Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J. Chem. Soc., Dalton Trans' loop_ _publ_author_name 'F. A. Cotton' 'Lin, Chun' 'C. A. Murillo' _publ_contact_author_name 'Prof F Albert Cotton' _publ_contact_author_address ; Prof F Albert Cotton Department of Chemistry & Laboratory for Molecular Strucutre and Bonding Texas A&M University PO Box 30012 College Station TX 77842-3012 UNITED STATES OF AMERICA ; data_cmpd_3 _database_code_CSD 154475 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Rh4(DAniF)4][O2CCH2CO2]2[1,3,5-C3N3(C5H4N)3]2(3CHCl3)(1CH2Cl2)' _chemical_formula_sum 'C212 H186 Cl22 N40 O32 Rh8' _chemical_formula_weight 5409.19 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' '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' _symmetry_cell_setting Orthorombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.777(2) _cell_length_b 28.965(3) _cell_length_c 29.868(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 24896(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2444 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.43 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10912 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58054 _diffrn_reflns_av_R_equivalents 0.1969 _diffrn_reflns_av_sigmaI/netI 0.2821 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 22.52 _reflns_number_total 15808 _reflns_number_gt 5459 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1993)' _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^)+(0.1096P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15808 _refine_ls_number_parameters 743 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.2347 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.1965 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.004 _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 0.45904(5) 0.16394(4) 0.61967(5) 0.0403(4) Uani 1 1 d . . . Rh2 Rh 0.46412(5) 0.21468(4) 0.55326(4) 0.0385(4) Uani 1 1 d . . . Rh3 Rh 0.30698(5) 0.31009(4) 0.69448(4) 0.0378(4) Uani 1 1 d . . . Rh4 Rh 0.31642(4) 0.34874(4) 0.62186(5) 0.0367(4) Uani 1 1 d . B . N1 N 0.4495(5) 0.1112(4) 0.5790(5) 0.054(4) Uiso 1 1 d . . . N2 N 0.4527(4) 0.1578(5) 0.5161(5) 0.052(4) Uiso 1 1 d . . . N3 N 0.5282(4) 0.1554(4) 0.6146(5) 0.048(4) Uiso 1 1 d . . . N4 N 0.5329(4) 0.2043(4) 0.5529(5) 0.040(3) Uiso 1 1 d . . . N5 N 0.2375(4) 0.3178(4) 0.6870(5) 0.043(4) Uiso 1 1 d . . . N6 N 0.2482(4) 0.3634(4) 0.6241(5) 0.044(4) Uiso 1 1 d . . . N7 N 0.3120(4) 0.3728(4) 0.7235(5) 0.045(4) Uiso 1 1 d . . . N8 N 0.3320(4) 0.4075(4) 0.6549(5) 0.047(4) Uiso 1 1 d . . . O2 O 0.4402(5) 0.1759(5) 0.3302(6) 0.088(5) Uiso 1 1 d . A . O3 O 0.6074(7) 0.0293(7) 0.7326(9) 0.167(8) Uiso 1 1 d . A . O4 O 0.6570(5) 0.2930(5) 0.4368(6) 0.110(5) Uiso 1 1 d . A . O5 O 0.1183(5) 0.2491(4) 0.8189(5) 0.083(4) Uiso 1 1 d . . . O7 O 0.3109(6) 0.4071(6) 0.9084(7) 0.131(6) Uiso 1 1 d . . . O8 O 0.4173(5) 0.5592(5) 0.5751(5) 0.095(5) Uiso 1 1 d . B . O201 O 0.4646(3) 0.2251(3) 0.6565(4) 0.042(3) Uiso 1 1 d . . . O202 O 0.4729(3) 0.2685(3) 0.5962(4) 0.043(3) Uiso 1 1 d . . . O203 O 0.3868(4) 0.1755(4) 0.6195(4) 0.056(3) Uiso 1 1 d . . . O204 O 0.3917(4) 0.2219(3) 0.5600(4) 0.045(3) Uiso 1 1 d . . . O205 O 0.3792(3) 0.3057(3) 0.6963(4) 0.043(3) Uiso 1 1 d . . . O206 O 0.3865(3) 0.3298(3) 0.6254(4) 0.034(3) Uiso 1 1 d . . . O207 O 0.3056(3) 0.2482(3) 0.6577(4) 0.044(3) Uiso 1 1 d . . . O208 O 0.3021(3) 0.2858(3) 0.5919(3) 0.036(3) Uiso 1 1 d . . . C1 C 0.4458(6) 0.1160(6) 0.5332(6) 0.049(5) Uiso 1 1 d . A . C2 C 0.5535(5) 0.1760(5) 0.5836(6) 0.043(5) Uiso 1 1 d . A . C3 C 0.2211(6) 0.3449(5) 0.6538(6) 0.047(5) Uiso 1 1 d . B . C4 C 0.3251(6) 0.4093(6) 0.6995(6) 0.050(5) Uiso 1 1 d . B . C5 C 0.4654(5) 0.2644(5) 0.6372(5) 0.030(4) Uiso 1 1 d . A . C6 C 0.4551(5) 0.3051(5) 0.6661(6) 0.041(4) Uiso 1 1 d . . . C7 C 0.4029(5) 0.3151(5) 0.6609(6) 0.037(4) Uiso 1 1 d . A . C8 C 0.3695(6) 0.2005(5) 0.5898(6) 0.044(5) Uiso 1 1 d . A . C9 C 0.3172(5) 0.2054(5) 0.5899(6) 0.041(4) Uiso 1 1 d . . . C10 C 0.3075(5) 0.2504(5) 0.6164(6) 0.041(4) Uiso 1 1 d . A . C11 C 0.4317(10) 0.0652(8) 0.5984(11) 0.035(6) Uiso 0.560(11) 1 d PD A 1 C12 C 0.3929(10) 0.0665(9) 0.6299(11) 0.046(7) Uiso 0.560(11) 1 d PD A 1 C13 C 0.3803(11) 0.0211(10) 0.6436(11) 0.059(9) Uiso 0.560(11) 1 d PD A 1 C14 C 0.4029(14) -0.0151(12) 0.6356(15) 0.075(11) Uiso 0.560(11) 1 d PD A 1 C15 C 0.4410(19) -0.0204(12) 0.604(2) 0.073(10) Uiso 0.560(11) 1 d PD A 1 C16 C 0.4587(11) 0.0249(8) 0.5828(12) 0.054(7) Uiso 0.560(11) 1 d PD A 1 O1 O 0.3852(7) -0.0579(8) 0.6544(8) 0.075(6) Uiso 0.560(11) 1 d PD A 1 C17 C 0.4032(14) -0.0954(10) 0.6498(13) 0.061(8) Uiso 0.560(11) 1 d PD A 1 C11' C 0.4491(13) 0.0607(9) 0.5851(13) 0.035(6) Uiso 0.440(11) 1 d PD A 2 C12' C 0.4124(13) 0.0469(11) 0.6163(14) 0.046(7) Uiso 0.440(11) 1 d PD A 2 C13' C 0.4122(16) -0.0016(12) 0.6247(17) 0.059(9) Uiso 0.440(11) 1 d PD A 2 C14' C 0.438(2) -0.0304(13) 0.605(3) 0.075(11) Uiso 0.440(11) 1 d PD A 2 C15' C 0.4753(14) -0.0206(11) 0.5733(15) 0.073(10) Uiso 0.440(11) 1 d PD A 2 C16' C 0.4805(13) 0.0303(11) 0.5596(14) 0.054(7) Uiso 0.440(11) 1 d PD A 2 O1' O 0.4326(9) -0.0793(8) 0.6132(10) 0.075(6) Uiso 0.440(11) 1 d PD A 2 C17' C 0.4001(17) -0.0996(12) 0.6290(16) 0.061(8) Uiso 0.440(11) 1 d PD A 2 C21 C 0.4475(6) 0.1613(6) 0.4681(6) 0.049(5) Uiso 1 1 d . A . C22 C 0.4792(6) 0.1379(6) 0.4399(7) 0.059(5) Uiso 1 1 d . . . C23 C 0.4751(6) 0.1444(6) 0.3934(7) 0.063(6) Uiso 1 1 d . A . C24 C 0.4390(7) 0.1715(7) 0.3761(8) 0.073(6) Uiso 1 1 d . . . C25 C 0.4054(7) 0.1949(7) 0.4033(8) 0.074(6) Uiso 1 1 d . A . C26 C 0.4110(6) 0.1886(6) 0.4507(7) 0.066(6) Uiso 1 1 d . . . C27 C 0.4089(9) 0.2071(9) 0.3081(10) 0.131(10) Uiso 1 1 d . . . C31 C 0.5524(5) 0.1252(5) 0.6446(6) 0.045(5) Uiso 1 1 d . A . C32 C 0.5662(6) 0.1416(6) 0.6863(7) 0.069(6) Uiso 1 1 d . . . C33 C 0.5870(7) 0.1106(8) 0.7201(8) 0.090(7) Uiso 1 1 d . A . C34 C 0.5892(8) 0.0662(9) 0.7036(9) 0.097(8) Uiso 1 1 d . . . C35 C 0.5780(7) 0.0483(8) 0.6626(9) 0.092(7) Uiso 1 1 d . A . C36 C 0.5582(6) 0.0796(6) 0.6306(7) 0.065(6) Uiso 1 1 d . . . C37 C 0.6048(11) 0.0406(11) 0.7773(14) 0.169(13) Uiso 1 1 d . . . C41 C 0.5655(6) 0.2261(6) 0.5230(6) 0.050(5) Uiso 1 1 d . A . C42 C 0.5712(6) 0.2732(5) 0.5263(6) 0.048(5) Uiso 1 1 d . . . C43 C 0.6023(6) 0.2963(6) 0.4969(7) 0.068(6) Uiso 1 1 d . A . C44 C 0.6245(7) 0.2683(7) 0.4652(7) 0.065(6) Uiso 1 1 d . . . C45 C 0.6219(7) 0.2220(7) 0.4609(7) 0.077(6) Uiso 1 1 d . A . C46 C 0.5876(6) 0.1993(6) 0.4909(7) 0.067(6) Uiso 1 1 d . . . C47 C 0.6837(9) 0.2672(8) 0.4069(10) 0.114(8) Uiso 1 1 d . . . C51 C 0.2043(6) 0.3000(5) 0.7205(6) 0.044(5) Uiso 1 1 d . . . C52 C 0.1741(6) 0.3305(5) 0.7422(6) 0.047(5) Uiso 1 1 d . . . C53 C 0.1435(6) 0.3165(6) 0.7750(6) 0.057(5) Uiso 1 1 d . . . C54 C 0.1459(6) 0.2687(6) 0.7849(6) 0.053(5) Uiso 1 1 d . . . C55 C 0.1743(6) 0.2367(6) 0.7638(7) 0.063(6) Uiso 1 1 d . . . C56 C 0.2055(6) 0.2542(5) 0.7302(6) 0.047(5) Uiso 1 1 d . . . C57 C 0.0860(7) 0.2807(7) 0.8446(8) 0.083(7) Uiso 1 1 d . . . C61 C 0.2204(16) 0.3907(11) 0.5940(13) 0.048(7) Uiso 0.52(3) 1 d PD B 1 C62 C 0.2239(14) 0.4398(12) 0.5979(12) 0.056(8) Uiso 0.52(3) 1 d PD B 1 C63 C 0.1920(19) 0.4668(11) 0.5714(16) 0.082(8) Uiso 0.52(3) 1 d PD B 1 C64 C 0.1739(14) 0.4437(13) 0.5369(15) 0.065(9) Uiso 0.52(3) 1 d PD B 1 C65 C 0.1743(14) 0.4002(12) 0.5255(14) 0.067(9) Uiso 0.52(3) 1 d PD B 1 C66 C 0.209(2) 0.3717(13) 0.5548(16) 0.082(8) Uiso 0.52(3) 1 d PD B 1 O6 O 0.1470(13) 0.4753(13) 0.5069(15) 0.139(10) Uiso 0.52(3) 1 d PD B 1 C67 C 0.125(2) 0.436(2) 0.468(2) 0.152(18) Uiso 0.52(3) 1 d P B 1 C61' C 0.2291(17) 0.3872(12) 0.5862(13) 0.048(7) Uiso 0.48(3) 1 d PD B 2 C62' C 0.2077(15) 0.4306(12) 0.5954(12) 0.056(8) Uiso 0.48(3) 1 d PD B 2 C63' C 0.192(2) 0.4571(13) 0.5575(16) 0.082(8) Uiso 0.48(3) 1 d PD B 2 C64' C 0.1835(16) 0.4315(12) 0.5212(14) 0.065(9) Uiso 0.48(3) 1 d PD B 2 C65' C 0.1955(16) 0.3894(12) 0.5107(13) 0.067(9) Uiso 0.48(3) 1 d PD B 2 C66' C 0.215(2) 0.3618(13) 0.5515(17) 0.082(8) Uiso 0.48(3) 1 d PD B 2 O6' O 0.1558(16) 0.4564(15) 