Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol BRISTOL BS8 4QQ UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_section_title ; Triazenide-bridged rhodium-palladium complexes: [I2Rh(p-MeC6H4NNNC6H4Me-p)2Pd(C3H5)]-, a stable paramagnetic [RhPd]4+ species with a localised Rh(II) centre ; loop_ _publ_author_name 'Neil Connelly' 'Chris Adams' 'R. Angharad Baber' 'Phimphaka Harding' 'Owen D. Hayward' 'Mathivathani Kandiah' ; A.Orpen ; data_7.[PdCl(PPh3)(mu-RNNR)2Rh(CO)2].1.0CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 145681' _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 # Attachment 'cifs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 286469' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H33 N6 O2 Pd Rh' _chemical_formula_weight 754.99 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.962(3) _cell_length_b 8.9123(10) _cell_length_c 26.282(6) _cell_angle_alpha 90.00 _cell_angle_beta 129.608(13) _cell_angle_gamma 90.00 _cell_volume 3241.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 3.87 _cell_measurement_theta_max 12.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.378 _exptl_absorpt_process_details XPrep _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'CCD area detector' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5127 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 27.40 _reflns_number_total 4572 _reflns_number_gt 4238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0387P)^2^+3.7808P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4572 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Pd1 Pd 0.793682(19) -0.06990(3) 0.489041(14) 0.03200(10) Uani 1 1 d . . . Rh1 Rh 0.87060(2) 0.09811(3) 0.604648(14) 0.03452(10) Uani 1 1 d . . . O1 O 1.0862(3) 0.0600(7) 0.7028(3) 0.114(2) Uani 1 1 d . . . O2 O 0.8500(4) -0.1423(7) 0.6734(3) 0.1049(17) Uani 1 1 d . . . N1 N 0.7250(2) 0.1643(3) 0.54057(14) 0.0321(6) Uani 1 1 d . . . N2 N 0.6491(2) 0.0941(3) 0.49134(15) 0.0325(6) Uani 1 1 d . . . N3 N 0.6634(2) -0.0252(3) 0.47061(15) 0.0317(6) Uani 1 1 d . . . N4 N 0.8947(2) 0.2556(3) 0.55834(14) 0.0309(6) Uani 1 1 d . . . N5 N 0.8470(2) 0.2651(3) 0.49520(14) 0.0305(6) Uani 1 1 d . . . N6 N 0.7936(2) 0.1516(3) 0.45991(14) 0.0296(6) Uani 1 1 d . . . C1 C 1.0046(4) 0.0680(7) 0.6662(3) 0.0688(15) Uani 1 1 d . . . C2 C 0.8544(4) -0.0506(7) 0.6480(3) 0.0606(12) Uani 1 1 d . . . C3 C 0.8162(5) -0.2975(6) 0.5185(4) 0.0689(15) Uani 1 1 d . . . H3A H 0.7578 -0.3615 0.4948 0.036(10) Uiso 1 1 d R . . H3B H 0.8632 -0.3175 0.5666 0.13(3) Uiso 1 1 d R . . C4 C 0.8544(5) -0.2723(7) 0.4861(4) 0.0804(19) Uani 1 1 d . . . H4A H 0.8238 -0.3216 0.4426 0.14(3) Uiso 1 1 d R . . C5 C 0.9194(4) -0.1518(7) 0.5072(4) 0.0727(15) Uani 1 1 d . . . H5A H 0.9796 -0.1532 0.5538 0.24(6) Uiso 1 1 d R . . H5B H 0.9293 -0.1191 0.4759 0.10(2) Uiso 1 1 d R . . C11 C 0.7006(3) 0.3087(4) 0.54974(18) 0.0324(7) Uani 1 1 d . . . C12 C 0.6284(3) 0.3942(4) 0.49580(19) 0.0379(8) Uani 1 1 d . . . H12 H 0.5956 0.3572 0.4523 0.037(10) Uiso 1 1 d R . . C13 C 0.6040(3) 0.5336(4) 0.5050(2) 0.0402(8) Uani 1 1 d . . . H13 H 0.5539 0.5902 0.4676 0.059(14) Uiso 1 1 d R . . C14 C 0.6516(3) 0.5916(4) 0.5678(2) 0.0381(8) Uani 1 1 d . . . C15 C 0.7253(3) 0.5063(5) 0.6214(2) 0.0411(8) Uani 1 1 d . . . H15 H 0.7596 0.5447 0.6648 0.056(13) Uiso 1 1 d R . . C16 C 0.7501(3) 0.3662(5) 0.61297(19) 0.0386(8) Uani 1 1 d . . . H16 H 0.8008 0.3101 0.6503 0.056(13) Uiso 1 1 d R . . C17 C 0.6234(4) 0.7422(5) 0.5764(2) 0.0497(10) Uani 1 1 d . . . H17A H 0.5549 0.7409 0.5560 0.041(11) Uiso 1 1 d R . . H17B H 0.6626 0.7646 0.6236 0.10(2) Uiso 1 1 d R . . H17C H 0.6343 0.8194 0.5552 0.075(17) Uiso 1 1 d R . . C21 C 0.5746(3) -0.0999(4) 0.4211(2) 0.0341(8) Uani 1 1 d . . . C22 C 0.5684(3) -0.1948(4) 0.3765(2) 0.0389(8) Uani 1 1 d . . . H22 H 0.6241 -0.2123 0.3805 0.036(11) Uiso 1 1 d R . . C23 C 0.4820(3) -0.2644(5) 0.3264(2) 0.0451(10) Uani 1 1 d . . . H23 H 0.4796 -0.3283 0.2964 0.044(11) Uiso 1 1 d R . . C24 C 0.3996(3) -0.2430(5) 0.3189(2) 0.0450(10) Uani 1 1 d . . . C25 C 0.4062(3) -0.1507(5) 0.3643(2) 0.0458(10) Uani 1 1 d . . . H25 H 0.3505 -0.1351 0.3605 0.072(17) Uiso 1 1 d R . . C26 C 0.4915(3) -0.0810(5) 0.4145(2) 0.0400(9) Uani 1 1 d . . . H26 H 0.4940 -0.0195 0.4452 0.042(11) Uiso 1 1 d R . . C27 C 0.3038(4) -0.3129(7) 0.2621(3) 0.0644(14) Uani 1 1 d . . . H27A H 0.3088 -0.4224 0.2665 0.11(2) Uiso 1 1 d R . . H27B H 0.2531 -0.2777 0.2631 0.11(3) Uiso 1 1 d R . . H27C H 0.2877 -0.2839 0.2201 0.19(5) Uiso 1 1 d R . . C31 C 0.9633(2) 0.3725(4) 0.59443(17) 0.0302(7) Uani 1 1 d . . . C32 C 0.9817(3) 0.4292(5) 0.65072(19) 0.0375(8) Uani 1 1 d . . . H32 H 0.9477 0.3902 0.6644 0.039(11) Uiso 1 1 d R . . C33 C 1.0490(3) 0.5419(5) 0.68706(19) 0.0385(8) Uani 1 1 d . . . H33 H 1.0608 0.5783 0.7256 0.044(11) Uiso 1 1 d R . . C34 C 1.1001(2) 0.6036(4) 