Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email BHKENLO@CITYU.EDU.HK _publ_contact_author_name 'Dr Kenneth Kam-Wing Lo' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Biology and Chemistry City University of Hong Kong Tat Chee Avenue Kowloon Hong Kong CHINA ; _publ_section_title ; Luminescent Cyclometallated Rhodium(III) Bis(pyridylbenzaldehyde) Complexes with Long-lived Excited States ; loop_ _publ_author_name 'Kenneth Kam-Wing Lo' 'Kin-Wai Lau' 'Chi-Kwan Li' 'Nianyong Zhu' data_mar975 _database_code_CSD 219240 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H38 Cl4 N4 O5 Rh2' _chemical_formula_sum 'C50 H38 Cl4 N4 O5 Rh2' _chemical_formula_weight 1122.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.769(2) _cell_length_b 12.909(3) _cell_length_c 18.272(4) _cell_angle_alpha 75.29(3) _cell_angle_beta 88.42(3) _cell_angle_gamma 70.97(3) _cell_volume 2318.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9859 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6014 _reflns_number_gt 3812 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0827P)^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 6014 _refine_ls_number_parameters 571 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.950 _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 0.72634(6) 0.42935(5) 0.74782(3) 0.0334(2) Uani 1 1 d . . . Rh2 Rh 0.60728(6) 0.18809(5) 0.73177(3) 0.0314(2) Uani 1 1 d . . . Cl1 Cl 0.82387(17) 0.21478(15) 0.76374(11) 0.0371(5) Uani 1 1 d . . . Cl2 Cl 0.51267(18) 0.40096(16) 0.71659(12) 0.0404(5) Uani 1 1 d . . . O1 O 0.4319(7) 0.8133(6) 0.8627(4) 0.070(2) Uani 1 1 d . . . O2 O 1.1597(7) 0.5906(7) 0.6508(4) 0.075(2) Uani 1 1 d . . . O3 O 0.7928(7) -0.2735(6) 0.9228(4) 0.078(2) Uani 1 1 d . . . O4 O 0.2391(7) 0.1261(7) 0.5316(4) 0.076(2) Uani 1 1 d . . . N1 N 0.7632(6) 0.4698(5) 0.6350(3) 0.0349(15) Uani 1 1 d . . . N2 N 0.7016(7) 0.4031(5) 0.8623(4) 0.0414(17) Uani 1 1 d . . . N3 N 0.6439(6) 0.2063(6) 0.6183(4) 0.0389(16) Uani 1 1 d . . . N4 N 0.5583(6) 0.1599(5) 0.8438(4) 0.0363(16) Uani 1 1 d . . . C1 C 0.8363(7) 0.3969(7) 0.5966(5) 0.040(2) Uani 1 1 d . . . H1 H 0.8727 0.3208 0.6224 0.048 Uiso 1 1 calc R . . C2 C 0.8595(8) 0.4290(7) 0.5221(5) 0.048(2) Uani 1 1 d . . . H2 H 0.9128 0.3765 0.4981 0.057 Uiso 1 1 calc R . . C3 C 0.8025(9) 0.5407(8) 0.4831(5) 0.056(2) Uani 1 1 d . . . H3 H 0.8137 0.5642 0.4315 0.067 Uiso 1 1 calc R . . C4 C 0.7283(9) 0.6180(7) 0.5211(5) 0.047(2) Uani 1 1 d . . . H4 H 0.6911 0.6941 0.4955 0.057 Uiso 1 1 calc R . . C5 C 0.7098(7) 0.5812(6) 0.5978(4) 0.0357(18) Uani 1 1 d . . . C6 C 0.6381(7) 0.6545(7) 0.6459(4) 0.0364(19) Uani 1 1 d . . . C7 C 0.6380(7) 0.5962(7) 0.7239(4) 0.0355(18) Uani 1 1 d . . . C8 C 0.5716(7) 0.6625(7) 0.7713(5) 0.0388(19) Uani 1 1 d . . . H8 H 0.5697 0.6281 0.8224 0.047 Uiso 1 1 calc R . . C9 C 0.5074(7) 0.7800(7) 0.7439(5) 0.0384(19) Uani 1 1 d . . . C10 C 0.5095(8) 0.8332(7) 0.6684(5) 0.043(2) Uani 1 1 d . . . H10 H 0.4665 0.9109 0.6505 0.052 Uiso 1 1 calc R . . C11 C 0.5767(8) 0.7701(7) 0.6183(4) 0.041(2) Uani 1 1 d . . . H11 H 0.5797 0.8056 0.5675 0.050 Uiso 1 1 calc R . . C12 C 0.4397(8) 0.8489(8) 0.7958(5) 0.051(2) Uani 1 1 d . . . H12 H 0.3998 0.9263 0.7749 0.061 Uiso 1 1 calc R . . C13 C 0.5910(9) 0.3956(6) 0.8966(5) 0.049(2) Uani 1 1 d . . . H13 H 0.5187 0.4016 0.8671 0.059 Uiso 1 1 calc R . . C14 C 0.5813(10) 0.3796(7) 0.9732(5) 0.057(3) Uani 1 1 d . . . H14 H 0.5037 0.3745 0.9950 0.068 Uiso 1 1 calc R . . C15 C 0.6869(12) 0.3710(9) 1.0178(6) 0.074(3) Uani 1 1 d . . . H15 H 0.6821 0.3591 1.0701 0.089 Uiso 1 1 calc R . . C16 C 0.8013(11) 0.3807(8) 0.9832(5) 0.062(3) Uani 1 1 d . . . H16 H 0.8734 0.3758 1.0124 0.074 Uiso 1 1 calc R . . C17 C 0.8077(9) 0.3977(7) 0.9048(5) 0.047(2) Uani 1 1 d . . . C18 C 0.9162(8) 0.4190(7) 0.8593(5) 0.041(2) Uani 1 1 d . . . C19 C 0.8924(8) 0.4485(6) 0.7803(4) 0.0376(19) Uani 1 1 d . . . C20 C 0.9810(7) 0.4870(7) 0.7349(5) 0.040(2) Uani 1 1 d . . . H20 H 0.9656 0.5083 0.6825 0.048 Uiso 1 1 calc R . . C21 C 1.0946(8) 0.4948(7) 0.7666(5) 0.045(2) Uani 1 1 d . . . C22 C 1.1215(8) 0.4586(8) 0.8445(6) 0.053(2) Uani 1 1 d . . . H22 H 1.1983 0.4602 0.8656 0.063 Uiso 1 1 calc R . . C23 C 1.0314(9) 0.4195(7) 0.8914(5) 0.054(3) Uani 1 1 d . . . H23 H 1.0490 0.3941 0.9436 0.065 Uiso 1 1 calc R . . C24 C 1.1810(9) 0.5475(8) 0.7180(6) 0.056(3) Uani 1 1 d . . . H24 H 1.2572 0.5476 0.7408 0.067 Uiso 1 1 calc R . . C25 C 0.6052(8) 0.3045(7) 0.5635(5) 0.047(2) Uani 1 1 d . . . H25 H 0.5560 0.3710 0.5759 0.057 Uiso 1 1 calc R . . C26 C 0.6372(9) 0.3087(9) 0.4890(5) 0.057(3) Uani 1 1 d . . . H26 H 0.6089 0.3772 0.4519 0.068 Uiso 1 1 calc R . . C27 C 0.7115(10) 0.2104(9) 0.4703(5) 0.060(3) Uani 1 1 d . . . H27 H 0.7372 0.2124 0.4211 0.072 Uiso 1 1 calc R . . C28 C 0.7465(9) 0.1106(9) 0.5252(5) 0.060(3) Uani 1 1 d . . . H28 H 0.7941 0.0435 0.5129 0.072 Uiso 1 1 calc R . . C29 C 0.7119(8) 0.1077(7) 0.5997(4) 0.0394(19) Uani 1 1 d . . . C30 C 0.7397(7) 0.0060(7) 0.6652(4) 0.0378(19) Uani 1 1 d . . . C31 C 0.6941(7) 0.0248(7) 0.7359(4) 0.0352(18) Uani 1 1 d . . . C32 C 0.7172(7) -0.0688(6) 0.7979(5) 0.0367(19) Uani 1 1 d . . . H32 H 0.6859 -0.0589 0.8444 0.044 Uiso 1 1 calc R . . C33 C 0.7867(7) -0.1776(7) 0.7910(5) 0.042(2) Uani 1 1 d . . . C34 C 0.8308(8) -0.1959(7) 0.7214(5) 0.046(2) Uani 1 1 d . . . H34 H 0.8760 -0.2690 0.7175 0.055 Uiso 1 1 calc R . . C35 C 0.8071(8) -0.1054(7) 0.6585(5) 0.046(2) Uani 1 1 d . . . H35 H 0.8352 -0.1172 0.6118 0.055 Uiso 1 1 calc R . . C36 C 0.8163(9) -0.2773(8) 0.8587(6) 0.057(3) Uani 1 1 d . . . H36 H 0.8566 -0.3486 0.8505 0.068 Uiso 1 1 calc R . . C37 C 0.6411(8) 0.1337(7) 0.9047(5) 0.043(2) Uani 1 1 d . . . H37 H 0.7302 0.1212 0.8979 0.051 Uiso 1 1 calc R . . C38 C 0.5965(9) 0.1250(7) 0.9772(5) 0.049(2) Uani 1 1 d . . . H38 H 0.6550 0.1063 1.0188 0.059 Uiso 1 1 calc R . . C39 C 0.4649(10) 0.1444(8) 0.9866(5) 0.056(3) Uani 1 1 d . . . H39 H 0.4330 0.1422 1.0346 0.067 Uiso 1 1 calc R . . C40 C 0.3779(9) 0.1677(8) 0.9241(5) 0.051(2) Uani 1 1 d . . . H40 H 0.2888 0.1795 0.9305 0.061 Uiso 1 1 calc R . . C41 C 0.4275(8) 0.1727(7) 0.8519(5) 0.041(2) Uani 1 1 d . . . C42 C 0.3546(7) 0.1824(6) 0.7815(5) 0.0365(19) Uani 1 1 d . . . C43 C 0.4302(7) 0.1752(6) 0.7173(4) 0.0361(19) Uani 1 1 d . . . C44 C 0.3725(8) 0.1631(7) 0.6546(5) 0.039(2) Uani 1 1 d . . . H44 H 0.4218 0.1534 0.6127 0.047 Uiso 1 1 calc R . . C45 C 0.2397(8) 0.1652(7) 0.6524(5) 0.044(2) Uani 1 1 d . . . C46 C 0.1644(9) 0.1833(7) 0.7142(5) 0.050(2) Uani 1 1 d . . . H46 H 0.0755 0.1914 0.7119 0.060 Uiso 1 1 calc R . . C47 C 0.2222(8) 0.1889(7) 0.7781(5) 0.052(2) Uani 1 1 d . . . H47 H 0.1728 0.1972 0.8200 0.063 Uiso 1 1 calc R . . C48 C 0.1822(10) 0.1483(8) 0.5861(6) 0.057(3) Uani 1 1 d . . . H48 H 0.0934 0.1554 0.5864 0.069 Uiso 1 1 calc R . . Cl3 Cl 0.1226(6) -0.0806(6) 0.6778(4) 0.112(3) Uiso 0.572(7) 1 d PD . . Cl4 Cl 0.1266(8) -0.2266(6) 0.8177(5) 0.139(3) Uiso 0.572(7) 1 d PD . . Cl3' Cl 0.1679(12) -0.1805(11) 0.7384(7) 0.180(6) Uiso 0.428(7) 1 d PD . . Cl4' Cl 0.0742(13) -0.1194(12) 0.8716(7) 0.184(6) Uiso 0.428(7) 1 d PD . . C49 C 0.0668(13) -0.0703(11) 0.7714(6) 0.105(4) Uiso 1 1 d D . . O5 O 0.9328(10) 0.8868(9) 0.9893(6) 0.152(4) Uiso 1 1 d . . . C50 C 0.9635(11) 0.9439(10) 1.0475(7) 0.085(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0396(4) 0.0282(4) 0.0311(4) -0.0066(3) 0.0059(3) -0.0105(3) Rh2 0.0337(4) 0.0288(4) 0.0307(4) -0.0067(3) 0.0058(3) -0.0099(3) Cl1 0.0325(10) 0.0309(11) 0.0459(12) -0.0094(9) 0.0039(9) -0.0085(8) Cl2 0.0354(11) 0.0317(11) 0.0504(13) -0.0088(9) 0.0061(9) -0.0080(8) O1 0.098(6) 0.064(5) 0.046(4) -0.021(4) 0.021(4) -0.022(4) O2 0.073(5) 0.110(6) 0.065(5) -0.035(5) 0.022(4) -0.052(4) O3 0.101(6) 0.042(4) 0.068(5) 0.002(4) -0.003(5) -0.005(4) O4 0.086(5) 0.091(6) 0.067(5) -0.028(4) 0.002(4) -0.045(4) N1 0.035(4) 0.040(4) 0.033(4) -0.013(3) 0.003(3) -0.015(3) N2 0.057(5) 0.025(4) 0.041(4) -0.011(3) 0.011(4) -0.010(3) N3 0.041(4) 0.045(4) 0.033(4) -0.009(3) 0.002(3) -0.019(3) N4 0.041(4) 0.027(4) 0.040(4) -0.008(3) 0.010(3) -0.012(3) C1 0.045(5) 0.032(5) 0.046(6) -0.015(4) 0.011(4) -0.013(4) C2 0.054(6) 0.044(6) 0.048(6) -0.023(4) 0.016(4) -0.014(4) C3 0.075(7) 0.064(7) 0.032(5) -0.010(5) 0.011(5) -0.029(5) C4 0.066(6) 0.036(5) 0.033(5) -0.001(4) 0.004(4) -0.013(4) C5 0.038(5) 0.029(5) 0.038(5) -0.006(4) 0.000(4) -0.011(3) C6 0.037(4) 0.038(5) 0.033(5) -0.005(4) 0.002(4) -0.013(4) C7 0.037(4) 0.035(5) 0.033(5) -0.005(4) 0.006(4) -0.014(3) C8 0.043(5) 0.037(5) 0.037(5) -0.009(4) 0.006(4) -0.014(4) C9 0.035(4) 0.035(5) 0.044(5) -0.013(4) 0.002(4) -0.009(3) C10 0.051(5) 0.029(5) 0.048(6) -0.011(4) 0.007(4) -0.011(4) C11 0.058(5) 0.033(5) 0.028(5) 0.000(4) 0.001(4) -0.015(4) C12 0.054(6) 0.045(6) 0.058(7) -0.017(5) 0.009(5) -0.018(4) C13 0.062(6) 0.024(5) 0.062(7) -0.016(4) 0.024(5) -0.014(4) C14 0.086(8) 0.039(6) 0.053(7) -0.019(5) 0.032(6) -0.029(5) C15 0.113(10) 0.060(7) 0.049(7) -0.012(5) 0.034(7) -0.032(6) C16 0.092(8) 0.054(7) 0.041(6) -0.011(5) 0.003(5) -0.025(5) C17 0.068(6) 0.027(5) 0.034(5) -0.005(4) 0.003(5) -0.001(4) C18 0.050(5) 0.033(5) 0.037(5) -0.008(4) -0.001(4) -0.010(4) C19 0.049(5) 0.021(4) 0.035(5) -0.007(3) 0.001(4) 0.000(3) C20 0.038(5) 0.043(5) 0.041(5) -0.016(4) -0.001(4) -0.009(4) C21 0.041(5) 0.040(5) 0.050(6) -0.012(4) -0.001(4) -0.009(4) C22 0.044(5) 0.051(6) 0.063(7) -0.020(5) -0.007(5) -0.011(4) C23 0.076(7) 0.033(5) 0.040(6) -0.004(4) -0.015(5) -0.004(5) C24 0.040(5) 0.071(7) 0.059(7) -0.029(6) 0.015(5) -0.012(5) C25 0.053(5) 0.045(5) 0.039(5) 0.004(4) -0.005(4) -0.021(4) C26 0.066(6) 0.066(7) 0.040(6) 0.000(5) 0.001(5) -0.035(5) C27 0.086(7) 0.065(7) 0.035(6) -0.012(5) 0.008(5) -0.034(6) C28 0.074(7) 0.067(7) 0.043(6) -0.026(5) 0.021(5) -0.022(5) C29 0.047(5) 0.044(5) 