0.4867(15) 0.139(10) Uiso 0.48(3) 1 d PD B 2 C67' C 0.105(2) 0.467(2) 0.481(3) 0.152(18) Uiso 0.48(3) 1 d P B 2 C71 C 0.3122(6) 0.3811(5) 0.7707(6) 0.047(5) Uiso 1 1 d . . . C72 C 0.3516(8) 0.3970(8) 0.7912(9) 0.100(8) Uiso 1 1 d . . . C73 C 0.3543(8) 0.4093(7) 0.8393(9) 0.094(8) Uiso 1 1 d . . . C74 C 0.3128(9) 0.3987(7) 0.8602(9) 0.090(7) Uiso 1 1 d . . . C75 C 0.2738(8) 0.3842(8) 0.8428(9) 0.099(8) Uiso 1 1 d . . . C76 C 0.2716(7) 0.3738(6) 0.7955(8) 0.072(6) Uiso 1 1 d . . . C77 C 0.3502(10) 0.4269(9) 0.9275(10) 0.133(10) Uiso 1 1 d . . . C81 C 0.3538(6) 0.4472(6) 0.6338(6) 0.046(5) Uiso 1 1 d . B . C82 C 0.3937(6) 0.4412(6) 0.6114(6) 0.051(5) Uiso 1 1 d . . . C83 C 0.4145(6) 0.4801(7) 0.5907(7) 0.070(6) Uiso 1 1 d . B . C84 C 0.3928(7) 0.5207(7) 0.5949(7) 0.065(6) Uiso 1 1 d . . . C85 C 0.3517(6) 0.5287(6) 0.6153(7) 0.060(5) Uiso 1 1 d . B . C86 C 0.3302(6) 0.4884(6) 0.6356(6) 0.055(5) Uiso 1 1 d . . . C87 C 0.4035(8) 0.6066(8) 0.5867(9) 0.103(8) Uiso 1 1 d . . . N101 N 0.4554(4) 0.3722(4) 0.1949(5) 0.043(4) Uiso 1 1 d . . . N102 N 0.4635(4) 0.4520(4) 0.3470(5) 0.042(4) Uiso 1 1 d . . . N103 N 0.4624(4) 0.4265(4) 0.4224(5) 0.042(4) Uiso 1 1 d . . . N104 N 0.4666(4) 0.3719(4) 0.3637(5) 0.047(4) Uiso 1 1 d . . . N105 N 0.4561(6) 0.5976(7) 0.4366(8) 0.107(7) Uiso 1 1 d . . . N108 N 0.3285(4) 0.3718(4) 0.5508(5) 0.044(4) Uiso 1 1 d . . . N121 N 0.3130(4) 0.2567(4) 0.7548(5) 0.044(4) Uiso 1 1 d . . . N122 N 0.3276(4) 0.1464(4) 0.8842(5) 0.047(4) Uiso 1 1 d . . . N123 N 0.3411(4) 0.0656(4) 0.8935(5) 0.048(4) Uiso 1 1 d . . . N124 N 0.3392(4) 0.0996(5) 0.8208(5) 0.053(4) Uiso 1 1 d . . . N125 N 0.3648(6) -0.0695(6) 0.7928(7) 0.087(6) Uiso 1 1 d . . . N141 N 0.4665(5) 0.2705(4) 0.4986(5) 0.054(4) Uiso 1 1 d . . . C101 C 0.4651(6) 0.4159(5) 0.2078(6) 0.049(5) Uiso 1 1 d . . . C102 C 0.4701(5) 0.4301(5) 0.2528(6) 0.043(5) Uiso 1 1 d . . . C103 C 0.4628(6) 0.3961(5) 0.2859(6) 0.046(5) Uiso 1 1 d . . . C104 C 0.4550(6) 0.3503(5) 0.2726(6) 0.051(5) Uiso 1 1 d . . . C105 C 0.4512(6) 0.3386(6) 0.2267(7) 0.057(5) Uiso 1 1 d . . . C106 C 0.4655(6) 0.4079(5) 0.3343(6) 0.046(5) Uiso 1 1 d . . . C107 C 0.4617(5) 0.4597(5) 0.3908(6) 0.040(4) Uiso 1 1 d . . . C108 C 0.4658(5) 0.3829(5) 0.4068(6) 0.043(4) Uiso 1 1 d . . . C109 C 0.4554(7) 0.5177(7) 0.4534(8) 0.079(6) Uiso 1 1 d . . . C110 C 0.4526(8) 0.5643(9) 0.4689(9) 0.106(8) Uiso 1 1 d . . . C111 C 0.4598(8) 0.5902(8) 0.3928(9) 0.103(8) Uiso 1 1 d . . . C112 C 0.4604(6) 0.5432(6) 0.3738(7) 0.061(5) Uiso 1 1 d . . . C113 C 0.4596(6) 0.5083(6) 0.4068(7) 0.055(5) Uiso 1 1 d . . . C121 C 0.2937(6) 0.2570(6) 0.7961(6) 0.052(5) Uiso 1 1 d . . . C122 C 0.3003(6) 0.2194(6) 0.8263(6) 0.055(5) Uiso 1 1 d . . . C123 C 0.3237(5) 0.1790(5) 0.8101(6) 0.039(4) Uiso 1 1 d . . . C124 C 0.3432(6) 0.1804(5) 0.7665(6) 0.048(5) Uiso 1 1 d . . . C125 C 0.3382(5) 0.2189(5) 0.7406(6) 0.045(5) Uiso 1 1 d . . . C126 C 0.3310(5) 0.1407(5) 0.8402(6) 0.037(4) Uiso 1 1 d . . . C127 C 0.3320(5) 0.1086(6) 0.9090(6) 0.047(5) Uiso 1 1 d . . . C128 C 0.3422(6) 0.0630(6) 0.8478(6) 0.048(5) Uiso 1 1 d . . . C129 C 0.3493(6) 0.0167(6) 0.8275(7) 0.055(5) Uiso 1 1 d . . . C130 C 0.3654(7) 0.0135(7) 0.7830(8) 0.087(7) Uiso 1 1 d . . . C131 C 0.3705(7) -0.0318(8) 0.7633(8) 0.094(7) Uiso 1 1 d . . . C132 C 0.3503(8) -0.0658(7) 0.8327(9) 0.089(7) Uiso 1 1 d . . . C133 C 0.3429(7) -0.0232(7) 0.8565(8) 0.079(6) Uiso 1 1 d . . . C134 C 0.3318(5) 0.1156(5) 0.9571(6) 0.044(5) Uiso 1 1 d . . . C135 C 0.3415(5) 0.1580(5) 0.9760(6) 0.043(5) Uiso 1 1 d . . . C136 C 0.3402(6) 0.1638(6) 1.0227(6) 0.053(5) Uiso 1 1 d . . . C137 C 0.3192(6) 0.4141(5) 0.5326(6) 0.048(5) Uiso 1 1 d . . . C138 C 0.3216(6) 0.0783(6) 0.9871(6) 0.051(5) Uiso 1 1 d . . . C141 C 0.4528(5) 0.3135(6) 0.5130(6) 0.049(5) Uiso 1 1 d . A . C142 C 0.4515(5) 0.3526(5) 0.4826(6) 0.050(5) Uiso 1 1 d . . . C143 C 0.4680(5) 0.3449(5) 0.4394(6) 0.043(4) Uiso 1 1 d . A . C144 C 0.4833(5) 0.3011(5) 0.4254(6) 0.048(5) Uiso 1 1 d . . . C145 C 0.4842(6) 0.2656(6) 0.4566(6) 0.049(5) Uiso 1 1 d . A . C1S C 0.5199(8) -0.0983(8) 0.7392(9) 0.098(8) Uiso 1 1 d . . . Cl1 Cl 0.5111(2) -0.0501(2) 0.7029(3) 0.129(3) Uiso 1 1 d . . . Cl2 Cl 0.4645(3) -0.1181(3) 0.7536(3) 0.147(3) Uiso 1 1 d . . . Cl3 Cl 0.5476(2) -0.0784(2) 0.7879(3) 0.114(2) Uiso 1 1 d . . . C2S C 0.5788(9) 0.2519(9) 0.3080(10) 0.124(9) Uiso 1 1 d . . . Cl4 Cl 0.5307(3) 0.2518(3) 0.2674(4) 0.191(4) Uiso 1 1 d . . . Cl5 Cl 0.5596(3) 0.2202(3) 0.3515(4) 0.182(4) Uiso 1 1 d . . . Cl6 Cl 0.5824(3) 0.3095(3) 0.3240(4) 0.179(4) Uiso 1 1 d . . . C3S C 0.7233(16) 0.4153(9) 0.5149(17) 0.17(3) Uiso 0.50 1 d PD . . Cl7 Cl 0.7292(6) 0.3754(6) 0.4777(7) 0.162(6) Uiso 0.50 1 d PD . . Cl8 Cl 0.6721(7) 0.4109(7) 0.5363(7) 0.188(8) Uiso 0.50 1 d PD . . Cl9 Cl 0.7398(5) 0.4654(6) 0.4983(6) 0.151(6) Uiso 0.50 1 d PD . . C4S C 0.2211(11) 0.2754(11) 0.9466(10) 0.17(3) Uiso 0.50 1 d PD . . Cl10 Cl 0.2039(6) 0.2848(7) 0.8957(7) 0.186(8) Uiso 0.50 1 d PD . . Cl11 Cl 0.2433(7) 0.2309(7) 0.9734(7) 0.190(8) Uiso 0.50 1 d PD . . Cl12 Cl 0.2770(9) 0.2945(9) 0.9390(10) 0.118(9) Uiso 0.25 1 d PD . . Cl13 Cl 0.1929(13) 0.2321(12) 0.9159(14) 0.194(16) Uiso 0.25 1 d PD . . C5S C 0.2013(19) 0.0840(11) 0.8744(11) 0.21(3) Uiso 0.60 1 d PD . . Cl14 Cl 0.2104(11) 0.1256(11) 0.8365(11) 0.168(13) Uiso 0.30 1 d PD . . Cl15 Cl 0.2210(11) 0.0314(10) 0.8865(14) 0.189(13) Uiso 0.30 1 d PD . . Cl16 Cl 0.2147(13) 0.0366(12) 0.8410(15) 0.230(17) Uiso 0.30 1 d PD . . Cl17 Cl 0.2160(11) 0.0985(12) 0.8209(9) 0.163(13) Uiso 0.30 1 d PD . . C6S C 0.256(2) 0.1000(16) 0.7215(16) 0.25(5) Uiso 0.40 1 d PD . . Cl18 Cl 0.2184(8) 0.1323(8) 0.6851(9) 0.176(9) Uiso 0.40 1 d PD . . Cl19 Cl 0.2622(15) 0.0380(14) 0.7133(17) 0.165(16) Uiso 0.20 1 d PD . . Cl20 Cl 0.2907(16) 0.0944(16) 0.6727(19) 0.190(19) Uiso 0.20 1 d PD . . 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 0.0495(10) 0.0387(7) 0.0327(9) 0.0070(7) 0.0002(8) 0.0051(7) Rh2 0.0504(9) 0.0365(7) 0.0286(8) 0.0024(7) 0.0033(7) 0.0075(7) Rh3 0.0420(9) 0.0440(8) 0.0274(8) 0.0019(7) 0.0027(7) 0.0054(7) Rh4 0.0445(9) 0.0393(7) 0.0261(8) 0.0014(7) 0.0003(7) 0.0046(7) _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 N1 1.970(14) . Y Rh1 N3 2.010(13) . Y Rh1 O201 2.091(10) . Y Rh1 O203 2.105(11) . Y Rh1 Rh2 2.4732(19) . Y Rh1 N101 2.482(14) 7_566 Y Rh2 N4 2.003(12) . Y Rh2 N2 2.014(14) . Y Rh2 O202 2.034(10) . Y Rh2 O204 2.103(10) . Y Rh2 N141 2.299(14) . Y Rh3 N7 2.017(13) . Y Rh3 N5 2.023(13) . Y Rh3 O205 2.083(10) . Y Rh3 O207 2.103(10) . Y Rh3 N121 2.379(13) . Y Rh3 Rh4 2.4560(19) . Y Rh4 N6 2.010(13) . Y Rh4 N8 2.017(13) . Y Rh4 O208 2.074(9) . Y Rh4 O206 2.093(9) . Y Rh4 N108 2.253(14) . Y N1 C1 1.38(2) . ? N1 C11' 1.47(3) . ? N1 C11 1.54(2) . ? N2 C1 1.327(18) . ? N2 C21 1.44(2) . ? N3 C2 1.322(19) . ? N3 C31 1.431(19) . ? N4 C2 1.365(18) . ? N4 C41 1.440(19) . ? N5 C3 1.352(19) . ? N5 C51 1.476(19) . ? N6 C3 1.297(19) . ? N6 C61' 1.43(3) . ? N6 C61 1.44(3) . ? N7 C4 1.333(19) . ? N7 C71 1.43(2) . ? N8 C4 1.35(2) . ? N8 C81 1.454(19) . ? O2 C24 1.38(2) . ? O2 C27 1.44(3) . ? O3 C37 1.38(4) . ? O3 C34 1.47(3) . ? O4 C47 1.40(3) . ? O4 C44 1.45(2) . ? O5 C54 1.41(2) . ? O5 C57 1.52(2) . ? O7 C77 1.39(3) . ? O7 C74 1.46(3) . ? O8 C84 1.45(2) . ? O8 C87 1.47(2) . ? O201 C5 1.277(15) . ? O202 C5 1.250(16) . ? O203 C8 1.250(18) . ? O204 C8 1.259(17) . ? O205 C7 1.286(17) . ? O206 C7 1.235(17) . ? O207 C10 1.237(18) . ? O208 C10 1.269(16) . ? C5 C6 1.49(2) . ? C6 C7 1.54(2) . ? C8 C9 1.51(2) . ? C9 C10 1.55(2) . ? C11 C12 1.46(3) . ? C11 C16 1.48(3) . ? C12 C13 1.43(3) . ? C13 C14 1.26(4) . ? C14 O1 1.45(3) . ? C14 C15 1.46(5) . ? C15 C16 1.54(4) . ? O1 C17 1.21(3) . ? C11' C12' 1.46(3) . ? C11' C16' 1.47(3) . ? C12' C13' 1.43(3) . ? C13' C14' 1.26(5) . ? C14' O1' 1.45(3) . ? C14' C15' 1.46(6) . ? C15' C16' 1.54(4) . ? O1' C17' 1.20(3) . ? C21 C26 1.41(2) . ? C21 C22 1.41(2) . ? C22 C23 1.41(2) . ? C23 C24 1.40(2) . ? C24 C25 1.43(3) . ? C25 C26 1.44(3) . ? C31 C32 1.39(2) . ? C31 C36 1.40(2) . ? C32 C33 1.48(3) . ? C33 C34 1.38(3) . ? C34 C35 1.37(3) . ? C35 C36 1.44(3) . ? C41 