# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Self-assembled half-sandwich Ir, Rh-based organometallic molecular boxes: remarkable ability for molecular recognition of halide guests ; loop_ _publ_author_name 'Guo-Xin Jin' 'Ying-Feng Han' # Attachment 'Complex 2a.cif' data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 712011' #TrackingRef 'Complex 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 F6 Ir2 O14 S2' _chemical_formula_weight 1341.34 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.805(6) _cell_length_b 12.633(6) _cell_length_c 14.270(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.027(5) _cell_angle_gamma 90.00 _cell_volume 2352.8(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1001 _cell_measurement_theta_min 2.976 _cell_measurement_theta_max 22.952 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 5.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5415 _exptl_absorpt_correction_T_max 0.6529 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.14 _diffrn_reflns_number 10906 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.20 _reflns_number_total 5038 _reflns_number_gt 3003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5038 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.919457(17) 0.66144(2) 0.227258(16) 0.04161(8) Uani 1 1 d . . . O1 O 1.0504(3) 0.6218(3) 0.3375(3) 0.0420(10) Uani 1 1 d . . . O2 O 0.8451(3) 0.5878(3) 0.3120(2) 0.0425(10) Uani 1 1 d . . . O3 O 0.9461(4) 0.4977(4) 0.1929(4) 0.0659(14) Uani 1 1 d . . . H3 H 1.000(6) 0.490(8) 0.188(6) 0.12(4) Uiso 1 1 d . . . O4 O 0.4446(7) 0.6507(7) 0.2755(5) 0.202(4) Uani 1 1 d . . . O5 O 0.3094(6) 0.7737(7) 0.2224(7) 0.190(4) Uani 1 1 d . . . O6 O 0.2784(6) 0.5942(6) 0.1796(7) 0.171(3) Uani 1 1 d . . . S1 S 0.35086(19) 0.6759(2) 0.20797(16) 0.0855(6) Uani 1 1 d . . . F1 F 0.3028(6) 0.7190(7) 0.0254(5) 0.207(4) Uani 1 1 d . . . F2 F 0.4421(6) 0.7780(8) 0.1104(7) 0.219(4) Uani 1 1 d . . . F3 F 0.4278(9) 0.6163(9) 0.0785(7) 0.260(6) Uani 1 1 d . . . C1 C 1.3445(4) 0.5245(5) 0.4678(4) 0.0501(17) Uani 1 1 d . . . H1 H 1.3942 0.5408 0.4390 0.060 Uiso 1 1 calc R . . C2 C 1.2452(4) 0.5568(5) 0.4240(4) 0.0385(14) Uani 1 1 d . . . H2 H 1.2280 0.5955 0.3654 0.046 Uiso 1 1 calc R . . C3 C 1.1697(4) 0.5329(4) 0.4655(3) 0.0338(13) Uani 1 1 d . . . C4 C 1.0624(4) 0.5630(4) 0.4143(4) 0.0322(13) Uani 1 1 d . . . C5 C 0.9857(4) 0.5285(4) 0.4524(3) 0.0303(12) Uani 1 1 d . . . C6 C 0.8823(4) 0.5487(4) 0.3993(4) 0.0310(13) Uani 1 1 d . . . C7 C 0.8045(4) 0.5233(4) 0.4460(4) 0.0326(13) Uani 1 1 d . . . C8 C 0.7022(4) 0.5550(5) 0.4014(4) 0.0416(15) Uani 1 1 d . . . H8 H 0.6838 0.5917 0.3417 0.050 Uiso 1 1 calc R . . C9 C 0.6297(4) 0.5331(5) 0.4440(4) 0.0492(17) Uani 1 1 d . . . H9 H 0.5628 0.5565 0.4144 0.059 Uiso 1 1 calc R . . C10 C 0.8786(6) 0.4325(6) 0.1221(6) 0.096(3) Uani 1 1 d . . . H10A H 0.8115 0.4372 0.1282 0.143 Uiso 1 1 calc R . . H10B H 0.9022 0.3606 0.1325 0.143 Uiso 1 1 calc R . . H10C H 0.8758 0.4549 0.0570 0.143 Uiso 1 1 calc R . . C11 C 0.9719(5) 0.8081(5) 0.1883(4) 0.0495(17) Uani 1 1 d . . . C12 C 0.9334(5) 0.7464(5) 0.1024(4) 0.0555(18) Uani 1 1 d . . . C13 C 0.8272(5) 0.7254(5) 0.0877(4) 0.0566(18) Uani 1 1 d . . . C14 C 0.8027(5) 0.7750(5) 0.1653(5) 0.0544(18) Uani 1 1 d . . . C15 C 0.8923(5) 0.8234(5) 0.2299(4) 0.0514(17) Uani 1 1 d . . . C16 C 1.0810(5) 0.8479(6) 0.2306(5) 0.081(2) Uani 1 1 d . . . H16A H 1.1041 0.8407 0.3015 0.121 Uiso 1 1 calc R . . H16B H 1.0837 0.9211 0.2134 0.121 Uiso 1 1 calc R . . H16C H 1.1245 0.8072 0.2038 0.121 Uiso 1 1 calc R . . C17 C 0.9911(6) 0.7101(7) 0.0339(5) 0.091(3) Uani 1 1 d . . . H17A H 0.9828 0.7614 -0.0177 0.137 Uiso 1 1 calc R . . H17B H 0.9644 0.6431 0.0051 0.137 Uiso 1 1 calc R . . H17C H 1.0625 0.7028 0.0711 0.137 Uiso 1 1 calc R . . C18 C 0.7532(6) 0.6680(6) 0.0025(5) 0.101(3) Uani 1 1 d . . . H18A H 0.6940 0.6479 0.0197 0.152 Uiso 1 1 calc R . . H18B H 0.7853 0.6057 -0.0123 0.152 Uiso 1 1 calc R . . H18C H 0.7326 0.7134 -0.0545 0.152 Uiso 1 1 calc R . . C19 C 0.6986(5) 0.7719(7) 0.1796(6) 0.102(3) Uani 1 1 d . . . H19A H 0.7013 0.8112 0.2380 0.153 Uiso 1 1 calc R . . H19B H 0.6803 0.6998 0.1869 0.153 Uiso 1 1 calc R . . H19C H 0.6483 0.8028 0.1229 0.153 Uiso 1 1 calc R . . C20 C 0.9013(7) 0.8907(6) 0.3192(5) 0.105(3) Uani 1 1 d . . . H20A H 0.8778 0.9611 0.2982 0.158 Uiso 1 1 calc R . . H20B H 0.9716 0.8933 0.3610 0.158 Uiso 1 1 calc R . . H20C H 0.8602 0.8608 0.3554 0.158 Uiso 1 1 calc R . . C21 C 0.3823(9) 0.6969(11) 0.0975(9) 0.123(4) Uani 1 1 d . . . O7 O 0.1239(5) 0.4576(7) 0.1749(6) 0.088(2) Uani 1 1 d . . . H7A H 0.167(5) 0.504(5) 0.182(5) 0.06(3) Uiso 1 1 d . . . H7B H 0.146(8) 0.410(8) 0.209(8) 0.14(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.04494(13) 0.04603(15) 0.03219(11) 0.00976(15) 0.01029(9) 0.00332(16) O1 0.045(2) 0.050(3) 0.035(2) 0.0154(19) 0.0192(18) 0.0009(19) O2 0.036(2) 0.055(3) 0.034(2) 0.015(2) 0.0073(17) 0.004(2) O3 0.063(3) 0.063(4) 0.069(3) -0.015(3) 0.018(3) 0.000(3) O4 0.198(8) 0.236(10) 0.106(5) 0.060(6) -0.039(5) 0.056(8) O5 0.177(7) 0.135(7) 0.286(11) -0.085(7) 0.115(7) 0.022(6) O6 0.179(7) 0.136(6) 0.223(8) 0.012(6) 0.100(6) -0.071(6) S1 0.1034(17) 0.0814(18) 0.0805(14) 0.0078(14) 0.0418(13) -0.0026(15) F1 0.224(8) 0.233(9) 0.108(5) 0.062(5) -0.023(5) -0.015(7) F2 0.162(6) 0.241(9) 0.275(10) 0.127(8) 0.102(7) -0.030(7) F3 0.358(13) 0.288(13) 0.195(8) 0.029(8) 0.175(9) 0.150(11) C1 0.037(3) 0.065(5) 0.051(4) -0.004(4) 0.018(3) 0.000(3) C2 0.037(3) 0.049(4) 0.033(3) 0.003(3) 0.016(3) -0.004(3) C3 0.034(3) 0.037(4) 0.029(3) -0.001(3) 0.008(2) -0.002(3) C4 0.033(3) 0.030(3) 0.032(3) -0.006(3) 0.008(3) 0.001(3) C5 0.030(3) 0.033(3) 0.029(3) 0.003(2) 0.010(2) 0.000(3) C6 0.038(3) 0.022(3) 0.031(3) -0.002(2) 0.010(3) 0.002(3) C7 0.026(3) 0.035(3) 0.034(3) 0.001(3) 0.006(2) -0.001(3) C8 0.036(3) 0.051(4) 0.033(3) 0.005(3) 0.005(3) 0.004(3) C9 0.030(3) 0.067(5) 0.048(4) 0.002(4) 0.010(3) 0.008(3) C10 0.087(6) 0.076(6) 0.133(8) -0.026(6) 0.048(6) -0.015(5) C11 0.056(4) 0.044(5) 0.044(4) 0.017(3) 0.009(3) -0.003(3) C12 0.071(5) 0.057(5) 0.040(4) 0.020(3) 0.020(3) 0.010(4) C13 0.067(5) 0.048(4) 0.040(4) 0.010(3) -0.001(3) -0.001(4) C14 0.053(4) 0.052(5) 0.061(4) 0.027(4) 0.023(4) 0.019(4) C15 0.075(5) 0.040(4) 0.035(3) 0.003(3) 0.014(3) 0.008(4) C16 0.079(5) 0.080(6) 0.071(4) 0.031(5) 0.005(4) -0.008(5) C17 0.127(7) 0.096(7) 0.067(5) 0.024(5) 0.054(5) 0.015(6) C18 0.114(6) 0.084(6) 0.061(4) 0.010(5) -0.034(5) -0.014(6) C19 0.083(6) 0.086(7) 0.151(8) 0.057(6) 0.057(6) 0.033(5) C20 0.177(9) 0.075(6) 0.069(5) 0.007(5) 0.048(6) 0.031(6) C21 0.102(8) 0.133(12) 0.127(9) 0.046(9) 0.028(8) -0.004(8) O7 0.079(5) 0.074(5) 0.112(5) -0.023(5) 0.034(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O1 2.035(4) . ? Ir1 O2 2.047(4) . ? Ir1 C15 2.083(6) . ? Ir1 C14 2.123(6) . ? Ir1 C11 2.128(6) . ? Ir1 C12 2.142(6) . ? Ir1 C13 2.142(6) . ? Ir1 O3 2.184(6) . ? O1 C4 1.289(6) . ? O2 C6 1.282(5) . ? O3 C10 1.398(8) . ? O4 S1 1.375(7) . ? O5 S1 1.404(7) . ? O6 S1 1.402(7) . ? S1 C21 1.786(12) . ? F1 C21 1.266(11) . ? F2 C21 1.291(12) . ? F3 C21 1.271(13) . ? C1 C2 1.371(7) . ? C1 C9 1.396(7) 3_766 ? C2 C3 1.389(7) . ? C3 C7 1.389(7) 3_766 ? C3 C4 1.473(7) . ? C4 C5 1.408(7) . ? C5 C6 1.404(6) . ? C5 C5 1.472(9) 3_766 ? C6 C7 1.472(7) . ? C7 C3 1.389(7) 3_766 ? C7 C8 1.406(7) . ? C8 C9 1.358(7) . ? C9 C1 1.396(7) 3_766 ? C11 C12 1.403(8) . ? C11 C15 1.422(8) . ? C11 C16 1.514(8) . ? C12 C13 1.436(9) . ? C12 C17 1.520(9) . ? C13 C14 1.407(8) . ? C13 C18 1.496(8) . ? C14 C15 1.418(8) . ? C14 C19 1.517(8) . ? C15 C20 1.503(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ir1 O2 85.48(14) . . ? O1 Ir1 C15 110.3(2) . . ? O2 Ir1 C15 108.0(2) . . ? O1 Ir1 C14 148.3(2) . . ? O2 Ir1 C14 95.4(2) . . ? C15 Ir1 C14 39.4(2) . . ? O1 Ir1 C11 97.12(19) . . ? O2 Ir1 C11 146.0(2) . . ? C15 Ir1 C11 39.4(2) . . ? C14 Ir1 C11 65.1(2) . . ? O1 Ir1 C12 118.0(2) . . ? O2 Ir1 C12 156.6(2) . . ? C15 Ir1 C12 65.7(2) . . ? C14 Ir1 C12 65.0(2) . . ? C11 Ir1 C12 38.4(2) . . ? O1 Ir1 C13 157.1(2) . . ? O2 Ir1 C13 117.4(2) . . ? C15 Ir1 C13 65.8(2) . . ? C14 Ir1 C13 38.5(2) . . ? C11 Ir1 C13 65.1(2) . . ? C12 Ir1 C13 39.2(2) . . ? O1 Ir1 O3 76.60(17) . . ? O2 Ir1 O3 81.70(19) . . ? C15 Ir1 O3 168.2(2) . . ? C14 Ir1 O3 135.0(2) . . ? C11 Ir1 O3 132.0(2) . . ? C12 Ir1 O3 102.7(2) . . ? C13 Ir1 O3 103.9(2) . . ? C4 O1 Ir1 129.4(3) . . ? C6 O2 Ir1 129.1(3) . . ? C10 O3 Ir1 126.8(5) . . ? O4 S1 O6 116.8(6) . . ? O4 S1 O5 115.9(6) . . ? O6 S1 O5 113.8(5) . . ? O4 S1 C21 102.0(6) . . ? O6 S1 C21 102.1(6) . . ? O5 S1 C21 103.2(6) . . ? C2 C1 C9 119.3(5) . 3_766 ? C1 C2 C3 121.2(5) . . ? C7 C3 C2 119.5(5) 3_766 . ? C7 C3 C4 120.1(5) 3_766 . ? C2 C3 C4 120.3(5) . . ? O1 C4 C5 127.1(5) . . ? O1 C4 C3 113.6(5) . . ? C5 C4 C3 119.3(5) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 C5 120.4(5) . 3_766 ? C4 C5 C5 119.9(5) . 3_766 ? O2 C6 C5 127.5(5) . . ? O2 C6 C7 113.8(4) . . ? C5 C6 C7 118.6(4) . . ? C3 C7 C8 118.6(5) 3_766 . ? C3 C7 C6 120.9(4) 3_766 . ? C8 C7 C6 120.4(5) . . ? C9 C8 C7 121.2(5) . . ? C8 C9 C1 120.1(5) . 3_766 ? C12 C11 C15 108.4(6) . . ? C12 C11 C16 125.3(6) . . ? C15 C11 C16 126.3(6) . . ? C12 C11 Ir1 71.3(4) . . ? C15 C11 Ir1 68.6(4) . . ? C16 C11 Ir1 124.3(4) . . ? C11 C12 C13 108.0(6) . . ? C11 C12 C17 126.9(7) . . ? C13 C12 C17 125.0(6) . . ? C11 C12 Ir1 70.3(3) . . ? C13 C12 Ir1 70.4(3) . . ? C17 C12 Ir1 126.3(5) . . ? C14 C13 C12 107.3(6) . . ? C14 C13 C18 125.5(7) . . ? C12 C13 C18 127.1(7) . . ? C14 C13 Ir1 70.0(3) . . ? C12 C13 Ir1 70.4(3) . . ? C18 C13 Ir1 127.9(5) . . ? C13 C14 C15 108.8(6) . . ? C13 C14 C19 125.1(7) . . ? C15 C14 C19 126.0(7) . . ? C13 C14 Ir1 71.5(4) . . ? C15 C14 Ir1 68.8(3) . . ? C19 C14 Ir1 123.4(5) . . ? C14 C15 C11 107.4(5) . . ? C14 C15 C20 127.5(7) . . ? C11 C15 C20 124.7(6) . . ? C14 C15 Ir1 71.8(4) . . ? C11 C15 Ir1 72.0(4) . . ? C20 C15 Ir1 127.3(4) . . ? F1 C21 F3 111.2(13) . . ? F1 C21 F2 106.6(11) . . ? F3 C21 F2 109.2(12) . . ? F1 C21 S1 110.7(9) . . ? F3 C21 S1 110.4(9) . . ? F2 C21 S1 108.6(10) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.020 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.120 # Attachment 'Complex 2b.cif' data_complex_2b _database_code_depnum_ccdc_archive 'CCDC 712012' #TrackingRef 'Complex 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 F6 O14 Rh2 S2' _chemical_formula_weight 1162.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.82(3) _cell_length_b 12.55(2) _cell_length_c 14.20(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.12(3) _cell_angle_gamma 90.00 _cell_volume 2327(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 594 _cell_measurement_theta_min 2.413 _cell_measurement_theta_max 20.19 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9165 _exptl_absorpt_correction_T_max 0.9324 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9372 _diffrn_reflns_av_R_equivalents 0.1277 _diffrn_reflns_av_sigmaI/netI 0.1744 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4091 _reflns_number_gt 1540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4091 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1793 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2222 _refine_ls_wR_factor_gt 0.1834 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.91877(7) 0.33880(8) 0.22647(7) 0.0662(4) Uani 1 1 d . . . O1 O 0.8452(5) 0.4111(7) 0.3107(6) 0.072(2) Uani 1 1 d . . . O2 O 1.0499(6) 0.3771(6) 0.3376(6) 0.073(2) Uani 1 1 d . . . O3 O 0.9455(10) 0.4996(9) 0.1807(8) 0.095(3) Uani 1 1 d . . . C1 C 1.0632(9) 0.4327(8) 0.4168(8) 0.060(3) Uani 1 1 d . . . C2 C 0.9845(8) 0.4714(8) 0.4514(7) 0.048(3) Uani 1 1 d . . . C3 C 0.8829(9) 0.4504(8) 0.4009(8) 0.055(3) Uani 1 1 d . . . C4 C 0.8041(9) 0.4765(9) 0.4470(8) 0.056(3) Uani 1 1 d . . . C5 C 0.7035(9) 0.4411(9) 0.4026(9) 0.061(3) Uani 1 1 d . . . H5 H 0.6863 0.4012 0.3443 0.073 Uiso 1 1 calc R . . C6 C 0.6318(9) 0.4649(10) 0.4442(9) 0.073(4) Uani 1 1 d . . . H6 H 0.5646 0.4426 0.4137 0.088 Uiso 1 1 calc R . . C7 C 0.6574(10) 0.5232(10) 0.5336(10) 0.081(4) Uani 1 1 d . . . H7 H 0.6083 0.5381 0.5635 0.097 Uiso 1 1 calc R . . C8 C 0.7577(9) 0.5581(9) 0.5761(9) 0.069(3) Uani 1 1 d . . . H8 H 0.7757 0.6002 0.6331 0.083 Uiso 1 1 calc R . . C9 C 0.8300(8) 0.5305(8) 0.5339(8) 0.053(3) Uani 1 1 d . . . C10 C 0.9336(12) 0.2531(11) 0.1009(9) 0.085(4) Uani 1 1 d . . . C11 C 0.8236(11) 0.2767(12) 0.0861(11) 0.080(4) Uani 1 1 d . . . C12 C 0.8019(11) 0.2302(12) 0.1605(12) 0.088(4) Uani 1 1 d . . . C13 C 0.8925(11) 0.1752(10) 0.2285(9) 0.081(4) Uani 1 1 d . . . C14 C 0.9704(10) 0.1889(10) 0.1881(9) 0.074(4) Uani 1 1 d . . . C15 C 0.9888(12) 0.2964(13) 0.0365(11) 0.113(5) Uani 1 1 d . . . H15A H 0.9772 0.3718 0.0287 0.169 Uiso 1 1 calc R . . H15B H 0.9645 0.2625 -0.0276 0.169 Uiso 1 1 calc R . . H15C H 1.0608 0.2830 0.0664 0.169 Uiso 1 1 calc R . . C16 C 0.7523(11) 0.3349(12) 0.0039(10) 0.110(5) Uani 1 1 d . . . H16A H 0.7001 0.2873 -0.0349 0.165 Uiso 1 1 calc R . . H16B H 0.7884 0.3644 -0.0374 0.165 Uiso 1 1 calc R . . H16C H 0.7214 0.3914 0.0297 0.165 Uiso 1 1 calc R . . C17 C 0.7003(12) 0.2279(14) 0.1789(13) 0.127(6) Uani 1 1 d . . . H17A H 0.6614 0.2900 0.1500 0.191 Uiso 1 1 calc R . . H17B H 0.7119 0.2270 0.2493 0.191 Uiso 1 1 calc R . . H17C H 0.6632 0.1651 0.1490 0.191 Uiso 1 1 calc R . . C18 C 0.8985(14) 0.1120(12) 0.3243(10) 0.127(6) Uani 1 1 d . . . H18A H 0.8639 0.0450 0.3062 0.190 Uiso 1 1 calc R . . H18B H 0.8664 0.1524 0.3633 0.190 Uiso 1 1 calc R . . H18C H 0.9689 0.0995 0.3626 0.190 Uiso 1 1 calc R . . C19 C 1.0755(11) 0.1504(11) 0.2332(11) 0.111(5) Uani 1 1 d . . . H19A H 1.0937 0.1525 0.3045 0.166 Uiso 1 1 calc R . . H19B H 1.1213 0.1950 0.2126 0.166 Uiso 1 1 calc R . . H19C H 1.0802 0.0785 0.2122 0.166 Uiso 1 1 calc R . . C20 C 0.8802(14) 0.5725(17) 0.1321(15) 0.145(7) Uani 1 1 d . . . H20A H 0.8540 0.5540 0.0628 0.218 Uiso 1 1 calc R . . H20B H 0.9140 0.6403 0.1395 0.218 Uiso 1 1 calc R . . H20C H 0.8246 0.5766 0.1585 0.218 Uiso 1 1 calc R . . S1 S 0.6499(4) 0.6762(4) 0.7937(4) 0.1144(15) Uani 1 1 d . . . O4 O 0.5542(15) 0.6554(16) 0.7218(12) 0.255(10) Uani 1 1 d . . . O5 O 0.6933(13) 0.7700(13) 0.7813(15) 0.224(8) Uani 1 1 d . . . O6 O 0.7147(13) 0.5884(12) 0.8251(15) 0.231(9) Uani 1 1 d . . . C21 C 0.615(2) 0.6936(18) 0.903(2) 0.167(11) Uani 1 1 d . . . F1 F 0.5573(12) 0.7788(16) 0.8914(15) 0.257(9) Uani 1 1 d . . . F2 F 0.6962(15) 0.7172(16) 0.9750(11) 0.264(9) Uani 1 1 d . . . F3 F 0.5747(17) 0.6116(18) 0.9217(13) 0.291(11) Uani 1 1 d . . . O7 O 0.6283(9) 0.9575(11) 0.6752(9) 0.112(4) Uani 1 1 d . . . H1 H 1.003(9) 0.504(10) 0.205(9) 0.07(5) Uiso 1 1 d . . . H3 H 0.673(12) 1.044(14) 0.685(10) 0.14(6) Uiso 1 1 d . . . H2 H 0.689(10) 0.929(11) 0.712(10) 0.10(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0670(7) 0.0632(6) 0.0624(6) -0.0094(6) 0.0132(4) -0.0031(6) O1 0.045(5) 0.087(6) 0.073(5) -0.009(5) 0.006(4) -0.008(4) O2 0.067(5) 0.089(6) 0.067(5) -0.011(4) 0.028(4) 0.001(5) O3 0.072(8) 0.082(8) 0.117(8) 0.020(6) 0.013(7) 0.005(7) C1 0.071(8) 0.039(7) 0.066(8) -0.007(5) 0.016(6) 0.002(6) C2 0.046(6) 0.046(7) 0.052(6) -0.009(5) 0.015(5) -0.003(5) C3 0.063(8) 0.044(7) 0.053(7) -0.004(5) 0.013(6) -0.002(6) C4 0.064(8) 0.055(7) 0.049(6) -0.008(5) 0.019(6) 0.004(6) C5 0.056(8) 0.059(8) 0.066(8) -0.003(6) 0.018(6) -0.001(6) C6 0.049(8) 0.085(10) 0.076(9) -0.013(7) 0.008(7) -0.005(7) C7 0.072(9) 0.074(9) 0.090(10) 0.011(7) 0.018(8) 0.024(8) C8 0.064(9) 0.062(8) 0.070(8) 0.006(6) 0.006(7) -0.001(7) C9 0.053(7) 0.047(7) 0.063(7) 0.005(5) 0.022(6) 0.005(6) C10 0.105(12) 0.080(10) 0.057(8) -0.025(7) 0.011(8) -0.006(9) C11 0.070(10) 0.089(10) 0.073(9) -0.009(8) 0.014(8) -0.005(8) C12 0.069(10) 0.085(11) 0.098(11) -0.033(8) 0.009(9) 0.018(8) C13 0.108(11) 0.058(9) 0.070(8) -0.012(7) 0.021(8) -0.011(8) C14 0.069(9) 0.084(10) 0.064(8) -0.011(7) 0.015(7) 0.006(7) C15 0.132(13) 0.129(14) 0.095(11) -0.005(9) 0.060(10) -0.019(11) C16 0.112(11) 0.106(11) 0.079(9) -0.008(9) -0.014(8) 0.032(10) C17 0.110(13) 0.126(14) 0.169(17) -0.066(12) 0.076(12) -0.042(11) C18 0.209(18) 0.083(10) 0.087(10) 0.007(8) 0.048(12) -0.048(12) C19 0.107(12) 0.090(11) 0.107(10) -0.034(9) -0.004(9) 0.041(10) C20 0.126(15) 0.160(19) 0.173(19) 0.031(15) 0.079(14) 0.048(15) S1 0.141(4) 0.104(4) 0.111(3) -0.007(3) 0.059(3) 0.002(3) O4 0.223(16) 0.32(3) 0.147(12) -0.072(14) -0.043(12) -0.069(16) O5 0.216(17) 0.150(13) 0.33(2) 0.083(14) 0.123(16) -0.018(12) O6 0.203(15) 0.125(12) 0.38(3) -0.015(14) 0.114(16) 0.086(12) C21 0.17(2) 0.080(16) 0.20(3) -0.013(15) -0.01(2) -0.018(15) F1 0.216(16) 0.217(16) 0.36(2) -0.125(16) 0.124(16) 0.032(13) F2 0.261(19) 0.29(2) 0.172(13) -0.049(13) -0.025(13) 0.035(16) F3 0.46(3) 0.26(2) 0.218(17) -0.061(15) 0.194(19) -0.17(2) O7 0.098(9) 0.100(9) 0.128(9) -0.021(7) 0.025(8) 0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.021(8) . ? Rh1 O2 2.033(8) . ? Rh1 C12 2.086(14) . ? Rh1 C13 2.086(13) . ? Rh1 C11 2.144(13) . ? Rh1 C14 2.144(13) . ? Rh1 C10 2.149(13) . ? Rh1 O3 2.188(11) . ? O1 C3 1.311(12) . ? O2 C1 1.285(12) . ? O3 C20 1.311(18) . ? C1 C2 1.418(14) . ? C1 C9 1.486(15) 3_766 ? C2 C3 1.377(14) . ? C2 C2 1.488(19) 3_766 ? C3 C4 1.480(14) . ? C4 C9 1.349(14) . ? C4 C5 1.398(15) . ? C5 C6 1.344(15) . ? C6 C7 1.406(17) . ? C7 C8 1.390(16) . ? C8 C9 1.367(15) . ? C9 C1 1.486(15) 3_766 ? C10 C14 1.424(17) . ? C10 C15 1.473(18) . ? C10 C11 1.496(18) . ? C11 C12 1.325(19) . ? C11 C16 1.453(17) . ? C12 C13 1.478(18) . ? C12 C17 1.510(18) . ? C13 C14 1.386(17) . ? C13 C18 1.553(18) . ? C14 C19 1.464(16) . ? S1 O5 1.358(14) . ? S1 O6 1.398(14) . ? S1 O4 1.406(15) . ? S1 C21 1.78(3) . ? C21 F3 1.24(2) . ? C21 F2 1.28(2) . ? C21 F1 1.31(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh1 O2 85.9(3) . . ? O1 Rh1 C12 95.3(5) . . ? O2 Rh1 C12 149.9(5) . . ? O1 Rh1 C13 108.0(5) . . ? O2 Rh1 C13 109.7(4) . . ? C12 Rh1 C13 41.5(5) . . ? O1 Rh1 C11 116.0(5) . . ? O2 Rh1 C11 158.0(5) . . ? C12 Rh1 C11 36.5(5) . . ? C13 Rh1 C11 66.4(5) . . ? O1 Rh1 C14 144.8(5) . . ? O2 Rh1 C14 96.8(4) . . ? C12 Rh1 C14 65.6(5) . . ? C13 Rh1 C14 38.2(5) . . ? C11 Rh1 C14 66.4(5) . . ? O1 Rh1 C10 156.8(5) . . ? O2 Rh1 C10 117.3(5) . . ? C12 Rh1 C10 64.6(6) . . ? C13 Rh1 C10 65.4(5) . . ? C11 Rh1 C10 40.8(5) . . ? C14 Rh1 C10 38.8(5) . . ? O1 Rh1 O3 85.9(4) . . ? O2 Rh1 O3 79.5(4) . . ? C12 Rh1 O3 130.5(6) . . ? C13 Rh1 O3 163.4(5) . . ? C11 Rh1 O3 99.8(5) . . ? C14 Rh1 O3 129.1(5) . . ? C10 Rh1 O3 98.2(5) . . ? C3 O1 Rh1 129.1(7) . . ? C1 O2 Rh1 130.0(7) . . ? C20 O3 Rh1 130.2(12) . . ? O2 C1 C2 125.8(10) . . ? O2 C1 C9 114.6(10) . 3_766 ? C2 C1 C9 119.1(9) . 3_766 ? C3 C2 C1 121.4(9) . . ? C3 C2 C2 120.6(11) . 3_766 ? C1 C2 C2 117.8(11) . 3_766 ? O1 C3 C2 126.3(10) . . ? O1 C3 C4 113.6(10) . . ? C2 C3 C4 120.0(9) . . ? C9 C4 C5 119.9(10) . . ? C9 C4 C3 120.2(10) . . ? C5 C4 C3 119.8(9) . . ? C6 C5 C4 119.9(11) . . ? C5 C6 C7 120.6(12) . . ? C8 C7 C6 118.5(12) . . ? C9 C8 C7 119.9(12) . . ? C4 C9 C8 121.0(11) . . ? C4 C9 C1 120.8(10) . 3_766 ? C8 C9 C1 118.1(10) . 3_766 ? C14 C10 C15 129.7(14) . . ? C14 C10 C11 106.9(13) . . ? C15 C10 C11 123.3(13) . . ? C14 C10 Rh1 70.4(7) . . ? C15 C10 Rh1 122.7(10) . . ? C11 C10 Rh1 69.4(7) . . ? C12 C11 C16 126.3(15) . . ? C12 C11 C10 106.6(13) . . ? C16 C11 C10 127.1(14) . . ? C12 C11 Rh1 69.4(8) . . ? C16 C11 Rh1 127.8(10) . . ? C10 C11 Rh1 69.8(7) . . ? C11 C12 C13 111.3(13) . . ? C11 C12 C17 127.8(15) . . ? C13 C12 C17 121.0(16) . . ? C11 C12 Rh1 74.1(9) . . ? C13 C12 Rh1 69.3(7) . . ? C17 C12 Rh1 124.2(10) . . ? C14 C13 C12 106.2(12) . . ? C14 C13 C18 126.8(14) . . ? C12 C13 C18 127.0(15) . . ? C14 C13 Rh1 73.1(7) . . ? C12 C13 Rh1 69.2(8) . . ? C18 C13 Rh1 123.7(9) . . ? C13 C14 C10 109.0(12) . . ? C13 C14 C19 124.8(13) . . ? C10 C14 C19 126.0(14) . . ? C13 C14 Rh1 68.6(7) . . ? C10 C14 Rh1 70.8(7) . . ? C19 C14 Rh1 122.9(9) . . ? O5 S1 O6 117.4(11) . . ? O5 S1 O4 114.7(12) . . ? O6 S1 O4 115.9(12) . . ? O5 S1 C21 105.3(12) . . ? O6 S1 C21 98.4(12) . . ? O4 S1 C21 101.5(13) . . ? F3 C21 F2 111(3) . . ? F3 C21 F1 114(3) . . ? F2 C21 F1 105(2) . . ? F3 C21 S1 110.5(19) . . ? F2 C21 S1 108(2) . . ? F1 C21 S1 108.3(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.031 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.116 # Attachment 'Complex 3a.cif' data_complex_3a _database_code_depnum_ccdc_archive 'CCDC 712013' #TrackingRef 'Complex 3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H88 F12 Ir4 N4 O22 S4' _chemical_formula_weight 2678.66 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.073(4) _cell_length_b 13.532(4) _cell_length_c 16.805(5) _cell_angle_alpha 66.754(4) _cell_angle_beta 76.431(4) _cell_angle_gamma 75.778(4) _cell_volume 2615.9(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 830 _cell_measurement_theta_min 2.918 _cell_measurement_theta_max 22.444 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 5.