0.036(5) -0.020(4) 0.008(4) -0.021(4) C30 0.035(4) 0.043(5) 0.037(5) -0.011(4) -0.001(4) -0.014(4) C31 0.039(4) 0.041(5) 0.030(5) -0.011(4) 0.004(4) -0.017(4) C32 0.042(5) 0.031(5) 0.037(5) -0.011(4) 0.006(4) -0.010(4) C33 0.036(5) 0.031(5) 0.056(6) -0.010(4) 0.004(4) -0.006(4) C34 0.052(5) 0.029(5) 0.052(6) -0.015(4) 0.000(4) -0.003(4) C35 0.047(5) 0.045(6) 0.055(6) -0.030(5) 0.008(4) -0.014(4) C36 0.066(6) 0.031(5) 0.062(7) -0.003(5) 0.002(5) -0.007(4) C37 0.041(5) 0.045(5) 0.041(5) -0.010(4) 0.000(4) -0.013(4) C38 0.063(6) 0.049(6) 0.029(5) -0.006(4) 0.006(4) -0.014(4) C39 0.088(8) 0.052(6) 0.033(5) -0.015(4) 0.019(5) -0.028(5) C40 0.056(6) 0.058(6) 0.045(6) -0.020(5) 0.027(5) -0.024(5) C41 0.048(5) 0.030(5) 0.040(5) -0.008(4) 0.012(4) -0.008(4) C42 0.028(4) 0.033(5) 0.048(5) -0.008(4) 0.006(4) -0.012(3) C43 0.045(5) 0.016(4) 0.038(5) -0.001(3) 0.012(4) -0.004(3) C44 0.044(5) 0.039(5) 0.034(5) -0.005(4) 0.006(4) -0.017(4) C45 0.042(5) 0.041(5) 0.047(6) -0.003(4) -0.008(4) -0.015(4) C46 0.039(5) 0.044(6) 0.062(7) -0.011(5) 0.003(5) -0.009(4) C47 0.050(6) 0.047(6) 0.055(6) -0.013(5) 0.027(5) -0.012(4) C48 0.055(6) 0.051(6) 0.069(7) -0.016(5) -0.002(5) -0.021(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 Rh1 C7 1.986(8) . ? Rh1 C19 2.008(8) . ? Rh1 N1 2.056(6) . ? Rh1 N2 2.058(7) . ? Rh1 Cl2 2.546(2) . ? Rh1 Cl1 2.563(2) . ? Rh2 C31 1.990(8) . ? Rh2 C43 1.998(8) . ? Rh2 N3 2.068(6) . ? Rh2 N4 2.071(6) . ? Rh2 Cl2 2.544(2) . ? Rh2 Cl1 2.570(2) . ? O1 C12 1.202(10) . ? O2 C24 1.207(11) . ? O3 C36 1.202(11) . ? O4 C48 1.202(11) . ? N1 C1 1.349(9) . ? N1 C5 1.359(9) . ? N2 C13 1.351(10) . ? N2 C17 1.372(11) . ? N3 C25 1.349(10) . ? N3 C29 1.368(10) . ? N4 C37 1.346(9) . ? N4 C41 1.372(9) . ? C1 C2 1.360(11) . ? C2 C3 1.374(12) . ? C3 C4 1.386(12) . ? C4 C5 1.392(11) . ? C5 C6 1.475(11) . ? C6 C11 1.383(11) . ? C6 C7 1.432(10) . ? C7 C8 1.391(10) . ? C8 C9 1.408(10) . ? C9 C10 1.380(11) . ? C9 C12 1.479(11) . ? C10 C11 1.408(11) . ? C13 C14 1.367(12) . ? C14 C15 1.376(14) . ? C15 C16 1.397(14) . ? C16 C17 1.396(12) . ? C17 C18 1.474(12) . ? C18 C23 1.389(12) . ? C18 C19 1.406(11) . ? C19 C20 1.379(11) . ? C20 C21 1.411(11) . ? C21 C22 1.388(12) . ? C21 C24 1.476(12) . ? C22 C23 1.408(12) . ? C25 C26 1.387(12) . ? C26 C27 1.382(13) . ? C27 C28 1.363(12) . ? C28 C29 1.395(11) . ? C29 C30 1.487(11) . ? C30 C35 1.418(11) . ? C30 C31 1.421(11) . ? C31 C32 1.388(10) . ? C32 C33 1.395(10) . ? C33 C34 1.394(12) . ? C33 C36 1.495(12) . ? C34 C35 1.374(12) . ? C37 C38 1.387(11) . ? C38 C39 1.371(12) . ? C39 C40 1.405(12) . ? C40 C41 1.403(11) . ? C41 C42 1.482(11) . ? C42 C47 1.403(11) . ? C42 C43 1.416(10) . ? C43 C44 1.384(11) . ? C44 C45 1.422(11) . ? C45 C46 1.395(12) . ? C45 C48 1.471(12) . ? C46 C47 1.367(12) . ? Cl3 Cl3' 1.422(13) . ? Cl3 C49 1.819(11) . ? Cl4 Cl3' 1.533(14) . ? Cl4 Cl4' 1.831(13) . ? Cl4 C49 1.875(13) . ? Cl3' C49 1.721(13) . ? Cl4' C49 1.773(12) . ? O5 C50 1.535(14) . ? 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 C7 Rh1 C19 89.8(3) . . ? C7 Rh1 N1 81.1(3) . . ? C19 Rh1 N1 92.7(3) . . ? C7 Rh1 N2 94.8(3) . . ? C19 Rh1 N2 81.1(3) . . ? N1 Rh1 N2 172.6(3) . . ? C7 Rh1 Cl2 90.9(2) . . ? C19 Rh1 Cl2 175.9(2) . . ? N1 Rh1 Cl2 91.39(17) . . ? N2 Rh1 Cl2 94.9(2) . . ? C7 Rh1 Cl1 172.7(2) . . ? C19 Rh1 Cl1 95.9(2) . . ? N1 Rh1 Cl1 94.10(19) . . ? N2 Rh1 Cl1 90.51(18) . . ? Cl2 Rh1 Cl1 83.63(7) . . ? C31 Rh2 C43 90.9(3) . . ? C31 Rh2 N3 81.9(3) . . ? C43 Rh2 N3 93.2(3) . . ? C31 Rh2 N4 95.1(3) . . ? C43 Rh2 N4 81.5(3) . . ? N3 Rh2 N4 173.9(2) . . ? C31 Rh2 Cl2 174.2(2) . . ? C43 Rh2 Cl2 92.8(2) . . ? N3 Rh2 Cl2 93.4(2) . . ? N4 Rh2 Cl2 89.80(18) . . ? C31 Rh2 Cl1 93.2(2) . . ? C43 Rh2 Cl1 173.1(2) . . ? N3 Rh2 Cl1 92.81(18) . . ? N4 Rh2 Cl1 92.66(18) . . ? Cl2 Rh2 Cl1 83.56(7) . . ? Rh1 Cl1 Rh2 95.86(7) . . ? Rh2 Cl2 Rh1 96.94(7) . . ? C1 N1 C5 118.7(7) . . ? C1 N1 Rh1 125.9(5) . . ? C5 N1 Rh1 115.3(5) . . ? C13 N2 C17 119.5(8) . . ? C13 N2 Rh1 125.7(6) . . ? C17 N2 Rh1 114.7(6) . . ? C25 N3 C29 119.4(7) . . ? C25 N3 Rh2 125.7(6) . . ? C29 N3 Rh2 114.9(5) . . ? C37 N4 C41 120.9(7) . . ? C37 N4 Rh2 126.0(5) . . ? C41 N4 Rh2 113.1(5) . . ? N1 C1 C2 123.3(8) . . ? C1 C2 C3 118.6(8) . . ? C2 C3 C4 119.5(8) . . ? C3 C4 C5 119.7(8) . . ? N1 C5 C4 120.2(7) . . ? N1 C5 C6 114.4(7) . . ? C4 C5 C6 125.5(7) . . ? C11 C6 C7 122.7(7) . . ? C11 C6 C5 122.8(7) . . ? C7 C6 C5 114.5(7) . . ? C8 C7 C6 116.3(7) . . ? C8 C7 Rh1 129.1(6) . . ? C6 C7 Rh1 114.6(6) . . ? C7 C8 C9 121.8(8) . . ? C10 C9 C8 120.3(7) . . ? C10 C9 C12 119.0(8) . . ? C8 C9 C12 120.7(8) . . ? C9 C10 C11 120.1(8) . . ? C6 C11 C10 118.9(8) . . ? O1 C12 C9 125.6(9) . . ? N2 C13 C14 122.4(9) . . ? C13 C14 C15 119.7(9) . . ? C14 C15 C16 118.7(10) . . ? C17 C16 C15 120.1(10) . . ? N2 C17 C16 119.5(9) . . ? N2 C17 C18 113.7(7) . . ? C16 C17 C18 126.6(9) . . ? C23 C18 C19 121.0(8) . . ? C23 C18 C17 