Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Paolo Pelagatti' 'Alessia Bacchi' 'Carla Bobbio' 'Mauro Carcelli' 'Mirco Costa' 'Andrea Fochi' 'Corrado Pelizzi' _publ_contact_author_name 'Dr Paolo Pelagatti' _publ_contact_author_address ; Dr Paolo Pelagatti Dipartimento di Chimica Generale ed Inorganica Universita degli Studi di Parma Parco Area delle Scienze 17/A Parma 43100 ITALY ; _publ_contact_author_email 'PAOLO.PELAGATTI@UNIPR.IT' _publ_section_title ; Reactivity of Rh(I) and Rh(III) complexes containing a PNO hydrazonic ligand toward HCl ; data_Compound-6 _database_code_CSD 174285 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Cl2 N2 O4 P Rh S3' _chemical_formula_weight 815.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.939(5) _cell_length_b 12.862(5) _cell_length_c 20.133(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.10(5) _cell_angle_gamma 90.00 _cell_volume 3607(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 32 _exptl_crystal_description 'irregular prisms' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 7.545 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 diffractometer' _diffrn_measurement_method '\w/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6996 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 70.02 _reflns_number_total 6806 _reflns_number_gt 4396 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6806 _refine_ls_number_parameters 444 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1728 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.936 _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 Rh Rh 0.06921(3) 0.11459(3) 0.33824(2) 0.04715(17) Uani 1 1 d . . . Cl1 Cl 0.05746(10) -0.06857(12) 0.34678(7) 0.0584(4) Uani 1 1 d . . . Cl2 Cl 0.10626(12) 0.10941(13) 0.22501(7) 0.0641(4) Uani 1 1 d . . . S1 S 0.06887(10) 0.29266(11) 0.34025(7) 0.0533(4) Uani 1 1 d . . . O2 O 0.1134(4) 0.3356(4) 0.4008(2) 0.0696(12) Uani 1 1 d . . . C27 C -0.0512(5) 0.3390(5) 0.3310(4) 0.0730(19) Uani 1 1 d . . . H27A H -0.0865 0.3188 0.3690 0.109 Uiso 1 1 calc R . . H27B H -0.0811 0.3098 0.2916 0.109 Uiso 1 1 calc R . . H27C H -0.0508 0.4135 0.3275 0.109 Uiso 1 1 calc R . . C28 C 0.1206(6) 0.3520(6) 0.2696(3) 0.0715(18) Uani 1 1 d . . . H28A H 0.1148 0.4262 0.2728 0.107 Uiso 1 1 calc R . . H28B H 0.0876 0.3282 0.2298 0.107 Uiso 1 1 calc R . . H28C H 0.1872 0.3334 0.2683 0.107 Uiso 1 1 calc R . . P1 P 0.22521(11) 0.10468(12) 0.37293(7) 0.0499(4) Uani 1 1 d . . . O1 O -0.0771(3) 0.1138(3) 0.31365(19) 0.0520(9) Uani 1 1 d . . . N1 N 0.0167(3) 0.1151(3) 0.4293(2) 0.0444(10) Uani 1 1 d . . . N2 N -0.0831(3) 0.1105(4) 0.4291(3) 0.0517(11) Uani 1 1 d . . . C1 C 0.2380(4) 0.1266(4) 0.4618(3) 0.0518(13) Uani 1 1 d . . . C2 C 0.3310(5) 0.1417(6) 0.4899(3) 0.0656(17) Uani 1 1 d . . . H2 H 0.3829 0.1427 0.4622 0.079 Uiso 1 1 calc R . . C3 C 0.3474(5) 0.1551(6) 0.5574(4) 0.0721(18) Uani 1 1 d . . . H3 H 0.4096 0.1647 0.5746 0.086 Uiso 1 1 calc R . . C4 C 0.2713(5) 0.1541(6) 0.5991(3) 0.0694(18) Uani 1 