Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #======================================================================= _journal_coden_Cambridge 0222 _publ_contact_author ; Therrien, Bruno Institut de Chimie, Universite de Neuchatel, Case postale 158, CH-2009 Neuchatel, Switzerland ; _publ_contact_author_phone '+41 32 718 2499' _publ_contact_author_fax '+41 32 718 2511' _publ_contact_author_email bruno.therrien@unine.ch _publ_section_title ; Chiral or not chiral? A case study of the homologous metalloprisms [Cp*6M6(tpt)2(C2O4)3]6+ (M = Rh, Ir, tpt = 2,4,6-tri(pyridin-4-yl)-1,3,5-triazine) ; loop_ _publ_author_name _publ_author_address P.Govindaswamy ; Institut de Chimie, Universite de Neuchatel, Case postale 158, CH-2009 Neuchatel, Switzerland ; D.Linder ; Department of Organic Chemistry, University of Geneva, Quai E. Ansermet 30, CH-1211, Geneva 4, Switzerland ; J.Lacour ; Department of Organic Chemistry, University of Geneva, Quai E. Ansermet 30, CH-1211, Geneva 4, Switzerland ; G.Suss-Fink ; Institut de Chimie, Universite de Neuchatel, Case postale 158, CH-2009 Neuchatel, Switzerland ; B.Therrien ; Institut de Chimie, Universite de Neuchatel, Case postale 158, CH-2009 Neuchatel, Switzerland ; _publ_section_references ; Sheldrick, G. M. (1990). "SHELXS-97 Program for Crystal Structure Determination", Acta Cryst., A46, 467-473. Sheldrick, G. M. (1997). SHELXL-97. Univ. of Gottingen, Gottingen, Germany. Stoe & Cie (2000). IPDS Software. Stoe & Cie GmbH, Darmstadt, Germany. ; _publ_section_acknowledgements ; This work was supported by the Swiss National Science Foundation (grant No 20-61227-00). ; _publ_contact_author_name 'Therrien, Bruno' data_d:compound1 _database_code_depnum_ccdc_archive 'CCDC 650992' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 Cl2 O4 Rh2' _chemical_formula_sum 'C22 H30 Cl2 O4 Rh2' _chemical_formula_weight 635.18 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' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2751(6) _cell_length_b 8.8048(7) _cell_length_c 16.7033(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.804(9) _cell_angle_gamma 90.00 _cell_volume 1214.33(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.95 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 1.604 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; A crystal was mounted at 173K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using MoK\a graphite monochromated radiation. Image plate distance 70mm, \f oscillation scans 0 - 200\%, step \D\f = 1.2\%, 3 minutes per frame. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8801 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2333 _reflns_number_gt 2048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+2.5561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2333 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.000 _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 C1 C 0.5654(4) -0.0007(4) -0.0310(2) 0.0157(7) Uani 1 1 d . . . C2 C 0.7100(4) 0.2748(4) 0.1952(2) 0.0227(8) Uani 1 1 d . . . C3 C 0.8276(5) 0.1708(4) 0.2303(2) 0.0206(8) Uani 1 1 d . . . C4 C 0.9582(4) 0.1580(4) 0.1773(2) 0.0165(7) Uani 1 1 d . . . C5 C 0.9182(4) 0.2524(4) 0.1089(2) 0.0163(7) Uani 1 1 d . . . C6 C 0.7653(5) 0.3248(4) 0.1198(2) 0.0226(8) Uani 1 1 d . . . C7 C 0.5547(5) 0.3192(6) 0.2295(3) 0.0425(13) Uani 1 1 d . . . H7A H 0.5213 0.2402 0.2644 0.064 Uiso 1 1 calc R . . H7B H 0.4728 0.3340 0.1867 0.064 Uiso 1 1 calc R . . H7C H 0.5701 0.4118 0.2593 0.064 Uiso 1 1 calc R . . C8 C 0.8274(7) 0.0947(6) 0.3105(2) 0.0394(12) Uani 1 1 d . . . H8A H 0.9067 0.1417 0.3470 0.059 Uiso 1 1 calc R . . H8B H 0.8530 -0.0110 0.3049 0.059 Uiso 1 1 calc R . . H8C H 0.7222 0.1045 0.3310 0.059 Uiso 1 1 calc R . . C9 C 1.1059(5) 0.0636(5) 0.1912(3) 0.0318(10) Uani 1 1 d . . . H9A H 1.1512 0.0431 0.1409 0.048 Uiso 1 1 calc R . . H9B H 1.0783 -0.0304 0.2160 0.048 Uiso 1 1 calc R . . H9C H 1.1839 0.1171 0.2258 0.048 Uiso 1 1 calc R . . C10 C 1.0171(6) 0.2678(5) 0.0378(2) 0.0345(10) Uani 1 1 d . . . H10A H 1.0858 0.3555 0.0444 0.052 Uiso 1 1 calc R . . H10B H 0.9466 0.2792 -0.0098 0.052 Uiso 1 1 calc R . . H10C H 1.0827 0.1787 0.0331 0.052 Uiso 1 1 calc R . . C11 C 0.6775(7) 0.4315(5) 0.0616(3) 0.0412(12) Uani 1 1 d . . . H11A H 0.5628 0.4204 0.0652 0.062 Uiso 1 1 calc R . . H11B H 0.7050 0.4080 0.0080 0.062 Uiso 1 1 calc R . . H11C H 0.7086 0.5341 0.0744 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.77173(13) -0.18096(10) 0.13919(6) 0.0266(2) Uani 1 1 d . . . O1 O 0.7053(3) 0.0402(3) -0.00832(14) 0.0176(5) Uani 1 1 d . . . O2 O 0.5213(3) -0.0441(3) -0.10072(14) 0.0176(5) Uani 1 1 d . . . Rh1 Rh 0.73497(3) 0.08548(3) 0.118206(15) 0.01260(11) 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 C1 0.0196(19) 0.0128(16) 0.0151(16) -0.0013(13) 0.0029(15) 0.0005(13) C2 0.0170(19) 0.0224(19) 0.0285(19) -0.0172(16) -0.0005(15) -0.0022(15) C3 0.024(2) 0.0229(19) 0.0142(16) -0.0059(14) -0.0020(14) -0.0081(15) C4 0.0113(17) 0.0188(17) 0.0181(17) -0.0034(13) -0.0078(13) -0.0044(13) C5 0.0097(16) 0.0171(17) 0.0212(17) -0.0028(14) -0.0048(13) -0.0048(14) C6 0.031(2) 0.0100(16) 0.0258(19) -0.0047(14) -0.0040(16) -0.0022(15) C7 0.017(2) 0.054(3) 0.056(3) -0.035(2) 0.005(2) 0.0004(19) C8 0.053(3) 0.051(3) 0.0147(19) 0.0025(18) 0.0009(19) -0.020(2) C9 0.024(2) 0.031(2) 0.040(2) -0.0051(18) -0.0067(19) 0.0045(17) C10 0.045(3) 0.033(2) 0.027(2) 0.0007(18) 0.0114(19) -0.014(2) C11 0.050(3) 0.018(2) 0.052(3) 0.0032(19) -0.022(2) 0.0068(19) Cl1 0.0325(6) 0.0140(4) 0.0334(5) -0.0001(4) 0.0039(4) 0.0010(4) O1 0.0096(13) 0.0280(14) 0.0149(12) -0.0047(10) -0.0012(10) -0.0028(10) O2 0.0093(13) 0.0279(14) 0.0153(12) -0.0064(10) 0.0003(10) -0.0036(10) Rh1 0.01227(17) 0.01296(16) 0.01241(16) -0.00285(10) -0.00043(11) -0.00083(10) _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 C1 O1 1.247(4) . ? C1 O2 1.257(4) . ? C1 C1 1.547(6) 3_655 ? C2 C3 1.433(6) . ? C2 C6 1.438(5) . ? C2 C7 1.494(5) . ? C2 Rh1 2.123(3) . ? C3 C4 1.446(5) . ? C3 C8 1.498(5) . ? C3 Rh1 2.114(3) . ? C4 C5 1.434(5) . ? C4 C9 1.484(5) . ? C4 Rh1 2.134(3) . ? C5 C6 1.439(5) . ? C5 C10 1.493(5) . ? C5 Rh1 2.125(3) . ? C6 C11 1.504(6) . ? C6 Rh1 2.122(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? Cl1 Rh1 2.3884(9) . ? O1 Rh1 2.149(2) . ? O2 Rh1 2.152(2) 3_655 ? Rh1 O2 2.152(2) 3_655 ? 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 O1 C1 O2 125.2(3) . . ? O1 C1 C1 118.1(4) . 3_655 ? O2 C1 C1 116.7(4) . 3_655 ? C3 C2 C6 107.9(3) . . ? C3 C2 C7 126.1(4) . . ? C6 C2 C7 126.0(4) . . ? C3 C2 Rh1 69.9(2) . . ? C6 C2 Rh1 70.13(19) . . ? C7 C2 Rh1 123.9(3) . . ? C2 C3 C4 108.3(3) . . ? C2 C3 C8 127.6(4) . . ? C4 C3 C8 123.9(4) . . ? C2 C3 Rh1 70.6(2) . . ? C4 C3 Rh1 70.83(19) . . ? C8 C3 Rh1 127.7(3) . . ? C5 C4 C3 107.5(3) . . ? C5 C4 C9 126.5(3) . . ? C3 C4 C9 126.1(4) . . ? C5 C4 Rh1 70.01(19) . . ? C3 C4 Rh1 69.4(2) . . ? C9 C4 Rh1 125.7(3) . . ? C4 C5 C6 108.4(3) . . ? C4 C5 C10 125.2(3) . . ? C6 C5 C10 126.4(3) . . ? C4 C5 Rh1 70.65(19) . . ? C6 C5 Rh1 70.07(19) . . ? C10 C5 Rh1 123.5(3) . . ? C2 C6 C5 108.0(3) . . ? C2 C6 C11 126.1(4) . . ? C5 C6 C11 125.9(4) . . ? C2 C6 Rh1 70.3(2) . . ? C5 C6 Rh1 70.33(19) . . ? C11 C6 Rh1 124.1(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 O1 Rh1 113.3(2) . . ? C1 O2 Rh1 113.6(2) . 3_655 ? C3 Rh1 C6 66.46(15) . . ? C3 Rh1 C2 39.53(15) . . ? C6 Rh1 C2 39.60(15) . . ? C3 Rh1 C5 66.44(13) . . ? C6 Rh1 C5 39.60(15) . . ? C2 Rh1 C5 66.41(14) . . ? C3 Rh1 C4 39.81(14) . . ? C6 Rh1 C4 66.36(15) . . ? C2 Rh1 C4 66.48(14) . . ? C5 Rh1 C4 39.34(13) . . ? C3 Rh1 O1 161.50(12) . . ? C6 Rh1 O1 101.65(12) . . ? C2 Rh1 O1 137.05(13) . . ? C5 Rh1 O1 95.28(11) . . ? C4 Rh1 O1 123.32(12) . . ? C3 Rh1 O2 118.47(12) . 3_655 ? C6 Rh1 O2 106.53(13) . 3_655 ? C2 Rh1 O2 94.63(12) . 3_655 ? C5 Rh1 O2 143.96(12) . 3_655 ? C4 Rh1 O2 158.20(12) . 3_655 ? O1 Rh1 O2 77.75(9) . 3_655 ? C3 Rh1 Cl1 100.59(11) . . ? C6 Rh1 Cl1 163.68(11) . . ? C2 Rh1 Cl1 134.31(12) . . ? C5 Rh1 Cl1 127.27(10) . . ? C4 Rh1 Cl1 97.36(10) . . ? O1 Rh1 Cl1 88.12(7) . . ? O2 Rh1 Cl1 88.18(7) 3_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C2 C3 C4 1.0(4) . . . . ? C7 C2 C3 C4 179.1(3) . . . . ? Rh1 C2 C3 C4 61.1(2) . . . . ? C6 C2 C3 C8 176.8(4) . . . . ? C7 C2 C3 C8 -5.2(6) . . . . ? Rh1 C2 C3 C8 -123.1(4) . . . . ? C6 C2 C3 Rh1 -60.1(2) . . . . ? C7 C2 C3 Rh1 117.9(4) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C8 C3 C4 C5 -177.0(3) . . . . ? Rh1 C3 C4 C5 59.9(2) . . . . ? C2 C3 C4 C9 179.2(3) . . . . ? C8 C3 C4 C9 3.2(6) . . . . ? Rh1 C3 C4 C9 -119.9(4) . . . . ? C2 C3 C4 Rh1 -61.0(2) . . . . ? C8 C3 C4 Rh1 123.1(4) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C9 C4 C5 C6 -179.5(3) . . . . ? Rh1 C4 C5 C6 60.2(2) . . . . ? C3 C4 C5 C10 -177.4(3) . . . . ? C9 C4 C5 C10 2.3(6) . . . . ? Rh1 C4 C5 C10 -118.0(4) . . . . ? C3 C4 C5 Rh1 -59.5(2) . . . . ? C9 C4 C5 Rh1 120.3(4) . . . . ? C3 C2 C6 C5 -0.6(4) . . . . ? C7 C2 C6 C5 -178.6(4) . . . . ? Rh1 C2 C6 C5 -60.5(2) . . . . ? C3 C2 C6 C11 178.3(4) . . . . ? C7 C2 C6 C11 0.3(6) . . . . ? Rh1 C2 C6 C11 118.4(4) . . . . ? C3 C2 C6 Rh1 59.9(2) . . . . ? C7 C2 C6 Rh1 -118.1(4) . . . . ? C4 C5 C6 C2 -0.1(4) . . . . ? C10 C5 C6 C2 178.0(3) . . . . ? Rh1 C5 C6 C2 60.5(2) . . . . ? C4 C5 C6 C11 -179.0(4) . . . . ? C10 C5 C6 C11 -0.9(6) . . . . ? Rh1 C5 C6 C11 -118.5(4) . . . . ? C4 C5 C6 Rh1 -60.5(2) . . . . ? C10 C5 C6 Rh1 117.6(4) . . . . ? O2 C1 O1 Rh1 -174.6(3) . . . . ? C1 C1 O1 Rh1 5.2(5) 3_655 . . . ? O1 C1 O2 Rh1 -174.7(3) . . . 3_655 ? C1 C1 O2 Rh1 5.5(5) 3_655 . . 3_655 ? C2 C3 Rh1 C6 37.6(2) . . . . ? C4 C3 Rh1 C6 -80.8(2) . . . . ? C8 C3 Rh1 C6 160.6(4) . . . . ? C4 C3 Rh1 C2 -118.3(3) . . . . ? C8 C3 Rh1 C2 123.1(5) . . . . ? C2 C3 Rh1 C5 80.9(2) . . . . ? C4 C3 Rh1 C5 -37.4(2) . . . . ? C8 C3 Rh1 C5 -156.0(4) . . . . ? C2 C3 Rh1 C4 118.3(3) . . . . ? C8 C3 Rh1 C4 -118.6(5) . . . . ? C2 C3 Rh1 O1 90.2(4) . . . . ? C4 C3 Rh1 O1 -28.2(5) . . . . ? C8 C3 Rh1 O1 -146.7(4) . . . . ? C2 C3 Rh1 O2 -59.1(2) . . . 