122.8(8) . . ? C19 C18 C17 116.0(7) . . ? C20 C19 C18 118.5(8) . . ? C20 C19 Rh1 127.9(6) . . ? C18 C19 Rh1 113.6(6) . . ? C19 C20 C21 121.1(8) . . ? C22 C21 C20 119.9(8) . . ? C22 C21 C24 119.5(8) . . ? C20 C21 C24 120.5(8) . . ? C21 C22 C23 119.4(8) . . ? C18 C23 C22 119.8(8) . . ? O2 C24 C21 124.5(9) . . ? N3 C25 C26 121.5(9) . . ? C27 C26 C25 119.5(9) . . ? C28 C27 C26 118.8(9) . . ? C27 C28 C29 120.8(9) . . ? N3 C29 C28 119.8(8) . . ? N3 C29 C30 113.0(7) . . ? C28 C29 C30 127.2(8) . . ? C35 C30 C31 120.6(8) . . ? C35 C30 C29 122.6(8) . . ? C31 C30 C29 116.8(7) . . ? C32 C31 C30 118.0(8) . . ? C32 C31 Rh2 128.7(6) . . ? C30 C31 Rh2 113.2(6) . . ? C31 C32 C33 120.7(8) . . ? C34 C33 C32 121.1(8) . . ? C34 C33 C36 118.5(8) . . ? C32 C33 C36 120.4(8) . . ? C35 C34 C33 119.7(8) . . ? C34 C35 C30 119.8(8) . . ? O3 C36 C33 125.8(9) . . ? N4 C37 C38 121.5(8) . . ? C39 C38 C37 118.9(8) . . ? C38 C39 C40 120.3(8) . . ? C41 C40 C39 119.0(8) . . ? N4 C41 C40 119.2(8) . . ? N4 C41 C42 114.2(7) . . ? C40 C41 C42 126.5(8) . . ? C47 C42 C43 120.5(8) . . ? C47 C42 C41 123.7(7) . . ? C43 C42 C41 115.6(6) . . ? C44 C43 C42 117.3(7) . . ? C44 C43 Rh2 129.8(6) . . ? C42 C43 Rh2 112.9(6) . . ? C43 C44 C45 121.8(8) . . ? C46 C45 C44 119.2(8) . . ? C46 C45 C48 120.2(8) . . ? C44 C45 C48 120.7(8) . . ? C47 C46 C45 119.6(8) . . ? C46 C47 C42 121.3(8) . . ? O4 C48 C45 126.1(9) . . ? Cl3' Cl3 C49 62.7(5) . . ? Cl3' Cl4 Cl4' 112.8(7) . . ? Cl3' Cl4 C49 59.6(5) . . ? Cl4' Cl4 C49 57.1(4) . . ? Cl3 Cl3' Cl4 137.7(9) . . ? Cl3 Cl3' C49 70.0(6) . . ? Cl4 Cl3' C49 70.1(6) . . ? C49 Cl4' Cl4 62.7(5) . . ? Cl3' C49 Cl4' 106.9(8) . . ? Cl3' C49 Cl3 47.3(5) . . ? Cl4' C49 Cl3 153.4(9) . . ? Cl3' C49 Cl4 50.2(6) . . ? Cl4' C49 Cl4 60.2(6) . . ? Cl3 C49 Cl4 96.5(7) . . ? _diffrn_measured_fraction_theta_max 0.709 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.709 _refine_diff_density_max 1.320 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.177 data_mar1016 _database_code_CSD 219241 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 Cl5 N4 O4 Rh' _chemical_formula_sum 'C38 H36 Cl5 N4 O4 Rh' _chemical_formula_weight 892.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 11.624(2) _cell_length_b 13.444(3) _cell_length_c 13.649(3) _cell_angle_alpha 83.27(3) _cell_angle_beta 83.22(3) _cell_angle_gamma 71.20(3) _cell_volume 1997.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(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 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12966 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.45 _reflns_number_total 6732 _reflns_number_gt 5463 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1447P)^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 6732 _refine_ls_number_parameters 463 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1985 _refine_ls_wR_factor_gt 0.1879 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.065 _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 0.76316(3) 0.34162(3) 0.73783(3) 0.03350(18) Uani 1 1 d . . . O1 O 0.1777(4) 0.4427(5) 0.6677(5) 0.0814(16) Uani 1 1 d . . . O2 O 0.6900(8) 0.6993(7) 0.9685(7) 0.126(3) Uani 1 1 d . . . N1 N 0.7910(4) 0.4759(3) 0.6642(3) 0.0362(9) Uani 1 1 d . . . N2 N 0.7141(4) 0.2198(4) 0.8144(3) 0.0396(10) Uani 1 1 d . . . N3 N 0.9495(4) 0.2714(4) 0.7748(3) 0.0390(10) Uani 1 1 d . . . N4 N 0.8524(4) 0.2537(3) 0.6130(3) 0.0361(9) Uani 1 1 d . . . C1 C 0.8971(5) 0.4961(5) 0.6500(4) 0.0445(13) Uani 1 1 d . . . H1 H 0.9654 0.4477 0.6764 0.053 Uiso 1 1 calc R . . C2 C 0.9079(6) 0.5862(5) 0.5976(5) 0.0567(16) Uani 1 1 d . . . H2 H 0.9829 0.5984 0.5886 0.068 Uiso 1 1 calc R . . C3 C 0.8074(6) 0.6589(5) 0.5580(5) 0.0581(16) Uani 1 1 d . . . H3 H 0.8133 0.7206 0.5222 0.070 Uiso 1 1 calc R . . C4 C 0.6999(6) 0.6382(5) 0.5727(5) 0.0523(15) Uani 1 1 d . . . H4 H 0.6309 0.6864 0.5469 0.063 Uiso 1 1 calc R . . C5 C 0.6915(4) 0.5465(4) 0.6253(4) 0.0391(12) Uani 1 1 d . . . C6 C 0.5815(4) 0.5129(4) 0.6431(4) 0.0393(12) Uani 1 1 d . . . C7 C 0.5974(4) 0.4125(4) 0.6922(4) 0.0344(11) Uani 1 1 d . . . C8 C 0.4974(5) 0.3756(4) 0.7024(4) 0.0402(12) Uani 1 1 d . . . H8 H 0.5055 0.3080 0.7320 0.048 Uiso 1 1 calc R . . C9 C 0.3848(5) 0.4377(5) 0.6692(4) 0.0440(13) Uani 1 1 d . . . C10 C 0.3708(5) 0.5377(5) 0.6237(5) 0.0531(15) Uani 1 1 d . . . H10 H 0.2957 0.5788 0.6021 0.064 Uiso 1 1 calc R . . C11 C 0.4675(5) 0.5763(5) 0.6102(5) 0.0524(15) Uani 1 1 d . . . H11 H 0.4585 0.6437 0.5797 0.063 Uiso 1 1 calc R . . C12 C 0.2827(5) 0.3928(6) 0.6835(5) 0.0589(16) Uani 1 1 d . . . H12 H 0.2997 0.3220 0.7061 0.071 Uiso 1 1 calc R . . C13 C 0.7125(6) 0.1326(5) 0.7747(5) 0.0508(14) Uani 1 1 d . . . H13 H 0.7380 0.1258 0.7079 0.061 Uiso 1 1 calc R . . C14 C 0.6751(6) 0.0536(5) 0.8285(5) 0.0622(18) Uani 1 1 d . . . H14 H 0.6788 -0.0070 0.7999 0.075 Uiso 1 1 calc R . . C15 C 0.6316(7) 0.0673(6) 0.9268(6) 