0.66864(19) 0.0346(7) Uani 1 1 d . . . C35 C 1.0809(3) 0.5444(5) 0.61186(19) 0.0355(7) Uani 1 1 d . . . H35 H 1.1148 0.5833 0.5981 0.061(15) Uiso 1 1 d R . . C36 C 1.0143(3) 0.4319(4) 0.57544(18) 0.0333(7) Uani 1 1 d . . . H36 H 1.0029 0.3944 0.5372 0.028(9) Uiso 1 1 d R . . C37 C 1.1733(3) 0.7233(5) 0.7082(2) 0.0474(10) Uani 1 1 d . . . H37A H 1.2382 0.6795 0.7351 0.068(16) Uiso 1 1 d R . . H37B H 1.1666 0.7991 0.6785 0.069(15) Uiso 1 1 d R . . H37C H 1.1633 0.7703 0.7372 0.062(14) Uiso 1 1 d R . . C41 C 0.7304(2) 0.1850(4) 0.39094(17) 0.0314(7) Uani 1 1 d . . . C42 C 0.6973(3) 0.0693(4) 0.3460(2) 0.0417(9) Uani 1 1 d . . . H42 H 0.7179 -0.0307 0.3613 0.054(13) Uiso 1 1 d R . . C43 C 0.6343(3) 0.0985(5) 0.2790(2) 0.0467(10) Uani 1 1 d . . . H43 H 0.6126 0.0176 0.2489 0.092(19) Uiso 1 1 d R . . C44 C 0.6020(3) 0.2406(5) 0.2544(2) 0.0421(9) Uani 1 1 d . . . C45 C 0.6348(3) 0.3564(5) 0.29985(19) 0.0395(8) Uani 1 1 d . . . H45 H 0.6135 0.4560 0.2841 0.045(11) Uiso 1 1 d R . . C46 C 0.6973(3) 0.3303(4) 0.36720(18) 0.0336(7) Uani 1 1 d . . . H46 H 0.7176 0.4110 0.3971 0.045(12) Uiso 1 1 d R . . C47 C 0.5364(3) 0.2726(8) 0.1815(2) 0.0562(12) Uani 1 1 d . . . H47A H 0.4726 0.2293 0.1604 0.10(2) Uiso 1 1 d R . . H47B H 0.5302 0.3813 0.1741 0.22(6) Uiso 1 1 d R . . H47C H 0.5637 0.2277 0.1625 0.079(19) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03334(17) 0.02400(14) 0.03858(18) 0.00351(10) 0.02288(15) 0.00245(10) Rh1 0.03509(18) 0.03449(16) 0.02819(16) 0.00686(11) 0.01748(14) -0.00165(11) O1 0.054(2) 0.091(4) 0.119(5) 0.038(4) 0.019(3) 0.009(2) O2 0.129(4) 0.096(4) 0.084(4) 0.021(3) 0.065(3) -0.032(3) N1 0.0321(14) 0.0340(15) 0.0307(15) -0.0077(12) 0.0203(14) -0.0079(13) N2 0.0345(15) 0.0303(14) 0.0354(17) -0.0049(12) 0.0235(15) -0.0058(12) N3 0.0343(15) 0.0256(13) 0.0379(17) -0.0014(12) 0.0243(15) -0.0022(12) N4 0.0302(14) 0.0323(14) 0.0259(14) 0.0030(12) 0.0158(13) -0.0021(12) N5 0.0296(14) 0.0305(14) 0.0303(15) 0.0042(12) 0.0185(13) 0.0012(12) N6 0.0318(14) 0.0252(13) 0.0311(15) -0.0003(11) 0.0197(13) -0.0021(11) C1 0.048(3) 0.064(4) 0.069(4) 0.020(3) 0.025(3) 0.005(2) C2 0.057(3) 0.062(3) 0.046(3) 0.007(2) 0.025(2) -0.012(2) C3 0.084(4) 0.032(2) 0.095(5) 0.015(3) 0.060(4) 0.005(2) C4 0.082(4) 0.044(3) 0.125(6) 0.002(3) 0.070(5) 0.015(3) C5 0.062(3) 0.068(4) 0.094(5) 0.002(3) 0.052(4) 0.003(3) C11 0.0354(18) 0.0333(17) 0.0343(19) -0.0078(14) 0.0250(17) -0.0093(15) C12 0.043(2) 0.0368(18) 0.0314(19) -0.0088(15) 0.0230(18) -0.0103(16) C13 0.043(2) 0.0368(19) 0.037(2) -0.0046(17) 0.0243(19) -0.0055(17) C14 0.042(2) 0.0396(19) 0.042(2) -0.0096(16) 0.0307(19) -0.0124(16) C15 0.042(2) 0.048(2) 0.037(2) -0.0134(17) 0.0270(19) -0.0106(18) C16 0.0367(19) 0.046(2) 0.0305(19) -0.0083(17) 0.0199(17) -0.0062(17) C17 0.062(3) 0.041(2) 0.059(3) -0.011(2) 0.045(2) -0.005(2) C21 0.0355(19) 0.0265(17) 0.037(2) -0.0015(15) 0.0217(19) -0.0042(15) C22 0.0384(19) 0.0329(18) 0.049(2) -0.0081(16) 0.0298(19) -0.0047(16) C23 0.053(2) 0.034(2) 0.054(3) -0.0136(19) 0.036(2) -0.0101(19) C24 0.043(2) 0.038(2) 0.049(3) -0.0111(19) 0.027(2) -0.0144(18) C25 0.043(2) 0.037(2) 0.063(3) -0.0093(19) 0.037(2) -0.0086(18) C26 0.041(2) 0.035(2) 0.051(3) -0.0096(18) 0.033(2) -0.0066(17) C27 0.049(3) 0.069(3) 0.068(4) -0.030(3) 0.034(3) -0.026(3) C31 0.0244(16) 0.0335(17) 0.0285(18) 0.0028(14) 0.0148(15) -0.0011(14) C32 0.0320(18) 0.049(2) 0.0314(19) -0.0014(16) 0.0204(17) -0.0070(16) C33 0.0338(18) 0.050(2) 0.0310(19) -0.0049(17) 0.0202(17) -0.0045(17) C34 0.0251(17) 0.0379(19) 0.034(2) 0.0005(15) 0.0156(17) 0.0014(15) C35 0.0286(17) 0.0443(19) 0.0347(19) 0.0002(16) 0.0206(17) -0.0032(16) C36 0.0316(18) 0.0387(19) 0.033(2) 0.0019(15) 0.0218(17) 0.0028(15) C37 0.039(2) 0.055(2) 0.047(2) -0.015(2) 0.027(2) -0.0135(19) C41 0.0325(17) 0.0334(17) 0.0307(18) -0.0018(14) 0.0214(16) -0.0061(14) C42 0.053(2) 0.0335(19) 0.043(2) -0.0036(16) 0.032(2) -0.0078(17) C43 0.051(2) 0.053(2) 0.036(2) -0.0166(19) 0.028(2) -0.020(2) C44 0.0339(18) 0.063(2) 0.0306(18) -0.0015(19) 0.0213(16) -0.0078(19) C45 0.0349(19) 0.047(2) 0.0318(19) 0.0054(16) 0.0192(17) 0.0041(17) C46 0.0321(17) 0.0347(17) 0.0315(18) -0.0032(14) 0.0191(16) -0.0050(15) C47 0.040(2) 0.095(4) 0.030(2) 0.001(2) 0.0199(19) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3 2.103(3) . ? Pd1 C3 2.116(5) . ? Pd1 N6 2.117(3) . ? Pd1 C5 2.118(5) . ? Pd1 C4 2.135(5) . ? Pd1 Rh1 2.8337(7) . ? Rh1 C1 1.875(6) . ? Rh1 C2 1.887(5) . ? Rh1 N4 2.076(3) . ? Rh1 N1 2.100(3) . ? O1 C1 1.132(7) . ? O2 C2 1.089(7) . ? N1 N2 1.294(4) . ? N1 C11 1.429(4) . ? N2 N3 1.293(4) . ? N3 C21 1.426(5) . ? N4 N5 1.297(4) . ? N4 C31 1.418(5) . ? N5 N6 1.292(4) . ? N6 C41 1.428(4) . ? C3 C4 1.411(9) . ? C4 C5 1.414(9) . ? C11 C12 1.388(6) . ? C11 C16 1.389(5) . ? C12 C13 1.389(5) . ? C13 C14 1.388(5) . ? C14 C15 1.392(6) . ? C14 C17 1.501(6) . ? C15 C16 1.390(6) . ? C21 