3_655 ? C4 C3 Rh1 O2 -177.48(18) . . . 3_655 ? C8 C3 Rh1 O2 63.9(4) . . . 3_655 ? C2 C3 Rh1 Cl1 -152.9(2) . . . . ? C4 C3 Rh1 Cl1 88.8(2) . . . . ? C8 C3 Rh1 Cl1 -29.8(4) . . . . ? C2 C6 Rh1 C3 -37.5(2) . . . . ? C5 C6 Rh1 C3 80.9(2) . . . . ? C11 C6 Rh1 C3 -158.4(4) . . . . ? C5 C6 Rh1 C2 118.4(3) . . . . ? C11 C6 Rh1 C2 -120.9(5) . . . . ? C2 C6 Rh1 C5 -118.4(3) . . . . ? C11 C6 Rh1 C5 120.7(5) . . . . ? C2 C6 Rh1 C4 -81.1(2) . . . . ? C5 C6 Rh1 C4 37.3(2) . . . . ? C11 C6 Rh1 C4 158.0(4) . . . . ? C2 C6 Rh1 O1 157.4(2) . . . . ? C5 C6 Rh1 O1 -84.2(2) . . . . ? C11 C6 Rh1 O1 36.5(4) . . . . ? C2 C6 Rh1 O2 76.9(2) . . . 3_655 ? C5 C6 Rh1 O2 -164.67(19) . . . 3_655 ? C11 C6 Rh1 O2 -44.0(4) . . . 3_655 ? C2 C6 Rh1 Cl1 -76.8(5) . . . . ? C5 C6 Rh1 Cl1 41.7(5) . . . . ? C11 C6 Rh1 Cl1 162.3(3) . . . . ? C6 C2 Rh1 C3 118.7(3) . . . . ? C7 C2 Rh1 C3 -120.6(5) . . . . ? C3 C2 Rh1 C6 -118.7(3) . . . . ? C7 C2 Rh1 C6 120.7(5) . . . . ? C3 C2 Rh1 C5 -81.0(2) . . . . ? C6 C2 Rh1 C5 37.7(2) . . . . ? C7 C2 Rh1 C5 158.4(4) . . . . ? C3 C2 Rh1 C4 -37.9(2) . . . . ? C6 C2 Rh1 C4 80.8(2) . . . . ? C7 C2 Rh1 C4 -158.5(4) . . . . ? C3 C2 Rh1 O1 -152.2(2) . . . . ? C6 C2 Rh1 O1 -33.5(3) . . . . ? C7 C2 Rh1 O1 87.1(4) . . . . ? C3 C2 Rh1 O2 130.8(2) . . . 3_655 ? C6 C2 Rh1 O2 -110.5(2) . . . 3_655 ? C7 C2 Rh1 O2 10.2(4) . . . 3_655 ? C3 C2 Rh1 Cl1 38.8(3) . . . . ? C6 C2 Rh1 Cl1 157.53(19) . . . . ? C7 C2 Rh1 Cl1 -81.8(4) . . . . ? C4 C5 Rh1 C3 37.8(2) . . . . ? C6 C5 Rh1 C3 -81.0(2) . . . . ? C10 C5 Rh1 C3 157.9(4) . . . . ? C4 C5 Rh1 C6 118.8(3) . . . . ? C10 C5 Rh1 C6 -121.1(4) . . . . ? C4 C5 Rh1 C2 81.1(2) . . . . ? C6 C5 Rh1 C2 -37.7(2) . . . . ? C10 C5 Rh1 C2 -158.8(4) . . . . ? C6 C5 Rh1 C4 -118.8(3) . . . . ? C10 C5 Rh1 C4 120.0(4) . . . . ? C4 C5 Rh1 O1 -139.2(2) . . . . ? C6 C5 Rh1 O1 101.9(2) . . . . ? C10 C5 Rh1 O1 -19.2(3) . . . . ? C4 C5 Rh1 O2 144.4(2) . . . 3_655 ? C6 C5 Rh1 O2 25.5(3) . . . 3_655 ? C10 C5 Rh1 O2 -95.6(4) . . . 3_655 ? C4 C5 Rh1 Cl1 -47.6(2) . . . . ? C6 C5 Rh1 Cl1 -166.42(17) . . . . ? C10 C5 Rh1 Cl1 72.5(3) . . . . ? C5 C4 Rh1 C3 -118.6(3) . . . . ? C9 C4 Rh1 C3 120.3(4) . . . . ? C5 C4 Rh1 C6 -37.6(2) . . . . ? C3 C4 Rh1 C6 81.0(2) . . . . ? C9 C4 Rh1 C6 -158.7(4) . . . . ? C5 C4 Rh1 C2 -80.9(2) . . . . ? C3 C4 Rh1 C2 37.7(2) . . . . ? C9 C4 Rh1 C2 157.9(4) . . . . ? C3 C4 Rh1 C5 118.6(3) . . . . ? C9 C4 Rh1 C5 -121.1(4) . . . . ? C5 C4 Rh1 O1 51.1(2) . . . . ? C3 C4 Rh1 O1 169.67(19) . . . . ? C9 C4 Rh1 O1 -70.1(4) . . . . ? C5 C4 Rh1 O2 -112.6(3) . . . 3_655 ? C3 C4 Rh1 O2 6.0(4) . . . 3_655 ? C9 C4 Rh1 O2 126.2(4) . . . 3_655 ? C5 C4 Rh1 Cl1 143.68(19) . . . . ? C3 C4 Rh1 Cl1 -97.7(2) . . . . ? C9 C4 Rh1 Cl1 22.5(3) . . . . ? C1 O1 Rh1 C3 -158.7(4) . . . . ? C1 O1 Rh1 C6 -110.7(3) . . . . ? C1 O1 Rh1 C2 -89.6(3) . . . . ? C1 O1 Rh1 C5 -150.2(2) . . . . ? C1 O1 Rh1 C4 -179.9(2) . . . . ? C1 O1 Rh1 O2 -6.0(2) . . . 3_655 ? C1 O1 Rh1 Cl1 82.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.930 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.147 #===END data_d:compound3 _database_code_depnum_ccdc_archive 'CCDC 650993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102H114N12O12Rh6, (CF3O3S)6, (C6H6)6' _chemical_formula_sum 'C144 H150 F18 N12 O30 Rh6 S6' _chemical_formula_weight 3680.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.082(2) _cell_length_b 20.0295(16) _cell_length_c 33.218(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.095(6) _cell_angle_gamma 90.00 _cell_volume 15672(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8611 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 23.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7464 _exptl_absorpt_coefficient_mu 0.792 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38450 _diffrn_reflns_av_R_equivalents 0.1676 _diffrn_reflns_av_sigmaI/netI 0.2901 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.19 _reflns_number_total 13863 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-RED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON03 (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.1513P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13863 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2556 _refine_ls_R_factor_gt 0.1092 _refine_ls_wR_factor_ref 0.3246 _refine_ls_wR_factor_gt 0.2626 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.854 _refine_ls_shift/su_max 0.003 _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 C1 C 0.6169(9) 0.1774(8) 0.4781(5) 0.050(4) Uani 1 1 d . . . C2 C 0.5869(9) 0.1104(8) 0.4558(6) 0.053(5) Uani 1 1 d . . . C3 C 0.5110(10) 0.7305(8) 0.2747(6) 0.062(5) Uani 1 1 d . . . C4 C 0.4733(8) 0.1882(8) 0.3883(6) 0.062(5) Uani 1 1 d . . . H4 H 0.4661 0.1431 0.3905 0.074 Uiso 1 1 calc R . . C5 C 0.4635(8) 0.2143(8) 0.3481(6) 0.063(5) Uani 1 1 d . . . H5 H 0.4527 0.1868 0.3241 0.075 Uiso 1 1 calc R . . C6 C 0.4700(7) 0.2824(8) 0.3442(5) 0.048(4) Uani 1 1 d . . . C7 C 0.4883(8) 0.3193(8) 0.3817(6) 0.057(5) Uani 1 1 d . . . H7 H 0.4922 0.3653 0.3802 0.068 Uiso 1 1 calc R . . C8 C 0.5006(9) 0.2896(8) 0.4206(6) 0.064(5) Uani 1 1 d . . . H8 H 0.5149 0.3152 0.4454 0.076 Uiso 1 1 calc R . . C9 C 0.4554(7) 0.3129(7) 0.3012(5) 0.044(4) Uani 1 1 d . . . C10 C 0.4260(7) 0.3045(7) 0.2285(5) 0.043(4) Uani 1 1 d . . . C11 C 0.4368(6) 0.4074(6) 0.2602(5) 0.036(4) Uani 1 1 d . . . C12 C 0.4295(6) 0.4809(8) 0.2566(5) 0.045(4) Uani 1 1 d . . . C13 C 0.4327(8) 0.5188(8) 0.2926(6) 0.062(5) Uani 1 1 d . . . H13 H 0.4412 0.4987 0.3193 0.075 Uiso 1 1 calc R . . C14 C 0.4229(8) 0.5863(9) 0.2878(6) 0.059(5) Uani 1 1 d . . . H14 H 0.4249 0.6115 0.3117 0.071 Uiso 1 1 calc R . . C15 C 0.4159(8) 0.5118(8) 0.2178(7) 0.065(5) Uani 1 1 d . . . H15 H 0.4111 0.4869 0.1932 0.078 Uiso 1 1 calc R . . C16 C 0.4093(8) 0.5802(8) 0.2154(6) 0.060(5) Uani 1 1 d . . . H16 H 0.4037 0.6017 0.1894 0.072 Uiso 1 1 calc R . . C17 C 0.6454(8) 0.2505(8) 0.3834(5) 0.057(5) Uani 1 1 d . . . H17 H 0.6686 0.2693 0.4091 0.068 Uiso 1 1 calc R . . C18 C 0.6252(8) 0.2906(8) 0.3487(6) 0.061(5) Uani 1 1 d . . . H18 H 0.6348 0.3356 0.3513 0.073 Uiso 1 1 calc R . . C19 C 0.5904(7) 0.2658(7) 0.3093(5) 0.042(4) Uani 1 1 d . . . C20 C 0.5767(6) 0.1965(7) 0.3088(5) 0.044(4) Uani 1 1 d . . . H20 H 0.5534 0.1765 0.2837 0.053 Uiso 1 1 calc R . . C21 C 0.5979(7) 0.1598(8) 0.3452(6) 0.051(4) Uani 1 1 d . . . H21 H 0.5874 0.1151 0.3445 0.061 Uiso 1 1 calc R . . C22 C 0.4937(9) 0.1407(10) 0.5411(6) 0.072(6) Uani 1 1 d . . . C23 C 0.4462(10) 0.1275(10) 0.5043(7) 0.075(6) Uani 1 1 d . . . C24 C 0.4227(8) 0.1888(9) 0.4852(6) 0.059(5) Uani 1 1 d . . . C25 C 0.4569(9) 0.2386(9) 0.5109(6) 0.064(5) Uani 1 1 d . . . C26 C 0.5000(9) 0.2117(10) 0.5446(7) 0.073(6) Uani 1 1 d . . . C27 C 0.5308(12) 0.0890(13) 0.5707(7) 0.111(9) Uani 1 1 d . . . H27A H 0.5690 0.1054 0.5823 0.166 Uiso 1 1 calc R . . H27B H 0.5302 0.0486 0.5550 0.166 Uiso 1 1 calc R . . H27C H 0.5168 0.0800 0.5937 0.166 Uiso 1 1 calc R . . C28 C 0.4251(11) 0.0608(12) 0.4880(8) 0.105(8) Uani 1 1 d . . . H28A H 0.4323 0.0525 0.4619 0.158 Uiso 1 1 calc R . . H28B H 0.3849 0.0587 0.4825 0.158 Uiso 1 1 calc R . . H28C H 0.4440 0.0278 0.5089 0.158 Uiso 1 1 calc R . . C29 C 0.3692(9) 0.1964(11) 0.4442(8) 0.090(7) Uani 1 1 d . . . H29A H 0.3583 0.1534 0.4311 0.136 Uiso 1 1 calc R . . H29B H 0.3775 0.2258 0.4244 0.136 Uiso 1 1 calc R . . H29C H 0.3386 0.2145 0.4519 0.136 Uiso 1 1 calc R . . C30 C 0.4469(10) 0.3132(11) 0.5040(8) 0.096(7) Uani 1 1 d . . . H30A H 0.4827 0.3358 0.5112 0.145 Uiso 1 1 calc R . . H30B H 0.4269 0.3294 0.5221 0.145 Uiso 1 1 calc R . . H30C H 0.4248 0.3217 0.4746 0.145 Uiso 1 1 calc R . . C31 C 0.5465(10) 0.2471(11) 0.5785(7) 0.093(7) Uani 1 1 d . . . H31A H 0.5335 0.2598 0.6014 0.139 Uiso 1 1 calc R . . H31B H 0.5573 0.2863 0.5665 0.139 Uiso 1 1 calc R . . H31C H 0.5787 0.2180 0.5894 0.139 Uiso 1 1 calc R . . C32 C 0.7286(8) 0.0414(9) 0.4145(7) 0.071(6) Uani 1 1 d . . . C33 C 0.7418(8) 0.0999(11) 0.3970(7) 0.074(6) Uani 1 1 d . . . C34 C 0.7705(8) 0.1470(10) 0.4315(6) 0.068(6) Uani 1 1 d . . . C35 C 0.7747(8) 0.1121(10) 0.4709(7) 0.069(5) Uani 1 1 d . . . C36 C 0.7481(9) 0.0487(9) 0.4623(6) 0.066(6) Uani 1 1 d . . . C37 C 0.7015(10) -0.0189(11) 0.3898(8) 0.105(9) Uani 1 1 d . . . H37A H 0.6977 -0.0132 0.3603 0.157 Uiso 1 1 calc R . . H37B H 0.6647 -0.0252 0.3921 0.157 Uiso 1 1 calc R . . H37C H 0.7247 -0.0573 0.4012 0.157 Uiso 1 1 calc R . . C38 C 0.7307(9) 0.1153(13) 0.3500(6) 0.091(7) Uani 1 1 d . . . H38A H 0.7019 0.0858 0.3324 0.137 Uiso 1 1 calc R . . H38B H 0.7650 0.1092 0.3438 0.137 Uiso 1 1 calc R . . H38C H 0.7181 0.1607 0.3441 0.137 Uiso 1 1 calc R . . C39 C 0.7927(9) 0.2124(10) 0.4254(8) 0.082(6) Uani 1 1 d . . . H39A H 0.7922 0.2419 0.4481 0.124 Uiso 1 1 calc R . . H39B H 0.7695 0.2306 0.3983 0.124 Uiso 1 1 calc R . . H39C H 0.8310 0.2075 0.4258 0.124 Uiso 1 1 calc R . . C40 C 0.8026(9) 0.1423(10) 0.5141(6) 0.078(6) Uani 1 1 d . . . H40A H 0.7873 0.1861 0.5148 0.117 Uiso 1 1 calc R . . H40B H 0.8427 0.1454 0.5201 0.117 Uiso 1 1 calc R . . H40C H 0.7955 0.1148 0.5354 0.117 Uiso 1 1 calc R . . C41 C 0.7435(12) -0.0038(11) 0.4935(8) 0.110(9) Uani 1 1 d . . . H41A H 0.7730 -0.0363 0.4976 0.165 Uiso 1 1 calc R . . H41B H 0.7071 -0.0254 0.4822 0.165 Uiso 1 1 calc R . . H41C H 0.7472 0.0168 0.5204 0.165 Uiso 1 1 calc R . . C42 C 0.3026(8) 0.7000(9) 0.2392(6) 0.062(5) Uani 1 1 d . . . C43 C 0.3027(9) 0.7320(13) 0.2029(7) 0.086(7) Uani 1 1 d . . . C44 C 0.3297(11) 0.7982(10) 0.2167(9) 0.085(7) Uani 1 1 d . . . C45 C 0.3456(9) 0.7998(8) 0.2621(9) 0.076(6) Uani 1 1 d . . . C46 C 0.3283(9) 0.7381(9) 0.2736(7) 0.066(5) Uani 1 1 d . . . C47 C 0.2772(10) 0.6303(11) 0.2407(10) 0.111(9) Uani 1 1 d . . . H47A H 0.3007 0.6068 0.2656 0.167 Uiso 1 1 calc R . . H47B H 0.2755 0.6057 0.2154 0.167 Uiso 1 1 calc R . . H47C H 0.2397 