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5722 _exptl_absorpt_correction_T_max 0.6794 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.30 _diffrn_reflns_number 10836 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8993 _reflns_number_gt 5468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8993 _refine_ls_number_parameters 575 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.925 _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 Ir1 Ir 0.72051(3) 0.53878(3) 0.29228(2) 0.04120(15) Uani 1 1 d . . . Ir2 Ir 0.78397(3) 0.79090(3) -0.26017(2) 0.03778(14) Uani 1 1 d . . . N1 N 0.8719(7) 0.4486(7) 0.2589(5) 0.042(2) Uani 1 1 d . . . N2 N 1.0677(6) 0.3182(6) 0.2451(5) 0.037(2) Uani 1 1 d . . . O1 O 0.7754(6) 0.6682(6) 0.1903(4) 0.0461(19) Uani 1 1 d . . . O2 O 0.6798(5) 0.5028(6) 0.1972(4) 0.0410(17) Uani 1 1 d . . . O3 O 0.7218(5) 0.6666(5) -0.1583(4) 0.0404(17) Uani 1 1 d . . . O4 O 0.8160(6) 0.8302(5) -0.1630(4) 0.0458(19) Uani 1 1 d . . . O5 O 0.6927(8) 0.1954(8) 0.3210(7) 0.102(4) Uani 1 1 d . . . O6 O 0.8420(8) 0.0924(9) 0.3935(7) 0.099(3) Uani 1 1 d . . . O7 O 0.6813(9) 0.0217(10) 0.4307(7) 0.125(4) Uani 1 1 d . . . O8 O 0.2579(16) 0.678(2) 0.2994(18) 0.413(19) Uiso 1 1 d D . . O9 O 0.146(2) 0.5464(15) 0.3325(17) 0.57(4) Uiso 1 1 d D . . O10 O 0.1643(18) 0.6708(19) 0.1836(9) 0.312(13) Uiso 1 1 d D . . F1 F 0.7163(11) 0.0245(12) 0.2512(8) 0.180(6) Uani 1 1 d . . . F2 F 0.8601(12) 0.0942(16) 0.2205(9) 0.235(9) Uani 1 1 d . . . F3 F 0.8454(10) -0.0752(15) 0.3219(13) 0.226(8) Uani 1 1 d . . . F4 F 0.0862(14) 0.8388(14) 0.2528(11) 0.262(8) Uiso 1 1 d D . . F5 F 0.0578(15) 0.7316(16) 0.3793(11) 0.298(9) Uiso 1 1 d D . . F6 F -0.0184(17) 0.7362(19) 0.2753(14) 0.369(13) Uiso 1 1 d D . . S1 S 0.7480(3) 0.0901(3) 0.3657(2) 0.0646(9) Uani 1 1 d D . . S2 S 0.1872(6) 0.6418(9) 0.2697(7) 0.234(5) Uani 1 1 d D . . C1 C 0.7700(8) 0.7036(8) 0.1073(6) 0.040(3) Uani 1 1 d . . . C2 C 0.7400(7) 0.6462(8) 0.0638(6) 0.031(2) Uani 1 1 d . . . C3 C 0.6974(7) 0.5511(8) 0.1125(6) 0.037(3) Uani 1 1 d . . . C4 C 0.6664(8) 0.4895(9) 0.0673(6) 0.043(3) Uani 1 1 d . . . C5 C 0.6311(10) 0.3912(10) 0.1141(7) 0.061(4) Uani 1 1 d . . . H5 H 0.6250 0.3628 0.1749 0.073 Uiso 1 1 calc R . . C6 C 0.6048(12) 0.3348(11) 0.0708(8) 0.079(5) Uani 1 1 d . . . H6 H 0.5807 0.2689 0.1032 0.095 Uiso 1 1 calc R . . C7 C 0.6136(12) 0.3738(12) -0.0180(9) 0.089(5) Uani 1 1 d . . . H7 H 0.5964 0.3347 -0.0464 0.106 Uiso 1 1 calc R . . C8 C 0.6491(10) 0.4748(12) -0.0666(8) 0.079(4) Uani 1 1 d . . . H8 H 0.6546 0.5020 -0.1273 0.095 Uiso 1 1 calc R . . C9 C 0.6768(8) 0.5360(9) -0.0246(6) 0.042(3) Uani 1 1 d . . . C10 C 0.7200(8) 0.6361(9) -0.0755(7) 0.039(3) Uani 1 1 d . . . C11 C 0.7514(7) 0.6906(8) -0.0314(6) 0.032(2) Uani 1 1 d . . . C12 C 0.7936(7) 0.7859(8) -0.0783(6) 0.037(2) Uani 1 1 d . . . C13 C 0.8152(9) 0.8470(8) -0.0312(7) 0.048(3) Uani 1 1 d . . . C14 C 0.8448(12) 0.9499(11) -0.0790(8) 0.085(5) Uani 1 1 d . . . H14 H 0.8499 0.9778 -0.1397 0.102 Uiso 1 1 calc R . . C15 C 0.8666(15) 1.0098(13) -0.0372(10) 0.124(7) Uani 1 1 d . . . H15 H 0.8855 1.0784 -0.0681 0.149 Uiso 1 1 calc R . . C16 C 0.8586(14) 0.9613(16) 0.0568(10) 0.119(7) Uani 1 1 d . . . H16 H 0.8749 0.9988 0.0869 0.143 Uiso 1 1 calc R . . C17 C 0.8287(11) 0.8645(9) 0.1019(8) 0.067(4) Uani 1 1 d . . . H17 H 0.8244 0.8347 0.1626 0.081 Uiso 1 1 calc R . . C18 C 0.8045(9) 0.8101(9) 0.0582(7) 0.048(3) Uani 1 1 d . . . C19 C 0.8821(9) 0.3455(9) 0.2601(7) 0.045(3) Uani 1 1 d . . . H19 H 0.8214 0.3163 0.2681 0.054 Uiso 1 1 calc R . . C20 C 0.9779(8) 0.2866(8) 0.2499(6) 0.038(3) Uani 1 1 d . . . H20 H 0.9822 0.2190 0.2459 0.046 Uiso 1 1 calc R . . C21 C 1.0621(9) 0.4184(10) 0.2410(7) 0.050(3) Uani 1 1 d . . . H21 H 1.1238 0.4458 0.2334 0.060 Uiso 1 1 calc R . . C22 C 0.9614(9) 0.4829(9) 0.2485(7) 0.047(3) Uani 1 1 d . . . H22 H 0.9577 0.5536 0.2459 0.057 Uiso 1 1 calc R . . C23 C 0.7291(14) 0.5328(16) 0.4186(8) 0.097(6) Uani 1 1 d . . . C24 C 0.6658(15) 0.6319(10) 0.3777(9) 0.078(5) Uani 1 1 d . . . C25 C 0.5770(12) 0.6056(14) 0.3585(9) 0.081(5) Uani 1 1 d . . . C26 C 0.5898(12) 0.4814(14) 0.3927(8) 0.075(4) Uani 1 1 d . . . C27 C 0.6866(12) 0.4412(12) 0.4274(7) 0.065(4) Uani 1 1 d . . . C28 C 0.8383(15) 0.516(3) 0.4520(12) 0.245(18) Uani 1 1 d . . . H28A H 0.8673 0.5824 0.4246 0.368 Uiso 1 1 calc R . . H28B H 0.8880 0.4584 0.4372 0.368 Uiso 1 1 calc R . . H28C H 0.8255 0.4971 0.5145 0.368 Uiso 1 1 calc R . . C29 C 0.6892(17) 0.7427(12) 0.3583(11) 0.155(10) Uani 1 1 d . . . H29A H 0.6740 0.7579 0.4115 0.233 Uiso 1 1 calc R . . H29B H 0.6454 0.7966 0.3170 0.233 Uiso 1 1 calc R . . H29C H 0.7631 0.7448 0.3339 0.233 Uiso 1 1 calc R . . C30 C 0.4865(14) 0.6771(17) 0.3200(13) 0.174(11) Uani 1 1 d . . . H30A H 0.5080 0.7131 0.2583 0.261 Uiso 1 1 calc R . . H30B H 0.4585 0.7307 0.3472 0.261 Uiso 1 1 calc R . . H30C H 0.4324 0.6355 0.3286 0.261 Uiso 1 1 calc R . . C31 C 0.5176(15) 0.412(2) 0.3889(12) 0.186(12) Uani 1 1 d . . . H31A H 0.4654 0.3966 0.4410 0.280 Uiso 1 1 calc R . . H31B H 0.5596 0.3445 0.3848 0.280 Uiso 1 1 calc R . . H31C H 0.4822 0.4503 0.3384 0.280 Uiso 1 1 calc R . . C32 C 0.7308(16) 0.3239(11) 0.4707(8) 0.140(9) Uani 1 1 d . . . H32A H 0.6908 0.2793 0.4619 0.211 Uiso 1 1 calc R . . H32B H 0.7258 0.3077 0.5324 0.211 Uiso 1 1 calc R . . H32C H 0.8043 0.3092 0.4458 0.211 Uiso 1 1 calc R . . C33 C 0.7338(17) 0.8000(10) -0.3748(10) 0.079(5) Uani 1 1 d . . . C34 C 0.6502(10) 0.8483(16) -0.3282(9) 0.076(5) Uani 1 1 d . . . C35 C 0.6878(15) 0.9378(12) -0.3239(9) 0.090(6) Uani 1 1 d . . . C36 C 0.7950(13) 0.9320(12) -0.3716(10) 0.080(5) Uani 1 1 d . . . C37 C 0.8206(12) 0.8502(13) -0.4004(8) 0.068(4) Uani 1 1 d . . . C38 C 0.727(3) 0.7083(18) -0.3992(16) 0.28(2) Uani 1 1 d . . . H38A H 0.7012 0.7366 -0.4544 0.424 Uiso 1 1 calc R . . H38B H 0.6784 0.6643 -0.3549 0.424 Uiso 1 1 calc R . . H38C H 0.7962 0.6644 -0.4040 0.424 Uiso 1 1 calc R . . C39 C 0.5460(13) 0.8138(18) -0.2906(13) 0.184(12) Uani 1 1 d . . . H39A H 0.4981 0.8503 -0.3329 0.276 Uiso 1 1 calc R . . H39B H 0.5174 0.8323 -0.2392 0.276 Uiso 1 1 calc R . . H39C H 0.5542 0.7363 -0.2751 0.276 Uiso 1 1 calc R . . C40 C 0.624(2) 1.022(3) -0.2832(15) 0.40(3) Uani 1 1 d . . . H40A H 0.5874 1.0823 -0.3262 0.605 Uiso 1 1 calc R . . H40B H 0.6721 1.0482 -0.2636 0.605 Uiso 1 1 calc R . . H40C H 0.5731 0.9890 -0.2342 0.605 Uiso 1 1 calc R . . C41 C 0.866(2) 1.024(3) -0.3888(15) 0.32(2) Uani 1 1 d . . . H41A H 0.8583 1.0810 -0.4448 0.485 Uiso 1 1 calc R . . H41B H 0.9401 0.9913 -0.3880 0.485 Uiso 1 1 calc R . . H41C H 0.8423 1.0553 -0.3437 0.485 Uiso 1 1 calc R . . C42 C 0.9269(14) 0.8216(16) -0.4539(9) 0.151(9) Uani 1 1 d . . . H42A H 0.9493 0.7438 -0.4333 0.227 Uiso 1 1 calc R . . H42B H 0.9796 0.8554 -0.4476 0.227 Uiso 1 1 calc R . . H42C H 0.9190 0.8475 -0.5145 0.227 Uiso 1 1 calc R . . C43 C 0.7990(17) 0.033(2) 0.2808(14) 0.119(7) Uani 1 1 d D . . C44 C 0.0705(13) 0.7380(14) 0.2979(12) 0.228(13) Uiso 1 1 d D . . O11 O 0.4908(11) 0.1146(11) 0.5314(9) 0.153(5) 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 Ir1 0.0496(3) 0.0442(3) 0.0258(2) -0.0123(2) -0.0020(2) -0.0050(2) Ir2 0.0403(3) 0.0409(3) 0.0267(2) -0.0048(2) -0.00561(18) -0.0092(2) N1 0.044(5) 0.044(6) 0.030(5) -0.005(4) -0.009(4) -0.001(5) N2 0.044(5) 0.023(5) 0.037(5) 0.001(4) -0.014(4) -0.006(4) O1 0.063(5) 0.055(5) 0.026(4) -0.013(3) -0.007(3) -0.020(4) O2 0.050(4) 0.050(5) 0.023(4) -0.008(3) -0.008(3) -0.015(4) O3 0.056(5) 0.041(4) 0.023(4) -0.005(3) -0.007(3) -0.017(4) O4 0.075(5) 0.034(4) 0.033(4) -0.010(3) -0.006(4) -0.022(4) O5 0.085(7) 0.057(6) 0.150(10) -0.020(6) -0.047(7) 0.009(6) O6 0.085(7) 0.115(9) 0.104(8) -0.034(7) -0.035(6) -0.021(6) O7 0.125(9) 0.151(11) 0.076(8) -0.018(7) 0.010(7) -0.049(9) F1 0.176(12) 0.277(17) 0.170(11) -0.162(12) 0.003(9) -0.078(12) F2 0.216(14) 0.42(3) 0.155(11) -0.188(15) 0.122(11) -0.212(17) F3 0.116(10) 0.218(16) 0.42(3) -0.224(18) -0.044(13) 0.035(11) S1 0.061(2) 0.070(2) 0.063(2) -0.0209(19) -0.0098(17) -0.0166(19) S2 0.151(6) 0.339(13) 0.315(12) -0.246(12) -0.059(7) 0.016(8) C1 0.045(6) 0.042(7) 0.033(6) -0.015(5) -0.004(5) -0.004(5) C2 0.031(5) 0.033(6) 0.029(6) -0.008(5) -0.005(4) -0.007(5) C3 0.031(6) 0.049(7) 0.024(5) -0.010(5) -0.002(4) -0.005(5) C4 0.041(6) 0.063(8) 0.026(6) -0.013(5) 0.002(5) -0.023(6) C5 0.086(9) 0.063(8) 0.032(6) -0.001(6) -0.002(6) -0.042(8) C6 0.141(13) 0.073(10) 0.033(7) -0.002(7) -0.009(7) -0.068(10) C7 0.145(14) 0.087(11) 0.058(9) -0.025(8) 0.002(9) -0.081(11) C8 0.095(10) 0.127(13) 0.042(7) -0.045(8) 0.012(7) -0.066(10) C9 0.036(6) 0.065(8) 0.030(6) -0.017(5) 0.001(5) -0.021(6) C10 0.031(6) 0.055(7) 0.036(6) -0.021(6) -0.002(5) -0.009(5) C11 0.024(5) 0.031(6) 0.040(6) -0.012(5) -0.005(4) -0.004(5) C12 0.032(6) 0.044(7) 0.032(6) -0.012(5) -0.003(4) -0.007(5) C13 0.079(8) 0.022(6) 0.040(7) -0.006(5) -0.002(6) -0.023(6) C14 0.144(14) 0.091(11) 0.039(8) -0.024(8) 0.006(8) -0.070(11) C15 0.24(2) 0.107(13) 0.070(11) -0.026(10) -0.010(12) -0.126(15) C16 0.175(18) 0.176(19) 0.061(10) -0.059(12) 0.002(10) -0.115(15) C17 0.132(12) 0.030(7) 0.044(7) 0.003(6) -0.020(7) -0.046(8) C18 0.074(8) 0.036(7) 0.036(6) -0.012(5) -0.002(6) -0.021(6) C19 0.050(7) 0.041(7) 0.050(7) -0.020(6) -0.003(5) -0.017(6) C20 0.046(7) 0.020(6) 0.045(6) -0.008(5) -0.010(5) -0.002(5) C21 0.045(7) 0.065(9) 0.051(7) -0.026(6) -0.009(5) -0.015(6) C22 0.056(8) 0.038(7) 0.055(7) -0.015(6) -0.014(6) -0.017(6) C23 0.146(15) 0.141(16) 0.028(7) -0.059(10) 0.035(8) -0.065(14) C24 0.124(14) 0.026(8) 0.051(8) -0.009(6) 0.024(9) 0.001(8) C25 0.055(9) 0.102(13) 0.058(9) -0.031(9) 0.022(7) 0.012(9) C26 0.069(10) 0.106(13) 0.040(8) -0.032(8) 0.034(7) -0.030(9) C27 0.099(11) 0.075(10) 0.021(6) -0.020(6) 0.011(6) -0.026(9) C28 0.145(18) 0.59(6) 0.123(17) -0.21(3) -0.009(14) -0.15(3) C29 0.26(3) 0.061(11) 0.106(14) -0.045(11) 0.068(15) -0.032(14) C30 0.106(15) 0.18(2) 0.145(19) -0.038(16) 0.014(14) 0.065(15) C31 0.137(17) 0.37(4) 0.157(19) -0.19(2) 0.079(14) -0.16(2) C32 0.28(3) 0.040(9) 0.040(9) 0.009(7) -0.007(12) 0.015(13) C33 0.143(15) 0.039(8) 0.062(10) 0.004(7) -0.076(10) -0.008(10) C34 0.038(8) 0.109(14) 0.050(8) 0.018(9) -0.020(6) -0.022(8) C35 0.119(14) 0.061(10) 0.049(9) -0.005(7) -0.045(9) 0.061(10) C36 0.093(12) 0.053(10) 0.059(9) 0.039(8) -0.036(9) -0.027(9) C37 0.087(11) 0.059(10) 0.045(8) -0.013(7) -0.013(7) 0.002(9) C38 0.61(6) 0.120(19) 0.21(3) -0.032(18) -0.30(4) -0.05(3) C39 0.073(12) 0.21(2) 0.158(18) 0.078(17) -0.036(12) -0.043(14) C40 0.39(4) 0.58(6) 0.16(2) -0.27(3) -0.20(3) 0.42(5) C41 0.44(5) 0.48(5) 0.15(2) 0.01(3) -0.10(3) -0.40(4) C42 0.135(15) 0.172(19) 0.040(9) 0.003(10) 0.032(9) 0.049(14) C43 0.104(16) 0.133(18) 0.16(2) -0.089(17) -0.020(15) -0.029(15) O11 0.175(13) 0.151(12) 0.149(12) -0.083(10) 0.019(10) -0.047(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 Ir1 O1 2.047(7) . ? Ir1 O2 2.053(6) . ? Ir1 C23 2.121(12) . ? Ir1 C27 2.132(11) . ? Ir1 N1 2.134(8) . ? Ir1 C25 2.135(12) . ? Ir1 C26 2.153(11) . ? Ir1 C24 2.159(13) . ? Ir2 O3 2.041(6) . ? Ir2 O4 2.060(7) . ? Ir2 C36 2.088(11) . ? Ir2 C35 2.099(11) . ? Ir2 C33 2.126(12) . ? Ir2 N2 2.129(8) 2_765 ? Ir2 C34 2.130(12) . ? Ir2 C37 2.144(13) . ? N1 C22 1.312(12) . ? N1 C19 1.361(13) . ? N2 C21 1.315(13) . ? N2 C20 1.320(12) . ? N2 Ir2 2.129(8) 2_765 ? O1 C1 1.298(11) . ? O2 C3 1.301(10) . ? O3 C10 1.283(11) . ? O4 C12 1.299(11) . ? O5 S1 1.421(9) . ? O6 S1 1.425(9) . ? O7 S1 1.402(10) . ? O8 S2 1.405(9) . ? O9 S2 1.437(9) . ? O10 S2 1.427(9) . ? F1 C43 1.34(2) . ? F2 C43 1.28(2) . ? F3 C43 1.40(2) . ? F4 C44 1.314(10) . ? F5 C44 1.309(10) . ? F6 C44 1.314(10) . ? S1 C43 1.803(15) . ? S2 C44 1.849(14) . ? C1 C2 1.423(13) . ? C1 C18 1.472(14) . ? C2 C3 1.394(13) . ? C2 C11 1.455(12) . ? C3 C4 1.499(14) . ? C4 C5 1.381(14) . ? C4 C9 1.406(13) . ? C5 C6 1.382(16) . ? C6 C7 1.360(16) . ? C7 C8 1.415(17) . ? C8 C9 1.430(15) . ? C9 C10 1.456(14) . ? C10 C11 1.408(13) . ? C11 C12 1.390(13) . ? C12 C13 1.458(14) . ? C13 C18 1.368(14) . ? C13 C14 1.403(15) . ? C14 C15 1.375(17) . ? C15 C16 1.440(19) . ? C16 C17 1.331(18) . ? C17 C18 1.353(14) . ? C19 C20 1.322(13) . ? C21 C22 1.398(14) . ? C23 C24 1.40(2) . ? C23 C27 1.422(19) . ? C23 C28 1.59(2) . ? C24 C25 1.43(2) . ? C24 C29 1.50(2) . ? C25 C30 1.43(2) . ? C25 C26 1.53(2) . ? C26 C27 1.412(18) . ? C26 C31 1.51(2) . ? C27 C32 1.489(17) . ? C33 C37 1.36(2) . ? C33 C34 1.37(2) . ? C33 C38 1.48(2) . ? C34 C35 1.45(2) . ? C34 C39 1.466(18) . ? C35 C36 1.44(2) . ? C35 C40 1.53(2) . ? C36 C37 1.32(2) . ? C36 C41 1.64(2) . ? C37 C42 1.521(18) . ? 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 Ir1 O2 85.1(3) . . ? O1 Ir1 C23 114.9(5) . . ? O2 Ir1 C23 159.6(5) . . ? O1 Ir1 C27 154.0(4) . . ? O2 Ir1 C27 120.9(4) . . ? C23 Ir1 C27 39.1(5) . . ? O1 Ir1 N1 84.4(3) . . ? O2 Ir1 N1 82.6(3) . . ? C23 Ir1 N1 102.5(6) . . ? C27 Ir1 N1 99.3(5) . . ? O1 Ir1 C25 106.2(5) . . ? O2 Ir1 C25 107.7(5) . . ? C23 Ir1 C25 64.4(6) . . ? C27 Ir1 C25 66.9(5) . . ? N1 Ir1 C25 165.6(5) . . ? O1 Ir1 C26 146.8(5) . . ? O2 Ir1 C26 96.6(5) . . ? C23 Ir1 C26 64.6(6) . . ? C27 Ir1 C26 38.5(5) . . ? N1 Ir1 C26 128.8(5) . . ? C25 Ir1 C26 41.7(5) . . ? O1 Ir1 C24 92.4(4) . . ? O2 Ir1 C24 144.0(6) . . ? C23 Ir1 C24 38.1(6) . . ? C27 Ir1 C24 66.2(5) . . ? N1 Ir1 C24 133.0(6) . . ? C25 Ir1 C24 38.9(6) . . ? C26 Ir1 C24 67.0(6) . . ? O3 Ir2 O4 84.4(3) . . ? O3 Ir2 C36 160.9(5) . . ? O4 Ir2 C36 104.3(5) . . ? O3 Ir2 C35 122.1(6) . . ? O4 Ir2 C35 99.4(5) . . ? C36 Ir2 C35 40.3(6) . . ? O3 Ir2 C33 106.9(5) . . ? O4 Ir2 C33 163.2(4) . . ? C36 Ir2 C33 61.4(6) . . ? C35 Ir2 C33 64.2(6) . . ? O3 Ir2 N2 84.7(3) . 2_765 ? O4 Ir2 N2 84.6(3) . 2_765 ? C36 Ir2 N2 112.7(5) . 2_765 ? C35 Ir2 N2 153.0(6) . 2_765 ? C33 Ir2 N2 108.4(6) . 2_765 ? O3 Ir2 C34 96.3(4) . . ? O4 Ir2 C34 130.6(6) . . ? C36 Ir2 C34 65.1(5) . . ? C35 Ir2 C34 40.0(6) . . ? C33 Ir2 C34 37.6(5) . . ? N2 Ir2 C34 144.7(6) 2_765 . ? O3 Ir2 C37 140.7(5) . . ? O4 Ir2 C37 134.6(5) . . ? C36 Ir2 C37 36.3(5) . . ? C35 Ir2 C37 65.2(5) . . ? C33 Ir2 C37 37.2(5) . . ? N2 Ir2 C37 92.9(4) 2_765 . ? C34 Ir2 C37 64.3(5) . . ? C22 N1 C19 115.9(9) . . ? C22 N1 Ir1 121.6(8) . . ? C19 N1 Ir1 121.7(7) . . ? C21 N2 C20 117.9(9) . . ? C21 N2 Ir2 118.8(7) . 2_765 ? C20 N2 Ir2 122.9(7) . 2_765 ? C1 O1 Ir1 130.9(7) . . ? C3 O2 Ir1 128.8(6) . . ? C10 O3 Ir2 130.8(6) . . ? C12 O4 Ir2 130.1(6) . . ? O7 S1 O5 113.4(7) . . ? O7 S1 O6 114.1(7) . . ? O5 S1 O6 113.7(6) . . ? O7 S1 C43 107.5(9) . . ? O5 S1 C43 103.4(10) . . ? O6 S1 C43 103.5(8) . . ? O8 S2 O10 130.6(13) . . ? O8 S2 O9 114.7(13) . . ? O10 S2 O9 113.6(12) . . ? O8 S2 C44 93.3(10) . . ? O10 S2 C44 93.2(10) . . ? O9 S2 C44 94.1(11) . . ? O1 C1 C2 125.6(9) . . ? O1 C1 C18 113.2(9) . . ? C2 C1 C18 121.1(9) . . ? C3 C2 C1 120.0(9) . . ? C3 C2 C11 121.2(8) . . ? C1 C2 C11 118.8(8) . . ? O2 C3 C2 128.7(9) . . ? O2 C3 C4 110.9(9) . . ? C2 C3 C4 120.4(8) . . ? C5 C4 C9 122.1(10) . . ? C5 C4 C3 121.3(9) . . ? C9 C4 C3 116.6(9) . . ? C4 C5 C6 120.2(11) . . ? C7 C6 C5 121.3(12) . . ? C6 C7 C8 118.9(12) . . ? C7 C8 C9 121.7(11) . . ? C4 C9 C8 115.8(10) . . ? C4 C9 C10 122.9(10) . . ? C8 C9 C10 121.2(10) . . ? O3 C10 C11 126.9(10) . . ? O3 C10 C9 113.9(9) . . ? C11 C10 C9 119.2(9) . . ? C12 C11 C10 120.5(9) . . ? C12 C11 C2 120.0(9) . . ? C10 C11 C2 119.6(9) . . ? O4 C12 C11 126.8(9) . . ? O4 C12 C13 113.7(9) . . ? C11 C12 C13 119.4(9) . . ? C18 C13 C14 118.1(10) . . ? C18 C13 C12 122.9(9) . . ? C14 C13 C12 119.0(10) . . ? C15 C14 C13 120.9(12) . . ? C14 C15 C16 116.8(13) . . ? C17 C16 C15 122.1(13) . . ? C16 C17 C18 119.0(12) . . ? C17 C18 C13 123.0(10) . . ? C17 C18 C1 119.7(10) . . ? C13 C18 C1 117.3(10) . . ? C20 C19 N1 120.3(10) . . ? N2 C20 C19 123.8(10) . . ? N2 C21 C22 118.5(10) . . ? N1 C22 C21 123.2(10) . . ? C24 C23 C27 112.5(16) . . ? C24 C23 C28 127.1(19) . . ? C27 C23 C28 120(2) . . ? C24 C23 Ir1 72.5(8) . . ? C27 C23 Ir1 70.9(7) . . ? C28 C23 Ir1 123.4(10) . . ? C23 C24 C25 106.7(13) . . ? C23 C24 C29 125.4(19) . . ? C25 C24 C29 127.9(17) . . ? C23 C24 Ir1 69.5(7) . . ? C25 C24 Ir1 69.6(8) . . ? C29 C24 Ir1 125.5(9) . . ? C24 C25 C30 129.3(19) . . ? C24 C25 C26 107.2(13) . . ? C30 C25 C26 123.4(18) . . ? C24 C25 Ir1 71.5(7) . . ? C30 C25 Ir1 126.9(11) . . ? C26 C25 Ir1 69.8(7) . . ? C27 C26 C31 125.3(17) . . ? C27 C26 C25 106.2(13) . . ? C31 C26 C25 128.4(17) . . ? C27 C26 Ir1 69.9(7) . . ? C31 C26 Ir1 124.7(10) . . ? C25 C26 Ir1 68.5(7) . . ? C26 C27 C23 107.5(14) . . ? C26 C27 C32 125.5(15) . . ? C23 C27 C32 126.9(16) . . ? C26 C27 Ir1 71.6(7) . . ? C23 C27 Ir1 70.1(7) . . ? C32 C27 Ir1 127.0(9) . . ? C37 C33 C34 112.5(13) . . ? C37 C33 C38 124(2) . . ? C34 C33 C38 123(2) . . ? C37 C33 Ir2 72.1(8) . . ? C34 C33 Ir2 71.4(8) . . ? C38 C33 Ir2 127.6(10) . . ? C33 C34 C35 105.5(12) . . ? C33 C34 C39 126(2) . . ? C35 C34 C39 128(2) . . ? C33 C34 Ir2 71.0(7) . . ? C35 C34 Ir2 68.8(7) . . ? C39 C34 Ir2 124.0(10) . . ? C36 C35 C34 103.5(13) . . ? C36 C35 C40 129(3) . . ? C34 C35 C40 127(2) . . ? C36 C35 Ir2 69.5(7) . . ? C34 C35 Ir2 71.2(7) . . ? C40 C35 Ir2 125.9(11) . . ? C37 C36 C35 111.6(15) . . ? C37 C36 C41 128(2) . . ? C35 C36 C41 120(2) . . ? C37 C36 Ir2 74.2(8) . . ? C35 C36 Ir2 70.2(7) . . ? C41 C36 Ir2 125.5(12) . . ? C36 C37 C33 106.8(14) . . ? C36 C37 C42 125.3(18) . . ? C33 C37 C42 127.8(18) . . ? C36 C37 Ir2 69.6(8) . . ? C33 C37 Ir2 70.7(8) . . ? C42 C37 Ir2 125.8(10) . . ? F2 C43 F1 112(2) . . ? F2 C43 F3 116(2) . . ? F1 C43 F3 104.0(17) . . ? F2 C43 S1 108.6(14) . . ? F1 C43 S1 108.5(13) . . ? F3 C43 S1 106.5(15) . . ? F5 C44 F6 112.5(14) . . ? F5 C44 F4 103.2(13) . . ? F6 C44 F4 102.8(13) . . ? F5 C44 S2 113.1(14) . . ? F6 C44 S2 114.5(16) . . ? F4 C44 S2 109.6(13) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.558 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.165 # Attachment 'Complex 3b.cif' data_complex_3b _database_code_depnum_ccdc_archive 'CCDC 749415' #TrackingRef 'Complex 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H88 F12 N4 O22 Rh4 S4' _chemical_formula_weight 2321.50 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.093(6) _cell_length_b 13.414(6) _cell_length_c 16.831(7) _cell_angle_alpha 66.904(6) _cell_angle_beta 77.127(6) _cell_angle_gamma 76.342(7) _cell_volume 2614(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 861 _cell_measurement_theta_min 2.585 _cell_measurement_theta_max 21.160 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8911 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.89 _diffrn_reflns_number 11906 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.01 _reflns_number_total 9995 _reflns_number_gt 5541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9995 _refine_ls_number_parameters 577 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1750 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.910 _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 Rh1 Rh 0.72924(4) 0.54344(4) 0.29234(3) 0.04208(18) Uani 1 1 d . . . Rh2 Rh 0.77942(4) 0.79541(4) -0.25667(3) 0.04096(18) Uani 1 1 d . . . N1 N 0.8789(4) 0.4503(4) 0.2588(3) 0.0394(13) Uani 1 1 d . . . N2 N 1.0724(4) 0.3189(4) 0.2429(3) 0.0412(14) Uani 1 1 d . . . O1 O 0.7791(4) 0.6761(4) 0.1913(3) 0.0504(13) Uani 1 1 d . . . O2 O 0.6808(4) 0.5087(4) 0.2000(3) 0.0425(11) Uani 1 1 d . . . O3 O 0.7162(4) 0.6702(4) -0.1546(3) 0.0488(13) Uani 1 1 d . . . O4 O 0.8131(4) 0.8381(4) -0.1612(3) 0.0483(12) Uani 1 1 d . . . O5 O 0.6873(5) 0.1927(6) 0.3260(5) 0.101(2) Uani 1 1 d . . . O6 O 0.8399(5) 0.0950(6) 0.3943(5) 0.098(2) Uani 1 1 d . . . O7 O 0.6825(6) 0.0095(6) 0.4286(5) 0.116(3) Uani 1 1 d . . . O8 O 0.2610(7) 0.6165(8) 0.3543(6) 0.168(4) Uiso 1 1 d D . . O9 O 0.1266(8) 0.5331(8) 0.3428(6) 0.174(4) Uiso 1 1 d D . . O10 O 0.2207(13) 0.6337(14) 0.2086(6) 0.313(9) Uiso 1 1 d D . . F1 F 0.7217(7) 0.0248(7) 0.2484(5) 0.150(3) Uani 1 1 d . . . F2 F 0.8617(7) 0.0991(9) 0.2209(6) 0.192(5) Uani 1 1 d . . . F3 F 0.8569(7) -0.0586(8) 0.3085(8) 0.203(5) Uani 1 1 d . . . F4 F 0.1323(12) 0.8269(12) 0.2516(9) 0.321(8) Uiso 1 1 d D . . F5 F 0.0497(9) 0.7307(10) 0.3730(7) 0.247(5) Uiso 1 1 d D . . F6 F 0.0189(9) 0.7443(10) 0.2490(7) 0.243(5) Uiso 1 1 d D . . S1 S 0.74583(19) 0.0875(2) 0.36878(15) 0.0651(6) Uani 1 1 d D . . S2 S 0.1974(3) 0.6167(5) 0.2969(3) 0.1635(19) Uani 1 1 d D . . C1 C 0.7718(5) 0.7091(6) 0.1104(4) 0.0417(17) Uani 1 1 d . . . C2 C 0.7404(5) 0.6529(5) 0.0669(4) 0.0343(15) Uani 1 1 d . . . C3 C 0.6960(5) 0.5544(5) 0.1165(4) 0.0361(16) Uani 1 1 d . . . C4 C 0.6657(5) 0.4967(6) 0.0706(4) 0.0450(18) Uani 1 1 d . . . C5 C 0.6298(7) 0.3957(7) 0.1165(5) 0.065(2) Uani 1 1 d . . . H5 H 0.6224 0.3672 0.1771 0.077 Uiso 1 1 calc R . . C6 C 0.6056(9) 0.3389(8) 0.0736(5) 0.095(4) Uani 1 1 d . . . H6 H 0.5821 0.2721 0.1051 0.114 Uiso 1 1 calc R . . C7 C 0.6158(9) 0.3798(8) -0.0166(6) 0.102(4) Uani 1 1 d . . . H7 H 0.6006 0.3396 -0.0454 0.123 Uiso 1 1 calc R . . C8 C 0.6481(7) 0.4797(8) -0.0636(5) 0.073(3) Uani 1 1 d . . . H8 H 0.6517 0.5084 -0.1241 0.088 Uiso 1 1 calc R . . C9 C 0.6754(6) 0.5376(6) -0.0214(4) 0.0435(17) Uani 1 1 d . . . C10 C 0.7159(5) 0.6409(5) -0.0728(4) 0.0365(15) Uani 1 1 d . . . C11 C 0.7494(5) 0.6954(5) -0.0293(4) 0.0353(15) Uani 1 1 d . . . C12 C 0.7904(5) 0.7953(6) -0.0775(4) 0.0413(17) Uani 1 1 d . . . C13 C 0.8140(6) 0.8570(6) -0.0316(5) 0.0512(19) Uani 1 1 d . . . C14 C 0.8437(9) 0.9612(8) -0.0792(5) 0.092(4) Uani 1 1 d . . . H14 H 0.8490 0.9895 -0.1398 0.110 Uiso 1 1 calc R . . C15 C 0.8651(12) 1.0215(9) -0.0363(6) 0.142(6) Uani 1 1 d . . . H15 H 0.8870 1.0891 -0.0682 0.171 Uiso 1 1 calc R . . C16 C 0.8542(13) 0.9821(10) 0.0533(7) 0.138(6) Uani 1 1 d . . . H16 H 0.8652 1.0246 0.0820 0.165 Uiso 1 1 calc R . . C17 C 0.8266(9) 0.8780(7) 0.1014(5) 0.087(3) Uani 1 1 d . . . H17 H 0.8225 0.8495 0.1618 0.104 Uiso 1 1 calc R . . C18 C 0.8053(7) 0.8177(6) 0.0578(5) 0.054(2) Uani 1 1 d . . . C19 C 0.8857(6) 0.3492(6) 0.2609(4) 0.0443(17) Uani 1 1 d . . . H19 H 0.8237 0.3224 0.2681 0.053 Uiso 1 1 calc R . . C20 C 0.9828(5) 0.2824(6) 0.2526(4) 0.0451(18) Uani 1 1 d . . . H20 H 0.9852 0.2120 0.2537 0.054 Uiso 1 1 calc R . . C21 C 1.0675(6) 0.4198(6) 0.2387(5) 0.0487(18) Uani 1 1 d . . . H21 H 1.1300 0.4465 0.2304 0.058 Uiso 1 1 calc R . . C22 C 0.9714(6) 0.4865(6) 0.2464(5) 0.053(2) Uani 1 1 d . . . H22 H 0.9698 0.5577 0.2429 0.064 Uiso 1 1 calc R . . C23 C 0.7500(8) 0.5267(9) 0.4196(5) 0.076(3) Uani 1 1 d . . . C24 C 0.6789(10) 0.6283(8) 0.3832(6) 0.082(3) Uani 1 1 d . . . C25 C 0.5898(8) 0.6020(9) 0.3652(6) 0.079(3) Uani 1 1 d . . . C26 C 0.6028(7) 0.4856(8) 0.3959(5) 0.066(2) Uani 1 1 d . . . C27 C 0.6997(8) 0.4424(7) 0.4270(5) 0.058(2) Uani 1 1 d . . . C28 C 0.8556(9) 0.5172(11) 0.4474(6) 0.117(4) Uani 1 1 d . . . H28A H 0.9030 0.5544 0.3976 0.176 Uiso 1 1 calc R . . H28B H 0.8862 0.4411 0.4715 0.176 Uiso 1 1 calc R . . H28C H 0.8445 0.5501 0.4906 0.176 Uiso 1 1 calc R . . C29 C 0.6991(11) 0.7429(8) 0.3609(7) 0.133(5) Uani 1 1 d . . . H29A H 0.6473 0.7952 0.3264 0.199 Uiso 1 1 calc R . . H29B H 0.7690 0.7501 0.3285 0.199 Uiso 1 1 calc R . . H29C H 0.6941 0.7563 0.4138 0.199 Uiso 1 1 calc R . . C30 C 0.4988(9) 0.6851(11) 0.3285(9) 0.172(7) Uani 1 1 d . . . H30A H 0.5220 0.7546 0.2957 0.259 Uiso 1 1 calc R . . H30B H 0.4437 0.6922 0.3753 0.259 Uiso 1 1 calc R . . H30C H 0.4720 0.6622 0.2909 0.259 Uiso 1 1 calc R . . C31 C 0.5234(8) 0.4244(10) 0.3881(7) 0.105(4) Uani 1 1 d . . . H31A H 0.4717 0.4091 0.4399 0.157 Uiso 1 1 calc R . . H31B H 0.5601 0.3566 0.3813 0.157 Uiso 1 1 calc R . . H31C H 0.4883 0.4689 0.3383 0.157 Uiso 1 1 calc R . . C32 C 0.7417(9) 0.3216(8) 0.4688(5) 0.106(4) Uani 1 1 d . . . H32A H 0.6832 0.2822 0.4966 0.158 Uiso 1 1 calc R . . H32B H 0.7847 0.3116 0.5116 0.158 Uiso 1 1 calc R . . H32C H 0.7838 0.2943 0.4249 0.158 Uiso 1 1 calc R . . C33 C 0.7087(14) 0.8053(8) -0.3616(8) 0.106(5) Uani 1 1 d . . . C34 C 0.6436(6) 0.8741(12) -0.3194(6) 0.093(4) Uani 1 1 d . . . C35 C 0.6999(8) 0.9551(8) -0.3267(5) 0.072(3) Uani 1 1 d . . . C36 C 0.7988(7) 0.9355(7) -0.3721(5) 