1 d . . . H4 H 0.2818 0.1626 0.6446 0.083 Uiso 1 1 calc R . . C5 C 0.1798(5) 0.1406(5) 0.5732(3) 0.0611(16) Uani 1 1 d . . . H5 H 0.1287 0.1409 0.6016 0.073 Uiso 1 1 calc R . . C6 C 0.1613(4) 0.1263(4) 0.5047(3) 0.0500(13) Uani 1 1 d . . . C7 C 0.0582(4) 0.1162(4) 0.4863(3) 0.0493(12) Uani 1 1 d . . . H7 H 0.0178 0.1097 0.5218 0.059 Uiso 1 1 calc R . . C8 C -0.1234(4) 0.1111(4) 0.3695(3) 0.0480(12) Uani 1 1 d . . . C9 C -0.2296(4) 0.1099(4) 0.3637(3) 0.0544(14) Uani 1 1 d . . . C10 C -0.2836(5) 0.1332(6) 0.4180(4) 0.076(2) Uani 1 1 d . . . H10 H -0.2532 0.1519 0.4581 0.091 Uiso 1 1 calc R . . C11 C -0.3819(6) 0.1287(8) 0.4128(5) 0.092(3) Uani 1 1 d . . . H11 H -0.4178 0.1427 0.4498 0.110 Uiso 1 1 calc R . . C12 C -0.4276(5) 0.1040(7) 0.3537(5) 0.085(3) Uani 1 1 d . . . H12 H -0.4942 0.1000 0.3507 0.102 Uiso 1 1 calc R . . C13 C -0.3748(5) 0.0850(6) 0.2985(4) 0.0710(19) Uani 1 1 d . . . H13 H -0.4061 0.0710 0.2579 0.085 Uiso 1 1 calc R . . C14 C -0.2748(5) 0.0867(5) 0.3031(4) 0.0641(16) Uani 1 1 d . . . H14 H -0.2390 0.0724 0.2661 0.077 Uiso 1 1 calc R . . C15 C 0.2824(4) -0.0217(5) 0.3587(4) 0.0598(15) Uani 1 1 d . . . C16 C 0.3296(5) -0.0761(6) 0.4095(4) 0.0716(18) Uani 1 1 d . . . H16 H 0.3330 -0.0487 0.4522 0.086 Uiso 1 1 calc R . . C17 C 0.3722(6) -0.1721(6) 0.3967(5) 0.087(2) Uani 1 1 d . . . H17 H 0.4053 -0.2069 0.4309 0.104 Uiso 1 1 calc R . . C18 C 0.3660(6) -0.2160(6) 0.3343(5) 0.085(2) Uani 1 1 d . . . H18 H 0.3945 -0.2800 0.3265 0.102 Uiso 1 1 calc R . . C19 C 0.3173(6) -0.1644(7) 0.2840(5) 0.086(2) Uani 1 1 d . . . H19 H 0.3126 -0.1936 0.2417 0.103 Uiso 1 1 calc R . . C20 C 0.2748(5) -0.0682(6) 0.2958(4) 0.0725(18) Uani 1 1 d . . . H20 H 0.2409 -0.0346 0.2614 0.087 Uiso 1 1 calc R . . C21 C 0.3066(4) 0.1981(5) 0.3361(3) 0.0563(14) Uani 1 1 d . . . C22 C 0.3291(5) 0.2916(6) 0.3667(4) 0.0702(18) Uani 1 1 d . . . H22 H 0.3033 0.3078 0.4073 0.084 Uiso 1 1 calc R . . C23 C 0.3901(6) 0.3613(6) 0.3370(5) 0.087(3) Uani 1 1 d . . . H23 H 0.4050 0.4242 0.3577 0.104 Uiso 1 1 calc R . . C24 C 0.4288(6) 0.3373(7) 0.2764(5) 0.089(3) Uani 1 1 d . . . H24 H 0.4705 0.3834 0.2567 0.107 Uiso 1 1 calc R . . C25 C 0.4058(5) 0.2472(7) 0.2463(4) 0.078(2) Uani 1 1 d . . . H25 H 0.4314 0.2319 0.2054 0.094 Uiso 1 1 calc R . . C26 C 0.3455(5) 0.1773(6) 0.2745(3) 0.0653(17) Uani 1 1 d . . . H26 H 0.3303 0.1156 0.2526 0.078 Uiso 1 1 calc R . . S2 S 0.8942(3) 0.1832(2) 0.04882(16) 0.1373(12) Uani 1 1 d D . . O3 O 0.8392(7) 0.1351(7) -0.0082(5) 0.158(3) Uani 1 1 d D . . C29 C 1.0018(9) 0.1234(12) 0.0548(6) 0.170(6) Uani 1 1 d D . . H29A H 0.9927 0.0494 0.0537 0.255 Uiso 1 1 calc R . . H29B H 1.0341 0.1426 0.0959 0.255 Uiso 1 1 calc R . . H29C H 1.0398 0.1442 0.0183 0.255 Uiso 1 1 calc R . . C30 C 0.8532(9) 0.1316(11) 0.1205(6) 0.165(6) Uani 1 1 d D . . H30A H 0.7854 0.1435 0.1224 0.248 Uiso 1 1 calc R . . H30B H 0.8855 0.1641 0.1579 0.248 Uiso 1 1 calc R . . H30C H 0.8656 0.0582 0.1214 0.248 Uiso 1 1 calc R . . S3 S 0.3808(5) 0.4579(6) 0.5608(5) 0.189(3) Uani 0.70 1 