15) 0.0204(14) -0.0961(18) C57 0.063(4) 0.077(4) 0.114(6) -0.043(4) -0.017(4) -0.013(3) Cl58 0.0666(13) 0.179(3) 0.266(4) -0.113(3) -0.0424(18) 0.0039(15) Cl59 0.169(3) 0.228(4) 0.123(2) -0.007(2) -0.007(2) -0.115(3) Cl60 0.161(3) 0.0791(14) 0.181(3) -0.0064(16) 0.006(2) -0.0212(15) _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 O7 2.049(3) . ? Rh1 O12 2.102(3) . ? Rh1 P33 2.2474(15) . ? Rh1 Cl4 2.3243(18) . ? Rh1 Rh2 2.5692(14) . ? Rh1 Cl52 2.5870(18) . ? Rh2 O11 2.050(3) . ? Rh2 O8 2.112(3) . ? Rh2 P13 2.2466(16) . ? Rh2 Cl3 2.3154(14) . ? Rh2 Cl32 2.5916(15) . ? C5 C6 1.507(6) . ? C5 H51 0.9600 . ? C5 H52 0.9600 . ? C5 H53 0.9600 . ? C6 O8 1.248(5) . ? C6 O7 1.265(6) . ? C9 C10 1.515(7) . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 O11 1.254(6) . ? C10 O12 1.257(6) . ? P13 C14 1.835(4) . ? P13 C20 1.836(4) . ? P13 C26 1.839(5) . ? C14 C19 1.380(6) . ? C14 C15 1.382(6) . ? C15 C17 1.383(7) . ? C15 H15 0.9300 . ? C16 C17 1.363(8) . ? C16 C18 1.378(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.384(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.390(7) . ? C20 C25 1.400(6) . ? C21 C22 1.379(7) . ? C21 H21 0.9300 . ? C22 C23 1.378(8) . ? C22 H22 0.9300 . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 C25 1.383(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.396(6) . ? C26 C27 1.400(7) . ? C27 C28 1.371(8) . ? C27 H27 0.9300 . ? C28 C29 1.390(9) . ? C28 H28 0.9300 . ? C29 C30 1.365(9) . ? C29 H29 0.9300 . ? C30 C31 1.376(7) . ? C30 H30 0.9300 . ? C31 Cl32 1.754(5) . ? P33 C34 1.832(4) . ? P33 C40 1.835(4) . ? P33 C46 1.839(4) . ? C34 C39 1.380(7) . ? C34 C35 1.390(6) . ? C35 C36 1.381(7) . ? C35 H35 0.9300 . ? C36 C37 1.380(8) . ? C36 H36 0.9300 . ? C37 C38 1.371(8) . ? C37 H37 0.9300 . ? C38 C39 1.377(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.374(6) . ? C40 C41 1.387(6) . ? C41 C42 1.392(7) . ? C41 H41 0.9300 . ? C42 C43 1.348(8) . ? C42 H42 0.9300 . ? C43 C44 1.367(8) . ? C43 H43 0.9300 . ? C44 C45 1.377(7) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.400(7) . ? C46 C47 1.403(6) . ? C47 C48 1.376(7) . ? C47 H47 0.9300 . ? C48 C49 1.379(8) . ? C48 H48 0.9300 . ? C49 C50 1.363(8) . ? C49 H49 0.9300 . ? C50 C51 1.373(7) . ? C50 H50 0.9300 . ? C51 Cl52 1.769(5) . ? C53 Cl54 1.734(6) . ? C53 Cl56 1.739(7) . ? C53 Cl55 1.759(7) . ? C53 H531 0.9800 . ? C57 Cl60 1.695(7) . ? C57 Cl58 1.722(7) . ? C57 Cl59 1.724(8) . ? C57 H571 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Rh1 O12 86.72(14) . . ? O7 Rh1 P33 92.38(10) . . ? O12 Rh1 P33 169.37(10) . . ? O7 Rh1 Cl4 172.24(10) . . ? O12 Rh1 Cl4 90.44(11) . . ? P33 Rh1 Cl4 89.08(6) . . ? O7 Rh1 Rh2 85.22(10) . . ? O12 Rh1 Rh2 84.13(10) . . ? P33 Rh1 Rh2 106.37(5) . . ? Cl4 Rh1 Rh2 101.69(5) . . ? O7 Rh1 Cl52 82.86(10) . . ? O12 Rh1 Cl52 86.03(11) . . ? P33 Rh1 Cl52 