0.067(3) Uani 1 1 d . . . C37 C 0.8062(9) 0.8495(9) -0.3970(5) 0.082(3) Uani 1 1 d . . . C38 C 0.694(2) 0.7096(12) -0.3788(12) 0.278(15) Uani 1 1 d . . . H38A H 0.6690 0.7346 -0.4339 0.417 Uiso 1 1 calc R . . H38B H 0.6432 0.6712 -0.3333 0.417 Uiso 1 1 calc R . . H38C H 0.7608 0.6609 -0.3803 0.417 Uiso 1 1 calc R . . C39 C 0.5311(10) 0.8631(16) -0.2764(10) 0.250(13) Uani 1 1 d . . . H39A H 0.4866 0.8824 -0.3201 0.376 Uiso 1 1 calc R . . H39B H 0.5067 0.9112 -0.2438 0.376 Uiso 1 1 calc R . . H39C H 0.5284 0.7885 -0.2376 0.376 Uiso 1 1 calc R . . C40 C 0.6590(15) 1.0420(11) -0.2888(10) 0.216(10) Uani 1 1 d . . . H40A H 0.6752 1.0153 -0.2304 0.324 Uiso 1 1 calc R . . H40B H 0.5834 1.0616 -0.2877 0.324 Uiso 1 1 calc R . . H40C H 0.6918 1.1054 -0.3237 0.324 Uiso 1 1 calc R . . C41 C 0.8885(9) 1.0025(10) -0.3967(8) 0.141(6) Uani 1 1 d . . . H41A H 0.8809 1.0616 -0.4516 0.212 Uiso 1 1 calc R . . H41B H 0.9558 0.9559 -0.4015 0.212 Uiso 1 1 calc R . . H41C H 0.8849 1.0320 -0.3524 0.212 Uiso 1 1 calc R . . C42 C 0.9034(13) 0.8062(14) -0.4465(7) 0.213(10) Uani 1 1 d . . . H42A H 0.9125 0.7275 -0.4252 0.319 Uiso 1 1 calc R . . H42B H 0.9641 0.8284 -0.4389 0.319 Uiso 1 1 calc R . . H42C H 0.8964 0.8350 -0.5073 0.319 Uiso 1 1 calc R . . C43 C 0.7981(10) 0.0362(10) 0.2824(8) 0.101(4) Uani 1 1 d D . . C44 C 0.0958(10) 0.7325(10) 0.2934(9) 0.186(7) Uiso 1 1 d D . . O11 O 0.5002(7) 0.1108(7) 0.5329(6) 0.142(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0500(4) 0.0424(3) 0.0305(3) -0.0119(3) -0.0027(3) -0.0065(3) Rh2 0.0426(4) 0.0430(3) 0.0308(3) -0.0040(3) -0.0071(2) -0.0098(3) N1 0.046(4) 0.039(3) 0.036(3) -0.015(3) -0.008(3) -0.007(3) N2 0.042(4) 0.039(3) 0.040(3) -0.008(3) -0.011(3) -0.008(3) O1 0.066(3) 0.048(3) 0.042(3) -0.013(2) -0.013(2) -0.020(3) O2 0.049(3) 0.043(3) 0.035(3) -0.009(2) -0.007(2) -0.015(2) O3 0.055(3) 0.059(3) 0.034(3) -0.010(2) -0.001(2) -0.029(3) O4 0.067(3) 0.039(3) 0.034(3) -0.004(2) 0.001(2) -0.025(2) O5 0.078(5) 0.086(5) 0.148(7) -0.055(5) -0.038(5) 0.015(4) O6 0.085(5) 0.121(6) 0.108(5) -0.047(5) -0.037(4) -0.021(4) O7 0.117(6) 0.125(6) 0.090(5) -0.007(5) 0.012(4) -0.070(5) F1 0.163(7) 0.186(8) 0.176(7) -0.122(7) -0.030(6) -0.060(6) F2 0.197(8) 0.279(12) 0.158(7) -0.133(8) 0.099(6) -0.168(9) F3 0.147(8) 0.162(8) 0.350(15) -0.180(10) -0.029(8) 0.028(6) S1 0.0646(15) 0.0723(15) 0.0623(14) -0.0253(12) -0.0109(11) -0.0148(12) S2 0.144(3) 0.283(6) 0.120(3) -0.135(4) -0.008(3) -0.040(4) C1 0.045(4) 0.042(4) 0.036(4) -0.011(3) -0.007(3) -0.008(3) C2 0.031(4) 0.036(4) 0.032(4) -0.008(3) -0.005(3) -0.004(3) C3 0.025(3) 0.039(4) 0.036(4) -0.006(3) -0.007(3) -0.001(3) C4 0.046(4) 0.049(4) 0.040(4) -0.008(3) -0.005(3) -0.024(4) C5 0.094(7) 0.066(5) 0.037(4) -0.006(4) 0.000(4) -0.050(5) C6 0.180(11) 0.081(7) 0.040(5) -0.002(5) -0.010(6) -0.093(8) C7 0.190(12) 0.093(7) 0.054(6) -0.013(5) -0.011(6) -0.110(8) C8 0.108(7) 0.091(7) 0.036(4) -0.017(4) -0.005(4) -0.059(6) C9 0.055(5) 0.046(4) 0.030(4) -0.008(3) -0.003(3) -0.023(4) C10 0.029(4) 0.045(4) 0.031(4) -0.011(3) -0.002(3) -0.004(3) C11 0.035(4) 0.031(3) 0.037(4) -0.008(3) -0.003(3) -0.010(3) C12 0.040(4) 0.043(4) 0.032(4) -0.011(3) -0.002(3) 0.000(3) C13 0.066(5) 0.039(4) 0.052(5) -0.013(4) -0.009(4) -0.021(4) C14 0.174(11) 0.074(6) 0.042(5) -0.010(5) -0.012(6) -0.068(7) C15 0.302(19) 0.101(9) 0.048(6) -0.007(6) -0.003(9) -0.133(11) C16 0.279(18) 0.094(8) 0.078(8) -0.023(7) -0.044(10) -0.096(11) C17 0.161(10) 0.074(6) 0.046(5) -0.017(5) 0.001(6) -0.081(7) C18 0.086(6) 0.042(4) 0.043(4) -0.011(4) -0.013(4) -0.027(4) C19 0.046(4) 0.042(4) 0.049(4) -0.015(4) -0.005(3) -0.020(4) C20 0.044(4) 0.046(4) 0.049(4) -0.015(4) -0.011(3) -0.014(4) C21 0.052(5) 0.050(5) 0.048(4) -0.016(4) -0.009(4) -0.015(4) C22 0.064(6) 0.049(5) 0.053(5) -0.018(4) -0.010(4) -0.021(4) C23 0.095(7) 0.111(8) 0.028(4) -0.036(5) 0.009(4) -0.022(7) C24 0.124(9) 0.057(6) 0.060(6) -0.034(5) 0.024(6) -0.019(6) C25 0.059(6) 0.098(8) 0.065(6) -0.040(6) 0.021(5) 0.004(6) C26 0.069(6) 0.080(7) 0.051(5) -0.031(5) 0.023(4) -0.033(5) C27 0.089(7) 0.050(5) 0.028(4) -0.015(4) 0.008(4) -0.017(5) C28 0.134(10) 0.185(13) 0.055(6) -0.052(8) -0.018(6) -0.046(9) C29 0.238(15) 0.077(7) 0.084(8) -0.048(7) 0.049(9) -0.065(9) C30 0.093(9) 0.147(12) 0.175(14) -0.016(11) 0.016(9) 0.062(9) C31 0.089(8) 0.150(11) 0.092(8) -0.059(8) 0.022(6) -0.055(8) C32 0.174(12) 0.081(7) 0.033(5) -0.006(5) -0.004(6) -0.004(7) C33 0.186(14) 0.047(6) 0.097(9) 0.023(6) -0.107(10) -0.047(8) C34 0.027(5) 0.126(10) 0.064(6) 0.028(7) -0.008(4) -0.008(6) C35 0.074(7) 0.065(6) 0.047(5) -0.005(4) -0.001(5) 0.013(5) C36 0.082(7) 0.050(5) 0.049(5) 0.017(4) -0.024(5) -0.022(5) C37 0.117(9) 0.070(7) 0.039(5) -0.012(5) -0.024(5) 0.022(6) C38 0.56(4) 0.111(12) 0.235(19) 0.012(13) -0.30(3) -0.098(19) C39 0.074(9) 0.34(3) 0.184(15) 0.116(16) -0.058(10) -0.088(13) C40 0.34(2) 0.126(12) 0.138(13) -0.074(11) -0.086(14) 0.138(14) C41 0.119(10) 0.141(11) 0.111(9) 0.055(8) -0.044(8) -0.075(9) C42 0.264(19) 0.220(17) 0.040(6) -0.030(9) -0.004(9) 0.120(15) C43 0.096(9) 0.093(9) 0.148(11) -0.074(9) -0.006(8) -0.033(7) O11 0.151(8) 0.115(7) 0.149(8) -0.039(6) 0.001(6) -0.040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.041(5) . ? Rh1 O2 2.045(4) . ? Rh1 C25 2.129(8) . ? Rh1 C23 2.137(8) . ? Rh1 C27 2.138(7) . ? Rh1 N1 2.151(6) . ? Rh1 C24 2.152(9) . ? Rh1 C26 2.155(7) . ? Rh2 O3 2.053(4) . ? Rh2 O4 2.065(5) . ? Rh2 C34 2.114(8) . ? Rh2 C33 2.116(9) . ? Rh2 C36 2.124(7) . ? Rh2 C35 2.139(8) . ? Rh2 C37 2.152(8) . ? Rh2 N2 2.164(6) 2_765 ? N1 C19 1.324(8) . ? N1 C22 1.353(9) . ? N2 C21 1.315(9) . ? N2 C20 1.330(8) . ? N2 Rh2 2.164(6) 2_765 ? O1 C1 1.274(8) . ? O2 C3 1.284(7) . ? O3 C10 1.275(7) . ? O4 C12 1.289(7) . ? O5 S1 1.426(7) . ? O6 S1 1.428(6) . ? O7 S1 1.416(6) . ? O8 S2 1.408(7) . ? O9 S2 1.485(7) . ? O10 S2 1.384(8) . ? F1 C43 1.322(12) . ? F2 C43 1.320(12) . ? F3 C43 1.285(14) . ? F4 C44 1.328(9) . ? F5 C44 1.335(9) . ? F6 C44 1.329(9) . ? S1 C43 1.781(11) . ? S2 C44 1.782(10) . ? C1 C2 1.409(9) . ? C1 C18 1.488(9) . ? C2 C3 1.435(8) . ? C2 C11 1.478(8) . ? C3 C4 1.450(9) . ? C4 C5 1.405(9) . ? C4 C9 1.413(9) . ? C5 C6 1.359(11) . ? C6 C7 1.383(11) . ? C7 C8 1.374(11) . ? C8 C9 1.383(10) . ? C9 C10 1.467(9) . ? C10 C11 1.406(9) . ? C11 C12 1.426(9) . ? C12 C13 1.453(10) . ? C13 C18 1.372(10) . ? C13 C14 1.409(10) . ? C14 C15 1.381(12) . ? C15 C16 1.374(13) . ? C16 C17 1.398(12) . ? C17 C18 1.391(10) . ? C19 C20 1.385(9) . ? C21 C22 1.374(10) . ? C23 C27 1.389(12) . ? C23 C24 1.450(13) . ? C23 C28 1.519(13) . ? C24 C25 1.419(14) . ? C24 C29 1.506(13) . ? C25 C26 1.420(13) . ? C25 C30 1.484(14) . ? C26 C27 1.390(12) . ? C26 C31 1.523(12) . ? C27 C32 1.510(11) . ? C33 C34 1.398(16) . ? C33 C37 1.441(16) . ? C33 C38 1.484(16) . ? C34 C35 1.404(15) . ? C34 C39 1.503(14) . ? C35 C36 1.374(12) . ? C35 C40 1.479(15) . ? C36 C37 1.351(13) . ? C36 C41 1.532(12) . ? C37 C42 1.486(15) . ? 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 Rh1 O2 85.85(18) . . ? O1 Rh1 C25 107.7(3) . . ? O2 Rh1 C25 107.0(3) . . ? O1 Rh1 C23 116.3(3) . . ? O2 Rh1 C23 157.7(3) . . ? C25 Rh1 C23 65.9(4) . . ? O1 Rh1 C27 154.2(3) . . ? O2 Rh1 C27 119.8(3) . . ? C25 Rh1 C27 64.6(3) . . ? C23 Rh1 C27 37.9(3) . . ? O1 Rh1 N1 86.6(2) . . ? O2 Rh1 N1 84.07(19) . . ? C25 Rh1 N1 162.2(3) . . ? C23 Rh1 N1 98.5(3) . . ? C27 Rh1 N1 97.8(3) . . ? O1 Rh1 C24 94.3(3) . . ? O2 Rh1 C24 143.7(4) . . ? C25 Rh1 C24 38.7(4) . . ? C23 Rh1 C24 39.5(4) . . ? C27 Rh1 C24 64.0(3) . . ? N1 Rh1 C24 132.2(4) . . ? O1 Rh1 C26 145.6(3) . . ? O2 Rh1 C26 96.7(3) . . ? C25 Rh1 C26 38.7(3) . . ? C23 Rh1 C26 64.2(4) . . ? C27 Rh1 C26 37.8(3) . . ? N1 Rh1 C26 127.8(3) . . ? C24 Rh1 C26 63.9(4) . . ? O3 Rh2 O4 85.32(18) . . ? O3 Rh2 C34 99.2(3) . . ? O4 Rh2 C34 122.1(5) . . ? O3 Rh2 C33 102.3(3) . . ? O4 Rh2 C33 159.7(4) . . ? C34 Rh2 C33 38.6(4) . . ? O3 Rh2 C36 163.0(3) . . ? O4 Rh2 C36 103.9(3) . . ? C34 Rh2 C36 63.8(3) . . ? C33 Rh2 C36 64.4(4) . . ? O3 Rh2 C35 128.4(3) . . ? O4 Rh2 C35 95.8(3) . . ? C34 Rh2 C35 38.6(4) . . ? C33 Rh2 C35 64.7(4) . . ? C36 Rh2 C35 37.6(3) . . ? O3 Rh2 C37 137.0(4) . . ? O4 Rh2 C37 137.6(4) . . ? C34 Rh2 C37 64.0(4) . . ? C33 Rh2 C37 39.4(4) . . ? C36 Rh2 C37 36.8(4) . . ? C35 Rh2 C37 62.8(3) . . ? O3 Rh2 N2 84.7(2) . 2_765 ? O4 Rh2 N2 86.7(2) . 2_765 ? C34 Rh2 N2 151.0(5) . 2_765 ? C33 Rh2 N2 112.4(5) . 2_765 ? C36 Rh2 N2 109.8(3) . 2_765 ? C35 Rh2 N2 146.9(3) . 2_765 ? C37 Rh2 N2 93.5(3) . 2_765 ? C19 N1 C22 116.9(6) . . ? C19 N1 Rh1 121.4(5) . . ? C22 N1 Rh1 121.1(5) . . ? C21 N2 C20 119.1(6) . . ? C21 N2 Rh2 120.4(5) . 2_765 ? C20 N2 Rh2 119.6(5) . 2_765 ? C1 O1 Rh1 129.7(4) . . ? C3 O2 Rh1 129.5(4) . . ? C10 O3 Rh2 129.9(4) . . ? C12 O4 Rh2 129.4(4) . . ? O7 S1 O5 114.5(5) . . ? O7 S1 O6 118.3(5) . . ? O5 S1 O6 112.5(4) . . ? O7 S1 C43 103.7(5) . . ? O5 S1 C43 102.9(6) . . ? O6 S1 C43 102.3(5) . . ? O10 S2 O8 130.2(8) . . ? O10 S2 O9 111.0(8) . . ? O8 S2 O9 110.3(6) . . ? O10 S2 C44 99.3(8) . . ? O8 S2 C44 103.1(6) . . ? O9 S2 C44 95.7(6) . . ? O1 C1 C2 127.4(6) . . ? O1 C1 C18 114.1(6) . . ? C2 C1 C18 118.4(6) . . ? C1 C2 C3 119.9(6) . . ? C1 C2 C11 121.0(5) . . ? C3 C2 C11 119.1(6) . . ? O2 C3 C2 126.5(6) . . ? O2 C3 C4 114.4(6) . . ? C2 C3 C4 119.1(6) . . ? C5 C4 C9 117.8(7) . . ? C5 C4 C3 120.8(6) . . ? C9 C4 C3 121.4(6) . . ? C6 C5 C4 121.0(7) . . ? C5 C6 C7 120.5(7) . . ? C8 C7 C6 120.2(8) . . ? C7 C8 C9 120.2(7) . . ? C8 C9 C4 120.2(6) . . ? C8 C9 C10 119.7(6) . . ? C4 C9 C10 120.1(6) . . ? O3 C10 C11 127.6(6) . . ? O3 C10 C9 113.4(6) . . ? C11 C10 C9 119.0(6) . . ? C10 C11 C12 120.3(6) . . ? C10 C11 C2 121.2(5) . . ? C12 C11 C2 118.5(6) . . ? O4 C12 C11 126.6(6) . . ? O4 C12 C13 113.6(6) . . ? C11 C12 C13 119.8(6) . . ? C18 C13 C14 118.9(7) . . ? C18 C13 C12 121.6(6) . . ? C14 C13 C12 119.6(7) . . ? C15 C14 C13 120.2(8) . . ? C16 C15 C14 120.3(9) . . ? C15 C16 C17 120.0(9) . . ? C18 C17 C16 119.3(8) . . ? C13 C18 C17 121.2(7) . . ? C13 C18 C1 120.3(6) . . ? C17 C18 C1 118.5(7) . . ? N1 C19 C20 121.8(6) . . ? N2 C20 C19 120.0(7) . . ? N2 C21 C22 120.9(7) . . ? N1 C22 C21 121.1(7) . . ? C27 C23 C24 106.3(9) . . ? C27 C23 C28 128.1(10) . . ? C24 C23 C28 125.5(11) . . ? C27 C23 Rh1 71.1(5) . . ? C24 C23 Rh1 70.8(5) . . ? C28 C23 Rh1 125.1(6) . . ? C25 C24 C23 108.0(9) . . ? C25 C24 C29 125.3(11) . . ? C23 C24 C29 126.4(12) . . ? C25 C24 Rh1 69.8(5) . . ? C23 C24 Rh1 69.7(5) . . ? C29 C24 Rh1 122.4(7) . . ? C24 C25 C26 106.7(9) . . ? C24 C25 C30 123.7(12) . . ? C26 C25 C30 129.4(12) . . ? C24 C25 Rh1 71.5(5) . . ? C26 C25 Rh1 71.6(5) . . ? C30 C25 Rh1 126.1(8) . . ? C27 C26 C25 108.6(8) . . ? C27 C26 C31 128.4(9) . . ? C25 C26 C31 122.9(10) . . ? C27 C26 Rh1 70.5(4) . . ? C25 C26 Rh1 69.7(5) . . ? C31 C26 Rh1 122.5(6) . . ? C23 C27 C26 110.2(8) . . ? C23 C27 C32 124.3(10) . . ? C26 C27 C32 125.3(9) . . ? C23 C27 Rh1 71.0(4) . . ? C26 C27 Rh1 71.8(4) . . ? C32 C27 Rh1 127.2(6) . . ? C34 C33 C37 105.6(9) . . ? C34 C33 C38 134.2(18) . . ? C37 C33 C38 120.0(18) . . ? C34 C33 Rh2 70.6(6) . . ? C37 C33 Rh2 71.6(5) . . ? C38 C33 Rh2 125.0(7) . . ? C33 C34 C35 108.6(8) . . ? C33 C34 C39 124.7(17) . . ? C35 C34 C39 126.7(15) . . ? C33 C34 Rh2 70.8(5) . . ? C35 C34 Rh2 71.7(5) . . ? C39 C34 Rh2 124.8(7) . . ? C36 C35 C34 107.4(9) . . ? C36 C35 C40 127.5(13) . . ? C34 C35 C40 125.1(13) . . ? C36 C35 Rh2 70.6(5) . . ? C34 C35 Rh2 69.8(5) . . ? C40 C35 Rh2 123.2(7) . . ? C37 C36 C35 110.2(9) . . ? C37 C36 C41 123.0(11) . . ? C35 C36 C41 126.7(11) . . ? C37 C36 Rh2 72.7(5) . . ? C35 C36 Rh2 71.8(5) . . ? C41 C36 Rh2 124.6(6) . . ? C36 C37 C33 108.1(10) . . ? C36 C37 C42 123.8(14) . . ? C33 C37 C42 127.9(14) . . ? C36 C37 Rh2 70.4(5) . . ? C33 C37 Rh2 68.9(5) . . ? C42 C37 Rh2 122.7(7) . . ? F3 C43 F2 104.2(11) . . ? F3 C43 F1 106.8(10) . . ? F2 C43 F1 110.2(11) . . ? F3 C43 S1 112.0(10) . . ? F2 C43 S1 111.6(8) . . ? F1 C43 S1 111.7(8) . . ? F4 C44 F6 102.3(10) . . ? F4 C44 F5 107.6(11) . . ? F6 C44 F5 107.2(11) . . ? F4 C44 S2 112.2(11) . . ? F6 C44 S2 114.6(10) . . ? F5 C44 S2 112.3(10) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.019 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.120 # Attachment 'Complex 3b.cif' data_Complex_3b' _database_code_depnum_ccdc_archive 'CCDC 749416' #TrackingRef 'Complex 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H92 Cl4 F12 N4 O22 Rh4 S4' _chemical_formula_weight 2491.36 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.091(6) _cell_length_b 13.658(6) _cell_length_c 16.821(8) _cell_angle_alpha 66.852(6) _cell_angle_beta 76.044(5) _cell_angle_gamma 76.112(6) _cell_volume 2648(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 852 _cell_measurement_theta_min 2.888 _cell_measurement_theta_max 23.412 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9017 _exptl_absorpt_correction_T_max 0.9329 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.81 _diffrn_reflns_number 10872 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9067 _reflns_number_gt 5774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9067 _refine_ls_number_parameters 605 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1929 _refine_ls_wR_factor_gt 0.1811 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.21635(4) 0.20968(4) 0.26013(3) 0.04042(19) Uani 1 1 d . . . Rh2 Rh 0.28452(4) 0.46659(4) -0.29047(3) 0.0443(2) Uani 1 1 d . . . N1 N 0.0688(4) 0.3177(4) 0.2432(4) 0.0439(14) Uani 1 1 d . . . N2 N -0.1315(4) 0.4445(4) 0.2605(4) 0.0439(14) Uani 1 1 d . . . O1 O 0.2813(4) 0.3349(4) 0.1598(3) 0.0477(12) Uani 1 1 d . . . O2 O 0.1914(4) 0.1676(4) 0.1626(3) 0.0514(12) Uani 1 1 d . . . O3 O 0.2282(4) 0.3365(4) -0.1909(3) 0.0511(12) Uani 1 1 d . . . O4 O 0.3229(4) 0.5011(4) -0.1955(3) 0.0453(11) Uani 1 1 d . . . C1 C 0.3911(8) 0.6180(7) 0.0257(6) 0.073(3) Uani 1 1 d . . . H1 H 0.4105 0.6538 0.0554 0.088 Uiso 1 1 calc R . . C2 C 0.3534(6) 0.5230(6) 0.0715(5) 0.054(2) Uani 1 1 d . . . H2 H 0.3458 0.4949 0.1323 0.065 Uiso 1 1 calc R . . C3 C 0.3263(5) 0.4677(5) 0.0270(4) 0.0401(15) Uani 1 1 d . . . C4 C 0.3366(5) 0.5100(5) -0.0641(4) 0.0410(16) Uani 1 1 d . . . C5 C 0.3719(7) 0.6094(6) -0.1084(5) 0.058(2) Uani 1 1 d . . . H5 H 0.3758 0.6404 -0.1689 0.070 Uiso 1 1 calc R . . C6 C 0.4006(8) 0.6617(7) -0.0658(5) 0.078(3) Uani 1 1 d . . . H6 H 0.4265 0.7264 -0.0971 0.093 Uiso 1 1 calc R . . C7 C 0.2843(5) 0.3666(5) 0.0771(4) 0.0358(15) Uani 1 1 d . . . C8 C 0.2509(5) 0.3134(5) 0.0324(4) 0.0363(15) Uani 1 1 d . . . C9 C 0.2622(5) 0.3581(5) -0.0648(4) 0.0371(15) Uani 1 1 d . . . C10 C 0.3055(5) 0.4550(5) -0.1108(4) 0.0371(15) Uani 1 1 d . . . C11 C 0.2122(5) 0.2134(5) 0.0791(4) 0.0416(16) Uani 1 1 d . . . C12 C 0.1909(7) 0.1533(6) 0.0304(5) 0.0545(19) Uani 1 1 d . . . C13 C 0.1988(7) 0.1992(6) -0.0595(5) 0.058(2) Uani 1 1 d . . . C14 C 0.2317(5) 0.3041(5) -0.1085(4) 0.0425(16) Uani 1 1 d . . . C15 C 0.1606(9) 0.0492(7) 0.0779(6) 0.085(3) Uani 1 1 d . . . H15 H 0.1540 0.0196 0.1387 0.101 Uiso 1 1 calc R . . C16 C 0.1417(12) -0.0051(10) 0.0323(7) 0.122(5) Uani 1 1 d . . . H16 H 0.1203 -0.0722 0.0622 0.147 Uiso 1 1 calc R . . C17 C 0.1540(13) 0.0383(10) -0.0589(7) 0.135(6) Uani 1 1 d . . . H17 H 0.1457 -0.0026 -0.0892 0.162 Uiso 1 1 calc R . . C18 C 0.1778(10) 0.1394(9) -0.1043(6) 0.098(4) Uani 1 1 d . . . H18 H 0.1802 0.1692 -0.1647 0.117 Uiso 1 1 calc R . . C19 C -0.0202(6) 0.2844(6) 0.2466(5) 0.0525(19) Uani 1 1 d . . . H19 H -0.0155 0.2168 0.2437 0.063 Uiso 1 1 calc R . . C20 C 0.0577(6) 0.4163(6) 0.2437(5) 0.0547(19) Uani 1 1 d . . . H20 H 0.1185 0.4431 0.2394 0.066 Uiso 1 1 calc R . . C21 C -0.0408(6) 0.4815(6) 0.2505(5) 0.0545(19) Uani 1 1 d . . . H21 H -0.0442 0.5514 0.2482 0.065 Uiso 1 1 calc R . . C22 C -0.1207(6) 0.3479(6) 0.2543(5) 0.0509(18) Uani 1 1 d . . . H22 H -0.1809 0.3224 0.2552 0.061 Uiso 1 1 calc R . . C23 C 0.3094(9) 0.0601(7) 0.3257(6) 0.078(3) Uani 1 1 d . . . C24 C 0.2034(8) 0.0615(7) 0.3674(6) 0.064(2) Uani 1 1 d . . . C25 C 0.1752(6) 0.1442(8) 0.3998(4) 0.061(2) Uani 1 1 d . . . C26 C 0.2564(8) 0.2011(7) 0.3776(5) 0.067(2) Uani 1 1 d . . . C27 C 0.3473(6) 0.1488(9) 0.3308(5) 0.076(3) Uani 1 1 d . . . C28 C 0.3813(14) -0.0104(12) 0.2797(9) 0.197(9) Uani 1 1 d . . . H28A H 0.3913 0.0288 0.2177 0.295 Uiso 1 1 calc R . . H28B H 0.3501 -0.0728 0.2924 0.295 Uiso 1 1 calc R . . H28C H 0.4491 -0.0328 0.2994 0.295 Uiso 1 1 calc R . . C29 C 0.1305(12) -0.0136(9) 0.3771(10) 0.145(6) Uani 1 1 d . . . H29A H 0.1093 -0.0531 0.4382 0.218 Uiso 1 1 calc R . . H29B H 0.1671 -0.0632 0.3479 0.218 Uiso 1 1 calc R . . H29C H 0.0684 0.0274 0.3515 0.218 Uiso 1 1 calc R . . C30 C 0.0651(9) 0.1768(13) 0.4515(6) 0.141(6) Uani 1 1 d . . . H30A H 0.0136 0.1395 0.4483 0.211 Uiso 1 1 calc R . . H30B H 0.0425 0.2532 0.4264 0.211 Uiso 1 1 calc R . . H30C H 0.0714 0.1576 0.5117 0.211 Uiso 1 1 calc R . . C31 C 0.2631(15) 0.2976(10) 0.4005(10) 0.163(8) Uani 1 1 d . . . H31A H 0.2021 0.3090 0.4428 0.245 Uiso 1 1 calc R . . H31B H 0.2645 0.3610 0.3484 0.245 Uiso 1 1 calc R . . H31C H 0.3270 0.2829 0.4245 0.245 Uiso 1 1 calc R . . C32 C 0.4532(8) 0.1860(13) 0.2938(8) 0.152(7) Uani 1 1 d . . . H32A H 0.5066 0.1338 0.3255 0.229 Uiso 1 1 calc R . . H32B H 0.4493 0.2542 0.2992 0.229 Uiso 1 1 calc R . . H32C H 0.4716 0.1937 0.2331 0.229 Uiso 1 1 calc R . . C33 C 0.4184(9) 0.5194(11) -0.3887(7) 0.092(4) Uani 1 1 d . . . C34 C 0.3223(10) 0.5627(8) -0.4251(5) 0.081(3) Uani 1 1 d . . . C35 C 0.2803(9) 0.4750(10) -0.4198(6) 0.082(3) Uani 1 1 d . . . C36 C 0.3421(12) 0.3819(8) -0.3778(7) 0.098(4) Uani 1 1 d . . . C37 C 0.4281(9) 0.4070(11) -0.3577(7) 0.093(3) Uani 1 1 d . . . C38 C 0.4906(12) 0.5824(14) -0.3810(9) 0.165(7) Uani 1 1 d . . . H38A H 0.5616 0.5631 -0.4088 0.248 Uiso 1 1 calc R . . H38B H 0.4907 0.5670 -0.3202 0.248 Uiso 1 1 calc R . . H38C H 0.4664 0.6581 -0.4091 0.248 Uiso 1 1 calc R . . C39 C 0.2810(14) 0.6791(9) -0.4696(7) 0.149(6) Uani 1 1 d . . . H39A H 0.2982 0.6972 -0.5320 0.224 Uiso 1 1 calc R . . H39B H 0.3132 0.7226 -0.4527 0.224 Uiso 1 1 calc R . . H39C H 0.2050 0.6924 -0.4527 0.224 Uiso 1 1 calc R . . C40 C 0.1755(12) 0.4806(15) -0.4509(9) 0.163(7) Uani 1 1 d . . . H40A H 0.1201 0.5312 -0.4323 0.244 Uiso 1 1 calc R . . H40B H 0.1545 0.4106 -0.4260 0.244 Uiso 1 1 calc R . . H40C H 0.1872 0.5036 -0.5137 0.244 Uiso 1 1 calc R . . C41 C 0.3217(16) 0.2650(11) -0.3573(9) 0.178(8) Uani 1 1 d . . . H41A H 0.3451 0.2471 -0.4093 0.267 Uiso 1 1 calc R . . H41B H 0.2468 0.2622 -0.3380 0.267 Uiso 1 1 calc R . . H41C H 0.3606 0.2143 -0.3121 0.267 Uiso 1 1 calc R . . C42 C 0.5166(13) 0.3221(18) -0.3124(12) 0.253(14) Uani 1 1 d . . . H42A H 0.5732 0.3057 -0.3559 0.379 Uiso 1 1 calc R . . H42B H 0.4882 0.2577 -0.2744 0.379 Uiso 1 1 calc R . . H42C H 0.5438 0.3497 -0.2787 0.379 Uiso 1 1 calc R . . S1 S 0.74699(18) 0.08508(19) 0.37271(15) 0.0674(6) Uani 1 1 d . . . O5 O 0.7000(6) 0.1850(6) 0.3174(6) 0.111(3) Uani 1 1 d . . . O6 O 0.8412(6) 0.0892(6) 0.3984(6) 0.108(3) Uani 1 1 d . . . O7 O 0.6728(7) 0.0242(7) 0.4393(5) 0.124(3) Uani 1 1 d . . . C43 C 0.7964(13) 0.0003(12) 0.3057(10) 0.116(4) Uani 1 1 d . . . F1 F 0.8720(9) 0.0390(13) 0.2453(8) 0.234(6) Uani 1 1 d . . . F2 F 0.8280(8) -0.0996(9) 0.3588(10) 0.206(5) Uani 1 1 d . . . F3 F 0.7150(10) 0.0050(9) 0.2671(6) 0.185(4) Uani 1 1 d . . . S2 S 0.1748(5) 0.6343(7) 0.2819(5) 0.255(4) Uani 1 1 d D . . O8 O 0.1860(15) 0.6497(16) 0.1946(8) 0.363(12) Uiso 1 1 d D . . O9 O 0.2584(11) 0.6417(18) 0.3156(14) 0.416(16) Uiso 1 1 d D . . O10 O 0.1312(18) 0.5366(11) 0.3375(15) 0.83(5) Uiso 1 1 d D . . C44 C 0.0716(9) 0.7350(10) 0.2987(9) 0.45(3) Uiso 1 1 d D . . F4 F -0.0177(9) 0.7339(14) 0.2753(13) 0.414(12) Uiso 1 1 d D . . F5 F 0.0488(11) 0.7281(11) 0.3807(8) 0.312(8) Uiso 1 1 d D . . F6 F 0.0913(12) 0.8343(8) 0.2538(10) 0.315(8) Uiso 1 1 d D . . C45 C 0.9068(13) 0.3116(15) 0.9724(14) 0.171(7) Uani 1 1 d . . . H45A H 0.8403 0.3423 0.9496 0.206 Uiso 1 1 calc R . . H45B H 0.9563 0.2795 0.9328 0.206 Uiso 1 1 calc R . . Cl1 Cl 0.9609(4) 0.4129(5) 0.9823(4) 0.192(2) Uani 1 1 d . . . Cl2 Cl 0.8857(6) 0.2169(6) 1.0746(7) 0.263(4) Uani 1 1 d . . . O11 O 0.4848(8) 0.1200(7) 0.5302(6) 0.139(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0448(3) 0.0433(3) 0.0278(3) -0.0039(2) -0.0082(2) -0.0102(2) Rh2 0.0539(4) 0.0470(4) 0.0297(3) -0.0130(3) -0.0062(2) -0.0058(3) N1 0.048(3) 0.040(3) 0.042(3) -0.008(3) -0.013(3) -0.009(3) N2 0.053(4) 0.043(3) 0.037(3) -0.013(3) -0.012(3) -0.008(3) O1 0.061(3) 0.054(3) 0.027(2) -0.002(2) -0.008(2) -0.029(2) O2 0.078(3) 0.047(3) 0.031(3) -0.007(2) -0.007(2) -0.027(3) O3 0.069(3) 0.053(3) 0.032(3) -0.009(2) -0.011(2) -0.019(3) O4 0.057(3) 0.049(3) 0.028(2) -0.007(2) -0.009(2) -0.015(2) C1 0.113(7) 0.064(5) 0.062(6) -0.022(5) -0.017(5) -0.047(5) C2 0.067(5) 0.066(5) 0.038(4) -0.018(4) -0.002(3) -0.033(4) C3 0.041(4) 0.043(4) 0.041(4) -0.014(3) -0.007(3) -0.016(3) C4 0.043(4) 0.042(4) 0.037(4) -0.009(3) -0.006(3) -0.013(3) C5 0.091(6) 0.057(5) 0.029(4) -0.004(3) -0.001(4) -0.042(5) C6 0.118(8) 0.078(6) 0.047(5) -0.010(4) 0.000(5) -0.070(6) C7 0.034(3) 0.037(3) 0.031(3) -0.006(3) -0.008(3) -0.003(3) C8 0.039(4) 0.033(3) 0.035(4) -0.009(3) -0.008(3) -0.005(3) C9 0.039(4) 0.034(3) 0.035(4) -0.009(3) -0.009(3) -0.003(3) C10 0.033(3) 0.036(3) 0.037(4) -0.008(3) -0.009(3) -0.002(3) C11 0.046(4) 0.041(4) 0.037(4) -0.008(3) -0.008(3) -0.014(3) C12 0.077(5) 0.050(4) 0.041(4) -0.011(3) -0.007(4) -0.028(4) C13 0.079(5) 0.060(5) 0.043(4) -0.016(4) -0.010(4) -0.031(4) C14 0.046(4) 0.044(4) 0.038(4) -0.011(3) -0.011(3) -0.008(3) C15 0.142(9) 0.069(6) 0.055(5) -0.017(5) -0.005(6) -0.059(6) C16 0.221(15) 0.106(9) 0.066(7) -0.018(6) -0.010(8) -0.109(10) C17 0.275(18) 0.098(9) 0.072(8) -0.035(7) -0.019(9) -0.106(11) C18 0.167(11) 0.106(8) 0.049(5) -0.033(5) 0.007(6) -0.091(8) C19 0.063(5) 0.043(4) 0.061(5) -0.023(4) -0.014(4) -0.014(4) C20 0.046(4) 0.062(5) 0.057(5) -0.018(4) -0.013(3) -0.014(4) C21 0.060(5) 0.046(4) 0.065(5) -0.025(4) -0.016(4) -0.007(4) C22 0.052(4) 0.055(5) 0.051(4) -0.020(4) -0.009(3) -0.015(4) C23 0.106(8) 0.061(6) 0.054(5) -0.017(4) -0.043(5) 0.033(6) C24 0.086(7) 0.044(5) 0.050(5) 0.004(4) -0.028(5) -0.011(4) C25 0.051(5) 0.086(6) 0.026(4) 0.002(4) -0.009(3) -0.011(4) C26 0.095(7) 0.061(5) 0.046(5) -0.007(4) -0.042(5) -0.004(5) C27 0.046(5) 0.111(8) 0.038(4) 0.018(5) -0.024(4) -0.013(5) C28 0.27(2) 0.161(13) 0.121(11) -0.091(11) -0.094(13) 0.156(14) C29 0.208(15) 0.073(7) 0.149(12) 0.027(8) -0.071(11) -0.085(9) C30 0.083(8) 0.239(17) 0.048(6) -0.023(8) 