0.071(2) Uani 1 1 d . . . H15 H 0.6036 0.0165 0.9651 0.085 Uiso 1 1 calc R . . C16 C 0.6305(7) 0.1547(6) 0.9659(5) 0.0662(19) Uani 1 1 d . . . H16 H 0.6015 0.1637 1.0318 0.079 Uiso 1 1 calc R . . C17 C 0.6718(5) 0.2328(5) 0.9100(4) 0.0489(14) Uani 1 1 d . . . C18 C 0.6683(5) 0.3347(5) 0.9421(4) 0.0497(14) Uani 1 1 d . . . C19 C 0.7017(5) 0.4039(4) 0.8669(4) 0.0413(12) Uani 1 1 d . . . C20 C 0.6978(5) 0.5034(5) 0.8937(4) 0.0473(13) Uani 1 1 d . . . H20 H 0.7169 0.5525 0.8463 0.057 Uiso 1 1 calc R . . C21 C 0.6650(6) 0.5272(6) 0.9917(5) 0.0591(17) Uani 1 1 d . . . C22 C 0.6332(6) 0.4591(6) 1.0627(5) 0.0651(19) Uani 1 1 d . . . H22 H 0.6108 0.4778 1.1274 0.078 Uiso 1 1 calc R . . C23 C 0.6341(6) 0.3621(6) 1.0387(5) 0.0616(17) Uani 1 1 d . . . H23 H 0.6119 0.3152 1.0869 0.074 Uiso 1 1 calc R . . C24 C 0.6621(8) 0.6279(7) 1.0228(8) 0.083(2) Uani 1 1 d . . . H24 H 0.6374 0.6400 1.0889 0.099 Uiso 1 1 calc R . . C25 C 0.9925(5) 0.2828(5) 0.8591(4) 0.0491(14) Uani 1 1 d . . . H25 H 0.9391 0.3232 0.9062 0.059 Uiso 1 1 calc R . . C26 C 1.1134(5) 0.2365(5) 0.8774(5) 0.0508(14) Uani 1 1 d . . . H26 H 1.1397 0.2442 0.9370 0.061 Uiso 1 1 calc R . . C27 C 1.1952(5) 0.1786(4) 0.8073(4) 0.0429(12) Uani 1 1 d . . . C28 C 1.1510(5) 0.1675(4) 0.7206(4) 0.0429(12) Uani 1 1 d . . . H28 H 1.2033 0.1289 0.6718 0.052 Uiso 1 1 calc R . . C29 C 1.0280(4) 0.2146(4) 0.7070(4) 0.0356(11) Uani 1 1 d . . . C30 C 0.9748(4) 0.2040(4) 0.6153(4) 0.0358(11) Uani 1 1 d . . . C31 C 1.0431(5) 0.1481(4) 0.5388(4) 0.0409(12) Uani 1 1 d . . . H31 H 1.1264 0.1148 0.5422 0.049 Uiso 1 1 calc R . . C32 C 0.9875(5) 0.1414(5) 0.4566(4) 0.0444(13) Uani 1 1 d . . . C33 C 0.8638(6) 0.1889(5) 0.4568(4) 0.0500(14) Uani 1 1 d . . . H33 H 0.8236 0.1837 0.4036 0.060 Uiso 1 1 calc R . . C34 C 0.7991(5) 0.2437(5) 0.5340(4) 0.0445(13) Uani 1 1 d . . . H34 H 0.7154 0.2751 0.5320 0.053 Uiso 1 1 calc R . . C35 C 1.3272(5) 0.1247(5) 0.8269(5) 0.0578(16) Uani 1 1 d . . . H35A H 1.3702 0.0885 0.7703 0.087 Uiso 1 1 calc R . . H35B H 1.3316 0.0749 0.8839 0.087 Uiso 1 1 calc R . . H35C H 1.3635 0.1765 0.8388 0.087 Uiso 1 1 calc R . . C36 C 1.0630(6) 0.0833(6) 0.3694(5) 0.0638(18) Uani 1 1 d . . . H36A H 1.0106 0.0865 0.3189 0.096 Uiso 1 1 calc R . . H36B H 1.1021 0.0109 0.3913 0.096 Uiso 1 1 calc R . . H36C H 1.1237 0.1158 0.3430 0.096 Uiso 1 1 calc R . . C37 C 1.5354(8) 0.1204(7) 0.3129(6) 0.085(2) Uani 1 1 d . . . H37A H 1.5366 0.0478 0.3288 0.102 Uiso 1 1 calc R . . H37B H 1.5123 0.1562 0.3733 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.53621(19) 0.14941(15) 0.57233(15) 0.0736(5) Uani 1 1 d . . . Cl2 Cl 1.4282(3) 0.1833(2) 0.22488(18) 0.0989(7) Uani 1 1 d . . . Cl3 Cl 1.6829(3) 0.1241(2) 0.26231(19) 0.1057(8) Uani 1 1 d . . . Cl4 Cl 0.9532(11) 0.2702(8) 1.1415(8) 0.181(4) Uiso 0.50 1 d PD A 1 Cl5 Cl 0.9811(7) 0.4638(6) 1.0640(6) 0.145(2) Uiso 0.50 1 d PD . 1 C38 C 0.941(5) 0.3942(17) 1.163(3) 0.212(9) Uiso 0.50 1 d PD A 1 H38A H 0.8576 0.4301 1.1862 0.255 Uiso 0.50 1 calc PR A 1 H38B H 0.9924 0.3913 1.2150 0.255 Uiso 0.50 1 calc PR A 1 Cl4' Cl 0.8780(13) 0.2816(11) 1.1820(10) 0.221(5) Uiso 0.50 1 d PD B 2 Cl5' Cl 1.0781(10) 0.3422(10) 1.1486(9) 0.215(4) Uiso 0.50 1 d PD B 2 C38' C 0.929(3) 0.383(3) 1.184(4) 0.212(9) Uiso 0.50 1 d PD B 2 H38C H 0.9153 0.4065 1.2505 0.255 Uiso 0.50 1 calc PR B 2 H38D H 0.8865 0.4418 1.1395 0.255 Uiso 0.50 1 calc PR B 2 O3' O 1.0289(10) -0.0079(10) 0.8949(9) 0.077(2) Uiso 0.50 1 d P C 2 O3 O 0.9754(10) 0.0077(10) 0.8973(9) 0.077(2) Uiso 0.50 1 d P D 1 O4 O 1.3309(4) 0.0734(4) 0.5105(5) 0.0804(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0272(3) 0.0381(3) 0.0341(3) -0.00315(17) -0.00154(16) -0.00891(18) O1 0.033(2) 0.091(4) 0.120(5) 0.004(3) -0.016(3) -0.020(2) O2 0.139(7) 0.113(6) 0.130(7) -0.058(5) -0.043(5) -0.016(5) N1 0.031(2) 0.041(2) 0.035(2) -0.0052(18) -0.0015(18) -0.0102(19) N2 0.035(2) 0.042(2) 0.040(2) 0.0009(19) -0.0013(19) -0.0115(19) N3 0.035(2) 0.042(2) 0.039(2) -0.0062(19) -0.0049(19) -0.0091(19) N4 0.030(2) 0.041(2) 0.036(2) -0.0019(18) -0.0048(17) -0.0099(19) C1 0.036(3) 0.050(3) 0.051(3) -0.004(3) -0.002(2) -0.019(3) C2 0.047(3) 0.060(4) 0.069(4) -0.003(3) 0.000(3) -0.028(3) C3 0.056(4) 0.049(3) 0.073(4) 0.004(3) -0.003(3) -0.026(3) C4 0.044(3) 0.044(3) 0.069(4) 0.005(3) -0.008(3) -0.017(3) C5 0.029(3) 0.040(3) 0.047(3) -0.004(2) -0.004(2) -0.009(2) C6 0.026(2) 0.043(3) 0.047(3) -0.003(2) -0.005(2) -0.008(2) C7 0.032(2) 0.038(3) 0.033(3) -0.007(2) 0.004(2) -0.013(2) C8 0.031(3) 0.042(3) 0.046(3) -0.002(2) -0.004(2) -0.010(2) C9 0.033(3) 0.053(3) 0.047(3) -0.005(3) -0.003(2) -0.015(2) C10 0.036(3) 0.056(4) 0.064(4) 0.001(3) -0.006(3) -0.012(3) C11 0.038(3) 0.046(3) 0.068(4) 0.013(3) -0.015(3) -0.008(3) C12 0.040(3) 0.069(4) 0.071(4) -0.003(3) -0.005(3) -0.022(3) C13 0.057(3) 0.046(3) 0.052(3) -0.001(3) -0.004(3) -0.020(3) C14 0.071(4) 0.050(4) 0.071(5) 