83.34(6) . . ? Cl4 Rh1 Cl52 89.74(6) . . ? Rh2 Rh1 Cl52 164.94(3) . . ? O11 Rh2 O8 88.87(13) . . ? O11 Rh2 P13 91.10(10) . . ? O8 Rh2 P13 169.33(9) . . ? O11 Rh2 Cl3 173.64(9) . . ? O8 Rh2 Cl3 87.46(10) . . ? P13 Rh2 Cl3 91.54(6) . . ? O11 Rh2 Rh1 85.65(10) . . ? O8 Rh2 Rh1 84.23(10) . . ? P13 Rh2 Rh1 106.41(6) . . ? Cl3 Rh2 Rh1 99.14(6) . . ? O11 Rh2 Cl32 84.36(11) . . ? O8 Rh2 Cl32 84.72(10) . . ? P13 Rh2 Cl32 84.66(7) . . ? Cl3 Rh2 Cl32 90.13(6) . . ? Rh1 Rh2 Cl32 165.22(3) . . ? C6 C5 H51 109.5 . . ? C6 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C6 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? O8 C6 O7 124.8(4) . . ? O8 C6 C5 118.2(4) . . ? O7 C6 C5 117.0(4) . . ? C6 O7 Rh1 122.3(3) . . ? C6 O8 Rh2 120.7(3) . . ? C10 C9 H91 109.5 . . ? C10 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? C10 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? O11 C10 O12 124.9(4) . . ? O11 C10 C9 117.1(5) . . ? O12 C10 C9 118.0(5) . . ? C10 O11 Rh2 122.2(3) . . ? C10 O12 Rh1 121.2(3) . . ? C14 P13 C20 105.1(2) . . ? C14 P13 C26 100.2(2) . . ? C20 P13 C26 101.4(2) . . ? C14 P13 Rh2 124.65(14) . . ? C20 P13 Rh2 115.41(15) . . ? C26 P13 Rh2 106.56(16) . . ? C19 C14 C15 119.0(4) . . ? C19 C14 P13 122.3(4) . . ? C15 C14 P13 118.6(3) . . ? C14 C15 C17 120.1(5) . . ? C14 C15 H15 119.9 . . ? C17 C15 H15 119.9 . . ? C17 C16 C18 119.0(5) . . ? C17 C16 H16 120.5 . . ? C18 C16 H16 120.5 . . ? C16 C17 C15 121.0(5) . . ? C16 C17 H17 119.5 . . ? C15 C17 H17 119.5 . . ? C16 C18 C19 120.6(5) . . ? C16 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 120.2(5) . . ? C14 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C25 118.7(4) . . ? C21 C20 P13 119.8(3) . . ? C25 C20 P13 121.5(4) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.0(5) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 120.2(5) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C31 C26 C27 116.5(4) . . ? C31 C26 P13 122.2(3) . . ? C27 C26 P13 121.1(4) . . ? C28 C27 C26 121.8(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 119.7(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 119.8(5) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C26 122.1(5) . . ? C30 C31 Cl32 117.4(4) . . ? C26 C31 Cl32 120.4(3) . . ? C31 Cl32 Rh2 101.56(16) . . ? C34 P33 C40 104.7(2) . . ? C34 P33 C46 102.7(2) . . ? C40 P33 C46 100.5(2) . . ? C34 P33 Rh1 112.83(15) . . ? C40 P33 Rh1 127.79(14) . . ? C46 P33 Rh1 104.95(15) . . ? C39 C34 C35 118.8(4) . . ? C39 C34 P33 121.6(4) . . ? C35 C34 P33 119.6(4) . . ? C36 C35 C34 120.2(5) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.4(5) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 119.3(5) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 120.7(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 120.6(5) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C45 