C42 1.38(2) . ? C41 C46 1.39(2) . ? C42 C43 1.42(2) . ? C43 C44 1.40(2) . ? C44 C45 1.35(2) . ? C45 C46 1.49(2) . ? C51 C56 1.36(2) . ? C51 C52 1.40(2) . ? C52 C53 1.38(2) . ? C53 C54 1.42(2) . ? C54 C55 1.39(2) . ? C55 C56 1.44(2) . ? C61 C66 1.33(3) . ? C61 C62 1.43(3) . ? C62 C63 1.44(3) . ? C63 C64 1.33(4) . ? C64 C65 1.31(3) . ? C64 O6 1.50(3) . ? C65 C66 1.57(3) . ? O6 C67 1.75(9) . ? C61' C66' 1.33(3) . ? C61' C62' 1.43(3) . ? C62' C63' 1.44(3) . ? C63' C64' 1.33(4) . ? C64' C65' 1.31(3) . ? C64' O6' 1.49(3) . ? C65' C66' 1.56(3) . ? O6' C67' 1.49(8) . ? C71 C72 1.37(2) . ? C71 C76 1.40(2) . ? C72 C73 1.48(3) . ? C73 C74 1.38(3) . ? C74 C75 1.31(3) . ? C75 C76 1.44(3) . ? C81 C82 1.34(2) . ? C81 C86 1.37(2) . ? C82 C83 1.42(2) . ? C83 C84 1.34(2) . ? C84 C85 1.35(2) . ? C85 C86 1.45(2) . ? N101 C101 1.352(18) . ? N101 C105 1.36(2) . ? N101 Rh1 2.482(14) 7_565 ? N102 C107 1.330(19) . ? N102 C106 1.333(17) . ? N103 C107 1.345(18) . ? N103 C108 1.351(17) . ? N104 C108 1.32(2) . ? N104 C106 1.364(19) . ? N105 C111 1.33(3) . ? N105 C110 1.37(3) . ? N108 C137 1.368(18) . ? N108 C136 1.369(19) 7_565 ? N121 C121 1.35(2) . ? N121 C125 1.382(18) . ? N122 C126 1.33(2) . ? N122 C127 1.329(19) . ? N123 C127 1.355(18) . ? N123 C128 1.36(2) . ? N124 C128 1.335(19) . ? N124 C126 1.342(18) . ? N125 C132 1.27(3) . ? N125 C131 1.41(3) . ? N141 C145 1.36(2) . ? N141 C141 1.374(18) . ? C101 C102 1.41(2) . ? C102 C103 1.41(2) . ? C103 C104 1.40(2) . ? C103 C106 1.49(2) . ? C104 C105 1.42(2) . ? C107 C113 1.49(2) . ? C108 C143 1.47(2) . ? C109 C113 1.42(3) . ? C109 C110 1.43(3) . ? C111 C112 1.47(3) . ? C112 C113 1.41(2) . ? C121 C122 1.43(2) . ? C122 C123 1.43(2) . ? C123 C124 1.42(2) . ? C123 C126 1.44(2) . ? C124 C125 1.37(2) . ? C127 C134 1.45(2) . ? C128 C129 1.49(2) . ? C129 C130 1.41(3) . ? C129 C133 1.45(2) . ? C130 C131 1.44(3) . ? C132 C133 1.44(3) . ? C134 C135 1.38(2) . ? C134 C138 1.44(2) . ? C135 C136 1.40(2) . ? C136 N108 1.369(19) 7_566 ? C137 C138 1.38(2) 7_565 ? C138 C137 1.38(2) 7_566 ? C141 C142 1.45(2) . ? C142 C143 1.39(2) . ? C143 C144 1.41(2) . ? C144 C145 1.39(2) . ? C1S Cl2 1.75(2) . ? C1S Cl3 1.75(2) . ? C1S Cl1 1.79(2) . ? C2S Cl5 1.68(3) . ? C2S Cl6 1.74(3) . ? C2S Cl4 1.84(3) . ? C3S Cl9 1.61(2) . ? C3S Cl7 1.61(2) . ? C3S Cl8 1.61(2) . ? C4S Cl10 1.622(19) . ? C4S Cl11 1.645(19) . ? C4S Cl12 1.716(19) . ? C4S Cl13 1.755(19) . ? C5S Cl15 1.664(19) . ? C5S Cl14 1.675(19) . ? C5S Cl17 1.707(19) . ? C5S Cl16 1.74(2) . ? C6S Cl20 1.78(2) . ? C6S Cl18 1.79(2) . ? C6S Cl19 1.82(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 N1 Rh1 N3 89.8(5) . . Y N1 Rh1 O201 172.5(5) . . Y N3 Rh1 O201 93.9(5) . . Y N1 Rh1 O203 89.1(5) . . Y N3 Rh1 O203 175.1(5) . . Y O201 Rh1 O203 86.7(4) . . Y N1 Rh1 Rh2 88.6(4) . . Y N3 Rh1 Rh2 87.4(4) . . Y O201 Rh1 Rh2 85.1(3) . . Y O203 Rh1 Rh2 87.8(3) . . Y N1 Rh1 N101 103.0(5) . 7_566 Y N3 Rh1 N101 93.3(5) . 7_566 Y O201 Rh1 N101 83.4(4) . 7_566 Y O203 Rh1 N101 91.6(4) . 7_566 Y Rh2 Rh1 N101 168.4(3) . 7_566 Y N4 Rh2 N2 92.0(5) . . Y N4 Rh2 O202 89.8(4) . . Y N2 Rh2 O202 174.1(5) . . Y N4 Rh2 O204 174.1(5) . . Y N2 Rh2 O204 88.4(5) . . Y O202 Rh2 O204 89.2(4) . . Y N4 Rh2 N141 94.1(5) . . Y N2 Rh2 N141 100.9(6) . . Y O202 Rh2 N141 84.5(5) . . Y O204 Rh2 N141 91.6(4) . . Y N4 Rh2 Rh1 88.5(4) . . Y N2 Rh2 Rh1 86.9(4) . . Y O202 Rh2 Rh1 87.6(3) . . Y O204 Rh2 Rh1 85.6(3) . . Y N141 Rh2 Rh1 171.7(4) . . Y N7 Rh3 N5 91.0(5) . . Y N7 Rh3 O205 88.5(4) . . Y N5 Rh3 O205 174.4(5) . . Y N7 Rh3 O207 173.3(5) . . Y N5 Rh3 O207 91.1(4) . . Y O205 Rh3 O207 88.8(4) . . Y N7 Rh3 N121 104.7(5) . . Y N5 Rh3 N121 103.1(5) . . Y O205 Rh3 N121 82.5(4) . . Y O207 Rh3 N121 81.0(4) . . Y N7 Rh3 Rh4 87.8(4) . . Y N5 Rh3 Rh4 87.8(4) . . Y O205 Rh3 Rh4 86.6(3) . . Y O207 Rh3 Rh4 85.9(3) . . Y N121 Rh3 Rh4 163.1(3) . . Y N6 Rh4 N8 91.3(5) . . Y N6 Rh4 O208 90.3(4) . . Y N8 Rh4 O208 175.9(5) . . Y N6 Rh4 O206 174.3(5) . . Y N8 Rh4 O206 89.0(4) . . Y O208 Rh4 O206 89.0(4) . . Y N6 Rh4 N108 96.9(5) . . Y N8 Rh4 N108 100.2(5) . . Y O208 Rh4 N108 83.3(4) . . Y O206 Rh4 N108 88.7(4) . . Y N6 Rh4 Rh3 87.7(4) . . Y N8 Rh4 Rh3 88.7(4) . . Y O208 Rh4 Rh3 87.6(3) . . Y O206 Rh4 Rh3 86.7(3) . . Y N108 Rh4 Rh3 169.9(3) . . Y C1 N1 C11' 102.8(19) . . ? C1 N1 C11 115.7(18) . . ? C11' N1 C11 24.9(12) . . ? C1 N1 Rh1 122.9(12) . . ? C11' N1 Rh1 134.0(18) . . ? C11 N1 Rh1 119.1(15) . . ? C1 N2 C21 115.6(15) . . ? C1 N2 Rh2 123.9(13) . . ? C21 N2 Rh2 120.3(11) . . ? C2 N3 C31 116.5(14) . . ? C2 N3 Rh1 122.8(12) . . ? C31 N3 Rh1 120.7(11) . . ? C2 N4 C41 113.4(13) . . ? C2 N4 Rh2 121.0(11) . . ? C41 N4 Rh2 125.6(11) . . ? C3 N5 C51 118.2(13) . . ? C3 N5 Rh3 119.4(11) . . ? C51 N5 Rh3 121.9(11) . . ? C3 N6 C61' 121(3) . . ? C3 N6 C61 109(2) . . ? C61' N6 C61 14(3) . . ? C3 N6 Rh4 121.5(12) . . ? C61' N6 Rh4 117(2) . . ? C61 N6 Rh4 130(2) . . ? C4 N7 C71 113.3(14) . . ? C4 N7 Rh3 120.1(12) . . ? C71 N7 Rh3 125.2(11) . . ? C4 N8 C81 117.4(14) . . ? C4 N8 Rh4 118.9(11) . . ? C81 N8 Rh4 123.5(12) . . ? C24 O2 C27 119.9(19) . . ? C37 O3 C34 112(2) . . ? C47 O4 C44 117.8(17) . . ? C54 O5 C57 117.9(14) . . ? C77 O7 C74 116(2) . . ? C84 O8 C87 119.5(16) . . ? C5 O201 Rh1 121.4(10) . . ? C5 O202 Rh2 121.6(10) . . ? C8 O203 Rh1 119.2(11) . . ? C8 O204 Rh2 121.5(11) . . ? C7 O205 Rh3 119.6(10) . . ? C7 O206 Rh4 120.1(10) . . ? C10 O207 Rh3 118.5(10) . . ? C10 O208 Rh4 116.0(10) . . ? N2 C1 N1 117.6(16) . . ? N3 C2 N4 120.3(15) . . ? N6 C3 N5 122.2(15) . . ? N7 C4 N8 123.0(16) . . ? O202 C5 O201 122.0(14) . . ? O202 C5 C6 121.8(14) . . ? O201 C5 C6 116.2(14) . . ? C5 C6 C7 106.4(13) . . ? O206 C7 O205 125.1(15) . . ? O206 C7 C6 121.6(15) . . ? O205 C7 C6 113.2(14) . . ? O203 C8 O204 125.7(16) . . ? O203 C8 C9 116.8(15) . . ? O204 C8 C9 117.5(15) . . ? C8 C9 C10 105.1(13) . . ? O207 C10 O208 127.6(15) . . ? O207 C10 C9 118.3(14) . . ? O208 C10 C9 114.0(15) . . ? C12 C11 C16 129(2) . . ? C12 C11 N1 118(2) . . ? C16 C11 N1 113(2) . . ? C13 C12 C11 111(3) . . ? C14 C13 C12 126(3) . . ? C13 C14 O1 117(3) . . ? C13 C14 C15 127(4) . . ? O1 C14 C15 115(3) . . ? C14 C15 C16 115(3) . . ? C11 C16 C15 112(3) . . ? C17 O1 C14 125(2) . . ? C12' C11' C16' 127(2) . . ? C12' C11' N1 111(2) . . ? C16' C11' N1 122(3) . . ? C13' C12' C11' 113(3) . . ? C14' C13' C12' 124(4) . . ? C13' C14' O1' 120(3) . . ? C13' C14' C15' 127(4) . . ? O1' C14' C15' 112(3) . . ? C14' C15' C16' 115(3) . . ? C11' C16' C15' 112(3) . . ? C17' O1' C14' 129(3) . . ? C26 C21 C22 121.8(19) . . ? C26 C21 N2 118.8(16) . . ? C22 C21 N2 119.4(16) . . ? C23 C22 C21 118.2(17) . . ? C24 C23 C22 120.0(19) . . ? O2 C24 C23 113.6(19) . . ? O2 C24 C25 123(2) . . ? C23 C24 C25 124(2) . . ? C24 C25 C26 115.0(19) . . ? C21 C26 C25 121.1(18) . . ? C32 C31 C36 123.9(18) . . ? C32 C31 N3 119.4(15) . . ? C36 C31 N3 116.6(17) . . ? C31 C32 C33 121.3(18) . . ? C34 C33 C32 110(2) . . ? C35 C34 C33 131(3) . . ? C35 C34 O3 109(2) . . ? C33 C34 O3 119(3) . . ? C34 C35 C36 117(2) . . ? C31 C36 C35 116(2) . . ? C42 C41 C46 123.3(18) . . ? C42 C41 N4 117.9(16) . . ? C46 C41 N4 118.7(15) . . ? C41 C42 C43 119.7(17) . . ? C44 C43 C42 115.8(17) . . ? C45 C44 C43 128(2) . . ? C45 C44 O4 118.0(19) . . ? C43 C44 O4 113.9(17) . . ? C44 C45 C46 114.7(19) . . ? C41 C46 C45 118.2(17) . . ? C56 C51 C52 122.2(16) . . ? C56 C51 N5 118.0(15) . . ? C52 C51 N5 119.8(14) . . ? C53 C52 C51 122.7(15) . . ? C52 C53 C54 113.9(16) . . ? C55 C54 O5 113.0(16) . . ? C55 C54 C53 125.8(18) . . ? O5 C54 C53 121.1(16) . . ? C54 C55 C56 116.7(16) . . ? C51 C56 C55 118.6(16) . . ? C66 C61 C62 120(3) . . ? C66 C61 N6 117(2) . . ? C62 C61 N6 117(3) . . ? C61 C62 C63 117(3) . . ? C64 C63 C62 114(3) . . ? C65 C64 C63 133(3) . . ? C65 C64 O6 116(3) . . ? C63 C64 O6 111(3) . . ? C64 C65 C66 111(3) . . ? C61 C66 C65 115(3) . . ? C64 O6 C67 101(3) . . ? C66' C61' C62' 120(3) . . ? C66' C61' N6 118(3) . . ? C62' C61' N6 116(3) . . ? C61' C62' C63' 117(3) . . ? C64' C63' C62' 113(3) . . ? C65' C64' C63' 132(3) . . ? C65' C64' O6' 115(3) . . ? C63' C64' O6' 113(3) . . ? C64' C65' C66' 113(3) . . ? C61' C66' C65' 116(3) . . ? C64' O6' C67' 134(4) . . ? C72 C71 C76 120(2) . . ? C72 C71 N7 120.2(18) . . ? C76 C71 N7 119.5(17) . . ? C71 C72 C73 124(2) . . ? C74 C73 C72 110(2) . . ? C75 C74 C73 129(3) . . ? C75 C74 O7 115(2) . . ? C73 C74 O7 116(2) . . ? C74 C75 C76 120(2) . . ? C71 C76 C75 116.7(19) . . ? C82 C81 C86 123.6(16) . . ? C82 C81 N8 119.0(15) . . ? C86 C81 N8 117.2(15) . . ? C81 C82 C83 118.5(16) . . ? C84 C83 C82 117.4(18) . . ? C83 C84 C85 127(2) . . ? C83 C84 O8 114.4(18) . . ? C85 C84 O8 118.5(17) . . ? C84 C85 C86 114.9(17) . . ? C81 C86 C85 118.2(16) . . ? C101 N101 C105 119.2(15) . . ? C101 N101 Rh1 130.1(11) . 