d PDU A 1 O4 O 0.4580(14) 0.4239(16) 0.6069(15) 0.193(9) Uani 0.70 1 d PDU A 1 C31 C 0.395(2) 0.5830(14) 0.5436(18) 0.223(15) Uani 0.70 1 d PDU A 1 H31A H 0.4553 0.5934 0.5237 0.334 Uiso 0.70 1 calc PR A 1 H31B H 0.3924 0.6227 0.5839 0.334 Uiso 0.70 1 calc PR A 1 H31C H 0.3438 0.6052 0.5133 0.334 Uiso 0.70 1 calc PR A 1 C32 C 0.2702(14) 0.414(2) 0.555(2) 0.253(16) Uani 0.70 1 d PDU A 1 H32A H 0.2707 0.3430 0.5392 0.379 Uiso 0.70 1 calc PR A 1 H32B H 0.2331 0.4557 0.5239 0.379 Uiso 0.70 1 calc PR A 1 H32C H 0.2421 0.4163 0.5975 0.379 Uiso 0.70 1 calc PR A 1 S31 S 0.3571(11) 0.5008(11) 0.6142(5) 0.137(4) Uani 0.30 1 d PDU B 2 C321 C 0.437(5) 0.403(5) 0.614(4) 0.173(18) Uani 0.30 1 d PDU B 2 H32D H 0.4387 0.3697 0.6568 0.259 Uiso 0.30 1 calc PR B 2 H32E H 0.4991 0.4304 0.6052 0.259 Uiso 0.30 1 calc PR B 2 H32F H 0.4179 0.3539 0.5804 0.259 Uiso 0.30 1 calc PR B 2 C311 C 0.358(4) 0.611(2) 0.571(3) 0.167(19) Uani 0.30 1 d PDU B 2 H31D H 0.2935 0.6371 0.5658 0.251 Uiso 0.30 1 calc PR B 2 H31E H 0.3826 0.5975 0.5278 0.251 Uiso 0.30 1 calc PR B 2 H31F H 0.3976 0.6610 0.5938 0.251 Uiso 0.30 1 calc PR B 2 O41 O 0.2686(18) 0.454(3) 0.5940(15) 0.139(10) Uani 0.30 1 d PDU B 2 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 Rh 0.0463(3) 0.0487(2) 0.0465(3) -0.00069(18) 0.00185(17) -0.00229(18) Cl1 0.0609(8) 0.0475(8) 0.0672(9) -0.0082(7) 0.0045(7) -0.0047(6) Cl2 0.0697(10) 0.0749(10) 0.0477(8) -0.0022(7) 0.0043(6) -0.0014(7) S1 0.0575(9) 0.0463(8) 0.0560(8) 0.0051(6) 0.0023(6) -0.0021(6) O2 0.091(3) 0.054(3) 0.064(3) -0.003(2) -0.001(2) -0.009(2) C27 0.070(4) 0.051(4) 0.098(5) 0.014(4) 0.006(4) 0.013(3) C28 0.087(5) 0.063(4) 0.065(4) 0.018(3) 0.006(3) -0.007(4) P1 0.0473(8) 0.0539(9) 0.0484(8) -0.0005(6) 0.0022(6) -0.0018(6) O1 0.042(2) 0.064(3) 0.049(2) 0.0032(18) -0.0048(16) -0.0023(17) N1 0.048(2) 0.034(2) 0.052(3) -0.0014(19) 0.0069(19) -0.0002(18) N2 0.043(2) 0.053(3) 0.059(3) 0.000(2) 0.004(2) -0.003(2) C1 0.055(3) 0.046(3) 0.054(3) -0.002(2) -0.002(2) -0.007(2) C2 0.057(4) 0.079(5) 0.061(4) 0.004(3) 0.004(3) -0.007(3) C3 0.059(4) 0.087(5) 0.069(4) 0.006(4) -0.013(3) -0.005(4) C4 0.081(5) 0.069(4) 0.057(4) 0.005(3) -0.011(3) -0.014(4) C5 0.064(4) 0.063(4) 0.057(4) 0.004(3) 0.003(3) -0.005(3) C6 0.060(3) 0.038(3) 0.051(3) 0.002(2) -0.001(2) -0.002(2) C7 0.055(3) 0.041(3) 0.052(3) 0.004(2) 0.006(2) -0.001(2) C8 0.052(3) 0.038(3) 0.054(3) 0.004(2) 0.003(2) 0.002(2) C9 0.054(3) 0.044(3) 0.066(4) 0.004(3) 0.005(3) 0.004(2) C10 0.055(4) 0.106(6) 0.066(4) 0.008(4) 0.009(3) 0.011(4) C11 0.056(4) 0.134(8) 0.085(6) 0.013(5) 0.006(4) 0.011(4) C12 0.043(4) 0.103(6) 0.110(6) 0.030(5) 0.002(4) 0.000(4) C13 0.059(4) 0.070(5) 0.083(5) 0.010(4) -0.007(3) 0.000(3) C14 0.063(4) 0.057(4) 0.073(4) -0.002(3) 0.000(3) 0.002(3) C15 0.047(3) 0.056(4) 0.076(4) 0.004(3) 0.011(3) 0.003(3) C16 0.065(4) 0.065(4) 0.085(5) 0.005(4) 0.002(4) 0.004(3) C17 0.074(5) 0.070(5) 0.116(7) 0.020(5) 0.003(4) 0.014(4) C18 0.069(5) 0.072(5) 0.115(7) -0.008(5) 0.029(5) 0.009(4) C19 0.095(6) 