C40 C41 118.7(4) . . ? C45 C40 P33 120.9(3) . . ? C41 C40 P33 119.9(3) . . ? C40 C41 C42 120.1(5) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.3(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.7(5) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 121.0(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C40 C45 C44 120.0(5) . . ? C40 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C51 C46 C47 116.4(4) . . ? C51 C46 P33 121.3(3) . . ? C47 C46 P33 122.2(4) . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 120.8(5) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C50 C49 C48 119.9(5) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 119.7(5) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C46 122.5(5) . . ? C50 C51 Cl52 118.2(4) . . ? C46 C51 Cl52 119.3(3) . . ? C51 Cl52 Rh1 100.15(16) . . ? Cl54 C53 Cl56 110.5(4) . . ? Cl54 C53 Cl55 109.4(4) . . ? Cl56 C53 Cl55 110.5(4) . . ? Cl54 C53 H531 108.8 . . ? Cl56 C53 H531 108.8 . . ? Cl55 C53 H531 108.8 . . ? Cl60 C57 Cl58 112.1(4) . . ? Cl60 C57 Cl59 110.9(4) . . ? Cl58 C57 Cl59 110.2(4) . . ? Cl60 C57 H571 107.8 . . ? Cl58 C57 H571 107.8 . . ? Cl59 C57 H571 107.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.976 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.087 #=END data_COMPOUND4 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C42 H40 Cl2 O6 P2 Rh2, (3/2CH2Cl2)' _chemical_formula_sum 'C43.50 H43 Cl5 O6 P2 Rh2' _chemical_formula_weight 1106.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.9125(10) _cell_length_b 13.0427(8) _cell_length_c 19.6074(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.8900(10) _cell_angle_gamma 90.00 _cell_volume 4564.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Siemens Smart CCD diffractometer ; _diffrn_ambient_temperature 293(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 'Siemens Smart CCD' _diffrn_measurement_method '\w scans\' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16640 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 23.33 _reflns_number_total 6475 _reflns_number_observed 5256 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+54.8599P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6475 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_obs 0.0768 _refine_ls_wR_factor_all 0.2031 _refine_ls_wR_factor_obs 0.1895 _refine_ls_goodness_of_fit_all 1.090 _refine_ls_goodness_of_fit_obs 1.136 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.136 _refine_ls_shift/esd_max 0.230 _refine_ls_shift/esd_mean 0.015 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.02956(4) -0.65382(6) 0.24500(4) 0.0281(2) Uani 1 d . . Rh2 Rh -0.00117(4) -0.74958(6) 0.13209(4) 0.0295(2) Uani 1 d . . O1 O 0.0179(4) -0.5201(5) 0.1844(3) 0.039(2) Uani 1 d . . O2 O 0.0179(4) -0.6104(6) 0.0872(3) 0.037(2) Uani 