C22 1.390(5) . ? C21 C26 1.399(5) . ? C22 C23 1.386(6) . ? C23 C24 1.377(5) . ? C24 C25 1.391(6) . ? C24 C27 1.517(7) . ? C25 C26 1.377(6) . ? C31 C32 1.389(5) . ? C31 C36 1.397(4) . ? C32 C33 1.382(6) . ? C33 C34 1.395(5) . ? C34 C35 1.402(5) . ? C34 C37 1.484(6) . ? C35 C36 1.376(5) . ? C41 C42 1.385(5) . ? C41 C46 1.396(5) . ? C42 C43 1.382(6) . ? C43 C44 1.371(6) . ? C44 C45 1.394(6) . ? C44 C47 1.503(6) . ? C45 C46 1.383(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd1 C3 101.01(16) . . ? N3 Pd1 N6 89.76(10) . . ? C3 Pd1 N6 169.12(15) . . ? N3 Pd1 C5 170.75(19) . . ? C3 Pd1 C5 70.1(2) . . ? N6 Pd1 C5 99.08(19) . . ? N3 Pd1 C4 132.12(19) . . ? C3 Pd1 C4 38.8(2) . . ? N6 Pd1 C4 131.12(19) . . ? C5 Pd1 C4 38.8(2) . . ? N3 Pd1 Rh1 81.79(8) . . ? C3 Pd1 Rh1 105.4(2) . . ? N6 Pd1 Rh1 77.43(8) . . ? C5 Pd1 Rh1 102.7(2) . . ? C4 Pd1 Rh1 125.0(2) . . ? C1 Rh1 C2 89.1(2) . . ? C1 Rh1 N4 88.3(2) . . ? C2 Rh1 N4 177.00(19) . . ? C1 Rh1 N1 171.6(2) . . ? C2 Rh1 N1 95.10(18) . . ? N4 Rh1 N1 87.62(11) . . ? C1 Rh1 Pd1 109.3(2) . . ? C2 Rh1 Pd1 96.82(18) . . ? N4 Rh1 Pd1 82.54(8) . . ? N1 Rh1 Pd1 77.41(8) . . ? N2 N1 C11 111.3(3) . . ? N2 N1 Rh1 130.2(2) . . ? C11 N1 Rh1 118.5(2) . . ? N3 N2 N1 117.0(3) . . ? N2 N3 C21 111.2(3) . . ? N2 N3 Pd1 123.3(2) . . ? C21 N3 Pd1 123.7(2) . . ? N5 N4 C31 113.1(3) . . ? N5 N4 Rh1 125.4(2) . . ? C31 N4 Rh1 121.4(2) . . ? N6 N5 N4 116.7(3) . . ? N5 N6 C41 111.9(3) . . ? N5 N6 Pd1 129.9(2) . . ? C41 N6 Pd1 118.0(2) . . ? O1 C1 Rh1 175.2(5) . . ? O2 C2 Rh1 174.8(6) . . ? C4 C3 Pd1 71.3(3) . . ? C3 C4 C5 118.8(7) . . ? C3 C4 Pd1 69.9(3) . . ? C5 C4 Pd1 70.0(3) . . ? C4 C5 Pd1 71.2(3) . . ? C12 C11 C16 119.2(3) . . ? C12 C11 N1 120.6(3) . . ? C16 C11 N1 120.2(3) . . ? C11 C12 C13 120.4(3) . . ? C14 C13 C12 121.1(4) . . ? C13 C14 C15 117.9(4) . . ? C13 C14 C17 120.0(4) . . ? C15 C14 C17 122.1(4) . . ? C16 C15 C14 121.6(4) . . ? C11 C16 C15 119.7(4) . . ? C22 C21 C26 117.6(3) . . ? C22 C21 N3 119.7(3) . . ? C26 C21 N3 122.7(3) . . ? C23 C22 C21 120.9(3) . . ? C24 C23 C22 121.6(3) . . ? C23 C24 C25 117.6(4) . . ? C23 C24 C27 121.6(4) . . ? C25 C24 C27 120.7(4) . . ? C26 C25 C24 121.6(4) . . ? C25 C26 C21 120.7(3) . . ? C32 C31 C36 118.5(3) . . ? C32 C31 N4 119.7(3) . . ? C36 C31 N4 121.8(3) . . ? C33 C32 C31 120.7(3) . . ? C32 C33 C34 121.7(3) . . ? C33 C34 C35 116.8(3) . . ? C33 C34 C37 121.6(3) . . ? C35 C34 C37 121.6(3) . . ? C36 C35 C34 122.0(3) . . ? C35 C36 C31 120.3(3) . . ? C42 C41 C46 118.8(3) . . ? C42 C41 N6 119.3(3) . . ? C46 C41 N6 121.9(3) . . ? C43 C42 C41 120.3(4) . . ? C44 C43 C42 122.1(4) . . ? C43 C44 C45 117.4(4) . . ? C43 C44 C47 121.9(4) . . ? C45 C44 C47 120.7(4) . . ? C46 C45 C44 121.8(4) . . ? C45 C46 C41 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.620 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.620 _refine_diff_density_max 0.754 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.059 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 286470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30.19 H31.37 I2 N6 Pd Rh,N C16 H36, C H2 Cl2' _chemical_formula_sum 'C47.19 H69.37 Cl0.37 I2 N7 Pd Rh' _chemical_formula_weight 1210.82 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' 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' I I -0.4742 1.8119 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0351(15) _cell_length_b 16.0530(16) _cell_length_c 20.138(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.057(2) _cell_angle_gamma 90.00 _cell_volume 5144.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min 2.6005 _cell_measurement_theta_max 23.625 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2419 _exptl_absorpt_coefficient_mu 1.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851357 _exptl_absorpt_correction_T_max 1.0 _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33507 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.1644 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11740 _reflns_number_gt 5488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0820P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11740 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1742 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1927 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Pd1 Pd 0.87638(5) 0.80205(5) 0.19432(4) 0.0354(2) Uani 1 1 d . . . Rh1 Rh 1.02012(5) 0.75755(4) 0.13267(3) 0.02575(19) Uani 1 1 d . . . I1 I 0.95974(6) 0.62384(5) 0.07256(4) 0.0610(3) Uani 1 1 d . . . I2 I 1.09595(5) 0.67105(4) 0.23248(4) 0.0472(2) Uani 1 1 d . . . N1 N 1.0693(5) 0.8635(5) 0.1792(4) 0.0289(18) Uani 1 1 d . . . N2 N 1.0389(5) 0.9064(5) 0.2255(4) 0.0297(18) Uani 1 1 d . . . N3 N 0.9652(5) 0.8888(5) 0.2396(4) 0.0326(19) Uani 1 1 d . . . N4 N 0.9671(5) 0.8323(4) 0.0553(4) 0.0282(18) Uani 1 1 d . . . N5 N 0.8981(5) 0.8755(5) 0.0545(4) 0.0290(18) Uani 