0.071(5) 0.093(6) -0.017(4) 0.026(5) 0.004(4) C20 0.070(4) 0.076(5) 0.072(4) -0.006(4) 0.009(3) -0.003(4) C21 0.048(3) 0.058(4) 0.063(4) 0.006(3) 0.004(3) -0.004(3) C22 0.063(4) 0.068(5) 0.079(5) 0.008(4) 0.003(3) -0.001(3) C23 0.068(5) 0.067(5) 0.124(7) 0.017(5) -0.005(5) -0.017(4) C24 0.068(5) 0.080(6) 0.121(7) 0.045(5) 0.023(5) 0.004(4) C25 0.065(4) 0.095(6) 0.075(5) 0.030(4) 0.013(4) 0.011(4) C26 0.056(4) 0.074(5) 0.066(4) 0.017(3) 0.000(3) 0.001(3) S2 0.220(4) 0.0760(17) 0.113(2) 0.0145(15) -0.029(2) -0.0111(19) O3 0.189(9) 0.144(7) 0.138(7) 0.013(5) -0.054(7) -0.013(6) C29 0.157(13) 0.262(19) 0.090(8) 0.048(9) -0.011(8) 0.017(11) C30 0.135(11) 0.225(17) 0.137(11) 0.042(10) 0.040(9) 0.066(10) S3 0.146(5) 0.153(5) 0.269(8) 0.081(6) 0.016(5) 0.011(4) O4 0.150(12) 0.118(11) 0.31(2) 0.085(13) -0.025(12) -0.016(10) C31 0.14(2) 0.168(15) 0.36(4) 0.13(2) 0.03(2) 0.029(13) C32 0.168(15) 0.18(2) 0.41(4) 0.01(3) -0.06(2) -0.005(16) S31 0.178(11) 0.149(9) 0.086(6) -0.006(6) 0.018(7) -0.025(8) C321 0.17(3) 0.14(3) 0.20(3) 0.10(3) -0.04(3) -0.03(2) C311 0.14(4) 0.065(17) 0.29(4) -0.010(19) -0.04(4) -0.025(17) O41 0.144(15) 0.12(2) 0.16(2) 0.024(17) 0.072(15) -0.018(13) _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 Rh N1 1.998(5) . ? Rh O1 2.081(4) . ? Rh P1 2.2630(18) . ? Rh S1 2.2906(18) . ? Rh Cl2 2.3567(17) . ? Rh Cl1 2.3683(18) . ? S1 O2 1.457(5) . ? S1 C27 1.781(7) . ? S1 C28 1.789(7) . ? P1 C1 1.814(6) . ? P1 C21 1.828(6) . ? P1 C15 1.837(7) . ? O1 C8 1.316(7) . ? N1 C7 1.267(7) . ? N1 N2 1.392(6) . ? N2 C8 1.306(7) . ? C1 C6 1.398(8) . ? C1 C2 1.408(9) . ? C2 C3 1.380(9) . ? C3 C4 1.377(10) . ? C4 C5 1.371(9) . ? C5 C6 1.405(8) . ? C6 C7 1.477(8) . ? C8 C9 1.480(8) . ? C9 C10 1.383(9) . ? C9 C14 1.384(9) . ? C10 C11 1.372(10) . ? C11 C12 1.366(12) . ? C12 C13 1.375(11) . ? C13 C14 1.394(9) . ? C15 C16 1.385(10) . ? C15 C20 1.401(9) . ? C16 C17 1.398(11) . ? C17 C18 1.376(12) . ? C18 C19 1.371(12) . ? C19 C20 1.396(11) . ? C21 C22 1.382(9) . ? C21 C26 1.397(9) . ? C22 C23 1.386(10) . ? C23 C24 1.387(13) . ? C24 C25 1.340(12) . ? C25 C26 1.369(10) . ? S2 O3 1.491(8) . ? S2 C29 1.686(11) . ? S2 C30 1.705(11) . ? S3 O4 1.462(18) . ? S3 C32 1.644(16) . ? S3 C31 1.658(15) . ? S31 O41 1.418(18) . ? S31 C311 1.662(17) . ? S31 C321 1.674(18) . ? 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 N1 Rh O1 80.18(18) . . ? N1 Rh P1 95.57(14) . . ? O1 Rh P1 174.49(11) . . ? N1 Rh S1 88.82(13) . . ? O1 Rh S1 90.36(12) . . ? P1 Rh S1 93.07(6) . . ? N1 Rh Cl2 171.07(14) . . ? O1 Rh Cl2 91.00(13) . . ? P1 Rh Cl2 93.15(7) . . ? S1 Rh Cl2 92.64(6) . . ? N1 Rh Cl1 84.73(13) . . ? O1 Rh Cl1 86.71(12) . . ? P1 Rh Cl1 89.41(5) . . ? S1 Rh Cl1 173.28(6) . . ? Cl2 Rh Cl1 93.46(6) . . ? O2 S1 C27 109.3(3) . . ? O2 S1 C28 109.4(3) . . ? C27 S1 C28 100.3(4) . . ? O2 S1 Rh 113.1(2) . . ? C27 S1 Rh 109.6(2) . . ? C28 S1 Rh 114.3(3) . . ? C1 P1 C21 105.0(3) . . ? C1 P1 C15 105.3(3) . . ? C21 P1 C15 103.8(3) . . ? C1 P1 Rh 110.8(2) . . ? C21 P1 Rh 116.2(2) . . ? C15 P1 Rh 