7_565 ? C105 N101 Rh1 109.4(11) . 7_565 ? C107 N102 C106 116.2(14) . . ? C107 N103 C108 115.3(15) . . ? C108 N104 C106 116.3(14) . . ? C111 N105 C110 126(2) . . ? C137 N108 C136 118.7(16) . 7_565 ? C137 N108 Rh4 127.5(11) . . ? C136 N108 Rh4 113.1(11) 7_565 . ? C121 N121 C125 120.0(14) . . ? C121 N121 Rh3 131.1(11) . . ? C125 N121 Rh3 108.7(11) . . ? C126 N122 C127 116.2(15) . . ? C127 N123 C128 113.3(15) . . ? C128 N124 C126 117.1(17) . . ? C132 N125 C131 124(2) . . ? C145 N141 C141 119.3(15) . . ? C145 N141 Rh2 126.3(11) . . ? C141 N141 Rh2 114.0(12) . . ? N101 C101 C102 124.4(16) . . ? C103 C102 C101 116.5(15) . . ? C104 C103 C102 119.1(16) . . ? C104 C103 C106 120.1(15) . . ? C102 C103 C106 120.8(15) . . ? C103 C104 C105 120.8(16) . . ? N101 C105 C104 119.7(16) . . ? N102 C106 N104 123.3(16) . . ? N102 C106 C103 119.7(15) . . ? N104 C106 C103 116.8(14) . . ? N102 C107 N103 124.8(14) . . ? N102 C107 C113 118.4(15) . . ? N103 C107 C113 116.8(15) . . ? N104 C108 N103 124.0(15) . . ? N104 C108 C143 117.6(14) . . ? N103 C108 C143 118.3(16) . . ? C113 C109 C110 120(2) . . ? N105 C110 C109 116(2) . . ? N105 C111 C112 122(2) . . ? C113 C112 C111 113.0(19) . . ? C112 C113 C109 123.3(17) . . ? C112 C113 C107 116.8(17) . . ? C109 C113 C107 119.9(17) . . ? N121 C121 C122 121.2(16) . . ? C121 C122 C123 118.2(17) . . ? C124 C123 C122 118.1(15) . . ? C124 C123 C126 122.4(15) . . ? C122 C123 C126 119.1(16) . . ? C125 C124 C123 120.2(16) . . ? C124 C125 N121 121.9(16) . . ? N122 C126 N124 123.3(15) . . ? N122 C126 C123 120.5(15) . . ? N124 C126 C123 116.1(16) . . ? N122 C127 N123 125.9(17) . . ? N122 C127 C134 115.8(15) . . ? N123 C127 C134 118.0(16) . . ? N124 C128 N123 124.0(16) . . ? N124 C128 C129 118.6(18) . . ? N123 C128 C129 117.3(16) . . ? C130 C129 C133 123.4(18) . . ? C130 C129 C128 119.2(18) . . ? C133 C129 C128 117.2(19) . . ? C129 C130 C131 119(2) . . ? N125 C131 C130 116(2) . . ? N125 C132 C133 126(2) . . ? C132 C133 C129 112(2) . . ? C135 C134 C138 117.1(17) . . ? C135 C134 C127 122.0(16) . . ? C138 C134 C127 120.9(15) . . ? C134 C135 C136 120.5(16) . . ? N108 C136 C135 121.6(16) 7_566 . ? N108 C137 C138 121.7(16) . 7_565 ? C137 C138 C134 120.3(16) 7_566 . ? N141 C141 C142 121.3(16) . . ? C143 C142 C141 116.5(15) . . ? C142 C143 C144 121.6(15) . . ? C142 C143 C108 118.7(15) . . ? C144 C143 C108 119.5(16) . . ? C145 C144 C143 118.4(17) . . ? N141 C145 C144 122.4(16) . . ? Cl2 C1S Cl3 108.6(14) . . ? Cl2 C1S Cl1 106.1(12) . . ? Cl3 C1S Cl1 108.1(12) . . ? Cl5 C2S Cl6 109.2(17) . . ? Cl5 C2S Cl4 105.2(14) . . ? Cl6 C2S Cl4 103.1(14) . . ? Cl9 C3S Cl7 114(2) . . ? Cl9 C3S Cl8 118(3) . . ? Cl7 C3S Cl8 108(2) . . ? Cl10 C4S Cl11 135(3) . . ? Cl10 C4S Cl12 96(2) . . ? Cl11 C4S Cl12 87.4(18) . . ? Cl12 C4S Cl13 127(3) . . ? Cl15 C5S Cl14 139(3) . . ? Cl15 C5S Cl17 110(3) . . ? Cl14 C5S Cl16 98(2) . . ? Cl20 C6S Cl18 84(2) . . ? Cl20 C6S Cl19 75(3) . . ? Cl18 C6S Cl19 120(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 22.52 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.953 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.133 data_cmpd_4 _database_code_CSD 154476 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[RH4(DAniF)4(C3H2O4)2]3[C3N3(C5H4N)3]4(4.1CH2Cl2)(1Et2O)(1H2O)' _chemical_formula_sum 'C278.10 H260.20 Cl8.20 N48 O50 Rh12' _chemical_formula_weight 6600.35 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1' 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 19.458(1) _cell_length_b 22.577(1) _cell_length_c 45.763(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.352(1) _cell_angle_gamma 90.00 _cell_volume 19980(2) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 6917 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.30 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6688 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69198 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 22.51 _reflns_number_total 24998 _reflns_number_gt 14907 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _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^)+(0.1793P)^2^+25.7321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24998 _refine_ls_number_parameters 931 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2941 _refine_ls_wR_factor_gt 0.2441 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.032 _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 Rh1 Rh -0.51178(5) -0.01439(4) 1.42632(2) 0.0530(3) Uani 1 1 d . . . Rh2 Rh -0.47429(5) -0.10783(4) 1.45118(2) 0.0518(3) Uani 1 1 d . . . Rh3 Rh -1.03575(5) 0.35529(4) 1.481207(19) 0.0439(3) Uani 1 1 d . . . Rh4 Rh -1.12364(4) 0.39992(4) 1.509149(19) 0.0410(3) Uani 1 1 d . . . Rh5 Rh -0.67411(5) 0.40014(5) 1.234365(19) 0.0493(3) Uani 1 1 d . C . Rh6 Rh -0.61866(5) 0.40579(4) 1.188918(18) 0.0463(3) Uani 1 1 d . C . N1 N -0.5775(5) -0.0621(5) 1.3989(2) 0.063(3) Uiso 1 1 d . . . N2 N -0.5330(5) -0.1509(4) 1.4193(2) 0.059(3) Uiso 1 1 d . . . N3 N -0.4360(5) -0.0274(5) 1.3997(2) 0.062(3) Uiso 1 1 d . . . N4 N -0.3922(5) -0.1054(4) 1.4278(2) 0.058(3) Uiso 1 1 d . . . N5 N -1.0432(5) 0.2812(4) 1.5055(2) 0.051(2) Uiso 1 1 d . . . N6 N -1.1132(5) 0.3295(4) 1.53632(19) 0.049(2) Uiso 1 1 d . . . N7 N -1.1139(5) 0.3276(4) 1.4512(2) 0.050(2) Uiso 1 1 d . . . N8 N -1.1967(5) 0.3583(4) 1.4815(2) 0.050(2) Uiso 1 1 d . . . N9 N -0.7363(5) 0.4673(4) 1.2201(2) 0.054(3) Uiso 1 1 d . . . N10 N -0.6965(5) 0.4617(4) 1.1736(2) 0.054(3) Uiso 1 1 d . . . N11 N -0.7405(5) 0.3397(5) 1.2136(2) 0.062(3) Uiso 1 1 d . . . N12 N -0.6712(5) 0.3322(4) 1.17473(19) 0.049(2) Uiso 1 1 d . . . N21 N -0.5556(5) 0.0789(4) 1.4139(2) 0.051(2) Uiso 1 1 d . . . N22 N -0.6773(5) 0.2600(4) 1.3713(2) 0.051(2) Uiso 1 1 d . A . N23 N -0.7716(5) 0.3195(4) 1.38092(19) 0.047(2) Uiso 1 1 d . A . N24 N -0.7287(5) 0.2476(4) 1.41582(19) 0.048(2) Uiso 1 1 d . A . N25 N -0.9395(5) 0.3323(4) 1.4570(2) 0.052(2) Uiso 1 1 d . . . N26 N -0.7005(5) 0.3872(4) 1.2823(2) 0.052(2) Uiso 1 1 d . . . N27 N -1.1954(4) 0.4577(4) 1.53276(18) 0.043(2) Uiso 1 1 d . . . N28 N -1.3565(5) 0.6282(4) 1.53606(19) 0.049(2) Uiso 1 1 d . . . N29 N -1.4504(4) 0.6568(4) 1.56181(19) 0.046(2) Uiso 1 1 d . . . N30 N -1.3861(4) 0.5695(4) 1.57555(18) 0.042(2) Uiso 1 1 d . . . N31 N -0.5603(5) 0.4148(4) 1.14868(19) 0.045(2) Uiso 1 1 d . . . N32 N -1.4500(5) 0.8094(4) 1.4807(2) 0.053(2) Uiso 1 1 d . . . O3 O -0.3940(9) 0.1031(8) 1.2992(4) 0.163(6) Uiso 1 1 d . A . O4 O -0.1734(7) -0.2629(6) 1.4619(3) 0.117(4) Uiso 1 1 d . A . O5 O -0.9469(13) 0.0514(11) 1.4792(5) 0.242(10) Uiso 1 1 d . . . O6 O -1.2302(9) 0.3264(8) 1.6424(4) 0.167(6) Uiso 1 1 d . . . O7 O -1.0945(10) 0.2601(9) 1.3346(4) 0.189(7) Uiso 1 1 d . . . O8 O -1.4725(7) 0.4041(6) 1.4942(3) 0.121(4) Uiso 1 1 d . . . O9 O -0.9265(8) 0.5840(7) 1.2831(3) 0.147(5) Uiso 1 1 d . . . O10 O -0.7392(6) 0.5538(5) 1.0595(2) 0.102(3) Uiso 1 1 d . . . O12 O -0.5798(5) 0.2004(5) 1.0832(2) 0.091(3) Uiso 1 1 d . C . O201 O -0.4423(4) 0.0287(3) 1.45633(16) 0.051(2) Uiso 1 1 d . . . O202 O -0.4170(4) -0.0552(3) 1.48284(16) 0.055(2) Uiso 1 1 d . . . O203 O -0.5834(4) -0.0089(4) 1.45608(17) 0.058(2) Uiso 1 1 d . . . O204 O -0.5585(4) -0.0987(3) 1.47511(17) 0.057(2) Uiso 1 1 d . . . O205 O -1.0347(4) 0.4354(3) 1.45911(15) 0.0464(18) Uiso 1 1 d . . . O206 O -1.1263(4) 0.4694(3) 1.47981(15) 0.0449(18) Uiso 1 1 d . . . O207 O -0.9637(4) 0.3918(3) 1.51362(15) 0.0462(18) Uiso 1 1 d . . . O208 O -1.0455(4) 0.4423(3) 