1 1 d . . . N6 N 0.8553(5) 0.8710(5) 0.1052(4) 0.0284(18) Uani 1 1 d . . . C3 C 0.8699(9) 0.7263(9) 0.2809(8) 0.075(4) Uani 1 1 d . . . H3A H 0.9234 0.7015 0.3017 0.090 Uiso 1 1 calc R . . H3B H 0.8337 0.7469 0.3138 0.090 Uiso 1 1 calc R . . C4 C 0.8334(18) 0.6896(13) 0.2300(10) 0.170(12) Uani 1 1 d . . . H4A H 0.8731 0.6457 0.2180 0.204 Uiso 1 1 calc R . . C5 C 0.7851(9) 0.7068(8) 0.1757(8) 0.070(4) Uani 1 1 d . . . H5B H 0.7264 0.7222 0.1806 0.084 Uiso 1 1 calc R . . H5C H 0.7901 0.6702 0.1367 0.084 Uiso 1 1 calc R . . C11 C 1.1502(6) 0.8914(6) 0.1652(4) 0.029(2) Uani 1 1 d . . . C12 C 1.1798(7) 0.9734(6) 0.1820(5) 0.038(3) Uani 1 1 d . . . H12A H 1.1455 1.0115 0.2025 0.045 Uiso 1 1 calc R . . C13 C 1.2589(7) 0.9971(7) 0.1681(5) 0.039(3) Uani 1 1 d . . . H13A H 1.2788 1.0515 0.1799 0.047 Uiso 1 1 calc R . . C14 C 1.3084(6) 0.9447(7) 0.1380(5) 0.039(3) Uani 1 1 d . . . C15 C 1.2788(6) 0.8666(6) 0.1204(4) 0.032(2) Uani 1 1 d . . . H15A H 1.3132 0.8298 0.0988 0.038 Uiso 1 1 calc R . . C16 C 1.2013(6) 0.8400(6) 0.1329(5) 0.031(2) Uani 1 1 d . . . H16A H 1.1825 0.7858 0.1194 0.038 Uiso 1 1 calc R . . C17 C 1.3963(7) 0.9718(8) 0.1235(5) 0.054(3) Uani 1 1 d . . . H17A H 1.4071 1.0290 0.1393 0.081 Uiso 1 1 calc R . . H17B H 1.3992 0.9692 0.0752 0.081 Uiso 1 1 calc R . . H17C H 1.4386 0.9344 0.1467 0.081 Uiso 1 1 calc R . . C21 C 0.9455(7) 0.9373(6) 0.2957(5) 0.037(3) Uani 1 1 d . . . C22 C 0.8622(7) 0.9530(7) 0.3005(5) 0.048(3) Uani 1 1 d . . . H22A H 0.8203 0.9308 0.2679 0.058 Uiso 1 1 calc R . . C23 C 0.8378(9) 1.0018(8) 0.3537(6) 0.063(4) Uani 1 1 d . . . H23A H 0.7801 1.0130 0.3563 0.076 Uiso 1 1 calc R . . C24 C 0.8992(9) 1.0331(8) 0.4016(6) 0.058(3) Uani 1 1 d . . . C25 C 0.9822(9) 1.0163(8) 0.3964(6) 0.059(3) Uani 1 1 d . . . H25A H 1.0243 1.0379 0.4293 0.071 Uiso 1 1 calc R . . C26 C 1.0059(8) 0.9689(7) 0.3446(5) 0.054(3) Uani 1 1 d . . . H26A H 1.0637 0.9578 0.3424 0.065 Uiso 1 1 calc R . . C27 C 0.8720(10) 1.0857(9) 0.4586(7) 0.089(5) Uani 1 1 d . . . H27A H 0.9218 1.1033 0.4884 0.133 Uiso 1 1 calc R . . H27B H 0.8355 1.0525 0.4839 0.133 Uiso 1 1 calc R . . H27C H 0.8414 1.1349 0.4400 0.133 Uiso 1 1 calc R . . C31 C 1.0075(6) 0.8438(5) -0.0043(4) 0.026(2) Uani 1 1 d . . . C32 C 0.9849(6) 0.9072(6) -0.0502(5) 0.035(2) Uani 1 1 d . . . H32A H 0.9409 0.9444 -0.0428 0.042 Uiso 1 1 calc R . . C33 C 1.0252(6) 0.9165(6) -0.1057(5) 0.039(3) Uani 1 1 d . . . H33A H 1.0070 0.9587 -0.1373 0.047 Uiso 1 1 calc R . . C34 C 1.0926(6) 0.8654(6) -0.1172(4) 0.031(2) Uani 1 1 d . . . C35 C 1.1144(6) 0.8048(6) -0.0692(5) 0.035(2) Uani 1 1 d . . . H35A H 1.1600 0.7689 -0.0749 0.042 Uiso 1 1 calc R . . C36 C 1.0739(6) 0.7939(6) -0.0140(5) 0.033(2) Uani 1 1 d . . . H36A H 1.0919 0.7516 0.0175 0.039 Uiso 1 1 calc R . . C37 C 1.1386(7) 0.8761(7) -0.1770(5) 0.049(3) Uani 1 1 d . . . H37A H 1.1834 0.8344 -0.1758 0.073 Uiso 1 1 calc R . . H37B H 1.1632 0.9320 -0.1764 0.073 Uiso 1 1 calc R . . H37C H 1.0994 0.8690 -0.2179 0.073 Uiso 1 1 calc R . . C41 C 0.7842(6) 0.9266(6) 0.0945(5) 0.033(2) Uani 1 1 d . . . C42 C 0.7192(6) 0.9162(7) 0.1328(5) 0.044(3) Uani 1 1 d . . . H42A H 0.7221 0.8723 0.1646 0.053 Uiso 1 1 calc R . . C43 C 0.6507(7) 0.9679(7) 0.1259(5) 0.050(3) Uani 1 1 d . . . H43A H 0.6065 0.9586 0.1524 0.060 Uiso 1 1 calc R . . C44 C 0.6451(7) 1.0341(7) 0.0804(5) 0.044(3) Uani 1 1 d . . . C45 C 0.7099(6) 1.0441(6) 0.0418(5) 0.037(3) Uani 1 1 d . . . H45A H 0.7075 1.0883 0.0102 0.045 Uiso 1 1 calc R . . C46 C 0.7782(6) 0.9906(6) 0.0484(5) 0.034(2) Uani 1 1 d . . . H46A H 0.8215 0.9981 0.0208 0.041 Uiso 1 1 calc R . . C47 C 0.5688(7) 1.0921(8) 0.0708(6) 0.062(4) Uani 1 1 d . . . H47A H 0.5770 1.1342 0.0369 0.093 Uiso 1 1 calc R . . H47B H 0.5625 1.1197 0.1133 0.093 Uiso 1 1 calc R . . H47C H 0.5182 1.0596 0.0561 0.093 Uiso 1 1 calc R . . N7 N 0.3564(5) 0.8426(5) 0.3527(4) 0.044(2) Uani 1 1 d . . . C50 C 0.6233(10) 0.8606(11) 0.2992(9) 0.106(6) Uani 1 1 d . . . H50A H 0.6843 0.8680 0.3080 0.160 Uiso 1 1 calc R . . H50B H 0.6058 0.8625 0.2508 0.160 Uiso 1 1 calc R . . H50C H 0.6079 0.8065 0.3168 0.160 Uiso 1 1 calc R . . C51 C 0.5827(8) 0.9250(8) 0.3308(7) 0.072(4) Uani 1 1 d . . . H51C H 0.6004 0.9791 0.3135 0.087 Uiso 1 1 calc R . . H51D H 0.6024 0.9233 0.3793 0.087 Uiso 1 1 calc R . . C52 C 0.4858(7) 0.9213(7) 0.3213(6) 0.055(3) Uani 1 1 d . . . H52A H 0.4635 0.9777 0.3283 0.067 Uiso 1 1 calc R . . H52B H 0.4663 0.9049 0.2745 0.067 Uiso 1 1 calc R . . C53 C 0.4506(7) 0.8619(7) 0.3676(5) 0.046(3) Uani 1 1 d . . . H53A H 0.4614 0.8846 0.4136 0.055 Uiso 1 1 calc R . . H53B H 0.4819 0.8088 0.3671 0.055 Uiso 1 1 calc R . . C54 C 0.4513(10) 0.7225(11) 0.1773(8) 0.103(6) Uani 1 1 d . . . H54A H 0.4502 0.7005 0.1318 0.154 Uiso 1 1 calc R . . H54B H 0.5053 0.7090 0.2033 0.154 Uiso 1 1 calc R . . H54C H 0.4440 0.7831 0.1755 0.154 Uiso 1 1 calc R . . C55 C 0.3826(12) 0.6847(8) 