114.8(2) . . ? C8 O1 Rh 107.7(3) . . ? C7 N1 N2 115.2(5) . . ? C7 N1 Rh 131.4(4) . . ? N2 N1 Rh 113.4(3) . . ? C8 N2 N1 113.5(5) . . ? C6 C1 C2 117.8(6) . . ? C6 C1 P1 123.9(4) . . ? C2 C1 P1 118.3(5) . . ? C3 C2 C1 122.0(6) . . ? C4 C3 C2 119.7(6) . . ? C5 C4 C3 119.8(6) . . ? C4 C5 C6 121.6(6) . . ? C1 C6 C5 119.2(6) . . ? C1 C6 C7 127.2(5) . . ? C5 C6 C7 113.5(5) . . ? N1 C7 C6 129.5(5) . . ? N2 C8 O1 125.2(5) . . ? N2 C8 C9 117.9(5) . . ? O1 C8 C9 116.9(5) . . ? C10 C9 C14 120.0(6) . . ? C10 C9 C8 120.5(6) . . ? C14 C9 C8 119.6(6) . . ? C11 C10 C9 120.1(8) . . ? C12 C11 C10 120.6(8) . . ? C11 C12 C13 119.9(7) . . ? C12 C13 C14 120.4(7) . . ? C9 C14 C13 118.9(7) . . ? C16 C15 C20 118.0(7) . . ? C16 C15 P1 121.9(6) . . ? C20 C15 P1 120.0(5) . . ? C15 C16 C17 120.3(8) . . ? C18 C17 C16 121.2(8) . . ? C19 C18 C17 119.3(8) . . ? C18 C19 C20 120.3(8) . . ? C19 C20 C15 121.0(7) . . ? C22 C21 C26 118.2(6) . . ? C22 C21 P1 121.7(5) . . ? C26 C21 P1 120.1(5) . . ? C21 C22 C23 120.3(8) . . ? C22 C23 C24 119.9(8) . . ? C25 C24 C23 119.7(7) . . ? C24 C25 C26 121.4(8) . . ? C25 C26 C21 120.5(7) . . ? O3 S2 C29 107.3(7) . . ? O3 S2 C30 108.2(7) . . ? C29 S2 C30 95.0(6) . . ? O4 S3 C32 127.6(17) . . ? O4 S3 C31 109.6(16) . . ? C32 S3 C31 115.8(16) . . ? O41 S31 C311 103(2) . . ? O41 S31 C321 105(4) . . ? C311 S31 C321 128(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 70.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.830 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.114 #===END data_Compound-8 _database_code_CSD 174286 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H26 Cl3.6 I0.4 N2 O2 P Rh' _chemical_formula_weight 746.81 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' 'N' 'N' 0.0061 0.0033 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.172(5) _cell_length_b 22.005(5) _cell_length_c 14.952(5) _cell_angle_alpha 90.000(0) _cell_angle_beta 90.000(0) _cell_angle_gamma 90.000(0) _cell_volume 5979(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2979 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7186 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.4380 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 22.04 _reflns_number_total 3671 _reflns_number_gt 791 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3671 _refine_ls_number_parameters 363 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2232 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.578 _refine_ls_restrained_S_all 0.578 _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 Rh Rh 0.14834(5) 0.09231(5) 0.07383(7) 0.0620(4) Uani 1 d . . . I1 I 0.2719(3) 0.1290(2) 0.0100(4) 0.0743(17) Uani 0.431(6) d P . . Cl1 Cl 0.2679(11) 0.1245(11) 0.0172(15) 0.198(17) Uani 0.569(6) d P . . Cl2 Cl 0.14513(16) -0.00093(13) -0.03802(18) 0.0568(9) Uani 1 d . . . Cl3 Cl 0.0048(3) 0.6240(3) 0.1011(3) 0.179(2) Uani 1 d . . . Cl4 Cl -0.0023(4) 0.7204(3) -0.0210(4) 0.214(3) Uani 1 d . . . P P 0.1970(2) 0.04956(19) 0.1957(2) 0.0608(12) Uani 1 d . . . O1 O 