# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1602 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Neil G. Connelly, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. ; _publ_contact_author_phone '0117 9288162' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email Neil.Connelly@bris.ac.uk _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this work for publication in Chemical Communications. ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Redox-active heteronuclear triazanide-bridged complexes; ancillary ligand dependence of electron distribution in a sigma^*^ rhodium-iridium orbital ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Conelly, Neil G.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Hayward, Owen D.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Klangsinsirikul, Phimphaka' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Rieger, Philip H.' ; Department of Chemistry Brown University Rhode Island RI 02912, USA ; #============================================================================== # 3. TEXT # # # N.G. CONNELLY # _publ_section_abstract ; ? ; data_1.[Rh(cod)(mu-RNNNR)2Ir(CO)2].0.14CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38.14 H40.28 Cl0.28 Ir N6 O2 Rh' _chemical_formula_weight 919.76 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' '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' 'Ir' 'Ir' -1.4442 7.9887 '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 15.052(4) _cell_length_b 13.982(2) _cell_length_c 17.202(3) _cell_angle_alpha 90.000(13) _cell_angle_beta 98.426(14) _cell_angle_gamma 90.000(10) _cell_volume 3581.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 174 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 4.236 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3630 _exptl_absorpt_correction_T_max 0.8161 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18420 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6288 _reflns_number_gt 4337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^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 6288 _refine_ls_number_parameters 446 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Ir1 Ir 0.12733(2) 1.00918(2) 0.791943(18) 0.02325(10) Uani 1 1 d . . . Rh1 Rh 0.13553(5) 0.83627(4) 0.88002(4) 0.02111(16) Uani 1 1 d . . . N1 N 0.2042(5) 1.0589(4) 0.8952(4) 0.0226(16) Uani 1 1 d . . . N2 N 0.2617(4) 1.0052(4) 0.9408(3) 0.0237(15) Uani 1 1 d . . . N3 N 0.2507(5) 0.9122(4) 0.9336(3) 0.0223(16) Uani 1 1 d . . . N4 N 0.2487(4) 0.9488(4) 0.7673(4) 0.0207(16) Uani 1 1 d . . . N5 N 0.2669(5) 0.8580(4) 0.7609(4) 0.0269(17) Uani 1 1 d . . . N6 N 0.2167(4) 0.7985(4) 0.7937(3) 0.0217(16) Uani 1 1 d . . . O1 O 0.0340(5) 0.9473(4) 0.6345(4) 0.0484(19) Uani 1 1 d . . . O2 O -0.0395(5) 1.1060(4) 0.8273(4) 0.0407(17) Uani 1 1 d . . . C1 C 0.0684(6) 0.9697(5) 0.6949(5) 0.032(2) Uani 1 1 d . . . C2 C 0.0232(6) 1.0688(6) 0.8134(5) 0.028(2) Uani 1 1 d . . . C3 C -0.0659(6) 0.8445(6) 0.8288(5) 0.037(2) Uani 1 1 d . . . H3A H -0.1206 0.8042 0.8210 0.044 Uiso 1 1 calc R . . H3B H -0.0746 0.8969 0.7897 0.044 Uiso 1 1 calc R . . C4 C -0.0554(6) 0.8876(6) 0.9109(5) 0.031(2) Uani 1 1 d . . . H4A H -0.0859 0.9504 0.9082 0.038 Uiso 1 1 calc R . . H4B H -0.0856 0.8455 0.9452 0.038 Uiso 1 1 calc R . . C5 C 0.0418(6) 0.9008(6) 0.9477(5) 0.030(2) Uani 1 1 d . . . H5B H 0.0571 0.9684 0.9633 0.036 Uiso 1 1 calc R . . C6 C 0.0935(6) 0.8333(5) 0.9940(4) 0.026(2) Uani 1 1 d . . . H6A H 0.1377 0.8608 1.0373 0.032 Uiso 1 1 calc R . . C7 C 0.0583(7) 0.7335(6) 1.0108(5) 0.042(3) Uani 1 1 d . . . H7A H 0.0159 0.7393 1.0494 0.051 Uiso 1 1 calc R . . H7B H 0.1093 0.6933 1.0347 0.051 Uiso 1 1 calc R . . C8 C 0.0107(6) 0.6839(5) 0.9365(5) 0.034(2) Uani 1 1 d . . . H8A H 0.0161 0.6137 0.9435 0.041 Uiso 1 1 calc R . . H8B H -0.0540 0.7002 0.9296 0.041 Uiso 1 1 calc R . . C9 C 0.0489(6) 0.7123(6) 0.8630(5) 0.032(2) Uani 1 1 d . . . H9A H 0.0741 0.6578 0.8355 0.039 Uiso 1 1 calc R . . C10 C 0.0134(6) 0.7848(5) 0.8140(5) 0.027(2) Uani 1 1 d . . . H10A H 0.0168 0.7733 0.7571 0.033 Uiso 1 1 calc R . . C11 C 0.2080(5) 1.1560(5) 0.9203(4) 0.0213(18) Uani 1 1 d . . . C12 C 0.1711(6) 1.2277(5) 0.8687(5) 0.031(2) Uani 1 1 d . . . H12A H 0.1481 1.2116 0.8160 0.037 Uiso 1 1 calc R . . C13 C 0.1675(6) 1.3217(6) 0.8932(5) 0.038(2) Uani 1 1 d . . . H13A H 0.1406 1.3683 0.8569 0.045 Uiso 1 1 calc R . . C14 C 0.2011(7) 1.3498(6) 0.9676(6) 0.043(3) Uani 1 1 d . . . C15 C 0.1972(8) 1.4521(6) 0.9965(6) 0.062(4) Uani 1 1 d . . . H15A H 0.2253 1.4558 1.0515 0.093 Uiso 1 1 calc R . . H15B H 0.1343 1.4725 0.9923 0.093 Uiso 1 1 calc R . . H15C H 0.2292 1.4941 0.9644 0.093 Uiso 1 1 calc R . . C16 C 0.2417(7) 1.2783(6) 1.0174(5) 0.044(3) Uani 1 1 d . . . H16A H 0.2694 1.2958 1.0686 0.053 Uiso 1 1 calc R . . C17 C 0.2434(6) 1.1828(6) 0.9955(5) 0.035(2) Uani 1 1 d . . . H17A H 0.2690 1.1362 1.0323 0.042 Uiso 1 1 calc R . . C18 C 0.3272(6) 0.8616(5) 0.9725(4) 0.0239(19) Uani 1 1 d . . . C19 C 0.3149(6) 0.7721(5) 1.0038(5) 0.032(2) Uani 1 1 d . . . H19A H 0.2565 0.7447 0.9985 0.039 Uiso 1 1 calc R . . C20 C 0.3876(7) 0.7226(6) 1.0429(5) 0.036(2) Uani 1 1 d . . . H20A H 0.3780 0.6617 1.0648 0.044 Uiso 1 1 calc R . . C21 C 0.4730(7) 0.7588(7) 1.0511(5) 0.042(2) Uani 1 1 d . . . C22 C 0.5543(8) 0.7055(8) 1.0932(6) 0.075(4) Uani 1 1 d . . . H22A H 0.6084 0.7442 1.0922 0.112 Uiso 1 1 calc R . . H22B H 0.5608 0.6444 1.0667 0.112 Uiso 1 1 calc R . . H22C H 0.5461 0.6936 1.1478 0.112 Uiso 1 1 calc R . . C23 C 0.4868(6) 0.8482(6) 1.0175(6) 0.046(3) Uani 1 1 d . . . H23A H 0.5454 0.8748 1.0222 0.055 Uiso 1 1 calc R . . C24 C 0.4140(7) 0.8972(6) 0.9775(6) 0.044(3) Uani 1 1 d . . . H24A H 0.4237 0.9564 0.9529 0.053 Uiso 1 1 calc R . . C25 C 0.3167(5) 1.0084(5) 0.7447(4) 0.0259(18) Uani 1 1 d . . . C26 C 0.4015(7) 0.9802(7) 0.7425(10) 0.106(6) Uani 1 1 d . . . H26A H 0.4174 0.9159 0.7561 0.128 Uiso 1 1 calc R . . C27 C 0.4660(9) 1.0395(8) 0.7217(12) 0.151(9) Uani 1 1 d . . . H27A H 0.5237 1.0142 0.7177 0.181 Uiso 1 1 calc R . . C28 C 0.4499(7) 1.1353(6) 0.7062(7) 0.055(3) Uani 1 1 d . . . C29 C 0.5224(8) 1.2013(7) 0.6850(8) 0.091(5) Uani 1 1 d . . . H29A H 0.5785 1.1654 0.6859 0.136 Uiso 1 1 calc R . . H29B H 0.5318 1.2538 0.7230 0.136 Uiso 1 1 calc R . . H29C H 0.5040 1.2274 0.6322 0.136 Uiso 1 1 calc R . . C30 C 0.3668(7) 1.1628(5) 0.7098(5) 0.042(2) Uani 1 1 d . . . H30A H 0.3524 1.2284 0.7006 0.050 Uiso 1 1 calc R . . C31 C 0.2998(7) 1.1022(6) 0.7262(6) 0.052(3) Uani 1 1 d . . . H31A H 0.2405 1.1262 0.7245 0.062 Uiso 1 1 calc R . . C32 C 0.2366(5) 0.7018(5) 0.7731(4) 0.0220(19) Uani 1 1 d . . . C33 C 0.2474(6) 0.6310(5) 0.8290(5) 0.025(2) Uani 1 1 d . . . H33A H 0.2390 0.6449 0.8815 0.030 Uiso 1 1 calc R . . C34 C 0.2706(6) 0.5387(5) 0.8088(5) 0.028(2) Uani 1 1 d . . . H34A H 0.2770 0.4902 0.8479 0.034 Uiso 1 1 calc R . . C35 C 0.2846(6) 0.5160(5) 0.7339(5) 0.029(2) Uani 1 1 d . . . C36 C 0.3107(7) 0.4157(5) 0.7125(5) 0.043(3) Uani 1 1 d . . . H36A H 0.3175 0.4136 0.6567 0.064 Uiso 1 1 calc R . . H36B H 0.2637 0.3707 0.7224 0.064 Uiso 1 1 calc R . . H36C H 0.3676 0.3980 0.7445 0.064 Uiso 1 1 calc R . . C37 C 0.2735(6) 0.5875(5) 0.6779(5) 0.034(2) Uani 1 1 d . . . H37A H 0.2823 0.5729 0.6256 0.041 Uiso 1 1 calc R . . C38 C 0.2497(6) 0.6811(6) 0.6962(4) 0.030(2) Uani 1 1 d . . . H38A H 0.2426 0.7295 0.6569 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.5815(11) 0.5253(8) 0.9683(7) 0.106(5) Uani 0.28 1 d PD . . C99 C 0.5321(18) 0.478(6) 1.043(3) 0.10(3) Uiso 0.14 1 d PD . . H99A H 0.5546 0.4120 1.0527 0.116 Uiso 0.14 1 calc PR . . H99B H 0.5531 0.5155 1.0914 0.116 Uiso 0.14 1 calc PR . . 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 Ir1 0.03036(19) 0.01721(16) 0.02340(16) 0.00011(15) 0.00805(13) 0.00300(17) Rh1 0.0294(4) 0.0161(3) 0.0198(3) -0.0019(3) 0.0101(3) -0.0013(3) N1 0.027(5) 0.009(3) 0.032(4) 0.003(3) 0.006(4) 0.005(3) N2 0.035(4) 0.016(3) 0.023(3) -0.004(3) 0.012(3) -0.003(3) N3 0.032(5) 0.019(3) 0.017(4) 0.002(3) 0.007(3) 0.000(3) N4 0.023(4) 0.017(3) 0.024(4) 0.009(3) 0.011(3) 0.005(3) N5 0.030(5) 0.015(3) 0.037(4) 0.004(3) 0.012(4) 0.004(3) N6 0.023(4) 0.019(3) 0.026(4) -0.001(3) 0.013(3) -0.003(3) O1 0.066(6) 0.044(4) 0.032(4) -0.013(3) -0.005(4) 0.006(4) O2 0.042(5) 0.037(4) 0.048(4) 0.003(3) 0.020(4) 0.010(3) C1 0.039(6) 0.026(5) 0.032(5) 0.004(4) 0.005(5) 0.013(4) C2 0.030(6) 0.027(5) 0.029(5) 0.008(4) 0.008(5) -0.004(4) C3 0.040(6) 0.034(5) 0.036(5) -0.008(4) -0.001(5) -0.007(5) C4 0.024(6) 0.028(5) 0.044(6) -0.008(4) 0.012(5) 0.002(4) C5 0.039(6) 0.024(4) 0.031(5) -0.006(4) 0.018(5) 0.003(4) C6 0.039(6) 0.020(4) 0.025(4) -0.010(4) 0.020(4) -0.007(4) C7 0.065(8) 0.029(5) 0.039(6) 0.005(4) 0.029(5) -0.003(5) C8 0.043(6) 0.017(4) 0.048(6) 0.001(4) 0.026(5) -0.001(4) C9 0.041(6) 0.023(4) 0.036(5) -0.007(4) 0.014(5) -0.009(4) C10 0.030(6) 0.023(4) 0.031(5) -0.008(4) 0.010(4) -0.002(4) C11 0.018(5) 0.020(4) 0.027(5) 0.004(4) 0.008(4) 0.001(4) C12 0.044(6) 0.019(4) 0.032(5) -0.007(4) 0.016(5) -0.001(4) C13 0.047(7) 0.025(5) 0.045(6) 0.007(4) 0.017(5) 0.002(4) C14 0.074(8) 0.015(4) 0.050(6) 0.000(4) 0.040(6) 0.000(5) C15 0.113(11) 0.024(5) 0.061(7) -0.008(5) 0.051(7) -0.007(6) C16 0.074(8) 0.031(5) 0.031(5) -0.013(4) 0.019(5) -0.016(5) C17 0.055(7) 0.023(5) 0.028(5) 0.000(4) 0.012(5) -0.004(4) C18 0.028(6) 0.023(4) 0.020(4) -0.001(3) 0.004(4) 0.003(4) C19 0.040(6) 0.027(5) 0.030(5) 0.004(4) 0.010(5) 0.000(4) C20 0.042(7) 0.031(5) 0.035(5) 0.008(4) 0.005(5) 0.009(5) C21 0.031(6) 0.049(6) 0.042(6) 0.000(5) -0.005(5) 0.014(5) C22 0.051(9) 0.094(9) 0.075(8) 0.030(7) -0.004(7) 0.020(7) C23 0.026(6) 0.040(6) 0.074(8) 0.002(5) 0.008(6) 0.002(5) C24 0.035(7) 0.025(5) 