0.010(5) 0.000(9) C31 0.31(2) 0.081(8) 0.158(13) -0.038(9) -0.161(15) -0.024(11) C32 0.060(7) 0.254(18) 0.097(9) 0.014(10) -0.028(6) -0.058(9) C33 0.101(8) 0.137(11) 0.064(6) -0.065(7) 0.035(6) -0.067(8) C34 0.125(9) 0.071(6) 0.032(5) -0.016(4) 0.006(5) -0.011(6) C35 0.111(8) 0.109(9) 0.034(5) -0.040(5) -0.004(5) -0.017(7) C36 0.174(12) 0.063(6) 0.056(6) -0.043(5) 0.021(7) -0.018(7) C37 0.087(8) 0.112(10) 0.075(7) -0.053(7) 0.011(6) 0.001(7) C38 0.182(14) 0.236(18) 0.120(11) -0.087(12) 0.062(10) -0.156(15) C39 0.267(18) 0.075(8) 0.054(7) -0.001(6) -0.012(9) 0.015(10) C40 0.161(13) 0.28(2) 0.104(10) -0.105(13) -0.042(9) -0.051(14) C41 0.32(2) 0.119(11) 0.101(10) -0.070(9) 0.078(12) -0.104(14) C42 0.161(15) 0.31(3) 0.168(17) -0.082(17) -0.026(13) 0.169(18) S1 0.0640(13) 0.0714(15) 0.0666(14) -0.0204(12) -0.0138(11) -0.0149(11) O5 0.111(6) 0.071(4) 0.136(7) -0.001(4) -0.055(5) -0.015(4) O6 0.109(6) 0.104(6) 0.132(7) -0.038(5) -0.067(5) -0.014(4) O7 0.120(6) 0.130(7) 0.091(6) -0.009(5) 0.014(5) -0.048(5) C43 0.122(11) 0.102(10) 0.117(11) -0.036(9) 0.002(9) -0.035(9) F1 0.176(9) 0.39(2) 0.172(10) -0.178(12) 0.059(8) -0.075(11) F2 0.170(9) 0.135(8) 0.341(17) -0.123(10) -0.073(10) 0.019(7) F3 0.251(12) 0.225(11) 0.160(8) -0.113(8) -0.053(8) -0.088(9) S2 0.172(5) 0.409(11) 0.308(9) -0.291(9) -0.088(5) 0.060(6) C45 0.127(13) 0.152(15) 0.23(2) -0.053(15) -0.030(13) -0.042(12) Cl1 0.140(4) 0.197(5) 0.208(5) -0.060(4) -0.021(3) -0.002(3) Cl2 0.263(8) 0.190(6) 0.353(11) -0.087(7) -0.098(8) -0.032(6) O11 0.172(9) 0.126(7) 0.124(7) -0.064(6) 0.008(6) -0.030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.055(5) . ? Rh1 O1 2.057(4) . ? Rh1 C26 2.117(8) . ? Rh1 C24 2.128(7) . ? Rh1 C23 2.134(8) . ? Rh1 N1 2.134(6) . ? Rh1 C27 2.136(7) . ? Rh1 C25 2.139(7) . ? Rh2 O4 2.031(4) . ? Rh2 O3 2.049(5) . ? Rh2 C37 2.107(10) . ? Rh2 C36 2.109(9) . ? Rh2 C34 2.129(8) . ? Rh2 N2 2.138(6) 2_565 ? Rh2 C33 2.144(9) . ? Rh2 C35 2.147(8) . ? N1 C20 1.322(9) . ? N1 C19 1.331(9) . ? N2 C22 1.335(9) . ? N2 C21 1.349(9) . ? N2 Rh2 2.138(6) 2_565 ? O1 C7 1.278(7) . ? O2 C11 1.282(8) . ? O3 C14 1.289(8) . ? O4 C10 1.298(8) . ? C1 C2 1.363(10) . ? C1 C6 1.401(12) . ? C2 C3 1.398(9) . ? C3 C4 1.394(9) . ? C3 C7 1.464(9) . ? C4 C5 1.397(9) . ? C4 C10 1.452(9) . ? C5 C6 1.352(11) . ? C7 C8 1.422(9) . ? C8 C11 1.427(9) . ? C8 C9 1.487(9) . ? C9 C14 1.398(9) . ? C9 C10 1.419(9) . ? C11 C12 1.474(10) . ? C12 C13 1.379(10) . ? C12 C15 1.428(10) . ? C13 C18 1.415(11) . ? C13 C14 1.454(10) . ? C15 C16 1.351(13) . ? C16 C17 1.394(14) . ? C17 C18 1.360(13) . ? C19 C22 1.399(10) . ? C20 C21 1.387(10) . ? C23 C24 1.395(13) . ? C23 C27 1.453(14) . ? C23 C28 1.488(14) . ? C24 C25 1.376(12) . ? C24 C29 1.502(14) . ? C25 C26 1.359(12) . ? C25 C30 1.557(13) . ? C26 C27 1.460(13) . ? C26 C31 1.537(14) . ? C27 C32 1.496(12) . ? C33 C37 1.398(16) . ? C33 C34 1.427(15) . ? C33 C38 1.479(15) . ? C34 C35 1.398(14) . ? C34 C39 1.493(13) . ? C35 C36 1.359(15) . ? C35 C40 1.558(16) . ? C36 C37 1.401(16) . ? C36 C41 1.570(15) . ? C37 C42 1.534(17) . ? S1 O5 1.407(7) . ? S1 O7 1.421(7) . ? S1 O6 1.421(7) . ? S1 C43 1.830(15) . ? C43 F1 1.278(15) . ? C43 F2 1.334(16) . ? C43 F3 1.352(16) . ? S2 O8 1.376(8) . ? S2 O9 1.389(8) . ? S2 O10 1.452(9) . ? S2 C44 1.740(8) . ? C44 F5 1.308(9) . ? C44 F6 1.320(9) . ? C44 F4 1.326(9) . ? C45 Cl2 1.703(18) . ? C45 Cl1 1.776(17) . ? 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 O2 Rh1 O1 85.51(18) . . ? O2 Rh1 C26 162.3(3) . . ? O1 Rh1 C26 107.4(3) . . ? O2 Rh1 C24 99.7(3) . . ? O1 Rh1 C24 161.0(3) . . ? C26 Rh1 C24 64.2(3) . . ? O2 Rh1 C23 97.1(3) . . ? O1 Rh1 C23 123.3(4) . . ? C26 Rh1 C23 65.8(3) . . ? C24 Rh1 C23 38.2(4) . . ? O2 Rh1 N1 86.1(2) . . ? O1 Rh1 N1 84.4(2) . . ? C26 Rh1 N1 106.8(3) . . ? C24 Rh1 N1 114.0(3) . . ? C23 Rh1 N1 152.2(4) . . ? O2 Rh1 C27 128.1(4) . . ? O1 Rh1 C27 97.0(3) . . ? C26 Rh1 C27 40.1(4) . . ? C24 Rh1 C27 65.3(3) . . ? C23 Rh1 C27 39.8(4) . . ? N1 Rh1 C27 145.8(4) . . ? O2 Rh1 C25 132.1(3) . . ? O1 Rh1 C25 142.3(3) . . ? C26 Rh1 C25 37.2(3) . . ? C24 Rh1 C25 37.6(3) . . ? C23 Rh1 C25 63.5(3) . . ? N1 Rh1 C25 94.0(3) . . ? C27 Rh1 C25 64.3(3) . . ? O4 Rh2 O3 86.11(18) . . ? O4 Rh2 C37 107.2(4) . . ? O3 Rh2 C37 107.2(4) . . ? O4 Rh2 C36 143.8(5) . . ? O3 Rh2 C36 93.3(3) . . ? C37 Rh2 C36 38.8(5) . . ? O4 Rh2 C34 120.9(4) . . ? O3 Rh2 C34 152.9(4) . . ? C37 Rh2 C34 65.0(4) . . ? C36 Rh2 C34 64.0(4) . . ? O4 Rh2 N2 84.2(2) . 2_565 ? O3 Rh2 N2 85.4(2) . 2_565 ? C37 Rh2 N2 163.2(4) . 2_565 ? C36 Rh2 N2 131.9(5) . 2_565 ? C34 Rh2 N2 98.8(3) . 2_565 ? O4 Rh2 C33 96.8(3) . . ? O3 Rh2 C33 144.7(4) . . ? C37 Rh2 C33 38.4(4) . . ? C36 Rh2 C33 64.1(4) . . ? C34 Rh2 C33 39.0(4) . . ? N2 Rh2 C33 129.9(4) 2_565 . ? O4 Rh2 C35 158.6(3) . . ? O3 Rh2 C35 114.8(3) . . ? C37 Rh2 C35 63.8(4) . . ? C36 Rh2 C35 37.2(4) . . ? C34 Rh2 C35 38.2(4) . . ? N2 Rh2 C35 101.2(3) 2_565 . ? C33 Rh2 C35 63.8(4) . . ? C20 N1 C19 116.2(6) . . ? C20 N1 Rh1 120.9(5) . . ? C19 N1 Rh1 121.9(5) . . ? C22 N2 C21 116.8(6) . . ? C22 N2 Rh2 121.8(5) . 2_565 ? C21 N2 Rh2 121.4(5) . 2_565 ? C7 O1 Rh1 130.3(4) . . ? C11 O2 Rh1 129.7(4) . . ? C14 O3 Rh2 128.6(4) . . ? C10 O4 Rh2 130.6(4) . . ? C2 C1 C6 120.1(7) . . ? C1 C2 C3 120.1(7) . . ? C4 C3 C2 120.2(6) . . ? C4 C3 C7 120.3(6) . . ? C2 C3 C7 119.5(6) . . ? C3 C4 C5 118.0(6) . . ? C3 C4 C10 120.7(6) . . ? C5 C4 C10 121.2(6) . . ? C6 C5 C4 121.9(7) . . ? C5 C6 C1 119.7(7) . . ? O1 C7 C8 126.1(6) . . ? O1 C7 C3 114.3(6) . . ? C8 C7 C3 119.6(6) . . ? C7 C8 C11 121.0(6) . . ? C7 C8 C9 120.2(5) . . ? C11 C8 C9 118.8(6) . . ? C14 C9 C10 121.8(6) . . ? C14 C9 C8 119.9(6) . . ? C10 C9 C8 118.3(6) . . ? O4 C10 C9 124.9(6) . . ? O4 C10 C4 114.2(6) . . ? C9 C10 C4 120.9(6) . . ? O2 C11 C8 126.6(6) . . ? O2 C11 C12 113.6(6) . . ? C8 C11 C12 119.8(6) . . ? C13 C12 C15 121.5(7) . . ? C13 C12 C11 119.5(6) . . ? C15 C12 C11 119.0(7) . . ? C12 C13 C18 118.1(7) . . ? C12 C13 C14 121.8(7) . . ? C18 C13 C14 120.1(7) . . ? O3 C14 C9 127.3(6) . . ? O3 C14 C13 112.8(6) . . ? C9 C14 C13 119.8(6) . . ? C16 C15 C12 118.3(9) . . ? C15 C16 C17 120.8(9) . . ? C18 C17 C16 121.2(9) . . ? C17 C18 C13 119.9(9) . . ? N1 C19 C22 122.1(7) . . ? N1 C20 C21 122.9(7) . . ? N2 C21 C20 120.6(7) . . ? N2 C22 C19 121.0(7) . . ? C24 C23 C27 107.7(8) . . ? C24 C23 C28 132.3(13) . . ? C27 C23 C28 120.0(13) . . ? C24 C23 Rh1 70.6(4) . . ? C27 C23 Rh1 70.2(4) . . ? C28 C23 Rh1 123.3(7) . . ? C25 C24 C23 108.5(8) . . ? C25 C24 C29 124.6(11) . . ? C23 C24 C29 126.9(11) . . ? C25 C24 Rh1 71.7(4) . . ? C23 C24 Rh1 71.2(5) . . ? C29 C24 Rh1 123.4(7) . . ? C26 C25 C24 111.2(8) . . ? C26 C25 C30 121.7(10) . . ? C24 C25 C30 127.1(10) . . ? C26 C25 Rh1 70.5(4) . . ? C24 C25 Rh1 70.7(4) . . ? C30 C25 Rh1 123.7(6) . . ? C25 C26 C27 107.6(8) . . ? C25 C26 C31 129.9(11) . . ? C27 C26 C31 122.3(11) . . ? C25 C26 Rh1 72.3(4) . . ? C27 C26 Rh1 70.6(4) . . ? C31 C26 Rh1 126.0(6) . . ? C23 C27 C26 105.0(7) . . ? C23 C27 C32 129.7(12) . . ? C26 C27 C32 125.2(12) . . ? C23 C27 Rh1 70.0(4) . . ? C26 C27 Rh1 69.2(4) . . ? C32 C27 Rh1 122.7(6) . . ? C37 C33 C34 107.3(9) . . ? C37 C33 C38 126.7(15) . . ? C34 C33 C38 126.0(14) . . ? C37 C33 Rh2 69.4(6) . . ? C34 C33 Rh2 69.9(5) . . ? C38 C33 Rh2 123.4(7) . . ? C35 C34 C33 106.8(9) . . ? C35 C34 C39 126.2(13) . . ? C33 C34 C39 126.6(13) . . ? C35 C34 Rh2 71.6(5) . . ? C33 C34 Rh2 71.1(5) . . ? C39 C34 Rh2 127.5(7) . . ? C36 C35 C34 109.1(10) . . ? C36 C35 C40 124.5(13) . . ? C34 C35 C40 126.3(12) . . ? C36 C35 Rh2 69.9(5) . . ? C34 C35 Rh2 70.2(5) . . ? C40 C35 Rh2 123.0(7) . . ? C35 C36 C37 109.0(10) . . ? C35 C36 C41 125.3(15) . . ? C37 C36 C41 125.6(14) . . ? C35 C36 Rh2 72.9(5) . . ? C37 C36 Rh2 70.5(6) . . ? C41 C36 Rh2 123.9(7) . . ? C33 C37 C36 107.6(11) . . ? C33 C37 C42 128.5(16) . . ? C36 C37 C42 123.8(15) . . ? C33 C37 Rh2 72.3(6) . . ? C36 C37 Rh2 70.7(6) . . ? C42 C37 Rh2 124.1(9) . . ? O5 S1 O7 114.1(5) . . ? O5 S1 O6 114.1(5) . . ? O7 S1 O6 116.5(5) . . ? O5 S1 C43 105.9(7) . . ? O7 S1 C43 100.9(6) . . ? O6 S1 C43 102.8(6) . . ? F1 C43 F2 112.4(16) . . ? F1 C43 F3 108.1(14) . . ? F2 C43 F3 112.1(12) . . ? F1 C43 S1 109.5(11) . . ? F2 C43 S1 107.6(11) . . ? F3 C43 S1 107.1(11) . . ? O8 S2 O9 120.6(9) . . ? O8 S2 O10 111.5(8) . . ? O9 S2 O10 109.9(8) . . ? O8 S2 C44 105.2(7) . . ? O9 S2 C44 105.4(7) . . ? O10 S2 C44 102.4(7) . . ? F5 C44 F6 105.1(9) . . ? F5 C44 F4 107.4(9) . . ? F6 C44 F4 104.0(8) . . ? F5 C44 S2 112.2(8) . . ? F6 C44 S2 114.5(8) . . ? F4 C44 S2 112.9(8) . . ? Cl2 C45 Cl1 106.8(12) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.232 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.126 # Attachment 'Complex 3b.cif' data_Complex_3b'' _database_code_depnum_ccdc_archive 'CCDC 749417' #TrackingRef 'Complex 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H86 Cl F12 N4 O22 Rh4 S4' _chemical_formula_weight 2366.95 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' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.116(5) _cell_length_b 13.323(5) _cell_length_c 16.789(6) _cell_angle_alpha 66.999(5) _cell_angle_beta 77.240(5) _cell_angle_gamma 76.853(5) _cell_volume 2601.1(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 2.592 _cell_measurement_theta_max 22.707 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1193 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9083 _exptl_absorpt_correction_T_max 0.9375 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.75 _diffrn_reflns_number 10768 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8961 _reflns_number_gt 5038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8961 _refine_ls_number_parameters 585 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1907 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.72721(5) 0.54410(5) 0.28983(4) 0.0425(2) Uani 1 1 d . . . Rh2 Rh 0.78273(5) 0.79320(5) -0.26010(4) 0.0402(2) Uani 1 1 d . . . N1 N 0.8789(5) 0.4510(6) 0.2600(4) 0.0442(17) Uani 1 1 d . . . N2 N 1.0697(5) 0.3187(5) 0.2450(4) 0.0419(16) Uani 1 1 d . . . O1 O 0.7782(5) 0.6763(4) 0.1889(4) 0.0497(15) Uani 1 1 d . . . O2 O 0.6817(4) 0.5075(4) 0.1972(3) 0.0445(14) Uani 1 1 d . . . O3 O 0.7178(5) 0.6670(4) -0.1578(3) 0.0469(14) Uani 1 1 d . . . O4 O 0.8146(5) 0.8371(4) -0.1647(3) 0.0496(15) Uani 1 1 d . . . O5 O 0.6818(7) 0.1901(7) 0.3352(6) 0.104(3) Uani 1 1 d . . . O6 O 0.8398(7) 0.0889(7) 0.3969(6) 0.098(3) Uani 1 1 d . . . O7 O 0.6858(8) 0.0028(9) 0.4289(5) 0.128(4) Uani 1 1 d . . . O8 O 0.2601(10) 0.6244(11) 0.3509(8) 0.201(6) Uiso 1 1 d D . . O9 O 0.1200(12) 0.5416(11) 0.3455(10) 0.237(8) Uiso 1 1 d D . . O10 O 0.2244(16) 0.6373(17) 0.2073(7) 0.337(12) Uiso 1 1 d D . . F1 F 0.7185(8) 0.0280(8) 0.2463(5) 0.136(3) Uani 1 1 d . . . F2 F 0.8494(9) 0.1117(10) 0.2171(6) 0.182(5) Uani 1 1 d . . . F3 F 0.8528(8) -0.0552(10) 0.2998(9) 0.185(5) Uani 1 1 d . . . F4 F 0.1143(16) 0.8394(14) 0.2554(12) 0.343(10) Uiso 1 1 d D . . F5 F 0.0572(12) 0.7262(11) 0.3749(9) 0.238(6) Uiso 1 1 d D . . F6 F 0.0071(13) 0.7459(13) 0.2574(9) 0.268(7) Uiso 1 1 d D . . S1 S 0.7448(2) 0.0849(2) 0.37026(17) 0.0652(7) Uani 1 1 d D . . S2 S 0.1939(5) 0.6240(7) 0.2953(4) 0.203(3) Uani 1 1 d D . . C1 C 0.7734(7) 0.7099(7) 0.1062(5) 0.043(2) Uani 1 1 d . . . C2 C 0.7396(6) 0.6510(6) 0.0640(5) 0.0352(18) Uani 1 1 d . . . C3 C 0.6975(6) 0.5524(6) 0.1129(5) 0.0388(19) Uani 1 1 d . . . C4 C 0.6647(6) 0.4934(6) 0.0688(5) 0.0399(19) Uani 1 1 d . . . C5 C 0.6319(8) 0.3920(8) 0.1139(6) 0.063(3) Uani 1 1 d . . . H5 H 0.6288 0.3618 0.1744 0.075 Uiso 1 1 calc R . . C6 C 0.6045(10) 0.3358(9) 0.0730(6) 0.087(4) Uani 1 1 d . . . H6 H 0.5786 0.2699 0.1057 0.104 Uiso 1 1 calc R . . C7 C 0.6146(11) 0.3756(9) -0.0196(7) 0.088(4) Uani 1 1 d . . . H7 H 0.5995 0.3346 -0.0483 0.106 Uiso 1 1 calc R . . C8 C 0.6470(9) 0.4760(9) -0.0657(6) 0.069(3) Uani 1 1 d . . . H8 H 0.6505 0.5051 -0.1262 0.083 Uiso 1 1 calc R . . C9 C 0.6748(7) 0.5356(7) -0.0238(5) 0.042(2) Uani 1 1 d . . . C10 C 0.7167(6) 0.6388(6) -0.0760(5) 0.0382(19) Uani 1 1 d . . . C11 C 0.7497(6) 0.6955(6) -0.0321(5) 0.0373(18) Uani 1 1 d . . . C12 C 0.7917(6) 0.7960(6) -0.0805(5) 0.0401(19) Uani 1 1 d . . . C13 C 0.8145(8) 0.8582(7) -0.0352(5) 0.055(2) Uani 1 1 d . . . C14 C 0.8408(11) 0.9626(9) -0.0809(7) 0.092(4) Uani 1 1 d . . . H14 H 0.8442 0.9912 -0.1415 0.111 Uiso 1 1 calc R . . C15 C 0.8620(15) 1.0248(11) -0.0409(8) 0.136(7) Uani 1 1 d . . . H15 H 0.8828 1.0933 -0.0738 0.163 Uiso 1 1 calc R . . C16 C 0.8521(14) 0.9848(10) 0.0512(8) 0.125(6) Uani 1 1 d . . . H16 H 0.8635 1.0281 0.0795 0.150 Uiso 1 1 calc R . . C17 C 0.8256(11) 0.8814(9) 0.0990(7) 0.095(5) Uani 1 1 d . . . H17 H 0.8207 0.8535 0.1596 0.114 Uiso 1 1 calc R . . C18 C 0.8054(8) 0.8173(7) 0.0544(5) 0.052(2) Uani 1 1 d . . . C19 C 0.8851(7) 0.3487(7) 0.2607(5) 0.045(2) Uani 1 1 d . . . H19 H 0.8234 0.3223 0.2653 0.055 Uiso 1 1 calc R . . C20 C 0.9795(7) 0.2838(7) 0.2547(5) 0.048(2) Uani 1 1 d . . . H20 H 0.9812 0.2123 0.2575 0.058 Uiso 1 1 calc R . . C21 C 1.0655(7) 0.4219(7) 0.2390(6) 0.051(2) Uani 1 1 d . . . H21 H 1.1275 0.4502 0.2296 0.062 Uiso 1 1 calc R . . C22 C 0.9669(7) 0.4877(7) 0.2470(6) 0.049(2) Uani 1 1 d . . . H22 H 0.9645 0.5599 0.2428 0.059 Uiso 1 1 calc R . . C23 C 0.7432(10) 0.5296(12) 0.4175(6) 0.082(4) Uani 1 1 d . . . C24 C 0.6777(13) 0.6319(9) 0.3762(7) 0.082(4) Uani 1 1 d . . . C25 C 0.5899(10) 0.6058(11) 0.3584(8) 0.085(4) Uani 1 1 d . . . C26 C 0.6000(10) 0.4883(10) 0.3895(7) 0.072(3) Uani 1 1 d . . . C27 C 0.6945(9) 0.4445(8) 0.4251(6) 0.060(3) Uani 1 1 d . . . C28 C 0.8487(13) 0.5179(14) 0.4482(8) 0.134(6) Uani 1 1 d . . . H28A H 0.8804 0.5830 0.4146 0.202 Uiso 1 1 calc R . . H28B H 0.8955 0.4546 0.4402 0.202 Uiso 1 1 calc R . . H28C H 0.8361 0.5087 0.5090 0.202 Uiso 1 1 calc R . . C29 C 0.7068(15) 0.7455(10) 0.3530(10) 0.142(7) Uani 1 1 d . . . H29A H 0.6709 0.7982 0.3058 0.213 Uiso 1 1 calc R . . H29B H 0.7819 0.7425 0.3354 0.213 Uiso 1 1 calc R . . H29C H 0.6860 0.7673 0.4031 0.213 Uiso 1 1 calc R . . C30 C 0.5014(12) 0.6878(14) 0.3153(12) 0.167(8) Uani 1 1 d . . . H30A H 0.4767 0.6599 0.2794 0.251 Uiso 1 1 calc R . . H30B H 0.5263 0.7563 0.2796 0.251 Uiso 1 1 calc R . . H30C H 0.4444 0.6996 0.3592 0.251 Uiso 1 1 calc R . . C31 C 0.5167(11) 0.4279(12) 0.3802(10) 0.123(5) Uani 1 1 d . . . H31A H 0.4648 0.4127 0.4319 0.184 Uiso 1 1 calc R . . H31B H 0.5515 0.3599 0.3728 0.184 Uiso 1 1 calc R . . H31C H 0.4825 0.4741 0.3302 0.184 Uiso 1 1 calc R . . C32 C 0.7340(12) 0.3231(9) 0.4678(7) 0.101(5) Uani 1 1 d . . . H32A H 0.6954 0.2958 0.5256 0.151 Uiso 1 1 calc R . . H32B H 0.8080 0.3126 0.4713 0.151 Uiso 1 1 calc R . . H32C H 0.7237 0.2838 0.4337 0.151 Uiso 1 1 calc R . . C33 C 0.7189(11) 0.8009(9) -0.3679(7) 0.073(3) Uani 1 1 d . . . C34 C 0.6473(8) 0.8658(11) -0.3255(7) 0.079(4) Uani 1 1 d . . . C35 C 0.7033(10) 0.9508(9) -0.3305(6) 0.070(3) Uani 1 1 d . . . C36 C 0.8015(9) 0.9353(8) -0.3741(6) 0.062(3) Uani 1 1 d . . . C37 C 0.8131(9) 0.8476(10) -0.4002(6) 0.069(3) Uani 1 1 d . . . C38 C 0.6947(18) 0.7041(12) -0.3802(12) 0.198(12) Uani 1 1 d . . . H38A H 0.6692 0.7281 -0.4352 0.297 Uiso 1 1 calc R . . H38B H 0.6415 0.6712 -0.3336 0.297 Uiso 1 1 calc R . . H38C H 0.7577 0.6507 -0.3798 0.297 Uiso 1 1 calc R . . C39 C 0.5373(10) 0.8532(19) -0.2840(10) 0.225(13) Uani 1 1 d . . . H39A H 0.4915 0.8853 -0.3280 0.338 Uiso 1 1 calc R . . H39B H 0.5164 0.8899 -0.2425 0.338 Uiso 1 1 calc R . . H39C H 0.5323 0.7762 -0.2546 0.338 Uiso 1 1 calc R . . C40 C 0.6528(15) 1.0403(12) -0.2909(10) 0.170(9) Uani 1 1 d . . . H40A H 0.6475 1.0081 -0.2284 0.256 Uiso 1 1 calc R . . H40B H 0.5834 1.0712 -0.3070 0.256 Uiso 1 1 calc R . . H40C H 0.6960 1.0974 -0.3127 0.256 Uiso 1 1 calc R . . C41 C 0.8842(11) 1.0092(11) -0.3933(10) 0.132(6) Uani 1 1 d . . . H41A H 0.9445 0.9891 -0.4315 0.199 Uiso 1 1 calc R . . H41B H 0.9058 1.0001 -0.3396 0.199 Uiso 1 1 calc R . . H41C H 0.8542 1.0849 -0.4210 0.199 Uiso 1 1 calc R . . C42 C 0.9132(12) 0.8066(13) -0.4538(7) 0.145(7) Uani 1 1 d . . . H42A H 0.9189 0.7284 -0.4389 0.218 Uiso 1 1 calc R . . H42B H 0.9745 0.8220 -0.4408 0.218 Uiso 1 1 calc R . . H42C H 0.9088 0.8437 -0.5150 0.218 Uiso 1 1 calc R . . C43 C 0.7944(12) 0.0378(12) 0.2805(9) 0.097(4) Uani 1 1 d D . . C44 C 0.0926(12) 0.7375(11) 0.2923(10) 0.247(12) Uiso 1 1 d D . . O11 O 0.4930(9) 0.1174(8) 0.5309(7) 0.133(4) Uani 1 1 d . . . C45 C 0.021(2) 0.5474(15) 0.9635(4) 0.127(11) Uiso 0.50 1 d PD . . H45A H -0.0316 0.5889 0.9257 0.152 Uiso 0.50 1 calc PR . . H45B H 0.0829 0.5201 0.9291 0.152 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0570(17) 0.6329(12) 1.0050(15) 0.345(11) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0525(5) 0.0435(4) 0.0275(4) -0.0121(3) -0.0006(3) -0.0065(3) Rh2 0.0424(4) 0.0443(4) 0.0272(4) -0.0049(3) -0.0040(3) -0.0096(3) N1 0.044(4) 0.050(4) 0.043(4) -0.020(3) -0.014(3) -0.004(3) N2 0.046(4) 0.042(4) 0.035(4) -0.008(3) -0.009(3) -0.011(3) O1 0.071(4) 0.047(3) 0.037(3) -0.011(3) -0.013(3) -0.020(3) O2 0.055(4) 0.043(3) 0.032(3) -0.004(3) -0.007(3) -0.017(3) O3 0.058(4) 0.053(4) 0.027(3) -0.008(3) -0.001(3) -0.021(3) O4 0.068(4) 0.048(3) 0.030(3) -0.006(3) 0.002(3) -0.027(3) O5 0.092(6) 0.090(6) 0.149(8) -0.062(6) -0.052(6) 0.019(5) O6 0.087(6) 0.119(7) 0.105(6) -0.037(5) -0.043(5) -0.026(5) O7 0.139(9) 0.164(9) 0.068(6) -0.002(6) 0.006(5) -0.091(7) F1 0.163(8) 0.181(9) 0.120(7) -0.088(6) -0.018(6) -0.073(7) F2 0.215(11) 0.273(13) 0.115(7) -0.118(8) 0.088(7) -0.171(10) F3 0.115(8) 0.172(10) 0.307(16) -0.162(11) -0.033(9) 0.043(7) S1 0.0601(17) 0.0785(19) 0.0587(16) -0.0240(14) -0.0099(13) -0.0145(14) S2 0.173(6) 0.340(9) 0.160(5) -0.175(6) -0.051(4) 0.017(6) C1 0.044(5) 0.052(5) 0.035(5) -0.017(4) -0.005(4) -0.007(4) C2 0.037(5) 0.031(4) 0.031(4) -0.007(3) 0.001(3) -0.004(3) C3 0.029(4) 0.045(5) 0.037(5) -0.010(4) -0.007(3) 0.000(4) C4 0.041(5) 0.042(5) 0.034(4) -0.008(4) -0.006(4) -0.010(4) C5 0.093(8) 0.061(6) 0.033(5) -0.004(5) 0.000(5) -0.043(6) C6 0.150(12) 0.083(8) 0.040(6) -0.007(5) 0.001(6) -0.084(8) C7 0.150(12) 0.076(8) 0.054(7) -0.010(6) -0.012(7) -0.073(8) C8 0.099(8) 0.083(7) 0.034(5) -0.017(5) 0.000(5) -0.048(7) C9 0.048(5) 0.047(5) 0.035(4) -0.009(4) -0.008(4) -0.020(4) C10 0.036(5) 0.046(5) 0.029(4) -0.009(4) -0.003(3) -0.010(4) C11 0.039(5) 0.040(5) 0.033(4) -0.012(4) -0.009(4) -0.004(4) C12 0.045(5) 0.039(5) 0.028(4) -0.002(4) -0.005(4) -0.007(4) C13 0.087(7) 0.045(5) 0.033(5) -0.008(4) -0.001(5) -0.031(5) C14 0.166(13) 0.080(8) 0.043(6) -0.015(6) -0.007(7) -0.066(8) C15 0.28(2) 0.103(10) 0.051(7) -0.020(7) -0.002(10) -0.124(13) C16 0.26(2) 0.084(9) 0.061(8) -0.015(7) -0.034(10) -0.098(11) C17 0.174(14) 0.089(8) 0.045(6) -0.014(6) -0.014(7) -0.083(9) C18 0.076(7) 0.044(5) 0.041(5) -0.014(4) -0.003(5) -0.024(5) C19 0.045(5) 0.043(5) 0.049(5) -0.015(4) -0.011(4) -0.005(4) C20 0.052(6) 0.046(5) 0.047(5) -0.015(4) -0.004(4) -0.014(5) C21 0.054(6) 0.057(6) 0.047(5) -0.015(5) -0.011(4) -0.018(5) C22 0.055(6) 0.045(5) 0.050(5) -0.021(4) -0.004(4) -0.010(5) C23 0.108(10) 0.117(11) 0.033(5) -0.036(6) 0.010(6) -0.046(9) C24 0.138(12) 0.060(7) 0.047(6) -0.037(6) 0.030(7) -0.023(8) C25 0.065(8) 0.085(9) 0.081(8) -0.034(7) 0.023(6) 0.012(7) C26 0.089(9) 0.079(8) 0.048(6) -0.029(6) 0.025(6) -0.035(7) C27 0.091(8) 0.059(6) 0.028(5) -0.014(4) 0.002(5) -0.022(6) C28 0.157(15) 0.209(17) 0.071(9) -0.056(10) -0.025(9) -0.077(13) C29 0.24(2) 0.080(10) 0.117(12) -0.065(9) 0.044(12) -0.067(11) C30 0.096(12) 0.162(16) 0.176(18) -0.050(14) 0.009(11) 0.061(11) C31 0.098(11) 0.130(12) 0.135(13) -0.037(10) 0.016(9) -0.060(10) C32 0.173(14) 0.074(8) 0.042(7) -0.008(6) -0.013(8) -0.022(8) C33 0.111(10) 0.056(7) 0.056(7) 0.002(5) -0.049(7) -0.026(7) C34 0.043(6) 0.107(10) 0.047(6) 0.020(6) -0.017(5) -0.012(6) C35 0.076(8) 0.068(7) 0.048(6) -0.015(5) -0.019(6) 0.025(6) C36 0.071(7) 0.053(6) 0.043(6) 0.007(5) -0.014(5) -0.013(5) C37 0.077(8) 0.080(8) 0.029(5) -0.004(5) -0.015(5) 0.006(6) C38 0.37(3) 0.090(11) 0.195(18) -0.012(11) -0.21(2) -0.062(15) C39 0.048(9) 0.38(3) 0.114(13) 0.072(15) -0.022(8) -0.062(14) C40 0.25(2) 0.119(12) 0.115(12) -0.057(10) -0.088(14) 0.115(14) C41 0.117(12) 0.109(11) 0.133(13) 0.041(9) -0.041(10) -0.075(10) C42 0.142(14) 0.183(15) 0.034(6) -0.019(8) 0.012(7) 0.061(11) C43 0.099(11) 0.102(11) 0.113(11) -0.069(10) 0.013(9) -0.033(9) O11 0.149(10) 0.120(8) 0.125(8) -0.050(7) 0.010(7) -0.028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.030(5) . ? Rh1 O2 2.037(5) . ? Rh1 C25 2.096(10) . ? Rh1 C24 2.111(9) . ? Rh1 C26 2.121(10) . ? Rh1 C23 2.128(10) . ? Rh1 C27 2.138(9) . ? Rh1 N1 2.161(7) . ? Rh2 O4 2.055(5) . ? Rh2 O3 2.062(5) . ? Rh2 C33 2.114(9) . ? Rh2 C36 2.117(9) . ? Rh2 C35 2.122(9) . ? Rh2 C34 2.133(9) . ? Rh2 C37 2.145(9) . ? Rh2 N2 2.154(7) 2_765 ? N1 C22 1.296(10) . ? N1 C19 1.343(10) . ? N2 C20 1.323(10) . ? N2 C21 1.328(10) . ? N2 Rh2 2.154(7) 2_765 ? O1 C1 1.292(9) . ? O2 C3 1.292(9) . ? O3 C10 1.271(9) . ? O4 C12 1.293(9) . ? O5 S1 1.427(8) . ? O6 S1 1.432(7) . ? O7 S1 1.404(8) . ? O8 S2 1.411(8) . ? O9 S2 1.501(8) . ? O10 S2 1.392(9) . ? F1 C43 1.307(15) . ? F2 C43 1.337(15) . ? F3 C43 1.261(16) . ? F4 C44 1.322(9) . ? F5 C44 1.321(10) . ? F6 C44 1.339(9) . ? S1 C43 1.791(11) . ? S2 C44 1.764(12) . ? C1 C2 1.431(11) . ? C1 C18 1.456(11) . ? C2 C3 1.411(11) . ? C2 C11 1.472(10) . ? C3 C4 1.449(11) . ? C4 C5 1.380(11) . ? C4 C9 1.417(11) . ? C5 C6 1.340(12) . ? C6 C7 1.419(13) . ? C7 C8 1.369(13) . ? C8 C9 1.392(11) . ? C9 C10 1.467(11) . ? C10 C11 1.423(10) . ? C11 C12 1.429(11) . ? C12 C13 1.437(11) . ? C13 C18 1.372(11) . ? C13 C14 1.382(12) . ? C14 C15 1.356(14) . ? C15 C16 1.411(15) . ? C16 C17 1.376(14) . ? C17 C18 1.432(12) . ? C19 C20 1.348(11) . ? C21 C22 1.399(12) . ? C23 C27 1.374(14) . ? C23 C24 1.439(17) . ? C23 C28 1.536(17) . ? C24 C25 1.398(17) . ? C24 C29 1.524(15) . ? C25 C26 1.428(15) . ? C25 C30 1.497(18) . ? C26 C27 1.400(15) . ? C26 C31 1.561(15) . ? C27 C32 1.508(14) . ? C33 C34 1.398(16) . ? C33 C37 1.414(15) . ? C33 C38 1.494(15) . ? C34 C35 1.451(16) . ? C34 C39 1.472(16) . ? C35 C36 1.349(14) . ? C35 C40 1.538(15) . ? C36 C37 1.367(14) . ? C36 C41 1.527(14) . ? C37 C42 1.539(15) . ? C45 C45 1.491(5) 2_567 ? C45 Cl1 1.733(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh1 O2 85.7(2) . . ? O1 Rh1 C25 106.5(4) . . ? O2 Rh1 C25 107.4(4) . . ? O1 Rh1 C24 93.1(3) . . ? O2 Rh1 C24 144.1(5) . . ? C25 Rh1 C24 38.8(5) . . ? O1 Rh1 C26 145.0(4) . . ? O2 Rh1 C26 96.3(3) . . ? C25 Rh1 C26 39.6(4) . . ? C24 Rh1 C26 65.2(4) . . ? O1 Rh1 C23 116.6(4) . . ? O2 Rh1 C23 157.5(4) . . ? C25 Rh1 C23 65.5(5) . . ? C24 Rh1 C23 39.7(5) . . ? C26 Rh1 C23 64.3(4) . . ? O1 Rh1 C27 154.1(3) . . ? O2 Rh1 C27 120.0(3) . . ? C25 Rh1 C27 65.2(4) . . ? C24 Rh1 C27 64.8(4) . . ? C26 Rh1 C27 38.4(4) . . ? C23 Rh1 C27 37.6(4) . . ? O1 Rh1 N1 86.6(3) . . ? O2 Rh1 N1 85.1(2) . . ? C25 Rh1 N1 162.2(4) . . ? C24 Rh1 N1 130.7(5) . . ? C26 Rh1 N1 128.4(4) . . ? C23 Rh1 N1 98.0(4) . . ? C27 Rh1 N1 97.7(4) . . ? O4 Rh2 O3 85.4(2) . . ? O4 Rh2 C33 160.8(4) . . ? O3 Rh2 C33 103.1(3) . . ? O4 Rh2 C36 103.1(3) . . ? O3 Rh2 C36 162.4(3) . . ? C33 Rh2 C36 64.4(4) . . ? O4 Rh2 C35 96.2(3) . . ? O3 Rh2 C35 127.6(4) . . ? C33 Rh2 C35 64.9(4) . . ? C36 Rh2 C35 37.1(4) . . ? O4 Rh2 C34 124.1(5) . . ? O3 Rh2 C34 97.9(3) . . ? C33 Rh2 C34 38.4(4) . . ? C36 Rh2 C34 64.6(4) . . ? C35 Rh2 C34 39.9(4) . . ? O4 Rh2 C37 136.8(4) . . ? O3 Rh2 C37 137.6(4) . . ? C33 Rh2 C37 38.8(4) . . ? C36 Rh2 C37 37.4(4) . . ? C35 Rh2 C37 62.8(4) . . ? C34 Rh2 C37 64.1(4) . . ? O4 Rh2 N2 86.2(2) . 