0.6349 0.2418 0.167 Uiso 1 1 calc R . . C48 C 0.2810(13) 0.714(2) 0.1552(9) 0.172(17) Uani 1 1 d . . . H48A H 0.2785 0.6662 0.1521 0.258 Uiso 1 1 calc R . . H48B H 0.3068 0.7309 0.1420 0.258 Uiso 1 1 calc R . . H48C H 0.2442 0.7332 0.1416 0.258 Uiso 1 1 calc R . . C49 C 0.3388(12) 0.8510(15) 0.1879(13) 0.18(2) Uani 1 1 d . . . H49A H 0.3027 0.8653 0.1682 0.274 Uiso 1 1 calc R . . H49B H 0.3614 0.8334 0.1722 0.274 Uiso 1 1 calc R . . H49C H 0.3580 0.8884 0.2049 0.274 Uiso 1 1 calc R . . C50 C 0.3773(10) 0.8555(11) 0.2945(9) 0.104(9) Uani 1 1 d . . . H50A H 0.3530 0.8723 0.3090 0.156 Uiso 1 1 calc R . . H50B H 0.3875 0.8913 0.2792 0.156 Uiso 1 1 calc R . . H50C H 0.4111 0.8372 0.3151 0.156 Uiso 1 1 calc R . . C51 C 0.3355(11) 0.7206(12) 0.3216(8) 0.097(7) Uani 1 1 d . . . H51A H 0.3084 0.7455 0.3301 0.145 Uiso 1 1 calc R . . H51B H 0.3732 0.7320 0.3400 0.145 Uiso 1 1 calc R . . H51C H 0.3293 0.6737 0.3239 0.145 Uiso 1 1 calc R . . C55 C 0.2847(7) 0.4070(10) 0.2520(10) 0.114(10) Uani 1 1 d G . . H55 H 0.2724 0.4477 0.2385 0.136 Uiso 1 1 calc R . . C56 C 0.3011(8) 0.4024(12) 0.2964(10) 0.120(10) Uani 1 1 d G . . H56 H 0.2998 0.4399 0.3125 0.144 Uiso 1 1 calc R . . C57 C 0.3195(7) 0.3416(16) 0.3166(6) 0.131(12) Uani 1 1 d G . . H57 H 0.3305 0.3385 0.3463 0.157 Uiso 1 1 calc R . . C58 C 0.3215(7) 0.2855(10) 0.2925(10) 0.140(15) Uani 1 1 d G . . H58 H 0.3338 0.2449 0.3060 0.168 Uiso 1 1 calc R . . C59 C 0.3050(7) 0.2902(11) 0.2481(9) 0.113(10) Uani 1 1 d G . . H59 H 0.3063 0.2527 0.2320 0.136 Uiso 1 1 calc R . . C60 C 0.2866(7) 0.3509(16) 0.2279(6) 0.141(15) Uani 1 1 d G . . H60 H 0.2756 0.3541 0.1982 0.170 Uiso 1 1 calc R . . C61 C 0.405(2) 0.4759(14) 0.1022(13) 0.261(7) Uiso 1 1 d G . . H61 H 0.4075 0.4296 0.1035 0.313 Uiso 1 1 calc R . . C62 C 0.3537(17) 0.507(2) 0.0985(13) 0.261(7) Uiso 1 1 d G . . H62 H 0.3222 0.4812 0.0973 0.313 Uiso 1 1 calc R . . C63 C 0.3496(15) 0.576(2) 0.0966(13) 0.261(7) Uiso 1 1 d G . . H63 H 0.3154 0.5967 0.0941 0.313 Uiso 1 1 calc R . . C64 C 0.397(2) 0.6143(14) 0.0983(12) 0.261(7) Uiso 1 1 d G . . H64 H 0.3938 0.6606 0.0971 0.313 Uiso 1 1 calc R . . C65 C 0.4476(17) 0.583(2) 0.1021(12) 0.261(7) Uiso 1 1 d G . . H65 H 0.4791 0.6090 0.1033 0.313 Uiso 1 1 calc R . . C66 C 0.4517(15) 0.514(2) 0.1040(13) 0.261(7) Uiso 1 1 d G . . H66 H 0.4859 0.4935 0.1065 0.313 Uiso 1 1 calc R . . C67 C 0.4544(14) 0.163(3) 0.6389(11) 0.261(7) Uiso 1 1 d G . . H67 H 0.4839 0.1711 0.6644 0.313 Uiso 1 1 calc R . . C68 C 0.4435(17) 0.098(2) 0.6236(15) 0.261(7) Uiso 1 1 d G . . H68 H 0.4656 0.0626 0.6389 0.313 Uiso 1 1 calc R . . C69 C 0.399(2) 0.0849(16) 0.5854(16) 0.261(7) Uiso 1 1 d G . . H69 H 0.3921 0.0414 0.5752 0.313 Uiso 1 1 calc R . . C70 C 0.3663(14) 0.137(3) 0.5625(10) 0.261(7) Uiso 1 1 d G . . H70 H 0.3368 0.1287 0.5369 0.313 Uiso 1 1 calc R . . C71 C 0.3773(17) 0.202(2) 0.5778(15) 0.261(7) Uiso 1 1 d G . . H71 H 0.3551 0.2372 0.5624 0.313 Uiso 1 1 calc R . . C72 C 0.421(2) 0.2149(17) 0.6159(16) 0.261(7) Uiso 1 1 d G . . H72 H 0.4287 0.2584 0.6262 0.313 Uiso 1 1 calc R . . N1 N 0.4924(6) 0.2235(7) 0.4238(5) 0.058(4) Uani 1 1 d . . . N2 N 0.4442(6) 0.2737(6) 0.2662(5) 0.050(3) Uani 1 1 d . . . N3 N 0.4239(6) 0.3730(7) 0.2243(4) 0.051(3) Uani 1 1 d . . . N4 N 0.4512(6) 0.3816(6) 0.2999(4) 0.051(3) Uani 1 1 d . . . N5 N 0.4109(6) 0.6169(6) 0.2505(5) 0.055(4) Uani 1 1 d . . . N6 N 0.6337(6) 0.1854(6) 0.3828(5) 0.053(4) Uani 1 1 d . . . O1 O 0.5915(5) 0.2114(5) 0.4970(4) 0.057(3) Uani 1 1 d . . . O2 O 0.5404(6) 0.0981(5) 0.4603(4) 0.062(3) Uani 1 1 d . . . O3 O 0.6641(5) 0.1905(5) 0.4745(4) 0.055(3) Uani 1 1 d . . . O4 O 0.6122(5) 0.0781(5) 0.4364(4) 0.055(3) Uani 1 1 d . . . O5 O 0.4701(5) 0.7320(5) 0.2907(4) 0.056(3) Uani 1 1 d . . . O6 O 0.4386(5) 0.7277(6) 0.2040(4) 0.057(3) Uani 1 1 d . . . Rh1 Rh 0.50637(7) 0.18033(6) 0.48494(5) 0.0551(4) Uani 1 1 d . . . Rh2 Rh 0.68663(7) 0.12404(7) 0.43222(5) 0.0551(4) Uani 1 1 d . . . Rh3 Rh 0.38759(6) 0.71859(6) 0.24368(5) 0.0546(4) Uani 1 1 d . . . S1 S 0.2058(2) 0.4027(2) 0.0954(2) 0.0911(18) Uiso 1 1 d G . . O7 O 0.1831(5) 0.3656(4) 0.1229(3) 0.153(8) Uiso 1 1 d G . . O8 O 0.1683(4) 0.4106(4) 0.0521(2) 0.107(5) Uiso 1 1 d G . . O9 O 0.2635(3) 0.3858(4) 0.1006(4) 0.116(6) Uiso 1 1 d G . . C52 C 0.2119(4) 0.4873(3) 0.1168(3) 0.261(7) Uiso 1 1 d G . . F1 F 0.1614(5) 0.5110(5) 0.1151(5) 0.226(10) Uiso 1 1 d G . . F2 F 0.2327(6) 0.5287(3) 0.0949(4) 0.178(8) Uiso 1 1 d G . . F3 F 0.2457(6) 0.4897(5) 0.1576(3) 0.182(8) Uiso 1 1 d G . . S2 S 0.8823(4) 0.0101(5) 0.3962(3) 0.189(5) Uiso 1 1 d G . . O10 O 0.8270(5) -0.0111(8) 0.3948(5) 0.231(13) Uiso 1 1 d G . . O11 O 0.8838(7) 0.0715(6) 0.3745(4) 0.157(8) Uiso 1 1 d G . . O12 O 0.9169(6) -0.0429(6) 0.3891(5) 0.143(7) Uiso 1 1 d G . . C53 C 0.9181(6) 0.0312(8) 0.4524(3) 0.261(7) Uiso 1 1 d G . . F4 F 0.8908(9) 0.0799(9) 0.4649(5) 0.226(10) Uiso 1 1 d G . . F5 F 0.9706(6) 0.0520(11) 0.4595(5) 0.47(3) Uiso 1 1 d G . . F6 F 0.9207(10) -0.0208(10) 0.4779(4) 0.35(2) Uiso 1 1 d G . . S3 S 0.5888(8) 0.0568(9) 0.2358(5) 0.316(10) Uiso 1 1 d G . . O13 O 0.5341(8) 0.0853(11) 0.2132(8) 0.223(13) Uiso 1 1 d G . . O14 O 0.5879(13) -0.0085(12) 0.2532(8) 0.68(8) Uiso 1 1 d G . . O15 O 0.6284(10) 0.1031(15) 0.2637(7) 0.59(6) Uiso 1 1 d G . . C54 C 0.6185(7) 0.0419(8) 0.1937(5) 0.261(7) Uiso 1 1 d G . . F7 F 0.5861(10) 0.0000(12) 0.1640(7) 0.292(15) Uiso 1 1 d G . . F8 F 0.6698(8) 0.0153(12) 0.2093(8) 0.265(13) Uiso 1 1 d G . . F9 F 0.6226(11) 0.0980(11) 0.1736(8) 0.336(19) Uiso 1 1 d G . . 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 C1 0.066(13) 0.051(10) 0.023(9) 0.003(7) 0.001(9) 0.011(9) C2 0.066(13) 0.049(10) 0.034(10) 0.011(8) 0.006(10) -0.004(10) C3 0.090(16) 0.043(9) 0.065(13) -0.007(8) 0.042(14) 0.005(10) C4 0.082(14) 0.044(9) 0.049(12) -0.011(8) 0.009(10) -0.023(9) C5 0.092(15) 0.048(9) 0.044(11) 0.001(8) 0.018(10) -0.002(10) C6 0.057(11) 0.045(9) 0.050(11) 0.005(8) 0.028(9) 0.013(8) C7 0.082(13) 0.032(8) 0.058(12) 0.000(8) 0.026(10) 0.001(8) C8 0.114(17) 0.039(9) 0.045(11) -0.009(8) 0.037(11) -0.005(10) C9 0.047(10) 0.047(9) 0.037(9) 0.003(7) 0.013(8) 0.003(8) C10 0.045(10) 0.047(9) 0.042(10) 0.004(7) 0.022(8) -0.003(7) C11 0.025(8) 0.029(7) 0.052(11) 0.011(7) 0.012(8) 0.002(6) C12 0.033(9) 0.055(9) 0.046(10) 0.002(8) 0.012(8) 0.001(7) C13 0.081(14) 0.042(9) 0.068(13) 0.009(9) 0.030(11) 0.017(9) C14 0.063(12) 0.063(11) 0.050(12) 0.003(9) 0.017(10) -0.013(9) C15 0.081(14) 0.048(10) 0.065(13) 0.007(9) 0.025(11) -0.004(9) C16 0.074(13) 0.052(10) 0.057(13) 0.014(9) 0.025(11) 0.019(9) C17 0.077(13) 0.053(10) 0.032(10) -0.008(8) 0.010(9) -0.003(9) C18 0.083(14) 0.032(8) 0.067(13) -0.007(8) 0.027(11) -0.010(9) C19 0.044(10) 0.038(8) 0.046(10) 0.001(7) 0.017(8) -0.005(7) C20 0.032(9) 0.047(9) 0.051(11) -0.002(7) 0.010(8) 0.006(7) C21 0.057(11) 0.045(9) 0.049(11) 0.003(8) 0.016(9) 0.007(8) C22 0.065(13) 0.089(15) 0.048(12) 0.000(10) 0.002(11) 0.010(11) C23 0.100(17) 0.072(13) 0.064(14) 0.000(11) 0.041(13) 0.007(13) C24 0.069(13) 0.058(10) 0.049(11) -0.004(9) 0.020(10) 0.010(10) C25 0.076(14) 0.057(11) 0.055(13) 0.005(9) 0.020(11) 0.024(10) C26 0.076(15) 0.077(13) 0.061(14) -0.015(11) 0.016(12) -0.010(11) C27 0.12(2) 0.15(2) 0.049(15) 0.018(14) 0.014(15) 0.014(18) C28 0.11(2) 0.102(18) 0.09(2) -0.010(14) 0.015(16) 0.011(15) C29 0.082(16) 0.103(17) 0.083(17) 0.000(13) 0.025(14) 0.022(13) C30 0.089(17) 0.115(18) 0.073(16) 0.010(13) 0.012(13) 0.027(14) C31 0.104(19) 0.106(17) 0.076(17) -0.024(13) 0.039(15) 0.005(14) C32 0.053(12) 0.067(12) 0.087(16) 0.009(11) 0.019(12) 0.033(10) C33 0.052(12) 0.097(15) 0.060(14) 0.010(12) 0.002(11) 0.017(11) C34 0.060(13) 0.079(13) 0.051(13) -0.007(10) 0.000(10) 0.025(10) C35 0.059(12) 0.080(13) 0.060(14) -0.016(11) 0.011(11) 0.017(10) C36 0.095(15) 0.063(11) 0.030(10) 0.002(8) 0.007(10) 0.031(11) C37 0.103(19) 0.092(16) 0.089(18) -0.049(14) -0.006(15) 0.029(14) C38 0.070(14) 0.17(2) 0.044(12) -0.002(13) 0.027(11) -0.007(15) C39 0.069(14) 0.073(13) 0.101(18) 0.005(12) 0.025(13) -0.005(11) C40 0.087(15) 0.083(13) 0.047(12) 0.011(10) 0.001(11) 0.023(11) C41 0.16(2) 0.076(14) 0.089(19) 0.010(13) 0.037(18) 0.046(16) C42 0.072(14) 0.073(12) 0.049(12) -0.023(10) 0.030(11) -0.015(10) C43 0.072(15) 0.114(18) 0.065(15) -0.007(13) 0.013(12) 0.044(14) C44 0.113(19) 0.072(14) 0.094(19) 0.021(12) 0.065(16) 0.039(13) C45 0.086(16) 0.037(10) 0.11(2) 0.003(10) 0.046(15) 0.014(9) C46 0.072(14) 0.064(12) 0.071(15) 0.016(10) 0.035(12) 0.025(10) C47 0.065(15) 0.098(17) 0.18(3) -0.034(17) 0.048(17) -0.034(13) C48 0.12(2) 0.29(4) 0.08(2) -0.06(2) -0.005(17) 0.11(3) C49 0.12(2) 0.15(3) 0.32(5) 0.19(3) 0.13(3) 0.09(2) C50 0.090(17) 0.081(15) 0.15(3) -0.043(15) 0.058(18) -0.018(13) C51 0.11(2) 0.096(16) 0.094(19) -0.003(14) 0.051(16) 0.008(15) C55 0.08(2) 0.12(2) 0.14(3) 0.00(2) 0.04(2) -0.021(17) C56 0.08(2) 0.13(3) 0.15(3) -0.01(2) 0.04(2) -0.025(18) C57 0.064(18) 0.20(3) 0.11(2) 0.04(3) -0.001(16) -0.01(2) C58 0.057(16) 0.088(19) 0.26(5) 0.05(2) 0.03(3) -0.019(15) C59 0.064(17) 0.14(3) 0.12(3) 0.00(2) 0.020(18) -0.024(17) C60 0.032(13) 0.23(4) 0.16(3) 0.09(3) 0.023(16) 0.030(19) N1 0.066(10) 0.058(9) 0.043(9) 0.003(7) 0.008(8) 0.012(8) N2 0.053(9) 0.041(7) 0.055(10) -0.010(7) 0.016(7) 0.002(7) N3 0.055(9) 0.052(8) 0.046(9) 0.005(7) 0.016(7) 0.004(7) N4 0.055(9) 0.045(7) 0.052(9) -0.001(7) 0.017(7) 0.010(7) N5 0.063(10) 0.042(7) 0.067(11) 0.005(8) 0.031(8) 0.005(7) N6 0.064(9) 0.034(7) 0.055(9) -0.007(6) 0.014(8) -0.009(7) O1 0.068(8) 0.054(6) 0.045(7) -0.016(6) 0.015(6) 0.000(6) O2 0.090(10) 0.052(7) 0.037(7) 0.007(5) 0.014(7) 0.009(7) O3 0.055(8) 0.063(7) 0.041(7) -0.007(5) 0.010(6) 0.004(6) O4 0.075(9) 0.040(6) 0.052(8) -0.009(5) 0.024(7) -0.004(6) O5 0.058(8) 0.049(6) 0.064(8) 0.001(6) 0.023(7) 0.004(6) O6 0.042(7) 0.062(7) 0.063(8) 0.008(6) 0.014(7) 0.002(6) Rh1 0.0689(10) 0.0513(8) 0.0412(8) 0.0009(6) 0.0138(7) 0.0074(7) Rh2 0.0695(10) 0.0526(7) 0.0398(8) -0.0031(6) 0.0143(7) 