0.004(3) -0.008(4) -0.029(3) C15 0.083(5) 0.070(5) 0.068(5) 0.017(4) -0.005(4) -0.043(4) C16 0.077(5) 0.076(5) 0.044(4) 0.012(3) 0.000(3) -0.030(4) C17 0.043(3) 0.059(4) 0.042(3) 0.004(3) -0.005(2) -0.015(3) C18 0.040(3) 0.064(4) 0.041(3) -0.006(3) -0.004(2) -0.011(3) C19 0.030(3) 0.050(3) 0.042(3) -0.005(2) -0.003(2) -0.009(2) C20 0.040(3) 0.054(3) 0.048(3) -0.014(3) -0.003(2) -0.011(3) C21 0.041(3) 0.071(4) 0.063(4) -0.026(3) -0.008(3) -0.006(3) C22 0.055(4) 0.089(5) 0.046(4) -0.021(4) 0.001(3) -0.012(4) C23 0.060(4) 0.083(5) 0.040(3) -0.009(3) 0.006(3) -0.023(4) C24 0.078(5) 0.074(5) 0.092(6) -0.028(5) -0.017(5) -0.008(5) C25 0.039(3) 0.062(4) 0.045(3) -0.013(3) -0.008(2) -0.010(3) C26 0.042(3) 0.058(4) 0.052(3) -0.006(3) -0.017(3) -0.010(3) C27 0.035(3) 0.043(3) 0.050(3) -0.002(2) -0.009(2) -0.009(2) C28 0.034(3) 0.047(3) 0.043(3) 0.001(2) -0.003(2) -0.006(2) C29 0.030(2) 0.040(3) 0.037(3) -0.002(2) -0.004(2) -0.011(2) C30 0.031(2) 0.038(3) 0.039(3) -0.003(2) 0.001(2) -0.012(2) C31 0.037(3) 0.039(3) 0.045(3) -0.005(2) 0.002(2) -0.011(2) C32 0.050(3) 0.047(3) 0.036(3) -0.005(2) 0.000(2) -0.016(3) C33 0.052(3) 0.060(4) 0.039(3) -0.004(3) -0.009(3) -0.018(3) C34 0.047(3) 0.052(3) 0.039(3) -0.009(2) -0.006(2) -0.019(3) C35 0.038(3) 0.066(4) 0.065(4) -0.009(3) -0.018(3) -0.005(3) C36 0.067(4) 0.070(4) 0.049(4) -0.023(3) 0.002(3) -0.011(4) C37 0.113(7) 0.083(6) 0.055(4) 0.007(4) -0.005(4) -0.030(5) Cl1 0.0862(13) 0.0688(11) 0.0729(12) -0.0176(9) -0.0138(10) -0.0274(10) Cl2 0.1135(18) 0.0967(16) 0.0807(15) 0.0002(12) -0.0133(13) -0.0255(14) Cl3 0.123(2) 0.129(2) 0.0836(15) 0.0009(14) -0.0242(14) -0.0623(18) O4 0.042(2) 0.075(3) 0.115(4) -0.017(3) 0.003(3) -0.006(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 Rh1 C7 1.992(5) . ? Rh1 C19 1.995(6) . ? Rh1 N2 2.040(4) . ? Rh1 N1 2.062(4) . ? Rh1 N4 2.153(4) . ? Rh1 N3 2.160(4) . ? O1 C12 1.219(7) . ? O2 C24 1.247(12) . ? N1 C1 1.334(7) . ? N1 C5 1.356(7) . ? N2 C17 1.349(7) . ? N2 C13 1.353(8) . ? N3 C29 1.338(7) . ? N3 C25 1.351(7) . ? N4 C34 1.346(7) . ? N4 C30 1.366(6) . ? C1 C2 1.366(9) . ? C2 C3 1.379(9) . ? C3 C4 1.353(8) . ? C4 C5 1.378(8) . ? C5 C6 1.474(7) . ? C6 C7 1.400(8) . ? C6 C11 1.416(8) . ? C7 C8 1.391(7) . ? C8 C9 1.401(8) . ? C9 C10 1.382(9) . ? C9 C12 1.480(8) . ? C10 C11 1.369(8) . ? C13 C14 1.378(9) . ? C14 C15 1.388(10) . ? C15 C16 1.342(11) . ? C16 C17 1.403(9) . ? C17 C18 1.474(9) . ? C18 C23 1.387(8) . ? C18 C19 1.408(8) . ? C19 C20 1.413(8) . ? C20 C21 1.392(9) . ? C21 C22 1.356(10) . ? C21 C24 1.454(11) . ? C22 C23 1.378(10) . ? C25 C26 1.381(8) . ? C26 C27 1.381(8) . ? C27 C28 1.386(8) . ? C27 C35 1.512(8) . ? C28 C29 1.389(7) . ? C29 C30 1.500(7) . ? C30 C31 1.375(7) . ? C31 C32 1.384(8) . ? C32 C33 1.372(8) . ? C32 C36 1.525(8) . ? C33 C34 1.362(8) . ? C37 Cl2 1.773(8) . ? C37 Cl3 1.785(9) . ? Cl4 C38 1.68(2) . ? Cl5 C38 1.66(2) . ? Cl5 Cl5 1.971(16) 2_767 ? Cl4' C38' 1.66(2) . ? Cl5' C38' 1.67(2) . ? 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 C7 Rh1 C19 88.2(2) . . ? C7 Rh1 N2 93.25(19) . . ? C19 Rh1 N2 80.7(2) . . ? C7 Rh1 N1 80.72(18) . . ? C19 Rh1 N1 95.5(2) . . ? N2 Rh1 N1 172.99(15) . . ? C7 Rh1 N4 100.81(18) . . ? C19 Rh1 N4 170.05(18) . . ? N2 Rh1 N4 94.45(17) . . ? N1 Rh1 N4 90.21(16) . . ? C7 Rh1 N3 174.65(18) . . ? C19 Rh1 N3 95.12(19) . . ? N2 Rh1 N3 91.44(17) . . ? N1 Rh1 N3 94.76(17) . . ? N4 Rh1 N3 76.23(16) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Rh1 125.7(4) . . ? C5 N1 Rh1 115.2(3) . . ? C17 N2 C13 118.9(5) . . ? C17 N2 Rh1 116.0(4) . . ? C13 N2 Rh1 125.0(4) . . ? C29 N3 C25 118.2(5) . . ? C29 N3 Rh1 116.7(3) . . ? C25 N3 Rh1 125.2(4) . . ? C34 N4 C30 117.6(5) . . ? C34 N4 Rh1 126.3(4) . . ? C30 N4 Rh1 116.1(3) . . ? N1 C1 C2 121.6(5) . . ? C1 C2 C3 119.9(6) . . ? C4 C3 C2 118.3(6) . . ? C3 C4 C5 120.7(6) . . ? N1 C5 C4 120.4(5) . . ? N1 C5 C6 113.6(5) . . ? C4 C5 C6 126.0(5) . . ? C7 C6 C11 121.9(5) . . ? C7 C6 C5 115.7(5) . . ? C11 C6 C5 122.4(5) . . ? C8 C7 C6 116.7(5) . . ? C8 C7 Rh1 128.8(4) . . ? C6 C7 Rh1 114.5(4) . . ? C7 C8 C9 121.6(5) . . ? C10 C9 C8 120.4(5) . . ? C10 C9 C12 121.3(6) . . ? C8 C9 C12 118.3(5) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 C6 119.5(6) . . ? O1 C12 C9 124.3(7) . . ? N2 C13 C14 123.1(6) . . ? C13 C14 C15 117.8(7) . . ? C16 C15 C14 119.3(6) . . ? C15 C16 C17 121.7(7) . . ? N2 C17 C16 119.2(6) . . ? N2 C17 C18 113.7(5) . . ? C16 C17 C18 126.9(6) . . ? C23 C18 C19 121.8(6) . . ? C23 C18 C17 123.3(6) . . ? C19 C18 C17 114.9(5) . . ? C18 C19 C20 117.1(5) . . ? C18 C19 Rh1 114.4(4) . . ? C20 C19 Rh1 128.3(4) . . ? C21 C20 C19 119.4(6) . . ? C22 C21 C20 122.3(7) . . ? C22 C21 C24 116.5(7) . . ? C20 C21 C24 121.2(8) . . ? C21 C22 C23 119.7(6) . . ? C22 C23 C18 119.7(7) . . ? O2 C24 C21 125.6(9) . . ? N3 C25 C26 122.1(5) . . ? C25 C26 C27 120.0(6) . . ? C26 C27 C28 117.8(5) . . ? C26 C27 C35 121.0(5) . . ? C28 C27 C35 121.1(5) . . ? C27 C28 C29 119.6(5) . . ? N3 C29 C28 122.3(5) . . ? N3 C29 C30 115.7(4) . . ? C28 C29 C30 121.9(5) . . ? N4 C30 C31 121.9(5) . . ? N4 C30 C29 115.2(4) . . ? C31 C30 C29 122.9(4) . . ? C30 C31 C32 119.7(5) . . ? C33 C32 C31 117.7(5) . . ? C33 C32 C36 122.0(5) . . ? C31 C32 C36 120.3(5) . . ? C34 C33 C32 120.9(5) . . ? N4 C34 C33 122.1(5) . . ? Cl2 C37 Cl3 109.1(4) . . ? C38 Cl5 Cl5 172.3(19) . 