0.073(7) 0.002(5) 0.007(6) 0.001(4) C25 0.028(5) 0.021(4) 0.030(4) -0.004(4) 0.010(4) -0.001(4) C26 0.041(8) 0.028(6) 0.256(18) 0.064(8) 0.043(10) 0.002(5) C27 0.049(9) 0.039(7) 0.39(3) 0.062(11) 0.102(14) 0.017(6) C28 0.032(7) 0.031(5) 0.106(9) 0.018(6) 0.015(7) 0.003(5) C29 0.053(8) 0.036(6) 0.189(14) 0.041(8) 0.036(9) -0.005(6) C30 0.054(7) 0.019(4) 0.059(6) 0.005(5) 0.028(6) -0.002(5) C31 0.057(8) 0.029(5) 0.078(8) 0.009(5) 0.042(7) 0.005(5) C32 0.022(5) 0.017(4) 0.029(5) -0.001(3) 0.008(4) -0.008(3) C33 0.037(6) 0.014(4) 0.026(5) 0.006(3) 0.010(4) 0.005(4) C34 0.033(6) 0.016(4) 0.037(5) 0.005(4) 0.013(5) -0.001(4) C35 0.036(5) 0.017(4) 0.035(5) -0.007(4) 0.006(4) 0.010(4) C36 0.062(8) 0.023(5) 0.043(6) -0.004(4) 0.005(6) 0.009(5) C37 0.054(7) 0.030(5) 0.018(5) -0.001(4) 0.005(5) 0.011(5) C38 0.044(6) 0.026(5) 0.021(4) 0.003(4) 0.008(4) 0.007(4) Cl1 0.173(16) 0.065(8) 0.092(9) -0.012(6) 0.060(10) -0.009(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.856(9) . ? Ir1 C2 1.859(10) . ? Ir1 N1 2.091(7) . ? Ir1 N4 2.111(6) . ? Ir1 Rh1 2.8462(8) . ? Rh1 N6 2.124(6) . ? Rh1 N3 2.125(7) . ? Rh1 C10 2.139(8) . ? Rh1 C6 2.147(7) . ? Rh1 C5 2.154(8) . ? Rh1 C9 2.163(8) . ? N1 N2 1.315(8) . ? N1 C11 1.423(9) . ? N2 N3 1.314(8) . ? N3 C18 1.431(10) . ? N4 N5 1.306(8) . ? N4 C25 1.418(10) . ? N5 N6 1.305(8) . ? N6 C32 1.441(9) . ? O1 C1 1.135(9) . ? O2 C2 1.134(10) . ? C3 C10 1.510(11) . ? C3 C4 1.521(10) . ? C4 C5 1.518(12) . ? C5 C6 1.397(11) . ? C6 C7 1.535(10) . ? C7 C8 1.537(11) . ? C8 C9 1.517(10) . ? C9 C10 1.376(11) . ? C11 C17 1.378(10) . ? C11 C12 1.399(10) . ? C12 C13 1.384(10) . ? C13 C14 1.364(12) . ? C14 C16 1.397(12) . ? C14 C15 1.518(11) . ? C16 C17 1.388(11) . ? C18 C19 1.387(10) . ? C18 C24 1.389(12) . ? C19 C20 1.383(12) . ? C20 C21 1.369(13) . ? C21 C23 1.405(12) . ? C21 C22 1.523(13) . ? C23 C24 1.386(12) . ? C25 C26 1.342(13) . ? C25 C31 1.365(11) . ? C26 C27 1.364(14) . ? C27 C28 1.379(13) . ? C28 C30 1.319(12) . ? C28 C29 1.514(13) . ? C30 C31 1.379(12) . ? C32 C33 1.374(10) . ? C32 C38 1.396(10) . ? C33 C34 1.395(10) . ? C34 C35 1.372(11) . ? C35 C37 1.382(10) . ? C35 C36 1.516(10) . ? C37 C38 1.406(10) . ? Cl1 C99 1.69(2) 3_667 ? Cl1 C99 1.71(2) . ? C99 Cl1 1.69(2) 3_667 ? 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 C1 Ir1 C2 90.4(4) . . ? C1 Ir1 N1 174.1(3) . . ? C2 Ir1 N1 93.4(3) . . ? C1 Ir1 N4 90.8(3) . . ? C2 Ir1 N4 176.9(3) . . ? N1 Ir1 N4 85.2(3) . . ? C1 Ir1 Rh1 101.8(2) . . ? C2 Ir1 Rh1 104.3(2) . . ? N1 Ir1 Rh1 81.65(16) . . ? N4 Ir1 Rh1 78.20(15) . . ? N6 Rh1 N3 84.9(2) . . ? N6 Rh1 C10 94.7(3) . . ? N3 Rh1 C10 169.0(3) . . ? N6 Rh1 C6 155.6(3) . . ? N3 Rh1 C6 86.8(3) . . ? C10 Rh1 C6 97.7(3) . . ? N6 Rh1 C5 166.3(3) . . ? N3 Rh1 C5 96.5(3) . . ? C10 Rh1 C5 81.3(3) . . ? C6 Rh1 C5 37.9(3) . . ? N6 Rh1 C9 95.9(3) . . ? N3 Rh1 C9 153.7(3) . . ? C10 Rh1 C9 37.3(3) . . ? C6 Rh1 C9 81.7(3) . . ? C5 Rh1 C9 88.8(3) . . ? N6 Rh1 Ir1 79.82(16) . . ? N3 Rh1 Ir1 77.02(16) . . ? C10 Rh1 Ir1 92.1(2) . . ? C6 Rh1 Ir1 120.5(2) . . ? C5 Rh1 Ir1 87.2(2) . . ? C9 Rh1 Ir1 129.1(2) . . ? N2 N1 C11 111.7(6) . . ? N2 N1 Ir1 123.4(4) . . ? C11 N1 Ir1 124.5(5) . . ? N3 N2 N1 116.5(6) . . ? N2 N3 C18 111.3(6) . . ? N2 N3 Rh1 128.2(5) . . ? C18 N3 Rh1 120.4(5) . . ? N5 N4 C25 112.3(6) . . ? N5 N4 Ir1 127.1(5) . . ? C25 N4 Ir1 120.0(5) . . ? N6 N5 N4 116.2(6) . . ? N5 N6 C32 109.7(6) . . ? N5 N6 Rh1 124.9(5) . . ? C32 N6 Rh1 124.5(5) . . ? O1 C1 Ir1 178.0(8) . . ? O2 C2 Ir1 179.0(9) . . ? C10 C3 C4 113.5(7) . . ? C5 C4 C3 113.5(7) . . ? C6 C5 C4 125.3(8) . . ? C6 C5 Rh1 70.8(5) . . ? C4 C5 Rh1 113.0(5) . . ? C5 C6 C7 122.9(8) . . ? C5 C6 Rh1 71.3(4) . . ? C7 C6 Rh1 110.2(5) . . ? C6 C7 C8 112.7(7) . . ? C9 C8 C7 112.8(7) . . ? C10 C9 C8 122.9(8) . . ? C10 C9 Rh1 70.4(5) . . ? C8 C9 Rh1 113.1(5) . . ? C9 C10 C3 123.3(8) . . ? C9 C10 Rh1 72.3(5) . . ? C3 C10 Rh1 111.3(5) . . ? C17 C11 C12 117.6(7) . . ? C17 C11 N1 122.5(7) . . ? C12 C11 N1 119.9(7) . . ? C13 C12 C11 121.2(8) . . ? C14 C13 C12 122.2(8) . . ? C13 C14 C16 116.0(8) . . ? C13 C14 C15 123.5(9) . . ? C16 C14 C15 120.6(9) . . ? C17 C16 C14 123.1(8) . . ? C11 C17 C16 119.8(8) . . ? C19 C18 C24 118.5(8) . . ? C19 C18 N3 118.9(8) . . ? C24 C18 N3 122.5(7) . . ? C20 C19 C18 120.0(9) . . ? C21 C20 C19 121.9(8) . . ? C20 C21 C23 118.7(9) . . ? C20 C21 C22 123.0(9) . . ? C23 C21 C22 118.3(9) . . ? C24 C23 C21 119.4(9) . . ? C23 C24 C18 121.4(9) . . ? C26 C25 C31 115.0(8) . . ? C26 C25 N4 124.2(8) . . ? C31 C25 N4 120.7(8) . . ? C25 C26 C27 123.0(9) . . ? C26 C27 C28 122.1(11) . . ? C30 C28 C27 114.5(9) . . ? C30 C28 C29 123.7(8) . . ? C27 C28 C29 121.8(10) . . ? C28 C30 C31 123.9(8) . . ? C25 C31 C30 121.4(10) . . ? C33 C32 C38 119.8(7) . . ? C33 C32 N6 120.8(7) . . ? C38 C32 N6 119.4(7) . . ? C32 C33 C34 120.0(7) . . ? C35 C34 C33 121.8(7) . . ? C34 C35 C37 118.0(7) . . ? C34 C35 C36 121.5(7) . . ? C37 C35 C36 120.5(7) . . ? C35 C37 C38 121.7(7) . . ? C32 C38 C37 118.7(7) . . ? C99 Cl1 C99 62(2) 3_667 . ? Cl1 C99 Cl1 118(2) 3_667 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.358 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.164 data_4.[Rh(CO)(PPh3)(mu-RNNNR)2Ir(CO)(PPh3)].3.0CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H62 Cl6 Ir N6 O2 P2 Rh' _chemical_formula_weight 1577.00 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 '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' _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 12.9339(10) _cell_length_b 15.1205(13) _cell_length_c 18.301(3) _cell_angle_alpha 83.50(8) _cell_angle_beta 71.74(6) _cell_angle_gamma 88.57(7) _cell_volume 3376.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 355 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 2.546 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.622757 _exptl_absorpt_correction_T_max 0.704112 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; ? ; _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_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34738 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.51 _reflns_number_total 15217 _reflns_number_gt 11985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^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 15217 _refine_ls_number_parameters 799 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.001 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 Ir1 Ir 0.413065(12) 0.300714(10) 0.264718(9) 0.01658(6) Uani 0.4792(8) 1 d P A 1 Rh1 Rh 0.183410(12) 0.332245(10) 0.275430(9) 0.01675(6) Uani 0.4792(8) 1 d P A 1 Ir2 Ir 0.183410(12) 0.332245(10) 0.275430(9) 0.01675(6) Uani 0.5208(8) 1 d P A 2 Rh2 Rh 0.413065(12) 0.300714(10) 0.264718(9) 0.01658(6) Uani 0.5208(8) 1 d P A 2 P1 P 0.44966(6) 0.37931(5) 0.35290(5) 0.01863(17) Uani 1 1 d . . . P2 P 0.16232(7) 0.39002(6) 0.16039(5) 0.02265(18) Uani 1 1 d . . . O1 O 0.5789(2) 0.41297(17) 0.14083(14) 0.0345(6) Uani 1 1 d . A . O2 O 0.1621(2) 0.51753(16) 0.31849(15) 0.0369(6) Uani 1 1 d . A . N1 N 0.3273(2) 0.19928(17) 0.35241(15) 0.0188(5) Uani 1 1 d . . . N2 N 0.2287(2) 0.20204(17) 0.40146(15) 0.0195(6) Uani 1 1 d . A . N3 N 0.1677(2) 0.26664(17) 0.38653(15) 0.0190(5) Uani 1 1 d . . . N4 N 0.3865(2) 0.21636(17) 0.18649(15) 0.0201(6) Uani 1 1 d . . . N5 N 0.2973(2) 0.17047(17) 0.19814(15) 0.0207(6) Uani 1 1 d . A . N6 N 0.2080(2) 0.20117(17) 0.24421(15) 0.0202(6) Uani 1 1 d . . . C1 C 0.5120(3) 0.3717(2) 0.18823(19) 0.0230(7) Uani 1 1 d . . . C2 C 0.1685(3) 0.4454(2) 0.30297(19) 0.0243(7) Uani 1 1 d . . . C3 C 0.3810(3) 0.1195(2) 0.37002(18) 0.0208(7) Uani 1 1 d . A . C4 C 0.4937(3) 0.1196(2) 0.3516(2) 0.0253(7) Uani 1 1 d . . . H4A H 0.5338 0.1706 0.3267 0.030 Uiso 1 1 calc R A . C5 C 0.5464(3) 0.0432(2) 0.3707(2) 0.0310(8) Uani 1 1 d . A . H5B H 0.6218 0.0444 0.3587 0.037 Uiso 1 1 calc R . . C6 C 0.4900(3) -0.0346(2) 0.4070(2) 0.0325(8) Uani 1 1 d . . . C7 C 0.3771(3) -0.0341(2) 0.4236(2) 0.0346(9) Uani 1 1 d . A . H7A H 0.3372 -0.0855 0.4476 0.042 Uiso 1 1 calc R . . C8 C 0.3229(3) 0.0414(2) 0.4051(2) 0.0291(8) Uani 1 1 d . . . H8A H 0.2476 0.0398 0.4161 0.035 Uiso 1 1 calc R A . C9 C 0.5481(3) -0.1174(3) 0.4276(3) 0.0475(11) Uani 1 1 d . A . H9A H 0.5849 -0.1049 0.4635 0.071 Uiso 1 1 calc R . . H9B H 0.6002 -0.1350 0.3816 0.071 Uiso 1 1 calc R . . H9C H 0.4959 -0.1646 0.4509 0.071 Uiso 1 1 calc R . . C10 C 0.0662(2) 0.2660(2) 0.44847(18) 0.0212(7) Uani 1 1 d . A . C11 C 0.0217(3) 0.3461(2) 0.47409(19) 0.0243(7) Uani 1 1 d . . . H11A H 0.0544 0.3998 0.4486 0.029 Uiso 1 1 calc R A . C12 C -0.0715(3) 0.3454(3) 0.5377(2) 0.0309(8) Uani 1 1 d . A . H12A H -0.0997 0.3992 0.5548 0.037 Uiso 1 1 calc R . . C13 C -0.1238(3) 0.2672(3) 0.5764(2) 0.0321(8) Uani 1 1 d . . . C14 C -0.0808(3) 0.1878(3) 0.5486(2) 0.0352(9) Uani 1 1 d . A . H14A H -0.1158 0.1343 0.5727 0.042 Uiso 1 1 calc R . . C15 C 0.0132(3) 0.1868(2) 0.4857(2) 0.0294(8) Uani 1 1 d . . . H15A H 0.0408 0.1329 0.4684 0.035 Uiso 1 1 calc R A . C16 C -0.2228(3) 0.2670(3) 0.6474(2) 0.0520(12) Uani 1 1 d . A . H16A H -0.2479 0.3268 0.6534 0.078 Uiso 1 1 calc R . . H16B H -0.2039 0.2428 0.6923 0.078 Uiso 1 1 calc R . . H16C H -0.2794 0.2312 0.6416 0.078 Uiso 1 1 calc R . . C17 C 0.4722(3) 0.1843(2) 0.12412(19) 0.0230(7) Uani 1 1 d . A . C18 C 0.4481(3) 0.1514(2) 0.0628(2) 0.0291(8) Uani 1 1 d . . . H18A H 0.3770 0.1533 0.0610 0.035 Uiso 1 1 calc R A . C19 C 0.5294(3) 0.1159(2) 0.0045(2) 0.0351(9) Uani 1 1 d . A . H19A H 0.5118 0.0936 -0.0354 0.042 Uiso 1 1 calc R . . C20 C 0.6367(3) 0.1131(2) 0.0049(2) 0.0343(9) Uani 1 1 d . . . C21 C 0.6597(3) 0.1476(2) 0.0649(2) 0.0322(8) Uani 1 1 d . A . H21A H 0.7312 0.1470 0.0657 0.039 Uiso 1 1 calc R . . C22 C 0.5797(3) 0.1834(2) 0.1240(2) 0.0269(7) Uani 1 1 d . . . H22A H 0.5982 0.2067 0.1633 0.032 Uiso 1 1 calc R A . C23 C 0.7248(4) 0.0728(3) -0.0583(3) 0.0565(13) Uani 1 1 d . A . H23A H 0.7883 0.0620 -0.0422 0.085 Uiso 1 1 calc R . . H23B H 0.7431 0.1134 -0.1049 0.085 Uiso 1 1 calc R . . H23C H 0.6987 0.0177 -0.0678 0.085 Uiso 1 1 calc R . . C24 C 0.1236(2) 0.1345(2) 0.27109(18) 0.0209(7) Uani 1 1 d . A . C25 C 0.0169(3) 0.1605(2) 0.3070(2) 0.0265(7) Uani 1 1 d . . . H25A H 0.0012 0.2206 0.3100 0.032 Uiso 1 1 calc R A . C26 C -0.0655(3) 0.0976(2) 0.3379(2) 0.0304(8) Uani 1 1 d . A . H26A H -0.1358 0.1164 0.3617 0.036 Uiso 1 1 calc R . . C27 C -0.0460(3) 0.0072(2) 0.3345(2) 0.0319(8) Uani 1 1 d . . . C28 C 0.0601(3) -0.0175(2) 0.2975(2) 0.0374(9) Uani 1 1 d . A . H28A H 0.0751 -0.0775 0.2930 0.045 Uiso 1 1 calc R . . C29 C 0.1448(3) 0.0445(2) 0.2668(2) 0.0305(8) Uani 1 1 d . . . H29A H 0.2153 0.0257 0.2436 0.037 Uiso 1 1 calc R A . C30 C -0.1371(3) -0.0614(3) 0.3702(3) 0.0498(12) Uani 1 1 d . A . H30A H -0.1996 -0.0335 0.4024 0.075 Uiso 1 1 calc R . . H30B H -0.1131 -0.1082 0.4010 0.075 Uiso 1 1 calc R . . H30C H -0.1559 -0.0859 0.3298 0.075 Uiso 1 1 calc R . . C31 C 0.4859(2) 0.4973(2) 0.32085(18) 0.0206(7) Uani 1 1 d . A . C32 C 0.4407(3) 0.5446(2) 0.26842(19) 0.0242(7) Uani 1 1 d . . . H32A H 0.3940 0.5157 0.2490 0.029 Uiso 1 1 calc R A . C33 C 0.4648(3) 0.6344(2) 0.2448(2) 0.0300(8) Uani 1 1 d . A . H33A H 0.4343 0.6652 0.2098 0.036 Uiso 1 1 calc R . . C34 C 0.5346(3) 0.6782(2) 0.2736(2) 0.0333(8) Uani 1 1 d . . . H34A H 0.5510 0.7382 0.2580 0.040 Uiso 1 1 calc R A . C35 C 0.5795(3) 0.6313(2) 0.3260(2) 0.0347(9) Uani 1 1 d . A . H35A H 0.6264 0.6604 0.3451 0.042 Uiso 1 1 calc R . . C36 C 0.5554(3) 0.5423(2) 0.3498(2) 0.0280(8) Uani 1 1 d . . . H36A H 0.5854 0.5120 0.3853 0.034 Uiso 1 1 calc R A . C37 C 0.5688(3) 0.3397(2) 0.3808(2) 0.0219(7) Uani 1 1 d . A . C38 C 0.6599(3) 0.3130(2) 0.3244(2) 0.0291(8) Uani 1 1 d . . . H38A H 0.6573 0.3123 0.2743 0.035 Uiso 1 1 calc R A . C39 C 0.7543(3) 0.2876(2) 0.3409(2) 0.0365(9) Uani 1 1 d . A . H39A H 0.8145 0.2703 0.3020 0.044 Uiso 1 1 calc R . . C40 C 0.7587(3) 0.2878(3) 0.4154(3) 0.0411(10) Uani 1 1 d . . . H40A H 0.8219 0.2704 0.4268 0.049 Uiso 1 1 calc R A . C41 C 0.6693(3) 0.3139(2) 0.4728(2) 0.0363(9) Uani 1 1 d . A . H41A H 0.6725 0.3137 0.5229 0.044 Uiso 1 1 calc R . . C42 C 0.5743(3) 0.3405(2) 0.4565(2) 0.0288(8) Uani 1 1 d . . . H42A H 0.5147 0.3587 0.4953 0.035 Uiso 1 1 calc R A . C43 C 0.3433(2) 0.3838(2) 0.44665(18) 0.0202(7) Uani 1 1 d . A . C44 C 0.3140(3) 0.3065(2) 0.4981(2) 0.0252(7) Uani 1 1 d . . . H44A H 0.3497 0.2536 0.4852 0.030 Uiso 1 1 calc R A . C45 C 0.2319(3) 0.3077(2) 0.5687(2) 0.0308(8) Uani 1 1 d . A . H45A H 0.2124 0.2556 0.6024 0.037 Uiso 1 1 calc R . . C46 C 0.1793(3) 0.3863(3) 0.5885(2) 0.0331(8) Uani 1 1 d . . . H46A H 0.1243 0.3870 0.6356 0.040 Uiso 1 1 calc R A . C47 C 0.2079(3) 0.4635(2) 0.5390(2) 0.0318(8) Uani 1 1 d . A . H47A H 0.1729 0.5163 0.5530 0.038 Uiso 1 1 calc R . . C48 C 0.2892(3) 0.4627(2) 0.4676(2) 0.0269(7) Uani 1 1 d . . . H48A H 0.3075 0.5149 0.4340 0.032 Uiso 1 1 calc R A . C49 C 0.1964(3) 0.3200(2) 0.0805(2) 0.0290(8) Uani 1 1 d . A . C50 C 0.2702(3) 0.3461(3) 0.0084(2) 0.0459(11) Uani 1 1 d . . . H50A H 0.3051 0.4012 -0.0013 0.055 Uiso 1 1 calc R A . C51 C 0.2919(4) 0.2899(4) -0.0494(3) 0.0649(15) Uani 1 1 d . A . H51A H 0.3428 0.3069 -0.0973 0.078 Uiso 1 1 calc R . . C52 C 0.2390(5) 0.2093(4) -0.0363(3) 0.0693(16) Uani 1 1 d . . . H52A H 0.2544 0.1720 -0.0753 0.083 Uiso 1 1 calc R A . C53 C 0.1636(4) 0.1835(3) 0.0339(3) 0.0557(13) Uani 1 1 d . A . H53A H 0.1269 0.1294 0.0420 0.067 Uiso 1 1 calc R . . C54 C 0.1419(3) 0.2378(3) 0.0932(2) 0.0369(9) Uani 1 1 d . . . H54A H 0.0914 0.2198 0.1411 0.044 Uiso 1 1 calc R A . C55 C 0.0220(3) 0.4226(2) 0.1674(2) 0.0287(8) Uani 1 1 d . A . C56 C -0.0459(3) 0.4544(3) 0.2341(2) 0.0400(10) Uani 1 1 d . . . H56A H -0.0223 0.4542 0.2771 0.048 Uiso 1 1 calc R A . C57 C -0.1483(3) 0.4862(3) 0.2373(3) 0.0461(11) Uani 1 1 d . A . H57A H -0.1921 0.5075 0.2824 0.055 Uiso 1 1 calc R . . C58 C -0.1858(3) 0.4870(3) 0.1756(3) 0.0489(11) Uani 1 1 d . . . H58A H -0.2541 0.5098 0.1780 0.059 Uiso 1 1 calc R A . C59 C -0.1213(4) 0.4533(4) 0.1095(3) 0.0733(17) Uani 1 1 d . A . H59A H -0.1470 0.4514 0.0676 0.088 Uiso 1 1 calc R . . C60 C -0.0176(4) 0.4223(4) 0.1055(3) 0.0667(16) Uani 1 1 d . . . H60A H 0.0259 0.4010 0.0603 0.080 Uiso 1 1 calc R A . C61 C 0.2393(3) 0.4931(2) 0.1161(2) 0.0306(8) Uani 1 1 d . A . C62 C 0.3491(3) 0.4929(3) 0.1064(3) 0.0464(11) Uani 1 1 d . . . H62A H 0.3808 0.4416 0.1226 0.056 Uiso 1 1 calc R A . C63 C 0.4135(4) 0.5678(3) 0.0730(3) 0.0505(12) Uani 1 1 d . A . H63A H 0.4876 0.5662 0.0672 0.061 Uiso 1 1 calc R . . C64 C 0.3697(4) 0.6431(3) 0.0487(3) 0.0626(14) Uani 1 1 d . . . H64A H 0.4129 0.6933 0.0262 0.075 Uiso 1 1 calc R A . C65 C 0.2606(5) 0.6439(4) 0.0580(4) 0.113(3) Uani 1 1 d . A . H65A H 0.2295 0.6956 0.0421 0.135 Uiso 1 1 calc R . . C66 C 0.1950(4) 0.5689(3) 0.0908(3) 0.0760(19) Uani 1 1 d . . . H66A H 0.1213 0.5704 0.0955 0.091 Uiso 1 1 calc R A . C101 C 0.5006(4) 0.9707(3) 0.2032(3) 0.0557(13) Uani 1 1 d . . . H10A H 0.4757 1.0080 0.2450 0.067 Uiso 1 1 calc R . . H10B H 0.5059 1.0074 0.1551 0.067 Uiso 1 1 calc R . . C102 C 0.8671(11) 0.0704(9) 0.1758(5) 0.267(9) Uani 1 1 d . . . H11B H 0.7955 0.0463 0.2052 0.320 Uiso 1 1 calc R . . H11C H 0.9146 0.0577 0.2075 0.320 Uiso 1 1 calc R . . C104 C -0.0560(7) 0.7393(8) 0.1635(6) 0.184(5) Uani 1 1 d D . . Cl1 Cl 0.40563(12) 0.88548(8) 0.21726(9) 0.0719(4) Uani 1 1 d . . . Cl2 Cl 0.62934(11) 0.92964(9) 0.19985(9) 0.0767(4) Uani 1 1 d . . . Cl3 Cl 0.91832(18) 0.01656(17) 0.08981(18) 0.1447(9) Uani 1 1 d . . . Cl4 Cl 0.85819(16) 0.1868(2) 0.15573(15) 0.1573(12) Uani 1 1 d . . . Cl5 Cl 0.0321(3) 0.7385(3) 0.2232(2) 0.2273(17) Uani 1 1 d D B . Cl6 Cl -0.1706(3) 0.7720(2) 0.22089(15) 0.1150(13) Uani 0.676(4) 1 d PD B 1 Cl6' Cl 0.0179(5) 0.7580(6) 0.0669(4) 0.143(4) Uani 0.324(4) 1 d PD 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 Ir1 0.01588(9) 0.01551(9) 0.01771(10) -0.00180(6) -0.00424(6) -0.00129(6) Rh1 0.01789(9) 0.01562(9) 0.01646(9) -0.00182(6) -0.00493(6) -0.00016(6) Ir2 0.01789(9) 0.01562(9) 0.01646(9) -0.00182(6) -0.00493(6) -0.00016(6) Rh2 0.01588(9) 0.01551(9) 0.01771(10) -0.00180(6) -0.00424(6) -0.00129(6) P1 0.0190(4) 0.0166(4) 0.0210(4) -0.0019(3) -0.0074(3) 0.0003(3) P2 0.0256(4) 0.0233(4) 0.0183(4) -0.0004(3) -0.0064(3) -0.0011(3) O1 0.0319(14) 0.0361(15) 0.0282(14) -0.0008(11) 0.0011(11) -0.0112(11) O2 0.0503(16) 0.0231(14) 0.0385(16) -0.0095(12) -0.0137(13) 0.0018(12) N1 0.0180(13) 0.0177(13) 0.0200(14) -0.0020(11) -0.0051(11) 0.0007(10) N2 0.0194(13) 0.0202(14) 0.0189(14) -0.0024(11) -0.0060(11) 0.0012(10) N3 0.0181(13) 0.0191(13) 0.0190(14) -0.0022(11) -0.0047(11) 0.0000(10) N4 0.0211(13) 0.0184(14) 0.0189(14) -0.0036(11) -0.0026(11) -0.0032(10) N5 0.0197(13) 0.0218(14) 0.0194(14) -0.0029(11) -0.0041(11) -0.0002(11) N6 0.0197(13) 0.0193(14) 0.0214(14) -0.0044(11) -0.0055(11) 0.0003(11) C1 0.0253(17) 0.0216(17) 0.0252(18) -0.0057(14) -0.0110(14) 0.0009(13) C2 0.0245(17) 0.0275(19) 0.0210(17) 0.0003(14) -0.0083(13) 0.0004(14) C3 0.0251(16) 0.0182(16) 0.0195(16) -0.0025(13) -0.0075(13) 0.0018(13) C4 0.0227(16) 0.0178(16) 0.033(2) 0.0015(14) -0.0061(14) -0.0024(13) C5 0.0236(17) 0.0259(19) 0.043(2) -0.0031(16) -0.0100(16) 0.0056(14) C6 0.033(2) 0.0241(19) 0.039(2) -0.0002(16) -0.0114(17) 0.0065(15) C7 0.034(2) 0.0204(18) 0.043(2) 0.0057(16) -0.0061(17) -0.0008(15) C8 0.0224(17) 0.0249(18) 0.037(2) -0.0005(15) -0.0068(15) 0.0001(14) C9 0.044(2) 0.030(2) 0.066(3) 0.003(2) -0.017(2) 0.0113(18) C10 0.0186(15) 0.0268(17) 0.0172(16) 0.0001(13) -0.0049(12) 0.0016(13) C11 0.0234(16) 0.0258(18) 0.0237(18) -0.0039(14) -0.0070(13) 0.0032(13) C12 0.0268(18) 0.039(2) 0.0271(19) -0.0101(16) -0.0075(15) 0.0098(16) C13 0.0197(17) 0.050(2) 0.0229(19) -0.0014(17) -0.0026(14) 0.0047(16) C14 0.0277(19) 0.034(2) 0.034(2) 0.0090(17) 0.0003(16) -0.0027(15) C15 0.0233(17) 0.0274(19) 0.032(2) 0.0014(15) -0.0028(15) 0.0029(14) C16 0.035(2) 0.072(3) 0.037(2) -0.001(2) 0.0045(18) 0.004(2) C17 0.0237(16) 0.0171(16) 0.0221(17) -0.0023(13) 0.0016(13) -0.0011(13) C18 0.0283(18) 0.0300(19) 0.0270(19) -0.0090(15) -0.0035(15) -0.0049(15) C19 0.038(2) 0.031(2) 0.031(2) -0.0115(16) -0.0001(16) -0.0052(16) C20 0.037(2) 0.0270(19) 0.031(2) -0.0067(16) 0.0024(16) 0.0022(16) C21 0.0246(18) 0.0273(19) 0.039(2) -0.0005(16) -0.0025(15) 0.0033(14) C22 0.0240(17) 0.0231(18) 0.031(2) -0.0026(15) -0.0051(14) -0.0021(13) C23 0.049(3) 0.061(3) 0.050(3) -0.026(2) 0.004(2) 0.009(2) C24 0.0225(16) 0.0229(17) 0.0190(16) -0.0031(13) -0.0083(13) -0.0028(13) C25 0.0195(16) 0.0240(18) 0.034(2) -0.0058(15) -0.0048(14) 0.0002(13) C26 0.0194(16) 0.0294(19) 0.040(2) -0.0039(16) -0.0052(15) -0.0039(14) C27 0.0270(18) 0.0285(19) 0.040(2) 0.0030(16) -0.0115(16) -0.0087(15) C28 0.032(2) 0.0205(18) 0.057(3) -0.0023(18) -0.0101(18) -0.0017(15) C29 0.0248(17) 0.0223(18) 0.041(2) -0.0036(16) -0.0057(15) 0.0006(14) C30 0.034(2) 0.040(2) 0.070(3) 0.004(2) -0.011(2) -0.0154(18) C31 0.0194(15) 0.0185(16) 0.0216(17) -0.0033(13) -0.0026(13) -0.0005(12) C32 0.0258(17) 0.0208(17) 0.0243(18) -0.0014(14) -0.0056(14) -0.0010(13) C33 0.036(2) 0.0240(18) 0.0268(19) 0.0014(15) -0.0066(15) 0.0031(15) C34 0.037(2) 0.0190(18) 0.038(2) 0.0003(15) -0.0039(17) -0.0051(15) C35 0.042(2) 0.0260(19) 0.040(2) -0.0036(16) -0.0172(18) -0.0090(16) C36 0.0332(19) 0.0251(18) 0.0279(19) -0.0010(15) -0.0130(15) -0.0038(14) C37 0.0238(16) 0.0152(15) 0.0309(19) -0.0025(13) -0.0145(14) -0.0007(12) C38 0.0275(18) 0.0282(19) 0.034(2) -0.0067(16) -0.0115(15) 0.0019(14) C39 0.0296(19) 0.036(2) 