1 d . . O3 O 0.1150(4) -0.7698(6) 0.1355(4) 0.043(2) Uani 1 d . . O4 O 0.1380(4) -0.6536(5) 0.2175(3) 0.035(2) Uani 1 d . . O5 O 0.0713(4) -0.5496(5) 0.3378(4) 0.043(2) Uani 1 d . . O6 O -0.0060(4) -0.8086(6) 0.0214(4) 0.046(2) Uani 1 d . . P1 P 0.05860(14) -0.7751(2) 0.32324(13) 0.0308(6) Uani 1 d . . P2 P -0.12555(14) -0.7461(2) 0.10494(13) 0.0317(6) Uani 1 d . . C1 C 0.0220(5) -0.5285(8) 0.1207(5) 0.033(2) Uani 1 d . . C2 C 0.0319(7) -0.4305(9) 0.0807(6) 0.053(3) Uani 1 d . . H2C H 0.0354(46) -0.3732(11) 0.1115(8) 0.079 Uiso 1 calc R . H2B H -0.0104(23) -0.4214(34) 0.0477(29) 0.079 Uiso 1 calc R . H2A H 0.0768(25) -0.4350(27) 0.0574(34) 0.079 Uiso 1 calc R . C3 C 0.1580(6) -0.7123(8) 0.1712(5) 0.035(2) Uani 1 d . . C4 C 0.2394(6) -0.7145(10) 0.1596(6) 0.051(3) Uani 1 d . . H4C H 0.2512(11) -0.6565(35) 0.1323(35) 0.076 Uiso 1 calc R . H4B H 0.2504(11) -0.7765(30) 0.1361(37) 0.076 Uiso 1 calc R . H4A H 0.2688(6) -0.7119(63) 0.2028(6) 0.076 Uiso 1 calc R . C10 C 0.0608(9) -0.4407(10) 0.3335(7) 0.068(4) Uani 1 d . . H10C H 0.0523(53) -0.4208(13) 0.2864(7) 0.102 Uiso 1 calc R . H10B H 0.1048(22) -0.4068(10) 0.3539(43) 0.102 Uiso 1 calc R . H10A H 0.0183(32) -0.4216(13) 0.3575(41) 0.102 Uiso 1 calc R . C11 C 0.0714(5) -0.7014(8) 0.4034(5) 0.032(2) Uani 1 d . . C12 C 0.0756(6) -0.5953(9) 0.4019(5) 0.041(3) Uani 1 d . . C13 C 0.0849(6) -0.5378(9) 0.4614(5) 0.045(3) Uani 1 d . . H13 H 0.0857(6) -0.4666(9) 0.4593(5) 0.054 Uiso 1 calc R . C14 C 0.0932(7) -0.5880(11) 0.5244(6) 0.054(3) Uani 1 d . . H14 H 0.1002(7) -0.5501(11) 0.5646(6) 0.065 Uiso 1 calc R . C15 C 0.0911(7) -0.6915(11) 0.5274(6) 0.057(3) Uani 1 d . . H15 H 0.0972(7) -0.7246(11) 0.5695(6) 0.068 Uiso 1 calc R . C16 C 0.0799(6) -0.7481(9) 0.4678(5) 0.044(3) Uani 1 d . . H16 H 0.0779(6) -0.8192(9) 0.4706(5) 0.053 Uiso 1 calc R . C21 C 0.1512(6) -0.8305(8) 0.3157(5) 0.035(2) Uani 1 d . . C22 C 0.2148(6) -0.7800(9) 0.3430(6) 0.041(3) Uani 1 d . . H22 H 0.2097(6) -0.7205(9) 0.3684(6) 0.049 Uiso 1 calc R . C23 C 0.2865(7) -0.8165(10) 0.3334(6) 0.054(3) Uani 1 d . . H23 H 0.3286(7) -0.7804(10) 0.3510(6) 0.064 Uiso 1 calc R . C24 C 0.2942(7) -0.9053(11) 0.2981(6) 0.057(3) Uani 1 d . . H24 H 0.3417(7) -0.9315(11) 0.2932(6) 0.068 Uiso 1 calc R . C25 C 0.2309(7) -0.9572(11) 0.2691(7) 0.061(4) Uani 1 d . . H25 H 0.2364(7) -1.0168(11) 0.2440(7) 0.073 Uiso 1 calc R . C26 C 0.1583(7) -0.9185(9) 0.2780(6) 0.051(3) Uani 1 d . . H26 H 0.1160(7) -0.9523(9) 0.2586(6) 0.061 Uiso 1 calc R . C31 C 0.0000(6) -0.8820(8) 0.3452(5) 0.036(2) Uani 1 d . . C32 C 0.0292(7) -0.9636(9) 0.3858(6) 0.055(3) Uani 1 d . . H32 H 0.0804(7) -0.9659(9) 0.3985(6) 0.066 Uiso 1 calc R . C33 C -0.0166(8) -1.0408(11) 0.4073(7) 0.069(4) Uani 1 d . . H33 H 0.0035(8) -1.0949(11) 0.4339(7) 0.083 Uiso 1 calc R . C34 C -0.0919(8) -1.0358(10) 0.3887(7) 0.068(4) Uani 1 d . . H34 H -0.1232(8) -1.0861(10) 0.4041(7) 0.082 Uiso 1 calc R . C35 C -0.1228(7) -0.9579(10) 0.3476(7) 0.056(3) Uani 1 d . . H35 H -0.1740(7) -0.9567(10) 0.3348(7) 0.068 Uiso 1 calc R . C36 C -0.0769(6) -0.8826(9) 0.3261(5) 0.040(3) Uani 1 d . . H36 H -0.0975(6) -0.8305(9) 0.2980(5) 0.048 Uiso 1 calc R . C40 C 0.0602(6) -0.8175(11) -0.0151(6) 0.054(3) Uani 1 d . . H40C H 0.0964(20) -0.7674(44) 0.0019(30) 0.081 Uiso 1 calc R . H40B H 0.0472(11) -0.8062(65) -0.0630(8) 0.081 Uiso 1 calc R . H40A H 0.0810(28) -0.8850(24) -0.0084(36) 0.081 Uiso 1 calc R . C41 C -0.1349(6) -0.8313(8) 0.0310(5) 0.036(2) Uani 1 d . . C42 C -0.0724(6) -0.8546(8) -0.0036(5) 0.037(3) Uani 1 d . . C43 C -0.0750(7) -0.9178(9) -0.0607(5) 0.049(3) Uani 1 d . . H43 H -0.0327(7) -0.9302(9) -0.0838(5) 0.059 Uiso 1 calc R . C44 C -0.1440(8) -0.9620(10) -0.0816(6) 0.057(3) Uani 1 d . . H44 H -0.1472(8) -1.0060(10) -0.1190(6) 0.069 Uiso 1 calc R . C45 C -0.2068(7) -0.9429(9) -0.0493(6) 0.053(3) Uani 1 d . . H45 H -0.2520(7) -0.9734(9) -0.0648(6) 0.064 Uiso 1 calc R . C46 C -0.2030(7) -0.8782(9) 0.0066(6) 0.047(3) Uani 1 d . . H46 H -0.2460(7) -0.8653(9) 0.0286(6) 0.056 Uiso 1 calc R . C51 C -0.1648(5) -0.6240(8) 0.0723(5) 0.035(2) Uani 1 d . . C52 C -0.2062(7) -0.6175(9) 0.0093(6) 0.050(3) Uani 1 d . . H52 H -0.2170(7) -0.6767(9) -0.0161(6) 0.061 Uiso 1 calc R . C53 C -0.2319(7) -0.5226(11) -0.0160(6) 0.061(4) Uani 1 d . . H53 H -0.2586(7) -0.5187(11) -0.0588(6) 0.073 Uiso 1 calc R . C54 C -0.2183(8) -0.4368(10) 0.0209(6) 0.061(4) Uani 1 d . . H54 H -0.2355(8) -0.3740(10) 0.0035(6) 0.074 Uiso 1 calc R . C55 C -0.1788(7) -0.4412(9) 0.0850(7) 0.054(3) Uani 1 d . . H55 H -0.1707(7) -0.3820(9) 0.1111(7) 0.065 Uiso 1 calc R . C56 C -0.1513(6) -0.5353(8) 0.1096(6) 0.043(3) Uani 1 d . . H56 H -0.1234(6) -0.5384(8) 0.1518(6) 0.051 Uiso 1 calc R . C61 C -0.1976(5) -0.7949(9) 0.1576(5) 0.036(3) Uani 1 d . . C66 C -0.2489(7) -0.7268(10) 0.1841(6) 0.053(3) Uani 1 d . . H66 H -0.2440(7) -0.6566(10) 0.1778(6) 0.064 Uiso 1 calc R . C62 C -0.2065(7) -0.8971(10) 0.1679(6) 0.051(3) Uani 1 d . . H62 H -0.1728(7) -0.9431(10) 0.1511(6) 0.062 Uiso 1 calc R . C63 C -0.2651(7) -0.9342(10) 0.2030(7) 0.059(4) Uani 1 d . . H63 H -0.2700(7) -1.0043(10) 0.2099(7) 0.071 Uiso 1 calc R . C64 C -0.3147(8) -0.8686(13) 0.2272(7) 0.067(4) Uani 1 d . . H64 H -0.3549(8) -0.8937(13) 0.2493(7) 0.080 Uiso 1 calc R . C65 C -0.3059(7) -0.7638(12) 0.2192(7) 0.066(4) Uani 1 d . . H65 H -0.3389(7) -0.7186(12) 0.2377(7) 0.079 Uiso 1 calc R . Cl1 Cl -0.08997(14) -0.6287(2) 0.27943(14) 0.0419(7) Uani 1 d . . Cl2 Cl -0.0140(2) -0.9152(2) 0.17230(14) 0.0417(6) Uani 1 d . . Cl4 Cl -0.3789(3) -0.2498(5) -0.0067(4) 0.130 Uani 1 d . . Cl3 Cl -0.2530(4) -0.1489(4) 0.0627(3) 0.134 Uani 1 d . . C5 C -0.3366(14) -0.2124(15) 0.0665(11) 0.148 Uani 1 d . . H5A H -0.3276(14) -0.2723(15) 0.0953(11) 0.177 Uiso 1 calc R . H5B H -0.3704(14) -0.1680(15) 0.0888(11) 0.177 Uiso 1 calc R . C6 C 0.0086(32) 0.1450(36) -0.2585(28) 0.165 Uani 0.50 d P . H6A H 0.0033(32) 0.0787(36) -0.2371(28) 0.199 Uiso 0.50 calc PR . H6B H 0.0478(32) 0.1406(36) -0.2897(28) 0.199 Uiso 0.50 calc PR . Cl6 Cl -0.0776(6) 0.1845(8) -0.3026(6) 0.114 Uani 0.50 d P . Cl5 Cl 0.0295(6) 0.2403(8) -0.1967(5) 0.109 Uani 0.50 d P . 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 0.0295(4) 0.0281(4) 0.0264(4) 0.0021(3) 0.0000(3) 0.0010(3) Rh2 0.0287(4) 0.0317(5) 0.0279(4) -0.0012(3) 0.0002(3) 0.0017(3) O1 0.043(4) 0.038(4) 0.034(4) 0.003(3) -0.004(3) -0.001(3) O2 0.039(4) 0.043(4) 0.029(4) 0.000(3) 0.003(3) -0.006(3) O3 0.031(4) 0.055(5) 0.042(4) -0.006(4) -0.002(3) 0.004(4) O4 0.026(4) 0.045(4) 0.037(4) 0.000(4) 0.005(3) -0.005(3) O5 0.059(5) 0.031(4) 0.038(4) -0.004(3) -0.001(3) 0.001(4) O6 0.037(4) 0.062(5) 0.040(4) -0.012(4) 0.007(3) 0.001(4) P1 0.0309(14) 0.0309(14) 0.0303(14) 0.0052(11) 0.0007(11) 0.0007(11) P2 0.0300(14) 0.0318(14) 0.0331(14) -0.0004(12) 0.0013(11) 0.0019(12) C1 0.024(5) 0.032(6) 0.043(7) 0.005(5) -0.006(4) -0.001(4) C2 0.066(8) 0.046(7) 0.045(7) 0.012(6) -0.006(6) -0.009(6) C3 0.032(6) 0.038(6) 0.034(6) 0.009(5) 0.005(5) 0.004(5) C4 0.044(7) 0.063(8) 0.046(7) 0.000(6) 0.007(5) 0.006(6) C10 0.103(12) 0.052(8) 0.049(8) 0.003(7) 0.010(7) 0.002(8) C11 0.030(5) 0.039(6) 0.028(5) -0.004(5) 0.000(4) 0.001(5) C12 0.038(6) 0.051(7) 0.034(6) -0.006(5) 0.001(5) 0.007(5) C13 0.046(7) 0.049(7) 0.039(7) -0.013(6) 0.002(5) 0.003(6) C14 0.051(7) 0.075(10) 0.037(7) -0.019(7) 0.003(5) 0.009(7) C15 0.059(8) 0.070(9) 0.039(7) 0.001(7) -0.007(6) 0.015(7) C16 0.059(7) 0.045(7) 0.027(6) 0.007(5) 0.002(5) -0.002(6) C21 0.038(6) 0.038(6) 0.029(5) 0.007(5) -0.005(4) 0.012(5) C22 0.035(6) 0.042(6) 0.044(6) 0.008(5) -0.004(5) 0.002(5) C23 0.042(7) 0.070(9) 0.047(7) 0.002(7) -0.010(5) 0.003(6) C24 0.052(8) 0.076(10) 0.042(7) 0.010(7) 0.007(6) 0.030(7) C25 0.060(9) 0.059(8) 0.061(8) -0.002(7) -0.007(7) 0.025(7) C26 0.046(7) 0.049(7) 0.056(7) 0.002(6) -0.006(6) 0.009(6) C31 0.039(6) 0.034(6) 0.034(6) 0.010(5) 0.005(5) 0.001(5) C32 0.053(7) 0.051(8) 0.059(8) 0.017(6) -0.004(6) -0.003(6) C33 0.074(10) 0.055(8) 0.075(10) 0.029(7) -0.010(8) -0.022(7) C34 0.076(10) 0.049(8) 0.081(10) 0.005(8) 0.008(8) -0.023(7) C35 0.037(7) 0.066(9) 0.068(8) -0.003(7) 0.013(6) -0.013(6) C36 0.038(6) 0.045(7) 0.037(6) 0.001(5) 0.008(5) -0.004(5) C40 0.042(7) 0.079(9) 0.043(7) 0.008(7) 0.018(5) 0.000(6) C41 0.038(6) 0.037(6) 0.032(6) -0.002(5) -0.002(5) 0.007(5) C42 0.035(6) 0.041(6) 0.035(6) 0.005(5) -0.010(5) 0.001(5) C43 0.061(8) 0.052(7) 0.033(6) -0.014(6) -0.004(5) 0.016(6) C44 0.080(10) 0.048(8) 0.040(7) -0.017(6) -0.018(7) 0.007(7) C45 0.054(8) 0.049(7) 0.054(8) -0.009(6) -0.013(6) -0.015(6) C46 