0.2094(7) 0.091(5) Uani 1 1 d . . . H55A H 0.3898 0.6235 0.2095 0.110 Uiso 1 1 calc R . . H55B H 0.3287 0.6974 0.1817 0.110 Uiso 1 1 calc R . . C56 C 0.3765(9) 0.7132(8) 0.2809(6) 0.070(4) Uani 1 1 d . . . H56A H 0.3433 0.6718 0.3030 0.085 Uiso 1 1 calc R . . H56B H 0.4337 0.7148 0.3058 0.085 Uiso 1 1 calc R . . C57 C 0.3360(8) 0.7988(7) 0.2853(5) 0.057(3) Uani 1 1 d . . . H57A H 0.2743 0.7924 0.2759 0.068 Uiso 1 1 calc R . . H57B H 0.3544 0.8349 0.2500 0.068 Uiso 1 1 calc R . . C58 C 0.2706(10) 1.1059(8) 0.4648(7) 0.084(5) Uani 1 1 d . . . H58A H 0.2334 1.1543 0.4569 0.126 Uiso 1 1 calc R . . H58B H 0.3290 1.1248 0.4739 0.126 Uiso 1 1 calc R . . H58C H 0.2556 1.0745 0.5033 0.126 Uiso 1 1 calc R . . C59 C 0.2611(7) 1.0509(7) 0.4038(6) 0.052(3) Uani 1 1 d . . . H59A H 0.2017 1.0331 0.3943 0.062 Uiso 1 1 calc R . . H59B H 0.2751 1.0834 0.3649 0.062 Uiso 1 1 calc R . . C60 C 0.3155(6) 0.9761(6) 0.4119(5) 0.041(3) Uani 1 1 d . . . H60A H 0.2995 0.9417 0.4491 0.050 Uiso 1 1 calc R . . H60B H 0.3747 0.9935 0.4235 0.050 Uiso 1 1 calc R . . C61 C 0.3080(7) 0.9251(6) 0.3495(5) 0.045(3) Uani 1 1 d . . . H61A H 0.3272 0.9595 0.3135 0.054 Uiso 1 1 calc R . . H61B H 0.2477 0.9128 0.3364 0.054 Uiso 1 1 calc R . . C62 C 0.1322(8) 0.6890(7) 0.4608(6) 0.065(4) Uani 1 1 d . . . H62A H 0.1247 0.6494 0.4965 0.097 Uiso 1 1 calc R . . H62B H 0.1096 0.6651 0.4175 0.097 Uiso 1 1 calc R . . H62C H 0.1025 0.7409 0.4681 0.097 Uiso 1 1 calc R . . C63 C 0.2245(7) 0.7070(7) 0.4609(6) 0.052(3) Uani 1 1 d . . . H63A H 0.2545 0.6543 0.4544 0.062 Uiso 1 1 calc R . . H63B H 0.2473 0.7301 0.5050 0.062 Uiso 1 1 calc R . . C64 C 0.2412(7) 0.7695(7) 0.4054(5) 0.051(3) Uani 1 1 d . . . H64A H 0.2207 0.7458 0.3610 0.062 Uiso 1 1 calc R . . H64B H 0.2099 0.8218 0.4109 0.062 Uiso 1 1 calc R . . C65 C 0.3337(7) 0.7884(7) 0.4087(5) 0.045(3) Uani 1 1 d . . . H65A H 0.3524 0.8164 0.4518 0.054 Uiso 1 1 calc R . . H65B H 0.3648 0.7352 0.4081 0.054 Uiso 1 1 calc R . . C99 C 0.418(4) 0.691(5) 0.947(4) 0.09(3) Uani 0.182(8) 1 d P . . H51A H 0.4581 0.7197 0.9206 0.102 Uiso 0.182(8) 1 calc PR . . H51B H 0.4204 0.6307 0.9375 0.102 Uiso 0.182(8) 1 calc PR . . Cl98 Cl 0.4469(18) 0.7091(18) 1.0320(14) 0.120(11) Uani 0.182(8) 1 d P . . Cl99 Cl 0.3183(13) 0.7279(15) 0.9237(14) 0.108(11) Uani 0.182(8) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0340(5) 0.0353(5) 0.0354(4) 0.0091(4) -0.0013(4) -0.0060(4) Rh1 0.0294(4) 0.0177(4) 0.0270(4) 0.0037(3) -0.0093(3) -0.0018(3) I1 0.0790(6) 0.0450(5) 0.0521(5) 0.0018(4) -0.0194(4) -0.0075(4) I2 0.0541(5) 0.0350(4) 0.0456(4) 0.0098(3) -0.0211(4) -0.0004(3) N1 0.027(5) 0.027(4) 0.029(4) 0.008(4) -0.010(4) 0.000(4) N2 0.026(5) 0.033(5) 0.029(4) 0.001(4) 0.001(4) 0.005(4) N3 0.033(5) 0.031(5) 0.033(5) -0.004(4) -0.002(4) 0.000(4) N4 0.033(5) 0.020(4) 0.029(4) -0.002(3) -0.009(4) -0.002(3) N5 0.023(5) 0.025(4) 0.036(5) 0.004(4) -0.010(4) 0.004(4) N6 0.026(5) 0.031(5) 0.027(4) 0.000(4) 0.001(4) -0.004(4) C3 0.054(9) 0.086(11) 0.087(11) 0.055(9) 0.009(8) -0.012(8) C4 0.27(3) 0.142(19) 0.092(14) 0.050(14) 0.008(18) -0.16(2) C5 0.067(9) 0.051(8) 0.091(11) 0.014(8) 0.009(8) -0.022(7) C11 0.025(6) 0.029(5) 0.030(5) 0.006(4) -0.007(4) -0.005(4) C12 0.051(7) 0.020(5) 0.037(6) -0.001(4) -0.015(5) -0.003(5) C13 0.038(7) 0.034(6) 0.042(6) -0.001(5) -0.007(5) -0.011(5) C14 0.035(6) 0.042(7) 0.035(6) 0.011(5) -0.011(5) -0.015(5) C15 0.033(6) 0.034(6) 0.025(5) -0.002(4) -0.007(4) 0.003(5) C16 0.031(6) 0.028(5) 0.033(5) -0.002(4) -0.006(4) -0.010(4) C17 0.044(7) 0.072(9) 0.043(7) 0.011(6) -0.004(6) -0.016(6) C21 0.051(7) 0.025(5) 0.034(6) 0.009(5) 0.001(5) -0.001(5) C22 0.047(8) 0.053(8) 0.042(7) 0.008(6) -0.005(6) -0.001(6) C23 0.089(11) 0.056(8) 0.048(7) 0.008(6) 0.027(8) 0.019(7) C24 0.071(10) 0.059(8) 0.041(7) -0.007(6) -0.010(7) 0.016(7) C25 0.068(10) 0.057(8) 0.051(7) -0.008(6) -0.002(7) 0.008(7) C26 0.054(8) 0.060(8) 0.045(7) -0.012(6) 0.000(6) 0.009(6) C27 0.110(13) 0.088(11) 0.069(10) -0.023(9) 0.016(9) 0.034(10) C31 0.023(5) 0.026(5) 0.026(5) 0.006(4) -0.002(4) -0.002(4) C32 0.039(6) 0.034(6) 0.029(5) -0.003(5) -0.004(5) -0.001(5) C33 0.042(7) 0.034(6) 0.038(6) 0.013(5) -0.005(5) 0.001(5) C34 0.036(6) 0.029(5) 0.028(5) -0.009(4) 0.001(5) -0.016(5) C35 0.035(6) 0.028(6) 0.039(6) -0.005(5) -0.008(5) 0.005(4) C36 0.035(6) 0.034(6) 0.026(5) -0.001(4) -0.004(5) 0.004(5) C37 0.060(8) 0.045(7) 0.039(6) -0.003(5) 0.001(6) -0.009(6) C41 0.039(6) 0.031(6) 0.026(5) 0.002(4) -0.012(5) 0.002(5) C42 0.034(7) 0.054(7) 0.045(6) 0.014(5) 0.012(5) 0.015(5) C43 0.041(7) 0.069(9) 0.041(6) 0.009(6) 0.007(6) -0.004(6) C44 0.036(7) 0.058(8) 0.037(6) -0.014(6) 0.000(5) 0.011(5) C45 0.033(6) 0.040(6) 0.037(6) -0.005(5) -0.002(5) 0.002(5) C46 0.026(6) 0.044(6) 0.031(5) -0.010(5) 0.001(4) 0.000(5) C47 0.051(8) 0.068(9) 0.065(8) -0.012(7) -0.001(7) 0.022(7) N7 0.040(6) 0.037(5) 0.049(5) 