0.049(3) -0.0146(19) -0.0176(18) 0.0082(16) C40 0.035(2) 0.036(2) 0.065(3) -0.011(2) -0.033(2) 0.0062(17) C41 0.043(2) 0.033(2) 0.043(2) -0.0049(18) -0.0282(19) 0.0003(17) C42 0.0310(18) 0.0245(18) 0.035(2) -0.0042(15) -0.0156(16) 0.0031(14) C43 0.0215(15) 0.0204(16) 0.0209(17) -0.0014(13) -0.0099(13) -0.0017(12) C44 0.0307(18) 0.0239(17) 0.0234(18) -0.0021(14) -0.0118(14) -0.0026(14) C45 0.038(2) 0.032(2) 0.0229(18) 0.0045(15) -0.0124(15) -0.0118(16) C46 0.0309(19) 0.043(2) 0.0215(19) -0.0045(16) -0.0022(15) -0.0074(16) C47 0.0324(19) 0.033(2) 0.028(2) -0.0096(16) -0.0047(15) 0.0058(15) C48 0.0307(18) 0.0238(18) 0.0253(18) 0.0000(14) -0.0083(15) 0.0003(14) C49 0.0338(19) 0.037(2) 0.0197(18) -0.0062(15) -0.0123(15) 0.0030(16) C50 0.046(2) 0.063(3) 0.026(2) -0.013(2) -0.0047(18) -0.004(2) C51 0.064(3) 0.097(4) 0.032(3) -0.027(3) -0.004(2) -0.003(3) C52 0.082(4) 0.089(4) 0.049(3) -0.043(3) -0.026(3) 0.012(3) C53 0.080(3) 0.049(3) 0.053(3) -0.021(2) -0.037(3) 0.002(2) C54 0.046(2) 0.039(2) 0.031(2) -0.0080(17) -0.0177(18) -0.0008(18) C55 0.0272(18) 0.0314(19) 0.0274(19) 0.0031(15) -0.0105(15) -0.0012(15) C56 0.0264(19) 0.061(3) 0.037(2) -0.014(2) -0.0130(17) 0.0009(18) C57 0.027(2) 0.064(3) 0.051(3) -0.018(2) -0.0134(19) 0.0059(19) C58 0.032(2) 0.061(3) 0.057(3) 0.001(2) -0.021(2) 0.008(2) C59 0.060(3) 0.124(5) 0.048(3) -0.014(3) -0.036(3) 0.035(3) C60 0.058(3) 0.118(5) 0.035(3) -0.023(3) -0.028(2) 0.037(3) C61 0.039(2) 0.0290(19) 0.0186(18) 0.0002(14) -0.0018(15) -0.0062(15) C62 0.049(2) 0.046(3) 0.048(3) 0.021(2) -0.029(2) -0.017(2) C63 0.053(3) 0.059(3) 0.041(3) 0.013(2) -0.022(2) -0.027(2) C64 0.076(4) 0.037(3) 0.052(3) 0.010(2) 0.009(3) -0.018(2) C65 0.064(4) 0.038(3) 0.173(7) 0.046(4) 0.033(4) 0.008(3) C66 0.044(3) 0.042(3) 0.106(5) 0.034(3) 0.014(3) 0.007(2) C101 0.084(4) 0.029(2) 0.049(3) -0.007(2) -0.012(2) 0.004(2) C102 0.392(18) 0.350(16) 0.103(7) 0.132(9) -0.171(10) -0.305(15) C104 0.094(7) 0.238(13) 0.207(13) 0.056(10) -0.056(8) 0.003(7) Cl1 0.0798(9) 0.0426(7) 0.0940(11) 0.0071(7) -0.0331(8) -0.0029(6) Cl2 0.0633(8) 0.0483(7) 0.0951(11) -0.0240(7) 0.0146(7) -0.0030(6) Cl3 0.1051(16) 0.143(2) 0.195(3) 0.0194(18) -0.0710(17) -0.0213(14) Cl4 0.0820(13) 0.299(4) 0.1213(19) -0.094(2) -0.0510(13) 0.0049(18) Cl5 0.218(4) 0.246(4) 0.200(4) -0.067(3) -0.019(3) -0.065(3) Cl6 0.113(2) 0.169(3) 0.0588(16) 0.0048(17) -0.0279(15) 0.004(2) Cl6' 0.086(4) 0.218(9) 0.113(6) 0.053(5) -0.041(4) 0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.832(4) . ? Ir1 N4 2.130(3) . ? Ir1 N1 2.138(3) . ? Ir1 P1 2.2764(15) . ? Ir1 Rh1 2.9452(7) . ? Rh1 C2 1.827(4) . ? Rh1 N3 2.111(3) . ? Rh1 N6 2.114(3) . ? Rh1 P2 2.2806(15) . ? P1 C37 1.837(3) . ? P1 C31 1.838(3) . ? P1 C43 1.839(4) . ? P2 C61 1.834(4) . ? P2 C49 1.837(4) . ? P2 C55 1.838(4) . ? O1 C1 1.151(4) . ? O2 C2 1.152(4) . ? N1 N2 1.312(4) . ? N1 C3 1.433(4) . ? N2 N3 1.298(3) . ? N3 C10 1.441(4) . ? N4 N5 1.308(4) . ? N4 C17 1.440(4) . ? N5 N6 1.309(4) . ? N6 C24 1.434(4) . ? C3 C4 1.389(4) . ? C3 C8 1.393(5) . ? C4 C5 1.393(4) . ? C5 C6 1.386(5) . ? C6 C7 1.395(5) . ? C6 C9 1.516(5) . ? C7 C8 1.390(5) . ? C10 C15 1.391(5) . ? C10 C11 1.393(4) . ? C11 C12 1.389(5) . ? C12 C13 1.381(5) . ? C13 C14 1.391(5) . ? C13 C16 1.511(5) . ? C14 C15 1.390(5) . ? C17 C22 1.390(4) . ? C17 C18 1.399(5) . ? C18 C19 1.389(5) . ? C19 C20 1.389(5) . ? C20 C21 1.381(5) . ? C20 C23 1.519(5) . ? C21 C22 1.392(5) . ? C24 C29 1.386(4) . ? C24 C25 1.399(4) . ? C25 C26 1.381(5) . ? C26 C27 1.389(5) . ? C27 C28 1.389(5) . ? C27 C30 1.522(5) . ? C28 C29 1.394(5) . ? C31 C32 1.396(5) . ? C31 C36 1.401(5) . ? C32 C33 1.388(5) . ? C33 C34 1.392(5) . ? C34 C35 1.390(5) . ? C35 C36 1.379(5) . ? C37 C38 1.386(5) . ? C37 C42 1.410(5) . ? C38 C39 1.382(5) . ? C39 C40 1.384(6) . ? C40 C41 1.381(6) . ? C41 C42 1.392(5) . ? C43 C44 1.395(5) . ? C43 C48 1.398(4) . ? C44 C45 1.393(5) . ? C45 C46 1.382(5) . ? C46 C47 1.376(5) . ? C47 C48 1.398(5) . ? C49 C50 1.386(5) . ? C49 C54 1.404(5) . ? C50 C51 1.387(6) . ? C51 C52 1.373(7) . ? C52 C53 1.369(7) . ? C53 C54 1.390(6) . ? C55 C60 1.382(5) . ? C55 C56 1.389(5) . ? C56 C57 1.383(5) . ? C57 C58 1.360(6) . ? C58 C59 1.381(7) . ? C59 C60 1.392(6) . ? C61 C66 1.367(6) . ? C61 C62 1.376(5) . ? C62 C63 1.386(6) . ? C63 C64 1.350(6) . ? C64 C65 1.368(8) . ? C65 C66 1.393(7) . ? C101 Cl1 1.744(5) . ? C101 Cl2 1.747(5) . ? C102 Cl4 1.766(13) . ? C102 Cl3 1.785(14) . ? C104 Cl6 1.629(10) . ? C104 Cl6' 1.721(11) . ? C104 Cl5 1.807(9) . ? 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 C1 Ir1 N4 93.67(13) . . ? C1 Ir1 N1 167.49(12) . . ? N4 Ir1 N1 84.58(10) . . ? C1 Ir1 P1 88.34(11) . . ? N4 Ir1 P1 174.35(7) . . ? N1 Ir1 P1 92.31(8) . . ? C1 Ir1 Rh1 115.22(11) . . ? N4 Ir1 Rh1 76.86(9) . . ? N1 Ir1 Rh1 76.50(9) . . ? P1 Ir1 Rh1 107.04(6) . . ? C2 Rh1 N3 96.78(14) . . ? C2 Rh1 N6 177.34(12) . . ? N3 Rh1 N6 82.42(12) . . ? C2 Rh1 P2 87.29(12) . . ? N3 Rh1 P2 167.11(7) . . ? N6 Rh1 P2 94.04(10) . . ? C2 Rh1 Ir1 100.11(12) . . ? N3 Rh1 Ir1 78.69(9) . . ? N6 Rh1 Ir1 77.25(9) . . ? P2 Rh1 Ir1 112.72(7) . . ? C37 P1 C31 101.11(15) . . ? C37 P1 C43 103.09(15) . . ? C31 P1 C43 102.70(16) . . ? C37 P1 Ir1 113.92(12) . . ? C31 P1 Ir1 115.89(12) . . ? C43 P1 Ir1 117.92(11) . . ? C61 P2 C49 103.08(17) . . ? C61 P2 C55 102.38(17) . . ? C49 P2 C55 102.04(17) . . ? C61 P2 Rh1 115.04(14) . . ? C49 P2 Rh1 118.39(12) . . ? C55 P2 Rh1 113.83(13) . . ? N2 N1 C3 110.6(3) . . ? N2 N1 Ir1 128.3(2) . . ? C3 N1 Ir1 120.7(2) . . ? N3 N2 N1 116.3(3) . . ? N2 N3 C10 110.1(3) . . ? N2 N3 Rh1 125.2(2) . . ? C10 N3 Rh1 121.2(2) . . ? N5 N4 C17 109.4(3) . . ? N5 N4 Ir1 124.9(2) . . ? C17 N4 Ir1 123.9(2) . . ? N4 N5 N6 116.4(3) . . ? N5 N6 C24 111.5(3) . . ? N5 N6 Rh1 126.3(2) . . ? C24 N6 Rh1 122.2(2) . . ? O1 C1 Ir1 176.0(3) . . ? O2 C2 Rh1 177.8(3) . . ? C4 C3 C8 119.1(3) . . ? C4 C3 N1 119.4(3) . . ? C8 C3 N1 121.5(3) . . ? C3 C4 C5 119.9(3) . . ? C6 C5 C4 122.0(3) . . ? C5 C6 C7 117.4(3) . . ? C5 C6 C9 121.6(3) . . ? C7 C6 C9 121.0(3) . . ? C8 C7 C6 121.6(3) . . ? C7 C8 C3 120.1(3) . . ? C15 C10 C11 118.9(3) . . ? C15 C10 N3 121.4(3) . . ? C11 C10 N3 119.7(3) . . ? C12 C11 C10 119.9(3) . . ? C13 C12 C11 122.0(3) . . ? C12 C13 C14 117.7(3) . . ? C12 C13 C16 121.6(4) . . ? C14 C13 C16 120.8(4) . . ? C15 C14 C13 121.3(3) . . ? C14 C15 C10 120.2(3) . . ? C22 C17 C18 118.6(3) . . ? C22 C17 N4 121.2(3) . . ? C18 C17 N4 120.3(3) . . ? C19 C18 C17 120.6(3) . . ? C18 C19 C20 121.2(4) . . ? C21 C20 C19 117.6(3) . . ? C21 C20 C23 121.6(4) . . ? C19 C20 C23 120.8(4) . . ? C20 C21 C22 122.4(3) . . ? C17 C22 C21 119.6(3) . . ? C29 C24 C25 118.6(3) . . ? C29 C24 N6 122.4(3) . . ? C25 C24 N6 118.8(3) . . ? C26 C25 C24 120.5(3) . . ? C25 C26 C27 121.8(3) . . ? C26 C27 C28 117.1(3) . . ? C26 C27 C30 121.2(3) . . ? C28 C27 C30 121.7(3) . . ? C27 C28 C29 122.2(3) . . ? C24 C29 C28 119.8(3) . . ? C32 C31 C36 118.6(3) . . ? C32 C31 P1 119.8(2) . . ? C36 C31 P1 121.5(3) . . ? C33 C32 C31 120.8(3) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 119.4(3) . . ? C36 C35 C34 120.8(3) . . ? C35 C36 C31 120.4(3) . . ? C38 C37 C42 118.3(3) . . ? C38 C37 P1 118.9(3) . . ? C42 C37 P1 122.6(3) . . ? C39 C38 C37 121.7(3) . . ? C38 C39 C40 119.7(4) . . ? C41 C40 C39 120.0(3) . . ? C40 C41 C42 120.7(4) . . ? C41 C42 C37 119.7(3) . . ? C44 C43 C48 118.6(3) . . ? C44 C43 P1 119.6(3) . . ? C48 C43 P1 121.7(3) . . ? C45 C44 C43 120.7(3) . . ? C46 C45 C44 119.9(3) . . ? C47 C46 C45 120.3(3) . . ? C46 C47 C48 120.3(3) . . ? C47 C48 C43 120.2(3) . . ? C50 C49 C54 119.2(4) . . ? C50 C49 P2 123.0(3) . . ? C54 C49 P2 117.8(3) . . ? C49 C50 C51 119.9(4) . . ? C52 C51 C50 120.6(5) . . ? C53 C52 C51 120.3(5) . . ? C52 C53 C54 120.3(5) . . ? C53 C54 C49 119.7(4) . . ? C60 C55 C56 117.5(4) . . ? C60 C55 P2 121.7(3) . . ? C56 C55 P2 120.7(3) . . ? C57 C56 C55 120.9(4) . . ? C58 C57 C56 121.2(4) . . ? C57 C58 C59 119.1(4) . . ? C58 C59 C60 119.9(4) . . ? C55 C60 C59 121.4(4) . . ? C66 C61 C62 118.3(4) . . ? C66 C61 P2 124.3(3) . . ? C62 C61 P2 117.4(3) . . ? C61 C62 C63 121.2(4) . . ? C64 C63 C62 120.6(4) . . ? C63 C64 C65 118.6(4) . . ? C64 C65 C66 121.4(5) . . ? C61 C66 C65 119.8(5) . . ? Cl1 C101 Cl2 112.1(2) . . ? Cl4 C102 Cl3 112.4(4) . . ? Cl6 C104 Cl6' 137.3(6) . . ? Cl6 C104 Cl5 101.9(6) . . ? Cl6' C104 Cl5 110.8(5) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.649 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.096 data_4+.[Rh(CO)(PPh3)(mu-RNNNR)2Ir(CO)(PPh3)][PF6].1.5CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.50 H60 Cl3 F6 Ir N6 O2 P3 Rh' _chemical_formula_weight 1595.58 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' 'F' 'F' 0.0171 0.0103 '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' 'Ir' 'Ir' -1.4442 7.9887 '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' _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 12.967(3) _cell_length_b 13.714(2) _cell_length_c 19.830(3) _cell_angle_alpha 97.712(12) _cell_angle_beta 98.499(19) _cell_angle_gamma 90.430(12) _cell_volume 3454.