1.53411(15) 0.0434(18) Uiso 1 1 d . . . O209 O -0.6089(4) 0.3300(3) 1.24570(16) 0.053(2) Uiso 1 1 d . . . O210 O -0.5401(4) 0.3510(3) 1.21072(16) 0.0496(19) Uiso 1 1 d . . . O211 O -0.5972(4) 0.4582(3) 1.25187(16) 0.052(2) Uiso 1 1 d . . . O212 O -0.5612(4) 0.4767(3) 1.20776(16) 0.052(2) Uiso 1 1 d . . . C501 C -0.4121(6) 0.0001(5) 1.4781(3) 0.055(3) Uiso 1 1 d . A . C502 C -0.9831(5) 0.4289(5) 1.5312(2) 0.039(3) Uiso 1 1 d . . . C503 C -1.0778(5) 0.4746(4) 1.4636(2) 0.038(2) Uiso 1 1 d . . . C504 C -1.0724(6) 0.5357(5) 1.4492(2) 0.046(3) Uiso 1 1 d . . . C505 C -0.5891(6) -0.0493(5) 1.4747(2) 0.050(3) Uiso 1 1 d . . . C506 C -0.3656(7) 0.0356(6) 1.5008(3) 0.063(3) Uiso 1 1 d . . . C521 C -0.5540(6) 0.3250(5) 1.2338(2) 0.045(3) Uiso 1 1 d . C . C522 C -0.5000 0.2848(7) 1.2500 0.053(4) Uiso 1 2 d S . . C523 C -0.5574(6) 0.4827(5) 1.2355(2) 0.047(3) Uiso 1 1 d . C . C524 C -0.5000 0.5214(8) 1.2500 0.058(5) Uiso 1 2 d S . . C201 C -0.5669(6) 0.1020(5) 1.3869(3) 0.058(3) Uiso 1 1 d . A . C202 C -0.6072(7) 0.1534(6) 1.3803(3) 0.063(3) Uiso 1 1 d . . . C203 C -0.6369(6) 0.1811(5) 1.4036(2) 0.049(3) Uiso 1 1 d . A . C204 C -0.6245(6) 0.1568(5) 1.4323(2) 0.050(3) Uiso 1 1 d . . . C205 C -0.5817(6) 0.1064(5) 1.4363(3) 0.052(3) Uiso 1 1 d . A . C206 C -0.6822(6) 0.2328(5) 1.3969(2) 0.045(3) Uiso 1 1 d . . . C207 C -0.7218(6) 0.3037(5) 1.3644(2) 0.048(3) Uiso 1 1 d . . . C208 C -0.7720(5) 0.2908(5) 1.4067(2) 0.039(3) Uiso 1 1 d . . . C209 C -0.8274(5) 0.3060(5) 1.4250(2) 0.042(3) Uiso 1 1 d . A . C210 C -0.8305(6) 0.2820(5) 1.4527(2) 0.053(3) Uiso 1 1 d . . . C211 C -0.8872(6) 0.2956(5) 1.4685(3) 0.057(3) Uiso 1 1 d . A . C212 C -0.9321(6) 0.3599(5) 1.4316(3) 0.058(3) Uiso 1 1 d . A . C213 C -0.8792(6) 0.3469(5) 1.4144(3) 0.057(3) Uiso 1 1 d . . . C215 C -0.7159(6) 0.3345(5) 1.3367(2) 0.045(3) Uiso 1 1 d . A . C216 C -0.6510(5) 0.3371(5) 1.3259(2) 0.044(3) Uiso 1 1 d . . . C217 C -0.6453(6) 0.3657(5) 1.2994(2) 0.047(3) Uiso 1 1 d . A . C218 C -0.7638(6) 0.3852(5) 1.2924(3) 0.053(3) Uiso 1 1 d . A . C219 C -0.7739(6) 0.3596(5) 1.3200(3) 0.059(3) Uiso 1 1 d . . . C221 C -1.1848(6) 0.5161(5) 1.5291(2) 0.046(3) Uiso 1 1 d . . . C222 C -1.2332(6) 0.5575(5) 1.5359(2) 0.052(3) Uiso 1 1 d . . . C223 C -1.2932(5) 0.5389(5) 1.5482(2) 0.042(3) Uiso 1 1 d . . . C224 C -1.3019(6) 0.4786(5) 1.5533(2) 0.045(3) Uiso 1 1 d . . . C225 C -1.2510(6) 0.4394(5) 1.5452(2) 0.046(3) Uiso 1 1 d . . . C226 C -1.3487(6) 0.5814(5) 1.5536(2) 0.044(3) Uiso 1 1 d . . . C227 C -1.4100(5) 0.6645(5) 1.5407(2) 0.042(3) Uiso 1 1 d . . . C228 C -1.4356(6) 0.6087(5) 1.5788(2) 0.044(3) Uiso 1 1 d . . . C229 C -1.4793(6) 0.5977(5) 1.6030(2) 0.044(3) Uiso 1 1 d . . . C230 C -1.4514(6) 0.5772(5) 1.6303(2) 0.048(3) Uiso 1 1 d . . . C231 C -0.4935(6) 0.4279(5) 1.1527(2) 0.046(3) Uiso 1 1 d . . . C232 C -0.5893(6) 0.3987(5) 1.1215(3) 0.051(3) Uiso 1 1 d . C . C233 C -0.5516(6) 0.3888(5) 1.0982(2) 0.046(3) Uiso 1 1 d . . . C234 C -1.4239(6) 0.7143(5) 1.5203(3) 0.052(3) Uiso 1 1 d . . . C235 C -1.3917(7) 0.7181(6) 1.4946(3) 0.074(4) Uiso 1 1 d . . . C236 C -1.4054(7) 0.7650(6) 1.4753(3) 0.075(4) Uiso 1 1 d . . . C237 C -1.4822(6) 0.8043(6) 1.5051(3) 0.060(3) Uiso 1 1 d . . . C238 C -1.4721(6) 0.7578(5) 1.5253(3) 0.054(3) Uiso 1 1 d . . . C1 C -0.5758(7) -0.1217(6) 1.3993(3) 0.067(4) Uiso 1 1 d . A . C2 C -0.3897(6) -0.0698(5) 1.4050(3) 0.055(3) Uiso 1 1 d . A . C3 C -1.0776(6) 0.2828(5) 1.5295(3) 0.053(3) Uiso 1 1 d . . . C4 C -1.1792(6) 0.3355(5) 1.4564(3) 0.054(3) Uiso 1 1 d . . . C5 C -0.7396(6) 0.4845(5) 1.1914(3) 0.057(3) Uiso 1 1 d . . . C6 C -0.7223(6) 0.3121(6) 1.1895(3) 0.060(3) Uiso 1 1 d . C . C11 C -0.6434(14) -0.0397(12) 1.3802(6) 0.068(5) Uiso 0.40(2) 1 d PG A 1 C12 C -0.6892(15) -0.0033(13) 1.3934(5) 0.083(6) Uiso 0.40(2) 1 d PG A 1 C13 C -0.7470(15) 0.0207(12) 1.3757(6) 0.095(7) Uiso 0.40(2) 1 d PG A 1 C14 C -0.7376(15) 0.0119(10) 1.3437(6) 0.123(9) Uiso 0.40(2) 1 d PG A 1 C15 C -0.7035(19) -0.0281(13) 1.3306(5) 0.132(10) Uiso 0.40(2) 1 d PG A 1 C16 C -0.6479(17) -0.0530(12) 1.3508(6) 0.102(8) Uiso 0.40(2) 1 d PG A 1 O1 O -0.8008(19) 0.0538(16) 1.3266(8) 0.213(12) Uiso 0.40(2) 1 d PG A 1 C17 C -0.823(2) 0.010(2) 1.3059(8) 0.34(4) Uiso 0.40(2) 1 d PG A 1 C11' C -0.6227(9) -0.0324(8) 1.3753(4) 0.068(5) Uiso 0.60(2) 1 d PG A 2 C12' C -0.6760(10) 0.0005(9) 1.3850(4) 0.083(6) Uiso 0.60(2) 1 d PG A 2 C13' C -0.7254(10) 0.0285(8) 1.3645(5) 0.095(7) Uiso 0.60(2) 1 d PG A 2 C14' C -0.7087(11) 0.0163(7) 1.3338(4) 0.123(9) Uiso 0.60(2) 1 d PG A 2 C15' C -0.6602(13) -0.0132(9) 1.3233(3) 0.132(10) Uiso 0.60(2) 1 d PG A 2 C16' C -0.6126(11) -0.0397(9) 1.3461(4) 0.102(8) Uiso 0.60(2) 1 d PG A 2 O1' O -0.7693(14) 0.0540(11) 1.3127(6) 0.213(12) Uiso 0.60(2) 1 d PG A 2 C17' C -0.7737(17) 0.0124(14) 1.2896(5) 0.34(4) Uiso 0.60(2) 1 d PG A 2 C21 C -0.5383(13) -0.2144(8) 1.4193(5) 0.057(4) Uiso 0.672(11) 1 d PD A 1 C22 C -0.5989(14) -0.2394(11) 1.4270(5) 0.099(7) Uiso 0.672(11) 1 d PD A 1 C23 C -0.6057(16) -0.3035(13) 1.4231(6) 0.116(9) Uiso 0.672(11) 1 d PD A 1 C24 C -0.5560(12) -0.3350(10) 1.4139(5) 0.081(7) Uiso 0.672(11) 1 d PD A 1 C25 C -0.4956(19) -0.3117(14) 1.4034(8) 0.121(10) Uiso 0.672(11) 1 d PD A 1 C26 C -0.4879(11) -0.2488(10) 1.4083(5) 0.084(6) Uiso 0.672(11) 1 d PD A 1 O2 O -0.5664(9) -0.3991(8) 1.4129(4) 0.108(5) Uiso 0.672(11) 1 d PD A 1 C27 C -0.5151(15) -0.4366(11) 1.4052(6) 0.096(7) Uiso 0.672(11) 1 d PD A 1 C21' C -0.538(3) -0.2143(13) 1.4122(11) 0.057(4) Uiso 0.328(11) 1 d PD A 2 C22' C -0.558(3) -0.2531(17) 1.4335(9) 0.099(7) Uiso 0.328(11) 1 d PD A 2 C23' C -0.543(3) -0.3160(19) 1.4277(11) 0.116(9) Uiso 0.328(11) 1 d PD A 2 C24' C -0.501(3) -0.3299(15) 1.4085(9) 0.081(7) Uiso 0.328(11) 1 d PD A 2 C25' C -0.479(3) -0.2927(18) 1.3858(11) 0.121(10) Uiso 0.328(11) 1 d PD A 2 C26' C -0.494(2) -0.2317(15) 1.3916(10) 0.084(6) Uiso 0.328(11) 1 d PD A 2 O2' O -0.4924(19) -0.3932(13) 1.4005(7) 0.108(5) Uiso 0.328(11) 1 d PD A 2 C27' C -0.505(3) -0.4348(17) 1.4218(11) 0.096(7) Uiso 0.328(11) 1 d PD A 2 C31 C -0.4252(6) 0.0089(6) 1.3743(3) 0.059(3) Uiso 1 1 d . A . C32 C -0.4304(11) -0.0225(9) 1.3467(5) 0.129(7) Uiso 1 1 d . . . C33 C -0.4214(12) 0.0172(11) 1.3206(5) 0.142(8) Uiso 1 1 d . A . C34 C -0.4040(9) 0.0735(8) 1.3259(4) 0.098(5) Uiso 1 1 d . . . C35 C -0.3952(8) 0.1011(7) 1.3523(4) 0.087(5) Uiso 1 1 d . A . C36 C -0.4082(7) 0.0668(7) 1.3769(3) 0.078(4) Uiso 1 1 d . . . C37 C -0.3706(13) 0.1638(12) 1.3025(5) 0.156(9) Uiso 1 1 d . . . C41 C -0.3324(7) -0.1455(6) 1.4347(3) 0.062(3) Uiso 1 1 d . A . C42 C -0.3147(7) -0.1852(6) 1.4138(3) 0.069(4) Uiso 1 1 d . . . C43 C -0.2580(8) -0.2251(7) 1.4224(3) 0.082(4) Uiso 1 1 d . A . C44 C -0.2282(9) -0.2214(7) 1.4508(4) 0.091(5) Uiso 1 1 d . . . C45 C -0.2441(9) -0.1822(8) 1.4708(4) 0.093(5) Uiso 1 1 d . A . C46 C -0.2980(8) -0.1421(7) 1.4632(3) 0.086(5) Uiso 1 1 d . . . C47 C -0.1482(10) -0.3029(9) 1.4413(4) 0.121(6) Uiso 1 1 d . . . C51 C -1.0131(7) 0.2237(6) 1.5002(3) 0.067(4) Uiso 1 1 d . . . C52 C -1.0181(10) 0.2029(9) 1.4723(4) 0.114(6) Uiso 1 1 d . . . C53 C -0.9917(13) 0.1433(11) 1.4666(5) 0.147(8) Uiso 1 1 d . . . C54 C -0.9608(11) 0.1185(10) 1.4912(5) 0.124(7) Uiso 1 1 d . . . C55 C -0.9465(12) 0.1371(11) 1.5185(5) 0.137(7) Uiso 1 1 d . . . C56 C -0.9751(9) 0.1950(8) 1.5223(4) 0.103(5) Uiso 1 1 d . . . C57 C -0.906(3) 0.036(2) 1.5062(11) 0.31(2) Uiso 1 1 d . . . C61 C -1.1441(6) 0.3263(5) 1.5633(3) 0.057(3) Uiso 1 1 d . . . C62 C -1.1278(8) 0.3697(6) 1.5842(3) 0.076(4) Uiso 1 1 d . . . C63 C -1.1595(9) 0.3674(8) 1.6116(4) 0.097(5) Uiso 1 1 d . . . C64 C -1.2035(10) 0.3234(9) 1.6136(4) 0.107(6) Uiso 1 1 d . . . C65 C -1.2235(10) 0.2812(9) 1.5952(4) 0.118(6) Uiso 1 1 d . . . C66 C -1.1911(8) 0.2834(7) 1.5674(4) 0.091(5) Uiso 1 1 d . . . C67 C -1.2807(19) 0.2865(16) 1.6430(7) 0.230(14) Uiso 1 1 d . . . C71 C -1.1077(7) 0.3090(7) 1.4222(3) 0.075(4) Uiso 1 1 d . . . C72 C -1.1266(11) 0.2464(9) 1.4157(5) 0.126(7) Uiso 1 1 d . . . C73 C -1.1205(11) 0.2286(10) 1.3844(5) 0.131(7) Uiso 1 1 d . . . C74 C -1.0987(10) 0.2762(10) 1.3662(5) 0.116(6) Uiso 1 1 d . . . C75 C -1.0934(10) 