2_765 ? O3 Rh2 N2 85.3(2) . 2_765 ? C33 Rh2 N2 111.4(4) . 2_765 ? C36 Rh2 N2 110.3(4) . 2_765 ? C35 Rh2 N2 147.1(4) . 2_765 ? C34 Rh2 N2 149.7(5) . 2_765 ? C37 Rh2 N2 93.3(3) . 2_765 ? C22 N1 C19 117.6(8) . . ? C22 N1 Rh1 122.0(6) . . ? C19 N1 Rh1 120.3(6) . . ? C20 N2 C21 118.0(8) . . ? C20 N2 Rh2 121.7(6) . 2_765 ? C21 N2 Rh2 119.5(6) . 2_765 ? C1 O1 Rh1 130.6(5) . . ? C3 O2 Rh1 130.3(5) . . ? C10 O3 Rh2 129.4(5) . . ? C12 O4 Rh2 130.6(5) . . ? O7 S1 O5 113.6(6) . . ? O7 S1 O6 115.9(6) . . ? O5 S1 O6 114.3(5) . . ? O7 S1 C43 102.6(6) . . ? O5 S1 C43 105.8(7) . . ? O6 S1 C43 102.5(6) . . ? O10 S2 O8 125.2(11) . . ? O10 S2 O9 115.1(10) . . ? O8 S2 O9 109.7(9) . . ? O10 S2 C44 103.0(9) . . ? O8 S2 C44 104.6(8) . . ? O9 S2 C44 92.9(8) . . ? O1 C1 C2 125.5(7) . . ? O1 C1 C18 115.2(7) . . ? C2 C1 C18 119.3(7) . . ? C3 C2 C1 121.0(7) . . ? C3 C2 C11 120.4(7) . . ? C1 C2 C11 118.5(7) . . ? O2 C3 C2 126.0(7) . . ? O2 C3 C4 113.8(7) . . ? C2 C3 C4 120.2(7) . . ? C5 C4 C9 118.4(7) . . ? C5 C4 C3 121.7(7) . . ? C9 C4 C3 119.6(7) . . ? C6 C5 C4 121.9(8) . . ? C5 C6 C7 120.8(9) . . ? C8 C7 C6 118.2(9) . . ? C7 C8 C9 121.4(9) . . ? C8 C9 C4 119.2(7) . . ? C8 C9 C10 119.6(7) . . ? C4 C9 C10 121.2(7) . . ? O3 C10 C11 127.8(7) . . ? O3 C10 C9 113.5(7) . . ? C11 C10 C9 118.7(7) . . ? C10 C11 C12 120.6(7) . . ? C10 C11 C2 119.8(7) . . ? C12 C11 C2 119.6(7) . . ? O4 C12 C11 125.4(7) . . ? O4 C12 C13 114.7(7) . . ? C11 C12 C13 120.0(7) . . ? C18 C13 C14 119.0(8) . . ? C18 C13 C12 120.5(7) . . ? C14 C13 C12 120.4(8) . . ? C15 C14 C13 122.5(10) . . ? C14 C15 C16 119.4(11) . . ? C17 C16 C15 119.7(10) . . ? C16 C17 C18 119.3(10) . . ? C13 C18 C17 120.0(8) . . ? C13 C18 C1 121.5(8) . . ? C17 C18 C1 118.5(8) . . ? N1 C19 C20 120.9(8) . . ? N2 C20 C19 121.9(8) . . ? N2 C21 C22 119.5(8) . . ? N1 C22 C21 121.9(8) . . ? C27 C23 C24 108.1(11) . . ? C27 C23 C28 126.2(13) . . ? C24 C23 C28 125.8(13) . . ? C27 C23 Rh1 71.6(5) . . ? C24 C23 Rh1 69.5(6) . . ? C28 C23 Rh1 124.8(8) . . ? C25 C24 C23 107.4(10) . . ? C25 C24 C29 128.5(14) . . ? C23 C24 C29 124.0(15) . . ? C25 C24 Rh1 70.0(6) . . ? C23 C24 Rh1 70.8(6) . . ? C29 C24 Rh1 121.8(8) . . ? C24 C25 C26 107.7(11) . . ? C24 C25 C30 125.3(14) . . ? C26 C25 C30 127.0(15) . . ? C24 C25 Rh1 71.2(6) . . ? C26 C25 Rh1 71.1(6) . . ? C30 C25 Rh1 123.7(9) . . ? C27 C26 C25 107.7(10) . . ? C27 C26 C31 129.8(11) . . ? C25 C26 C31 122.5(13) . . ? C27 C26 Rh1 71.5(6) . . ? C25 C26 Rh1 69.3(6) . . ? C31 C26 Rh1 123.4(8) . . ? C23 C27 C26 109.2(10) . . ? C23 C27 C32 125.7(12) . . ? C26 C27 C32 125.0(10) . . ? C23 C27 Rh1 70.8(6) . . ? C26 C27 Rh1 70.1(5) . . ? C32 C27 Rh1 127.0(7) . . ? C34 C33 C37 107.7(10) . . ? C34 C33 C38 124.6(15) . . ? C37 C33 C38 127.5(15) . . ? C34 C33 Rh2 71.5(6) . . ? C37 C33 Rh2 71.8(5) . . ? C38 C33 Rh2 125.1(8) . . ? C33 C34 C35 105.7(9) . . ? C33 C34 C39 128.3(16) . . ? C35 C34 C39 126.0(16) . . ? C33 C34 Rh2 70.1(6) . . ? C35 C34 Rh2 69.6(5) . . ? C39 C34 Rh2 124.9(8) . . ? C36 C35 C34 108.2(10) . . ? C36 C35 C40 128.9(14) . . ? C34 C35 C40 122.8(13) . . ? C36 C35 Rh2 71.3(6) . . ? C34 C35 Rh2 70.5(6) . . ? C40 C35 Rh2 124.0(7) . . ? C35 C36 C37 109.9(10) . . ? C35 C36 C41 123.8(12) . . ? C37 C36 C41 126.3(12) . . ? C35 C36 Rh2 71.6(6) . . ? C37 C36 Rh2 72.4(5) . . ? C41 C36 Rh2 124.3(7) . . ? C36 C37 C33 108.3(10) . . ? C36 C37 C42 125.2(13) . . ? C33 C37 C42 126.5(13) . . ? C36 C37 Rh2 70.2(5) . . ? C33 C37 Rh2 69.4(6) . . ? C42 C37 Rh2 125.0(7) . . ? F3 C43 F1 105.3(11) . . ? F3 C43 F2 108.4(13) . . ? F1 C43 F2 106.7(13) . . ? F3 C43 S1 114.5(12) . . ? F1 C43 S1 112.3(10) . . ? F2 C43 S1 109.2(8) . . ? F5 C44 F4 104.1(12) . . ? F5 C44 F6 105.4(12) . . ? F4 C44 F6 101.9(11) . . ? F5 C44 S2 105.5(10) . . ? F4 C44 S2 120.4(14) . . ? F6 C44 S2 117.9(12) . . ? C45 C45 Cl1 110.1(5) 2_567 . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.395 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.144 # Attachment 'Complex 3b.cif' data_Complex_3b''' _database_code_depnum_ccdc_archive 'CCDC 749418' #TrackingRef 'Complex 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H88 Cl4 F12 N4 O22 Rh4 S4' _chemical_formula_weight 2487.32 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.060(5) _cell_length_b 13.310(5) _cell_length_c 16.752(7) _cell_angle_alpha 67.037(6) _cell_angle_beta 77.428(5) _cell_angle_gamma 77.261(6) _cell_volume 2586.8(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 643 _cell_measurement_theta_min 2.242 _cell_measurement_theta_max 20.040 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9153 _exptl_absorpt_correction_T_max 0.9314 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.28 _diffrn_reflns_number 10794 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.2610 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8958 _reflns_number_gt 3432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8958 _refine_ls_number_parameters 604 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 0.741 _refine_ls_restrained_S_all 0.747 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.73120(6) 0.54214(6) 0.29117(5) 0.0393(3) Uani 1 1 d . . . Rh2 Rh 0.78027(6) 0.79371(6) -0.25956(5) 0.0386(2) Uani 1 1 d . . . N1 N 0.8800(6) 0.4523(6) 0.2560(4) 0.0364(19) Uani 1 1 d . . . N2 N 1.0734(6) 0.3180(6) 0.2408(4) 0.041(2) Uani 1 1 d . . . O1 O 0.7814(5) 0.6769(5) 0.1888(4) 0.0453(17) Uani 1 1 d . . . O2 O 0.6838(5) 0.5048(5) 0.1988(4) 0.0434(17) Uani 1 1 d . . . O3 O 0.7148(4) 0.6697(5) -0.1568(4) 0.0442(17) Uani 1 1 d . . . O4 O 0.8085(5) 0.8396(5) -0.1629(4) 0.0521(18) Uani 1 1 d . . . O5 O 0.6866(6) 0.1878(7) 0.3332(6) 0.102(3) Uani 1 1 d . . . O6 O 0.8419(6) 0.0868(6) 0.3977(5) 0.086(2) Uani 1 1 d . . . O7 O 0.6850(7) 0.0016(7) 0.4306(5) 0.112(3) Uani 1 1 d . . . O8 O 0.2655(8) 0.6181(9) 0.3505(7) 0.182(5) Uiso 1 1 d D . . O9 O 0.1277(9) 0.5375(9) 0.3384(7) 0.197(6) Uiso 1 1 d D . . O10 O 0.2255(12) 0.6406(12) 0.2057(6) 0.272(8) Uiso 1 1 d D . . F1 F 0.7190(7) 0.0278(7) 0.2455(5) 0.133(3) Uani 1 1 d . . . F2 F 0.8503(8) 0.1097(9) 0.2167(6) 0.176(5) Uani 1 1 d . . . F3 F 0.8569(7) -0.0540(9) 0.2995(8) 0.175(5) Uani 1 1 d . . . F4 F 0.1258(11) 0.8353(12) 0.2596(9) 0.311(7) Uiso 1 1 d D . . F5 F 0.0521(9) 0.7309(9) 0.3748(7) 0.206(4) Uiso 1 1 d D . . F6 F 0.0185(9) 0.7473(10) 0.2527(7) 0.238(5) Uiso 1 1 d D . . S1 S 0.7477(2) 0.0818(3) 0.3715(2) 0.0633(8) Uani 1 1 d D . . S2 S 0.1985(4) 0.6240(5) 0.2936(3) 0.165(2) Uani 1 1 d D . . C1 C 0.7734(7) 0.7087(7) 0.1085(6) 0.039(2) Uani 1 1 d . . . C2 C 0.7387(6) 0.6513(7) 0.0657(6) 0.032(2) Uani 1 1 d . . . C3 C 0.6982(6) 0.5521(7) 0.1149(6) 0.033(2) Uani 1 1 d . . . C4 C 0.6648(7) 0.4926(8) 0.0697(6) 0.039(2) Uani 1 1 d . . . C5 C 0.6301(8) 0.3901(8) 0.1170(6) 0.058(3) Uani 1 1 d . . . H5 H 0.6235 0.3619 0.1779 0.070 Uiso 1 1 calc R . . C6 C 0.6060(9) 0.3317(9) 0.0741(7) 0.074(4) Uani 1 1 d . . . H6 H 0.5850 0.2629 0.1063 0.088 Uiso 1 1 calc R . . C7 C 0.6121(9) 0.3726(10) -0.0161(7) 0.081(4) Uani 1 1 d . . . H7 H 0.5932 0.3333 -0.0446 0.097 Uiso 1 1 calc R . . C8 C 0.6469(7) 0.4732(8) -0.0629(6) 0.053(3) Uani 1 1 d . . . H8 H 0.6525 0.5009 -0.1237 0.063 Uiso 1 1 calc R . . C9 C 0.6738(7) 0.5339(7) -0.0213(6) 0.037(2) Uani 1 1 d . . . C10 C 0.7144(6) 0.6385(7) -0.0740(6) 0.034(2) Uani 1 1 d . . . C11 C 0.7479(6) 0.6947(7) -0.0298(6) 0.032(2) Uani 1 1 d . . . C12 C 0.7860(7) 0.7975(8) -0.0785(6) 0.042(3) Uani 1 1 d . . . C13 C 0.8102(9) 0.8608(8) -0.0339(6) 0.059(3) Uani 1 1 d . . . C14 C 0.8370(12) 0.9647(10) -0.0805(8) 0.117(6) Uani 1 1 d . . . H14 H 0.8382 0.9958 -0.1409 0.141 Uiso 1 1 calc R . . C15 C 0.8619(17) 1.0216(13) -0.0356(9) 0.197(11) Uani 1 1 d . . . H15 H 0.8821 1.0908 -0.0673 0.236 Uiso 1 1 calc R . . C16 C 0.8584(15) 0.9811(12) 0.0526(9) 0.170(9) Uani 1 1 d . . . H16 H 0.8745 1.0222 0.0809 0.204 Uiso 1 1 calc R . . C17 C 0.8307(10) 0.8788(10) 0.0989(7) 0.099(5) Uani 1 1 d . . . H17 H 0.8274 0.8502 0.1595 0.119 Uiso 1 1 calc R . . C18 C 0.8072(8) 0.8162(8) 0.0569(6) 0.057(3) Uani 1 1 d . . . C19 C 0.8859(7) 0.3504(9) 0.2578(6) 0.049(3) Uani 1 1 d . . . H19 H 0.8235 0.3236 0.2638 0.059 Uiso 1 1 calc R . . C20 C 0.9810(8) 0.2837(8) 0.2510(6) 0.046(3) Uani 1 1 d . . . H20 H 0.9814 0.2126 0.2535 0.056 Uiso 1 1 calc R . . C21 C 1.0675(8) 0.4227(8) 0.2349(6) 0.047(3) Uani 1 1 d . . . H21 H 1.1299 0.4513 0.2251 0.056 Uiso 1 1 calc R . . C22 C 0.9716(8) 0.4885(8) 0.2430(6) 0.046(3) Uani 1 1 d . . . H22 H 0.9708 0.5602 0.2393 0.055 Uiso 1 1 calc R . . C23 C 0.7523(9) 0.5291(11) 0.4177(7) 0.059(3) Uani 1 1 d . . . C24 C 0.6869(11) 0.6278(10) 0.3799(7) 0.061(3) Uani 1 1 d . . . C25 C 0.5954(10) 0.6008(10) 0.3643(7) 0.066(3) Uani 1 1 d . . . C26 C 0.6046(9) 0.4845(10) 0.3943(6) 0.057(3) Uani 1 1 d . . . C27 C 0.7030(9) 0.4391(9) 0.4257(6) 0.052(3) Uani 1 1 d . . . C28 C 0.8581(9) 0.5164(11) 0.4473(7) 0.107(5) Uani 1 1 d . . . H28A H 0.8876 0.5838 0.4172 0.161 Uiso 1 1 calc R . . H28B H 0.9061 0.4572 0.4339 0.161 Uiso 1 1 calc R . . H28C H 0.8475 0.5002 0.5093 0.161 Uiso 1 1 calc R . . C29 C 0.7085(11) 0.7400(9) 0.3588(7) 0.112(5) Uani 1 1 d . . . H29A H 0.6637 0.7710 0.3997 0.168 Uiso 1 1 calc R . . H29B H 0.6944 0.7852 0.3004 0.168 Uiso 1 1 calc R . . H29C H 0.7816 0.7370 0.3624 0.168 Uiso 1 1 calc R . . C30 C 0.5065(10) 0.6795(12) 0.3297(8) 0.128(6) Uani 1 1 d . . . H30A H 0.5316 0.7424 0.2828 0.192 Uiso 1 1 calc R . . H30B H 0.4623 0.7025 0.3752 0.192 Uiso 1 1 calc R . . H30C H 0.4662 0.6461 0.3079 0.192 Uiso 1 1 calc R . . C31 C 0.5266(8) 0.4184(11) 0.3905(8) 0.099(5) Uani 1 1 d . . . H31A H 0.4756 0.4039 0.4429 0.149 Uiso 1 1 calc R . . H31B H 0.5639 0.3498 0.3857 0.149 Uiso 1 1 calc R . . H31C H 0.4907 0.4596 0.3405 0.149 Uiso 1 1 calc R . . C32 C 0.7410(9) 0.3207(9) 0.4659(6) 0.083(4) Uani 1 1 d . . . H32A H 0.7366 0.3012 0.5280 0.125 Uiso 1 1 calc R . . H32B H 0.8134 0.3045 0.4412 0.125 Uiso 1 1 calc R . . H32C H 0.6978 0.2791 0.4550 0.125 Uiso 1 1 calc R . . C33 C 0.7175(9) 0.7975(9) -0.3682(6) 0.051(3) Uani 1 1 d . . . C34 C 0.6469(7) 0.8710(9) -0.3294(6) 0.053(3) Uani 1 1 d . . . C35 C 0.7014(8) 0.9539(8) -0.3335(6) 0.047(3) Uani 1 1 d . . . C36 C 0.8055(8) 0.9310(9) -0.3750(6) 0.048(3) Uani 1 1 d . . . C37 C 0.8138(9) 0.8408(9) -0.3993(6) 0.054(3) Uani 1 1 d . . . C38 C 0.6909(10) 0.7031(9) -0.3800(8) 0.112(5) Uani 1 1 d . . . H38A H 0.6657 0.7275 -0.4352 0.168 Uiso 1 1 calc R . . H38B H 0.6365 0.6717 -0.3335 0.168 Uiso 1 1 calc R . . H38C H 0.7529 0.6485 -0.3789 0.168 Uiso 1 1 calc R . . C39 C 0.5344(8) 0.8564(10) -0.2880(8) 0.105(5) Uani 1 1 d . . . H39A H 0.4904 0.8802 -0.3330 0.157 Uiso 1 1 calc R . . H39B H 0.5097 0.8997 -0.2514 0.157 Uiso 1 1 calc R . . H39C H 0.5314 0.7799 -0.2533 0.157 Uiso 1 1 calc R . . C40 C 0.6561(10) 1.0430(9) -0.3004(8) 0.104(5) Uani 1 1 d . . . H40A H 0.7121 1.0769 -0.2973 0.156 Uiso 1 1 calc R . . H40B H 0.6168 1.0137 -0.2430 0.156 Uiso 1 1 calc R . . H40C H 0.6096 1.0970 -0.3391 0.156 Uiso 1 1 calc R . . C41 C 0.8886(8) 1.0052(8) -0.3942(7) 0.077(4) Uani 1 1 d . . . H41A H 0.9581 0.9656 -0.4045 0.115 Uiso 1 1 calc R . . H41B H 0.8840 1.0268 -0.3450 0.115 Uiso 1 1 calc R . . H41C H 0.8761 1.0697 -0.4453 0.115 Uiso 1 1 calc R . . C42 C 0.9114(9) 0.7981(10) -0.4502(7) 0.101(4) Uani 1 1 d . . . H42A H 0.9145 0.7202 -0.4351 0.151 Uiso 1 1 calc R . . H42B H 0.9733 0.8115 -0.4361 0.151 Uiso 1 1 calc R . . H42C H 0.9087 0.8352 -0.5118 0.151 Uiso 1 1 calc R . . C43 C 0.7933(11) 0.0423(15) 0.2780(10) 0.091(5) Uani 1 1 d D . . C44 C 0.0974(10) 0.7366(10) 0.2945(8) 0.193(8) Uiso 1 1 d D . . O11 O 0.4951(7) 0.1170(8) 0.5300(6) 0.129(3) Uani 1 1 d . . . Cl1 Cl 0.5375(5) 0.1475(5) -0.0994(4) 0.210(3) Uani 1 1 d D . . Cl2 Cl 0.5392(7) 0.0561(7) 0.0853(4) 0.329(5) Uani 1 1 d D . . C45 C 0.514(2) 0.0383(11) -0.0046(10) 0.174(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0477(6) 0.0393(5) 0.0308(5) -0.0136(4) -0.0048(4) -0.0052(4) Rh2 0.0410(5) 0.0421(6) 0.0297(5) -0.0094(4) -0.0039(4) -0.0084(4) N1 0.049(5) 0.033(5) 0.035(5) -0.015(4) -0.009(4) -0.014(4) N2 0.046(5) 0.037(5) 0.039(5) -0.014(4) -0.006(4) -0.007(4) O1 0.066(5) 0.043(4) 0.032(4) -0.015(4) -0.013(3) -0.010(4) O2 0.055(4) 0.048(4) 0.031(4) -0.013(3) -0.006(3) -0.019(3) O3 0.050(4) 0.050(4) 0.030(4) -0.010(3) 0.004(3) -0.020(3) O4 0.071(5) 0.054(5) 0.034(4) -0.012(4) -0.001(4) -0.031(4) O5 0.091(6) 0.074(6) 0.155(9) -0.059(6) -0.050(6) 0.023(5) O6 0.070(5) 0.110(7) 0.095(7) -0.042(5) -0.033(5) -0.018(5) O7 0.103(7) 0.129(8) 0.091(7) -0.014(6) 0.011(5) -0.067(6) F1 0.145(7) 0.181(9) 0.132(7) -0.108(7) -0.019(6) -0.045(7) F2 0.197(10) 0.275(13) 0.114(8) -0.122(8) 0.074(7) -0.149(10) F3 0.104(7) 0.170(10) 0.302(14) -0.173(11) -0.018(8) 0.031(7) S1 0.055(2) 0.077(2) 0.062(2) -0.0284(18) -0.0080(16) -0.0133(19) S2 0.133(4) 0.271(7) 0.140(5) -0.143(5) -0.030(3) 0.008(4) C1 0.052(6) 0.029(6) 0.034(6) -0.008(5) 0.000(5) -0.014(5) C2 0.041(6) 0.027(6) 0.028(6) -0.009(5) 0.006(4) -0.013(5) C3 0.036(6) 0.035(6) 0.031(6) -0.013(5) -0.006(5) -0.006(5) C4 0.049(6) 0.037(6) 0.035(6) -0.013(5) -0.008(5) -0.011(5) C5 0.090(8) 0.065(8) 0.031(6) -0.010(6) -0.005(6) -0.051(7) C6 0.115(10) 0.067(8) 0.047(8) -0.011(7) 0.001(7) -0.060(8) C7 0.135(11) 0.079(9) 0.055(8) -0.030(7) 0.007(8) -0.076(9) C8 0.069(7) 0.060(8) 0.031(6) -0.010(6) -0.007(5) -0.026(6) C9 0.046(6) 0.030(6) 0.042(6) -0.015(5) -0.003(5) -0.016(5) C10 0.027(5) 0.035(6) 0.029(6) -0.008(5) -0.001(4) 0.005(5) C11 0.035(6) 0.030(6) 0.037(6) -0.016(5) -0.004(4) -0.010(5) C12 0.053(7) 0.039(7) 0.030(6) -0.008(5) -0.007(5) -0.002(5) C13 0.118(10) 0.033(7) 0.029(6) -0.009(5) 0.002(6) -0.036(7) C14 0.252(18) 0.069(10) 0.046(8) -0.007(7) -0.006(10) -0.097(11) C15 0.45(3) 0.140(15) 0.049(10) -0.017(10) -0.002(14) -0.218(19) C16 0.39(3) 0.107(13) 0.057(10) -0.010(9) -0.015(14) -0.174(16) C17 0.195(15) 0.087(10) 0.038(8) -0.021(7) 0.002(8) -0.086(10) C18 0.100(9) 0.046(7) 0.034(7) -0.012(6) -0.001(6) -0.043(7) C19 0.025(6) 0.082(9) 0.055(7) -0.037(7) 0.006(5) -0.025(6) C20 0.047(7) 0.051(7) 0.046(7) -0.017(5) 0.001(5) -0.026(6) C21 0.047(7) 0.055(7) 0.048(7) -0.023(6) -0.006(5) -0.019(6) C22 0.053(7) 0.040(6) 0.037(6) -0.012(5) -0.005(5) 0.001(6) C23 0.082(9) 0.072(9) 0.033(7) -0.027(7) 0.000(6) -0.027(8) C24 0.094(10) 0.048(8) 0.034(7) -0.016(6) 0.013(7) -0.020(8) C25 0.067(9) 0.056(9) 0.045(7) -0.007(6) 0.009(6) 0.011(7) C26 0.061(8) 0.073(9) 0.035(7) -0.025(6) 0.013(6) -0.013(7) C27 0.067(8) 0.041(7) 0.031(6) -0.004(5) 0.003(6) 0.003(7) C28 0.114(11) 0.172(15) 0.054(9) -0.044(9) -0.019(8) -0.043(10) C29 0.208(16) 0.062(9) 0.073(10) -0.039(8) 0.025(10) -0.050(10) C30 0.083(10) 0.155(14) 0.104(12) -0.043(11) 0.006(9) 0.038(10) C31 0.072(9) 0.151(13) 0.101(11) -0.051(10) -0.009(7) -0.060(9) C32 0.138(11) 0.064(9) 0.033(7) -0.007(6) -0.015(7) -0.004(8) C33 0.066(8) 0.052(8) 0.037(7) -0.009(6) -0.022(6) -0.014(7) C34 0.036(6) 0.070(8) 0.028(6) 0.015(6) -0.012(5) -0.010(6) C35 0.046(7) 0.046(7) 0.038(6) -0.006(5) -0.011(5) 0.004(6) C36 0.043(7) 0.063(8) 0.021(6) 0.006(5) -0.006(5) -0.013(6) C37 0.069(8) 0.057(8) 0.033(6) -0.014(6) -0.012(6) 0.000(7) C38 0.162(13) 0.079(10) 0.131(13) -0.043(9) -0.091(10) -0.012(9) C39 0.043(8) 0.151(13) 0.096(11) -0.010(9) -0.007(7) -0.034(8) C40 0.127(12) 0.074(9) 0.095(11) -0.041(8) -0.009(9) 0.028(9) C41 0.084(9) 0.057(8) 0.073(9) 0.010(6) -0.021(7) -0.032(7) C42 0.096(10) 0.129(12) 0.042(8) -0.027(8) 0.018(7) 0.018(9) C43 0.067(10) 0.137(15) 0.113(13) -0.087(12) 0.008(9) -0.046(10) O11 0.133(8) 0.128(8) 0.118(8) -0.046(7) -0.007(6) -0.011(7) Cl1 0.340(8) 0.154(5) 0.136(5) -0.033(4) 0.000(5) -0.107(5) Cl2 0.539(14) 0.413(11) 0.162(6) -0.139(7) 0.015(7) -0.323(11) C45 0.20(2) 0.10(2) 0.208(19) -0.09(2) 0.064(15) -0.013(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.044(6) . ? Rh1 O1 2.054(6) . ? Rh1 C25 2.108(10) . ? Rh1 C24 2.121(10) . ? Rh1 C23 2.131(10) . ? Rh1 C27 2.132(10) . ? Rh1 N1 2.140(7) . ? Rh1 C26 2.142(9) . ? Rh2 O3 2.046(6) . ? Rh2 O4 2.064(6) . ? Rh2 C36 2.102(9) . ? Rh2 C33 2.132(9) . ? Rh2 C37 2.144(9) . ? Rh2 N2 2.146(7) 2_765 ? Rh2 C34 2.150(9) . ? Rh2 C35 2.160(9) . ? N1 C19 1.330(10) . ? N1 C22 1.330(10) . ? N2 C20 1.336(10) . ? N2 C21 1.343(10) . ? N2 Rh2 2.146(7) 2_765 ? O1 C1 1.263(9) . ? O2 C3 1.286(9) . ? O3 C10 1.281(9) . ? O4 C12 1.293(9) . ? O5 S1 1.435(8) . ? O6 S1 1.416(7) . ? O7 S1 1.412(7) . ? O8 S2 1.397(7) . ? O9 S2 1.497(7) . ? O10 S2 1.378(8) . ? F1 C43 1.291(12) . ? F2 C43 1.287(15) . ? F3 C43 1.327(17) . ? F4 C44 1.314(9) . ? F5 C44 1.326(9) . ? F6 C44 1.320(9) . ? S1 C43 1.784(11) . ? S2 C44 1.769(11) . ? C1 C2 1.423(11) . ? C1 C18 1.461(11) . ? C2 C3 1.404(11) . ? C2 C11 1.460(10) . ? C3 C4 1.467(11) . ? C4 C9 1.392(11) . ? C4 C5 1.402(11) . ? C5 C6 1.365(11) . ? C6 C7 1.382(13) . ? C7 C8 1.381(12) . ? C8 C9 1.391(11) . ? C9 C10 1.471(11) . ? C10 C11 1.419(11) . ? C11 C12 1.429(11) . ? C12 C13 1.442(12) . ? C13 C14 1.376(13) . ? C13 C18 1.395(12) . ? C14 C15 1.381(14) . ? C15 C16 1.354(16) . ? C16 C17 1.362(14) . ? C17 C18 1.394(12) . ? C19 C20 1.369(12) . ? C21 C22 1.375(11) . ? C23 C24 1.396(14) . ? C23 C27 1.430(13) . ? C23 C28 1.521(14) . ? C24 C25 1.421(14) . ? C24 C29 1.472(13) . ? C25 C26 1.415(14) . ? C25 C30 1.437(14) . ? C26 C27 1.413(13) . ? C26 C31 1.510(12) . ? C27 C32 1.467(12) . ? C33 C37 1.409(12) . ? C33 C34 1.438(13) . ? C33 C38 1.468(12) . ? C34 C35 1.414(12) . ? C34 C39 1.500(12) . ? C35 C36 1.412(12) . ? C35 C40 1.457(12) . ? C36 C37 1.387(12) . ? C36 C41 1.526(12) . ? C37 C42 1.503(12) . ? Cl1 C45 1.707(14) . ? Cl2 C45 1.722(15) . ? C45 C45 1.10(3) 2_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 O2 Rh1 O1 85.9(2) . . ? O2 Rh1 C25 108.6(4) . . ? O1 Rh1 C25 107.2(4) . . ? O2 Rh1 C24 145.7(4) . . ? O1 Rh1 C24 93.2(3) . . ? C25 Rh1 C24 39.3(4) . . ? O2 Rh1 C23 158.5(4) . . ? O1 Rh1 C23 115.5(4) . . ? C25 Rh1 C23 64.9(4) . . ? C24 Rh1 C23 38.3(4) . . ? O2 Rh1 C27 119.4(4) . . ? O1 Rh1 C27 154.7(4) . . ? C25 Rh1 C27 65.3(4) . . ? C24 Rh1 C27 65.4(4) . . ? C23 Rh1 C27 39.2(4) . . ? O2 Rh1 N1 83.2(2) . . ? O1 Rh1 N1 85.9(3) . . ? C25 Rh1 N1 162.6(4) . . ? C24 Rh1 N1 130.9(4) . . ? C23 Rh1 N1 99.3(4) . . ? C27 Rh1 N1 97.9(3) . . ? O2 Rh1 C26 96.9(3) . . ? O1 Rh1 C26 145.0(4) . . ? C25 Rh1 C26 38.9(4) . . ? C24 Rh1 C26 65.2(4) . . ? C23 Rh1 C26 64.8(4) . . ? C27 Rh1 C26 38.6(4) . . ? N1 Rh1 C26 129.1(4) . . ? O3 Rh2 O4 84.3(2) . . ? O3 Rh2 C36 164.2(3) . . ? O4 Rh2 C36 103.9(3) . . ? O3 Rh2 C33 103.1(3) . . ? O4 Rh2 C33 161.0(4) . . ? C36 Rh2 C33 65.0(4) . . ? O3 Rh2 C37 136.7(4) . . ? O4 Rh2 C37 138.8(4) . . ? C36 Rh2 C37 38.1(3) . . ? C33 Rh2 C37 38.5(3) . . ? O3 Rh2 N2 84.7(3) . 2_765 ? O4 Rh2 N2 86.4(3) . 2_765 ? C36 Rh2 N2 109.0(3) . 2_765 ? C33 Rh2 N2 111.5(4) . 2_765 ? C37 Rh2 N2 92.7(3) . 2_765 ? O3 Rh2 C34 100.1(3) . . ? O4 Rh2 C34 122.7(4) . . ? C36 Rh2 C34 64.0(4) . . ? C33 Rh2 C34 39.2(3) . . ? C37 Rh2 C34 63.9(4) . . ? N2 Rh2 C34 150.7(4) 2_765 . ? O3 Rh2 C35 128.1(3) . . ? O4 Rh2 C35 95.9(3) . . ? C36 Rh2 C35 38.7(3) . . ? C33 Rh2 C35 65.7(4) . . ? C37 Rh2 C35 64.4(4) . . ? N2 Rh2 C35 147.2(3) 2_765 . ? C34 Rh2 C35 38.3(3) . . ? C19 N1 C22 116.6(8) . . ? C19 N1 Rh1 120.7(6) . . ? C22 N1 Rh1 122.1(6) . . ? C20 N2 C21 116.1(8) . . ? C20 N2 Rh2 122.4(6) . 2_765 ? C21 N2 Rh2 120.3(6) . 2_765 ? C1 O1 Rh1 129.3(6) . . ? C3 O2 Rh1 129.1(5) . . ? C10 O3 Rh2 131.2(6) . . ? C12 O4 Rh2 130.9(6) . . ? O7 S1 O6 117.2(5) . . ? O7 S1 O5 113.3(5) . . ? O6 S1 O5 113.8(5) . . ? O7 S1 C43 105.4(6) . . ? O6 S1 C43 104.1(6) . . ? O5 S1 C43 100.7(7) . . ? O10 S2 O8 127.0(9) . . ? O10 S2 O9 111.0(8) . . ? O8 S2 O9 109.9(8) . . ? O10 S2 C44 102.8(8) . . ? O8 S2 C44 105.5(7) . . ? O9 S2 C44 95.4(6) . . ? O1 C1 C2 127.5(8) . . ? O1 C1 C18 113.2(8) . . ? C2 C1 C18 119.3(9) . . ? C3 C2 C1 120.2(8) . . ? C3 C2 C11 120.2(7) . . ? C1 C2 C11 119.7(7) . . ? O2 C3 C2 127.4(8) . . ? O2 C3 C4 113.1(8) . . ? C2 C3 C4 119.6(8) . . ? C9 C4 C5 119.1(8) . . ? C9 C4 C3 120.2(8) . . ? C5 C4 C3 120.6(9) . . ? C6 C5 C4 120.3(9) . . ? C5 C6 C7 121.4(10) . . ? C8 C7 C6 118.4(10) . . ? C7 C8 C9 121.6(9) . . ? C8 C9 C4 119.2(8) . . ? C8 C9 C10 119.6(9) . . ? C4 C9 C10 121.2(8) . . ? O3 C10 C11 126.8(9) . . ? O3 C10 C9 115.1(8) . . ? C11 C10 C9 118.2(8) . . ? C10 C11 C12 119.9(9) . . ? C10 C11 C2 120.7(8) . . ? C12 C11 C2 119.3(7) . . ? O4 C12 C11 125.7(9) . . ? O4 C12 C13 113.7(9) . . ? C11 C12 C13 120.5(9) . . ? C14 C13 C18 119.9(9) . . ? C14 C13 C12 120.3(10) . . ? C18 C13 C12 119.8(9) . . ? C13 C14 C15 118.5(12) . . ? C16 C15 C14 122.9(12) . . ? C15 C16 C17 118.5(12) . . ? C16 C17 C18 121.1(11) . . ? C17 C18 C13 119.0(9) . . ? C17 C18 C1 120.0(10) . . ? C13 C18 C1 120.9(9) . . ? N1 C19 C20 122.0(8) . . ? N2 C20 C19 121.8(9) . . ? N2 C21 C22 121.6(9) . . ? N1 C22 C21 121.7(9) . . ? C24 C23 C27 108.7(10) . . ? C24 C23 C28 126.8(12) . . ? C27 C23 C28 124.5(12) . . ? C24 C23 Rh1 70.4(6) . . ? C27 C23 Rh1 70.4(5) . . ? C28 C23 Rh1 125.7(7) . . ? C23 C24 C25 107.7(10) . . ? C23 C24 C29 126.5(13) . . ? C25 C24 C29 125.8(13) . . ? C23 C24 Rh1 71.2(6) . . ? C25 C24 Rh1 69.9(6) . . ? C29 C24 Rh1 123.8(7) . . ? C26 C25 C24 108.3(11) . . ? C26 C25 C30 126.7(14) . . ? C24 C25 C30 124.9(13) . . ? C26 C25 Rh1 71.9(6) . . ? C24 C25 Rh1 70.8(6) . . ? C30 C25 Rh1 126.3(8) . . ? C27 C26 C25 108.0(10) . . ? C27 C26 C31 125.0(11) . . ? C25 C26 C31 127.0(12) . . ? C27 C26 Rh1 70.3(6) . . ? C25 C26 Rh1 69.2(6) . . ? C31 C26 Rh1 124.0(7) . . ? C26 C27 C23 107.3(9) . . ? C26 C27 C32 125.2(11) . . ? C23 C27 C32 127.3(11) . . ? C26 C27 Rh1 71.1(6) . . ? C23 C27 Rh1 70.4(6) . . ? C32 C27 Rh1 127.8(7) . . ? C37 C33 C34 105.8(9) . . ? C37 C33 C38 127.3(11) . . ? C34 C33 C38 126.6(11) . . ? C37 C33 Rh2 71.2(5) . . ? C34 C33 Rh2 71.1(5) . . ? C38 C33 Rh2 126.6(7) . . ? C35 C34 C33 109.4(8) . . ? C35 C34 C39 126.6(11) . . ? C33 C34 C39 124.0(11) . . ? C35 C34 Rh2 71.3(5) . . ? C33 C34 Rh2 69.7(5) . . ? C39 C34 Rh2 123.2(7) . . ? C36 C35 C34 105.7(9) . . ? C36 C35 C40 128.8(11) . . ? C34 C35 C40 125.4(10) . . ? C36 C35 Rh2 68.4(5) . . ? C34 C35 Rh2 70.4(5) . . ? C40 C35 Rh2 125.5(7) . . ? C37 C36 C35 110.0(9) . . ? C37 C36 C41 128.2(10) . . ? C35 C36 C41 121.7(10) . . ? C37 C36 Rh2 72.6(6) . . ? C35 C36 Rh2 72.9(5) . . ? C41 C36 Rh2 125.0(6) . . ? C36 C37 C33 108.9(9) . . ? C36 C37 C42 124.3(11) . . ? C33 C37 C42 126.9(11) . . ? C36 C37 Rh2 69.3(5) . . ? C33 C37 Rh2 70.3(5) . . ? C42 C37 Rh2 126.1(7) . . ? F2 C43 F1 109.1(14) . . ? F2 C43 F3 104.8(12) . . ? F1 C43 F3 105.1(12) . . ? F2 C43 S1 112.8(10) . . ? F1 C43 S1 114.4(9) . . ? F3 C43 S1 110.1(12) . . ? F4 C44 F6 103.0(11) . . ? F4 C44 F5 103.1(11) . . ? F6 C44 F5 105.3(11) . . ? F4 C44 S2 116.7(12) . . ? F6 C44 S2 114.6(10) . . ? F5 C44 S2 112.8(9) . . ? C45 C45 Cl1 129(2) 2_655 . ? C45 C45 Cl2 118.8(19) 2_655 . ? Cl1 C45 Cl2 112.6(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.781 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.110 # Attachment 'Complex 3b.cif' data_Complex_3b'''' _database_code_depnum_ccdc_archive 'CCDC 749419' #TrackingRef 'Complex 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H90 Cl6 F12 N4 O22 Rh4 S4' _chemical_formula_weight 2560.