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 142 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour "Dark orange" _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1590 _exptl_absorpt_coefficient_mu 2.412 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.422135 _exptl_absorpt_correction_T_max 0.719334 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29499 _diffrn_reflns_av_R_equivalents 0.1239 _diffrn_reflns_av_sigmaI/netI 0.1873 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12092 _reflns_number_gt 6560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^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 12092 _refine_ls_number_parameters 844 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1494 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.947 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.73773(4) 0.30918(4) 0.24838(3) 0.0184(2) Uani 0.531(3) 1 d P A 1 Rh2 Rh 0.90353(4) 0.18990(4) 0.26047(3) 0.0196(2) Uani 0.469(3) 1 d P A 2 Ir1 Ir 0.90353(4) 0.18990(4) 0.26047(3) 0.0196(2) Uani 0.531(3) 1 d P A 1 Ir2 Ir 0.73773(4) 0.30918(4) 0.24838(3) 0.0184(2) Uani 0.469(3) 1 d P A 2 P1 P 0.9014(2) 0.11201(19) 0.35734(15) 0.0232(7) Uani 1 1 d . . . P2 P 0.6190(2) 0.24781(18) 0.15164(14) 0.0213(6) Uani 1 1 d . . . P6 P 0.6340(3) 1.2590(2) 0.72318(18) 0.0365(8) Uani 1 1 d . . . F1 F 0.5312(6) 1.2619(5) 0.7609(4) 0.066(2) Uani 1 1 d . . . F2 F 0.7372(5) 1.2563(5) 0.6879(4) 0.053(2) Uani 1 1 d . . . F3 F 0.6711(7) 1.1645(5) 0.7569(5) 0.088(3) Uani 1 1 d . . . F4 F 0.6957(6) 1.3246(5) 0.7893(4) 0.065(2) Uani 1 1 d . . . F5 F 0.5752(7) 1.1926(7) 0.6590(5) 0.118(4) Uani 1 1 d . . . F6 F 0.6001(6) 1.3565(6) 0.6923(4) 0.079(3) Uani 1 1 d . . . O1 O 0.8111(6) 0.0086(5) 0.1691(4) 0.038(2) Uani 1 1 d . A . O2 O 0.6187(6) 0.2279(5) 0.3492(4) 0.035(2) Uani 1 1 d . A . N1 N 0.9424(6) 0.2534(6) 0.1758(4) 0.023(2) Uani 1 1 d . . . N2 N 0.9085(7) 0.3374(6) 0.1582(5) 0.027(2) Uani 1 1 d . A . N3 N 0.8341(6) 0.3762(5) 0.1894(4) 0.020(2) Uani 1 1 d . . . N4 N 0.9720(7) 0.3212(5) 0.3171(4) 0.021(2) Uani 1 1 d . . . N5 N 0.9251(6) 0.3929(5) 0.3491(4) 0.021(2) Uani 1 1 d . A . N6 N 0.8252(6) 0.3907(5) 0.3355(4) 0.020(2) Uani 1 1 d . . . C1 C 0.8463(8) 0.0760(8) 0.2050(5) 0.023(3) Uani 1 1 d . . . C2 C 0.6596(9) 0.2577(7) 0.3080(6) 0.033(3) Uani 1 1 d . . . C3 C 0.8842(8) 0.1841(7) 0.4382(6) 0.026(3) Uani 1 1 d . A . C4 C 0.7981(10) 0.1679(8) 0.4698(7) 0.045(3) Uani 1 1 d . . . H4A H 0.7481 0.1181 0.4483 0.055 Uiso 1 1 calc R A . C5 C 0.7821(11) 0.2224(8) 0.5325(6) 0.051(4) Uani 1 1 d . A . H5B H 0.7230 0.2092 0.5533 0.061 Uiso 1 1 calc R . . C6 C 0.8545(10) 0.2957(8) 0.5633(6) 0.043(3) Uani 1 1 d . . . H6A H 0.8451 0.3337 0.6055 0.052 Uiso 1 1 calc R A . C7 C 0.9400(10) 0.3136(8) 0.5327(6) 0.041(3) Uani 1 1 d . A . H7A H 0.9897 0.3635 0.5546 0.049 Uiso 1 1 calc R . . C8 C 0.9554(9) 0.2599(7) 0.4700(6) 0.030(3) Uani 1 1 d . . . H8A H 1.0139 0.2746 0.4490 0.036 Uiso 1 1 calc R A . C9 C 0.8180(8) 0.0019(7) 0.3515(5) 0.023(3) Uani 1 1 d . A . C10 C 0.7171(9) -0.0051(7) 0.3128(6) 0.032(3) Uani 1 1 d . . . H10A H 0.6922 0.0476 0.2888 0.039 Uiso 1 1 calc R A . C11 C 0.6538(9) -0.0887(7) 0.3095(6) 0.035(3) Uani 1 1 d . A . H11A H 0.5858 -0.0932 0.2835 0.042 Uiso 1 1 calc R . . C12 C 0.6910(10) -0.1652(7) 0.3445(6) 0.035(3) Uani 1 1 d . . . H12A H 0.6484 -0.2226 0.3421 0.042 Uiso 1 1 calc R A . C13 C 0.7890(10) -0.1592(7) 0.3827(6) 0.038(3) Uani 1 1 d . A . H13A H 0.8133 -0.2119 0.4067 0.046 Uiso 1 1 calc R . . C14 C 0.8521(9) -0.0761(7) 0.3862(6) 0.032(3) Uani 1 1 d . . . H14A H 0.9197 -0.0726 0.4126 0.038 Uiso 1 1 calc R A . C15 C 1.0306(8) 0.0609(7) 0.3700(6) 0.024(3) Uani 1 1 d . A . C16 C 1.1023(9) 0.0821(8) 0.4284(6) 0.034(3) Uani 1 1 d . . . H16A H 1.0838 0.1219 0.4676 0.041 Uiso 1 1 calc R A . C17 C 1.2034(9) 0.0449(9) 0.4302(7) 0.048(4) Uani 1 1 d U A . H17A H 1.2527 0.0591 0.4710 0.058 Uiso 1 1 calc R . . C18 C 1.2318(10) -0.0128(9) 0.3725(7) 0.052(4) Uani 1 1 d . . . H18A H 1.3009 -0.0360 0.3736 0.062 Uiso 1 1 calc R A . C19 C 1.1600(9) -0.0358(8) 0.3147(7) 0.044(3) Uani 1 1 d . A . H19A H 1.1786 -0.0762 0.2758 0.053 Uiso 1 1 calc R . . C20 C 1.0595(9) -0.0002(7) 0.3127(6) 0.032(3) Uani 1 1 d . . . H20A H 1.0097 -0.0172 0.2725 0.039 Uiso 1 1 calc R A . C21 C 0.5079(8) 0.3287(7) 0.1501(5) 0.022(3) Uani 1 1 d . A . C22 C 0.5290(8) 0.4313(7) 0.1634(5) 0.024(3) Uani 1 1 d . . . H22A H 0.5990 0.4561 0.1738 0.029 Uiso 1 1 calc R A . C23 C 0.4471(10) 0.4953(8) 0.1612(6) 0.037(3) Uani 1 1 d . A . H23A H 0.4621 0.5641 0.1717 0.044 Uiso 1 1 calc R . . C24 C 0.3445(10) 0.4631(9) 0.1444(7) 0.049(4) Uani 1 1 d . . . H24A H 0.2895 0.5083 0.1408 0.059 Uiso 1 1 calc R A . C25 C 0.3244(9) 0.3632(9) 0.1332(7) 0.053(4) Uani 1 1 d . A . H25A H 0.2541 0.3395 0.1252 0.063 Uiso 1 1 calc R . . C26 C 0.4040(9) 0.2958(8) 0.1332(6) 0.043(3) Uani 1 1 d . . . H26A H 0.3877 0.2274 0.1217 0.052 Uiso 1 1 calc R A . C27 C 0.6588(8) 0.2470(7) 0.0670(5) 0.023(3) Uani 1 1 d . A . C28 C 0.7503(8) 0.1993(7) 0.0541(6) 0.028(3) Uani 1 1 d . . . H28A H 0.7898 0.1676 0.0887 0.033 Uiso 1 1 calc R A . C29 C 0.7833(10) 0.1988(8) -0.0104(6) 0.039(3) Uani 1 1 d . A . H29A H 0.8446 0.1654 -0.0198 0.047 Uiso 1 1 calc R . . C30 C 0.7277(10) 0.2460(8) -0.0595(6) 0.042(3) Uani 1 1 d . . . H30A H 0.7509 0.2460 -0.1027 0.051 Uiso 1 1 calc R A . C31 C 0.6375(11) 0.2942(8) -0.0468(6) 0.048(4) Uani 1 1 d . A . H31A H 0.5989 0.3266 -0.0814 0.057 Uiso 1 1 calc R . . C32 C 0.6035(9) 0.2950(7) 0.0166(6) 0.033(3) Uani 1 1 d . . . H32A H 0.5421 0.3287 0.0254 0.040 Uiso 1 1 calc R A . C33 C 0.5596(8) 0.1250(7) 0.1495(5) 0.022(3) Uani 1 1 d . A . C34 C 0.5005(9) 0.1093(7) 0.2007(6) 0.032(3) Uani 1 1 d . . . H34A H 0.4934 0.1610 0.2365 0.038 Uiso 1 1 calc R A . C35 C 0.4522(8) 0.0186(8) 0.1992(6) 0.034(3) Uani 1 1 d . A . H35A H 0.4117 0.0086 0.2340 0.041 Uiso 1 1 calc R . . C36 C 0.4623(8) -0.0580(8) 0.1473(6) 0.033(3) Uani 1 1 d . . . H36A H 0.4297 -0.1205 0.1465 0.040 Uiso 1 1 calc R A . C37 C 0.5207(8) -0.0413(7) 0.0974(6) 0.030(3) Uani 1 1 d . A . H37A H 0.5276 -0.0934 0.0618 0.036 Uiso 1 1 calc R . . C38 C 0.5701(8) 0.0491(7) 0.0969(6) 0.027(3) Uani 1 1 d . . . H38A H 0.6100 0.0588 0.0617 0.032 Uiso 1 1 calc R A . C39 C 1.0199(9) 0.2090(7) 0.1356(6) 0.032(3) Uani 1 1 d . A . C40 C 1.0781(8) 0.1335(7) 0.1592(6) 0.031(3) Uani 1 1 d . . . H40A H 1.0690 0.1116 0.2015 0.038 Uiso 1 1 calc R A . C41 C 1.1512(9) 0.0893(8) 0.1200(6) 0.038(3) Uani 1 1 d . A . H41A H 1.1905 0.0366 0.1360 0.046 Uiso 1 1 calc R . . C42 C 1.1673(9) 0.1194(7) 0.0603(6) 0.029(3) Uani 1 1 d . . . C43 C 1.2484(10) 0.0731(8) 0.0185(6) 0.044(3) Uani 1 1 d . A . H43A H 1.2854 0.0230 0.0429 0.067 Uiso 1 1 calc R . . H43B H 1.2983 0.1241 0.0125 0.067 Uiso 1 1 calc R . . H43C H 1.2137 0.0424 -0.0267 0.067 Uiso 1 1 calc R . . C44 C 1.1094(9) 0.1950(8) 0.0367(6) 0.033(3) Uani 1 1 d . A . H44A H 1.1189 0.2157 -0.0059 0.039 Uiso 1 1 calc R . . C45 C 1.0359(8) 0.2421(7) 0.0751(5) 0.028(3) Uani 1 1 d . . . H45A H 0.9981 0.2958 0.0595 0.034 Uiso 1 1 calc R A . C46 C 1.0820(8) 0.3410(7) 0.3192(5) 0.024(3) Uani 1 1 d . A . C47 C 1.1510(8) 0.2652(7) 0.3195(6) 0.027(3) Uani 1 1 d . . . H47A H 1.1263 0.1998 0.3195 0.032 Uiso 1 1 calc R A . C48 C 1.2572(8) 0.2842(8) 0.3199(6) 0.033(3) Uani 1 1 d . A . H48A H 1.3035 0.2308 0.3178 0.040 Uiso 1 1 calc R . . C49 C 1.2964(9) 0.3793(8) 0.3231(6) 0.031(3) Uani 1 1 d . . . C50 C 1.4127(9) 0.4008(9) 0.3265(6) 0.047(3) Uani 1 1 d . A . H50A H 1.4337 0.4594 0.3599 0.070 Uiso 1 1 calc R . . H50B H 1.4270 0.4124 0.2810 0.070 Uiso 1 1 calc R . . H50C H 1.4522 0.3444 0.3407 0.070 Uiso 1 1 calc R . . C51 C 1.2258(9) 0.4533(8) 0.3226(6) 0.038(3) Uani 1 1 d . A . H51A H 1.2509 0.5189 0.3243 0.046 Uiso 1 1 calc R . . C52 C 1.1194(9) 0.4368(8) 0.3198(6) 0.033(3) Uani 1 1 d . . . H52A H 1.0729 0.4898 0.3184 0.040 Uiso 1 1 calc R A . C53 C 0.7765(8) 0.4656(7) 0.3779(5) 0.022(3) Uani 1 1 d . A . C54 C 0.8238(8) 0.5055(7) 0.4436(5) 0.022(3) Uani 1 1 d . . . H54A H 0.8888 0.4813 0.4624 0.027 Uiso 1 1 calc R A . C55 C 0.7775(9) 0.5796(7) 0.4816(6) 0.034(3) Uani 1 1 d . A . H55A H 0.8122 0.6073 0.5257 0.041 Uiso 1 1 calc R . . C56 C 0.6796(9) 0.6152(7) 0.4563(5) 0.028(3) Uani 1 1 d . . . C57 C 0.6253(10) 0.6952(8) 0.4965(6) 0.050(4) Uani 1 1 d . A . H57A H 0.5506 0.6923 0.4783 0.074 Uiso 1 1 calc R . . H57B H 0.6550 0.7595 0.4922 0.074 Uiso 1 1 calc R . . H57C H 0.6348 0.6856 0.5451 0.074 Uiso 1 1 calc R . . C58 C 0.6330(8) 0.5728(7) 0.3918(6) 0.026(3) Uani 1 1 d . A . H58A H 0.5674 0.5958 0.3732 0.032 Uiso 1 1 calc R . . C59 C 0.6791(8) 0.4967(7) 0.3527(5) 0.021(2) Uani 1 1 d . . . H59A H 0.6436 0.4671 0.3093 0.025 Uiso 1 1 calc R A . C60 C 0.8045(8) 0.4686(7) 0.1671(6) 0.023(3) Uani 1 1 d . A . C61 C 0.7814(8) 0.4773(7) 0.0966(6) 0.026(3) Uani 1 1 d . . . H61A H 0.7922 0.4236 0.0630 0.031 Uiso 1 1 calc R A . C62 C 0.7424(9) 0.5652(8) 0.0762(7) 0.040(3) Uani 1 1 d . A . H62A H 0.7263 0.5707 0.0286 0.048 Uiso 1 1 calc R . . C63 C 0.7271(9) 0.6446(8) 0.1247(7) 0.038(3) Uani 1 1 d . . . C64 C 0.6821(11) 0.7389(8) 0.1016(7) 0.061(4) Uani 1 1 d . A . H64A H 0.7381 0.7890 0.1069 0.091 Uiso 1 1 calc R . . H64B H 0.6291 0.7625 0.1299 0.091 Uiso 1 1 calc R . . H64C H 0.6503 0.7259 0.0532 0.091 Uiso 1 1 calc R . . C65 C 0.7511(9) 0.6340(8) 0.1930(6) 0.036(3) Uani 1 1 d . A . H65A H 0.7403 0.6878 0.2265 0.043 Uiso 1 1 calc R . . C66 C 0.7907(9) 0.5475(7) 0.2155(6) 0.032(3) Uani 1 1 d . . . H66A H 0.8078 0.5431 0.2632 0.038 Uiso 1 1 calc R A . C102 C 1.042(2) 0.6361(14) 0.1450(12) 0.137(12) Uani 0.632(7) 1 d PDU B 1 H15A H 1.1032 0.6281 0.1796 0.164 Uiso 0.632(7) 1 calc PR B 1 H15B H 0.9819 0.6037 0.1599 0.164 Uiso 0.632(7) 1 calc PR B 1 C101 C 1.034(3) 0.7065(19) 0.2062(11) 0.056(11) Uani 0.368(7) 1 d PDU B 2 H20B H 0.9978 0.6453 0.1811 0.068 Uiso 0.368(7) 1 calc PR B 2 H20C H 1.1090 0.6938 0.2158 0.068 Uiso 0.368(7) 1 calc PR B 2 C100 C 0.497(3) 1.0512(14) 0.5266(16) 0.077(10) Uiso 0.50 1 d PD . . Cl5 Cl 1.0157(16) 0.7675(14) 0.1539(10) 0.174(8) Uani 0.632(7) 1 d PD B 1 Cl6 Cl 1.0642(6) 0.5639(8) 0.0663(5) 0.141(4) Uani 0.632(7) 1 d PD B 1 Cl4 Cl 1.014(2) 0.8035(16) 0.1528(8) 0.075(6) Uani 0.368(7) 1 d PD B 2 Cl3 Cl 0.9848(7) 0.7378(7) 0.2848(4) 0.056(3) Uani 0.368(7) 1 d PD B 2 Cl1 Cl 0.478(2) 0.9254(16) 0.534(2) 0.069(11) Uiso 0.23(4) 1 d PD . 1 Cl1' Cl 0.4840(8) 0.9438(10) 0.5583(8) 0.176(7) Uani 0.77(4) 1 d PD . 