0.004(4) -0.022(4) -0.002(4) C50 0.079(12) 0.121(15) 0.119(14) -0.008(12) 0.012(11) 0.004(11) C51 0.066(10) 0.059(9) 0.090(11) -0.014(8) 0.003(8) 0.013(7) C52 0.065(9) 0.047(7) 0.052(7) -0.002(6) 0.001(6) -0.007(6) C53 0.049(7) 0.039(6) 0.045(6) -0.003(5) -0.016(5) 0.004(5) C54 0.098(14) 0.109(15) 0.095(13) -0.018(11) -0.012(11) 0.020(11) C55 0.147(17) 0.045(9) 0.070(10) 0.007(7) -0.034(10) 0.012(9) C56 0.112(12) 0.045(8) 0.047(7) -0.006(6) -0.021(8) 0.011(7) C57 0.087(10) 0.039(7) 0.036(6) 0.003(5) -0.024(6) -0.013(6) C58 0.107(13) 0.039(8) 0.109(12) 0.003(8) 0.031(10) 0.004(8) C59 0.045(7) 0.045(7) 0.066(8) 0.015(6) 0.008(6) 0.008(6) C60 0.036(6) 0.026(6) 0.058(7) -0.001(5) -0.007(5) -0.004(5) C61 0.037(7) 0.027(6) 0.065(7) 0.011(5) -0.020(6) 0.000(5) C62 0.080(10) 0.050(8) 0.060(8) -0.003(6) -0.009(7) -0.021(7) C63 0.068(9) 0.029(6) 0.054(7) 0.002(5) -0.015(6) -0.011(6) C64 0.055(8) 0.047(7) 0.044(6) 0.015(5) -0.028(6) -0.005(6) C65 0.049(7) 0.037(6) 0.045(6) 0.011(5) -0.012(5) 0.005(5) C99 0.05(5) 0.10(6) 0.12(7) 0.00(5) 0.02(5) -0.05(4) Cl98 0.13(2) 0.12(2) 0.11(2) 0.007(17) 0.006(17) 0.014(18) Cl99 0.053(14) 0.098(19) 0.17(3) 0.039(17) 0.019(15) 0.003(12) _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 C4 2.090(14) . ? Pd1 N6 2.100(7) . ? Pd1 N3 2.116(8) . ? Pd1 C5 2.118(12) . ? Pd1 C3 2.139(12) . ? Pd1 Rh1 2.8404(11) . ? Rh1 N1 2.052(8) . ? Rh1 N4 2.064(7) . ? Rh1 I1 2.5927(11) . ? Rh1 I2 2.6165(9) . ? N1 N2 1.300(10) . ? N1 C11 1.433(11) . ? N2 N3 1.281(10) . ? N3 C21 1.439(12) . ? N4 N5 1.305(10) . ? N4 C31 1.445(11) . ? N5 N6 1.301(10) . ? N6 C41 1.442(12) . ? C3 C4 1.26(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.29(2) . ? C4 H4A 1.0000 . ? C5 H5B 0.9900 . ? C5 H5C 0.9900 . ? C11 C16 1.380(13) . ? C11 C12 1.426(12) . ? C12 C13 1.386(14) . ? C12 H12A 0.9500 . ? C13 C14 1.350(14) . ? C13 H13A 0.9500 . ? C14 C15 1.371(13) . ? C14 C17 1.538(14) . ? C15 C16 1.366(13) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.374(14) . ? C21 C26 1.390(15) . ? C22 C23 1.420(15) . ? C22 H22A 0.9500 . ? C23 C24 1.385(17) . ? C23 H23A 0.9500 . ? C24 C25 1.374(17) . ? C24 C27 1.532(16) . ? C25 C26 1.383(15) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C36 1.365(12) . ? C31 C32 1.392(12) . ? C32 C33 1.367(13) . ? C32 H32A 0.9500 . ? C33 C34 1.399(14) . ? C33 H33A 0.9500 . ? C34 C35 1.387(13) . ? C34 C37 1.496(13) . ? C35 C36 1.364(13) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C46 1.380(13) . ? C41 C42 1.381(13) . ? C42 C43 1.370(14) . ? C42 H42A 0.9500 . ? C43 C44 1.401(15) . ? C43 H43A 0.9500 . ? C44 C45 1.380(14) . ? C44 C47 1.530(14) . ? C45 C46 1.385(13) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? N7 C65 1.503(13) . ? N7 C57 1.527(13) . ? N7 C61 1.534(12) . ? N7 C53 1.535(13) . ? C50 C51 1.414(18) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.544(16) . ? C51 H51C 0.9900 . ? C51 H51D 0.9900 . ? C52 C53 1.494(14) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.47(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.527(17) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.526(16) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.506(17) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.482(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.491(14) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.507(16) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.550(14) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.508(15) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C99 Cl99 1.72(8) . ? C99 Cl98 1.74(8) . ? C99 H51A 0.9900 . ? C99 H51B 0.9900 . ? 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 C4 Pd1 N6 136.3(7) . . ? C4 Pd1 N3 130.8(7) . . ? N6 Pd1 N3 92.9(3) . . ? C4 Pd1 C5 35.7(7) . . ? N6 Pd1 C5 101.2(5) . . ? N3 Pd1 C5 164.8(5) . . ? C4 Pd1 C3 34.7(6) . . ? N6 Pd1 C3 167.8(4) . . ? N3 Pd1 C3 96.9(5) . . ? C5 Pd1 C3 68.4(6) . . ? C4 Pd1 Rh1 104.6(8) . . ? N6 Pd1 Rh1 79.2(2) . . ? N3 Pd1 Rh1 79.3(2) . . ? C5 Pd1 Rh1 108.7(4) . . ? C3 Pd1 Rh1 109.7(4) . . ? N1 Rh1 N4 87.9(3) . . ? N1 Rh1 I1 179.1(2) . . ? N4 Rh1 I1 91.9(2) . . ? N1 Rh1 I2 88.41(19) . . ? N4 Rh1 I2 175.8(2) . . ? I1 Rh1 I2 91.77(3) . . ? N1 Rh1 Pd1 83.0(2) . . ? N4 Rh1 Pd1 84.4(2) . . ? I1 Rh1 Pd1 97.80(3) . . ? I2 Rh1 Pd1 97.07(3) . . ? N2 N1 C11 113.8(8) . . ? N2 N1 Rh1 127.5(6) . . ? C11 N1 Rh1 118.4(6) . . ? N3 N2 N1 118.7(8) . . ? N2 N3 C21 110.6(8) . . ? N2 N3 Pd1 129.8(6) . . ? C21 N3 Pd1 119.6(6) . . ? N5 N4 C31 112.8(7) . . ? N5 N4 Rh1 126.1(6) . . ? C31 N4 Rh1 121.1(6) . . ? N6 N5 N4 119.2(7) . . ? N5 N6 C41 109.4(7) . . ? N5 N6 Pd1 131.0(6) . . ? C41 N6 Pd1 119.7(6) . . ? C4 C3 Pd1 70.5(9) . . ? C4 C3 H3A 116.6 . . ? Pd1 C3 H3A 116.6 . . ? C4 C3 H3B 116.6 . . ? Pd1 C3 H3B 116.6 . . ? H3A C3 H3B 113.6 . . ? C3 C4 C5 139(2) . . ? C3 C4 Pd1 74.7(9) . . ? C5 C4 Pd1 73.4(9) . . ? C3 C4 H4A 106.2 . . ? C5 C4 H4A 106.2 . . ? Pd1 C4 H4A 106.2 . . ? C4 C5 Pd1 71.0(9) . . ? C4 C5 H5B 116.5 . . ? Pd1 C5 H5B 116.5 . . ? C4 C5 H5C 116.5 . . ? Pd1 C5 H5C 116.5 . . ? H5B C5 H5C 113.5 . . ? C16 C11 C12 117.6(9) . . ? C16 C11 N1 120.7(8) . . ? C12 C11 N1 121.6(9) . . ? C13 C12 C11 119.4(10) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C12 121.5(10) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 118.8(9) . . ? C13 C14 C17 120.8(10) . . ? C15 C14 C17 120.4(10) . . ? C16 C15 C14 122.1(10) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C15 C16 C11 120.4(9) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C21 C26 118.8(10) . . ? C22 C21 N3 117.7(10) . . ? C26 C21 N3 123.5(10) . . ? C21 C22 C23 121.0(11) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 119.1(12) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C23 119.3(11) . . ? C25 C24 C27 122.1(12) . . ? C23 C24 C27 118.6(12) . . ? C24 C25 C26 121.6(12) . . ? C24 C25 H25A 119.2 . . ? C26 C25 H25A 119.2 . . ? C25 C26 C21 120.2(12) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C36 C31 C32 118.6(9) . . ? C36 C31 N4 118.8(8) . . ? C32 C31 N4 122.5(8) . . ? C33 C32 C31 120.8(9) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C34 121.6(9) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 115.4(9) . . ? C35 C34 C37 122.4(9) . . ? C33 C34 C37 122.2(9) . . ? C36 C35 C34 123.6(9) . . ? C36 C35 H35A 118.2 . . ? C34 C35 H35A 118.2 . . ? C35 C36 C31 119.9(9) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C46 C41 C42 118.0(9) . . ? C46 C41 N6 123.4(9) . . ? C42 C41 N6 118.6(8) . . ? C43 C42 C41 121.4(10) . . ? C43 C42 H42A 119.3 . . ? C41 C42 H42A 119.3 . . ? C42 C43 C44 120.8(10) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C45 C44 C43 117.7(10) . . ? C45 C44 C47 120.2(11) . . ? C43 C44 C47 122.0(11) . . ? C44 C45 C46 120.9(10) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C41 C46 C45 121.1(10) . . ? C41 C46 H46A 119.4 . . ? C45 C46 H46A 119.4 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C65 N7 C57 110.8(8) . . ? C65 N7 C61 111.3(8) . . ? C57 N7 C61 108.0(8) . . ? C65 N7 C53 107.0(8) . . ? C57 N7 C53 111.4(9) . . ? C61 N7 C53 108.4(8) . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C50 C51 C52 115.4(12) . . ? C50 C51 H51C 108.4 . . ? C52 C51 H51C 108.4 . . ? C50 C51 H51D 108.4 . . ? C52 C51 H51D 108.4 . . ? H51C C51 H51D 107.5 . . ? C53 C52 C51 113.5(10) . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52B 108.9 . . ? C51 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 N7 116.4(9) . . ? C52 C53 H53A 108.2 . . ? N7 C53 H53A 108.2 . . ? C52 C53 H53B 108.2 . . ? N7 C53 H53B 108.2 . . ? H53A C53 H53B 107.3 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C54 C55 C56 115.4(14) . . ? C54 C55 H55A 108.4 . . ? C56 C55 H55A 108.4 . . ? C54 C55 H55B 108.4 . . ? C56 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C57 C56 C55 113.7(10) . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56B 108.8 . . ? C55 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C56 C57 N7 114.8(9) . . ? C56 C57 H57A 108.6 . . ? N7 C57 H57A 108.6 . . ? C56 C57 H57B 108.6 . . ? N7 C57 H57B 108.6 . . ? H57A C57 H57B 107.5 . . ? C59 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C58 112.7(10) . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59B 109.0 . . ? C58 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C59 C60 C61 111.5(9) . . ? C59 C60 H60A 109.3 . . ? C61 C60 H60A 109.3 . . ? C59 C60 H60B 109.3 . . ? C61 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C60 C61 N7 116.8(8) . . ? C60 C61 H61A 108.1 . . ? N7 C61 H61A 108.1 . . ? C60 C61 H61B 108.1 . . ? N7 C61 H61B 108.1 . . ? H61A C61 H61B 107.3 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C62 C63 C64 112.3(10) . . ? C62 C63 H63A 109.1 . . ? C64 C63 H63A 109.1 . . ? C62 C63 H63B 109.1 . . ? C64 C63 H63B 109.1 . . ? H63A C63 H63B 107.9 . . ? C65 C64 C63 110.8(8) . . ? C65 C64 H64A 109.5 . . ? C63 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? N7 C65 C64 114.3(8) . . ? N7 C65 H65A 108.7 . . ? C64 C65 H65A 108.7 . . ? N7 C65 H65B 108.7 . . ? C64 C65 H65B 108.7 . . ? H65A C65 H65B 107.6 . . ? Cl99 C99 Cl98 110(5) . . ? Cl99 C99 H51A 109.8 . . ? Cl98 C99 H51A 109.8 . . ? Cl99 C99 H51B 109.8 . . ? Cl98 C99 H51B 109.8 . . ? H51A C99 H51B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.150 _refine_diff_density_min -2.180 _refine_diff_density_rms 0.173 #===END #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 290021' _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 ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _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 1.013 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.010 _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 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) -0.0365(2) 0.0488(2) 