0.044(7) 0.045(7) 0.049(7) 0.000(6) -0.008(5) 0.004(6) C51 0.029(5) 0.042(6) 0.035(6) 0.002(5) 0.002(4) 0.005(5) C52 0.062(8) 0.049(7) 0.039(6) -0.001(6) -0.006(6) 0.006(6) C53 0.063(8) 0.072(10) 0.045(7) 0.011(7) -0.012(6) 0.027(7) C54 0.089(10) 0.044(8) 0.051(8) 0.008(6) 0.008(7) 0.025(7) C55 0.056(8) 0.041(7) 0.065(8) -0.010(6) 0.001(6) 0.001(6) C56 0.042(6) 0.043(7) 0.040(6) 0.005(5) -0.007(5) 0.010(5) C61 0.025(5) 0.048(7) 0.035(6) 0.011(5) -0.009(4) -0.012(5) C66 0.048(7) 0.055(8) 0.057(8) -0.001(6) 0.010(6) -0.003(6) C62 0.045(7) 0.051(8) 0.058(8) 0.014(6) 0.001(6) -0.013(6) C63 0.061(8) 0.053(8) 0.062(8) 0.017(7) -0.007(7) -0.023(7) C64 0.055(8) 0.092(12) 0.054(8) 0.007(8) 0.012(7) -0.023(8) C65 0.049(8) 0.095(12) 0.058(8) -0.002(8) 0.025(6) -0.001(8) Cl1 0.0357(14) 0.043(2) 0.047(2) 0.0053(13) 0.0085(12) 0.0092(12) Cl2 0.050(2) 0.0316(14) 0.043(2) 0.0018(12) 0.0027(12) 0.0036(12) Cl4 0.116 0.116 0.156 0.015 0.008 0.012 Cl3 0.150 0.104 0.152 0.000 0.030 0.000 C5 0.234 0.079 0.152 0.000 0.151 0.000 C6 0.207 0.094 0.192 0.000 0.000 0.018 Cl6 0.107 0.103 0.131 0.000 0.007 0.003 Cl5 0.110 0.120 0.100 0.000 0.017 0.000 _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 O4 2.061(6) . ? Rh1 O1 2.111(7) . ? Rh1 P1 2.234(3) . ? Rh1 Cl1 2.322(3) . ? Rh1 O5 2.342(7) . ? Rh1 Rh2 2.5605(11) . ? Rh2 O2 2.058(7) . ? Rh2 O3 2.094(7) . ? Rh2 P2 2.247(3) . ? Rh2 O6 2.298(7) . ? Rh2 Cl2 2.318(3) . ? O1 C1 1.261(12) . ? O2 C1 1.253(12) . ? O3 C3 1.246(13) . ? O4 C3 1.262(12) . ? O5 C12 1.387(13) . ? O5 C10 1.434(14) . ? O6 C42 1.385(12) . ? O6 C40 1.439(12) . ? P1 C31 1.819(10) . ? P1 C21 1.827(10) . ? P1 C11 1.840(10) . ? P2 C41 1.824(10) . ? P2 C61 1.834(10) . ? P2 C51 1.834(11) . ? C1 C2 1.518(14) . ? C3 C4 1.494(14) . ? C11 C12 1.39(2) . ? C11 C16 1.398(14) . ? C12 C13 1.384(15) . ? C13 C14 1.40(2) . ? C14 C15 1.35(2) . ? C15 C16 1.38(2) . ? C21 C26 1.38(2) . ? C21 C22 1.384(15) . ? C22 C23 1.40(2) . ? C23 C24 1.36(2) . ? C24 C25 1.40(2) . ? C25 C26 1.42(2) . ? C31 C36 1.398(14) . ? C31 C32 1.403(15) . ? C32 C33 1.39(2) . ? C33 C34 1.37(2) . ? C34 C35 1.38(2) . ? C35 C36 1.37(2) . ? C41 C42 1.390(15) . ? C41 C46 1.41(2) . ? C42 C43 1.388(15) . ? C43 C44 1.39(2) . ? C44 C45 1.36(2) . ? C45 C46 1.38(2) . ? C51 C56 1.379(15) . ? C51 C52 1.388(15) . ? C52 C53 1.40(2) . ? C53 C54 1.34(2) . ? C54 C55 1.39(2) . ? C55 C56 1.39(2) . ? C61 C62 1.36(2) . ? C61 C66 1.41(2) . ? C66 C65 1.37(2) . ? C62 C63 1.39(2) . ? C63 C64 1.35(2) . ? C64 C65 1.39(2) . ? Cl4 C5 1.64(3) . ? Cl3 C5 1.72(2) . ? C6 Cl5 1.75(5) . ? C6 Cl6 1.78(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 O4 Rh1 O1 84.3(3) . . ? O4 Rh1 P1 90.6(2) . . ? O1 Rh1 P1 167.9(2) . . ? O4 Rh1 Cl1 171.6(2) . . ? O1 Rh1 Cl1 89.9(2) . . ? P1 Rh1 Cl1 93.83(10) . . ? O4 Rh1 O5 87.6(3) . . ? O1 Rh1 O5 88.2(3) . . ? P1 Rh1 O5 80.6(2) . . ? Cl1 