0.0922(5) 0.1356(4) -0.0336(5) 0.061(3) Uani 1 d . . . O2 O 0.0755(6) 0.1712(5) 0.1855(8) 0.106(4) Uani 1 d . . . N1 N 0.0463(5) 0.0637(6) 0.0991(9) 0.060(4) Uani 1 d . . . N2 N 0.0007(6) 0.0788(5) 0.0289(9) 0.069(4) Uani 1 d . . . H2N H -0.0417 0.0619 0.0233 0.083 Uiso 1 calc R . . C1 C 0.1265(8) 0.0198(6) 0.2710(10) 0.056(4) Uani 1 d . . . C2 C 0.1426(9) 0.0044(6) 0.3581(10) 0.065(4) Uani 1 d . . . H2 H 0.1892 0.0140 0.3795 0.078 Uiso 1 calc R . . C3 C 0.0948(8) -0.0240(7) 0.4156(10) 0.080(5) Uani 1 d . . . H3 H 0.1089 -0.0359 0.4728 0.096 Uiso 1 calc R . . C4 C 0.0226(8) -0.0341(6) 0.3825(11) 0.087(5) Uani 1 d . . . H4 H -0.0124 -0.0521 0.4195 0.104 Uiso 1 calc R . . C5 C 0.0038(9) -0.0183(7) 0.2988(10) 0.079(6) Uani 1 d . . . H5 H -0.0437 -0.0260 0.2785 0.095 Uiso 1 calc R . . C6 C 0.0546(10) 0.0095(6) 0.2416(11) 0.061(4) Uani 1 d . . . C7 C 0.0159(8) 0.0302(6) 0.1590(12) 0.065(5) Uani 1 d . . . H7 H -0.0327 0.0182 0.1505 0.078 Uiso 1 calc R . . C8 C 0.0225(8) 0.1182(7) -0.0272(11) 0.057(5) Uani 1 d . . . C9 C -0.0236(9) 0.1414(7) -0.1045(10) 0.062(4) Uani 1 d . . . C10 C -0.0995(10) 0.1302(7) -0.1039(11) 0.102(6) Uani 1 d . . . H10 H -0.1204 0.1084 -0.0570 0.122 Uiso 1 calc R . . C11 C -0.1436(10) 0.1514(8) -0.1728(12) 0.126(7) Uani 1 d U . . H11 H -0.1936 0.1423 -0.1731 0.151 Uiso 1 calc R . . C12 C -0.1153(12) 0.1845(9) -0.2383(13) 0.115(7) Uani 1 d U . . H12 H -0.1450 0.1988 -0.2844 0.138 Uiso 1 calc R . . C13 C -0.0389(13) 0.1977(8) -0.2369(12) 0.107(7) Uani 1 d . . . H13 H -0.0197 0.2212 -0.2830 0.128 Uiso 1 calc R . . C14 C 0.0085(10) 0.1779(8) -0.1711(11) 0.102(6) Uani 1 d . . . H14 H 0.0582 0.1880 -0.1708 0.122 Uiso 1 calc R . . C15 C 0.2583(7) -0.0122(7) 0.1835(12) 0.063(5) Uani 1 d . . . C16 C 0.2808(8) -0.0316(7) 0.0986(12) 0.084(6) Uani 1 d . . . H16 H 0.2633 -0.0104 0.0491 0.101 Uiso 1 calc R . . C17 C 0.3271(8) -0.0799(8) 0.0837(11) 0.083(5) Uani 1 d . . . H17 H 0.3411 -0.0900 0.0258 0.100 Uiso 1 calc R . . C18 C 0.3534(8) -0.1145(7) 0.1576(12) 0.079(5) Uani 1 d . . . H18 H 0.3842 -0.1478 0.1485 0.095 Uiso 1 calc R . . C19 C 0.3323(7) -0.0975(7) 0.2445(11) 0.074(5) Uani 1 d . . . H19 H 0.3501 -0.1183 0.2941 0.089 Uiso 1 calc R . . C20 C 0.2853(8) -0.0502(7) 0.2547(9) 0.068(5) Uani 1 d . . . H20 H 0.2692 -0.0416 0.3124 0.081 Uiso 1 calc R . . C21 C 0.2497(8) 0.0987(7) 0.2674(8) 0.057(4) Uani 1 d . . . C22 C 0.2169(8) 0.1367(7) 0.3311(12) 0.081(5) Uani 1 d . . . H22 H 0.1663 0.1350 0.3396 0.098 Uiso 1 calc R . . C23 C 0.2595(13) 0.1776(9) 0.3829(10) 0.119(7) Uani 1 d . . . H23 H 0.2361 0.2017 0.4254 0.143 Uiso 1 calc R . . C24 C 0.3350(13) 0.1828(9) 0.3722(13) 0.116(7) Uani 1 d . . . H24 H 0.3625 0.2099 0.4063 0.139 Uiso 1 calc R . . C25 C 0.3683(9) 0.1449(8) 0.3070(13) 0.090(6) Uani 1 d . . . H25 H 0.4189 0.1466 0.2976 0.108 Uiso 1 calc R . . C27 C 0.1315(8) 0.1705(8) 0.1474(11) 0.076(5) Uani 1 d . . . C28 C 0.1792(8) 0.2200(5) 0.1399(10) 0.130(7) Uani 1 d . . . H28A H 0.1700 0.2408 0.0847 0.195 Uiso 1 calc R . . H28B H 0.2292 0.2058 