0.0067(7) Rh3 0.0613(9) 0.0439(7) 0.0617(10) 0.0053(7) 0.0251(8) 0.0007(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 C1 O1 1.24(2) . ? C1 O3 1.26(2) . ? C1 C2 1.59(2) . ? C2 O4 1.23(2) . ? C2 O2 1.25(2) . ? C3 O6 1.22(2) 2_655 ? C3 O5 1.31(2) . ? C3 C3 1.54(4) 2_655 ? C4 N1 1.32(2) . ? C4 C5 1.37(2) . ? C4 H4 0.9300 . ? C5 C6 1.38(2) . ? C5 H5 0.9300 . ? C6 C7 1.38(2) . ? C6 C9 1.48(2) . ? C7 C8 1.36(2) . ? C7 H7 0.9300 . ? C8 N1 1.35(2) . ? C8 H8 0.9300 . ? C9 N2 1.35(2) . ? C9 N4 1.378(19) . ? C10 N2 1.33(2) . ? C10 N3 1.379(19) . ? C10 C19 1.41(2) 2_655 ? C11 N3 1.32(2) . ? C11 N4 1.343(19) . ? C11 C12 1.48(2) . ? C12 C15 1.36(2) . ? C12 C13 1.40(2) . ? C13 C14 1.37(2) . ? C13 H13 0.9300 . ? C14 N5 1.32(2) . ? C14 H14 0.9300 . ? C15 C16 1.38(2) . ? C15 H15 0.9300 . ? C16 N5 1.37(2) . ? C16 H16 0.9300 . ? C17 N6 1.337(19) . ? C17 C18 1.35(2) . ? C17 H17 0.9300 . ? C18 C19 1.39(2) . ? C18 H18 0.9300 . ? C19 C10 1.41(2) 2_655 ? C19 C20 1.43(2) . ? C20 C21 1.36(2) . ? C20 H20 0.9300 . ? C21 N6 1.36(2) . ? C21 H21 0.9300 . ? C22 C23 1.41(3) . ? C22 C26 1.43(3) . ? C22 C27 1.51(3) . ? C22 Rh1 2.15(2) . ? C23 C24 1.41(3) . ? C23 C28 1.47(3) . ? C23 Rh1 2.11(2) . ? C24 C25 1.40(3) . ? C24 C29 1.56(3) . ? C24 Rh1 2.108(19) . ? C25 C26 1.37(3) . ? C25 C30 1.52(3) . ? C25 Rh1 2.092(18) . ? C26 C31 1.49(3) . ? C26 Rh1 2.14(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.40(3) . ? C32 C37 1.49(3) . ? C32 C36 1.50(3) . ? C32 Rh2 2.149(17) . ? C33 C34 1.47(3) . ? C33 C38 1.52(3) . ? C33 Rh2 2.15(2) . ? C34 C35 1.45(3) . ? C34 C39 1.46(3) . ? C34 Rh2 2.16(2) . ? C35 C36 1.42(3) . ? C35 C40 1.49(3) . ? C35 Rh2 2.154(19) . ? C36 C41 1.51(3) . ? C36 Rh2 2.143(17) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C46 1.34(3) . ? C42 C43 1.37(3) . ? C42 C47 1.54(3) . ? C42 Rh3 2.119(19) . ? C43 C44 1.49(3) . ? C43 C48 1.53(3) . ? C43 Rh3 2.11(2) . ? C44 C45 1.42(3) . ? C44 C49 1.49(3) . ? C44 Rh3 2.13(2) . ? C45 C46 1.40(2) . ? C45 C50 1.56(3) . ? C45 Rh3 2.139(18) . ? C46 C51 1.58(3) . ? C46 Rh3 2.090(19) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C55 H55 0.9300 . ? C56 C57 1.3900 . ? C56 H56 0.9300 . ? C57 C58 1.3900 . ? C57 H57 0.9300 . ? C58 C59 1.3900 . ? C58 H58 0.9300 . ? C59 C60 1.3900 . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 H61 0.9300 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 C65 1.3900 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C67 H67 0.9300 . ? C68 C69 1.3900 . ? C68 H68 0.9300 . ? C69 C70 1.3900 . ? C69 H69 0.9300 . ? C70 C71 1.3900 . ? C70 H70 0.9300 . ? C71 C72 1.3900 . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? N1 Rh1 2.124(14) . ? N5 Rh3 2.110(13) . ? N6 Rh2 2.114(14) . ? O1 Rh1 2.127(12) . ? O2 Rh1 2.143(12) . ? O3 Rh2 2.147(11) . ? O4 Rh2 2.129(12) . ? O5 Rh3 2.139(12) . ? O6 C3 1.22(2) 2_655 ? O6 Rh3 2.136(12) . ? S1 O8 1.4319 . ? S1 O7 1.4366 . ? S1 O9 1.4398 . ? S1 C52 1.8236 . ? C52 F2 1.3225 . ? C52 F3 1.3301 . ? C52 F1 1.3359 . ? S2 O11 1.4318 . ? S2 O10 1.4366 . ? S2 O12 1.4398 . ? S2 C53 1.8236 . ? C53 F5 1.3225 . ? C53 F6 1.3301 . ? C53 F4 1.3359 . ? S3 O14 1.4318 . ? S3 O13 1.4366 . ? S3 O15 1.4398 . ? S3 C54 1.8237 . ? C54 F8 1.3225 . ? C54 F9 1.3301 . ? C54 F7 1.3359 . ? 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 O1 C1 O3 126.7(16) . . ? O1 C1 C2 117.0(18) . . ? O3 C1 C2 116.3(17) . . ? O4 C2 O2 128.9(16) . . ? O4 C2 C1 116.1(18) . . ? O2 C2 C1 115.0(18) . . ? O6 C3 O5 124.6(18) 2_655 . ? O6 C3 C3 122(2) 2_655 2_655 ? O5 C3 C3 113(3) . 2_655 ? N1 C4 C5 123.7(16) . . ? N1 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C6 118.4(16) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C7 C6 C5 117.2(15) . . ? C7 C6 C9 122.9(14) . . ? C5 C6 C9 119.9(15) . . ? C8 C7 C6 121.3(15) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N1 C8 C7 120.7(16) . . ? N1 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? N2 C9 N4 124.1(14) . . ? N2 C9 C6 120.0(14) . . ? N4 C9 C6 115.8(13) . . ? N2 C10 N3 123.2(14) . . ? N2 C10 C19 118.9(13) . 2_655 ? N3 C10 C19 117.9(14) . 2_655 ? N3 C11 N4 125.8(13) . . ? N3 C11 C12 117.4(14) . . ? N4 C11 C12 116.5(14) . . ? C15 C12 C13 119.1(16) . . ? C15 C12 C11 120.7(16) . . ? C13 C12 C11 120.1(15) . . ? C14 C13 C12 118.6(17) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? N5 C14 C13 122.7(18) . . ? N5 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C12 C15 C16 119.5(18) . . ? C12 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N5 C16 C15 121.0(17) . . ? N5 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? N6 C17 C18 123.4(16) . . ? N6 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C17 C18 C19 121.4(15) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C10 122.6(14) . 2_655 ? C18 C19 C20 115.2(14) . . ? C10 C19 C20 121.9(15) 2_655 . ? C21 C20 C19 119.9(15) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 N6 123.1(15) . . ? C20 C21 H21 118.5 . . ? N6 C21 H21 118.5 . . ? C23 C22 C26 107.2(18) . . ? C23 C22 C27 126(2) . . ? C26 C22 C27 127(2) . . ? C23 C22 Rh1 69.4(12) . . ? C26 C22 Rh1 70.1(12) . . ? C27 C22 Rh1 125.3(16) . . ? C22 C23 C24 108.9(18) . . ? C22 C23 C28 126(2) . . ? C24 C23 C28 125(2) . . ? C22 C23 Rh1 72.0(13) . . ? C24 C23 Rh1 70.2(12) . . ? C28 C23 Rh1 123.2(16) . . ? C25 C24 C23 105.8(17) . . ? C25 C24 C29 128.9(17) . . ? C23 C24 C29 125.4(18) . . ? C25 C24 Rh1 70.0(11) . . ? C23 C24 Rh1 70.7(12) . . ? C29 C24 Rh1 124.5(14) . . ? C26 C25 C24 111.3(16) . . ? C26 C25 C30 123.5(19) . . ? C24 C25 C30 125.2(18) . . ? C26 C25 Rh1 72.8(11) . . ? C24 C25 Rh1 71.1(11) . . ? C30 C25 Rh1 125.4(15) . . ? C25 C26 C22 106.7(17) . . ? C25 C26 C31 128(2) . . ? C22 C26 C31 125(2) . . ? C25 C26 Rh1 69.3(12) . . ? C22 C26 Rh1 70.9(12) . . ? C31 C26 Rh1 123.5(15) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 126(2) . . ? C33 C32 C36 108.7(18) . . ? C37 C32 C36 126(2) . . ? C33 C32 Rh2 71.2(11) . . ? C37 C32 Rh2 127.1(14) . . ? C36 C32 Rh2 69.4(10) . . ? C32 C33 C34 110(2) . . ? C32 C33 C38 128(2) . . ? C34 C33 C38 123(2) . . ? C32 C33 Rh2 70.9(12) . . ? C34 C33 Rh2 70.4(12) . . ? C38 C33 Rh2 126.0(14) . . ? C35 C34 C39 129.9(19) . . ? C35 C34 C33 105.0(18) . . ? C39 C34 C33 125(2) . . ? C35 C34 Rh2 70.0(12) . . ? C39 C34 Rh2 127.6(13) . . ? C33 C34 Rh2 69.8(12) . . ? C36 C35 C34 111.6(17) . . ? C36 C35 C40 126.0(19) . . ? C34 C35 C40 122.4(19) . . ? C36 C35 Rh2 70.4(11) . . ? C34 C35 Rh2 70.6(11) . . ? C40 C35 Rh2 124.9(13) . . ? C35 C36 C32 105.1(17) . . ? C35 C36 C41 129.1(19) . . ? C32 C36 C41 125.7(19) . . ? C35 C36 Rh2 71.2(10) . . ? C32 C36 Rh2 69.7(9) . . ? C41 C36 Rh2 126.7(16) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C46 C42 C43 109.8(19) . . ? C46 C42 C47 125(2) . . ? C43 C42 C47 125(2) . . ? C46 C42 Rh3 70.2(12) . . ? C43 C42 Rh3 70.8(12) . . ? C47 C42 Rh3 124.9(14) . . ? C42 C43 C44 106.6(19) . . ? C42 C43 C48 134(3) . . ? C44 C43 C48 119(3) . . ? C42 C43 Rh3 71.5(13) . . ? C44 C43 Rh3 70.3(13) . . ? C48 C43 Rh3 123.7(16) . . ? C45 C44 C43 106.1(18) . . ? C45 C44 C49 128(3) . . ? C43 C44 C49 126(3) . . ? C45 C44 Rh3 70.7(12) . . ? C43 C44 Rh3 68.6(11) . . ? C49 C44 Rh3 124.6(16) . . ? C46 C45 C44 105.5(19) . . ? C46 C45 C50 125(2) . . ? C44 C45 C50 130(2) . . ? C46 C45 Rh3 68.7(10) . . ? C44 C45 Rh3 70.4(11) . . ? C50 C45 Rh3 123.7(15) . . ? C42 C46 C45 111.9(19) . . ? C42 C46 C51 126.0(19) . . ? C45 C46 C51 122(2) . . ? C42 C46 Rh3 72.6(12) . . ? C45 C46 Rh3 72.5(11) . . ? C51 C46 Rh3 125.8(14) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C56 C55 C60 120.0 . . ? C56 C55 H55 120.0 . . ? C60 C55 H55 120.0 . . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 H61 120.0 . . ? C66 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C68 C67 C72 120.0 . . ? C68 C67 H67 120.0 . . ? C72 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C71 C70 C69 120.0 . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? C4 N1 C8 118.4(15) . . ? C4 N1 Rh1 121.9(12) . . ? C8 N1 Rh1 119.6(11) . . ? C10 N2 C9 116.4(13) . . ? C11 N3 C10 116.1(13) . . ? C11 N4 C9 114.1(13) . . ? C14 N5 C16 118.8(15) . . ? C14 N5 Rh3 120.9(12) . . ? C16 N5 Rh3 120.1(12) . . ? C17 N6 C21 116.9(14) . . ? C17 N6 Rh2 118.7(11) . . ? C21 N6 Rh2 122.2(10) . . ? C1 O1 Rh1 113.7(11) . . ? C2 O2 Rh1 113.9(12) . . ? C1 O3 Rh2 113.7(11) . . ? C2 O4 Rh2 115.4(11) . . ? C3 O5 Rh3 113.4(12) . . ? C3 O6 Rh3 111.6(12) 2_655 . ? C25 Rh1 C24 38.9(7) . . ? C25 Rh1 C23 64.5(8) . . ? C24 Rh1 C23 39.1(7) . . ? C25 Rh1 N1 103.9(6) . . ? C24 Rh1 N1 97.7(6) . . ? C23 Rh1 N1 126.5(7) . . ? C25 Rh1 O1 117.3(7) . . ? C24 Rh1 O1 155.9(6) . . ? C23 Rh1 O1 149.8(7) . . ? N1 Rh1 O1 83.4(5) . . ? C25 Rh1 C26 37.9(7) . . ? C24 Rh1 C26 65.3(8) . . ? C23 Rh1 C26 65.0(8) . . ? N1 Rh1 C26 136.7(7) . . ? O1 Rh1 C26 97.4(6) . . ? C25 Rh1 O2 163.1(7) . . ? C24 Rh1 O2 126.2(6) . . ? C23 Rh1 O2 98.7(7) . . ? N1 Rh1 O2 84.5(5) . . ? O1 Rh1 O2 77.9(5) . . ? C26 Rh1 O2 138.3(7) . . ? C25 Rh1 C22 64.1(7) . . ? C24 Rh1 C22 65.3(7) . . ? C23 Rh1 C22 38.5(7) . . ? N1 Rh1 C22 162.9(7) . . ? O1 Rh1 C22 112.5(6) . . ? C26 Rh1 C22 39.0(7) . . ? O2 Rh1 C22 104.2(6) . . ? N6 Rh2 O4 88.3(5) . . ? N6 Rh2 C36 158.5(6) . . ? O4 Rh2 C36 99.9(7) . . ? N6 Rh2 O3 84.9(5) . . ? O4 Rh2 O3 77.9(5) . . ? C36 Rh2 O3 116.1(6) . . ? N6 Rh2 C32 118.1(7) . . ? O4 Rh2 C32 102.0(6) . . ? C36 Rh2 C32 40.9(7) . . ? O3 Rh2 C32 157.0(7) . . ? N6 Rh2 C33 93.3(7) . . ? O4 Rh2 C33 133.0(7) . . ? C36 Rh2 C33 66.5(8) . . ? O3 Rh2 C33 149.1(7) . . ? C32 Rh2 C33 37.9(7) . . ? N6 Rh2 C35 140.3(7) . . ? O4 Rh2 C35 131.0(7) . . ? C36 Rh2 C35 38.5(7) . . ? O3 Rh2 C35 97.2(6) . . ? C32 Rh2 C35 65.1(7) . . ? C33 Rh2 C35 65.1(7) . . ? N6 Rh2 C34 102.8(7) . . ? O4 Rh2 C34 166.3(6) . . ? C36 Rh2 C34 66.9(8) . . ? O3 Rh2 C34 110.6(6) . . ? C32 Rh2 C34 65.9(7) . . ? C33 Rh2 C34 39.8(7) . . ? C35 Rh2 C34 39.3(7) . . ? C46 Rh3 N5 110.3(6) . . ? C46 Rh3 C43 63.6(9) . . ? N5 Rh3 C43 111.9(8) . . ? C46 Rh3 C42 37.2(7) . . ? N5 Rh3 C42 94.2(6) . . ? C43 Rh3 C42 37.7(8) . . ? C46 Rh3 C44 64.4(8) . . ? N5 Rh3 C44 152.8(9) . . ? C43 Rh3 C44 41.0(9) . . ? C42 Rh3 C44 65.1(8) . . ? C46 Rh3 O6 162.2(6) . . ? N5 Rh3 O6 86.9(5) . . ? C43 Rh3 O6 106.2(8) . . ? C42 Rh3 O6 140.6(6) . . ? C44 Rh3 O6 98.1(7) . . ? C46 Rh3 O5 107.3(7) . . ? N5 Rh3 O5 83.1(5) . . ? C43 Rh3 O5 164.2(7) . . ? C42 Rh3 O5 140.5(6) . . ? C44 Rh3 O5 124.1(8) . . ? O6 Rh3 O5 78.8(5) . . ? C46 Rh3 C45 38.8(7) . . ? N5 Rh3 C45 148.1(7) . . ? C43 Rh3 C45 66.4(9) . . ? C42 Rh3 C45 64.6(7) . . ? C44 Rh3 C45 38.9(8) . . ? O6 Rh3 C45 124.7(7) . . ? O5 Rh3 C45 98.3(7) . . ? O8 S1 O7 115.5 . . ? O8 S1 O9 115.5 . . ? O7 S1 O9 113.9 . . ? O8 S1 C52 103.1 . . ? O7 S1 C52 103.4 . . ? O9 S1 C52 103.0 . . ? F2 C52 F3 107.7 . . ? F2 C52 F1 107.5 . . ? F3 C52 F1 107.0 . . ? F2 C52 S1 111.5 . . ? F3 C52 S1 111.7 . . ? F1 C52 S1 111.3 . . ? O11 S2 O10 115.5 . . ? O11 S2 O12 115.5 . . ? O10 S2 O12 113.9 . . ? O11 S2 C53 103.1 . . ? O10 S2 C53 103.4 . . ? O12 S2 C53 103.0 . . ? F5 C53 F6 107.7 . . ? F5 C53 F4 107.5 . . ? F6 C53 F4 107.0 . . ? F5 C53 S2 111.5 . . ? F6 C53 S2 111.7 . . ? F4 C53 S2 111.3 . . ? O14 S3 O13 115.5 . . ? O14 S3 O15 115.5 . . ? O13 S3 O15 113.9 . . ? O14 S3 C54 103.1 . . ? O13 S3 C54 103.4 . . ? O15 S3 C54 103.0 . . ? F8 C54 F9 107.7 . . ? F8 C54 F7 107.5 . . ? F9 C54 F7 107.0 . . ? F8 C54 S3 111.5 . . ? F9 C54 S3 111.7 . . ? F7 C54 S3 111.