0.3359(10) 1.3691(4) 0.120(6) Uiso 1 1 d . . . C76 C -1.1011(10) 0.3513(8) 1.4010(4) 0.109(6) Uiso 1 1 d . . . C77 C -1.1189(17) 0.1990(16) 1.3258(7) 0.211(13) Uiso 1 1 d . . . C81 C -1.2682(6) 0.3684(5) 1.4831(2) 0.052(3) Uiso 1 1 d . . . C82 C -1.3081(9) 0.3265(7) 1.4964(3) 0.090(5) Uiso 1 1 d . B . C83 C -1.3787(9) 0.3404(8) 1.4990(4) 0.095(5) Uiso 1 1 d . . . C84 C -1.4040(8) 0.3903(7) 1.4905(3) 0.075(4) Uiso 1 1 d . B . C85 C -1.3686(8) 0.4339(7) 1.4775(3) 0.085(4) Uiso 1 1 d . . . C86 C -1.2975(7) 0.4215(6) 1.4737(3) 0.072(4) Uiso 1 1 d . B . C87 C -1.496(2) 0.3995(17) 1.5201(9) 0.110(12) Uiso 0.50 1 d P B 1 C87' C -1.500(3) 0.451(2) 1.4972(11) 0.156(17) Uiso 0.50 1 d P B 2 C91 C -0.7827(7) 0.4948(6) 1.2361(3) 0.065(4) Uiso 1 1 d . . . C92 C -0.7606(8) 0.5193(6) 1.2630(3) 0.077(4) Uiso 1 1 d . . . C93 C -0.8058(9) 0.5495(7) 1.2802(3) 0.089(5) Uiso 1 1 d . . . C94 C -0.8749(9) 0.5522(8) 1.2682(4) 0.100(5) Uiso 1 1 d . . . C95 C -0.9027(10) 0.5290(8) 1.2416(4) 0.112(6) Uiso 1 1 d . . . C96 C -0.8544(9) 0.5002(8) 1.2251(4) 0.096(5) Uiso 1 1 d . . . C97 C -0.9109(17) 0.6096(14) 1.3119(7) 0.211(13) Uiso 1 1 d . . . C101 C -0.7039(6) 0.4870(5) 1.1447(2) 0.053(3) Uiso 1 1 d . . . C102 C -0.7543(7) 0.4624(6) 1.1238(3) 0.066(4) Uiso 1 1 d . . . C103 C -0.7653(7) 0.4864(6) 1.0950(3) 0.076(4) Uiso 1 1 d . . . C104 C -0.7261(7) 0.5310(6) 1.0896(3) 0.071(4) Uiso 1 1 d . . . C105 C -0.6703(8) 0.5572(7) 1.1086(3) 0.089(5) Uiso 1 1 d . . . C106 C -0.6602(7) 0.5308(6) 1.1382(3) 0.076(4) Uiso 1 1 d . . . C107 C -0.6959(10) 0.5978(8) 1.0494(4) 0.113(6) Uiso 1 1 d . . . C111 C -0.7832(10) 0.2988(10) 1.2302(4) 0.055(5) Uiso 0.616(17) 1 d PD C 1 C112 C -0.7505(13) 0.2544(12) 1.2491(6) 0.089(6) Uiso 0.616(17) 1 d PD C 1 C113 C -0.7944(17) 0.2168(14) 1.2661(6) 0.111(8) Uiso 0.616(17) 1 d PD C 1 C114 C -0.8665(17) 0.2399(16) 1.2635(7) 0.114(9) Uiso 0.616(17) 1 d PD C 1 C115 C -0.8944(14) 0.2783(15) 1.2485(6) 0.099(8) Uiso 0.616(17) 1 d PD C 1 C116 C -0.8504(11) 0.3165(13) 1.2321(5) 0.083(6) Uiso 0.616(17) 1 d PD C 1 O11 O -0.913(2) 0.1980(18) 1.2785(9) 0.228(14) Uiso 0.616(17) 1 d PD C 1 C131 C -0.7893(14) 0.3228(16) 1.2318(7) 0.055(5) Uiso 0.384(17) 1 d PD C 2 C132 C -0.776(2) 0.2665(17) 1.2456(10) 0.089(6) Uiso 0.384(17) 1 d PD C 2 C133 C -0.821(2) 0.246(2) 1.2679(10) 0.111(8) Uiso 0.384(17) 1 d PD C 2 C134 C -0.884(2) 0.285(3) 1.2658(10) 0.114(9) Uiso 0.384(17) 1 d PD C 2 C135 C -0.9041(17) 0.322(2) 1.2484(9) 0.099(8) Uiso 0.384(17) 1 d PD C 2 C136 C -0.8541(17) 0.3493(19) 1.2305(8) 0.083(6) Uiso 0.384(17) 1 d PD C 2 O13 O -0.937(3) 0.264(3) 1.2858(11) 0.228(14) Uiso 0.384(17) 1 d PD C 2 C137 C -0.902(3) 0.219(2) 1.2982(11) 0.28(2) Uiso 1 1 d . . . C121 C -0.6531(6) 0.2964(5) 1.1518(3) 0.057(3) Uiso 1 1 d . C . C122 C -0.7014(8) 0.2802(6) 1.1271(3) 0.077(4) Uiso 1 1 d . . . C123 C -0.6769(7) 0.2453(6) 1.1034(3) 0.073(4) Uiso 1 1 d . C . C124 C -0.6113(7) 0.2320(6) 1.1053(3) 0.069(4) Uiso 1 1 d . . . C125 C -0.5607(7) 0.2464(6) 1.1279(3) 0.070(4) Uiso 1 1 d . C . C126 C -0.5841(7) 0.2796(6) 1.1514(3) 0.067(4) Uiso 1 1 d . . . C127 C -0.6280(9) 0.1810(8) 1.0583(4) 0.104(5) Uiso 1 1 d . . . C1S C -1.078(2) 0.445(3) 1.1577(11) 0.13(3) Uiso 0.25 1 d PD . . Cl1 Cl -1.030(3) 0.477(2) 1.1329(10) 0.179(18) Uiso 0.15 1 d PD . . Cl2 Cl -1.0360(17) 0.4169(15) 1.1895(7) 0.196(12) Uiso 0.25 1 d PD . . Cl3 Cl -0.994(2) 0.466(3) 1.1610(14) 0.15(2) Uiso 0.10 1 d PD . . C2S C -0.421(3) 0.1209(10) 1.1986(8) 0.19(2) Uiso 0.50 1 d PD . . Cl4 Cl -0.365(3) 0.079(2) 1.2300(11) 0.167(17) Uiso 0.15 1 d P . . Cl5 Cl -0.4220(14) 0.1937(9) 1.1948(5) 0.131(8) Uiso 0.25 1 d PD . . Cl6 Cl -0.3814(9) 0.1882(7) 1.2024(4) 0.124(5) Uiso 0.35 1 d PD . . Cl7 Cl -0.4177(18) 0.0844(13) 1.2305(6) 0.166(10) Uiso 0.25 1 d PD . . C3S C -1.3050(12) 0.4621(11) 1.6328(5) 0.144(10) Uiso 0.80 1 d PD . . Cl8 Cl -1.2460(7) 0.5169(6) 1.6336(3) 0.181(5) Uiso 0.60 1 d PD . . Cl9 Cl -1.3573(9) 0.4443(8) 1.6611(3) 0.183(6) Uiso 0.50 1 d PD . . Cl10 Cl -1.3297(10) 0.4785(9) 1.6642(4) 0.203(7) Uiso 0.50 1 d PD . . C4S C -1.209(2) 0.138(2) 1.5296(7) 0.095(14) Uiso 0.35 1 d PD . . Cl11 Cl -1.2567(16) 0.1167(14) 1.5606(6) 0.220(12) Uiso 0.30 1 d PD . . Cl12 Cl -1.209(2) 0.1724(17) 1.4934(7) 0.226(15) Uiso 0.25 1 d PD . . Cl13 Cl -1.159(4) 0.099(4) 1.5590(15) 0.32(4) Uiso 0.15 1 d PD . . C5S C -0.7663(16) 0.0752(14) 1.4578(7) 0.083(9) Uiso 0.50 1 d P . . C6S C -0.802(3) 0.109(2) 1.4412(11) 0.137(15) Uiso 0.50 1 d P . . O1S O -0.845(3) 0.104(2) 1.4178(11) 0.225(18) Uiso 0.50 1 d P . . C7S C -0.866(3) 0.140(2) 1.3980(11) 0.141(16) Uiso 0.50 1 d P . . C8S C -0.923(4) 0.183(3) 1.3801(15) 0.22(3) Uiso 0.50 1 d P . . C9S C -1.402(3) 0.369(3) 1.6952(18) 0.08(3) Uiso 0.15 1 d PD . . Cl14 Cl -1.486(3) 0.356(3) 1.6842(15) 0.24(3) Uiso 0.15 1 d PD . . Cl15 Cl -1.407(2) 0.435(2) 1.6776(10) 0.155(15) Uiso 0.15 1 d PD . . O2S O -0.2519(19) 0.0227(16) 1.4370(8) 0.181(13) Uiso 0.50 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 0.0652(7) 0.0469(6) 0.0486(6) 0.0080(4) 0.0144(5) 0.0225(5) Rh2 0.0649(7) 0.0434(6) 0.0489(6) 0.0066(4) 0.0151(5) 0.0191(5) Rh3 0.0442(5) 0.0408(5) 0.0492(6) 0.0002(4) 0.0171(4) 0.0096(4) Rh4 0.0383(5) 0.0400(5) 0.0467(5) -0.0003(4) 0.0141(4) 0.0051(4) Rh5 0.0369(5) 0.0757(7) 0.0367(5) 0.0057(5) 0.0103(4) 0.0018(5) Rh6 0.0379(5) 0.0682(7) 0.0340(5) 0.0035(4) 0.0090(4) -0.0003(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 N1 2.004(10) . Y Rh1 N3 2.035(10) . Y Rh1 O203 2.057(8) . Y Rh1 O201 2.062(7) . Y Rh1 N21 2.320(9) . Y Rh1 Rh2 2.4685(13) . Y Rh2 N2 2.004(10) . Y Rh2 N4 2.019(10) . Y Rh2 O204 2.079(8) . Y Rh2 O202 2.097(8) . Y Rh2 N32 2.322(9) 1_645 Y Rh3 N5 2.024(9) . Y Rh3 N7 2.031(9) . Y Rh3 O205 2.074(7) . Y Rh3 O207 2.095(7) . Y Rh3 N25 2.337(10) . Y Rh3 Rh4 2.4615(12) . Y Rh4 N6 2.016(9) . Y Rh4 N8 2.026(9) . Y Rh4 O208 2.037(7) . Y Rh4 O206 2.061(7) . Y Rh4 N27 2.271(9) . Y Rh5 N9 2.003(10) . Y Rh5 N11 2.040(10) . Y Rh5 O209 2.059(8) . Y Rh5 O211 2.081(8) . Y Rh5 N26 2.327(9) . Y Rh5 Rh6 2.4499(12) . Y Rh6 N12 2.021(9) . Y Rh6 N10 2.035(9) . Y Rh6 O212 2.084(8) . Y Rh6 O210 2.127(7) . Y Rh6 N31 2.277(9) . Y N1 C1 1.346(16) . ? N1 C11' 1.476(17) . ? N1 C11 1.54(2) . ? N2 C1 1.341(15) . ? N2 C21 1.44(2) . ? N2 C21' 1.47(3) . ? N3 C2 1.319(15) . ? N3 C31 1.454(15) . ? N4 C2 1.322(14) . ? N4 C41 1.482(15) . ? N5 C3 1.347(14) . ? N5 C51 1.457(15) . ? N6 C3 1.316(14) . ? N6 C61 1.434(14) . ? N7 C4 1.331(14) . ? N7 C71 1.411(16) . ? N8 C4 1.334(14) . ? N8 C81 1.421(14) . ? N9 C5 1.362(14) . ? N9 C91 1.375(15) . ? N10 C5 1.335(14) . ? N10 C101 1.435(14) . ? N11 C6 1.348(15) . ? N11 C131 1.38(3) . ? N11 C111 1.50(2) . ? N12 C6 1.342(14) . ? N12 C121 1.398(14) . ? N21 C201 1.338(14) . ? N21 C205 1.344(14) . ? N22 C207 1.328(14) . ? N22 C206 1.337(13) . ? N23 C207 1.342(14) . ? N23 C208 1.346(13) . ? N24 C208 1.325(13) . ? N24 C206 1.360(13) . ? N25 C212 1.341(14) . ? N25 C211 1.372(14) . ? N26 C217 1.346(14) . ? N26 C218 1.363(14) . ? N27 C225 1.342(13) . ? N27 C221 1.348(13) . ? N28 C226 1.323(13) . ? N28 C227 1.360(13) . ? N29 C227 1.324(13) . ? N29 C228 1.346(13) . ? N30 C228 1.330(13) . ? N30 C226 1.333(13) . ? N31 C231 1.326(13) . ? N31 C232 1.357(14) . ? N32 C237 1.345(14) . ? N32 C236 1.366(16) . ? N32 Rh2 2.322(9) 1_465 ? O3 C34 1.43(2) . ? O3 C37 1.45(3) . ? O4 C47 1.43(2) . ? O4 C44 1.468(18) . ? O5 C57 1.44(5) . ? O5 C54 1.64(3) . ? O6 C67 1.33(4) . ? O6 C64 1.47(2) . ? O7 C77 1.50(3) . ? O7 C74 1.51(2) . ? O8 C87' 1.20(5) . ? O8 C87 1.32(4) . ? O8 C84 1.398(18) . ? O9 C97 1.44(3) . ? O9 C94 1.46(2) . ? O10 C107 1.41(2) . ? O10 C104 1.465(16) . ? O12 C124 1.429(16) . ? O12 C127 1.463(19) . ? O201 C501 1.275(13) . ? O202 C501 1.271(13) . ? O203 C505 1.262(13) . ? O204 C505 1.265(13) . ? O205 C503 1.251(12) . ? O206 C503 1.270(12) . ? O207 C502 1.247(12) . ? O208 C502 1.273(12) . ? O209 C521 1.257(12) . ? O210 C521 1.265(12) . ? O211 C523 1.265(13) . ? O212 C523 1.270(12) . ? C501 C506 1.527(17) . ? C502 C504 1.548(14) 3_368 ? C503 C504 1.536(15) . ? C504 C502 1.548(14) 3_368 ? C505 C506 1.532(16) 3_458 ? C506 C505 