2_767 ? Cl5 C38 Cl4 114(2) . . ? Cl4' C38' Cl5' 106.8(18) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 1.469 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.150 data_mar977 _database_code_CSD 219242 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 Cl N4 O4 Rh' _chemical_formula_sum 'C36 H28 Cl N4 O4 Rh' _chemical_formula_weight 718.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 9.838(2) _cell_length_b 10.038(2) _cell_length_c 16.961(3) _cell_angle_alpha 72.98(3) _cell_angle_beta 86.01(3) _cell_angle_gamma 86.16(3) _cell_volume 1595.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4625 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.90 _reflns_number_total 2662 _reflns_number_gt 1760 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0558P)^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 2662 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 0.74460(10) 0.24029(10) 0.23883(5) 0.0502(4) Uani 1 1 d . . . O1 O 0.714(2) 0.841(2) 0.1341(12) 0.119(7) Uiso 0.50 1 d P A 1 O1' O 0.5726(19) 0.916(2) 0.0438(11) 0.102(6) Uiso 0.50 1 d P A 2 O2 O 0.9118(8) 0.1234(8) -0.1259(5) 0.079(2) Uiso 1 1 d . . . N1 N 0.6566(8) 0.2257(9) 0.3620(5) 0.047(2) Uiso 1 1 d . . . N2 N 0.8468(9) 0.0530(9) 0.3135(5) 0.057(2) Uiso 1 1 d . . . N3 N 0.5786(8) 0.1493(9) 0.2152(4) 0.042(2) Uiso 1 1 d . . . N4 N 0.9080(8) 0.3503(8) 0.2473(4) 0.041(2) Uiso 1 1 d . . . C1 C 0.5539(10) 0.3084(11) 0.3833(6) 0.050(3) Uiso 1 1 d . . . H1 H 0.5141 0.3809 0.3426 0.060 Uiso 1 1 calc R . . C2 C 0.5060(12) 0.2845(12) 0.4690(7) 0.068(3) Uiso 1 1 d . . . H2 H 0.4403 0.3449 0.4839 0.081 Uiso 1 1 calc R . . C3 C 0.5579(11) 0.1742(12) 0.5262(7) 0.068(3) Uiso 1 1 d . . . H3 H 0.5242 0.1566 0.5806 0.081 Uiso 1 1 calc R . . C4 C 0.6619(12) 0.0840(12) 0.5065(7) 0.063(3) Uiso 1 1 d . . . C5 C 0.7082(10) 0.1127(11) 0.4217(6) 0.051(3) Uiso 1 1 d . . . C6 C 0.8128(11) 0.0218(11) 0.3955(6) 0.055(3) Uiso 1 1 d . . . C7 C 0.8722(11) -0.0921(12) 0.4564(6) 0.057(3) Uiso 1 1 d . . . C8 C 0.9767(11) -0.1734(12) 0.4278(7) 0.066(3) Uiso 1 1 d . . . H8 H 1.0202 -0.2477 0.4655 0.079 Uiso 1 1 calc R . . C9 C 1.0145(12) -0.1450(12) 0.3465(7) 0.073(4) Uiso 1 1 d . . . H9 H 1.0833 -0.1988 0.3282 0.087 Uiso 1 1 calc R . . C10 C 0.9462(11) -0.0303(12) 0.2892(7) 0.063(3) Uiso 1 1 d . . . H10 H 0.9706 -0.0119 0.2332 0.076 Uiso 1 1 calc R . . C11 C 0.7254(11) -0.0342(12) 0.5642(7) 0.068(3) Uiso 1 1 d . . . H11 H 0.6968 -0.0544 0.6197 0.081 Uiso 1 1 calc R . . C12 C 0.8244(12) -0.1171(13) 0.5417(7) 0.070(4) Uiso 1 1 d . . . H12 H 0.8627 -0.1918 0.5818 0.084 Uiso 1 1 calc R . . C13 C 0.5529(12) 0.0110(13) 0.2452(7) 0.070(4) Uiso 1 1 d . . . H13 H 0.6163 -0.0499 0.2776 0.084 Uiso 1 1 calc R . . C14 C 0.4320(12) -0.0414(14) 0.2282(7) 0.073(4) Uiso 1 1 d . . . H14 H 0.4148 -0.1355 0.2497 0.087 Uiso 1 1 calc R . . C15 C 0.3403(13) 0.0500(13) 0.1791(7) 0.073(4) Uiso 1 1 d . . . H15 H 0.2611 0.0175 0.1659 0.088 Uiso 1 1 calc R . . C16 C 0.3664(12) 0.1926(13) 0.1488(7) 0.070(4) Uiso 1 1 d . . . H16 H 0.3036 0.2551 0.1168 0.084 Uiso 1 1 calc R . . C17 C 0.4871(9) 0.2391(10) 0.1673(5) 0.040(3) Uiso 1 1 d . . . C18 C 0.5211(11) 0.3886(11) 0.1410(6) 0.055(3) Uiso 1 1 d . . . C19 C 0.6414(10) 0.4158(11) 0.1755(6) 0.050(3) Uiso 1 1 d . . . C20 C 0.6737(10) 0.5540(11) 0.1597(6) 0.048(3) Uiso 1 1 d . . . H20 H 0.7506 0.5756 0.1816 0.058 Uiso 1 1 calc R . . C21 C 0.5891(12) 0.6627(13) 0.1101(7) 0.072(4) Uiso 1 1 d . A . C22 C 0.4804(11) 0.6357(12) 0.0743(6) 0.059(3) Uiso 1 1 d . . . H22 H 0.4306 0.7090 0.0398 0.071 Uiso 1 1 calc R . . C23 C 0.4414(12) 0.4999(13) 0.0883(7) 0.076(4) Uiso 1 1 d . . . H23 H 0.3655 0.4816 0.0642 0.091 Uiso 1 1 calc R . . C24 C 0.6305(13) 0.8140(14) 0.0958(7) 0.076(4) Uiso 1 1 d . . . H24A H 0.5879 0.8856 0.0559 0.091 Uiso 0.50 1 calc PR A 1 H24B H 0.6993 0.8310 0.1261 0.091 Uiso 0.50 1 d PR A 2 C25 C 0.9276(11) 0.4002(11) 0.3109(7) 0.058(3) Uiso 1 1 d . . . H25 H 0.8659 0.3813 0.3564 0.070 Uiso 1 1 calc R . . C26 C 1.0383(12) 0.4796(12) 0.3095(7) 0.069(3) Uiso 1 1 d . . . H26 H 1.0520 0.5098 0.3551 0.083 Uiso 1 1 calc R . . C27 C 1.1266(11) 0.5137(11) 0.2428(6) 0.058(3) Uiso 1 1 d . . . H27 H 1.1997 0.5684 0.2419 0.069 Uiso 1 1 calc R . . C28 C 1.1071(11) 0.4663(11) 0.1759(6) 0.059(3) Uiso 1 1 d . . . H28 H 1.1676 0.4882 0.1298 0.071 Uiso 1 1 calc R . . C29 C 0.9955(10) 0.3850(11) 0.1775(6) 0.051(3) Uiso 1 1 d . . . C30 C 0.9616(10) 0.3220(10) 0.1119(6) 0.044(3) Uiso 1 1 d . . . C31 