Rh1 O5 86.2(2) . . ? O4 Rh1 Rh2 85.0(2) . . ? O1 Rh1 Rh2 85.0(2) . . ? P1 Rh1 Rh2 105.59(8) . . ? Cl1 Rh1 Rh2 100.64(8) . . ? O5 Rh1 Rh2 170.3(2) . . ? O2 Rh2 O3 85.7(3) . . ? O2 Rh2 P2 94.5(2) . . ? O3 Rh2 P2 166.7(2) . . ? O2 Rh2 O6 83.5(3) . . ? O3 Rh2 O6 86.8(3) . . ? P2 Rh2 O6 80.0(2) . . ? O2 Rh2 Cl2 172.8(2) . . ? O3 Rh2 Cl2 89.9(2) . . ? P2 Rh2 Cl2 88.55(10) . . ? O6 Rh2 Cl2 90.7(2) . . ? O2 Rh2 Rh1 84.7(2) . . ? O3 Rh2 Rh1 83.9(2) . . ? P2 Rh2 Rh1 109.32(7) . . ? O6 Rh2 Rh1 165.5(2) . . ? Cl2 Rh2 Rh1 100.42(7) . . ? C1 O1 Rh1 118.3(6) . . ? C1 O2 Rh2 122.2(6) . . ? C3 O3 Rh2 120.5(7) . . ? C3 O4 Rh1 121.3(6) . . ? C12 O5 C10 118.4(9) . . ? C12 O5 Rh1 116.4(6) . . ? C10 O5 Rh1 119.9(7) . . ? C42 O6 C40 120.5(9) . . ? C42 O6 Rh2 116.2(6) . . ? C40 O6 Rh2 122.0(7) . . ? C31 P1 C21 105.2(5) . . ? C31 P1 C11 103.3(5) . . ? C21 P1 C11 103.2(5) . . ? C31 P1 Rh1 126.9(3) . . ? C21 P1 Rh1 112.6(3) . . ? C11 P1 Rh1 102.8(3) . . ? C41 P2 C61 102.4(5) . . ? C41 P2 C51 104.2(5) . . ? C61 P2 C51 103.3(5) . . ? C41 P2 Rh2 101.4(3) . . ? C61 P2 Rh2 126.2(3) . . ? C51 P2 Rh2 116.3(3) . . ? O2 C1 O1 125.9(9) . . ? O2 C1 C2 116.8(9) . . ? O1 C1 C2 117.3(9) . . ? O3 C3 O4 124.7(9) . . ? O3 C3 C4 117.9(10) . . ? O4 C3 C4 117.5(10) . . ? C12 C11 C16 116.8(10) . . ? C12 C11 P1 120.4(8) . . ? C16 C11 P1 122.7(8) . . ? C13 C12 C11 121.8(11) . . ? C13 C12 O5 121.5(10) . . ? C11 C12 O5 116.7(9) . . ? C12 C13 C14 119.2(11) . . ? C15 C14 C13 120.4(11) . . ? C14 C15 C16 119.9(12) . . ? C15 C16 C11 121.9(11) . . ? C26 C21 C22 119.6(10) . . ? C26 C21 P1 120.0(8) . . ? C22 C21 P1 120.2(8) . . ? C21 C22 C23 121.4(11) . . ? C24 C23 C22 119.4(12) . . ? C23 C24 C25 120.3(12) . . ? C24 C25 C26 119.8(12) . . ? C21 C26 C25 119.4(12) . . ? C36 C31 C32 117.4(10) . . ? C36 C31 P1 121.1(8) . . ? C32 C31 P1 121.4(8) . . ? C33 C32 C31 121.5(12) . . ? C34 C33 C32 118.6(12) . . ? C33 C34 C35 121.9(12) . . ? C36 C35 C34 119.0(12) . . ? C35 C36 C31 121.6(11) . . ? C42 C41 C46 116.7(10) . . ? C42 C41 P2 119.8(8) . . ? C46 C41 P2 123.5(8) . . ? O6 C42 C43 120.7(10) . . ? O6 C42 C41 115.9(9) . . ? C43 C42 C41 123.4(10) . . ? C42 C43 C44 116.8(11) . . ? C45 C44 C43 122.4(11) . . ? C44 C45 C46 119.6(11) . . ? C45 C46 C41 121.1(11) . . ? C56 C51 C52 118.5(10) . . ? C56 C51 P2 119.9(8) . . ? C52 C51 P2 121.6(9) . . ? C51 C52 C53 120.3(12) . . ? C54 C53 C52 120.5(11) . . ? C53 C54 C55 120.5(12) . . ? C56 C55 C54 119.1(11) . . ? C51 C56 C55 121.0(10) . . ? C62 C61 C66 118.4(11) . . ? C62 C61 P2 121.3(9) . . ? C66 C61 P2 120.1(9) . . ? C65 C66 C61 120.2(12) . . ? C61 C62 C63 121.1(13) . . ? C64 C63 C62 120.1(13) . . ? C63 C64 C65 120.0(12) . . ? C66 C65 C64 120.2(13) . . ? Cl4 C5 Cl3 116.5(10) . . ? Cl5 C6 Cl6 104.8(25) . . ? _refine_diff_density_max 1.235 _refine_diff_density_min -3.341 _refine_diff_density_rms 0.158