1.532(16) 3_458 ? C521 C522 1.517(14) . ? C522 C521 1.517(14) 2_457 ? C523 C524 1.511(15) . ? C524 C523 1.511(15) 2_457 ? C201 C202 1.413(17) . ? C202 C203 1.414(16) . ? C203 C204 1.419(15) . ? C203 C206 1.474(15) . ? C204 C205 1.410(15) . ? C207 C215 1.462(15) . ? C208 C209 1.479(14) . ? C209 C210 1.384(15) . ? C209 C213 1.413(15) . ? C210 C211 1.419(16) . ? C212 C213 1.392(16) . ? C215 C216 1.406(15) . ? C215 C219 1.410(16) . ? C216 C217 1.392(15) . ? C218 C219 1.421(16) . ? C221 C222 1.385(15) . ? C222 C223 1.417(15) . ? C223 C224 1.393(15) . ? C223 C226 1.486(14) . ? C224 C225 1.408(15) . ? C227 C234 1.467(15) . ? C228 C229 1.492(15) . ? C229 C230 1.383(15) . ? C229 C233 1.432(15) 4_466 ? C230 C231 1.386(15) 4_466 ? C231 C230 1.385(15) 4_665 ? C232 C233 1.379(15) . ? C233 C229 1.432(15) 4_665 ? C234 C235 1.394(17) . ? C234 C238 1.395(16) . ? C235 C236 1.385(18) . ? C237 C238 1.399(16) . ? C11 C16 1.3721 . ? C11 C12 1.3955 . ? C12 C13 1.4178 . ? C13 C14 1.5070 . ? C14 C15 1.3058 . ? C14 O1 1.6756 . ? C15 C16 1.4567 . ? O1 C17 1.3998 . ? C11' C16' 1.3814 . ? C11' C12' 1.3872 . ? C12' C13' 1.4156 . ? C13' C14' 1.5044 . ? C14' C15' 1.2888 . ? C14' O1' 1.6723 . ? C15' C16' 1.4463 . ? O1' C17' 1.4105 . ? C21 C26 1.39(2) . ? C21 C22 1.39(3) . ? C22 C23 1.46(3) . ? C23 C24 1.31(4) . ? C24 C25 1.42(4) . ? C24 O2 1.46(2) . ? C25 C26 1.44(3) . ? O2 C27 1.38(3) . ? C21' C22' 1.40(3) . ? C21' C26' 1.40(3) . ? C22' C23' 1.48(3) . ? C23' C24' 1.31(4) . ? C24' C25' 1.43(4) . ? C24' O2' 1.49(3) . ? C25' C26' 1.44(3) . ? O2' C27' 1.40(3) . ? C31 C36 1.351(18) . ? C31 C32 1.44(2) . ? C32 C33 1.52(3) . ? C33 C34 1.33(3) . ? C34 C35 1.35(2) . ? C35 C36 1.41(2) . ? C41 C42 1.383(17) . ? C41 C46 1.400(18) . ? C42 C43 1.445(19) . ? C43 C44 1.368(19) . ? C44 C45 1.33(2) . ? C45 C46 1.40(2) . ? C51 C56 1.35(2) . ? C51 C52 1.35(2) . ? C52 C53 1.47(3) . ? C53 C54 1.34(3) . ? C54 C55 1.32(3) . ? C55 C56 1.44(3) . ? C61 C66 1.358(19) . ? C61 C62 1.382(18) . ? C62 C63 1.45(2) . ? C63 C64 1.32(2) . ? C64 C65 1.30(2) . ? C65 C66 1.48(2) . ? C71 C76 1.38(2) . ? C71 C72 1.48(2) . ? C72 C73 1.50(3) . ? C73 C74 1.45(3) . ? C74 C75 1.36(2) . ? C75 C76 1.53(2) . ? C81 C86 1.375(17) . ? C81 C82 1.405(19) . ? C82 C83 1.43(2) . ? C83 C84 1.27(2) . ? C84 C85 1.37(2) . ? C85 C86 1.44(2) . ? C91 C92 1.371(18) . ? C91 C96 1.43(2) . ? C92 C93 1.42(2) . ? C93 C94 1.40(2) . ? C94 C95 1.38(2) . ? C95 C96 1.42(2) . ? C101 C106 1.359(17) . ? C101 C102 1.406(16) . ? C102 C103 1.419(18) . ? C103 C104 1.304(18) . ? C104 C105 1.44(2) . ? C105 C106 1.473(19) . ? C111 C116 1.38(2) . ? C111 C112 1.43(2) . ? C112 C113 1.48(3) . ? C113 C114 1.49(4) . ? C114 C115 1.20(4) . ? C114 O11 1.53(4) . ? C114 C137 1.86(5) . ? C115 C116 1.48(3) . ? O11 C137 1.02(5) . ? C131 C136 1.39(3) . ? C131 C132 1.43(3) . ? C132 C133 1.50(3) . ? C133 C134 1.50(4) . ? C134 C135 1.19(4) . ? C134 O13 1.53(4) . ? C135 C136 1.48(3) . ? O13 C137 1.34(6) . ? C121 C126 1.398(17) . ? C121 C122 1.437(17) . ? C122 C123 1.460(19) . ? C123 C124 1.306(18) . ? C124 C125 1.386(17) . ? C125 C126 1.426(18) . ? C1S Cl3 1.68(2) . ? C1S Cl1 1.71(2) . ? C1S Cl2 1.71(2) . ? C2S Cl5 1.654(18) . ? C2S Cl7 1.672(19) . ? C2S Cl6 1.707(19) . ? C2S Cl4 1.95(7) . ? C3S Cl10 1.607(17) . ? C3S Cl8 1.686(16) . ? C3S Cl9 1.781(17) . ? C4S Cl13 1.80(2) . ? C4S Cl12 1.835(19) . ? C4S Cl11 1.838(19) . ? C5S C6S 1.23(5) . ? C6S O1S 1.29(5) . ? O1S C7S 1.26(6) . ? C7S C8S 1.62(7) . ? C9S Cl14 1.69(2) . ? C9S Cl15 1.69(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 N1 Rh1 N3 90.1(4) . . ? N1 Rh1 O203 90.9(4) . . ? N3 Rh1 O203 173.6(4) . . ? N1 Rh1 O201 175.5(4) . . ? N3 Rh1 O201 90.1(4) . . ? O203 Rh1 O201 88.4(3) . . ? N1 Rh1 N21 98.3(4) . . ? N3 Rh1 N21 104.8(4) . . ? O203 Rh1 N21 81.3(3) . . ? O201 Rh1 N21 86.0(3) . . ? N1 Rh1 Rh2 88.0(3) . . ? N3 Rh1 Rh2 87.5(3) . . ? O203 Rh1 Rh2 86.2(2) . . ? O201 Rh1 Rh2 87.6(2) . . ? N21 Rh1 Rh2 166.1(2) . . ? N2 Rh2 N4 92.7(4) . . ? N2 Rh2 O204 90.7(4) . . ? N4 Rh2 O204 172.8(4) . . ? N2 Rh2 O202 174.5(4) . . ? N4 Rh2 O202 87.7(4) . . ? O204 Rh2 O202 88.3(3) . . ? N2 Rh2 N32 95.5(4) . 1_645 ? N4 Rh2 N32 102.0(4) . 1_645 ? O204 Rh2 N32 84.0(3) . 1_645 ? O202 Rh2 N32 89.8(3) . 1_645 ? N2 Rh2 Rh1 87.9(3) . . ? N4 Rh2 Rh1 86.7(3) . . ? O204 Rh2 Rh1 87.1(2) . . ? O202 Rh2 Rh1 86.6(2) . . ? N32 Rh2 Rh1 170.4(2) 1_645 . ? N5 Rh3 N7 91.3(4) . . ? N5 Rh3 O205 174.1(3) . . ? N7 Rh3 O205 89.2(3) . . ? N5 Rh3 O207 91.1(3) . . ? N7 Rh3 O207 172.9(3) . . ? O205 Rh3 O207 87.7(3) . . ? N5 Rh3 N25 100.8(4) . . ? N7 Rh3 N25 101.0(3) . . ? O205 Rh3 N25 84.9(3) . . ? O207 Rh3 N25 85.1(3) . . ? N5 Rh3 Rh4 87.5(3) . . ? N7 Rh3 Rh4 88.1(3) . . ? O205 Rh3 Rh4 86.6(2) . . ? O207 Rh3 Rh4 85.4(2) . . ? N25 Rh3 Rh4 167.5(2) . . ? N6 Rh4 N8 92.1(4) . . ? N6 Rh4 O208 90.4(3) . . ? N8 Rh4 O208 175.2(3) . . ? N6 Rh4 O206 174.8(3) . . ? N8 Rh4 O206 88.8(3) . . ? O208 Rh4 O206 88.4(3) . . ? N6 Rh4 N27 100.7(3) . . ? N8 Rh4 N27 97.9(3) . . ? O208 Rh4 N27 85.6(3) . . ? O206 Rh4 N27 84.3(3) . . ? N6 Rh4 Rh3 88.2(3) . . ? N8 Rh4 Rh3 88.0(3) . . ? O208 Rh4 Rh3 88.0(2) . . ? O206 Rh4 Rh3 86.7(2) . . ? N27 Rh4 Rh3 169.1(2) . . ? N9 Rh5 N11 91.4(4) . . ? N9 Rh5 O209 175.6(3) . . ? N11 Rh5 O209 86.8(4) . . ? N9 Rh5 O211 91.8(3) . . ? N11 Rh5 O211 172.6(4) . . ? O209 Rh5 O211 89.5(3) . . ? N9 Rh5 N26 102.4(4) . . ? N11 Rh5 N26 99.3(4) . . ? O209 Rh5 N26 82.0(3) . . ? O211 Rh5 N26 86.6(3) . . ? N9 Rh5 Rh6 89.5(3) . . ? N11 Rh5 Rh6 87.4(3) . . ? O209 Rh5 Rh6 86.4(2) . . ? O211 Rh5 Rh6 85.9(2) . . ? N26 Rh5 Rh6 166.2(2) . . ? N12 Rh6 N10 93.9(4) . . ? N12 Rh6 O212 173.8(3) . . ? N10 Rh6 O212 90.6(3) . . ? N12 Rh6 O210 89.1(3) . . ? N10 Rh6 O210 172.2(3) . . ? O212 Rh6 O210 85.9(3) . . ? N12 Rh6 N31 95.4(3) . . ? N10 Rh6 N31 94.9(3) . . ? O212 Rh6 N31 88.5(3) . . ? O210 Rh6 N31 92.0(3) . . ? N12 Rh6 Rh5 88.6(3) . . ? N10 Rh6 Rh5 86.8(3) . . ? O212 Rh6 Rh5 87.4(2) . . ? O210 Rh6 Rh5 86.1(2) . . ? N31 Rh6 Rh5 175.6(2) . . ? C1 N1 C11' 118.4(12) . . ? C1 N1 C11 110.6(14) . . ? C11' N1 C11 19.3(13) . . ? C1 N1 Rh1 121.1(9) . . ? C11' N1 Rh1 120.0(10) . . ? C11 N1 Rh1 127.1(12) . . ? C1 N2 C21 116.9(15) . . ? C1 N2 C21' 108(2) . . ? C21 N2 C21' 13(2) . . ? C1 N2 Rh2 121.3(9) . . ? C21 N2 Rh2 121.3(12) . . ? C21' N2 Rh2 131(2) . . ? C2 N3 C31 113.6(11) . . ? C2 N3 Rh1 121.3(8) . . ? C31 N3 Rh1 125.1(8) . . ? C2 N4 C41 116.3(10) . . ? C2 N4 Rh2 122.4(8) . . ? C41 N4 Rh2 121.3(8) . . ? C3 N5 C51 114.0(10) . . ? C3 N5 Rh3 119.8(8) . . ? C51 N5 Rh3 126.1(8) . . ? C3 N6 C61 116.5(10) . . ? C3 N6 Rh4 120.3(8) . . ? C61 N6 Rh4 123.2(7) . . ? C4 N7 C71 113.1(10) . . ? C4 N7 Rh3 119.7(8) . . ? C71 N7 Rh3 126.3(8) . . ? C4 N8 C81 116.7(9) . . ? C4 N8 Rh4 119.2(8) . . ? C81 N8 Rh4 121.2(7) . . ? C5 N9 C91 114.9(11) . . ? C5 N9 Rh5 119.5(8) . . ? C91 N9 Rh5 125.3(8) . . ? C5 N10 C101 113.8(10) . . ? C5 N10 Rh6 121.5(8) . . ? C101 N10 Rh6 124.0(8) . . ? C6 N11 C131 128.6(19) . . ? C6 N11 C111 109.8(13) . . ? C131 N11 C111 21.9(16) . . ? C6 N11 Rh5 118.7(9) . . ? C131 N11 Rh5 110.3(17) . . ? C111 N11 Rh5 122.2(10) . . ? C6 N12 C121 116.4(10) . . ? C6 N12 Rh6 119.5(8) . . ? C121 N12 Rh6 123.7(8) . . ? C201 N21 C205 119.2(10) . . ? C201 N21 Rh1 126.7(8) . . ? C205 N21 Rh1 113.1(7) . . ? C207 N22 C206 116.2(10) . . ? C207 N23 C208 116.1(9) . . ? C208 N24 C206 115.2(9) . . ? C212 N25 C211 117.8(10) . . ? C212 N25 Rh3 118.6(8) . . ? C211 N25 Rh3 123.4(8) . . ? C217 N26 C218 119.0(10) . . ? C217 N26 Rh5 110.3(7) . . ? C218 N26 Rh5 128.7(8) . . ? C225 N27 C221 119.7(9) . . ? C225 N27 Rh4 126.3(7) . . ? C221 N27 Rh4 113.1(7) . . ? C226 N28 C227 115.2(9) . . ? C227 N29 C228 114.9(9) . . ? C228 N30 C226 114.3(9) . . ? C231 N31 C232 119.2(10) . . ? C231 N31 Rh6 118.5(7) . . ? C232 N31 Rh6 121.5(7) . . ? C237 N32 C236 116.7(11) . . ? C237 N32 Rh2 117.9(8) . 1_465 ? C236 N32 Rh2 125.4(8) . 