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O4 178.4(14) . . . . ? O3 C1 C2 O4 -1(2) . . . . ? O1 C1 C2 O2 -1(2) . . . . ? O3 C1 C2 O2 179.2(14) . . . . ? N1 C4 C5 C6 -5(3) . . . . ? C4 C5 C6 C7 2(3) . . . . ? C4 C5 C6 C9 -175.2(17) . . . . ? C5 C6 C7 C8 2(3) . . . . ? C9 C6 C7 C8 179.1(17) . . . . ? C6 C7 C8 N1 -4(3) . . . . ? C7 C6 C9 N2 172.3(16) . . . . ? C5 C6 C9 N2 -10(2) . . . . ? C7 C6 C9 N4 -11(2) . . . . ? C5 C6 C9 N4 166.3(16) . . . . ? N3 C11 C12 C15 -7(2) . . . . ? N4 C11 C12 C15 178.9(16) . . . . ? N3 C11 C12 C13 168.7(15) . . . . ? N4 C11 C12 C13 -6(2) . . . . ? C15 C12 C13 C14 -1(3) . . . . ? C11 C12 C13 C14 -176.8(15) . . . . ? C12 C13 C14 N5 0(3) . . . . ? C13 C12 C15 C16 4(3) . . . . ? C11 C12 C15 C16 179.9(16) . . . . ? C12 C15 C16 N5 -6(3) . . . . ? N6 C17 C18 C19 0(3) . . . . ? C17 C18 C19 C10 -172.7(17) . . . 2_655 ? C17 C18 C19 C20 2(3) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C10 C19 C20 C21 174.0(15) 2_655 . . . ? C19 C20 C21 N6 -2(2) . . . . ? C26 C22 C23 C24 -1(2) . . . . ? C27 C22 C23 C24 180(2) . . . . ? Rh1 C22 C23 C24 -60.8(14) . . . . ? C26 C22 C23 C28 179(2) . . . . ? C27 C22 C23 C28 -1(4) . . . . ? Rh1 C22 C23 C28 118(2) . . . . ? C26 C22 C23 Rh1 60.2(15) . . . . ? C27 C22 C23 Rh1 -119(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C28 C23 C24 C25 -179(2) . . . . ? Rh1 C23 C24 C25 -61.6(14) . . . . ? C22 C23 C24 C29 -178.9(19) . . . . ? C28 C23 C24 C29 2(3) . . . . ? Rh1 C23 C24 C29 119.1(19) . . . . ? C22 C23 C24 Rh1 61.9(15) . . . . ? C28 C23 C24 Rh1 -117(2) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C29 C24 C25 C26 179(2) . . . . ? Rh1 C24 C25 C26 -62.1(15) . . . . ? C23 C24 C25 C30 -177(2) . . . . ? C29 C24 C25 C30 2(3) . . . . ? Rh1 C24 C25 C30 120(2) . . . . ? C23 C24 C25 Rh1 62.1(13) . . . . ? C29 C24 C25 Rh1 -119(2) . . . . ? C24 C25 C26 C22 0(2) . . . . ? C30 C25 C26 C22 177(2) . . . . ? Rh1 C25 C26 C22 -61.4(15) . . . . ? C24 C25 C26 C31 178(2) . . . . ? C30 C25 C26 C31 -5(4) . . . . ? Rh1 C25 C26 C31 117(2) . . . . ? C24 C25 C26 Rh1 61.0(15) . . . . ? C30 C25 C26 Rh1 -121(2) . . . . ? C23 C22 C26 C25 1(2) . . . . ? C27 C22 C26 C25 -180(2) . . . . ? Rh1 C22 C26 C25 60.3(15) . . . . ? C23 C22 C26 C31 -178(2) . . . . ? C27 C22 C26 C31 2(4) . . . . ? Rh1 C22 C26 C31 -118(2) . . . . ? C23 C22 C26 Rh1 -59.8(15) . . . . ? C27 C22 C26 Rh1 120(2) . . . . ? C37 C32 C33 C34 -177.3(18) . . . . ? C36 C32 C33 C34 1(2) . . . . ? Rh2 C32 C33 C34 60.0(14) . . . . ? C37 C32 C33 C38 1(3) . . . . ? C36 C32 C33 C38 179.4(19) . . . . ? Rh2 C32 C33 C38 -121(2) . . . . ? C37 C32 C33 Rh2 123(2) . . . . ? C36 C32 C33 Rh2 -59.4(13) . . . . ? C32 C33 C34 C35 1(2) . . . . ? C38 C33 C34 C35 -177.5(18) . . . . ? Rh2 C33 C34 C35 61.6(13) . . . . ? C32 C33 C34 C39 177.4(18) . . . . ? C38 C33 C34 C39 -2(3) . . . . ? Rh2 C33 C34 C39 -122.4(19) . . . . ? C32 C33 C34 Rh2 -60.3(14) . . . . ? C38 C33 C34 Rh2 120.8(19) . . . . ? C39 C34 C35 C36 -178.7(19) . . . . ? C33 C34 C35 C36 -3(2) . . . . ? Rh2 C34 C35 C36 58.5(14) . . . . ? C39 C34 C35 C40 3(3) . . . . ? C33 C34 C35 C40 178.8(18) . . . . ? Rh2 C34 C35 C40 -119.7(18) . . . . ? C39 C34 C35 Rh2 123(2) . . . . ? C33 C34 C35 Rh2 -61.5(13) . . . . ? C34 C35 C36 C32 3(2) . . . . ? C40 C35 C36 C32 -178.6(17) . . . . ? Rh2 C35 C36 C32 61.9(12) . . . . ? C34 C35 C36 C41 179(2) . . . . ? C40 C35 C36 C41 -3(3) . . . . ? Rh2 C35 C36 C41 -122(2) . . . . ? C34 C35 C36 Rh2 -58.7(14) . . . . ? C40 C35 C36 Rh2 119.5(19) . . . . ? C33 C32 C36 C35 -2(2) . . . . ? C37 C32 C36 C35 175.6(18) . . . . ? Rh2 C32 C36 C35 -62.9(13) . . . . ? C33 C32 C36 C41 -178(2) . . . . ? C37 C32 C36 C41 0(3) . . . . ? Rh2 C32 C36 C41 121(2) . . . . ? C33 C32 C36 Rh2 60.6(13) . . . . ? C37 C32 C36 Rh2 -122(2) . . . . ? C46 C42 C43 C44 -2(2) . . . . ? C47 C42 C43 C44 178.3(19) . . . . ? Rh3 C42 C43 C44 -62.0(14) . . . . ? C46 C42 C43 C48 179(2) . . . . ? C47 C42 C43 C48 0(4) . . . . ? Rh3 C42 C43 C48 119(3) . . . . ? C46 C42 C43 Rh3 59.6(15) . . . . ? C47 C42 C43 Rh3 -120(2) . . . . ? C42 C43 C44 C45 2(2) . . . . ? C48 C43 C44 C45 -179.5(19) . . . . ? Rh3 C43 C44 C45 -61.1(15) . . . . ? C42 C43 C44 C49 -179(2) . . . . ? C48 C43 C44 C49 0(3) . . . . ? Rh3 C43 C44 C49 118(2) . . . . ? C42 C43 C44 Rh3 62.7(14) . . . . ? C48 C43 C44 Rh3 -118.4(19) . . . . ? C43 C44 C45 C46 0(2) . . . . ? C49 C44 C45 C46 -179(2) . . . . ? Rh3 C44 C45 C46 -60.0(13) . . . . ? C43 C44 C45 C50 178(2) . . . . ? C49 C44 C45 C50 -1(4) . . . . ? Rh3 C44 C45 C50 118(2) . . . . ? C43 C44 C45 Rh3 59.8(14) . . . . ? C49 C44 C45 Rh3 -119(2) . . . . ? C43 C42 C46 C45 2(2) . . . . ? C47 C42 C46 C45 -178.3(19) . . . . ? Rh3 C42 C46 C45 62.3(15) . . . . ? C43 C42 C46 C51 178.0(19) . . . . ? C47 C42 C46 C51 -3(3) . . . . ? Rh3 C42 C46 C51 -122(2) . . . . ? C43 C42 C46 Rh3 -60.0(15) . . . . ? C47 C42 C46 Rh3 119(2) . . . . ? C44 C45 C46 C42 -1(2) . . . . ? C50 C45 C46 C42 -179.4(19) . . . . ? Rh3 C45 C46 C42 -62.4(15) . . . . ? C44 C45 C46 C51 -177.1(19) . . . . ? C50 C45 C46 C51 5(3) . . . . ? Rh3 C45 C46 C51 121.8(19) . . . . ? C44 C45 C46 Rh3 61.1(14) . . . . ? C50 C45 C46 Rh3 -117(2) . . . . ? C60 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C58 0.0 . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C55 0.0 . . . . ? C56 C55 C60 C59 0.0 . . . . ? C66 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C72 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C71 0.0 . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C67 0.0 . . . . ? C68 C67 C72 C71 0.0 . . . . ? C5 C4 N1 C8 3(3) . . . . ? C5 C4 N1 Rh1 179.7(15) . . . . ? C7 C8 N1 C4 1(3) . . . . ? C7 C8 N1 Rh1 -175.5(14) . . . . ? N3 C10 N2 C9 7(2) . . . . ? C19 C10 N2 C9 -175.2(14) 2_655 . . . ? N4 C9 N2 C10 -3(2) . . . . ? C6 C9 N2 C10 173.5(14) . . . . ? N4 C11 N3 C10 -1(2) . . . . ? C12 C11 N3 C10 -174.2(13) . . . . ? N2 C10 N3 C11 -5(2) . . . . ? C19 C10 N3 C11 176.6(14) 2_655 . . . ? N3 C11 N4 C9 4(2) . . . . ? C12 C11 N4 C9 177.8(13) . . . . ? N2 C9 N4 C11 -2(2) . . . . ? C6 C9 N4 C11 -178.8(13) . . . . ? C13 C14 N5 C16 -2(3) . . . . ? C13 C14 N5 Rh3 173.2(14) . . . . ? C15 C16 N5 C14 5(3) . . . . ? C15 C16 N5 Rh3 -170.0(14) . . . . ? C18 C17 N6 C21 -2(3) . . . . ? C18 C17 N6 Rh2 161.4(15) . . . . ? C20 C21 N6 C17 4(2) . . . . ? C20 C21 N6 Rh2 -159.5(13) . . . . ? O3 C1 O1 Rh1 168.9(13) . . . . ? C2 C1 O1 Rh1 -10.8(17) . . . . ? O4 C2 O2 Rh1 -167.1(14) . . . . ? C1 C2 O2 Rh1 12.4(17) . . . . ? O1 C1 O3 Rh2 -172.5(13) . . . . ? C2 C1 O3 Rh2 7.1(17) . . . . ? O2 C2 O4 Rh2 174.0(14) . . . . ? C1 C2 O4 Rh2 -5.5(18) . . . . ? O6 C3 O5 Rh3 -169.3(13) 2_655 . . . ? C3 C3 O5 Rh3 9.0(9) 2_655 . . . ? C26 C25 Rh1 C24 120.5(17) . . . . ? C30 C25 Rh1 C24 -120(2) . . . . ? C26 C25 Rh1 C23 81.5(13) . . . . ? C24 C25 Rh1 C23 -39.1(11) . . . . ? C30 C25 Rh1 C23 -159(2) . . . . ? C26 C25 Rh1 N1 -154.5(11) . . . . ? C24 C25 Rh1 N1 85.0(11) . . . . ? C30 C25 Rh1 N1 -35.2(19) . . . . ? C26 C25 Rh1 O1 -64.7(13) . . . . ? C24 C25 Rh1 O1 174.7(10) . . . . ? C30 C25 Rh1 O1 54.5(19) . . . . ? C24 C25 Rh1 C26 -120.5(17) . . . . ? C30 C25 Rh1 C26 119(2) . . . . ? C26 C25 Rh1 O2 87(3) . . . . ? C24 C25 Rh1 O2 -33(3) . . . . ? C30 C25 Rh1 O2 -153.5(17) . . . . ? C26 C25 Rh1 C22 38.5(12) . . . . ? C24 C25 Rh1 C22 -82.0(12) . . . . ? C30 C25 Rh1 C22 158(2) . . . . ? C23 C24 Rh1 C25 -115.7(16) . . . . ? C29 C24 Rh1 C25 124(2) . . . . ? C25 C24 Rh1 C23 115.7(16) . . . . ? C29 C24 Rh1 C23 -120(2) . . . . ? C25 C24 Rh1 N1 -102.6(11) . . . . ? C23 C24 Rh1 N1 141.6(12) . . . . ? C29 C24 Rh1 N1 21.4(16) . . . . ? C25 C24 Rh1 O1 -12(2) . . . . ? C23 C24 Rh1 O1 -127.3(15) . . . . ? C29 C24 Rh1 O1 112.5(18) . . . . ? C25 C24 Rh1 C26 35.6(11) . . . . ? C23 C24 Rh1 C26 -80.1(13) . . . . ? C29 C24 Rh1 C26 159.6(18) . . . . ? C25 C24 Rh1 O2 168.6(9) . . . . ? C23 C24 Rh1 O2 52.8(13) . . . . ? C29 C24 Rh1 O2 -67.4(17) . . . . ? C25 C24 Rh1 C22 78.7(12) . . . . ? C23 C24 Rh1 C22 -37.0(11) . . . . ? C29 C24 Rh1 C22 -157.2(18) . . . . ? C22 C23 Rh1 C25 -79.8(12) . . . . ? C24 C23 Rh1 C25 38.8(11) . . . . ? C28 C23 Rh1 C25 159(2) . . . . ? C22 C23 Rh1 C24 -118.6(16) . . . . ? C28 C23 Rh1 C24 120(2) . . . . ? C22 C23 Rh1 N1 -168.5(10) . . . . ? C24 C23 Rh1 N1 -49.9(14) . . . . ? C28 C23 Rh1 N1 70(2) . . . . ? C22 C23 Rh1 O1 21.1(19) . . . . ? C24 C23 Rh1 O1 139.7(12) . . . . ? C28 C23 Rh1 O1 -100(2) . . . . ? C22 C23 Rh1 C26 -37.7(12) . . . . ? C24 C23 Rh1 C26 80.9(12) . . . . ? C28 C23 Rh1 C26 -159(2) . . . . ? C22 C23 Rh1 O2 101.9(11) . . . . ? C24 C23 Rh1 O2 -139.5(11) . . . . ? C28 C23 Rh1 O2 -19(2) . . . . ? C24 C23 Rh1 C22 118.6(16) . . . . ? C28 C23 Rh1 C22 -121(2) . . . . ? C4 N1 Rh1 C25 -123.7(15) . . . . ? C8 N1 Rh1 C25 53.1(16) . . . . ? C4 N1 Rh1 C24 -84.5(15) . . . . ? C8 N1 Rh1 C24 92.2(15) . . . . ? C4 N1 Rh1 C23 -55.4(17) . . . . ? C8 N1 Rh1 C23 121.4(15) . . . . ? C4 N1 Rh1 O1 119.8(15) . . . . ? C8 N1 Rh1 O1 -63.5(14) . . . . ? C4 N1 Rh1 C26 -146.4(15) . . . . ? C8 N1 Rh1 C26 30.4(19) . . . . ? C4 N1 Rh1 O2 41.4(15) . . . . ? C8 N1 Rh1 O2 -141.9(15) . . . . ? C4 N1 Rh1 C22 -80(3) . . . . ? C8 N1 Rh1 C22 96(3) . . . . ? C1 O1 Rh1 C25 -175.0(11) . . . . ? C1 O1 Rh1 C24 -166.9(15) . . . . ? C1 O1 Rh1 C23 99.5(16) . . . . ? C1 O1 Rh1 N1 -72.8(11) . . . . ? C1 O1 Rh1 C26 150.9(12) . . . . ? C1 O1 Rh1 O2 13.0(11) . . . . ? C1 O1 Rh1 C22 113.5(12) . . . . ? C22 C26 Rh1 C25 117.2(17) . . . . ? C31 C26 Rh1 C25 -123(2) . . . . ? C25 C26 Rh1 C24 -36.6(11) . . . . ? C22 C26 Rh1 C24 80.6(12) . . . . ? C31 C26 Rh1 C24 -160(2) . . . . ? C25 C26 Rh1 C23 -79.9(13) . . . . ? C22 C26 Rh1 C23 37.3(12) . . . . ? C31 C26 Rh1 C23 157(2) . . . . ? C25 C26 Rh1 N1 37.6(16) . . . . ? C22 C26 Rh1 N1 154.8(11) . . . . ? C31 C26 Rh1 N1 -86(2) . . . . ? C25 C26 Rh1 O1 125.8(12) . . . . ? C22 C26 Rh1 O1 -117.0(12) . . . . ? C31 C26 Rh1 O1 2.7(19) . . . . ? C25 C26 Rh1 O2 -154.0(12) . . . . ? C22 C26 Rh1 O2 -36.9(17) . . . . ? C31 C26 Rh1 O2 83(2) . . . . ? C25 C26 Rh1 C22 -117.2(17) . . . . ? C31 C26 Rh1 C22 120(2) . . . . ? C2 O2 Rh1 C25 -169(2) . . . . ? C2 O2 Rh1 C24 166.1(11) . . . . ? C2 O2 Rh1 C23 -163.3(12) . . . . ? C2 O2 Rh1 N1 70.6(11) . . . . ? C2 O2 Rh1 O1 -13.8(11) . . . . ? C2 O2 Rh1 C26 -101.4(14) . . . . ? C2 O2 Rh1 C22 -124.3(12) . . . . ? C23 C22 Rh1 C25 80.8(13) . . . . ? C26 C22 Rh1 C25 -37.4(12) . . . . ? C27 C22 Rh1 C25 -159(2) . . . . ? C23 C22 Rh1 C24 37.6(11) . . . . ? C26 C22 Rh1 C24 -80.6(12) . . . . ? C27 C22 Rh1 C24 158(2) . . . . ? C26 C22 Rh1 C23 -118.2(17) . . . . ? C27 C22 Rh1 C23 120(2) . . . . ? C23 C22 Rh1 N1 33(3) . . . . ? C26 C22 Rh1 N1 -85(3) . . . . ? C27 C22 Rh1 N1 153(2) . . . . ? C23 C22 Rh1 O1 -168.7(10) . . . . ? C26 C22 Rh1 O1 73.1(12) . . . . ? C27 C22 Rh1 O1 -49(2) . . . . ? C23 C22 Rh1 C26 118.2(17) . . . . ? C27 C22 Rh1 C26 -122(2) . . . . ? C23 C22 Rh1 O2 -86.1(12) . . . . ? C26 C22 Rh1 O2 155.7(12) . . . . ? C27 C22 Rh1 O2 34(2) . . . . ? C17 N6 Rh2 O4 135.7(13) . . . . ? C21 N6 Rh2 O4 -61.5(13) . . . . ? C17 N6 Rh2 C36 -111(2) . . . . ? C21 N6 Rh2 C36 52(2) . . . . ? C17 N6 Rh2 O3 57.7(13) . . . . ? C21 N6 Rh2 O3 -139.5(14) . . . . ? C17 N6 Rh2 C32 -121.5(14) . . . . ? C21 N6 Rh2 C32 41.3(16) . . . . ? C17 N6 Rh2 C33 -91.3(14) . . . . ? C21 N6 Rh2 C33 71.4(14) . . . . ? C17 N6 Rh2 C35 -37.5(18) . . . . ? C21 N6 Rh2 C35 125.3(14) . . . . ? C17 N6 Rh2 C34 -52.2(14) . . . . ? C21 N6 Rh2 C34 110.5(14) . . . . ? C2 O4 Rh2 N6 -78.2(12) . . . . ? C2 O4 Rh2 C36 121.8(12) . . . . ? C2 O4 Rh2 O3 7.0(11) . . . . ? C2 O4 Rh2 C32 163.5(12) . . . . ? C2 O4 Rh2 C33 -171.1(12) . . . . ? C2 O4 Rh2 C35 96.1(13) . . . . ? C2 O4 Rh2 C34 137(3) . . . . ? C35 C36 Rh2 N6 100.4(19) . . . . ? C32 C36 Rh2 N6 -14(3) . . . . ? C41 C36 Rh2 N6 -134.5(19) . . . . ? C35 C36 Rh2 O4 -148.3(11) . . . . ? C32 C36 Rh2 O4 97.0(12) . . . . ? C41 C36 Rh2 O4 -23.1(19) . . . . ? C35 C36 Rh2 O3 -67.0(13) . . . . ? C32 C36 Rh2 O3 178.3(10) . . . . ? C41 C36 Rh2 O3 58(2) . . . . ? C35 C36 Rh2 C32 114.8(17) . . . . ? C41 C36 Rh2 C32 -120(2) . . . . ? C35 C36 Rh2 C33 79.0(13) . . . . ? C32 C36 Rh2 C33 -35.8(11) . . . . ? C41 C36 Rh2 C33 -156(2) . . . . ? C32 C36 Rh2 C35 -114.8(17) . . . . ? C41 C36 Rh2 C35 125(2) . . . . ? C35 C36 Rh2 C34 35.5(11) . . . . ? C32 C36 Rh2 C34 -79.3(12) . . . . ? C41 C36 Rh2 C34 161(2) . . . . ? C1 O3 Rh2 N6 81.8(11) . . . . ? C1 O3 Rh2 O4 -7.6(10) . . . . ? C1 O3 Rh2 C36 -102.8(12) . . . . ? C1 O3 Rh2 C32 -99.9(19) . . . . ? C1 O3 Rh2 C33 169.8(13) . . . . ? C1 O3 Rh2 C35 -138.1(12) . . . . ? C1 O3 Rh2 C34 -176.4(11) . . . . ? C33 C32 Rh2 N6 54.7(13) . . . . ? C37 C32 Rh2 N6 -66(2) . . . . ? C36 C32 Rh2 N6 174.1(11) . . . . ? C33 C32 Rh2 O4 149.3(11) . . . . ? C37 C32 Rh2 O4 29(2) . . . . ? C36 C32 Rh2 O4 -91.3(12) . . . . ? C33 C32 Rh2 C36 -119.4(17) . . . . ? C37 C32 Rh2 C36 120(3) . . . . ? C33 C32 Rh2 O3 -123.3(17) . . . . ? C37 C32 Rh2 O3 116(2) . . . . ? C36 C32 Rh2 O3 -4(2) . . . . ? C37 C32 Rh2 C33 -121(3) . . . . ? C36 C32 Rh2 C33 119.4(17) . . . . ? C33 C32 Rh2 C35 -80.8(13) . . . . ? C37 C32 Rh2 C35 158(2) . . . . ? C36 C32 Rh2 C35 38.5(12) . . . . ? C33 C32 Rh2 C34 -37.4(12) . . . . ? C37 C32 Rh2 C34 -158(2) . . . . ? C36 C32 Rh2 C34 82.0(13) . . . . ? C32 C33 Rh2 N6 -133.8(12) . . . . ? C34 C33 Rh2 N6 106.1(11) . . . . ? C38 C33 Rh2 N6 -11(2) . . . . ? C32 C33 Rh2 O4 -43.0(15) . . . . ? C34 C33 Rh2 O4 -163.0(10) . . . . ? C38 C33 Rh2 O4 80(2) . . . . ? C32 C33 Rh2 C36 38.5(12) . . . . ? C34 C33 Rh2 C36 -81.5(12) . . . . ? C38 C33 Rh2 C36 162(2) . . . . ? C32 C33 Rh2 O3 140.5(13) . . . . ? C34 C33 Rh2 O3 20.5(18) . . . . ? C38 C33 Rh2 O3 -96(2) . . . . ? C34 C33 Rh2 C32 -120.0(17) . . . . ? C38 C33 Rh2 C32 123(3) . . . . ? C32 C33 Rh2 C35 80.8(13) . . . . ? C34 C33 Rh2 C35 -39.2(11) . . . . ? C38 C33 Rh2 C35 -156(2) . . . . ? C32 C33 Rh2 C34 120.0(17) . . . . ? C38 C33 Rh2 C34 -117(2) . . . . ? C36 C35 Rh2 N6 -145.7(11) . . . . ? C34 C35 Rh2 N6 -23.0(15) . . . . ? C40 C35 Rh2 N6 94(2) . . . . ? C36 C35 Rh2 O4 43.4(14) . . . . ? C34 C35 Rh2 O4 166.0(9) . . . . ? C40 C35 Rh2 O4 -77.5(19) . . . . ? C34 C35 Rh2 C36 122.6(16) . . . . ? C40 C35 Rh2 C36 -121(2) . . . . ? C36 C35 Rh2 O3 123.6(11) . . . . ? C34 C35 Rh2 O3 -113.8(11) . . . . ? C40 C35 Rh2 O3 2.8(19) . . . . ? C36 C35 Rh2 C32 -41.0(11) . . . . ? C34 C35 Rh2 C32 81.7(12) . . . . ? C40 C35 Rh2 C32 -162(2) . . . . ? C36 C35 Rh2 C33 -83.0(12) . . . . ? C34 C35 Rh2 C33 39.7(11) . . . . ? C40 C35 Rh2 C33 156(2) . . . . ? C36 C35 Rh2 C34 -122.6(16) . . . . ? C40 C35 Rh2 C34 117(2) . . . . ? C35 C34 Rh2 N6 165.1(10) . . . . ? C39 C34 Rh2 N6 39.6(19) . . . . ? C33 C34 Rh2 N6 -79.6(12) . . . . ? C35 C34 Rh2 O4 -51(3) . . . . ? C39 C34 Rh2 O4 -176(2) . . . . ? C33 C34 Rh2 O4 65(3) . . . . ? C35 C34 Rh2 C36 -34.7(10) . . . . ? C39 C34 Rh2 C36 -160(2) . . . . ? C33 C34 Rh2 C36 80.5(12) . . . . ? C35 C34 Rh2 O3 75.8(11) . . . . ? C39 C34 Rh2 O3 -49.8(19) . . . . ? C33 C34 Rh2 O3 -168.9(10) . . . . ? C35 C34 Rh2 C32 -79.6(12) . . . . ? C39 C34 Rh2 C32 155(2) . . . . ? C33 C34 Rh2 C32 35.7(11) . . . . ? C35 C34 Rh2 C33 -115.3(16) . . . . ? C39 C34 Rh2 C33 119(2) . . . . ? C39 C34 Rh2 C35 -126(2) . . . . ? C33 C34 Rh2 C35 115.3(16) . . . . ? C42 C46 Rh3 N5 -69.1(13) . . . . ? C45 C46 Rh3 N5 170.4(13) . . . . ? C51 C46 Rh3 N5 53.1(19) . . . . ? C42 C46 Rh3 C43 36.0(13) . . . . ? C45 C46 Rh3 C43 -84.5(15) . . . . ? C51 C46 Rh3 C43 158(2) . . . . ? C45 C46 Rh3 C42 -120.5(19) . . . . ? C51 C46 Rh3 C42 122(2) . . . . ? C42 C46 Rh3 C44 81.9(14) . . . . ? C45 C46 Rh3 C44 -38.6(14) . . . . ? C51 C46 Rh3 C44 -156(2) . . . . ? C42 C46 Rh3 O6 94(2) . . . . ? C45 C46 Rh3 O6 -26(3) . . . . ? C51 C46 Rh3 O6 -143.3(19) . . . . ? C42 C46 Rh3 O5 -158.0(11) . . . . ? C45 C46 Rh3 O5 81.5(14) . . . . ? C51 C46 Rh3 O5 -35.7(19) . . . . ? C42 C46 Rh3 C45 120.5(19) . . . . ? C51 C46 Rh3 C45 -117(2) . . . . ? C14 N5 Rh3 C46 -45.2(16) . . . . ? C16 N5 Rh3 C46 129.4(14) . . . . ? C14 N5 Rh3 C43 -114.0(15) . . . . ? C16 N5 Rh3 C43 60.6(15) . . . . ? C14 N5 Rh3 C42 -79.7(15) . . . . ? C16 N5 Rh3 C42 95.0(14) . . . . ? C14 N5 Rh3 C44 -118.4(19) . . . . ? C16 N5 Rh3 C44 56(2) . . . . ? C14 N5 Rh3 O6 139.8(14) . . . . ? C16 N5 Rh3 O6 -45.6(13) . . . . ? C14 N5 Rh3 O5 60.7(14) . . . . ? C16 N5 Rh3 O5 -124.6(14) . . . . ? C14 N5 Rh3 C45 -34(2) . . . . ? C16 N5 Rh3 C45 140.8(17) . . . . ? C42 C43 Rh3 C46 -35.5(11) . . . . ? C44 C43 Rh3 C46 80.5(13) . . . . ? C48 C43 Rh3 C46 -167(3) . . . . ? C42 C43 Rh3 N5 67.0(13) . . . . ? C44 C43 Rh3 N5 -176.9(12) . . . . ? C48 C43 Rh3 N5 -64(3) . . . . ? C44 C43 Rh3 C42 116.1(18) . . . . ? C48 C43 Rh3 C42 -131(3) . . . . ? C42 C43 Rh3 C44 -116.1(18) . . . . ? C48 C43 Rh3 C44 113(3) . . . . ? C42 C43 Rh3 O6 160.2(11) . . . . ? C44 C43 Rh3 O6 -83.7(13) . . . . ? C48 C43 Rh3 O6 29(3) . . . . ? C42 C43 Rh3 O5 -93(3) . . . . ? C44 C43 Rh3 O5 23(4) . . . . ? C48 C43 Rh3 O5 135(3) . . . . ? C42 C43 Rh3 C45 -78.4(13) . . . . ? C44 C43 Rh3 C45 37.7(12) . . . . ? C48 C43 Rh3 C45 150(3) . . . . ? C43 C42 Rh3 C46 120.4(18) . . . . ? C47 C42 Rh3 C46 -119(2) . . . . ? C46 C42 Rh3 N5 118.5(12) . . . . ? C43 C42 Rh3 N5 -121.1(13) . . . . ? C47 C42 Rh3 N5 -0.8(19) . . . . ? C46 C42 Rh3 C43 -120.4(18) . . . . ? C47 C42 Rh3 C43 120(2) . . . . ? C46 C42 Rh3 C44 -79.9(13) . . . . ? C43 C42 Rh3 C44 40.5(13) . . . . ? C47 C42 Rh3 C44 161(2) . . . . ? C46 C42 Rh3 O6 -151.2(10) . . . . ? C43 C42 Rh3 O6 -30.8(17) . . . . ? C47 C42 Rh3 O6 89(2) . . . . ? C46 C42 Rh3 O5 34.3(16) . . . . ? C43 C42 Rh3 O5 154.7(12) . . . . ? C47 C42 Rh3 O5 -85(2) . . . . ? C46 C42 Rh3 C45 -36.7(12) . . . . ? C43 C42 Rh3 C45 83.7(14) . . . . ? C47 C42 Rh3 C45 -156(2) . . . . ? C45 C44 Rh3 C46 38.5(12) . . . . ? C43 C44 Rh3 C46 -78.5(14) . . . . ? C49 C44 Rh3 C46 162(3) . . . . ? C45 C44 Rh3 N5 123.2(17) . . . . ? C43 C44 Rh3 N5 6(2) . . . . ? C49 C44 Rh3 N5 -114(3) . . . . ? C45 C44 Rh3 C43 117.0(19) . . . . ? C49 C44 Rh3 C43 -120(3) . . . . ? C45 C44 Rh3 C42 79.7(13) . . . . ? C43 C44 Rh3 C42 -37.2(12) . . . . ? C49 C44 Rh3 C42 -157(3) . . . . ? C45 C44 Rh3 O6 -137.6(12) . . . . ? C43 C44 Rh3 O6 105.4(13) . . . . ? C49 C44 Rh3 O6 -14(3) . . . . ? C45 C44 Rh3 O5 -55.8(15) . . . . ? C43 C44 Rh3 O5 -172.7(12) . . . . ? C49 C44 Rh3 O5 67(3) . . . . ? C43 C44 Rh3 C45 -117.0(19) . . . . ? C49 C44 Rh3 C45 123(3) . . . . ? C3 O6 Rh3 C46 117(2) 2_655 . . . ? C3 O6 Rh3 N5 -78.0(12) 2_655 . . . ? C3 O6 Rh3 C43 170.1(13) 2_655 . . . ? C3 O6 Rh3 C42 -170.9(12) 2_655 . . . ? C3 O6 Rh3 C44 128.8(13) 2_655 . . . ? C3 O6 