C 0.8441(10) 0.2459(11) 0.1310(6) 0.048(3) Uiso 1 1 d . . . C32 C 0.8121(10) 0.1773(11) 0.0734(6) 0.053(3) Uiso 1 1 d . . . H32 H 0.7354 0.1242 0.0831 0.063 Uiso 1 1 calc R . . C33 C 0.8975(11) 0.1894(11) -0.0002(6) 0.053(3) Uiso 1 1 d . . . C34 C 1.0097(11) 0.2672(11) -0.0165(6) 0.056(3) Uiso 1 1 d . . . H34 H 1.0614 0.2776 -0.0657 0.067 Uiso 1 1 calc R . . C35 C 1.0466(11) 0.3313(11) 0.0409(6) 0.056(3) Uiso 1 1 d . . . H35 H 1.1265 0.3794 0.0322 0.067 Uiso 1 1 calc R . . C36 C 0.8518(12) 0.1141(12) -0.0576(7) 0.066(3) Uiso 1 1 d . . . H36 H 0.7766 0.0590 -0.0416 0.079 Uiso 1 1 calc R . . Cl1 Cl 0.8162(18) 0.4778(18) 0.4978(10) 0.069(7) Uiso 0.33 1 d P . . Cl2 Cl 0.657(2) 0.662(2) 0.3501(11) 0.073(7) Uiso 0.33 1 d P . . Cl3 Cl 0.6304(18) 0.3774(18) 0.6627(10) 0.100(6) Uiso 0.33 1 d P . . O3 O 0.8362(17) 0.5023(17) 0.4906(9) 0.032(6) Uiso 0.67 1 d P . . O4 O 0.677(2) 0.686(2) 0.3442(14) 0.084(10) Uiso 0.67 1 d P . . O5 O 0.663(2) 0.380(2) 0.6412(11) 0.092(7) Uiso 0.67 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 Rh1 0.0543(6) 0.0439(6) 0.0528(6) -0.0168(4) 0.0014(4) 0.0024(4) _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 C31 2.002(10) . ? Rh1 C19 2.023(10) . ? Rh1 N3 2.041(8) . ? Rh1 N4 2.046(8) . ? Rh1 N2 2.163(8) . ? Rh1 N1 2.173(8) . ? O1 C24 1.18(2) . ? O1' C24 1.268(18) . ? O2 C36 1.245(11) . ? N1 C1 1.361(11) . ? N1 C5 1.376(11) . ? N2 C6 1.355(12) . ? N2 C10 1.364(12) . ? N3 C17 1.359(10) . ? N3 C13 1.366(13) . ? N4 C25 1.345(12) . ? N4 C29 1.386(12) . ? C1 C2 1.451(13) . ? C2 C3 1.338(13) . ? C3 C4 1.408(14) . ? C4 C5 1.428(14) . ? C4 C11 1.437(14) . ? C5 C6 1.462(13) . ? C6 C7 1.421(13) . ? C7 C8 1.418(14) . ? C7 C12 1.445(14) . ? C8 C9 1.354(13) . ? C9 C10 1.433(14) . ? C11 C12 1.346(14) . ? C13 C14 1.412(15) . ? C14 C15 1.378(14) . ? C15 C16 1.406(15) . ? C16 C17 1.392(14) . ? C17 C18 1.489(14) . ? C18 C19 1.432(13) . ? C18 C23 1.434(14) . ? C19 C20 1.388(13) . ? C20 C21 1.426(13) . ? C21 C22 1.346(14) . ? C21 C24 1.544(16) . ? C22 C23 1.389(15) . ? C25 C26 1.387(14) . ? C26 C27 1.353(14) . ? C27 C28 1.382(13) . ? C28 C29 1.405(14) . ? C29 C30 1.498(13) . ? C30 C31 1.395(13) . ? C30 C35 1.401(13) . ? C31 C32 1.412(13) . ? C32 C33 1.434(13) . ? C33 C34 1.360(13) . ? C33 C36 1.504(14) . ? C34 C35 1.392(13) . ? 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 C31 Rh1 C19 86.1(4) . . ? C31 Rh1 N3 94.5(4) . . ? C19 Rh1 N3 81.9(4) . . ? C31 Rh1 N4 80.6(4) . . ? C19 Rh1 N4 91.8(4) . . ? N3 Rh1 N4 172.3(3) . . ? C31 Rh1 N2 97.6(4) . . ? C19 Rh1 N2 176.3(4) . . ? N3 Rh1 N2 97.5(3) . . ? N4 Rh1 N2 89.0(3) . . ? C31 Rh1 N1 174.0(4) . . ? C19 Rh1 N1 98.8(4) . . ? N3 Rh1 N1 89.7(3) . . ? N4 Rh1 N1 95.7(3) . . ? N2 Rh1 N1 77.5(3) . . ? C1 N1 C5 119.3(8) . . ? C1 N1 Rh1 127.3(6) . . ? C5 N1 Rh1 113.2(6) . . ? C6 N2 C10 117.0(9) . . ? C6 N2 Rh1 114.6(7) . . ? C10 N2 Rh1 128.3(7) . . ? C17 N3 C13 119.7(9) . . ? C17 N3 Rh1 114.7(7) . . ? C13 N3 Rh1 125.5(7) . . ? C25 N4 C29 119.4(9) . . ? C25 N4 Rh1 125.0(7) . . ? C29 N4 Rh1 115.2(6) . . ? N1 C1 C2 120.6(9) . . ? C3 C2 C1 119.0(11) . . ? C2 C3 C4 122.1(11) . . ? C3 C4 C5 117.2(10) . . ? C3 C4 C11 125.6(10) . . ? C5 C4 C11 117.2(10) . . ? N1 C5 C4 121.7(9) . . ? N1 C5 C6 117.6(9) . . ? C4 C5 C6 120.8(9) . . ? N2 C6 C7 124.3(10) . . ? N2 C6 C5 117.0(9) . . ? C7 C6 C5 118.7(9) . . ? C8 C7 C6 116.3(10) . . ? C8 C7 C12 124.6(10) . . ? C6 C7 C12 119.1(10) . . ? C9 C8 C7 121.3(11) . . ? C8 C9 C10 118.5(11) . . ? N2 C10 C9 122.6(10) . . ? C12 C11 C4 123.0(11) . . ? C11 C12 C7 121.1(11) . . ? N3 C13 C14 121.4(11) . . ? C15 C14 C13 118.4(13) . . ? C14 C15 C16 120.0(12) . . ? C17 C16 C15 119.3(11) . . ? N3 C17 C16 121.0(10) . . ? N3 C17 C18 115.7(9) . . ? C16 C17 C18 123.2(9) . . ? C19 C18 C23 121.0(11) . . ? C19 C18 C17 114.0(9) . . ? C23 C18 C17 125.0(10) . . ? C20 C19 C18 117.6(9) . . ? C20 C19 Rh1 129.1(8) . . ? C18 C19 Rh1 113.2(8) . . ? C19 C20 C21 120.0(10) . . ? C22 C21 C20 121.9(12) . . ? C22 C21 C24 120.9(11) . . ? C20 C21 C24 117.2(11) . . ? C21 C22 C23 121.0(11) . . ? C22 C23 C18 118.4(11) . . ? O1 C24 O1' 116.7(19) . . ? O1 C24 C21 121.9(16) . . ? O1' C24 C21 121.3(14) . . ? N4 C25 C26 121.0(11) . . ? C27 C26 C25 120.9(11) . . ? C26 C27 C28 119.2(11) . . ? C27 C28 C29 119.9(11) . . ? N4 C29 C28 119.5(9) . . ? N4 C29 C30 113.6(9) . . ? C28 C29 C30 126.8(10) . . ? C31 C30 C35 123.7(9) . . ? C31 C30 C29 113.9(9) . . ? C35 C30 C29 122.3(9) . . ? C30 C31 C32 116.2(9) . . ? C30 C31 Rh1 116.3(7) . . ? C32 C31 Rh1 127.5(8) . . ? C31 C32 C33 120.1(10) . . ? C34 C33 C32 121.3(10) . . ? C34 C33 C36 123.4(10) . . ? C32 C33 C36 115.3(10) . . ? C33 C34 C35 119.7(10) . . ? C34 C35 C30 118.9(10) . . ? O2 C36 C33 121.8(11) . . ? _diffrn_measured_fraction_theta_max 0.479 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.479 _refine_diff_density_max 0.494 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.082