1_465 ? C34 O3 C37 115.1(18) . . ? C47 O4 C44 117.5(14) . . ? C57 O5 C54 92(3) . . ? C67 O6 C64 109(2) . . ? C77 O7 C74 116(2) . . ? C87' O8 C87 76(3) . . ? C87' O8 C84 131(3) . . ? C87 O8 C84 121(2) . . ? C97 O9 C94 123(2) . . ? C107 O10 C104 120.4(13) . . ? C124 O12 C127 114.4(12) . . ? C501 O201 Rh1 119.5(7) . . ? C501 O202 Rh2 118.9(7) . . ? C505 O203 Rh1 121.3(8) . . ? C505 O204 Rh2 118.5(7) . . ? C503 O205 Rh3 119.7(7) . . ? C503 O206 Rh4 119.1(6) . . ? C502 O207 Rh3 119.6(7) . . ? C502 O208 Rh4 119.4(6) . . ? C521 O209 Rh5 119.3(7) . . ? C521 O210 Rh6 116.9(7) . . ? C523 O211 Rh5 120.6(7) . . ? C523 O212 Rh6 117.7(7) . . ? O202 C501 O201 126.5(11) . . ? O202 C501 C506 116.7(10) . . ? O201 C501 C506 116.8(11) . . ? O207 C502 O208 126.0(9) . . ? O207 C502 C504 118.6(9) . 3_368 ? O208 C502 C504 115.4(9) . 3_368 ? O205 C503 O206 125.7(9) . . ? O205 C503 C504 119.1(9) . . ? O206 C503 C504 115.1(9) . . ? C503 C504 C502 106.9(8) . 3_368 ? O203 C505 O204 124.9(11) . . ? O203 C505 C506 116.7(11) . 3_458 ? O204 C505 C506 118.3(10) . 3_458 ? C501 C506 C505 104.9(10) . 3_458 ? O209 C521 O210 126.2(10) . . ? O209 C521 C522 114.8(9) . . ? O210 C521 C522 119.0(9) . . ? C521 C522 C521 106.5(13) . 2_457 ? O211 C523 O212 125.0(10) . . ? O211 C523 C524 117.6(9) . . ? O212 C523 C524 117.4(9) . . ? C523 C524 C523 109.5(14) . 2_457 ? N21 C201 C202 123.2(12) . . ? C201 C202 C203 117.8(11) . . ? C202 C203 C204 118.9(11) . . ? C202 C203 C206 118.6(10) . . ? C204 C203 C206 122.4(10) . . ? C205 C204 C203 118.1(10) . . ? N21 C205 C204 122.7(10) . . ? N22 C206 N24 124.1(10) . . ? N22 C206 C203 116.6(10) . . ? N24 C206 C203 119.2(10) . . ? N22 C207 N23 123.8(10) . . ? N22 C207 C215 116.6(10) . . ? N23 C207 C215 119.6(10) . . ? N24 C208 N23 124.4(10) . . ? N24 C208 C209 118.0(9) . . ? N23 C208 C209 117.4(9) . . ? C210 C209 C213 118.0(10) . . ? C210 C209 C208 122.5(10) . . ? C213 C209 C208 119.6(10) . . ? C209 C210 C211 119.8(11) . . ? N25 C211 C210 121.4(11) . . ? N25 C212 C213 123.3(11) . . ? C212 C213 C209 119.2(11) . . ? C216 C215 C219 119.3(10) . . ? C216 C215 C207 118.9(10) . . ? C219 C215 C207 121.8(10) . . ? C217 C216 C215 119.1(10) . . ? N26 C217 C216 122.6(10) . . ? N26 C218 C219 122.2(11) . . ? C215 C219 C218 117.7(11) . . ? N27 C221 C222 121.0(10) . . ? C221 C222 C223 119.9(11) . . ? C224 C223 C222 118.5(10) . . ? C224 C223 C226 120.0(10) . . ? C222 C223 C226 121.3(10) . . ? C223 C224 C225 117.9(10) . . ? N27 C225 C224 122.8(10) . . ? N28 C226 N30 125.6(10) . . ? N28 C226 C223 117.0(10) . . ? N30 C226 C223 117.4(9) . . ? N29 C227 N28 124.1(10) . . ? N29 C227 C234 118.9(10) . . ? N28 C227 C234 117.0(10) . . ? N30 C228 N29 125.8(10) . . ? N30 C228 C229 116.8(9) . . ? N29 C228 C229 117.4(9) . . ? C230 C229 C233 119.4(10) . 4_466 ? C230 C229 C228 121.9(10) . . ? C233 C229 C228 118.7(9) 4_466 . ? C229 C230 C231 119.3(10) . 4_466 ? N31 C231 C230 122.1(10) . 4_665 ? N31 C232 C233 123.3(10) . . ? C232 C233 C229 116.3(10) . 4_665 ? C235 C234 C238 117.9(11) . . ? C235 C234 C227 121.1(11) . . ? C238 C234 C227 121.0(11) . . ? C236 C235 C234 120.8(13) . . ? N32 C236 C235 121.9(13) . . ? N32 C237 C238 124.7(11) . . ? C234 C238 C237 117.9(11) . . ? N2 C1 N1 120.8(12) . . ? N3 C2 N4 120.2(11) . . ? N6 C3 N5 122.5(10) . . ? N7 C4 N8 123.0(10) . . ? N10 C5 N9 120.8(11) . . ? N12 C6 N11 122.2(12) . . ? C16 C11 C12 125.2 . . ? C16 C11 N1 115.4(17) . . ? C12 C11 N1 119.1(17) . . ? C11 C12 C13 119.0 . . ? C12 C13 C14 109.2 . . ? C15 C14 C13 131.3 . . ? C15 C14 O1 124.0 . . ? C13 C14 O1 102.6 . . ? C14 C15 C16 110.8 . . ? C11 C16 C15 120.0 . . ? C17 O1 C14 94.0 . . ? C16' C11' C12' 124.4 . . ? C16' C11' N1 121.0(12) . . ? C12' C11' N1 114.6(12) . . ? C11' C12' C13' 120.2 . . ? C12' C13' C14' 109.7 . . ? C15' C14' C13' 133.2 . . ? C15' C14' O1' 123.2 . . ? C13' C14' O1' 103.6 . . ? C14' C15' C16' 112.5 . . ? C11' C16' C15' 120.0 . . ? C17' O1' C14' 94.2 . . ? C26 C21 C22 121.3(19) . . ? C26 C21 N2 120.3(18) . . ? C22 C21 N2 117.9(18) . . ? C21 C22 C23 116(2) . . ? C24 C23 C22 121(3) . . ? C23 C24 C25 125(3) . . ? C23 C24 O2 116(2) . . ? C25 C24 O2 118(2) . . ? C24 C25 C26 113(3) . . ? C21 C26 C25 123(2) . . ? C27 O2 C24 120.8(18) . . ? C22' C21' C26' 122(3) . . ? C22' C21' N2 118(3) . . ? C26' C21' N2 113(3) . . ? C21' C22' C23' 114(3) . . ? C24' C23' C22' 120(3) . . ? C23' C24' C25' 127(3) . . ? C23' C24' O2' 120(3) . . ? C25' C24' O2' 109(3) . . ? C24' C25' C26' 110(3) . . ? C21' C26' C25' 123(3) . . ? C27' O2' C24' 116(3) . . ? C36 C31 C32 122.9(14) . . ? C36 C31 N3 122.2(12) . . ? C32 C31 N3 114.8(13) . . ? C31 C32 C33 113.4(18) . . ? C34 C33 C32 118(2) . . ? C33 C34 C35 128(2) . . ? C33 C34 O3 110.3(19) . . ? C35 C34 O3 122.2(18) . . ? C34 C35 C36 116.2(16) . . ? C31 C36 C35 121.8(14) . . ? C42 C41 C46 123.4(13) . . ? C42 C41 N4 119.8(11) . . ? C46 C41 N4 116.7(12) . . ? C41 C42 C43 117.2(12) . . ? C44 C43 C42 116.8(14) . . ? C45 C44 C43 125.9(17) . . ? C45 C44 O4 113.7(15) . . ? C43 C44 O4 120.4(15) . . ? C44 C45 C46 119.1(16) . . ? C45 C46 C41 117.5(15) . . ? C56 C51 C52 121.1(16) . . ? C56 C51 N5 120.0(13) . . ? C52 C51 N5 118.6(14) . . ? C51 C52 C53 119.6(18) . . ? C54 C53 C52 111(2) . . ? C55 C54 C53 134(3) . . ? C55 C54 O5 126(2) . . ? C53 C54 O5 100(2) . . ? C54 C55 C56 111(2) . . ? C51 C56 C55 122.2(18) . . ? C66 C61 C62 121.1(13) . . ? C66 C61 N6 120.4(12) . . ? C62 C61 N6 118.4(12) . . ? C61 C62 C63 119.0(14) . . ? C64 C63 C62 115.2(16) . . ? C65 C64 C63 131(2) . . ? C65 C64 O6 120.2(19) . . ? C63 C64 O6 108.9(18) . . ? C64 C65 C66 113.9(19) . . ? C61 C66 C65 119.9(15) . . ? C76 C71 N7 118.7(14) . . ? C76 C71 C72 124.1(16) . . ? N7 C71 C72 115.4(14) . . ? C71 C72 C73 113.7(18) . . ? C74 C73 C72 113.9(19) . . ? C75 C74 C73 135(2) . . ? C75 C74 O7 108.8(19) . . ? C73 C74 O7 114.9(19) . . ? C74 C75 C76 107.7(18) . . ? C71 C76 C75 122.8(17) . . ? C86 C81 C82 119.4(13) . . ? C86 C81 N8 119.9(11) . . ? C82 C81 N8 120.5(12) . . ? C81 C82 C83 118.2(15) . . ? C84 C83 C82 120.7(17) . . ? C83 C84 C85 124.9(16) . . ? C83 C84 O8 120.0(16) . . ? C85 C84 O8 115.1(14) . . ? C84 C85 C86 116.6(14) . . ? C81 C86 C85 120.2(13) . . ? C92 C91 N9 120.0(12) . . ? C92 C91 C96 118.5(14) . . ? N9 C91 C96 121.4(13) . . ? C91 C92 C93 122.5(14) . . ? C94 C93 C92 115.6(15) . . ? C95 C94 C93 126.7(18) . . ? C95 C94 O9 112.1(17) . . ? C93 C94 O9 121.2(16) . . ? C94 C95 C96 115.0(18) . . ? C95 C96 C91 121.7(15) . . ? C106 C101 C102 123.0(12) . . ? C106 C101 N10 119.3(11) . . ? C102 C101 N10 117.5(11) . . ? C101 C102 C103 120.1(12) . . ? C104 C103 C102 116.2(13) . . ? C103 C104 C105 128.3(14) . . ? C103 C104 O10 114.0(13) . . ? C105 C104 O10 117.6(13) . . ? C104 C105 C106 113.8(14) . . ? C101 C106 C105 118.2(13) . . ? C116 C111 C112 121.8(19) . . ? C116 C111 N11 115.8(18) . . ? C112 C111 N11 120.3(17) . . ? C111 C112 C113 118(2) . . ? C112 C113 C114 111(3) . . ? C115 C114 C113 131(3) . . ? C115 C114 O11 117(3) . . ? C113 C114 O11 110(3) . . ? C115 C114 C137 119(3) . . ? C113 C114 C137 106(3) . . ? O11 C114 C137 33(2) . . ? C114 C115 C116 118(3) . . ? C111 C116 C115 118(2) . . ? C137 O11 C114 92(5) . . ? N11 C131 C136 122(2) . . ? N11 C131 C132 114(2) . . ? C136 C131 C132 121(2) . . ? C131 C132 C133 119(3) . . ? C132 C133 C134 108(3) . . ? C135 C134 C133 132(4) . . ? C135 C134 O13 115(4) . . ? C133 C134 O13 113(3) . . ? C134 C135 C136 118(3) . . ? C131 C136 C135 116(3) . . ? C137 O13 C134 98(4) . . ? O11 C137 O13 86(5) . . ? O11 C137 C114 55(4) . . ? O13 C137 C114 70(3) . . ? N12 C121 C126 119.3(11) . . ? N12 C121 C122 122.7(11) . . ? C126 C121 C122 117.8(12) . . ? C121 C122 C123 118.9(13) . . ? C124 C123 C122 118.2(13) . . ? C123 C124 C125 127.2(14) . . ? C123 C124 O12 124.2(13) . . ? C125 C124 O12 108.6(12) . . ? C124 C125 C126 115.3(13) . . ? C121 C126 C125 122.7(12) . . ? Cl3 C1S Cl2 71(3) . . ? Cl1 C1S Cl2 119(3) . . ? Cl5 C2S Cl7 126(3) . . ? Cl5 C2S Cl6 28.8(9) . . ? Cl7 C2S Cl6 112(2) . . ? Cl5 C2S Cl4 124(3) . . ? Cl6 C2S Cl4 98(3) . . ? Cl10 C3S Cl8 94.8(14) . . ? Cl8 C3S Cl9 126.4(15) . . ? Cl13 C4S Cl12 146(4) . . ? Cl12 C4S Cl11 149(3) . . ? C5S C6S O1S 137(5) . . ? C7S O1S C6S 132(6) . . ? O1S C7S C8S 154(5) . . ? Cl14 C9S Cl15 90(4) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.962 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.155