Rh3 O5 5.5(11) 2_655 . . . ? C3 O6 Rh3 C45 97.8(14) 2_655 . . . ? C3 O5 Rh3 C46 -170.8(11) . . . . ? C3 O5 Rh3 N5 80.1(11) . . . . ? C3 O5 Rh3 C43 -118(3) . . . . ? C3 O5 Rh3 C42 168.3(12) . . . . ? C3 O5 Rh3 C44 -100.4(12) . . . . ? C3 O5 Rh3 O6 -8.2(10) . . . . ? C3 O5 Rh3 C45 -132.1(12) . . . . ? C44 C45 Rh3 C46 -116.3(19) . . . . ? C50 C45 Rh3 C46 119(3) . . . . ? C46 C45 Rh3 N5 -17(2) . . . . ? C44 C45 Rh3 N5 -133.6(16) . . . . ? C50 C45 Rh3 N5 101(2) . . . . ? C46 C45 Rh3 C43 76.7(14) . . . . ? C44 C45 Rh3 C43 -39.7(14) . . . . ? C50 C45 Rh3 C43 -165(2) . . . . ? C46 C45 Rh3 C42 35.2(12) . . . . ? C44 C45 Rh3 C42 -81.2(15) . . . . ? C50 C45 Rh3 C42 154(2) . . . . ? C46 C45 Rh3 C44 116.3(19) . . . . ? C50 C45 Rh3 C44 -125(3) . . . . ? C46 C45 Rh3 O6 170.6(11) . . . . ? C44 C45 Rh3 O6 54.2(16) . . . . ? C50 C45 Rh3 O6 -71(2) . . . . ? C46 C45 Rh3 O5 -107.4(13) . . . . ? C44 C45 Rh3 O5 136.3(13) . . . . ? C50 C45 Rh3 O5 11(2) . . . . ? O8 S1 C52 F2 -59.5 . . . . ? O7 S1 C52 F2 179.9 . . . . ? O9 S1 C52 F2 61.0 . . . . ? O8 S1 C52 F3 179.9 . . . . ? O7 S1 C52 F3 59.3 . . . . ? O9 S1 C52 F3 -59.6 . . . . ? O8 S1 C52 F1 60.4 . . . . ? O7 S1 C52 F1 -60.2 . . . . ? O9 S1 C52 F1 -179.1 . . . . ? O11 S2 C53 F5 -59.5 . . . . ? O10 S2 C53 F5 179.9 . . . . ? O12 S2 C53 F5 61.0 . . . . ? O11 S2 C53 F6 179.9 . . . . ? O10 S2 C53 F6 59.3 . . . . ? O12 S2 C53 F6 -59.6 . . . . ? O11 S2 C53 F4 60.4 . . . . ? O10 S2 C53 F4 -60.2 . . . . ? O12 S2 C53 F4 -179.1 . . . . ? O14 S3 C54 F8 -59.5 . . . . ? O13 S3 C54 F8 179.9 . . . . ? O15 S3 C54 F8 61.0 . . . . ? O14 S3 C54 F9 179.9 . . . . ? O13 S3 C54 F9 59.3 . . . . ? O15 S3 C54 F9 -59.6 . . . . ? O14 S3 C54 F7 60.4 . . . . ? O13 S3 C54 F7 -60.2 . . . . ? O15 S3 C54 F7 -179.1 . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.856 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.185 #===END data_d:compound4 _database_code_depnum_ccdc_archive 'CCDC 650994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102H114N12O12Ir6, (CF3O3S)6' _chemical_formula_sum 'C108 H114 F18 Ir6 N12 O30 S6' _chemical_formula_weight 3747.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F d-3c' _symmetry_space_group_name_Hall 'F 4d 2 3 -1cd' _symmetry_Int_Tables_number 228 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/4, -z+1/4' '-x+1/4, -y+3/4, z+1/2' '-x+1/4, y+1/2, -z+3/4' '-y+1/2, x+1/4, z+1/4' 'y+1/4, x+1/4, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y, -x+1/2, -z' 'y, z, x' '-y+1/4, -z+3/4, x+1/2' 'y, -z+1/4, -x+1/4' '-y+1/4, z+1/2, -x+3/4' '-z+1/2, y+1/4, x+1/4' '-z+1/2, -y, -x' 'z+3/4, -y+1/2, x+3/4' 'z+3/4, y+3/4, -x+1/2' 'z, x, y' '-z+3/4, x+1/2, -y+1/4' '-z+1/4, -x+1/4, y' 'z+1/2, -x+3/4, -y+1/4' '-x+1/2, -z, -y' '-x+1/2, z+3/4, y+3/4' 'x+1/4, -z+1/2, y+1/4' 'x+3/4, z+3/4, -y+1/2' 'x, y+1/2, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, -y+5/4, z+1' '-x+1/4, y+1, -z+5/4' '-y+1/2, x+3/4, z+3/4' 'y+1/4, x+3/4, -z+1' 'y+3/4, -x+1, z+5/4' '-y, -x+1, -z+1/2' 'y, z+1/2, x+1/2' '-y+1/4, -z+5/4, x+1' 'y, -z+3/4, -x+3/4' '-y+1/4, z+1, -x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1/2, -y+1/2, -x+1/2' 'z+3/4, -y+1, x+5/4' 'z+3/4, y+5/4, -x+1' 'z, x+1/2, y+1/2' '-z+3/4, x+1, -y+3/4' '-z+1/4, -x+3/4, y+1/2' 'z+1/2, -x+5/4, -y+3/4' '-x+1/2, -z+1/2, -y+1/2' '-x+1/2, z+5/4, y+5/4' 'x+1/4, -z+1, y+3/4' 'x+3/4, z+5/4, -y+1' 'x+1/2, y, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, -y+3/4, z+1' '-x+3/4, y+1/2, -z+5/4' '-y+1, x+1/4, z+3/4' 'y+3/4, x+1/4, -z+1' 'y+5/4, -x+1/2, z+5/4' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, z, x+1/2' '-y+3/4, -z+3/4, x+1' 'y+1/2, -z+1/4, -x+3/4' '-y+3/4, z+1/2, -x+5/4' '-z+1, y+1/4, x+3/4' '-z+1, -y, -x+1/2' 'z+5/4, -y+1/2, x+5/4' 'z+5/4, y+3/4, -x+1' 'z+1/2, x, y+1/2' '-z+5/4, x+1/2, -y+3/4' '-z+3/4, -x+1/4, y+1/2' 'z+1, -x+3/4, -y+3/4' '-x+1, -z, -y+1/2' '-x+1, z+3/4, y+5/4' 'x+3/4, -z+1/2, y+3/4' 'x+5/4, z+3/4, -y+1' 'x+1/2, y+1/2, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1, -z+3/4' '-y+1, x+3/4, z+1/4' 'y+3/4, x+3/4, -z+1/2' 'y+5/4, -x+1, z+3/4' '-y+1/2, -x+1, -z' 'y+1/2, z+1/2, x' '-y+3/4, -z+5/4, x+1/2' 'y+1/2, -z+3/4, -x+1/4' '-y+3/4, z+1, -x+3/4' '-z+1, y+3/4, x+1/4' '-z+1, -y+1/2, -x' 'z+5/4, -y+1, x+3/4' 'z+5/4, y+5/4, -x+1/2' 'z+1/2, x+1/2, y' '-z+5/4, x+1, -y+1/4' '-z+3/4, -x+3/4, y' 'z+1, -x+5/4, -y+1/4' '-x+1, -z+1/2, -y' '-x+1, z+5/4, y+3/4' 'x+3/4, -z+1, y+1/4' 'x+5/4, z+5/4, -y+1/2' '-x, -y, -z' '-x, y-1/4, z-1/4' 'x-1/4, y-3/4, -z-1/2' 'x-1/4, -y-1/2, z-3/4' 'y-1/2, -x-1/4, -z-1/4' '-y-1/4, -x-1/4, z-1/2' '-y-3/4, x-1/2, -z-3/4' 'y, x-1/2, z' '-y, -z, -x' 'y-1/4, z-3/4, -x-1/2' '-y, z-1/4, x-1/4' 'y-1/4, -z-1/2, x-3/4' 'z-1/2, -y-1/4, -x-1/4' 'z-1/2, y, x' '-z-3/4, y-1/2, -x-3/4' '-z-3/4, -y-3/4, x-1/2' '-z, -x, -y' 'z-3/4, -x-1/2, y-1/4' 'z-1/4, x-1/4, -y' '-z-1/2, x-3/4, y-1/4' 'x-1/2, z, y' 'x-1/2, -z-3/4, -y-3/4' '-x-1/4, z-1/2, -y-1/4' '-x-3/4, -z-3/4, y-1/2' '-x, -y+1/2, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, y-1/4, -z' 'x-1/4, -y, z-1/4' 'y-1/2, -x+1/4, -z+1/4' '-y-1/4, -x+1/4, z' '-y-3/4, x, -z-1/4' 'y, x, z+1/2' '-y, -z+1/2, -x+1/2' 'y-1/4, z-1/4, -x' '-y, z+1/4, x+1/4' 'y-1/4, -z, x-1/4' 'z-1/2, -y+1/4, -x+1/4' 'z-1/2, y+1/2, x+1/2' '-z-3/4, y, -x-1/4' '-z-3/4, -y-1/4, x' '-z, -x+1/2, -y+1/2' 'z-3/4, -x, y+1/4' 'z-1/4, x+1/4, -y+1/2' '-z-1/2, x-1/4, y+1/4' 'x-1/2, z+1/2, y+1/2' 'x-1/2, -z-1/4, -y-1/4' '-x-1/4, z, -y+1/4' '-x-3/4, -z-1/4, y' '-x+1/2, -y, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, y-3/4, -z' 'x+1/4, -y-1/2, z-1/4' 'y, -x-1/4, -z+1/4' '-y+1/4, -x-1/4, z' '-y-1/4, x-1/2, -z-1/4' 'y+1/2, x-1/2, z+1/2' '-y+1/2, -z, -x+1/2' 'y+1/4, z-3/4, -x' '-y+1/2, z-1/4, x+1/4' 'y+1/4, -z-1/2, x-1/4' 'z, -y-1/4, -x+1/4' 'z, y, x+1/2' '-z-1/4, y-1/2, -x-1/4' '-z-1/4, -y-3/4, x' '-z+1/2, -x, -y+1/2' 'z-1/4, -x-1/2, y+1/4' 'z+1/4, x-1/4, -y+1/2' '-z, x-3/4, y+1/4' 'x, z, y+1/2' 'x, -z-3/4, -y-1/4' '-x+1/4, z-1/2, -y+1/4' '-x-1/4, -z-3/4, y' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, y-1/4, -z-1/2' 'x+1/4, -y, z-3/4' 'y, -x+1/4, -z-1/4' '-y+1/4, -x+1/4, z-1/2' '-y-1/4, x, -z-3/4' 'y+1/2, x, z' '-y+1/2, -z+1/2, -x' 'y+1/4, z-1/4, -x-1/2' '-y+1/2, z+1/4, x-1/4' 'y+1/4, -z, x-3/4' 'z, -y+1/4, -x-1/4' 'z, y+1/2, x' '-z-1/4, y, -x-3/4' '-z-1/4, -y-1/4, x-1/2' '-z+1/2, -x+1/2, -y' 'z-1/4, -x, y-1/4' 'z+1/4, x+1/4, -y' '-z, x-1/4, y-1/4' 'x, z+1/2, y' 'x, -z-1/4, -y-3/4' '-x+1/4, z, -y-1/4' '-x-1/4, -z-1/4, y-1/2' _cell_length_a 50.159(6) _cell_length_b 50.159(6) _cell_length_c 50.159(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 126196(26) _cell_formula_units_Z 32 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 84715 _cell_measurement_theta_min 1.15 _cell_measurement_theta_max 24.68 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 57792 _exptl_absorpt_coefficient_mu 5.204 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11934 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -59 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.17 _reflns_number_total 4537 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-RED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON03 (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4537 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.003 _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 C1 C 0.1165(2) 0.98810(19) 0.85311(19) 0.068(3) Uani 1 1 d . . . C2 C 0.0351(2) 0.9932(2) 0.8513(3) 0.102(4) Uani 1 1 d . . . H2 H 0.0342 1.0051 0.8655 0.122 Uiso 1 1 calc R . . C3 C 0.0176(2) 0.9965(3) 0.8312(3) 0.118(5) Uani 1 1 d . . . H3 H 0.0052 1.0103 0.8316 0.141 Uiso 1 1 calc R . . C4 C 0.0183(2) 0.9792(3) 0.8101(3) 0.096(3) Uani 1 1 d . . . C5 C 0.0375(2) 0.9596(3) 0.8092(3) 0.119(5) Uani 1 1 d . . . H5 H 0.0387 0.9480 0.7948 0.143 Uiso 1 1 calc R . . C6 C 0.0549(2) 0.9580(3) 0.8309(3) 0.119(5) Uani 1 1 d . . . H6 H 0.0682 0.9451 0.8304 0.143 Uiso 1 1 calc R . . C7 C -0.0017(3) 0.9804(3) 0.7880(2) 0.095(3) Uani 1 1 d . . . C8 C 0.0645(3) 0.96682(17) 0.92833(17) 0.26(2) Uani 1 1 d G . . C9 C 0.0883(3) 0.9518(2) 0.92465(19) 0.185(9) Uani 1 1 d G . . C10 C 0.0824(2) 0.93022(17) 0.9073(2) 0.160(7) Uani 1 1 d G . . C11 C 0.0550(2) 0.93187(18) 0.90029(19) 0.149(6) Uani 1 1 d G . . C12 C 0.0440(2) 0.9545(2) 0.9133(2) 0.28(2) Uani 1 1 d G . . C13 C 0.0617(5) 0.9915(2) 0.9453(2) 0.52(4) Uani 1 1 d G . . H13A H 0.0647 0.9871 0.9636 0.783 Uiso 1 1 calc R . . H13B H 0.0440 0.9986 0.9433 0.783 Uiso 1 1 calc R . . H13C H 0.0745 1.0046 0.9397 0.783 Uiso 1 1 calc R . . C14 C 0.1151(3) 0.9578(4) 0.9370(3) 0.40(3) Uani 1 1 d G . . H14A H 0.1246 0.9414 0.9398 0.593 Uiso 1 1 calc R . . H14B H 0.1125 0.9666 0.9538 0.593 Uiso 1 1 calc R . . H14C H 0.1251 0.9691 0.9253 0.593 Uiso 1 1 calc R . . C15 C 0.1018(3) 0.9092(2) 0.8980(3) 0.41(3) Uani 1 1 d G . . H15A H 0.1157 0.9174 0.8877 0.614 Uiso 1 1 calc R . . H15B H 0.0926 0.8964 0.8872 0.614 Uiso 1 1 calc R . . H15C H 0.1095 0.9004 0.9132 0.614 Uiso 1 1 calc R . . C16 C 0.0402(3) 0.9129(3) 0.8822(3) 0.306(17) Uani 1 1 d G . . H16A H 0.0526 0.9047 0.8701 0.459 Uiso 1 1 calc R . . H16B H 0.0270 0.9226 0.8722 0.459 Uiso 1 1 calc R . . H16C H 0.0316 0.8994 0.8927 0.459 Uiso 1 1 calc R . . C17 C 0.0154(2) 0.9638(3) 0.9114(4) 0.37(3) Uani 1 1 d G . . H17A H 0.0048 0.9544 0.9243 0.558 Uiso 1 1 calc R . . H17B H 0.0087 0.9603 0.8938 0.558 Uiso 1 1 calc R . . H17C H 0.0146 0.9826 0.9149 0.558 Uiso 1 1 calc R . . N1 N 0.05357(17) 0.9740(2) 0.85230(18) 0.089(3) Uani 1 1 d . . . N2 N -0.0200(2) 0.9996(2) 0.7897(2) 0.103(3) Uani 1 1 d . . . O1 O 0.10884(13) 0.96552(13) 0.86007(13) 0.0789(18) Uani 1 1 d . . . O2 O 0.08477(12) 1.00738(12) 0.88351(12) 0.0691(16) Uani 1 1 d . . . Ir1 Ir 0.075530(10) 0.966396(8) 0.886836(10) 0.0902(2) 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 C1 0.088(7) 0.053(5) 0.064(6) -0.013(5) -0.030(6) 0.012(5) C2 0.053(6) 0.115(9) 0.138(11) -0.045(8) -0.017(7) -0.008(7) C3 0.075(8) 0.105(9) 