0.0661(9) Uani 1 1 d . . . N3 N 1.0072(2) 0.3273(2) 0.19380(15) 0.0231(5) Uani 1 1 d . . . N2 N 0.9625(2) 0.3106(2) 0.11412(16) 0.0235(5) Uani 1 1 d . . . N1 N 0.8464(2) 0.2745(2) 0.07936(16) 0.0232(5) Uani 1 1 d . . . N6 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 . . . N4 N 0.6956(2) 0.3765(2) 0.15893(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 1.5359 0.4456 0.3875 0.077 Uiso 1 1 calc R . . H17B H 1.5575 0.4832 0.3118 0.077 Uiso 1 1 calc R . . H17C H 1.5270 0.3511 0.3043 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) 0.3547(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 1.2583 0.9484 0.4888 0.065 Uiso 1 1 calc R . . H37B H 1.2134 0.9860 0.4109 0.065 Uiso 1 1 calc R . . H37C H 1.3120 0.9277 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 0.2565 -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 0.3875 -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) 0.1170(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) 0.1193(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) 0.1276(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) 0.28532(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 1.6061 0.2362 0.5562 0.174 Uiso 1 1 calc R A 1 Cl2 Cl 1.43061(13) 0.26140(16) 0.52617(12) 0.1174(7) Uani 1 1 d . B . Cl3 Cl 1.5382(4) 0.1407(3) 0.4180(3) 0.0681(15) Uani 0.58(2) 1 d P B 1 Cl3' Cl 1.5496(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) 0.0681(19) 0.078(2) 0.0389(17) 0.0285(16) 0.0106(14) O2 0.0547(19) 0.0214(13) 0.091(2) -0.0029(14) -0.0029(17) 0.0135(13) N3 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) N1 0.0212(13) 0.0230(12) 0.0248(13) 0.0090(10) 0.0058(11) 0.0081(10) N6 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) N4 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) 0.0051(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) 0.0430(19) 0.0386(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) 0.0267(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) 0.0266(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) 0.0137(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) 0.0096(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) 0.0217(19) 0.0323(19) C56 0.0314(19) 0.0338(18) 0.0341(19) 0.0125(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) 0.0298(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) 0.0052(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) 0.0279(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) 0.0394(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 N3 2.037(2) . ? Pd1 N6 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 N4 2.090(2) . ? Rh1 N1 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) . ? N3 N2 1.292(3) . ? N3 C11 1.434(4) . ? N2 N1 1.307(3) . ? N1 C21 1.440(4) . ? N6 N5 1.296(3) . ? N6 C31 1.436(4) . ? N5 N4 1.305(3) . ? N4 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 1.391(4) . ? C41 C46 1.396(4) . ? C42 C43 1.388(4) . ? C43 C44 1.391(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 N3 Pd1 N6 86.78(10) . . ? N3 Pd1 P1 92.94(7) . . ? N6 Pd1 P1 176.77(7) . . ? N3 Pd1 Cl1 174.09(7) . . ? N6 Pd1 Cl1 88.81(7) . . ? P1 Pd1 Cl1 91.25(3) . . ? N3 Pd1 Rh1 84.57(7) . . ? N6 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 N4 170.20(13) . . ? C1 Rh1 N4 91.08(12) . . ? C2 Rh1 N1 90.86(13) . . ? C1 Rh1 N1 178.60(12) . . ? N4 Rh1 N1 87.91(9) . . ? C2 Rh1 Pd1 106.89(10) . . ? C1 Rh1 Pd1 103.10(11) . . ? N4 Rh1 Pd1 82.35(7) . . ? N1 Rh1 Pd1 77.73(7) . . ? C61 P1 C51 104.48(14) . . ? C61 P1 C71 103.51(13) . . ? C51 P1 C71 102.76(14) . . ? C61 P1 Pd1 112.16(10) . . ? C51 P1 Pd1 115.45(10) . . ? C71 P1 Pd1 116.97(10) . . ? N2 N3 C11 113.5(2) . . ? N2 N3 Pd1 126.00(19) . . ? C11 N3 Pd1 120.34(19) . . ? N3 N2 N1 118.4(2) . . ? N2 N1 C21 111.4(2) . . ? N2 N1 Rh1 129.66(19) . . ? C21 N1 Rh1 118.86(19) . . ? N5 N6 C31 111.2(2) . . ? N5 N6 Pd1 129.86(19) . . ? C31 N6 Pd1 118.92(18) . . ? N6 N5 N4 117.5(2) . . ? N5 N4 C41 111.8(2) . . ? N5 N4 Rh1 126.13(18) . . ? C41 N4 Rh1 121.65(18) . . ? O1 C1 Rh1 179.2(4) . . ? O2 C2 Rh1 175.0(3) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 N3 118.4(3) . . ? C16 C11 N3 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 N1 118.9(3) . . ? C22 C21 N1 122.2(3) . . ? C23 C22 C21 120.1(3) . . ? C24 C23 C22 121.8(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 N6 119.7(3) . . ? C32 C31 N6 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 N4 123.2(3) . . ? C46 C41 N4 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 120.8(3) . . ? Cl3' C101 Cl3 11.8(8) . . ? Cl3' C101 Cl2 119.3(5) . . ? Cl3 C101 Cl2 115.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Pd1 N3 -12.67(9) . . . . ? N4 Rh1 Pd1 N6 -14.46(10) . . . . ? C1 Rh1 Pd1 P1 76.79(11) . . . . ? C2 Rh1 Pd1 Cl1 -110.64(13) . . . . ? _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