0.1409 0.195 Uiso 1 calc R . . H28C H 0.1713 0.2473 0.1891 0.195 Uiso 1 calc R . . C26 C 0.3252(9) 0.1048(6) 0.2567(8) 0.071(4) Uani 1 d . . . H26 H 0.3483 0.0810 0.2137 0.085 Uiso 1 calc R . . C29 C 0.0488(9) 0.6849(8) 0.0588(16) 0.216(12) Uani 1 d . . . H29A H 0.0953 0.6720 0.0330 0.259 Uiso 1 calc R . . H29B H 0.0595 0.7133 0.1067 0.259 Uiso 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 Rh 0.0551(7) 0.0762(8) 0.0546(7) 0.0037(8) -0.0003(8) -0.0041(8) I1 0.054(3) 0.077(3) 0.092(4) -0.002(3) 0.001(3) 0.001(2) Cl1 0.103(16) 0.40(3) 0.093(16) -0.014(17) 0.029(12) -0.080(15) Cl2 0.0481(19) 0.064(2) 0.058(2) -0.0042(17) 0.005(2) -0.010(2) Cl3 0.179(5) 0.229(7) 0.128(5) 0.034(4) 0.011(4) -0.022(5) Cl4 0.313(8) 0.159(6) 0.170(6) -0.012(5) -0.066(6) 0.007(6) P 0.049(3) 0.071(3) 0.063(3) 0.004(2) 0.002(2) -0.007(3) O1 0.069(6) 0.073(6) 0.043(6) 0.017(5) -0.013(5) 0.014(6) O2 0.065(8) 0.100(10) 0.151(11) -0.042(8) 0.006(8) -0.004(8) N1 0.041(8) 0.091(10) 0.049(9) -0.010(7) -0.022(7) -0.015(7) N2 0.065(9) 0.079(11) 0.064(9) 0.012(8) -0.009(8) -0.042(8) C1 0.049(12) 0.063(11) 0.054(12) 0.016(8) 0.002(9) 0.001(8) C2 0.077(12) 0.070(11) 0.047(11) 0.000(9) -0.019(11) 0.023(11) C3 0.045(10) 0.126(14) 0.069(11) 0.025(12) -0.003(11) 0.037(9) C4 0.063(13) 0.115(15) 0.081(15) 0.021(11) -0.006(10) 0.005(10) C5 0.053(10) 0.170(19) 0.015(9) 0.012(10) 0.004(9) -0.008(12) C6 0.058(13) 0.071(13) 0.053(13) -0.001(10) -0.004(11) 0.018(10) C7 0.069(13) 0.048(12) 0.079(14) -0.010(10) -0.002(12) -0.036(10) C8 0.034(10) 0.056(12) 0.083(13) 0.003(10) 0.001(10) 0.015(9) C9 0.060(11) 0.065(12) 0.061(13) -0.006(10) -0.015(11) 0.013(10) C10 0.104(15) 0.097(13) 0.105(16) 0.018(11) -0.056(13) -0.021(12) C11 0.095(14) 0.18(2) 0.097(14) 0.080(13) -0.060(14) -0.058(15) C12 0.12(2) 0.130(17) 0.101(16) 0.056(14) -0.053(15) -0.009(14) C13 0.140(19) 0.127(17) 0.054(14) 0.028(12) 0.006(14) -0.024(16) C14 0.160(18) 0.119(15) 0.026(11) 0.033(11) 0.006(12) 0.004(14) C15 0.037(10) 0.077(14) 0.076(12) -0.002(12) -0.011(10) -0.019(9) C16 0.072(12) 0.074(13) 0.106(17) -0.023(12) -0.015(12) 0.032(10) C17 0.070(12) 0.117(15) 0.063(11) 0.028(14) -0.027(11) -0.020(11) C18 0.054(10) 0.097(15) 0.086(12) -0.043(12) 0.026(12) -0.022(11) C19 0.053(12) 0.059(11) 0.110(15) 0.049(12) 0.012(10) 0.026(10) C20 0.058(11) 0.090(14) 0.055(11) 0.019(10) 0.001(9) 0.022(10) C21 0.051(11) 0.081(12) 0.038(9) 0.005(9) -0.001(8) 0.004(11) C22 0.092(13) 0.060(12) 0.092(14) 0.001(10) -0.012(12) -0.011(11) C23 0.18(2) 0.134(19) 0.045(12) 0.004(11) -0.067(15) -0.053(18) C24 0.16(2) 0.081(16) 0.109(17) 0.024(12) 0.004(17) -0.063(17) C25 0.066(13) 0.080(14) 0.123(17) 0.012(12) -0.037(12) -0.042(12) C27 0.049(12) 0.058(12) 0.122(14) 0.041(11) -0.020(11) 0.013(11) C28 0.202(18) 0.034(11) 0.154(15) -0.035(10) 0.049(15) -0.052(12) C26 0.069(13) 0.087(13) 0.056(10) 0.030(10) -0.013(9) -0.020(11) C29 0.129(16) 0.127(17) 0.39(4) 0.14(2) -0.08(2) -0.048(14) _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 Rh N1 