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.101(10) _cell_length_b 13.368(11) _cell_length_c 16.793(13) _cell_angle_alpha 66.969(10) _cell_angle_beta 77.398(11) _cell_angle_gamma 77.072(11) _cell_volume 2610(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 919 _cell_measurement_theta_min 2.587 _cell_measurement_theta_max 21.742 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8951 _exptl_absorpt_correction_T_max 0.9114 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.71 _diffrn_reflns_number 11799 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.01 _reflns_number_total 9933 _reflns_number_gt 5028 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9933 _refine_ls_number_parameters 616 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1838 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.73075(5) 0.54228(5) 0.29113(4) 0.0373(2) Uani 1 1 d . . . Rh2 Rh 0.78026(5) 0.79378(5) -0.25918(4) 0.0365(2) Uani 1 1 d . . . N1 N 0.8806(5) 0.4507(5) 0.2567(4) 0.0359(15) Uani 1 1 d . . . N2 N 1.0730(5) 0.3194(5) 0.2416(4) 0.0381(15) Uani 1 1 d . . . O1 O 0.7810(4) 0.6757(4) 0.1891(3) 0.0458(14) Uani 1 1 d . . . O2 O 0.6818(4) 0.5062(4) 0.1989(3) 0.0390(13) Uani 1 1 d . . . O3 O 0.7132(4) 0.6692(4) -0.1561(3) 0.0437(14) Uani 1 1 d . . . O4 O 0.8078(5) 0.8402(4) -0.1638(3) 0.0485(15) Uani 1 1 d . . . O5 O 0.6859(6) 0.1882(6) 0.3344(6) 0.100(3) Uani 1 1 d . . . O6 O 0.8416(6) 0.0869(6) 0.3985(5) 0.092(2) Uani 1 1 d . . . O7 O 0.6850(7) 0.0034(8) 0.4300(5) 0.120(3) Uani 1 1 d . . . O8 O 0.2656(9) 0.6192(10) 0.3511(7) 0.188(5) Uiso 1 1 d D . . O9 O 0.1263(10) 0.5387(9) 0.3400(8) 0.196(6) Uiso 1 1 d D . . O10 O 0.2268(13) 0.6432(13) 0.2065(6) 0.282(9) Uiso 1 1 d D . . F1 F 0.7182(7) 0.0284(7) 0.2458(5) 0.123(3) Uani 1 1 d . . . F2 F 0.8531(8) 0.1087(9) 0.2182(5) 0.174(5) Uani 1 1 d . . . F3 F 0.8556(7) -0.0527(9) 0.2981(8) 0.189(5) Uani 1 1 d . . . F4 F 0.1238(13) 0.8341(12) 0.2592(10) 0.308(8) Uiso 1 1 d D . . F5 F 0.0541(9) 0.7298(8) 0.3748(7) 0.189(4) Uiso 1 1 d D . . F6 F 0.0154(10) 0.7461(10) 0.2548(8) 0.236(5) Uiso 1 1 d D . . S1 S 0.7474(2) 0.0829(2) 0.37103(16) 0.0601(6) Uani 1 1 d D . . S2 S 0.1981(4) 0.6230(5) 0.2948(3) 0.158(2) Uani 1 1 d D . . C1 C 0.7737(6) 0.7077(6) 0.1074(5) 0.040(2) Uani 1 1 d . . . C2 C 0.7389(6) 0.6517(6) 0.0649(4) 0.0346(18) Uani 1 1 d . . . C3 C 0.6973(6) 0.5529(6) 0.1144(4) 0.0333(17) Uani 1 1 d . . . C4 C 0.6642(6) 0.4935(6) 0.0698(5) 0.0369(18) Uani 1 1 d . . . C5 C 0.6314(7) 0.3903(7) 0.1159(5) 0.057(3) Uani 1 1 d . . . H5 H 0.6271 0.3607 0.1764 0.068 Uiso 1 1 calc R . . C6 C 0.6057(9) 0.3328(8) 0.0738(6) 0.077(3) Uani 1 1 d . . . H6 H 0.5826 0.2654 0.1056 0.092 Uiso 1 1 calc R . . C7 C 0.6144(9) 0.3758(8) -0.0184(6) 0.076(3) Uani 1 1 d . . . H7 H 0.5978 0.3361 -0.0473 0.091 Uiso 1 1 calc R . . C8 C 0.6463(7) 0.4730(7) -0.0640(5) 0.055(2) Uani 1 1 d . . . H8 H 0.6513 0.5005 -0.1246 0.066 Uiso 1 1 calc R . . C9 C 0.6727(6) 0.5350(6) -0.0225(5) 0.0380(19) Uani 1 1 d . . . C10 C 0.7131(6) 0.6391(6) -0.0734(4) 0.0342(18) Uani 1 1 d . . . C11 C 0.7485(6) 0.6958(5) -0.0302(4) 0.0318(17) Uani 1 1 d . . . C12 C 0.7877(7) 0.7968(6) -0.0786(5) 0.042(2) Uani 1 1 d . . . C13 C 0.8103(7) 0.8600(6) -0.0339(5) 0.048(2) Uani 1 1 d . . . C14 C 0.8362(12) 0.9643(9) -0.0800(6) 0.110(5) Uani 1 1 d . . . H14 H 0.8377 0.9939 -0.1404 0.132 Uiso 1 1 calc R . . C15 C 0.8596(15) 1.0246(10) -0.0393(7) 0.151(8) Uani 1 1 d . . . H15 H 0.8807 1.0928 -0.0721 0.181 Uiso 1 1 calc R . . C16 C 0.8520(15) 0.9842(11) 0.0521(8) 0.159(8) Uani 1 1 d . . . H16 H 0.8630 1.0274 0.0805 0.191 Uiso 1 1 calc R . . C17 C 0.8282(11) 0.8797(9) 0.0992(6) 0.105(5) Uani 1 1 d . . . H17 H 0.8279 0.8498 0.1594 0.126 Uiso 1 1 calc R . . C18 C 0.8044(8) 0.8191(7) 0.0562(5) 0.057(3) Uani 1 1 d . . . C19 C 0.8874(6) 0.3495(6) 0.2579(5) 0.043(2) Uani 1 1 d . . . H19 H 0.8256 0.3222 0.2642 0.051 Uiso 1 1 calc R . . C20 C 0.9825(6) 0.2843(7) 0.2503(5) 0.043(2) Uani 1 1 d . . . H20 H 0.9841 0.2140 0.2513 0.052 Uiso 1 1 calc R . . C21 C 1.0687(6) 0.4217(7) 0.2349(5) 0.044(2) Uani 1 1 d . . . H21 H 1.1309 0.4504 0.2241 0.053 Uiso 1 1 calc R . . C22 C 0.9721(7) 0.4865(7) 0.2437(5) 0.047(2) Uani 1 1 d . . . H22 H 0.9708 0.5578 0.2405 0.056 Uiso 1 1 calc R . . C23 C 0.7527(8) 0.5272(8) 0.4190(5) 0.060(3) Uani 1 1 d . . . C24 C 0.6844(9) 0.6275(7) 0.3811(6) 0.061(3) Uani 1 1 d . . . C25 C 0.5946(8) 0.6013(8) 0.3629(6) 0.063(3) Uani 1 1 d . . . C26 C 0.6040(8) 0.4841(8) 0.3950(5) 0.057(2) Uani 1 1 d . . . C27 C 0.7020(8) 0.4402(7) 0.4264(5) 0.052(2) Uani 1 1 d . . . C28 C 0.8586(11) 0.5182(11) 0.4454(7) 0.117(5) Uani 1 1 d . . . H28A H 0.8915 0.5809 0.4070 0.176 Uiso 1 1 calc R . . H28B H 0.9031 0.4522 0.4414 0.176 Uiso 1 1 calc R . . H28C H 0.8483 0.5157 0.5044 0.176 Uiso 1 1 calc R . . C29 C 0.7086(11) 0.7422(9) 0.3588(7) 0.106(5) Uani 1 1 d . . . H29A H 0.6778 0.7670 0.4065 0.159 Uiso 1 1 calc R . . H29B H 0.6795 0.7917 0.3070 0.159 Uiso 1 1 calc R . . H29C H 0.7839 0.7404 0.3488 0.159 Uiso 1 1 calc R . . C30 C 0.5059(10) 0.6829(11) 0.3289(8) 0.134(6) Uani 1 1 d . . . H30A H 0.5311 0.7499 0.2895 0.200 Uiso 1 1 calc R . . H30B H 0.4568 0.6967 0.3764 0.200 Uiso 1 1 calc R . . H30C H 0.4711 0.6561 0.2982 0.200 Uiso 1 1 calc R . . C31 C 0.5256(9) 0.4216(10) 0.3859(7) 0.096(4) Uani 1 1 d . . . H31A H 0.4733 0.4057 0.4373 0.145 Uiso 1 1 calc R . . H31B H 0.5626 0.3540 0.3794 0.145 Uiso 1 1 calc R . . H31C H 0.4915 0.4658 0.3355 0.145 Uiso 1 1 calc R . . C32 C 0.7405(10) 0.3186(7) 0.4684(6) 0.089(4) Uani 1 1 d . . . H32A H 0.7145 0.2945 0.5299 0.134 Uiso 1 1 calc R . . H32B H 0.8165 0.3055 0.4598 0.134 Uiso 1 1 calc R . . H32C H 0.7149 0.2786 0.4422 0.134 Uiso 1 1 calc R . . C33 C 0.7164(9) 0.7982(7) -0.3674(6) 0.059(3) Uani 1 1 d . . . C34 C 0.6469(7) 0.8666(8) -0.3266(5) 0.058(3) Uani 1 1 d . . . C35 C 0.7007(7) 0.9529(7) -0.3323(5) 0.054(2) Uani 1 1 d . . . C36 C 0.8040(7) 0.9325(7) -0.3738(5) 0.053(2) Uani 1 1 d . . . C37 C 0.8130(8) 0.8430(8) -0.3992(5) 0.058(3) Uani 1 1 d . . . C38 C 0.6899(13) 0.7042(10) -0.3791(8) 0.134(6) Uani 1 1 d . . . H38A H 0.6647 0.7285 -0.4342 0.201 Uiso 1 1 calc R . . H38B H 0.6357 0.6730 -0.3327 0.201 Uiso 1 1 calc R . . H38C H 0.7518 0.6497 -0.3780 0.201 Uiso 1 1 calc R . . C39 C 0.5345(8) 0.8554(11) -0.2879(8) 0.122(5) Uani 1 1 d . . . H39A H 0.4910 0.8865 -0.3336 0.183 Uiso 1 1 calc R . . H39B H 0.5116 0.8936 -0.2476 0.183 Uiso 1 1 calc R . . H39C H 0.5283 0.7790 -0.2576 0.183 Uiso 1 1 calc R . . C40 C 0.6547(11) 1.0435(9) -0.2978(8) 0.118(5) Uani 1 1 d . . . H40A H 0.7109 1.0721 -0.2893 0.177 Uiso 1 1 calc R . . H40B H 0.6102 1.0153 -0.2430 0.177 Uiso 1 1 calc R . . H40C H 0.6136 1.1011 -0.3389 0.177 Uiso 1 1 calc R . . C41 C 0.8866(9) 1.0058(8) -0.3939(7) 0.090(4) Uani 1 1 d . . . H41A H 0.9461 0.9858 -0.4325 0.135 Uiso 1 1 calc R . . H41B H 0.9093 0.9967 -0.3405 0.135 Uiso 1 1 calc R . . H41C H 0.8565 1.0812 -0.4214 0.135 Uiso 1 1 calc R . . C42 C 0.9088(9) 0.7988(10) -0.4505(6) 0.102(4) Uani 1 1 d . . . H42A H 0.9119 0.7209 -0.4337 0.154 Uiso 1 1 calc R . . H42B H 0.9715 0.8132 -0.4388 0.154 Uiso 1 1 calc R . . H42C H 0.9040 0.8340 -0.5119 0.154 Uiso 1 1 calc R . . C43 C 0.7935(10) 0.0385(11) 0.2796(8) 0.084(3) Uani 1 1 d D . . C44 C 0.0969(10) 0.7349(10) 0.2950(9) 0.179(8) Uiso 1 1 d D . . O11 O 0.4966(8) 0.1173(7) 0.5296(6) 0.126(3) Uani 1 1 d . . . Cl1 Cl 0.5364(6) 0.1458(5) -0.0974(4) 0.239(3) Uani 1 1 d D . . Cl2 Cl 0.5382(9) 0.0577(8) 0.0811(5) 0.371(7) Uani 1 1 d D . . C45 C 0.5092(17) 0.0347(11) -0.0045(10) 0.064(6) Uani 0.50 1 d PD . . Cl3 Cl 0.0209(11) 0.5399(11) 1.0114(9) 0.214(5) Uiso 0.50 1 d PD . . Cl4 Cl 0.083(3) 0.700(3) 1.035(2) 0.59(2) Uiso 0.50 1 d PD . . C46 C 0.062(2) 0.6484(17) 0.9679(15) 0.102(8) Uiso 0.50 1 d PD . . H46A H 0.0109 0.7009 0.9316 0.122 Uiso 0.50 1 calc PR . . H46B H 0.1273 0.6387 0.9297 0.122 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0457(4) 0.0382(4) 0.0247(3) -0.0085(3) -0.0046(3) -0.0056(3) Rh2 0.0396(4) 0.0395(4) 0.0240(3) -0.0030(3) -0.0051(3) -0.0088(3) N1 0.037(4) 0.041(4) 0.032(3) -0.013(3) -0.003(3) -0.012(3) N2 0.046(4) 0.039(4) 0.032(3) -0.010(3) -0.006(3) -0.014(3) O1 0.065(4) 0.047(3) 0.030(3) -0.012(3) -0.013(3) -0.015(3) O2 0.049(3) 0.039(3) 0.027(3) -0.003(2) -0.012(2) -0.011(3) O3 0.051(4) 0.055(3) 0.025(3) -0.008(2) -0.008(2) -0.019(3) O4 0.075(4) 0.043(3) 0.026(3) -0.001(2) -0.003(3) -0.029(3) O5 0.085(6) 0.092(6) 0.149(8) -0.070(6) -0.051(5) 0.018(5) O6 0.080(6) 0.114(6) 0.098(6) -0.040(5) -0.029(4) -0.028(5) O7 0.115(7) 0.165(8) 0.065(5) -0.002(5) 0.006(5) -0.080(6) F1 0.132(7) 0.175(8) 0.119(6) -0.099(6) -0.012(5) -0.059(6) F2 0.212(10) 0.261(11) 0.105(6) -0.109(7) 0.074(6) -0.163(9) F3 0.108(7) 0.181(9) 0.341(15) -0.191(11) -0.035(8) 0.036(7) S1 0.0539(16) 0.0710(17) 0.0575(15) -0.0206(13) -0.0123(12) -0.0143(14) S2 0.124(4) 0.270(6) 0.125(3) -0.130(4) -0.024(3) -0.001(4) C1 0.048(5) 0.044(5) 0.023(4) -0.006(4) -0.003(3) -0.010(4) C2 0.047(5) 0.028(4) 0.026(4) -0.008(3) 0.002(3) -0.010(4) C3 0.035(4) 0.041(4) 0.022(4) -0.008(3) -0.001(3) -0.009(4) C4 0.042(5) 0.036(4) 0.032(4) -0.010(3) -0.003(3) -0.009(4) C5 0.085(7) 0.059(6) 0.033(5) -0.009(4) -0.002(4) -0.041(5) C6 0.129(10) 0.064(6) 0.044(6) -0.007(5) -0.005(6) -0.060(7) C7 0.124(10) 0.079(7) 0.049(6) -0.029(5) -0.004(6) -0.062(7) C8 0.085(7) 0.061(6) 0.028(4) -0.014(4) -0.002(4) -0.036(5) C9 0.044(5) 0.038(4) 0.030(4) -0.006(3) -0.004(3) -0.017(4) C10 0.031(4) 0.041(4) 0.026(4) -0.007(3) -0.001(3) -0.008(4) C11 0.040(5) 0.027(4) 0.027(4) -0.007(3) -0.008(3) -0.006(3) C12 0.057(6) 0.038(5) 0.029(4) -0.006(4) -0.004(4) -0.014(4) C13 0.080(7) 0.035(5) 0.029(4) -0.010(4) 0.001(4) -0.022(4) C14 0.240(17) 0.073(7) 0.039(6) -0.015(5) -0.004(8) -0.095(9) C15 0.34(2) 0.089(9) 0.052(7) -0.008(7) -0.014(10) -0.129(13) C16 0.35(2) 0.113(11) 0.056(8) -0.023(7) -0.003(11) -0.157(14) C17 0.210(15) 0.096(9) 0.036(5) -0.028(6) 0.012(7) -0.096(10) C18 0.095(8) 0.047(5) 0.034(5) -0.012(4) 0.004(5) -0.038(5) C19 0.038(5) 0.043(5) 0.049(5) -0.017(4) -0.010(4) -0.009(4) C20 0.047(5) 0.041(5) 0.040(5) -0.012(4) -0.007(4) -0.010(4) C21 0.041(5) 0.046(5) 0.048(5) -0.015(4) -0.011(4) -0.009(4) C22 0.063(6) 0.044(5) 0.038(5) -0.018(4) -0.010(4) -0.009(5) C23 0.083(8) 0.081(7) 0.028(4) -0.028(5) -0.003(5) -0.025(6) C24 0.092(8) 0.047(6) 0.038(5) -0.017(4) 0.012(5) -0.013(6) C25 0.063(7) 0.062(6) 0.042(5) -0.017(5) 0.013(5) 0.007(5) C26 0.060(6) 0.073(7) 0.035(5) -0.019(5) 0.012(4) -0.021(5) C27 0.080(7) 0.051(5) 0.019(4) -0.012(4) 0.003(4) -0.006(5) C28 0.149(13) 0.175(13) 0.058(7) -0.048(8) -0.024(8) -0.065(11) C29 0.180(14) 0.071(8) 0.066(7) -0.035(6) 0.020(8) -0.033(8) C30 0.086(10) 0.144(12) 0.099(10) -0.010(9) -0.001(8) 0.048(9) C31 0.077(8) 0.123(10) 0.091(9) -0.033(8) 0.017(7) -0.055(8) C32 0.153(12) 0.060(7) 0.040(6) -0.006(5) -0.018(6) -0.006(7) C33 0.094(8) 0.047(6) 0.038(5) -0.002(4) -0.031(5) -0.018(6) C34 0.043(6) 0.075(7) 0.034(5) 0.013(5) -0.015(4) -0.014(5) C35 0.057(6) 0.050(6) 0.040(5) -0.004(4) -0.015(4) 0.006(5) C36 0.047(6) 0.051(6) 0.037(5) 0.010(4) -0.008(4) -0.010(4) C37 0.065(7) 0.066(6) 0.022(4) -0.001(4) -0.007(4) 0.007(5) C38 0.228(18) 0.099(10) 0.103(10) -0.015(8) -0.097(11) -0.051(11) C39 0.044(7) 0.169(13) 0.096(9) 0.017(8) -0.014(6) -0.021(8) C40 0.139(13) 0.070(8) 0.127(11) -0.046(8) -0.029(9) 0.047(8) C41 0.088(9) 0.076(7) 0.078(8) 0.031(6) -0.036(6) -0.043(7) C42 0.095(9) 0.128(10) 0.040(6) -0.013(6) 0.006(6) 0.021(8) C43 0.072(9) 0.087(9) 0.102(10) -0.049(8) 0.003(7) -0.022(7) O11 0.135(8) 0.108(7) 0.124(8) -0.046(6) 0.015(6) -0.023(6) Cl1 0.339(10) 0.198(6) 0.181(6) -0.054(5) -0.008(6) -0.099(6) Cl2 0.575(18) 0.426(13) 0.221(8) -0.128(8) -0.004(9) -0.325(13) C45 0.072(14) 0.034(12) 0.087(14) -0.035(13) 0.005(11) -0.006(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.047(5) . ? Rh1 O2 2.051(5) . ? Rh1 C25 2.106(8) . ? Rh1 C24 2.141(9) . ? Rh1 C27 2.143(8) . ? Rh1 C23 2.154(8) . ? Rh1 C26 2.157(8) . ? Rh1 N1 2.161(6) . ? Rh2 O4 2.051(5) . ? Rh2 O3 2.068(5) . ? Rh2 C36 2.108(8) . ? Rh2 C34 2.127(8) . ? Rh2 C33 2.136(9) . ? Rh2 C37 2.150(8) . ? Rh2 C35 2.154(8) . ? Rh2 N2 2.160(6) 2_765 ? N1 C19 1.328(9) . ? N1 C22 1.331(10) . ? N2 C21 1.317(9) . ? N2 C20 1.329(10) . ? N2 Rh2 2.160(6) 2_765 ? O1 C1 1.286(8) . ? O2 C3 1.296(8) . ? O3 C10 1.285(8) . ? O4 C12 1.308(8) . ? O5 S1 1.429(7) . ? O6 S1 1.428(7) . ? O7 S1 1.411(7) . ? O8 S2 1.408(8) . ? O9 S2 1.493(8) . ? O10 S2 1.380(8) . ? F1 C43 1.294(13) . ? F2 C43 1.333(13) . ? F3 C43 1.270(14) . ? F4 C44 1.318(9) . ? F5 C44 1.317(9) . ? F6 C44 1.336(9) . ? S1 C43 1.795(11) . ? S2 C44 1.763(11) . ? C1 C2 1.410(10) . ? C1 C18 1.495(10) . ? C2 C3 1.414(10) . ? C2 C11 1.457(9) . ? C3 C4 1.463(10) . ? C4 C5 1.404(10) . ? C4 C9 1.415(10) . ? C5 C6 1.359(12) . ? C6 C7 1.412(12) . ? C7 C8 1.333(11) . ? C8 C9 1.404(11) . ? C9 C10 1.466(10) . ? C10 C11 1.433(10) . ? C11 C12 1.420(10) . ? C12 C13 1.438(11) . ? C13 C14 1.383(11) . ? C13 C18 1.384(10) . ? C14 C15 1.358(14) . ? C15 C16 1.402(15) . ? C16 C17 1.377(14) . ? C17 C18 1.394(12) . ? C19 C20 1.363(10) . ? C21 C22 1.379(11) . ? C23 C27 1.416(12) . ? C23 C24 1.430(13) . ? C23 C28 1.512(14) . ? C24 C25 1.422(14) . ? C24 C29 1.520(13) . ? C25 C26 1.430(12) . ? C25 C30 1.449(14) . ? C26 C27 1.410(13) . ? C26 C31 1.525(13) . ? C27 C32 1.512(11) . ? C33 C34 1.407(13) . ? C33 C37 1.429(13) . ? C33 C38 1.468(14) . ? C34 C35 1.444(13) . ? C34 C39 1.490(13) . ? C35 C36 1.401(12) . ? C35 C40 1.495(13) . ? C36 C37 1.394(12) . ? C36 C41 1.516(12) . ? C37 C42 1.504(12) . ? Cl1 C45 1.718(14) . ? Cl2 C45 1.715(15) . ? C45 C45 0.96(3) 2_655 ? Cl3 Cl3 1.50(2) 2_567 ? Cl3 C46 1.507(16) . ? Cl4 C46 1.623(18) . ? 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 Rh1 O2 85.8(2) . . ? O1 Rh1 C25 107.2(3) . . ? O2 Rh1 C25 107.5(4) . . ? O1 Rh1 C24 93.9(3) . . ? O2 Rh1 C24 144.6(4) . . ? C25 Rh1 C24 39.1(4) . . ? O1 Rh1 C27 154.4(3) . . ? O2 Rh1 C27 119.7(3) . . ? C25 Rh1 C27 65.3(3) . . ? C24 Rh1 C27 64.5(3) . . ? O1 Rh1 C23 116.0(3) . . ? O2 Rh1 C23 158.1(3) . . ? C25 Rh1 C23 65.8(4) . . ? C24 Rh1 C23 38.9(4) . . ? C27 Rh1 C23 38.5(3) . . ? O1 Rh1 C26 145.4(3) . . ? O2 Rh1 C26 96.6(3) . . ? C25 Rh1 C26 39.2(3) . . ? C24 Rh1 C26 64.7(4) . . ? C27 Rh1 C26 38.3(3) . . ? C23 Rh1 C26 64.7(4) . . ? O1 Rh1 N1 86.1(2) . . ? O2 Rh1 N1 84.1(2) . . ? C25 Rh1 N1 162.7(3) . . ? C24 Rh1 N1 131.3(4) . . ? C27 Rh1 N1 97.9(3) . . ? C23 Rh1 N1 98.6(3) . . ? C26 Rh1 N1 128.5(3) . . ? O4 Rh2 O3 85.0(2) . . ? O4 Rh2 C36 103.0(3) . . ? O3 Rh2 C36 163.4(3) . . ? O4 Rh2 C34 122.8(3) . . ? O3 Rh2 C34 98.3(3) . . ? C36 Rh2 C34 65.1(3) . . ? O4 Rh2 C33 160.3(3) . . ? O3 Rh2 C33 102.4(3) . . ? C36 Rh2 C33 65.5(4) . . ? C34 Rh2 C33 38.5(3) . . ? O4 Rh2 C37 138.1(3) . . ? O3 Rh2 C37 136.8(3) . . ? C36 Rh2 C37 38.2(3) . . ? C34 Rh2 C37 64.2(3) . . ? C33 Rh2 C37 39.0(4) . . ? O4 Rh2 C35 95.5(3) . . ? O3 Rh2 C35 127.3(3) . . ? C36 Rh2 C35 38.3(3) . . ? C34 Rh2 C35 39.4(3) . . ? C33 Rh2 C35 65.4(3) . . ? C37 Rh2 C35 63.9(3) . . ? O4 Rh2 N2 87.6(2) . 2_765 ? O3 Rh2 N2 85.2(2) . 2_765 ? C36 Rh2 N2 109.5(3) . 2_765 ? C34 Rh2 N2 149.5(3) . 2_765 ? C33 Rh2 N2 111.1(3) . 2_765 ? C37 Rh2 N2 92.7(3) . 2_765 ? C35 Rh2 N2 147.5(3) . 2_765 ? C19 N1 C22 116.1(7) . . ? C19 N1 Rh1 121.4(5) . . ? C22 N1 Rh1 122.0(5) . . ? C21 N2 C20 118.0(7) . . ? C21 N2 Rh2 120.2(5) . 2_765 ? C20 N2 Rh2 121.1(5) . 2_765 ? C1 O1 Rh1 129.4(5) . . ? C3 O2 Rh1 129.0(5) . . ? C10 O3 Rh2 130.0(5) . . ? C12 O4 Rh2 131.0(5) . . ? O7 S1 O6 116.5(5) . . ? O7 S1 O5 112.6(6) . . ? O6 S1 O5 114.0(5) . . ? O7 S1 C43 103.8(6) . . ? O6 S1 C43 104.6(5) . . ? O5 S1 C43 103.4(6) . . ? O10 S2 O8 125.0(9) . . ? O10 S2 O9 113.8(9) . . ? O8 S2 O9 110.9(8) . . ? O10 S2 C44 101.6(8) . . ? O8 S2 C44 105.3(7) . . ? O9 S2 C44 94.2(7) . . ? O1 C1 C2 127.7(7) . . ? O1 C1 C18 112.6(7) . . ? C2 C1 C18 119.7(6) . . ? C1 C2 C3 120.0(6) . . ? C1 C2 C11 119.2(6) . . ? C3 C2 C11 120.8(6) . . ? O2 C3 C2 127.3(7) . . ? O2 C3 C4 113.0(6) . . ? C2 C3 C4 119.8(6) . . ? C5 C4 C9 117.9(7) . . ? C5 C4 C3 121.5(7) . . ? C9 C4 C3 120.4(7) . . ? C6 C5 C4 121.4(8) . . ? C5 C6 C7 119.8(8) . . ? C8 C7 C6 120.2(8) . . ? C7 C8 C9 121.4(8) . . ? C8 C9 C4 119.2(7) . . ? C8 C9 C10 121.1(7) . . ? C4 C9 C10 119.7(7) . . ? O3 C10 C11 126.6(7) . . ? O3 C10 C9 113.3(7) . . ? C11 C10 C9 120.1(6) . . ? C12 C11 C10 120.8(6) . . ? C12 C11 C2 119.9(6) . . ? C10 C11 C2 119.2(6) . . ? O4 C12 C11 125.5(7) . . ? O4 C12 C13 114.2(7) . . ? C11 C12 C13 120.3(7) . . ? C14 C13 C18 118.4(8) . . ? C14 C13 C12 120.6(7) . . ? C18 C13 C12 121.0(7) . . ? C15 C14 C13 121.5(9) . . ? C14 C15 C16 120.2(10) . . ? C17 C16 C15 119.2(10) . . ? C16 C17 C18 119.7(9) . . ? C13 C18 C17 120.9(8) . . ? C13 C18 C1 119.2(7) . . ? C17 C18 C1 120.0(8) . . ? N1 C19 C20 121.8(8) . . ? N2 C20 C19 121.3(8) . . ? N2 C21 C22 120.1(8) . . ? N1 C22 C21 122.4(8) . . ? C27 C23 C24 106.8(9) . . ? C27 C23 C28 127.5(10) . . ? C24 C23 C28 125.7(10) . . ? C27 C23 Rh1 70.3(5) . . ? C24 C23 Rh1 70.0(5) . . ? C28 C23 Rh1 124.5(7) . . ? C25 C24 C23 108.5(8) . . ? C25 C24 C29 126.3(10) . . ? C23 C24 C29 125.0(11) . . ? C25 C24 Rh1 69.1(5) . . ? C23 C24 Rh1 71.1(5) . . ? C29 C24 Rh1 122.6(6) . . ? C24 C25 C26 107.4(9) . . ? C24 C25 C30 123.5(11) . . ? C26 C25 C30 128.7(12) . . ? C24 C25 Rh1 71.7(5) . . ? C26 C25 Rh1 72.3(5) . . ? C30 C25 Rh1 127.5(7) . . ? C27 C26 C25 107.7(9) . . ? C27 C26 C31 127.6(9) . . ? C25 C26 C31 124.3(10) . . ? C27 C26 Rh1 70.3(5) . . ? C25 C26 Rh1 68.5(5) . . ? C31 C26 Rh1 121.5(6) . . ? C26 C27 C23 109.4(8) . . ? C26 C27 C32 124.2(9) . . ? C23 C27 C32 126.2(10) . . ? C26 C27 Rh1 71.4(5) . . ? C23 C27 Rh1 71.2(5) . . ? C32 C27 Rh1 127.8(6) . . ? C34 C33 C37 106.4(8) . . ? C34 C33 C38 125.6(11) . . ? C37 C33 C38 127.8(11) . . ? C34 C33 Rh2 70.4(5) . . ? C37 C33 Rh2 71.0(5) . . ? C38 C33 Rh2 126.5(7) . . ? C33 C34 C35 108.8(8) . . ? C33 C34 C39 125.6(11) . . ? C35 C34 C39 125.5(11) . . ? C33 C34 Rh2 71.1(5) . . ? C35 C34 Rh2 71.3(5) . . ? C39 C34 Rh2 125.9(6) . . ? C36 C35 C34 106.5(8) . . ? C36 C35 C40 127.5(10) . . ? C34 C35 C40 126.0(10) . . ? C36 C35 Rh2 69.0(5) . . ? C34 C35 Rh2 69.3(5) . . ? C40 C35 Rh2 125.1(7) . . ? C37 C36 C35 109.2(8) . . ? C37 C36 C41 127.2(9) . . ? C35 C36 C41 123.4(10) . . ? C37 C36 Rh2 72.5(5) . . ? C35 C36 Rh2 72.6(5) . . ? C41 C36 Rh2 125.6(6) . . ? C36 C37 C33 108.9(8) . . ? C36 C37 C42 126.1(10) . . ? C33 C37 C42 125.0(11) . . ? C36 C37 Rh2 69.3(5) . . ? C33 C37 Rh2 70.0(5) . . ? C42 C37 Rh2 126.0(6) . . ? F3 C43 F1 107.2(11) . . ? F3 C43 F2 103.5(11) . . ? F1 C43 F2 109.3(11) . . ? F3 C43 S1 113.1(10) . . ? F1 C43 S1 113.8(8) . . ? F2 C43 S1 109.5(8) . . ? F5 C44 F4 102.6(11) . . ? F5 C44 F6 104.9(11) . . ? F4 C44 F6 102.3(11) . . ? F5 C44 S2 112.1(9) . . ? F4 C44 S2 117.2(12) . . ? F6 C44 S2 116.1(10) . . ? C45 C45 Cl2 120(2) 2_655 . ? C45 C45 Cl1 132(2) 2_655 . ? Cl2 C45 Cl1 107.2(8) . . ? Cl3 Cl3 C46 140.0(18) 2_567 . ? Cl3 C46 Cl4 115(2) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.099 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.129 # Attachment 'Complex 4a.cif' data_complex_4a _database_code_depnum_ccdc_archive 'CCDC 712024' #TrackingRef 'Complex 4a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H100 F12 Ir4 N4 O24 S4' _chemical_formula_weight 2866.88 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.834(5) _cell_length_b 16.026(7) _cell_length_c 16.992(7) _cell_angle_alpha 72.393(7) _cell_angle_beta 79.832(6) _cell_angle_gamma 66.762(6) _cell_volume 3054(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 654 _cell_measurement_theta_min 2.206 _cell_measurement_theta_max 18.252 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_T_max 0.6622 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.38 _diffrn_reflns_number 12706 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.2960 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10555 _reflns_number_gt 4059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10555 _refine_ls_number_parameters 620 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1440 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 0.780 _refine_ls_restrained_S_all 0.785 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.86642(6) 0.14774(5) 0.77021(4) 0.0387(2) Uani 1 1 d . . . Ir2 Ir 0.61502(6) 0.74185(5) 0.62759(4) 0.0397(2) Uani 1 1 d . . . N1 N 0.7686(11) 0.1892(8) 0.8759(8) 0.034(3) Uani 1 1 d . . . N2 N 0.5376(11) 0.7268(8) 0.7484(7) 0.030(3) Uani 1 1 d . . . O1 O 0.9237(8) 0.2562(8) 0.7632(7) 0.044(3) Uani 1 1 d . . . O2 O 0.7307(8) 0.2549(7) 0.7095(7) 0.036(3) Uani 1 1 d . . . O3 O 0.5643(9) 0.6349(8) 0.6283(7) 0.043(3) Uani 1 1 d . . . O4 O 0.7580(9) 0.6334(8) 0.6803(6) 0.042(3) Uani 1 1 d . . . C1 C 1.1204(14) 0.3968(15) 0.7716(12) 