0.173(14) -0.053(10) -0.018(9) -0.003(7) C4 0.070(7) 0.093(8) 0.126(10) -0.004(8) -0.015(7) 0.000(6) C5 0.068(7) 0.136(12) 0.153(12) -0.042(10) -0.015(8) -0.024(8) C6 0.075(8) 0.112(10) 0.169(14) -0.035(10) 0.012(9) 0.004(7) C7 0.098(9) 0.104(9) 0.082(8) -0.027(7) 0.006(7) -0.018(8) C8 0.53(6) 0.105(14) 0.136(16) 0.056(13) 0.11(3) 0.06(2) C9 0.25(3) 0.163(19) 0.140(16) 0.076(15) -0.031(16) -0.059(18) C10 0.25(2) 0.077(9) 0.157(16) 0.014(10) 0.060(15) -0.009(12) C11 0.144(14) 0.113(12) 0.189(17) 0.000(11) 0.018(13) -0.043(11) C12 0.34(4) 0.156(19) 0.33(3) 0.09(2) 0.27(3) 0.11(2) C13 1.29(13) 0.116(16) 0.16(2) -0.036(15) 0.31(4) -0.07(4) C14 0.48(5) 0.45(5) 0.26(3) 0.22(4) -0.21(4) -0.18(5) C15 0.56(5) 0.157(17) 0.51(5) 0.23(3) 0.40(4) 0.24(3) C16 0.36(4) 0.27(3) 0.29(3) 0.06(2) -0.06(3) -0.23(3) C17 0.24(3) 0.36(4) 0.51(5) 0.22(4) 0.26(3) 0.18(3) N1 0.062(5) 0.108(7) 0.096(6) -0.025(6) -0.011(5) -0.009(5) N2 0.100(8) 0.092(7) 0.117(9) -0.013(6) 0.003(7) -0.015(6) O1 0.090(5) 0.066(4) 0.081(4) -0.010(3) -0.002(4) 0.011(4) O2 0.069(4) 0.080(4) 0.059(4) -0.005(3) 0.003(3) 0.009(3) Ir1 0.1030(4) 0.0673(3) 0.1003(4) -0.0062(2) 0.0132(3) -0.0019(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 C1 O1 1.246(11) . ? C1 O2 1.274(12) 87_365 ? C1 C1 1.527(18) 87_365 ? C2 N1 1.338(13) . ? C2 C3 1.348(16) . ? C2 H2 0.9300 . ? C3 C4 1.368(16) . ? C3 H3 0.9300 . ? C4 C5 1.375(16) . ? C4 C7 1.497(16) . ? C5 C6 1.397(18) . ? C5 H5 0.9300 . ? C6 N1 1.343(15) . ? C6 H6 0.9300 . ? C7 N2 1.331(14) . ? C7 N2 1.356(13) 35_465 ? C8 C9 1.4200 . ? C8 C12 1.4200 . ? C8 C13 1.5095 . ? C8 Ir1 2.153(7) . ? C9 C10 1.4200 . ? C9 C14 1.5095 . ? C9 Ir1 2.131(9) . ? C10 C11 1.4200 . ? C10 C15 1.5095 . ? C10 Ir1 2.114(7) . ? C11 C12 1.4200 . ? C11 C16 1.5095 . ? C11 Ir1 2.125(8) . ? C12 C17 1.5095 . ? C12 Ir1 2.149(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? N1 Ir1 2.088(9) . ? N2 C7 1.356(13) 42_556 ? O1 Ir1 2.144(7) . ? O2 C1 1.274(12) 87_365 ? O2 Ir1 2.114(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.8(8) . 87_365 ? O1 C1 C1 116.8(13) . 87_365 ? O2 C1 C1 118.3(12) 87_365 87_365 ? N1 C2 C3 124.5(11) . . ? N1 C2 H2 117.7 . . ? C3 C2 H2 117.7 . . ? C2 C3 C4 119.0(12) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.8(12) . . ? C3 C4 C7 122.0(12) . . ? C5 C4 C7 118.3(13) . . ? C4 C5 C6 117.0(13) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? N1 C6 C5 123.8(12) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N2 C7 N2 127.8(14) . 35_465 ? N2 C7 C4 116.4(12) . . ? N2 C7 C4 115.5(15) 35_465 . ? C9 C8 C12 108.0 . . ? C9 C8 C13 126.0 . . ? C12 C8 C13 126.0 . . ? C9 C8 Ir1 69.8(3) . . ? C12 C8 Ir1 70.6(3) . . ? C13 C8 Ir1 125.3(7) . . ? C8 C9 C10 108.0 . . ? C8 C9 C14 126.0 . . ? C10 C9 C14 126.0 . . ? C8 C9 Ir1 71.5(3) . . ? C10 C9 Ir1 69.8(3) . . ? C14 C9 Ir1 124.3(9) . . ? C11 C10 C9 108.0 . . ? C11 C10 C15 126.0 . . ? C9 C10 C15 126.0 . . ? C11 C10 Ir1 70.9(3) . . ? C9 C10 Ir1 71.1(3) . . ? C15 C10 Ir1 123.7(8) . . ? C10 C11 C12 108.0 . . ? C10 C11 C16 126.0 . . ? C12 C11 C16 126.0 . . ? C10 C11 Ir1 70.0(3) . . ? C12 C11 Ir1 71.5(3) . . ? C16 C11 Ir1 124.1(8) . . ? C11 C12 C8 108.0 . . ? C11 C12 C17 126.0 . . ? C8 C12 C17 126.0 . . ? C11 C12 Ir1 69.7(3) . . ? C8 C12 Ir1 70.9(3) . . ? C17 C12 Ir1 125.0(9) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C2 N1 C6 115.8(11) . . ? C2 N1 Ir1 121.9(8) . . ? C6 N1 Ir1 121.9(9) . . ? C7 N2 C7 112.1(14) . 42_556 ? C1 O1 Ir1 113.5(6) . . ? C1 O2 Ir1 112.6(6) 87_365 . ? N1 Ir1 C10 130.3(5) . . ? N1 Ir1 O2 82.7(3) . . ? C10 Ir1 O2 146.9(4) . . ? N1 Ir1 C11 99.0(4) . . ? C10 Ir1 C11 39.2(4) . . ? O2 Ir1 C11 157.5(3) . . ? N1 Ir1 C9 163.6(4) . . ? C10 Ir1 C9 39.1(4) . . ? O2 Ir1 C9 109.8(3) . . ? C11 Ir1 C9 65.4(4) . . ? N1 Ir1 O1 84.0(3) . . ? C10 Ir1 O1 99.2(3) . . ? O2 Ir1 O1 78.4(2) . . ? C11 Ir1 O1 124.1(3) . . ? C9 Ir1 O1 108.5(4) . . ? N1 Ir1 C12 100.0(4) . . ? C10 Ir1 C12 65.3(4) . . ? O2 Ir1 C12 118.7(3) . . ? C11 Ir1 C12 38.8(4) . . ? C9 Ir1 C12 64.9(5) . . ? O1 Ir1 C12 162.7(3) . . ? N1 Ir1 C8 131.7(5) . . ? C10 Ir1 C8 65.2(4) . . ? O2 Ir1 C8 97.1(3) . . ? C11 Ir1 C8 65.0(4) . . ? C9 Ir1 C8 38.8(5) . . ? O1 Ir1 C8 143.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C2 C3 C4 C7 175.5(12) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C7 C4 C5 C6 -176.4(11) . . . . ? C4 C5 C6 N1 1(2) . . . . ? C3 C4 C7 N2 1.2(18) . . . . ? C5 C4 C7 N2 179.6(12) . . . . ? C3 C4 C7 N2 -172.9(12) . . . 35_465 ? C5 C4 C7 N2 5.5(18) . . . 35_465 ? C12 C8 C9 C10 0.0 . . . . ? C13 C8 C9 C10 180.0 . . . . ? Ir1 C8 C9 C10 -60.5(3) . . . . ? C12 C8 C9 C14 180.0 . . . . ? C13 C8 C9 C14 0.0 . . . . ? Ir1 C8 C9 C14 119.5(3) . . . . ? C12 C8 C9 Ir1 60.5(3) . . . . ? C13 C8 C9 Ir1 -119.5(3) . . . . ? C8 C9 C10 C11 0.0 . . . . ? C14 C9 C10 C11 180.0 . . . . ? Ir1 C9 C10 C11 -61.6(3) . . . . ? C8 C9 C10 C15 180.0 . . . . ? C14 C9 C10 C15 0.0 . . . . ? Ir1 C9 C10 C15 118.4(3) . . . . ? C8 C9 C10 Ir1 61.6(3) . . . . ? C14 C9 C10 Ir1 -118.4(3) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C15 C10 C11 C12 180.0 . . . . ? Ir1 C10 C11 C12 -61.8(3) . . . . ? C9 C10 C11 C16 180.0 . . . . ? C15 C10 C11 C16 0.0 . . . . ? Ir1 C10 C11 C16 118.2(3) . . . . ? C9 C10 C11 Ir1 61.8(3) . . . . ? C15 C10 C11 Ir1 -118.2(3) . . . . ? C10 C11 C12 C8 0.0 . . . . ? C16 C11 C12 C8 180.0 . . . . ? Ir1 C11 C12 C8 -60.8(3) . . . . ? C10 C11 C12 C17 180.0 . . . . ? C16 C11 C12 C17 0.0 . . . . ? Ir1 C11 C12 C17 119.2(3) . . . . ? C10 C11 C12 Ir1 60.8(3) . . . . ? C16 C11 C12 Ir1 -119.2(3) . . . . ? C9 C8 C12 C11 0.0 . . . . ? C13 C8 C12 C11 180.0 . . . . ? Ir1 C8 C12 C11 60.0(3) . . . . ? C9 C8 C12 C17 180.0 . . . . ? C13 C8 C12 C17 0.0 . . . . ? Ir1 C8 C12 C17 -120.0(3) . . . . ? C9 C8 C12 Ir1 -60.0(3) . . . . ? C13 C8 C12 Ir1 120.0(3) . . . . ? C3 C2 N1 C6 2.9(19) . . . . ? C3 C2 N1 Ir1 -169.6(10) . . . . ? C5 C6 N1 C2 -3.7(19) . . . . ? C5 C6 N1 Ir1 168.8(10) . . . . ? N2 C7 N2 C7 -4(2) 35_465 . . 42_556 ? C4 C7 N2 C7 -177.0(7) . . . 42_556 ? O2 C1 O1 Ir1 -170.3(7) 87_365 . . . ? C1 C1 O1 Ir1 5.7(6) 87_365 . . . ? C2 N1 Ir1 C10 128.9(9) . . . . ? C6 N1 Ir1 C10 -43.1(11) . . . . ? C2 N1 Ir1 O2 -55.0(9) . . . . ? C6 N1 Ir1 O2 133.0(9) . . . . ? C2 N1 Ir1 C11 102.3(9) . . . . ? C6 N1 Ir1 C11 -69.7(10) . . . . ? C2 N1 Ir1 C9 85.4(18) . . . . ? C6 N1 Ir1 C9 -86.6(19) . . . . ? C2 N1 Ir1 O1 -134.1(9) . . . . ? C6 N1 Ir1 O1 53.9(9) . . . . ? C2 N1 Ir1 C12 63.0(9) . . . . ? C6 N1 Ir1 C12 -109.1(9) . . . . ? C2 N1 Ir1 C8 37.9(11) . . . . ? C6 N1 Ir1 C8 -134.1(9) . . . . ? C11 C10 Ir1 N1 -44.4(6) . . . . ? C9 C10 Ir1 N1 -162.1(6) . . . . ? C15 C10 Ir1 N1 76.7(6) . . . . ? C11 C10 Ir1 O2 142.7(6) . . . . ? C9 C10 Ir1 O2 25.0(5) . . . . ? C15 C10 Ir1 O2 -96.2(6) . . . . ? C15 C10 Ir1 C11 121.1(11) . . . . ? C11 C10 Ir1 C9 117.6(9) . . . . ? C11 C10 Ir1 O1 -134.4(4) . . . . ? C9 C10 Ir1 O1 108.0(4) . . . . ? C15 C10 Ir1 O1 -13.3(5) . . . . ? C11 C10 Ir1 C12 37.6(6) . . . . ? C9 C10 Ir1 C12 -80.0(8) . . . . ? C11 C10 Ir1 C8 80.2(2) . . . . ? C9 C10 Ir1 C8 -37.5(8) . . . . ? C1 O2 Ir1 N1 -80.1(6) 87_365 . . . ? C1 O2 Ir1 C10 94.5(7) 87_365 . . . ? C1 O2 Ir1 C11 -176.0(9) 87_365 . . . ? C1 O2 Ir1 C9 110.9(7) 87_365 . . . ? C1 O2 Ir1 O1 5.3(6) 87_365 . . . ? C1 O2 Ir1 C12 -177.5(6) 87_365 . . . ? C1 O2 Ir1 C8 148.6(7) 87_365 . . . ? C10 C11 Ir1 N1 147.3(5) . . . . ? C12 C11 Ir1 N1 -94.8(5) . . . . ? C16 C11 Ir1 N1 26.7(5) . . . . ? C12 C11 Ir1 C10 117.9(8) . . . . ? C10 C11 Ir1 O2 -120.1(10) . . . . ? C12 C11 Ir1 O2 -2.2(10) . . . . ? C16 C11 Ir1 O2 119.3(9) . . . . ? C10 C11 Ir1 C9 -37.9(6) . . . . ? C12 C11 Ir1 C9 80.02(17) . . . . ? C10 C11 Ir1 O1 58.4(5) . . . . ? C12 C11 Ir1 O1 176.4(5) . . . . ? C16 C11 Ir1 O1 -62.2(5) . . . . ? C10 C11 Ir1 C12 -117.9(8) . . . . ? C10 C11 Ir1 C8 -80.7(2) . . . . ? C12 C11 Ir1 C8 37.1(6) . . . . ? C8 C9 Ir1 N1 -61.7(18) . . . . ? C10 C9 Ir1 N1 56.4(18) . . . . ? C14 C9 Ir1 N1 176.8(17) . . . . ? C8 C9 Ir1 C10 -118.1(10) . . . . ? C8 C9 Ir1 O2 76.1(3) . . . . ? C10 C9 Ir1 O2 -165.8(4) . . . . ? C14 C9 Ir1 O2 -45.3(4) . . . . ? C8 C9 Ir1 C11 -80.1(2) . . . . ? C10 C9 Ir1 C11 38.0(6) . . . . ? C8 C9 Ir1 O1 160.1(4) . . . . ? C10 C9 Ir1 O1 -81.8(4) . . . . ? C14 C9 Ir1 O1 38.7(4) . . . . ? C8 C9 Ir1 C12 -37.1(6) . . . . ? C10 C9 Ir1 C12 80.92(19) . . . . ? C10 C9 Ir1 C8 118.1(10) . . . . ? C1 O1 Ir1 N1 77.7(6) . . . . ? C1 O1 Ir1 C10 -152.4(7) . . . . ? C1 O1 Ir1 O2 -6.0(6) . . . . ? C1 O1 Ir1 C11 174.6(6) . . . . ? C1 O1 Ir1 C9 -113.2(7) . . . . ? C1 O1 Ir1 C12 -177.8(13) . . . . ? C1 O1 Ir1 C8 -92.2(7) . . . . ? C11 C12 Ir1 N1 92.0(4) . . . . ? C8 C12 Ir1 N1 -149.5(5) . . . . ? C17 C12 Ir1 N1 -28.4(5) . . . . ? C11 C12 Ir1 C10 -37.9(6) . . . . ? C8 C12 Ir1 C10 80.6(2) . . . . ? C11 C12 Ir1 O2 179.1(4) . . . . ? C8 C12 Ir1 O2 -62.4(4) . . . . ? C17 C12 Ir1 O2 58.7(4) . . . . ? C8 C12 Ir1 C11 118.6(8) . . . . ? C11 C12 Ir1 C9 -81.20(17) . . . . ? C8 C12 Ir1 C9 37.4(6) . . . . ? C11 C12 Ir1 O1 -10.2(14) . . . . ? C8 C12 Ir1 O1 108.3(15) . . . . ? C17 C12 Ir1 O1 -130.6(14) . . . . ? C11 C12 Ir1 C8 -118.6(8) . . . . ? C9 C8 Ir1 N1 160.6(5) . . . . ? C12 C8 Ir1 N1 42.0(5) . . . . ? C13 C8 Ir1 N1 -79.0(6) . . . . ? C9 C8 Ir1 C10 37.81(15) . . . . ? C12 C8 Ir1 C10 -80.8(2) . . . . ? C9 C8 Ir1 O2 -113.0(4) . . . . ? C12 C8 Ir1 O2 128.4(4) . . . . ? C13 C8 Ir1 O2 7.5(4) . . . . ? C9 C8 Ir1 C11 81.18(18) . . . . ? C12 C8 Ir1 C11 -37.43(15) . . . . ? C12 C8 Ir1 C9 -118.6(8) . . . . ? C9 C8 Ir1 O1 -32.9(5) . . . . ? C12 C8 Ir1 O1 -151.5(6) . . . . ? C13 C8 Ir1 O1 87.6(5) . . . . ? C9 C8 Ir1 C12 118.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.583 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.094 _vrf_CHEMW03_d_compound4 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The SQUEEZE option in PLATON03 was used to calculate the volume used by the extremely disordered anions. Therefore six triflate molecules were included per unit cell for all further calculations. ;