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 Rh1 0.0149(4) 0.0177(4) 0.0228(4) 0.0023(3) 0.0040(3) 0.0006(2) Rh2 0.0180(4) 0.0189(3) 0.0227(4) 0.0034(3) 0.0049(3) 0.0014(2) Ir1 0.0180(4) 0.0189(3) 0.0227(4) 0.0034(3) 0.0049(3) 0.0014(2) Ir2 0.0149(4) 0.0177(4) 0.0228(4) 0.0023(3) 0.0040(3) 0.0006(2) P1 0.0224(17) 0.0212(15) 0.0264(18) 0.0034(13) 0.0050(14) 0.0000(12) P2 0.0204(16) 0.0204(14) 0.0226(17) 0.0043(12) 0.0005(13) 0.0010(12) P6 0.037(2) 0.0296(17) 0.044(2) 0.0008(15) 0.0139(17) -0.0025(15) F1 0.053(5) 0.043(4) 0.112(7) -0.003(4) 0.057(5) -0.004(4) F2 0.044(5) 0.068(5) 0.057(5) 0.016(4) 0.032(4) 0.000(4) F3 0.113(8) 0.038(4) 0.142(9) 0.035(5) 0.091(7) 0.034(5) F4 0.054(5) 0.076(5) 0.057(5) -0.010(4) 0.004(4) 0.010(4) F5 0.055(6) 0.158(9) 0.114(8) -0.088(7) 0.020(6) -0.049(6) F6 0.062(6) 0.095(6) 0.095(7) 0.065(5) 0.012(5) 0.024(5) O1 0.040(5) 0.033(5) 0.034(5) -0.002(4) -0.006(4) -0.003(4) O2 0.033(5) 0.035(5) 0.039(5) 0.010(4) 0.011(4) -0.003(4) N1 0.016(5) 0.029(5) 0.023(5) 0.002(4) 0.002(4) 0.004(4) N2 0.024(6) 0.020(5) 0.041(6) 0.010(4) 0.011(5) -0.001(4) N3 0.013(5) 0.018(4) 0.027(5) -0.006(4) 0.005(4) 0.004(4) N4 0.029(5) 0.015(4) 0.019(5) -0.003(4) 0.009(4) -0.002(4) N5 0.014(5) 0.025(5) 0.023(5) 0.004(4) 0.005(4) -0.004(4) N6 0.014(5) 0.021(5) 0.027(6) 0.010(4) 0.003(4) 0.000(4) C1 0.023(6) 0.031(6) 0.018(6) 0.008(5) 0.012(5) 0.012(5) C2 0.034(8) 0.022(6) 0.041(8) 0.000(6) 0.001(6) 0.006(5) C3 0.022(6) 0.025(6) 0.032(7) 0.004(5) 0.005(5) -0.007(5) C4 0.046(9) 0.029(7) 0.058(10) -0.004(6) 0.009(7) -0.007(6) C5 0.065(10) 0.048(8) 0.045(9) -0.010(7) 0.043(8) -0.007(7) C6 0.061(10) 0.048(8) 0.021(7) -0.009(6) 0.021(7) -0.017(7) C7 0.056(9) 0.027(6) 0.031(8) -0.006(6) -0.009(7) -0.006(6) C8 0.033(7) 0.029(6) 0.031(7) 0.008(5) 0.006(6) -0.009(5) C9 0.029(7) 0.025(6) 0.015(6) -0.002(5) 0.007(5) -0.001(5) C10 0.045(8) 0.024(6) 0.029(7) 0.006(5) 0.007(6) -0.005(5) C11 0.035(8) 0.030(7) 0.038(8) -0.002(6) 0.001(6) -0.006(5) C12 0.056(9) 0.020(6) 0.031(7) 0.003(5) 0.010(7) -0.002(6) C13 0.048(9) 0.025(6) 0.045(8) 0.020(6) 0.007(7) 0.001(6) C14 0.030(7) 0.029(6) 0.035(7) 0.002(5) 0.000(6) -0.006(5) C15 0.023(7) 0.023(6) 0.033(7) 0.016(5) 0.011(6) -0.003(5) C16 0.025(7) 0.040(7) 0.037(8) 0.005(6) 0.006(6) 0.005(5) C17 0.037(8) 0.057(8) 0.041(9) 0.006(7) -0.028(7) 0.014(7) C18 0.035(8) 0.058(9) 0.061(10) 0.006(8) 0.002(8) 0.021(7) C19 0.034(8) 0.046(8) 0.052(9) 0.003(7) 0.010(7) 0.014(6) C20 0.039(8) 0.034(7) 0.027(7) 0.012(5) 0.008(6) 0.014(6) C21 0.018(6) 0.019(6) 0.027(7) 0.003(5) -0.006(5) 0.004(5) C22 0.022(6) 0.028(6) 0.023(7) 0.002(5) 0.005(5) 0.001(5) C23 0.049(9) 0.019(6) 0.040(8) 0.007(5) -0.003(7) 0.008(6) C24 0.035(9) 0.034(7) 0.075(11) 0.001(7) 0.005(8) 0.003(6) C25 0.017(7) 0.051(8) 0.085(11) -0.003(8) 0.003(7) 0.002(6) C26 0.038(8) 0.023(6) 0.062(9) -0.005(6) -0.004(7) 0.009(6) C27 0.026(7) 0.017(5) 0.024(7) -0.001(5) -0.006(5) -0.003(5) C28 0.028(7) 0.030(6) 0.025(7) 0.009(5) 0.001(5) -0.005(5) C29 0.051(9) 0.043(7) 0.021(7) -0.002(6) -0.002(6) -0.007(6) C30 0.052(9) 0.048(8) 0.034(8) 0.011(6) 0.027(7) -0.015(7) C31 0.078(11) 0.042(8) 0.019(7) 0.014(6) -0.015(7) -0.022(7) C32 0.039(8) 0.035(7) 0.026(8) 0.012(6) -0.002(6) -0.005(6) C33 0.023(6) 0.019(6) 0.020(6) 0.001(5) -0.012(5) 0.004(5) C34 0.030(7) 0.025(6) 0.042(8) 0.004(5) 0.014(6) -0.005(5) C35 0.026(7) 0.041(7) 0.038(8) 0.001(6) 0.017(6) -0.009(6) C36 0.023(7) 0.035(7) 0.041(8) 0.009(6) -0.003(6) -0.009(5) C37 0.027(7) 0.019(6) 0.043(8) 0.006(5) 0.005(6) 0.004(5) C38 0.027(7) 0.023(6) 0.031(7) 0.005(5) 0.003(5) 0.006(5) C39 0.035(7) 0.026(6) 0.036(8) -0.001(5) 0.018(6) 0.002(5) C40 0.028(7) 0.034(7) 0.033(8) 0.006(6) 0.006(6) 0.008(5) C41 0.043(8) 0.040(7) 0.034(8) 0.005(6) 0.014(6) 0.013(6) C42 0.034(7) 0.025(6) 0.029(7) 0.002(5) 0.006(6) 0.008(5) C43 0.054(9) 0.043(7) 0.040(8) 0.002(6) 0.025(7) 0.011(6) C44 0.034(7) 0.041(7) 0.026(7) 0.010(6) 0.012(6) -0.002(6) C45 0.028(7) 0.027(6) 0.037(8) 0.012(5) 0.023(6) 0.002(5) C46 0.024(7) 0.020(6) 0.026(7) -0.002(5) 0.004(5) -0.006(5) C47 0.013(6) 0.025(6) 0.046(8) 0.010(5) 0.013(5) -0.004(5) C48 0.014(6) 0.030(6) 0.054(8) 0.006(6) 0.003(6) 0.009(5) C49 0.023(7) 0.032(7) 0.032(7) -0.006(5) 0.000(6) -0.001(5) C50 0.025(7) 0.056(8) 0.059(9) -0.006(7) 0.016(7) -0.003(6) C51 0.027(7) 0.029(6) 0.060(9) 0.008(6) 0.011(6) -0.005(5) C52 0.029(7) 0.028(6) 0.046(8) 0.010(6) 0.010(6) 0.005(5) C53 0.018(6) 0.024(6) 0.026(7) 0.002(5) 0.014(5) -0.002(5) C54 0.011(6) 0.035(6) 0.018(6) 0.000(5) -0.002(5) 0.007(5) C55 0.033(7) 0.031(6) 0.035(8) -0.008(5) 0.000(6) -0.001(5) C56 0.038(7) 0.032(6) 0.017(7) -0.004(5) 0.017(6) -0.007(5) C57 0.059(9) 0.034(7) 0.054(9) -0.015(6) 0.022(8) 0.012(6) C58 0.022(6) 0.021(6) 0.040(8) 0.006(5) 0.016(6) 0.006(5) C59 0.021(6) 0.027(6) 0.015(6) 0.001(5) 0.002(5) -0.007(5) C60 0.022(6) 0.019(6) 0.032(7) 0.007(5) 0.015(5) 0.014(5) C61 0.021(6) 0.028(6) 0.033(7) 0.008(5) 0.012(5) 0.007(5) C62 0.043(8) 0.032(7) 0.051(9) 0.019(6) 0.016(7) 0.002(6) C63 0.031(7) 0.024(6) 0.064(10) 0.020(6) 0.009(7) 0.005(5) C64 0.067(11) 0.043(8) 0.078(11) 0.029(8) 0.012(9) 0.021(7) C65 0.034(8) 0.036(7) 0.042(8) 0.011(6) 0.016(6) 0.004(6) C66 0.040(8) 0.023(6) 0.038(8) 0.010(5) 0.018(6) 0.004(5) C102 0.083(18) 0.142(19) 0.19(2) 0.067(17) 0.005(16) -0.055(15) C101 0.059(19) 0.072(18) 0.038(17) 0.030(15) -0.010(15) -0.010(15) Cl5 0.088(12) 0.235(19) 0.184(15) -0.023(13) 0.019(10) -0.046(13) Cl6 0.062(6) 0.202(10) 0.162(10) 0.061(8) -0.001(6) -0.034(6) Cl4 0.094(14) 0.109(11) 0.019(7) 0.020(7) -0.015(7) 0.030(10) Cl3 0.046(6) 0.080(7) 0.033(6) -0.013(5) -0.001(5) -0.032(5) Cl1' 0.094(6) 0.258(15) 0.155(10) -0.093(11) 0.067(7) -0.095(9) _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 1.868(13) . ? Rh1 N6 2.098(8) . ? Rh1 N3 2.116(8) . ? Rh1 P2 2.331(3) . ? Rh2 C1 1.865(11) . ? Rh2 N4 2.105(8) . ? Rh2 N1 2.113(8) . ? Rh2 P1 2.323(3) . ? P1 C3 1.812(11) . ? P1 C15 1.816(11) . ? P1 C9 1.832(10) . ? P2 C21 1.824(10) . ? P2 C27 1.827(11) . ? P2 C33 1.839(10) . ? P6 F5 1.556(8) . ? P6 F6 1.582(7) . ? P6 F3 1.583(8) . ? P6 F4 1.592(8) . ? P6 F2 1.597(7) . ? P6 F1 1.620(7) . ? O1 C1 1.137(11) . ? O2 C2 1.152(12) . ? N1 N2 1.309(10) . ? N1 C39 1.459(12) . ? N2 N3 1.301(10) . ? N3 C60 1.434(11) . ? N4 N5 1.303(10) . ? N4 C46 1.443(12) . ? N5 N6 1.283(10) . ? N6 C53 1.447(12) . ? C3 C4 1.390(15) . ? C3 C8 1.402(13) . ? C4 C5 1.405(15) . ? C5 C6 1.384(16) . ? C6 C7 1.376(15) . ? C7 C8 1.399(14) . ? C9 C14 1.389(14) . ? C9 C10 1.411(14) . ? C10 C11 1.394(14) . ? C11 C12 1.386(14) . ? C12 C13 1.375(15) . ? C13 C14 1.385(14) . ? C15 C16 1.370(15) . ? C15 C20 1.417(13) . ? C16 C17 1.408(15) . ? C17 C18 1.400(16) . ? C18 C19 1.365(16) . ? C19 C20 1.392(15) . ? C21 C26 1.395(14) . ? C21 C22 1.413(13) . ? C22 C23 1.383(14) . ? C23 C24 1.377(16) . ? C24 C25 1.374(15) . ? C25 C26 1.391(14) . ? C27 C32 1.384(13) . ? C27 C28 1.398(14) . ? C28 C29 1.407(14) . ? C29 C30 1.361(15) . ? C30 C31 1.385(17) . ? C31 C32 1.392(15) . ? C33 C38 1.394(13) . ? C33 C34 1.396(14) . ? C34 C35 1.383(14) . ? C35 C36 1.389(14) . ? C36 C37 1.373(14) . ? C37 C38 1.394(13) . ? C39 C40 1.378(14) . ? C39 C45 1.381(14) . ? C40 C41 1.403(14) . ? C41 C42 1.349(14) . ? C42 C44 1.376(14) . ? C42 C43 1.524(14) . ? C44 C45 1.413(13) . ? C46 C47 1.376(13) . ? C46 C52 1.395(13) . ? C47 C48 1.400(13) . ? C48 C49 1.386(14) . ? C49 C51 1.371(14) . ? C49 C50 1.524(14) . ? C51 C52 1.388(14) . ? C53 C59 1.381(13) . ? C53 C54 1.393(13) . ? C54 C55 1.379(13) . ? C55 C56 1.410(15) . ? C56 C58 1.379(14) . ? C56 C57 1.509(13) . ? C58 C59 1.405(12) . ? C60 C66 1.378(13) . ? C60 C61 1.406(14) . ? C61 C62 1.398(13) . ? C62 C63 1.388(15) . ? C63 C65 1.373(15) . ? C63 C64 1.520(14) . ? C65 C66 1.398(14) . ? C102 Cl6 1.796(13) . ? C102 Cl5 1.826(12) . ? C101 Cl3 1.768(13) . ? C101 Cl4 1.805(13) . ? C100 Cl1 1.37(4) 2_676 ? C100 C100 1.65(5) 2_676 ? C100 Cl1' 1.693(17) . ? C100 Cl1' 1.75(3) 2_676 ? C100 Cl1 1.769(19) . ? Cl1 C100 1.37(4) 2_676 ? Cl1' C100 1.75(3) 2_676 ? 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 N6 87.6(4) . . ? C2 Rh1 N3 174.4(4) . . ? N6 Rh1 N3 86.9(3) . . ? C2 Rh1 P2 92.5(4) . . ? N6 Rh1 P2 167.9(2) . . ? N3 Rh1 P2 92.8(2) . . ? C1 Rh2 N4 176.1(4) . . ? C1 Rh2 N1 93.0(4) . . ? N4 Rh2 N1 83.2(3) . . ? C1 Rh2 P1 89.7(3) . . ? N4 Rh2 P1 93.9(2) . . ? N1 Rh2 P1 166.7(2) . . ? C3 P1 C15 106.8(5) . . ? C3 P1 C9 104.6(5) . . ? C15 P1 C9 101.5(5) . . ? C3 P1 Rh2 119.5(3) . . ? C15 P1 Rh2 102.9(3) . . ? C9 P1 Rh2 119.4(3) . . ? C21 P2 C27 104.1(5) . . ? C21 P2 C33 103.5(5) . . ? C27 P2 C33 105.0(5) . . ? C21 P2 Rh1 106.6(3) . . ? C27 P2 Rh1 118.2(3) . . ? C33 P2 Rh1 117.7(3) . . ? F5 P6 F6 92.2(6) . . ? F5 P6 F3 90.4(6) . . ? F6 P6 F3 177.3(6) . . ? F5 P6 F4 178.6(6) . . ? F6 P6 F4 89.1(4) . . ? F3 P6 F4 88.3(5) . . ? F5 P6 F2 90.1(4) . . ? F6 P6 F2 90.6(4) . . ? F3 P6 F2 89.2(4) . . ? F4 P6 F2 89.4(4) . . ? F5 P6 F1 91.2(5) . . ? F6 P6 F1 90.2(4) . . ? F3 P6 F1 90.0(4) . . ? F4 P6 F1 89.3(4) . . ? F2 P6 F1 178.5(5) . . ? N2 N1 C39 114.1(8) . . ? N2 N1 Rh2 124.9(6) . . ? C39 N1 Rh2 120.7(6) . . ? N3 N2 N1 116.2(8) . . ? N2 N3 C60 111.4(8) . . ? N2 N3 Rh1 128.5(6) . . ? C60 N3 Rh1 118.8(6) . . ? N5 N4 C46 113.3(7) . . ? N5 N4 Rh2 127.3(7) . . ? C46 N4 Rh2 119.3(6) . . ? N6 N5 N4 116.0(8) . . ? N5 N6 C53 113.7(8) . . ? N5 N6 Rh1 124.8(6) . . ? C53 N6 Rh1 120.4(6) . . ? O1 C1 Rh2 177.3(9) . . ? O2 C2 Rh1 174.0(11) . . ? C4 C3 C8 117.7(10) . . ? C4 C3 P1 120.9(8) . . ? C8 C3 P1 121.3(8) . . ? C3 C4 C5 122.5(11) . . ? C6 C5 C4 118.5(11) . . ? C7 C6 C5 120.0(11) . . ? C6 C7 C8 121.4(11) . . ? C7 C8 C3 119.8(11) . . ? C14 C9 C10 118.4(10) . . ? C14 C9 P1 120.6(8) . . ? C10 C9 P1 121.0(8) . . ? C11 