0.056(6) Uani 1 1 d U . . H1 H 1.1948 0.3636 0.7906 0.067 Uiso 1 1 calc R . . C2 C 1.0562(16) 0.3450(13) 0.7633(11) 0.059(6) Uani 1 1 d . . . H2 H 1.0865 0.2785 0.7734 0.070 Uiso 1 1 calc R . . C3 C 0.9467(13) 0.3988(13) 0.7395(12) 0.048(5) Uani 1 1 d . . . C4 C 0.9051(12) 0.4947(11) 0.7196(11) 0.038(5) Uani 1 1 d . . . C5 C 0.9655(13) 0.5449(13) 0.7244(11) 0.054(5) Uani 1 1 d . . . H5 H 0.9351 0.6116 0.7095 0.065 Uiso 1 1 calc R . . C6 C 1.0772(15) 0.4939(14) 0.7528(13) 0.072(7) Uani 1 1 d . . . H6 H 1.1218 0.5266 0.7587 0.086 Uiso 1 1 calc R . . C7 C 0.8735(15) 0.3466(12) 0.7350(10) 0.042(5) Uani 1 1 d . . . C8 C 0.7642(13) 0.3941(11) 0.7079(9) 0.034(4) Uani 1 1 d . . . C9 C 0.7206(13) 0.4968(12) 0.6878(10) 0.038(4) Uani 1 1 d . . . C10 C 0.7913(15) 0.5418(11) 0.6948(10) 0.038(5) Uani 1 1 d . . . C11 C 0.7033(12) 0.3409(12) 0.6965(10) 0.032(4) Uani 1 1 d . . . C12 C 0.5915(14) 0.3939(11) 0.6676(10) 0.039(4) Uani 1 1 d . . . C13 C 0.5477(14) 0.4938(12) 0.6440(11) 0.050(5) Uani 1 1 d . . . C14 C 0.6124(14) 0.5478(12) 0.6478(11) 0.038(5) Uani 1 1 d . . . C15 C 0.5177(16) 0.3520(13) 0.6611(13) 0.066(6) Uani 1 1 d . . . H15 H 0.5448 0.2853 0.6775 0.080 Uiso 1 1 calc R . . C16 C 0.4112(17) 0.3963(14) 0.6338(16) 0.102(10) Uani 1 1 d . . . H16 H 0.3652 0.3634 0.6306 0.123 Uiso 1 1 calc R . . C17 C 0.376(2) 0.4906(17) 0.612(2) 0.187(19) Uani 1 1 d . . . H17 H 0.3012 0.5247 0.5942 0.225 Uiso 1 1 calc R . . C18 C 0.4394(15) 0.5411(13) 0.6121(16) 0.088(9) Uani 1 1 d . . . H18 H 0.4111 0.6075 0.5912 0.105 Uiso 1 1 calc R . . C19 C 0.6684(14) 0.1897(11) 0.8931(10) 0.038(4) Uani 1 1 d . . . H19 H 0.6360 0.1752 0.8552 0.045 Uiso 1 1 calc R . . C20 C 0.6046(15) 0.2096(11) 0.9620(11) 0.047(5) Uani 1 1 d . . . H20 H 0.5298 0.2088 0.9700 0.057 Uiso 1 1 calc R . . C21 C 0.6447(14) 0.2315(10) 1.0226(11) 0.037(4) Uani 1 1 d . . . C22 C 0.7549(15) 0.2303(10) 1.0037(10) 0.044(5) Uani 1 1 d . . . H22 H 0.7884 0.2458 1.0402 0.053 Uiso 1 1 calc R . . C23 C 0.8162(14) 0.2075(11) 0.9342(10) 0.044(5) Uani 1 1 d . . . H23 H 0.8929 0.2040 0.9250 0.052 Uiso 1 1 calc R . . C24 C 0.4320(14) 0.7325(10) 0.7674(10) 0.035(4) Uani 1 1 d . . . H24 H 0.3943 0.7263 0.7274 0.042 Uiso 1 1 calc R . . C25 C 0.3716(15) 0.7466(11) 0.8396(12) 0.046(5) Uani 1 1 d . . . H25 H 0.2937 0.7537 0.8458 0.055 Uiso 1 1 calc R . . C26 C 0.4176(14) 0.7505(11) 0.9008(10) 0.032(4) Uani 1 1 d . . . C27 C 0.5354(17) 0.7377(11) 0.8895(10) 0.055(6) Uani 1 1 d . . . H27 H 0.5754 0.7368 0.9319 0.066 Uiso 1 1 calc R . . C28 C 0.5876(16) 0.7268(11) 0.8126(11) 0.050(5) Uani 1 1 d . . . H28 H 0.6659 0.7186 0.8040 0.060 Uiso 1 1 calc R . . C29 C 0.8758(19) 0.0504(14) 0.7053(15) 0.072(7) Uani 1 1 d . . . C30 C 0.8518(19) 0.0141(14) 0.7868(14) 0.062(6) Uani 1 1 d . . . C31 C 0.9472(19) -0.0013(12) 0.8302(13) 0.068(7) Uani 1 1 d . . . C32 C 1.0196(16) 0.0308(13) 0.7783(12) 0.053(5) Uiso 1 1 d . . . C33 C 0.9882(18) 0.0699(13) 0.6931(12) 0.072(7) Uani 1 1 d . . . C34 C 1.062(3) 0.1036(18) 0.625(2) 0.34(4) Uani 1 1 d . . . H34A H 1.1111 0.0522 0.6003 0.505 Uiso 1 1 calc R . . H34B H 1.1099 0.1255 0.6472 0.505 Uiso 1 1 calc R . . H34C H 1.0157 0.1556 0.5833 0.505 Uiso 1 1 calc R . . C35 C 0.804(2) 0.0808(16) 0.6291(17) 0.20(2) Uani 1 1 d . . . H35A H 0.8206 0.0262 0.6078 0.307 Uiso 1 1 calc R . . H35B H 0.8248 0.1293 0.5857 0.307 Uiso 1 1 calc R . . H35C H 0.7234 0.1059 0.6458 0.307 Uiso 1 1 calc R . . C36 C 0.7554(19) -0.0199(15) 0.8229(15) 0.107(9) Uani 1 1 d . . . H36A H 0.6832 0.0307 0.8060 0.161 Uiso 1 1 calc R . . H36B H 0.7555 -0.0387 0.8834 0.161 Uiso 1 1 calc R . . H36C H 0.7649 -0.0739 0.8029 0.161 Uiso 1 1 calc R . . C37 C 0.960(2) -0.0499(14) 0.9229(12) 0.109(9) Uani 1 1 d . . . H37A H 1.0212 -0.1119 0.9297 0.163 Uiso 1 1 calc R . . H37B H 0.8890 -0.0571 0.9489 0.163 Uiso 1 1 calc R . . H37C H 0.9797 -0.0116 0.9492 0.163 Uiso 1 1 calc R . . C38 C 1.1309(19) 0.0209(16) 0.8097(14) 0.114(9) Uiso 1 1 d . . . H38A H 1.1203 0.0162 0.8692 0.171 Uiso 1 1 calc R . . H38B H 1.1508 0.0761 0.7804 0.171 Uiso 1 1 calc R . . H38C H 1.1923 -0.0358 0.7994 0.171 Uiso 1 1 calc R . . C39 C 0.709(2) 0.8305(13) 0.5578(13) 0.079(8) Uani 1 1 d . . . C40 C 0.613(2) 0.8809(13) 0.6087(14) 0.068(8) Uani 1 1 d . . . C41 C 0.517(2) 0.8820(12) 0.5776(12) 0.066(7) Uani 1 1 d . . . C42 C 0.5537(17) 0.8310(12) 0.5157(11) 0.053(5) Uani 1 1 d . . . C43 C 0.6743(16) 0.7932(13) 0.5015(11) 0.047(5) Uani 1 1 d . . . C44 C 0.8350(18) 0.8019(17) 0.5808(14) 0.112(10) Uani 1 1 d . . . H44A H 0.8358 0.7928 0.6404 0.168 Uiso 1 1 calc R . . H44B H 0.8639 0.8519 0.5505 0.168 Uiso 1 1 calc R . . H44C H 0.8834 0.7433 0.5658 0.168 Uiso 1 1 calc R . . C45 C 0.605(2) 0.9288(14) 0.6737(15) 0.130(11) Uani 1 1 d . . . H45A H 0.6486 0.9705 0.6540 0.195 Uiso 1 1 calc R . . H45B H 0.6364 0.8816 0.7243 0.195 Uiso 1 1 calc R . . H45C H 0.5254 0.9658 0.6854 0.195 Uiso 1 1 calc R . . C46 C 0.3958(19) 0.9330(14) 0.5995(14) 0.109(9) Uani 1 1 d . . . H46A H 0.3813 0.9160 0.6598 0.163 Uiso 1 1 calc R . . H46B H 0.3475 0.9160 0.5735 0.163 Uiso 1 1 calc R . . H46C H 0.3788 1.0009 0.5798 0.163 Uiso 1 1 calc R . . C47 C 0.4855(16) 0.8107(15) 0.4623(12) 0.085(7) Uani 1 1 d . . . H47A H 0.5001 0.8394 0.4038 0.127 Uiso 1 1 calc R . . H47B H 0.4042 0.8373 0.4779 0.127 Uiso 1 1 calc R . . H47C H 0.5089 0.7427 0.4712 0.127 Uiso 1 1 calc R . . C48 C 0.7442(16) 0.7464(13) 0.4436(10) 0.074(7) Uani 1 1 d . . . H48A H 0.7247 0.6925 0.4458 0.111 Uiso 1 1 calc R . . H48B H 0.8237 0.7245 0.4562 0.111 Uiso 1 1 calc R . . H48C H 0.7333 0.7894 0.3881 0.111 Uiso 1 1 calc R . . C49 C 0.399(3) 0.0295(17) 0.874(2) 0.115(11) Uani 1 1 d . . . F1 F 0.5065(17) -0.0249(14) 0.8958(14) 0.253(13) Uani 1 1 d . . . F2 F 0.3907(14) -0.0237(10) 0.8305(12) 0.157(7) Uani 1 1 d . . . F3 F 0.3268(16) 0.0342(13) 0.9351(10) 0.157(9) Uani 1 1 d . . . S1 S 0.4046(5) 0.1368(4) 0.8047(4) 0.0657(16) Uani 1 1 d . . . O5 O 0.4924(15) 0.1210(11) 0.7442(10) 0.137(7) Uani 1 1 d . . . O6 O 0.413(2) 0.1900(16) 0.8608(14) 0.196(11) Uani 1 1 d . . . O7 O 0.3000(16) 0.1715(12) 0.7736(12) 0.147(8) Uani 1 1 d . . . C50 C 0.1173(14) 0.8251(11) 0.6415(9) 0.095(8) Uiso 1 1 d D . . F4 F 0.0271(13) 0.8882(10) 0.6124(9) 0.170(7) Uiso 1 1 d D . . F5 F 0.2007(18) 0.8578(18) 0.6388(15) 0.48(2) Uiso 1 1 d D . . F6 F 0.1657(19) 0.7578(13) 0.5930(11) 0.310(13) Uiso 1 1 d D . . O8 O 0.200(2) 0.6666(12) 0.7456(14) 0.255(13) Uiso 1 1 d D . . S2 S 0.1015(15) 0.7551(11) 0.7444(8) 0.320(8) Uiso 1 1 d D . . O9 O 0.090(3) 0.812(2) 0.7985(12) 0.38(2) Uiso 1 1 d D . . O10 O -0.008(2) 0.749(2) 0.7513(16) 0.338(19) Uiso 1 1 d D . . O11 O 0.3536(18) 0.4287(15) 0.8795(14) 0.204(11) Uani 1 1 d . . . O12 O 0.814(3) 0.751(2) 0.8293(19) 0.293(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0289(4) 0.0365(5) 0.0480(5) -0.0101(4) -0.0044(4) -0.0091(4) Ir2 0.0399(5) 0.0360(5) 0.0465(5) -0.0107(4) 0.0029(4) -0.0194(4) N1 0.032(8) 0.029(8) 0.034(9) -0.009(7) 0.016(7) -0.012(7) N2 0.034(8) 0.031(8) 0.020(8) 0.004(6) -0.013(6) -0.011(6) O1 0.027(7) 0.053(8) 0.055(8) -0.015(7) -0.009(6) -0.014(6) O2 0.027(6) 0.021(7) 0.061(8) -0.010(6) -0.010(6) -0.009(5) O3 0.032(7) 0.034(8) 0.063(9) -0.006(7) -0.021(6) -0.010(6) O4 0.037(7) 0.058(9) 0.045(8) -0.012(7) -0.019(6) -0.024(6) C1 0.022(9) 0.078(13) 0.077(13) -0.025(11) -0.022(9) -0.016(9) C2 0.059(14) 0.043(13) 0.071(15) -0.026(11) -0.010(12) -0.006(11) C3 0.006(9) 0.064(14) 0.080(15) -0.029(12) -0.013(9) -0.006(9) C4 0.008(9) 0.030(11) 0.080(14) -0.021(10) -0.011(9) -0.003(8) C5 0.016(10) 0.051(13) 0.083(15) -0.001(11) 0.000(10) -0.013(9) C6 0.032(12) 0.057(15) 0.14(2) -0.024(14) -0.012(13) -0.030(11) C7 0.042(12) 0.025(11) 0.045(12) -0.013(9) 0.017(9) -0.003(9) C8 0.023(9) 0.026(10) 0.035(11) 0.010(8) -0.008(8) -0.001(8) C9 0.029(10) 0.047(12) 0.040(11) -0.026(9) 0.014(9) -0.012(9) C10 0.059(13) 0.017(10) 0.044(12) -0.013(9) 0.007(10) -0.020(9) C11 0.010(9) 0.035(11) 0.046(11) -0.006(9) 0.007(8) -0.010(8) C12 0.034(11) 0.027(11) 0.053(12) -0.017(9) 0.001(9) -0.006(9) C13 0.027(11) 0.045(12) 0.080(15) -0.003(11) -0.019(10) -0.017(9) C14 0.037(11) 0.037(12) 0.054(13) -0.028(10) -0.001(9) -0.017(9) C15 0.049(14) 0.046(13) 0.114(19) -0.022(12) -0.008(13) -0.025(11) C16 0.049(15) 0.036(14) 0.23(3) -0.023(17) -0.045(17) -0.012(11) C17 0.11(2) 0.051(18) 0.40(6) -0.07(3) -0.16(3) 0.027(17) C18 0.043(13) 0.028(12) 0.20(3) -0.027(14) -0.079(16) 0.002(10) C19 0.040(11) 0.048(12) 0.041(12) -0.030(9) 0.016(9) -0.026(9) C20 0.049(12) 0.029(11) 0.065(14) -0.007(10) -0.017(11) -0.014(9) C21 0.041(11) 0.025(10) 0.041(12) -0.008(9) -0.016(9) -0.002(8) C22 0.055(13) 0.031(11) 0.048(12) -0.025(9) -0.002(10) -0.007(9) C23 0.041(11) 0.036(11) 0.039(12) -0.009(9) 0.009(9) -0.004(9) C24 0.038(11) 0.031(10) 0.043(12) -0.014(9) -0.011(9) -0.012(8) C25 0.034(11) 0.040(12) 0.064(14) -0.020(10) 0.016(11) -0.016(9) C26 0.032(11) 0.039(11) 0.024(10) -0.002(8) -0.006(9) -0.014(8) C27 0.092(17) 0.040(12) 0.023(11) 0.003(9) 0.005(11) -0.026(11) C28 0.061(13) 0.048(12) 0.035(12) 0.006(10) -0.015(10) -0.022(10) C29 0.078(17) 0.050(14) 0.083(18) -0.049(13) -0.030(15) 0.016(12) C30 0.070(17) 0.048(14) 0.058(16) -0.011(12) -0.020(14) -0.007(12) C31 0.071(16) 0.024(11) 0.065(16) 0.001(10) 0.008(13) 0.014(11) C33 0.070(15) 0.043(13) 0.062(15) -0.006(10) 0.038(12) -0.001(11) C34 0.25(4) 0.08(2) 0.38(5) 0.05(3) 0.27(4) 0.06(2) C35 0.26(4) 0.09(2) 0.23(3) -0.10(2) -0.23(3) 0.11(2) C36 0.10(2) 0.072(17) 0.17(3) -0.034(17) 0.001(18) -0.056(15) C37 0.14(2) 0.060(16) 0.075(17) -0.001(13) -0.035(16) 0.021(15) C39 0.12(2) 0.025(12) 0.069(16) 0.008(11) 0.034(16) -0.036(13) C40 0.13(2) 0.026(12) 0.067(17) 0.033(11) -0.072(16) -0.047(13) C41 0.093(18) 0.020(11) 0.050(14) -0.013(10) 0.043(13) -0.001(11) C42 0.079(15) 0.045(12) 0.046(13) 0.010(10) -0.023(11) -0.044(12) C43 0.049(13) 0.062(14) 0.046(13) -0.044(11) 0.001(10) -0.016(11) C44 0.092(18) 0.17(3) 0.12(2) 0.011(18) -0.028(16) -0.122(19) C45 0.24(3) 0.044(15) 0.12(2) -0.041(15) -0.05(2) -0.041(18) C46 0.12(2) 0.057(16) 0.15(2) -0.037(15) 0.064(18) -0.050(15) C47 0.073(16) 0.13(2) 0.086(17) -0.028(15) -0.031(13) -0.057(15) C48 0.082(16) 0.084(17) 0.042(13) -0.026(12) 0.010(11) -0.014(13) C49 0.16(3) 0.039(16) 0.15(3) -0.008(19) -0.10(3) -0.012(18) F1 0.143(17) 0.21(2) 0.30(3) 0.167(19) -0.107(17) -0.089(15) F2 0.146(15) 0.065(11) 0.25(2) -0.060(12) -0.012(14) -0.018(10) F3 0.169(18) 0.166(17) 0.114(13) 0.001(11) 0.064(12) -0.097(14) S1 0.045(3) 0.064(4) 0.087(5) -0.015(3) -0.007(3) -0.022(3) O5 0.117(15) 0.103(14) 0.117(14) -0.004(11) 0.038(12) -0.002(11) O6 0.25(3) 0.20(2) 0.18(2) 0.033(18) -0.09(2) -0.15(2) O7 0.151(18) 0.124(15) 0.182(19) 0.014(13) -0.104(15) -0.068(13) O11 0.17(2) 0.18(2) 0.22(2) -0.039(18) -0.126(19) 0.007(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O2 2.062(10) . ? Ir1 O1 2.104(11) . ? Ir1 C32 2.104(18) . ? Ir1 C33 2.108(17) . ? Ir1 C29 2.124(19) . ? Ir1 N1 2.124(12) . ? Ir1 C30 2.15(2) . ? Ir1 C31 2.183(17) . ? Ir2 O3 2.057(11) . ? Ir2 C42 2.067(16) . ? Ir2 O4 2.077(11) . ? Ir2 C41 2.084(18) . ? Ir2 N2 2.104(12) . ? Ir2 C40 2.145(17) . ? Ir2 C43 2.168(18) . ? Ir2 C39 2.173(19) . ? N1 C19 1.266(18) . ? N1 C23 1.404(19) . ? N2 C24 1.311(18) . ? N2 C28 1.360(18) . ? O1 C7 1.302(17) . ? O2 C11 1.238(16) . ? O3 C14 1.245(17) . ? O4 C10 1.311(16) . ? C1 C6 1.38(2) . ? C1 C2 1.43(2) . ? C2 C3 1.39(2) . ? C3 C4 1.37(2) . ? C3 C7 1.51(2) . ? C4 C5 1.35(2) . ? C4 C10 1.43(2) . ? C5 C6 1.43(2) . ? C7 C8 1.39(2) . ? C8 C11 1.43(2) . ? C8 C9 1.462(19) . ? C9 C10 1.40(2) . ? C9 C14 1.47(2) . ? C11 C12 1.43(2) . ? C12 C15 1.40(2) . ? C12 C13 1.42(2) . ? C13 C18 1.41(2) . ? C13 C14 1.44(2) . ? C15 C16 1.36(2) . ? C16 C17 1.35(3) . ? C17 C18 1.35(3) . ? C19 C20 1.35(2) . ? C20 C21 1.42(2) . ? C21 C22 1.39(2) . ? C21 C26 1.45(2) 2_667 ? C22 C23 1.36(2) . ? C24 C25 1.36(2) . ? C25 C26 1.31(2) . ? C26 C27 1.43(2) . ? C26 C21 1.45(2) 2_667 ? C27 C28 1.39(2) . ? C29 C30 1.36(3) . ? C29 C33 1.56(3) . ? C29 C35 1.56(3) . ? C30 C31 1.44(3) . ? C30 C36 1.51(3) . ? C31 C32 1.31(2) . ? C31 C37 1.54(2) . ? C32 C33 1.45(2) . ? C32 C38 1.55(3) . ? C33 C34 1.47(3) . ? C39 C40 1.48(3) . ? C39 C43 1.48(3) . ? C39 C44 1.58(3) . ? C40 C41 1.42(3) . ? C40 C45 1.49(3) . ? C41 C42 1.43(2) . ? C41 C46 1.48(3) . ? C42 C43 1.43(2) . ? C42 C47 1.54(2) . ? C43 C48 1.39(2) . ? C49 F3 1.26(4) . ? C49 F2 1.32(3) . ? C49 F1 1.36(3) . ? C49 S1 1.78(3) . ? S1 O7 1.370(16) . ? S1 O5 1.384(16) . ? S1 O6 1.50(2) . ? C50 F4 1.258(14) . ? C50 F5 1.353(15) . ? C50 F6 1.435(15) . ? C50 S2 1.796(18) . ? O8 S2 1.481(10) . ? S2 O10 1.426(10) . ? S2 O9 1.436(10) . ? 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 O2 Ir1 O1 84.3(4) . . ? O2 Ir1 C32 154.3(6) . . ? O1 Ir1 C32 101.8(6) . . ? O2 Ir1 C33 114.0(7) . . ? O1 Ir1 C33 103.0(7) . . ? C32 Ir1 C33 40.4(7) . . ? O2 Ir1 C29 94.8(6) . . ? O1 Ir1 C29 142.2(8) . . ? C32 Ir1 C29 65.0(7) . . ? C33 Ir1 C29 43.2(8) . . ? O2 Ir1 N1 82.5(5) . . ? O1 Ir1 N1 83.2(5) . . ? C32 Ir1 N1 122.8(6) . . ? C33 Ir1 N1 162.6(6) . . ? C29 Ir1 N1 134.3(8) . . ? O2 Ir1 C30 110.2(7) . . ? O1 Ir1 C30 165.1(7) . . ? C32 Ir1 C30 63.7(8) . . ? C33 Ir1 C30 68.7(8) . . ? C29 Ir1 C30 37.1(7) . . ? N1 Ir1 C30 101.4(7) . . ? O2 Ir1 C31 148.7(7) . . ? O1 Ir1 C31 126.9(7) . . ? C32 Ir1 C31 35.6(6) . . ? C33 Ir1 C31 65.8(7) . . ? C29 Ir1 C31 63.0(8) . . ? N1 Ir1 C31 97.3(6) . . ? C30 Ir1 C31 38.8(7) . . ? O3 Ir2 C42 97.9(5) . . ? O3 Ir2 O4 84.2(4) . . ? C42 Ir2 O4 142.6(7) . . ? O3 Ir2 C41 121.3(8) . . ? C42 Ir2 C41 40.2(7) . . ? O4 Ir2 C41 154.4(8) . . ? O3 Ir2 N2 83.2(5) . . ? C42 Ir2 N2 131.4(7) . . ? O4 Ir2 N2 86.0(4) . . ? C41 Ir2 N2 98.5(6) . . ? O3 Ir2 C40 160.5(7) . . ? C42 Ir2 C40 66.9(7) . . ? O4 Ir2 C40 115.4(7) . . ? C41 Ir2 C40 39.2(8) . . ? N2 Ir2 C40 97.5(8) . . ? O3 Ir2 C43 106.9(6) . . ? C42 Ir2 C43 39.3(7) . . ? O4 Ir2 C43 104.2(6) . . ? C41 Ir2 C43 68.3(7) . . ? N2 Ir2 C43 166.1(6) . . ? C40 Ir2 C43 69.8(8) . . ? O3 Ir2 C39 145.1(7) . . ? C42 Ir2 C39 63.6(8) . . ? O4 Ir2 C39 93.7(7) . . ? C41 Ir2 C39 64.5(8) . . ? N2 Ir2 C39 131.6(7) . . ? C40 Ir2 C39 40.0(8) . . ? C43 Ir2 C39 39.8(7) . . ? C19 N1 C23 117.0(14) . . ? C19 N1 Ir1 121.2(12) . . ? C23 N1 Ir1 121.4(10) . . ? C24 N2 C28 112.7(14) . . ? C24 N2 Ir2 124.6(11) . . ? C28 N2 Ir2 121.7(11) . . ? C7 O1 Ir1 129.1(11) . . ? C11 O2 Ir1 129.1(10) . . ? C14 O3 Ir2 132.2(10) . . ? C10 O4 Ir2 131.9(10) . . ? C6 C1 C2 121.8(16) . . ? C3 C2 C1 115.2(17) . . ? C4 C3 C2 122.7(16) . . ? C4 C3 C7 120.3(14) . . ? C2 C3 C7 116.9(17) . . ? C5 C4 C3 122.9(15) . . ? C5 C4 C10 119.8(16) . . ? C3 C4 C10 117.2(14) . . ? C4 C5 C6 117.4(17) . . ? C1 C6 C5 119.9(16) . . ? O1 C7 C8 127.0(17) . . ? O1 C7 C3 111.5(15) . . ? C8 C7 C3 121.4(16) . . ? C7 C8 C11 118.7(16) . . ? C7 C8 C9 117.5(15) . . ? C11 C8 C9 123.7(13) . . ? C10 C9 C8 118.8(14) . . ? C10 C9 C14 122.6(16) . . ? C8 C9 C14 117.8(14) . . ? O4 C10 C9 122.8(16) . . ? O4 C10 C4 112.5(14) . . ? C9 C10 C4 124.7(15) . . ? O2 C11 C12 113.6(14) . . ? O2 C11 C8 130.2(14) . . ? C12 C11 C8 116.1(15) . . ? C15 C12 C13 115.1(15) . . ? C15 C12 C11 122.9(16) . . ? C13 C12 C11 122.0(15) . . ? C18 C13 C12 118.8(16) . . ? C18 C13 C14 119.0(17) . . ? C12 C13 C14 122.1(15) . . ? O3 C14 C13 116.7(15) . . ? O3 C14 C9 124.9(15) . . ? C13 C14 C9 117.4(16) . . ? C16 C15 C12 127.0(19) . . ? C17 C16 C15 114(2) . . ? C16 C17 C18 125(2) . . ? C17 C18 C13 119.1(19) . . ? N1 C19 C20 124.0(17) . . ? C19 C20 C21 122.6(17) . . ? C22 C21 C20 113.1(16) . . ? C22 C21 C26 121.7(16) . 2_667 ? C20 C21 C26 125.2(17) . 2_667 ? C23 C22 C21 121.7(17) . . ? C22 C23 N1 121.4(16) . . ? N2 C24 C25 125.6(16) . . ? C26 C25 C24 122.0(17) . . ? C25 C26 C27 117.3(16) . . ? C25 C26 C21 123.6(16) . 2_667 ? C27 C26 C21 119.1(16) . 2_667 ? C28 C27 C26 115.8(18) . . ? N2 C28 C27 126.3(18) . . ? C30 C29 C33 110.7(19) . . ? C30 C29 C35 130(3) . . ? C33 C29 C35 119(2) . . ? C30 C29 Ir1 72.6(13) . . ? C33 C29 Ir1 67.9(10) . . ? C35 C29 Ir1 121.8(13) . . ? C29 C30 C31 107(2) . . ? C29 C30 C36 127(2) . . ? C31 C30 C36 126(2) . . ? C29 C30 Ir1 70.3(13) . . ? C31 C30 Ir1 71.7(12) . . ? C36 C30 Ir1 131.1(15) . . ? C32 C31 C30 109.4(19) . . ? C32 C31 C37 126(2) . . ? C30 C31 C37 124(2) . . ? C32 C31 Ir1 68.9(11) . . ? C30 C31 Ir1 69.4(11) . . ? C37 C31 Ir1 128.8(14) . . ? C31 C32 C33 115.0(19) . . ? C31 C32 C38 119(2) . . ? C33 C32 C38 125(2) . . ? C31 C32 Ir1 75.5(11) . . ? C33 C32 Ir1 70.0(10) . . ? C38 C32 Ir1 126.0(14) . . ? C32 C33 C34 123(3) . . ? C32 C33 C29 97.8(15) . . ? C34 C33 C29 139(3) . . ? C32 C33 Ir1 69.6(10) . . ? C34 C33 Ir1 127.0(17) . . ? C29 C33 Ir1 68.9(9) . . ? C40 C39 C43 113(2) . . ? C40 C39 C44 119(2) . . ? C43 C39 C44 126(2) . . ? C40 C39 Ir2 69.0(10) . . ? C43 C39 Ir2 69.9(11) . . ? C44 C39 Ir2 117.8(13) . . ? C41 C40 C39 103.3(19) . . ? C41 C40 C45 123(2) . . ? C39 C40 C45 133(2) . . ? C41 C40 Ir2 68.1(10) . . ? C39 C40 Ir2 71.0(11) . . ? C45 C40 Ir2 127.1(14) . . ? C40 C41 C42 109.3(19) . . ? C40 C41 C46 127(2) . . ? C42 C41 C46 124(2) . . ? C40 C41 Ir2 72.7(11) . . ? C42 C41 Ir2 69.2(10) . . ? C46 C41 Ir2 127.6(14) . . ? C43 C42 C41 113.5(17) . . ? C43 C42 C47 115.5(18) . . ? C41 C42 C47 131(2) . . ? C43 C42 Ir2 74.2(11) . . ? C41 C42 Ir2 70.5(10) . . ? C47 C42 Ir2 123.8(12) . . ? C48 C43 C42 132.3(18) . . ? C48 C43 C39 126.6(19) . . ? C42 C43 C39 100.5(16) . . ? C48 C43 Ir2 131.7(14) . . ? C42 C43 Ir2 66.5(10) . . ? C39 C43 Ir2 70.3(10) . . ? F3 C49 F2 112(3) . . ? F3 C49 F1 113(3) . . ? F2 C49 F1 96(3) . . ? F3 C49 S1 118(2) . . ? F2 C49 S1 109(2) . . ? F1 C49 S1 107(2) . . ? O7 S1 O5 112.4(13) . . ? O7 S1 O6 113.2(13) . . ? O5 S1 O6 115.1(13) . . ? O7 S1 C49 98.8(13) . . ? O5 S1 C49 111.9(15) . . ? O6 S1 C49 103.8(13) . . ? F4 C50 F5 113.4(13) . . ? F4 C50 F6 110.8(12) . . ? F5 C50 F6 103.9(11) . . ? F4 C50 S2 115.4(11) . . ? F5 C50 S2 108.6(11) . . ? F6 C50 S2 103.8(10) . . ? O10 S2 O9 104(3) . . ? O10 S2 O8 116(3) . . ? O9 S2 O8 122(3) . . ? O10 S2 C50 105.9(11) . . ? O9 S2 C50 105.7(11) . . ? O8 S2 C50 102.0(10) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.154 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.196 # Attachment 'Complex 4b.cif' data_complex_4b _database_code_depnum_ccdc_archive 'CCDC 749420' #TrackingRef 'Complex 4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H116 F12 N4 O28 Rh4 S4' _chemical_formula_weight 2637.89 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.662(10) _cell_length_b 16.174(13) _cell_length_c 16.710(14) _cell_angle_alpha 101.244(12) _cell_angle_beta 97.315(12) _cell_angle_gamma 110.118(11) _cell_volume 3081(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 761 _cell_measurement_theta_min 2.176 _cell_measurement_theta_max 21.590 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9228 _exptl_absorpt_correction_T_max 0.9351 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.21 _diffrn_reflns_number 12809 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.1755 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10638 _reflns_number_gt 5434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10638 _refine_ls_number_parameters 714 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1586 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2587 _refine_ls_wR_factor_gt 0.2365 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.13436(7) 0.25823(5) 0.12676(5) 0.0341(3) Uani 1 1 d . . . Rh2 Rh 0.45315(7) 0.83194(5) 0.27460(5) 0.0334(3) Uani 1 1 d . . . N1 N 0.2230(7) 0.2631(5) 0.2452(5) 0.033(2) Uani 1 1 d . . . N2 N 0.5212(8) 0.8053(6) 0.3839(5) 0.035(2) Uani 1 1 d . . . O1 O 0.2865(6) 0.3569(4) 0.1217(5) 0.043(2) Uani 1 1 d . . . O2 O 0.0987(6) 0.3641(5) 0.1885(5) 0.0415(19) Uani 1 1 d . . . O3 O 0.2993(6) 0.7327(4) 0.2759(4) 0.0335(17) Uani 1 1 d . . . O4 O 0.4922(6) 0.7233(5) 0.2170(5) 0.0391(18) Uani 1 1 d . . . O5 O 0.0489(10) 0.8430(7) 0.3049(7) 0.095(4) Uani 1 1 d . . . O6 O -0.1263(10) 0.8414(8) 0.3426(8) 0.111(4) Uani 1 1 d . . . O7 O -0.0737(12) 0.8911(9) 0.2240(6) 0.114(5) Uani 1 1 d . . . O8 O 0.5706(13) 0.1546(8) 0.2734(9) 0.134(6) Uani 1 1 d . . . O9 O 0.4576(11) 0.1395(13) 0.1388(10) 0.212(11) Uani 1 1 d . . . O10 O 0.6178(10) 0.0997(7) 0.1396(8) 0.112(5) Uani 1 1 d . . . F1 F -0.0365(10) 1.0388(7) 0.3678(8) 0.141(5) Uani 1 1 d . . . F2 F 0.0925(10) 1.0008(8) 0.4401(7) 0.126(4) Uani 1 1 d . . . F3 F 0.1184(11) 1.0434(8) 0.3305(9) 0.150(5) Uani 1 1 d . . . F4 F 0.5957(8) 0.3215(5) 0.2268(6) 0.091(3) Uani 1 1 d . . . F5 F 0.7479(11) 0.2936(10) 0.2279(11) 0.187(7) Uani 1 1 d . . . F6 F 0.6510(13) 0.2798(7) 0.1147(7) 0.143(5) Uani 1 1 d . . . S1 S -0.0360(3) 0.8807(3) 0.3017(2) 0.0624(10) Uani 1 1 d . . . S2 S 0.5676(4) 0.1510(2) 0.1866(3) 0.0683(11) Uani 1 1 d . . . C1 C 0.3239(9) 0.4408(8) 0.1472(7) 0.036(3) Uani 1 1 d . . . C2 C 0.2669(9) 0.4944(7) 0.1883(6) 0.031(2) Uani 1 1 d . . . C3 C 0.1532(9) 0.4493(7) 0.2010(7) 0.033(3) Uani 1 1 d . . . C4 C 0.0919(9) 0.5053(7) 0.2320(7) 0.042(3) Uani 1 1 d . . . C5 C -0.0242(10) 0.4632(8) 0.2387(10) 0.066(4) Uani 1 1 d . . . H5 H -0.0587 0.3986 0.2249 0.080 Uiso 1 1 calc R . . C6 C -0.0869(11) 0.5121(9) 0.2640(11) 0.087(6) Uani 1 1 d . . . H6 H -0.1640 0.4823 0.2689 0.104 Uiso 1 1 calc R . . C7 C -0.0356(11) 0.6095(9) 0.2836(12) 0.095(6) Uani 1 1 d . . . H7 H -0.0787 0.6452 0.3004 0.114 Uiso 1 1 calc R . . C8 C 0.0767(10) 0.6508(8) 0.2777(8) 0.053(4) Uani 1 1 d . . . H8 H 0.1103 0.7153 0.2896 0.063 Uiso 1 1 calc R . . C9 C 0.1422(9) 0.6003(7) 0.2547(7) 0.038(3) Uani 1 1 d . . . C10 C 0.2623(9) 0.6474(7) 0.2493(6) 0.029(2) Uani 1 1 d . . . C11 C 0.3226(9) 0.5939(7) 0.2136(6) 0.031(2) Uani 1 1 d . . . C12 C 0.4368(8) 0.6393(7) 0.2018(6) 0.029(2) Uani 1 1 d . . . C13 C 0.4956(10) 0.5826(8) 0.1616(8) 0.054(3) Uani 1 1 d . . . C14 C 0.6106(12) 0.6270(10) 0.1557(10) 0.074(4) Uani 1 1 d . . . H14 H 0.6467 0.6915 0.1740 0.088 Uiso 1 1 calc R . . C15 C 0.6699(14) 0.5763(10) 0.1233(14) 0.121(8) Uani 1 1 d . . . H15 H 0.7482 0.6042 0.1204 0.145 Uiso 1 1 calc R . . C16 C 0.6093(14) 0.4800(11) 0.0942(13) 0.111(7) Uani 1 1 d . . . H16 H 0.6499 0.4443 0.0722 0.133 Uiso 1 1 calc R . . C17 C 0.4975(12) 0.4365(10) 0.0960(11) 0.083(5) Uani 1 1 d . . . H17 H 0.4588 0.3729 0.0717 0.100 Uiso 1 1 calc R . . C18 C 0.4404(9) 0.4884(8) 0.1352(7) 0.040(3) Uani 1 1 d . . . C19 C 0.3191(10) 0.2453(8) 0.2514(7) 0.047(3) Uani 1 1 d . . . H19 H 0.3507 0.2381 0.2031 0.057 Uiso 1 1 calc R . . C20 C 0.3738(10) 0.2369(8) 0.3226(7) 0.043(3) Uani 1 1 d . . . H20 H 0.4434 0.2267 0.3238 0.052 