1.994(10) . ? Rh C27 2.064(18) . ? Rh O1 2.129(7) . ? Rh P 2.233(4) . ? Rh Cl1 2.44(2) . ? Rh I1 2.569(6) . ? Rh Cl2 2.648(3) . ? Cl3 C29 1.685(16) . ? Cl4 C29 1.702(16) . ? P C15 1.767(15) . ? P C21 1.799(14) . ? P C1 1.828(12) . ? O1 C8 1.326(13) . ? O2 C27 1.167(14) . ? N1 C7 1.286(13) . ? N1 N2 1.377(12) . ? N2 C8 1.270(14) . ? C1 C2 1.377(14) . ? C1 C6 1.397(15) . ? C2 C3 1.373(15) . ? C3 C4 1.421(15) . ? C4 C5 1.344(15) . ? C5 C6 1.400(17) . ? C6 C7 1.492(17) . ? C8 C9 1.516(17) . ? C9 C10 1.401(15) . ? C9 C14 1.406(16) . ? C10 C11 1.387(17) . ? C11 C12 1.323(18) . ? C12 C13 1.419(18) . ? C13 C14 1.379(19) . ? C15 C16 1.401(16) . ? C15 C20 1.440(16) . ? C16 C17 1.374(15) . ? C17 C18 1.424(17) . ? C18 C19 1.406(15) . ? C19 C20 1.355(15) . ? C21 C26 1.387(14) . ? C21 C22 1.400(16) . ? C22 C23 1.418(16) . ? C23 C24 1.385(19) . ? C24 C25 1.420(19) . ? C25 C26 1.399(15) . ? C27 C28 1.396(16) . ? 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 N1 Rh C27 91.4(5) . . ? N1 Rh O1 80.7(5) . . ? C27 Rh O1 87.6(4) . . ? N1 Rh P 94.7(4) . . ? C27 Rh P 88.6(4) . . ? O1 Rh P 173.9(3) . . ? N1 Rh Cl1 170.5(6) . . ? C27 Rh Cl1 94.3(7) . . ? O1 Rh Cl1 92.0(6) . . ? P Rh Cl1 93.0(5) . . ? N1 Rh I1 169.1(4) . . ? C27 Rh I1 93.7(5) . . ? O1 Rh I1 89.9(3) . . ? P Rh I1 95.12(17) . . ? Cl1 Rh I1 2.2(6) . . ? N1 Rh Cl2 81.6(3) . . ? C27 Rh Cl2 168.2(4) . . ? O1 Rh Cl2 81.9(2) . . ? P Rh Cl2 101.40(13) . . ? Cl1 Rh Cl2 91.5(5) . . ? I1 Rh Cl2 91.63(14) . . ? C15 P C21 100.9(7) . . ? C15 P C1 103.3(7) . . ? C21 P C1 102.8(7) . . ? C15 P Rh 119.3(6) . . ? C21 P Rh 116.3(4) . . ? C1 P Rh 112.1(6) . . ? C8 O1 Rh 105.9(9) . . ? C7 N1 N2 114.2(12) . . ? C7 N1 Rh 135.5(11) . . ? N2 N1 Rh 109.9(9) . . ? C8 N2 N1 118.7(12) . . ? C2 C1 C6 117.1(14) . . ? C2 C1 P 121.5(14) . . ? C6 C1 P 121.3(13) . . ? C3 C2 C1 124.8(15) . . ? C2 C3 C4 115.9(14) . . ? C5 C4 C3 121.3(15) . . ? C4 C5 C6 120.9(15) . . ? C1 C6 C5 119.7(14) . . ? C1 C6 C7 130.7(15) . . ? C5 C6 C7 109.1(16) . . ? N1 C7 C6 123.3(14) . . ? N2 C8 O1 122.9(14) . . ? N2 C8 C9 124.1(15) . . ? O1 C8 C9 112.0(15) . . ? C10 C9 C14 120.9(15) . . ? C10 C9 C8 118.7(16) . . ? C14 C9 C8 120.2(17) . . ? C11 C10 C9 120.3(16) . . ? C12 C11 C10 120.8(18) . . ? C11 C12 C13 118.7(18) . . ? C14 C13 C12 124.0(18) . . ? C13 C14 C9 115.2(17) . . ? C16 C15 C20 113.3(14) . . ? C16 C15 P 120.7(14) . . ? C20 C15 P 125.8(14) . . ? C17 C16 C15 124.1(17) . . ? C16 C17 C18 119.7(16) . . ? C19 C18 C17 118.8(15) . . ? C20 C19 C18 118.8(14) . . ? C19 C20 C15 125.3(14) . . ? C26 C21 C22 116.2(14) . . ? C26 C21 P 121.0(13) . . ? C22 C21 P 122.5(13) . . ? C21 C22 C23 121.2(16) . . ? C24 C23 C22 122(2) . . ? C23 C24 C25 117(2) . . ? C26 C25 C24 120.0(17) . . ? O2 C27 C28 124.8(18) . . ? O2 C27 Rh 113.6(14) . . ? C28 C27 Rh 121.0(12) . . ? C21 C26 C25 123.6(15) . . ? Cl3 C29 Cl4 111.7(9) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 22.04 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.593 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.083