C10 C9 120.4(10) . . ? C12 C11 C10 119.3(11) . . ? C13 C12 C11 120.8(11) . . ? C12 C13 C14 120.1(10) . . ? C13 C14 C9 120.9(11) . . ? C16 C15 C20 118.9(10) . . ? C16 C15 P1 124.9(8) . . ? C20 C15 P1 116.1(8) . . ? C15 C16 C17 119.9(11) . . ? C18 C17 C16 120.5(11) . . ? C19 C18 C17 119.7(11) . . ? C18 C19 C20 120.1(12) . . ? C19 C20 C15 120.8(11) . . ? C26 C21 C22 118.2(9) . . ? C26 C21 P2 124.1(7) . . ? C22 C21 P2 117.6(8) . . ? C23 C22 C21 119.5(10) . . ? C24 C23 C22 122.4(10) . . ? C25 C24 C23 117.8(11) . . ? C24 C25 C26 122.0(12) . . ? C25 C26 C21 120.0(10) . . ? C32 C27 C28 119.5(11) . . ? C32 C27 P2 122.0(8) . . ? C28 C27 P2 118.5(8) . . ? C27 C28 C29 119.5(11) . . ? C30 C29 C28 120.2(12) . . ? C29 C30 C31 120.6(12) . . ? C30 C31 C32 119.9(12) . . ? C27 C32 C31 120.3(12) . . ? C38 C33 C34 119.9(10) . . ? C38 C33 P2 121.2(8) . . ? C34 C33 P2 118.8(8) . . ? C35 C34 C33 120.1(10) . . ? C34 C35 C36 120.7(11) . . ? C37 C36 C35 118.5(10) . . ? C36 C37 C38 122.6(10) . . ? C37 C38 C33 118.2(10) . . ? C40 C39 C45 120.0(10) . . ? C40 C39 N1 119.0(10) . . ? C45 C39 N1 121.1(9) . . ? C39 C40 C41 119.1(11) . . ? C42 C41 C40 122.0(11) . . ? C41 C42 C44 119.0(10) . . ? C41 C42 C43 122.0(10) . . ? C44 C42 C43 119.0(10) . . ? C42 C44 C45 120.7(10) . . ? C39 C45 C44 119.2(10) . . ? C47 C46 C52 119.2(10) . . ? C47 C46 N4 120.3(9) . . ? C52 C46 N4 120.5(9) . . ? C46 C47 C48 120.2(9) . . ? C49 C48 C47 121.4(10) . . ? C51 C49 C48 117.0(11) . . ? C51 C49 C50 121.4(10) . . ? C48 C49 C50 121.6(10) . . ? C49 C51 C52 123.1(11) . . ? C51 C52 C46 118.9(10) . . ? C59 C53 C54 119.2(9) . . ? C59 C53 N6 118.7(9) . . ? C54 C53 N6 122.1(9) . . ? C55 C54 C53 120.7(9) . . ? C54 C55 C56 121.2(10) . . ? C58 C56 C55 116.9(10) . . ? C58 C56 C57 120.0(11) . . ? C55 C56 C57 123.0(10) . . ? C56 C58 C59 122.4(10) . . ? C53 C59 C58 119.3(10) . . ? C66 C60 C61 119.8(9) . . ? C66 C60 N3 119.2(9) . . ? C61 C60 N3 120.8(9) . . ? C62 C61 C60 119.7(10) . . ? C63 C62 C61 120.8(11) . . ? C65 C63 C62 118.1(10) . . ? C65 C63 C64 121.8(11) . . ? C62 C63 C64 120.2(12) . . ? C63 C65 C66 122.8(11) . . ? C60 C66 C65 118.8(11) . . ? Cl6 C102 Cl5 124.3(16) . . ? Cl3 C101 Cl4 111.5(14) . . ? Cl1 C100 C100 71(2) 2_676 2_676 ? Cl1 C100 Cl1' 134(2) 2_676 . ? C100 C100 Cl1' 63.1(11) 2_676 . ? Cl1 C100 Cl1' 12.5(13) 2_676 2_676 ? C100 C100 Cl1' 59.6(17) 2_676 2_676 ? Cl1' C100 Cl1' 122.7(16) . 2_676 ? Cl1 C100 Cl1 118(2) 2_676 . ? C100 C100 Cl1 46.9(14) 2_676 . ? Cl1' C100 Cl1 16.8(12) . . ? Cl1' C100 Cl1 106.4(19) 2_676 . ? C100 Cl1 C100 62(2) 2_676 . ? C100 Cl1' C100 57.3(16) . 2_676 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.125 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.171 data_7.[PdCl(PPh3)(mu-RNNR)2Rh(CO)2].1.0CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H45 Cl3 N6 O2 P Pd Rh' _chemical_formula_weight 1096.54 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' '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' 'Pd' 'Pd' -0.9988 1.0072 '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 12.3160(19) _cell_length_b 12.5698(9) _cell_length_c 17.359(2) _cell_angle_alpha 105.290(15) _cell_angle_beta 104.369(14) _cell_angle_gamma 104.954(17) _cell_volume 2355.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.707649 _exptl_absorpt_correction_T_max 0.849559 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; ? ; _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_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20155 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10641 _reflns_number_gt 8088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0357P] 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 10641 _refine_ls_number_parameters 582 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.915361(19) 0.324130(18) 0.276412(14) 0.01951(6) Uani 1 1 d . . . Rh1 Rh 0.71082(2) 0.209843(19) 0.127967(15) 0.02193(7) Uani 1 1 d . . . Cl1 Cl 0.81984(7) 0.34150(6) 0.37591(5) 0.02902(17) Uani 1 1 d . . . P1 P 0.96555(7) 0.17226(6) 0.30689(5) 0.02114(16) Uani 1 1 d . . . O1 O 0.5152(2) 0.1204(3) 0.1937(2) 0.0586(8) Uani 1 1 d . . . O2 O 0.6988(3) -0.0366(2) 0.0488(2) 0.0661(9) Uani 1 1 d . . . N1 N 1.0072(2) 0.3273(2) 0.19379(15) 0.0231(5) Uani 1 1 d . . . N2 N 0.9625(2) 0.3106(2) 0.11413(16) 0.0235(5) Uani 1 1 d . . . N3 N 0.8464(2) 0.2745(2) 0.07936(16) 0.0232(5) Uani 1 1 d . . . N4 N 0.8787(2) 0.4697(2) 0.25375(16) 0.0223(5) Uani 1 1 d . . . N5 N 0.7813(2) 0.4754(2) 0.20788(15) 0.0214(5) Uani 1 1 d . . . N6 N 0.6956(2) 0.3765(2) 0.15892(15) 0.0213(5) Uani 1 1 d . . . C1 C 0.5901(3) 0.1551(3) 0.1691(2) 0.0344(8) Uani 1 1 d . . . C2 C 0.7072(3) 0.0576(3) 0.0821(2) 0.0369(8) Uani 1 1 d . . . C11 C 1.1344(3) 0.3571(3) 0.22337(19) 0.0240(6) Uani 1 1 d . . . C12 C 1.1971(3) 0.4192(3) 0.3090(2) 0.0280(7) Uani 1 1 d . . . H12 H 1.1575 0.4466 0.3447 0.034 Uiso 1 1 calc R . . C13 C 1.3190(3) 0.4406(3) 0.3416(2) 0.0323(7) Uani 1 1 d . . . H13 H 1.3599 0.4818 0.3993 0.039 Uiso 1 1 calc R . . C14 C 1.3802(3) 0.4019(3) 0.2902(2) 0.0342(8) Uani 1 1 d . . . C15 C 1.3178(3) 0.3433(3) 0.2043(2) 0.0321(7) Uani 1 1 d . . . H15 H 1.3584 0.3189 0.1685 0.039 Uiso 1 1 calc R . . C16 C 1.1958(3) 0.3201(3) 0.1703(2) 0.0295(7) Uani 1 1 d . . . H16 H 1.1555 0.2802 0.1124 0.035 Uiso 1 1 calc R . . C17 C 1.5123(3) 0.4223(4) 0.3268(3) 0.0516(10) Uani 1 1 d . . . H17A H 1.5363 0.4472 0.3876 0.077 Uiso 1 1 calc R . . H17B H 1.5574 0.4821 0.3108 0.077 Uiso 1 1 calc R . . H17C H 1.5267 0.3507 0.3052 0.077 Uiso 1 1 calc R . . C21 C 0.8118(3) 0.2776(3) -0.00533(19) 0.0247(6) Uani 1 1 d . . . C22 C 0.8886(3) 0.3484(3) -0.0328(2) 0.0303(7) Uani 1 1 d . . . H22 H 0.9671 0.3916 0.0026 0.036 Uiso 1 1 calc R . . C23 C 0.8486(3) 0.3548(3) -0.1130(2) 0.0357(8) Uani 1 1 d . . . H23 H 0.9013 0.4024 -0.1305 0.043 Uiso 1 1 calc R . . C24 C 0.7322(3) 0.2920(3) -0.1678(2) 0.0340(8) Uani 1 1 d . . . C25 C 0.6581(3) 0.2198(3) -0.1403(2) 0.0344(8) Uani 1 1 d . . . H25 H 0.5804 0.1746 -0.1764 0.041 Uiso 1 1 calc R . . C26 C 0.6961(3) 0.2126(3) -0.0598(2) 0.0299(7) Uani 1 1 d . . . H26 H 0.6437 0.1641 -0.0427 0.036 Uiso 1 1 calc R . . C27 C 0.6869(4) 0.3065(4) -0.2523(2) 0.0494(10) Uani 1 1 d . . . H27A H 0.6356 0.2315 -0.2943 0.074 Uiso 1 1 calc R . . H27B H 0.7534 0.3379 -0.2690 0.074 Uiso 1 1 calc R . . H27C H 0.6430 0.3594 -0.2472 0.074 Uiso 1 1 calc R . . C31 C 0.9692(3) 0.5841(2) 0.29646(19) 0.0219(6) Uani 1 1 d . . . C32 C 0.9844(3) 0.6660(3) 0.2561(2) 0.0270(7) Uani 1 1 d . . . H32 H 0.9364 0.6467 0.2003 0.032 Uiso 1 1 calc R . . C33 C 1.0720(3) 0.7771(3) 0.2996(2) 0.0315(7) Uani 1 1 d . . . H33 H 1.0817 0.8314 0.2721 0.038 Uiso 1 1 calc R . . C34 C 1.1449(3) 0.8083(3) 0.3827(2) 0.0294(7) Uani 1 1 d . . . C35 C 1.1284(3) 0.7253(3) 0.4219(2) 0.0281(7) Uani 1 1 d . . . H35 H 1.1760 0.7447 0.4778 0.034 Uiso 1 1 calc R . . C36 C 1.0424(3) 0.6140(3) 0.37941(19) 0.0244(6) Uani 1 1 d . . . H36 H 1.0338 0.5594 0.4066 0.029 Uiso 1 1 calc R . . C37 C 1.2410(3) 0.9286(3) 0.4287(3) 0.0437(9) Uani 1 1 d . . . H37A H 1.2584 0.9484 0.4888 0.065 Uiso 1 1 calc R . . H37B H 1.2134 0.9860 0.4110 0.065 Uiso 1 1 calc R . . H37C H 1.3119 0.9278 0.4154 0.065 Uiso 1 1 calc R . . C41 C 0.5887(3) 0.3949(2) 0.11856(19) 0.0220(6) Uani 1 1 d . . . C42 C 0.5676(3) 0.4994(2) 0.1467(2) 0.0253(7) Uani 1 1 d . . . H42 H 0.6241 0.5610 0.1943 0.030 Uiso 1 1 calc R . . C43 C 0.4632(3) 0.5131(3) 0.1048(2) 0.0276(7) Uani 1 1 d . . . H43 H 0.4520 0.5845 0.1242 0.033 Uiso 1 1 calc R . . C44 C 0.3751(3) 0.4227(3) 0.0344(2) 0.0253(6) Uani 1 1 d . . . C45 C 0.3963(3) 0.3186(3) 0.0076(2) 0.0284(7) Uani 1 1 d . . . H45 H 0.3387 0.2564 -0.0391 0.034 Uiso 1 1 calc R . . C46 C 0.5006(3) 0.3037(3) 0.04795(19) 0.0259(7) Uani 1 1 d . . . H46 H 0.5120 0.2326 0.0279 0.031 Uiso 1 1 calc R . . C47 C 0.2598(3) 0.4365(3) -0.0097(2) 0.0365(8) Uani 1 1 d . . . H47A H 0.2297 0.3874 -0.0685 0.055 Uiso 1 1 calc R . . H47B H 0.2746 0.5171 -0.0053 0.055 Uiso 1 1 calc R . . H47C H 0.2020 0.4138 0.0166 0.055 Uiso 1 1 calc R . . C51 C 1.0588(3) 0.1171(3) 0.2512(2) 0.0248(6) Uani 1 1 d . . . C52 C 1.0109(3) 0.0590(3) 0.1631(2) 0.0340(8) Uani 1 1 d . . . H52 H 0.9350 0.0553 0.1337 0.041 Uiso 1 1 calc R . . C53 C 1.0735(4) 0.0074(3) 0.1192(2) 0.0436(9) Uani 1 1 d . . . H53 H 1.0391 -0.0340 0.0611 0.052 Uiso 1 1 calc R . . C54 C 1.1894(4) 0.0176(4) 0.1629(3) 0.0478(10) Uani 1 1 d . . . H54 H 1.2326 -0.0172 0.1338 0.057 Uiso 1 1 calc R . . C55 C 1.2399(3) 0.0790(4) 0.2487(3) 0.0449(9) Uani 1 1 d . . . H55 H 1.3183 0.0879 0.2770 0.054 Uiso 1 1 calc R . . C56 C 1.1747(3) 0.1281(3) 0.2937(2) 0.0327(7) Uani 1 1 d . . . H56 H 1.2088 0.1680 0.3520 0.039 Uiso 1 1 calc R . . C61 C 1.0498(3) 0.2136(2) 0.41880(18) 0.0221(6) Uani 1 1 d . . . C62 C 1.1066(3) 0.3316(3) 0.47055(19) 0.0255(7) Uani 1 1 d . . . H62 H 1.0977 0.3898 0.4484 0.031 Uiso 1 1 calc R . . C63 C 1.1758(3) 0.3629(3) 0.5544(2) 0.0276(7) Uani 1 1 d . . . H63 H 1.2142 0.4419 0.5881 0.033 Uiso 1 1 calc R . . C64 C 1.1880(3) 0.2775(3) 0.5878(2) 0.0323(7) Uani 1 1 d . . . H64 H 1.2348 0.2988 0.6442 0.039 Uiso 1 1 calc R . . C65 C 1.1310(3) 0.1594(3) 0.5381(2) 0.0325(7) Uani 1 1 d . . . H65 H 1.1388 0.1018 0.5612 0.039 Uiso 1 1 calc R . . C66 C 1.0624(3) 0.1277(3) 0.4537(2) 0.0299(7) Uani 1 1 d . . . H66 H 1.0245 0.0486 0.4202 0.036 Uiso 1 1 calc R . . C71 C 0.8419(3) 0.0376(2) 0.28531(19) 0.0240(6) Uani 1 1 d . . . C72 C 0.7470(3) 0.0449(3) 0.3133(2) 0.0339(8) Uani 1 1 d . . . H72 H 0.7433 0.1183 0.3388 0.041 Uiso 1 1 calc R . . C73 C 0.6575(3) -0.0558(3) 0.3036(2) 0.0359(8) Uani 1 1 d . . . H73 H 0.5959 -0.0494 0.3244 0.043 Uiso 1 1 calc R . . C74 C 0.6594(3) -0.1661(3) 0.2631(2) 0.0336(8) Uani 1 1 d . . . H74 H 0.5979 -0.2335 0.2550 0.040 Uiso 1 1 calc R . . C75 C 0.7526(3) -0.1748(3) 0.2351(2) 0.0333(8) Uani 1 1 d . . . H75 H 0.7548 -0.2484 0.2085 0.040 Uiso 1 1 calc R . . C76 C 0.8441(3) -0.0738(3) 0.2463(2) 0.0326(7) Uani 1 1 d . . . H76 H 0.9073 -0.0807 0.2276 0.039 Uiso 1 1 calc R . . C101 C 1.5584(6) 0.2492(7) 0.5083(4) 0.145(4) Uani 1 1 d D . . H10A H 1.6041 0.3235 0.5067 0.174 Uiso 1 1 calc R A 1 H10B H 1.6062 0.2362 0.5562 0.174 Uiso 1 1 calc R A 1 Cl2 Cl 1.43062(13) 0.26140(16) 0.52617(12) 0.1174(7) Uani 1 1 d . B . Cl3 Cl 1.5382(3) 0.1407(3) 0.4180(3) 0.0681(15) Uani 0.58(2) 1 d P B 1 Cl3' Cl 1.5495(11) 0.170(2) 0.4184(5) 0.182(6) Uani 0.42(2) 1 d PD 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 Pd1 0.01801(12) 0.01921(11) 0.02232(12) 0.00869(9) 0.00606(9) 0.00732(9) Rh1 0.01870(12) 0.01702(11) 0.02759(13) 0.00776(9) 0.00470(10) 0.00534(9) Cl1 0.0352(4) 0.0269(4) 0.0341(4) 0.0136(3) 0.0194(4) 0.0150(3) P1 0.0209(4) 0.0199(4) 0.0231(4) 0.0084(3) 0.0062(3) 0.0081(3) O1 0.0385(16) 0.0680(19) 0.078(2) 0.0389(17) 0.0285(16) 0.0105(14) O2 0.0547(19) 0.0214(13) 0.091(2) -0.0029(14) -0.0029(17) 0.0135(13) N1 0.0195(13) 0.0263(13) 0.0238(13) 0.0108(10) 0.0060(11) 0.0078(10) N2 0.0237(14) 0.0247(13) 0.0246(13) 0.0108(10) 0.0075(11) 0.0106(11) N3 0.0212(13) 0.0230(12) 0.0248(13) 0.0090(10) 0.0058(11) 0.0081(10) N4 0.0194(13) 0.0215(12) 0.0263(13) 0.0093(10) 0.0051(11) 0.0089(10) N5 0.0189(13) 0.0215(12) 0.0231(13) 0.0073(10) 0.0060(10) 0.0074(10) N6 0.0168(12) 0.0180(12) 0.0258(13) 0.0065(10) 0.0038(10) 0.0051(10) C1 0.0274(18) 0.0306(17) 0.040(2) 0.0141(15) 0.0050(16) 0.0063(14) C2 0.0259(18) 0.0273(18) 0.046(2) 0.0088(15) -0.0015(16) 0.0078(14) C11 0.0190(15) 0.0265(15) 0.0298(17) 0.0155(13) 0.0066(13) 0.0089(12) C12 0.0227(16) 0.0324(17) 0.0299(17) 0.0123(14) 0.0098(14) 0.0087(13) C13 0.0227(17) 0.0371(18) 0.0285(17) 0.0103(14) 0.0011(14) 0.0050(14) C14 0.0217(17) 0.044(2) 0.039(2) 0.0224(16) 0.0089(15) 0.0086(15) C15 0.0259(17) 0.0429(19) 0.0387(19) 0.0213(16) 0.0169(15) 0.0169(15) C16 0.0262(17) 0.0362(18) 0.0297(17) 0.0171(14) 0.0097(14) 0.0109(14) C17 0.027(2) 0.077(3) 0.050(2) 0.022(2) 0.0097(18) 0.019(2) C21 0.0267(16) 0.0266(15) 0.0235(16) 0.0073(12) 0.0069(13) 0.0165(13) C22 0.0251(17) 0.0371(18) 0.0293(17) 0.0126(14) 0.0081(14) 0.0119(14) C23 0.037(2) 0.045(2) 0.0316(18) 0.0175(16) 0.0146(16) 0.0167(16) C24 0.036(2) 0.045(2) 0.0254(17) 0.0096(15) 0.0098(15) 0.0254(17) C25 0.0297(18) 0.0420(19) 0.0260(17) 0.0062(15) 0.0017(15) 0.0170(16) C26 0.0257(17) 0.0326(17) 0.0291(17) 0.0075(14) 0.0065(14) 0.0123(14) C27 0.046(2) 0.078(3) 0.030(2) 0.021(2) 0.0123(18) 0.029(2) C31 0.0184(15) 0.0196(14) 0.0281(16) 0.0073(12) 0.0078(13) 0.0083(12) C32 0.0210(16) 0.0311(16) 0.0294(17) 0.0141(13) 0.0054(13) 0.0094(13) C33 0.0275(18) 0.0253(16) 0.042(2) 0.0166(14) 0.0084(15) 0.0079(13) C34 0.0246(17) 0.0244(15) 0.0362(18) 0.0093(14) 0.0066(14) 0.0085(13) C35 0.0245(17) 0.0294(16) 0.0247(16) 0.0052(13) 0.0035(13) 0.0092(13) C36 0.0248(16) 0.0242(15) 0.0267(16) 0.0107(12) 0.0083(13) 0.0109(13) C37 0.036(2) 0.0249(17) 0.053(2) 0.0089(16) 0.0008(18) 0.0022(15) C41 0.0171(15) 0.0238(14) 0.0258(16) 0.0108(12) 0.0064(12) 0.0069(12) C42 0.0184(15) 0.0194(14) 0.0310(17) 0.0044(12) 0.0029(13) 0.0052(12) C43 0.0251(16) 0.0221(15) 0.0372(18) 0.0106(13) 0.0094(14) 0.0115(13) C44 0.0230(16) 0.0274(15) 0.0303(17) 0.0136(13) 0.0102(13) 0.0118(13) C45 0.0236(16) 0.0262(16) 0.0276(17) 0.0063(13) 0.0013(13) 0.0062(13) C46 0.0247(16) 0.0213(14) 0.0288(16) 0.0059(12) 0.0046(13) 0.0104(13) C47 0.0287(18) 0.0390(19) 0.041(2) 0.0134(16) 0.0049(16) 0.0177(15) C51 0.0267(16) 0.0229(15) 0.0302(16) 0.0128(13) 0.0115(14) 0.0120(13) C52 0.0346(19) 0.0384(19) 0.0280(17) 0.0097(15) 0.0095(15) 0.0144(15) C53 0.056(3) 0.045(2) 0.033(2) 0.0097(16) 0.0203(19) 0.0214(19) C54 0.059(3) 0.055(2) 0.050(2) 0.020(2) 0.032(2) 0.039(2) C55 0.036(2) 0.061(2) 0.056(3) 0.028(2) 0.0218(19) 0.0323(19) C56 0.0314(19) 0.0338(18) 0.0341(19) 0.0124(15) 0.0093(15) 0.0146(15) C61 0.0204(15) 0.0242(15) 0.0232(15) 0.0092(12) 0.0076(12) 0.0090(12) C62 0.0262(17) 0.0237(15) 0.0299(17) 0.0104(13) 0.0103(14) 0.0120(13) C63 0.0245(16) 0.0243(15) 0.0276(16) 0.0029(13) 0.0049(13) 0.0085(13) C64 0.0290(18) 0.0401(19) 0.0243(16) 0.0108(14) 0.0033(14) 0.0123(15) C65 0.0327(19) 0.0327(17) 0.0335(18) 0.0192(15) 0.0053(15) 0.0116(14) C66 0.0319(18) 0.0245(15) 0.0298(17) 0.0111(13) 0.0047(14) 0.0078(13) C71 0.0228(16) 0.0216(14) 0.0225(15) 0.0072(12) 0.0022(12) 0.0056(12) C72 0.0294(18) 0.0246(16) 0.045(2) 0.0063(14) 0.0132(16) 0.0100(14) C73 0.0240(17) 0.0278(17) 0.055(2) 0.0125(16) 0.0161(16) 0.0068(14) C74 0.0287(18) 0.0261(16) 0.0355(19) 0.0105(14) 0.0010(15) 0.0024(14) C75 0.040(2) 0.0188(15) 0.0343(18) 0.0057(13) 0.0085(16) 0.0076(14) C76 0.0370(19) 0.0252(16) 0.0395(19) 0.0113(14) 0.0173(16) 0.0128(14) C101 0.072(4) 0.192(8) 0.101(5) -0.052(5) -0.007(4) 0.073(5) Cl2 0.0564(8) 0.1232(14) 0.1171(13) -0.0316(11) 0.0152(9) 0.0316(9) Cl3 0.0429(19) 0.074(3) 0.064(2) -0.0079(16) 0.0082(15) 0.0258(14) Cl3' 0.116(6) 0.394(17) 0.077(5) 0.110(8) 0.051(5) 0.109(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.037(2) . ? Pd1 N4 2.104(2) . ? Pd1 P1 2.2991(8) . ? Pd1 Cl1 2.3145(8) . ? Pd1 Rh1 2.8298(8) . ? Rh1 C2 1.853(3) . ? Rh1 C1 1.858(4) . ? Rh1 N6 2.090(2) . ? Rh1 N3 2.126(3) . ? P1 C61 1.819(3) . ? P1 C51 1.828(3) . ? P1 C71 1.838(3) . ? O1 C1 1.145(4) . ? O2 C2 1.136(4) . ? N1 N2 1.292(3) . ? N1 C11 1.434(4) . ? N2 N3 1.307(3) . ? N3 C21 1.440(4) . ? N4 N5 1.296(3) . ? N4 C31 1.436(4) . ? N5 N6 1.305(3) . ? N6 C41 1.437(4) . ? C11 C12 1.386(4) . ? C11 C16 1.392(4) . ? C12 C13 1.392(4) . ? C13 C14 1.378(5) . ? C14 C15 1.383(5) . ? C14 C17 1.516(5) . ? C15 C16 1.391(4) . ? C21 C26 1.384(4) . ? C21 C22 1.388(4) . ? C22 C23 1.388(4) . ? C23 C24 1.388(5) . ? C24 C25 1.380(5) . ? C24 C27 1.511(5) . ? C25 C26 1.393(4) . ? C31 C36 1.387(4) . ? C31 C32 1.389(4) . ? C32 C33 1.396(4) . ? C33 C34 1.386(5) . ? C34 C35 1.387(4) . ? C34 C37 1.515(4) . ? C35 C36 1.388(4) . ? C41 C42 1.390(4) . ? C41 C46 1.396(4) . ? C42 C43 1.388(4) . ? C43 C44 1.392(4) . ? C44 C45 1.383(4) . ? C44 C47 1.513(4) . ? C45 C46 1.386(4) . ? C51 C56 1.387(4) . ? C51 C52 1.400(4) . ? C52 C53 1.373(5) . ? C53 C54 1.394(5) . ? C54 C55 1.374(5) . ? C55 C56 1.397(5) . ? C61 C66 1.394(4) . ? C61 C62 1.395(4) . ? C62 C63 1.381(4) . ? C63 C64 1.372(4) . ? C64 C65 1.388(5) . ? C65 C66 1.386(4) . ? C71 C72 1.387(4) . ? C71 C76 1.396(4) . ? C72 C73 1.386(4) . ? C73 C74 1.388(4) . ? C74 C75 1.371(5) . ? C75 C76 1.393(4) . ? C101 Cl3' 1.575(11) . ? C101 Cl3 1.698(7) . ? C101 Cl2 1.715(6) . ? 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 Pd1 N4 86.78(10) . . ? N1 Pd1 P1 92.93(7) . . ? N4 Pd1 P1 176.77(7) . . ? N1 Pd1 Cl1 174.09(7) . . ? N4 Pd1 Cl1 88.81(7) . . ? P1 Pd1 Cl1 91.25(3) . . ? N1 Pd1 Rh1 84.58(7) . . ? N4 Pd1 Rh1 79.30(7) . . ? P1 Pd1 Rh1 103.88(3) . . ? Cl1 Pd1 Rh1 98.47(3) . . ? C2 Rh1 C1 89.97(16) . . ? C2 Rh1 N6 170.20(13) . . ? C1 Rh1 N6 91.08(12) . . ? C2 Rh1 N3 90.86(13) . . ? C1 Rh1 N3 178.60(12) . . ? N6 Rh1 N3 87.91(9) . . ? C2 Rh1 Pd1 106.89(10) . . ? C1 Rh1 Pd1 103.11(11) . . ? N6 Rh1 Pd1 82.35(7) . . ? N3 Rh1 Pd1 77.73(7) . . ? C61 P1 C51 104.48(14) . . ? C61 P1 C71 103.51(13) . . ? C51 P1 C71 102.77(14) . . ? C61 P1 Pd1 112.16(10) . . ? C51 P1 Pd1 115.45(10) . . ? C71 P1 Pd1 116.97(10) . . ? N2 N1 C11 113.5(2) . . ? N2 N1 Pd1 126.00(19) . . ? C11 N1 Pd1 120.35(19) . . ? N1 N2 N3 118.4(2) . . ? N2 N3 C21 111.4(2) . . ? N2 N3 Rh1 129.66(19) . . ? C21 N3 Rh1 118.86(19) . . ? N5 N4 C31 111.2(2) . . ? N5 N4 Pd1 129.86(19) . . ? C31 N4 Pd1 118.92(18) . . ? N4 N5 N6 117.5(2) . . ? N5 N6 C41 111.8(2) . . ? N5 N6 Rh1 126.13(18) . . ? C41 N6 Rh1 121.65(18) . . ? O1 C1 Rh1 179.3(4) . . ? O2 C2 Rh1 175.0(3) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 N1 118.4(3) . . ? C16 C11 N1 122.3(3) . . ? C11 C12 C13 120.2(3) . . ? C14 C13 C12 121.2(3) . . ? C13 C14 C15 118.2(3) . . ? C13 C14 C17 120.8(3) . . ? C15 C14 C17 121.0(3) . . ? C14 C15 C16 121.6(3) . . ? C15 C16 C11 119.6(3) . . ? C26 C21 C22 118.8(3) . . ? C26 C21 N3 118.9(3) . . ? C22 C21 N3 122.2(3) . . ? C23 C22 C21 120.1(3) . . ? C24 C23 C22 121.9(3) . . ? C25 C24 C23 117.2(3) . . ? C25 C24 C27 121.4(3) . . ? C23 C24 C27 121.4(3) . . ? C24 C25 C26 121.9(3) . . ? C21 C26 C25 120.1(3) . . ? C36 C31 C32 119.3(3) . . ? C36 C31 N4 119.7(3) . . ? C32 C31 N4 121.0(3) . . ? C31 C32 C33 119.8(3) . . ? C34 C33 C32 121.4(3) . . ? C33 C34 C35 117.9(3) . . ? C33 C34 C37 120.9(3) . . ? C35 C34 C37 121.2(3) . . ? C34 C35 C36 121.5(3) . . ? C31 C36 C35 120.1(3) . . ? C42 C41 C46 117.8(3) . . ? C42 C41 N6 123.2(3) . . ? C46 C41 N6 119.0(3) . . ? C43 C42 C41 120.9(3) . . ? C42 C43 C44 121.6(3) . . ? C45 C44 C43 117.1(3) . . ? C45 C44 C47 121.4(3) . . ? C43 C44 C47 121.6(3) . . ? C44 C45 C46 122.2(3) . . ? C45 C46 C41 120.4(3) . . ? C56 C51 C52 118.8(3) . . ? C56 C51 P1 122.1(2) . . ? C52 C51 P1 119.1(2) . . ? C53 C52 C51 121.4(3) . . ? C52 C53 C54 119.2(3) . . ? C55 C54 C53 120.1(3) . . ? C54 C55 C56 120.6(3) . . ? C51 C56 C55 119.8(3) . . ? C66 C61 C62 118.7(3) . . ? C66 C61 P1 120.5(2) . . ? C62 C61 P1 120.8(2) . . ? C63 C62 C61 120.7(3) . . ? C64 C63 C62 119.9(3) . . ? C63 C64 C65 120.5(3) . . ? C66 C65 C64 119.7(3) . . ? C65 C66 C61 120.4(3) . . ? C72 C71 C76 118.3(3) . . ? C72 C71 P1 119.8(2) . . ? C76 C71 P1 121.7(2) . . ? C73 C72 C71 120.8(3) . . ? C72 C73 C74 120.4(3) . . ? C75 C74 C73 119.5(3) . . ? C74 C75 C76 120.3(3) . . ? C75 C76 C71 120.7(3) . . ? Cl3' C101 Cl3 11.8(8) . . ? Cl3' C101 Cl2 119.3(5) . . ? Cl3 C101 Cl2 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.580 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.085