Uiso 1 1 calc R . . C21 C 0.3282(9) 0.2431(7) 0.3943(6) 0.036(3) Uani 1 1 d . . . C22 C 0.2320(10) 0.2649(8) 0.3899(7) 0.045(3) Uani 1 1 d . . . H22 H 0.1998 0.2734 0.4377 0.054 Uiso 1 1 calc R . . C23 C 0.1823(10) 0.2743(8) 0.3148(8) 0.046(3) Uani 1 1 d . . . H23 H 0.1160 0.2894 0.3129 0.055 Uiso 1 1 calc R . . C24 C 0.6302(9) 0.8099(7) 0.3978(7) 0.039(3) Uani 1 1 d . . . H24 H 0.6745 0.8245 0.3571 0.047 Uiso 1 1 calc R . . C25 C 0.6815(10) 0.7940(7) 0.4697(7) 0.039(3) Uani 1 1 d . . . H25 H 0.7594 0.7992 0.4771 0.047 Uiso 1 1 calc R . . C26 C 0.6202(10) 0.7710(7) 0.5292(8) 0.042(3) Uani 1 1 d . . . C27 C 0.5068(11) 0.7643(8) 0.5143(7) 0.046(3) Uani 1 1 d . . . H27 H 0.4611 0.7483 0.5540 0.055 Uiso 1 1 calc R . . C28 C 0.4591(9) 0.7806(7) 0.4426(6) 0.036(3) Uani 1 1 d . . . H28 H 0.3808 0.7745 0.4339 0.043 Uiso 1 1 calc R . . C29 C -0.0089(9) 0.1330(8) 0.0989(7) 0.041(3) Uani 1 1 d . . . C30 C -0.0340(10) 0.1891(7) 0.0507(7) 0.043(3) Uani 1 1 d . . . C31 C 0.0460(9) 0.2102(7) -0.0024(7) 0.038(3) Uani 1 1 d . . . C32 C 0.1249(11) 0.1637(7) 0.0140(7) 0.048(3) Uani 1 1 d . . . C33 C 0.0897(9) 0.1160(7) 0.0758(6) 0.036(3) Uani 1 1 d . . . C34 C -0.0764(10) 0.0934(8) 0.1599(8) 0.055(3) Uani 1 1 d . . . H34A H -0.1028 0.1383 0.1902 0.082 Uiso 1 1 calc R . . H34B H -0.0272 0.0778 0.1996 0.082 Uiso 1 1 calc R . . H34C H -0.1431 0.0384 0.1295 0.082 Uiso 1 1 calc R . . C35 C -0.1301(10) 0.2248(8) 0.0592(7) 0.051(3) Uani 1 1 d . . . H35A H -0.1082 0.2846 0.0469 0.076 Uiso 1 1 calc R . . H35B H -0.1430 0.2306 0.1163 0.076 Uiso 1 1 calc R . . H35C H -0.2010 0.1822 0.0198 0.076 Uiso 1 1 calc R . . C36 C 0.0519(11) 0.2651(8) -0.0614(7) 0.050(3) Uani 1 1 d . . . H36A H 0.0433 0.2278 -0.1175 0.074 Uiso 1 1 calc R . . H36B H 0.1264 0.3163 -0.0459 0.074 Uiso 1 1 calc R . . H36C H -0.0101 0.2883 -0.0610 0.074 Uiso 1 1 calc R . . C37 C 0.2217(11) 0.1705(8) -0.0256(8) 0.052(3) Uani 1 1 d . . . H37A H 0.2822 0.2312 -0.0026 0.078 Uiso 1 1 calc R . . H37B H 0.1967 0.1604 -0.0858 0.078 Uiso 1 1 calc R . . H37C H 0.2516 0.1243 -0.0151 0.078 Uiso 1 1 calc R . . C38 C 0.1373(11) 0.0538(8) 0.1053(9) 0.064(4) Uani 1 1 d . . . H38A H 0.0862 -0.0093 0.0776 0.096 Uiso 1 1 calc R . . H38B H 0.1441 0.0640 0.1658 0.096 Uiso 1 1 calc R . . H38C H 0.2135 0.0652 0.0922 0.096 Uiso 1 1 calc R . . C39 C 0.3775(10) 0.9075(7) 0.2137(7) 0.039(3) Uani 1 1 d . . . C40 C 0.4291(11) 0.9576(7) 0.2988(8) 0.046(3) Uani 1 1 d . . . C41 C 0.5446(12) 0.9774(8) 0.3131(8) 0.052(3) Uani 1 1 d . . . C42 C 0.5752(11) 0.9399(8) 0.2365(9) 0.057(4) Uani 1 1 d . . . C43 C 0.4684(10) 0.8965(8) 0.1748(7) 0.041(3) Uani 1 1 d . . . C44 C 0.2531(11) 0.8753(10) 0.1718(7) 0.061(4) Uani 1 1 d . . . H44A H 0.2093 0.8187 0.1853 0.092 Uiso 1 1 calc R . . H44B H 0.2462 0.8643 0.1112 0.092 Uiso 1 1 calc R . . H44C H 0.2227 0.9219 0.1915 0.092 Uiso 1 1 calc R . . C45 C 0.3590(14) 0.9840(9) 0.3625(9) 0.077(5) Uani 1 1 d . . . H45A H 0.3962 0.9875 0.4188 0.116 Uiso 1 1 calc R . . H45B H 0.2806 0.9378 0.3482 0.116 Uiso 1 1 calc R . . H45C H 0.3560 1.0433 0.3604 0.116 Uiso 1 1 calc R . . C46 C 0.6309(12) 1.0292(9) 0.3909(9) 0.076(5) Uani 1 1 d . . . H46A H 0.6497 1.0945 0.3973 0.114 Uiso 1 1 calc R . . H46B H 0.7007 1.0161 0.3885 0.114 Uiso 1 1 calc R . . H46C H 0.5998 1.0115 0.4385 0.114 Uiso 1 1 calc R . . C47 C 0.6883(11) 0.9470(12) 0.2251(11) 0.099(6) Uani 1 1 d . . . H47A H 0.7442 0.9810 0.2776 0.148 Uiso 1 1 calc R . . H47B H 0.7082 0.9789 0.1816 0.148 Uiso 1 1 calc R . . H47C H 0.6894 0.8858 0.2082 0.148 Uiso 1 1 calc R . . C48 C 0.4511(13) 0.8473(10) 0.0860(8) 0.071(4) Uani 1 1 d . . . H48A H 0.3788 0.7938 0.0705 0.107 Uiso 1 1 calc R . . H48B H 0.5152 0.8278 0.0789 0.107 Uiso 1 1 calc R . . H48C H 0.4477 0.8880 0.0501 0.107 Uiso 1 1 calc R . . C49 C 0.0365(17) 0.9933(12) 0.3671(13) 0.091(5) Uani 1 1 d . . . C50 C 0.6354(18) 0.2647(11) 0.1845(15) 0.110(8) Uani 1 1 d . . . C51 C 0.066(2) 0.774(2) 0.515(3) 0.26(2) Uani 1 1 d . . . O11 O -0.0628(19) 0.7542(12) 0.4669(10) 0.180(8) Uani 1 1 d . . . C52 C 0.612(4) 0.523(3) 0.380(3) 0.37(3) Uani 1 1 d . . . H52A H 0.6448 0.5801 0.3633 0.554 Uiso 1 1 calc R . . H52B H 0.6008 0.4715 0.3336 0.554 Uiso 1 1 calc R . . H52C H 0.6641 0.5235 0.4285 0.554 Uiso 1 1 calc R . . O12 O 0.497(3) 0.5153(17) 0.402(3) 0.38(2) Uani 1 1 d . . . O13 O 0.1144(13) 0.5441(8) 0.0085(7) 0.128(5) Uani 1 1 d . . . O14 O 0.6744(8) 0.0105(7) 0.9979(6) 0.078(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0353(6) 0.0226(5) 0.0472(6) 0.0095(4) 0.0273(5) 0.0076(4) Rh2 0.0359(6) 0.0229(5) 0.0396(5) 0.0110(4) 0.0195(4) 0.0035(4) N1 0.037(5) 0.027(5) 0.038(5) 0.006(4) 0.023(4) 0.010(4) N2 0.047(6) 0.029(5) 0.036(5) 0.018(4) 0.025(5) 0.013(4) O1 0.054(5) 0.013(4) 0.071(5) 0.013(4) 0.043(4) 0.013(4) O2 0.025(4) 0.024(4) 0.072(5) 0.010(4) 0.028(4) -0.001(3) O3 0.036(4) 0.019(4) 0.039(4) 0.001(3) 0.015(3) 0.003(3) O4 0.034(4) 0.028(4) 0.055(5) 0.014(4) 0.023(4) 0.004(4) O5 0.131(10) 0.069(7) 0.142(10) 0.056(7) 0.087(8) 0.069(7) O6 0.091(8) 0.106(10) 0.150(11) 0.047(8) 0.085(8) 0.024(7) O7 0.178(13) 0.131(11) 0.054(7) 0.012(7) 0.036(7) 0.087(10) O8 0.204(15) 0.098(10) 0.194(14) 0.087(9) 0.162(12) 0.100(10) O9 0.058(9) 0.29(2) 0.187(15) -0.140(15) -0.026(10) 0.064(12) O10 0.128(10) 0.052(6) 0.200(12) 0.042(7) 0.139(10) 0.046(7) F1 0.139(10) 0.095(8) 0.201(12) 0.002(8) 0.040(9) 0.078(8) F2 0.122(10) 0.137(11) 0.088(8) 0.002(7) -0.011(7) 0.036(8) F3 0.130(10) 0.110(9) 0.236(14) 0.098(10) 0.066(10) 0.039(8) F4 0.120(7) 0.041(5) 0.129(7) 0.020(5) 0.070(6) 0.037(5) F5 0.082(9) 0.161(13) 0.271(18) 0.006(12) 0.091(10) -0.002(8) F6 0.274(16) 0.093(8) 0.136(9) 0.073(7) 0.141(11) 0.100(10) S1 0.071(3) 0.062(2) 0.073(3) 0.022(2) 0.043(2) 0.036(2) S2 0.087(3) 0.0327(19) 0.088(3) 0.0138(18) 0.052(2) 0.0160(19) C1 0.035(7) 0.041(7) 0.043(7) 0.020(6) 0.027(6) 0.015(6) C2 0.031(6) 0.023(6) 0.044(6) 0.011(5) 0.027(5) 0.008(5) C3 0.034(6) 0.026(6) 0.050(7) 0.017(5) 0.023(6) 0.015(5) C4 0.031(6) 0.030(6) 0.065(8) 0.005(6) 0.031(6) 0.009(5) C5 0.031(7) 0.025(7) 0.135(13) 0.006(7) 0.042(8) 0.000(5) C6 0.035(8) 0.048(9) 0.171(16) 0.002(10) 0.062(9) 0.008(7) C7 0.039(8) 0.042(8) 0.199(19) 0.002(10) 0.061(11) 0.012(7) C8 0.041(7) 0.037(7) 0.084(9) -0.001(6) 0.042(7) 0.019(6) C9 0.029(6) 0.023(6) 0.065(8) 0.012(5) 0.025(6) 0.008(5) C10 0.032(6) 0.021(6) 0.041(6) 0.016(5) 0.024(5) 0.011(5) C11 0.028(6) 0.028(6) 0.039(6) 0.015(5) 0.016(5) 0.007(5) C12 0.025(6) 0.022(6) 0.044(6) 0.018(5) 0.020(5) 0.005(5) C13 0.040(7) 0.046(8) 0.087(10) 0.026(7) 0.047(7) 0.012(6) C14 0.066(10) 0.052(9) 0.117(13) 0.034(9) 0.062(9) 0.019(8) C15 0.068(11) 0.050(10) 0.27(3) 0.065(14) 0.109(14) 0.016(9) C16 0.079(12) 0.076(12) 0.22(2) 0.056(14) 0.108(14) 0.039(10) C17 0.068(10) 0.047(9) 0.159(16) 0.041(10) 0.081(11) 0.024(8) C18 0.039(7) 0.038(7) 0.066(8) 0.033(6) 0.037(6) 0.023(6) C19 0.047(8) 0.060(8) 0.041(7) 0.008(6) 0.025(6) 0.023(7) C20 0.034(7) 0.048(7) 0.056(8) 0.010(6) 0.028(6) 0.021(6) C21 0.037(7) 0.034(6) 0.035(6) 0.011(5) 0.011(5) 0.009(5) C22 0.045(7) 0.047(7) 0.041(7) 0.003(6) 0.027(6) 0.015(6) C23 0.034(7) 0.051(8) 0.059(8) 0.007(6) 0.028(6) 0.020(6) C24 0.029(6) 0.037(7) 0.052(7) 0.015(6) 0.022(6) 0.007(5) C25 0.034(7) 0.045(7) 0.042(7) 0.016(6) 0.020(6) 0.015(6) C26 0.050(8) 0.022(6) 0.060(8) 0.011(5) 0.023(6) 0.016(5) C27 0.057(8) 0.055(8) 0.037(7) 0.018(6) 0.031(6) 0.025(7) C28 0.024(6) 0.051(7) 0.042(7) 0.016(6) 0.020(5) 0.019(5) C29 0.035(7) 0.037(7) 0.037(7) 0.003(5) 0.011(6) 0.001(5) C30 0.050(8) 0.029(6) 0.049(7) 0.014(5) 0.031(6) 0.004(6) C31 0.038(7) 0.034(6) 0.038(6) 0.004(5) 0.021(5) 0.005(5) C32 0.075(9) 0.028(6) 0.049(7) 0.012(5) 0.049(7) 0.017(6) C33 0.035(7) 0.030(6) 0.034(6) 0.005(5) -0.001(5) 0.006(5) C34 0.041(7) 0.041(8) 0.070(9) 0.021(7) 0.026(7) -0.007(6) C35 0.038(7) 0.055(8) 0.052(8) 0.013(6) 0.018(6) 0.006(6) C36 0.059(8) 0.040(7) 0.059(8) 0.021(6) 0.033(7) 0.019(6) C37 0.067(9) 0.030(7) 0.078(9) 0.024(6) 0.051(7) 0.023(6) C38 0.063(9) 0.041(8) 0.091(10) 0.016(7) 0.045(8) 0.015(7) C39 0.048(7) 0.023(6) 0.054(7) 0.017(5) 0.032(6) 0.011(5) C40 0.064(9) 0.009(5) 0.064(8) 0.013(5) 0.016(7) 0.011(6) C41 0.062(9) 0.025(7) 0.048(8) 0.013(6) 0.005(7) -0.009(6) C42 0.055(9) 0.030(7) 0.102(11) 0.043(7) 0.042(8) 0.014(6) C43 0.043(7) 0.038(7) 0.042(7) 0.021(6) 0.012(6) 0.010(6) C44 0.053(9) 0.088(11) 0.049(8) 0.023(7) 0.030(7) 0.025(8) C45 0.129(14) 0.043(8) 0.080(10) 0.012(7) 0.069(10) 0.042(9) C46 0.073(10) 0.033(8) 0.089(11) 0.006(8) 0.001(9) -0.009(7) C47 0.045(9) 0.125(15) 0.171(17) 0.118(14) 0.058(10) 0.032(9) C48 0.081(11) 0.093(12) 0.054(9) 0.023(8) 0.039(8) 0.040(10) C49 0.091(14) 0.077(13) 0.110(15) 0.010(12) 0.038(13) 0.038(11) C50 0.123(16) 0.047(10) 0.19(2) 0.033(12) 0.135(16) 0.029(10) C51 0.10(2) 0.22(4) 0.41(5) -0.06(3) 0.01(3) 0.09(2) O11 0.28(2) 0.173(16) 0.144(13) 0.064(12) 0.152(15) 0.097(17) C52 0.51(8) 0.36(6) 0.29(5) -0.08(4) 0.12(5) 0.30(7) O12 0.29(3) 0.15(2) 0.69(7) 0.02(3) 0.20(4) 0.08(2) O13 0.249(16) 0.098(10) 0.089(8) 0.067(7) 0.064(9) 0.094(11) O14 0.076(7) 0.087(8) 0.086(7) 0.013(6) 0.049(6) 0.043(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.040(7) . ? Rh1 O1 2.061(7) . ? Rh1 N1 2.119(9) . ? Rh1 C29 2.121(11) . ? Rh1 C30 2.127(12) . ? Rh1 C33 2.134(11) . ? Rh1 C32 2.143(10) . ? Rh1 C31 2.156(11) . ? Rh2 O3 2.060(7) . ? Rh2 O4 2.077(7) . ? Rh2 N2 2.103(8) . ? Rh2 C39 2.119(11) . ? Rh2 C40 2.127(10) . ? Rh2 C43 2.128(11) . ? Rh2 C41 2.153(11) . ? Rh2 C42 2.161(12) . ? N1 C23 1.337(13) . ? N1 C19 1.341(13) . ? N2 C24 1.344(13) . ? N2 C28 1.369(13) . ? O1 C1 1.236(12) . ? O2 C3 1.271(12) . ? O3 C10 1.258(11) . ? O4 C12 1.253(11) . ? O5 S1 1.407(10) . ? O6 S1 1.430(11) . ? O7 S1 1.387(11) . ? O8 S2 1.435(14) . ? O9 S2 1.448(13) . ? O10 S2 1.394(9) . ? F1 C49 1.365(18) . ? F2 C49 1.29(2) . ? F3 C49 1.37(2) . ? F4 C50 1.322(15) . ? F5 C50 1.39(3) . ? F6 C50 1.26(2) . ? S1 C49 1.781(19) . ? S2 C50 1.750(16) . ? C1 C2 1.438(13) . ? C1 C18 1.470(14) . ? C2 C3 1.438(14) . ? C2 C11 1.464(13) . ? C3 C4 1.446(13) . ? C4 C9 1.396(14) . ? C4 C5 1.422(15) . ? C5 C6 1.350(16) . ? C6 C7 1.433(18) . ? C7 C8 1.373(16) . ? C8 C9 1.388(14) . ? C9 C10 1.471(14) . ? C10 C11 1.436(13) . ? C11 C12 1.437(13) . ? C12 C13 1.484(15) . ? C13 C18 1.389(16) . ? C13 C14 1.411(16) . ? C14 C15 1.372(19) . ? C15 C16 1.43(2) . ? C16 C17 1.355(19) . ? C17 C18 1.408(16) . ? C19 C20 1.353(15) . ? C20 C21 1.396(15) . ? C21 C22 1.377(15) . ? C21 C26 1.455(15) 2_666 ? C22 C23 1.389(16) . ? C24 C25 1.403(15) . ? C25 C26 1.368(15) . ? C26 C27 1.388(15) . ? C26 C21 1.455(15) 2_666 ? C27 C28 1.385(15) . ? C29 C30 1.411(15) . ? C29 C33 1.450(15) . ? C29 C34 1.510(15) . ? C30 C31 1.429(14) . ? C30 C35 1.526(15) . ? C31 C36 1.442(15) . ? C31 C32 1.472(16) . ? C32 C33 1.433(15) . ? C32 C37 1.447(15) . ? C33 C38 1.467(16) . ? C39 C40 1.433(16) . ? C39 C43 1.438(15) . ? C39 C44 1.501(16) . ? C40 C41 1.363(17) . ? C40 C45 1.558(17) . ? C41 C42 1.464(18) . ? C41 C46 1.473(17) . ? C42 C47 1.436(17) . ? C42 C43 1.447(17) . ? C43 C48 1.490(16) . ? C51 O11 1.62(3) . ? C52 O12 1.52(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rh1 O1 85.4(3) . . ? O2 Rh1 N1 85.9(3) . . ? O1 Rh1 N1 85.2(3) . . ? O2 Rh1 C29 111.7(4) . . ? O1 Rh1 C29 161.5(4) . . ? N1 Rh1 C29 102.5(4) . . ? O2 Rh1 C30 94.3(4) . . ? O1 Rh1 C30 137.0(4) . . ? N1 Rh1 C30 137.7(4) . . ? C29 Rh1 C30 38.8(4) . . ? O2 Rh1 C33 151.2(4) . . ? O1 Rh1 C33 123.5(4) . . ? N1 Rh1 C33 95.5(4) . . ? C29 Rh1 C33 39.8(4) . . ? C30 Rh1 C33 65.6(4) . . ? O2 Rh1 C32 151.1(4) . . ? O1 Rh1 C32 95.3(4) . . ? N1 Rh1 C32 123.0(4) . . ? C29 Rh1 C32 66.3(4) . . ? C30 Rh1 C32 65.8(5) . . ? C33 Rh1 C32 39.1(4) . . ? O2 Rh1 C31 111.5(4) . . ? O1 Rh1 C31 101.8(4) . . ? N1 Rh1 C31 161.5(4) . . ? C29 Rh1 C31 66.1(4) . . ? C30 Rh1 C31 39.0(4) . . ? C33 Rh1 C31 66.3(4) . . ? C32 Rh1 C31 40.0(4) . . ? O3 Rh2 O4 84.7(3) . . ? O3 Rh2 N2 86.5(3) . . ? O4 Rh2 N2 82.7(3) . . ? O3 Rh2 C39 95.3(4) . . ? O4 Rh2 C39 126.2(4) . . ? N2 Rh2 C39 151.0(4) . . ? O3 Rh2 C40 106.6(4) . . ? O4 Rh2 C40 161.2(4) . . ? N2 Rh2 C40 112.5(4) . . ? C39 Rh2 C40 39.4(4) . . ? O3 Rh2 C43 120.5(4) . . ? O4 Rh2 C43 95.7(4) . . ? N2 Rh2 C43 152.8(4) . . ? C39 Rh2 C43 39.6(4) . . ? C40 Rh2 C43 65.6(5) . . ? O3 Rh2 C41 141.2(4) . . ? O4 Rh2 C41 134.2(5) . . ? N2 Rh2 C41 96.2(4) . . ? C39 Rh2 C41 64.8(5) . . ? C40 Rh2 C41 37.1(5) . . ? C43 Rh2 C41 65.5(4) . . ? O3 Rh2 C42 159.6(4) . . ? O4 Rh2 C42 99.1(4) . . ? N2 Rh2 C42 113.8(5) . . ? C39 Rh2 C42 66.2(5) . . ? C40 Rh2 C42 65.1(5) . . ? C43 Rh2 C42 39.4(5) . . ? C41 Rh2 C42 39.7(5) . . ? C23 N1 C19 116.3(10) . . ? C23 N1 Rh1 123.4(8) . . ? C19 N1 Rh1 119.9(7) . . ? C24 N2 C28 116.5(9) . . ? C24 N2 Rh2 119.9(7) . . ? C28 N2 Rh2 123.5(7) . . ? C1 O1 Rh1 131.1(7) . . ? C3 O2 Rh1 129.5(7) . . ? C10 O3 Rh2 130.8(6) . . ? C12 O4 Rh2 130.2(7) . . ? O7 S1 O5 114.9(7) . . ? O7 S1 O6 114.4(9) . . ? O5 S1 O6 113.6(7) . . ? O7 S1 C49 105.6(9) . . ? O5 S1 C49 103.6(8) . . ? O6 S1 C49 103.0(9) . . ? O10 S2 O8 121.1(8) . . ? O10 S2 O9 110.1(8) . . ? O8 S2 O9 114.7(9) . . ? O10 S2 C50 107.8(7) . . ? O8 S2 C50 104.5(9) . . ? O9 S2 C50 94.7(13) . . ? O1 C1 C2 126.9(10) . . ? O1 C1 C18 114.9(9) . . ? C2 C1 C18 118.2(10) . . ? C1 C2 C3 119.2(9) . . ? C1 C2 C11 120.1(9) . . ? C3 C2 C11 120.6(8) . . ? O2 C3 C2 127.2(9) . . ? O2 C3 C4 114.9(9) . . ? C2 C3 C4 117.9(9) . . ? C9 C4 C5 118.1(10) . . ? C9 C4 C3 122.3(10) . . ? C5 C4 C3 119.6(10) . . ? C6 C5 C4 122.1(11) . . ? C5 C6 C7 119.0(12) . . ? C8 C7 C6 119.2(11) . . ? C7 C8 C9 121.5(11) . . ? C8 C9 C4 119.9(10) . . ? C8 C9 C10 119.7(10) . . ? C4 C9 C10 120.3(9) . . ? O3 C10 C11 127.4(9) . . ? O3 C10 C9 114.1(8) . . ? C11 C10 C9 118.5(9) . . ? C10 C11 C12 119.1(9) . . ? C10 C11 C2 119.9(9) . . ? C12 C11 C2 120.9(9) . . ? O4 C12 C11 127.5(9) . . ? O4 C12 C13 114.2(9) . . ? C11 C12 C13 118.1(9) . . ? C18 C13 C14 121.6(11) . . ? C18 C13 C12 120.4(10) . . ? C14 C13 C12 117.9(11) . . ? C15 C14 C13 119.5(13) . . ? C14 C15 C16 117.4(13) . . ? C17 C16 C15 124.0(14) . . ? C16 C17 C18 117.9(14) . . ? C13 C18 C17 119.2(11) . . ? C13 C18 C1 122.1(10) . . ? C17 C18 C1 118.6(11) . . ? N1 C19 C20 123.7(10) . . ? C19 C20 C21 120.3(10) . . ? C22 C21 C20 116.7(10) . . ? C22 C21 C26 121.0(10) . 2_666 ? C20 C21 C26 122.3(10) . 2_666 ? C21 C22 C23 119.4(10) . . ? N1 C23 C22 123.4(10) . . ? N2 C24 C25 123.0(10) . . ? C26 C25 C24 120.5(11) . . ? C25 C26 C27 116.7(11) . . ? C25 C26 C21 121.9(11) . 2_666 ? C27 C26 C21 121.3(11) . 2_666 ? C28 C27 C26 121.2(11) . . ? N2 C28 C27 122.0(10) . . ? C30 C29 C33 107.6(10) . . ? C30 C29 C34 126.3(11) . . ? C33 C29 C34 126.0(11) . . ? C30 C29 Rh1 70.8(7) . . ? C33 C29 Rh1 70.6(6) . . ? C34 C29 Rh1 126.6(8) . . ? C29 C30 C31 110.4(10) . . ? C29 C30 C35 123.4(10) . . ? C31 C30 C35 126.1(11) . . ? C29 C30 Rh1 70.4(7) . . ? C31 C30 Rh1 71.6(7) . . ? C35 C30 Rh1 122.4(8) . . ? C30 C31 C36 128.8(11) . . ? C30 C31 C32 106.2(10) . . ? C36 C31 C32 125.0(10) . . ? C30 C31 Rh1 69.4(6) . . ? C36 C31 Rh1 125.9(8) . . ? C32 C31 Rh1 69.5(6) . . ? C33 C32 C37 128.6(11) . . ? C33 C32 C31 107.8(9) . . ? C37 C32 C31 123.6(10) . . ? C33 C32 Rh1 70.1(6) . . ? C37 C32 Rh1 123.4(9) . . ? C31 C32 Rh1 70.4(6) . . ? C32 C33 C29 108.0(10) . . ? C32 C33 C38 126.4(11) . . ? C29 C33 C38 125.4(11) . . ? C32 C33 Rh1 70.8(6) . . ? C29 C33 Rh1 69.6(6) . . ? C38 C33 Rh1 129.5(8) . . ? C40 C39 C43 106.9(10) . . ? C40 C39 C44 126.9(10) . . ? C43 C39 C44 126.1(11) . . ? C40 C39 Rh2 70.6(6) . . ? C43 C39 Rh2 70.6(6) . . ? C44 C39 Rh2 125.5(8) . . ? C41 C40 C39 109.9(11) . . ? C41 C40 C45 127.1(12) . . ? C39 C40 C45 123.0(12) . . ? C41 C40 Rh2 72.4(7) . . ? C39 C40 Rh2 70.0(6) . . ? C45 C40 Rh2 124.2(8) . . ? C40 C41 C42 109.4(11) . . ? C40 C41 C46 128.1(13) . . ? C42 C41 C46 122.4(14) . . ? C40 C41 Rh2 70.4(6) . . ? C42 C41 Rh2 70.5(6) . . ? C46 C41 Rh2 126.2(9) . . ? C47 C42 C43 127.6(14) . . ? C47 C42 C41 126.8(14) . . ? C43 C42 C41 105.5(11) . . ? C47 C42 Rh2 126.5(9) . . ? C43 C42 Rh2 69.1(6) . . ? C41 C42 Rh2 69.8(7) . . ? C39 C43 C42 108.3(10) . . ? C39 C43 C48 124.1(11) . . ? C42 C43 C48 127.6(12) . . ? C39 C43 Rh2 69.9(6) . . ? C42 C43 Rh2 71.5(6) . . ? C48 C43 Rh2 123.9(9) . . ? F2 C49 F1 114.3(16) . . ? F2 C49 F3 104.3(17) . . ? F1 C49 F3 101.1(16) . . ? F2 C49 S1 116.4(15) . . ? F1 C49 S1 109.6(13) . . ? F3 C49 S1 109.7(13) . . ? F6 C50 F4 112.4(17) . . ? F6 C50 F5 101.1(14) . . ? F4 C50 F5 103.2(17) . . ? F6 C50 S2 117.2(15) . . ? F4 C50 S2 114.3(10) . . ? F5 C50 S2 106.5(16) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.318 _refine_diff_density_min -2.298 _refine_diff_density_rms 0.179 # Attachment 'Complex 5b.cif' data_complex_5b _database_code_depnum_ccdc_archive 'CCDC 749421' #TrackingRef 'Complex 5b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H96 F12 N4 O20 Rh4 S4' _chemical_formula_weight 2489.73 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.643(9) _cell_length_b 16.438(9) _cell_length_c 22.817(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.573(7) _cell_angle_gamma 90.00 _cell_volume 5951(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 901 _cell_measurement_theta_min 2.246 _cell_measurement_theta_max 24.706 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9212 _exptl_absorpt_correction_T_max 0.9337 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.69 _diffrn_reflns_number 27964 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.19 _reflns_number_total 12751 _reflns_number_gt 7178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12751 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.58683(2) 0.44389(2) 0.774205(18) 0.03883(13) Uani 1 1 d . . . Rh2 Rh 0.87737(2) 0.80910(2) 0.682297(18) 0.03519(12) Uani 1 1 d . . . N1 N 0.6710(3) 0.4081(3) 0.85905(19) 0.0435(10) Uani 1 1 d . . . N2 N 0.9536(2) 0.7756(2) 0.77234(19) 0.0368(9) Uani 1 1 d . . . O1 O 0.6913(2) 0.44729(19) 0.74448(16) 0.0410(8) Uani 1 1 d . . . O2 O 0.6227(2) 0.5607(2) 0.80383(16) 0.0415(8) Uani 1 1 d . . . O3 O 0.7818(2) 0.80142(18) 0.72248(15) 0.0369(8) Uani 1 1 d . . . O4 O 0.8593(2) 0.6862(2) 0.66737(16) 0.0425(8) Uani 1 1 d . . . O5 O 0.7821(7) 0.1369(6) 0.8491(5) 0.228(5) Uani 1 1 d . . . O6 O 0.9142(7) 0.1235(5) 0.8323(4) 0.207(5) Uani 1 1 d . . . O7 O 0.8176(5) 0.0130(3) 0.8118(3) 0.129(2) Uani 1 1 d . . . F1 F 0.8393(6) 0.0081(6) 0.9424(3) 0.223(4) Uani 1 1 d . . . F2 F 0.9163(5) 0.1077(4) 0.9614(3) 0.160(3) Uani 1 1 d . . . F3 F 0.9516(5) 0.0000(6) 0.9225(4) 0.217(4) Uani 1 1 d . . . S1 S 0.84220(19) 0.08265(14) 0.84512(12) 0.1080(8) Uani 1 1 d . . . C1 C 0.7252(3) 0.5100(3) 0.7282(2) 0.0333(11) Uani 1 1 d . . . C2 C 0.7186(3) 0.5906(3) 0.7472(2) 0.0292(10) Uani 1 1 d . . . C3 C 0.6718(3) 0.6095(3) 0.7880(2) 0.0336(11) Uani 1 1 d . . . C4 C 0.6794(3) 0.6898(3) 0.8156(2) 0.0334(10) Uani 1 1 d . . . C5 C 0.6508(3) 0.7038(3) 0.8659(2) 0.0429(12) Uani 1 1 d . . . H5 H 0.6250 0.6620 0.8810 0.051 Uiso 1 1 calc R . . C6 C 0.6603(3) 0.7785(3) 0.8934(3) 0.0501(14) Uani 1 1 d . . . H6 H 0.6426 0.7868 0.9279 0.060 Uiso 1 1 calc R . . C7 C 0.6968(3) 0.8428(3) 0.8699(3) 0.0464(13) Uani 1 1 d . . . H7 H 0.7022 0.8940 0.8880 0.056 Uiso 1 1 calc R . . C8 C 0.7243(3) 0.8292(3) 0.8199(2) 0.0397(12) Uani 1 1 d . . . H8 H 0.7479 0.8719 0.8040 0.048 Uiso 1 1 calc R . . C9 C 0.7177(3) 0.7530(3) 0.7924(2) 0.0351(11) Uani 1 1 d . . . C10 C 0.7557(3) 0.7378(3) 0.7436(2) 0.0303(10) Uani 1 1 d . . . C11 C 0.7646(3) 0.6562(3) 0.7259(2) 0.0297(10) Uani 1 1 d . . . C12 C 0.8142(3) 0.6373(3) 0.6872(2) 0.0327(11) Uani 1 1 d . . . C13 C 0.8169(3) 0.5526(3) 0.6664(2) 0.0362(11) Uani 1 1 d . . . C14 C 0.8625(3) 0.5341(3) 0.6262(3) 0.0458(13) Uani 1 1 d . . . H14 H 0.8921 0.5749 0.6133 0.055 Uiso 1 1 calc R . . C15 C 0.8642(4) 0.4563(3) 0.6055(3) 0.0597(16) Uani 1 1 d . . . H15 H 0.8934 0.4441 0.5778 0.072 Uiso 1 1 calc R . . C16 C 0.8216(4) 0.3958(3) 0.6265(3) 0.0560(15) Uani 1 1 d . . . H16 H 0.8224 0.3427 0.6125 0.067 Uiso 1 1 calc R . . C17 C 0.7791(3) 0.4125(3) 0.6668(3) 0.0459(13) Uani 1 1 d . . . H17 H 0.7522 0.3708 0.6812 0.055 Uiso 1 1 calc R . . C18 C 0.7751(3) 0.4917(3) 0.6871(2) 0.0339(11) Uani 1 1 d . . . C19 C 0.6669(4) 0.4427(4) 0.9114(3) 0.0549(15) Uani 1 1 d . . . H19 H 0.6272 0.4832 0.9096 0.066 Uiso 1 1 calc R . . C20 C 0.7200(4) 0.4197(4) 0.9674(3) 0.0580(16) Uani 1 1 d . . . H20 H 0.7156 0.4449 1.0028 0.070 Uiso 1 1 calc R . . C21 C 0.7788(3) 0.3607(3) 0.9723(2) 0.0452(13) Uani 1 1 d . . . C22 C 0.7808(3) 0.3247(3) 0.9179(3) 0.0488(13) Uani 1 1 d . . . H22 H 0.8184 0.2824 0.9191 0.059 Uiso 1 1 calc R . . C23 C 0.7283(3) 0.3504(3) 0.8621(3) 0.0477(13) Uani 1 1 d . . . H23 H 0.7328 0.3272 0.8260 0.057 Uiso 1 1 calc R . . C24 C 0.8336(4) 0.3359(4) 1.0333(3) 0.0564(15) Uani 1 1 d . . . H24 H 0.8206 0.3586 1.0667 0.068 Uiso 1 1 calc R . . C25 C 0.8952(4) 0.2886(4) 1.0463(3) 0.0531(15) Uani 1 1 d . . . H25 H 0.9081 0.2633 1.0138 0.064 Uiso 1 1 calc R . . C26 C 0.9456(3) 0.8126(3) 0.8224(2) 0.0429(12) Uani 1 1 d . . . H26 H 0.9059 0.8540 0.8169 0.051 Uiso 1 1 calc R . . C27 C 0.9922(3) 0.7937(4) 0.8814(3) 0.0503(14) Uani 1 1 d . . . H27 H 0.9849 0.8224 0.9145 0.060 Uiso 1 1 calc R . . C28 C 1.0506(3) 0.7307(3) 0.8910(3) 0.0481(14) Uani 1 1 d . . . C29 C 1.0581(3) 0.6918(3) 0.8397(3) 0.0505(14) Uani 1 1 d . . . H29 H 1.0963 0.6493 0.8439 0.061 Uiso 1 1 calc R . . C30 C 1.0087(3) 0.7158(3) 0.7812(3) 0.0472(13) Uani 1 1 d . . . H30 H 1.0149 0.6885 0.7472 0.057 Uiso 1 1 calc R . . C31 C 0.5107(4) 0.3897(5) 0.6921(3) 0.0628(18) Uani 1 1 d . . . C32 C 0.5125(4) 0.3398(3) 0.7470(4) 0.080(3) Uani 1 1 d . . . C33 C 0.4739(4) 0.3897(5) 0.7814(3) 0.069(2) Uani 1 1 d . . . C34 C 0.4525(4) 0.4606(5) 0.7544(4) 0.077(2) Uani 1 1 d . . . C35 C 0.4733(4) 0.4619(4) 0.7021(3) 0.0654(19) Uani 1 1 d . . . C36 C 0.5419(6) 0.3705(11) 0.6417(5) 0.223(9) Uani 1 1 d . . . H36A H 0.4954 0.3622 0.6052 0.334 Uiso 1 1 calc R . . H36B H 0.5753 0.3219 0.6509 0.334 Uiso 1 1 calc R . . H36C H 0.5760 0.4146 0.6351 0.334 Uiso 1 1 calc R . . C37 C 0.5412(6) 0.2546(5) 0.7622(8) 0.250(10) Uani 1 1 d . . . H37A H 0.5457 0.2436 0.8044 0.375 Uiso 1 1 calc R . . H37B H 0.5953 0.2473 0.7560 0.375 Uiso 1 1 calc R . . H37C H 0.5013 0.2179 0.7361 0.375 Uiso 1 1 calc R . . C38 C 0.4580(6) 0.3649(9) 0.8394(4) 0.194(7) Uani 1 1 d . . . H38A H 0.4764 0.4073 0.8694 0.292 Uiso 1 1 calc R . . H38B H 0.4887 0.3158 0.8545 0.292 Uiso 1 1 calc R . . H38C H 0.3989 0.3554 0.8319 0.292 Uiso 1 1 calc R . . C39 C 0.4125(6) 0.5318(7) 0.7781(7) 0.183(7) Uani 1 1 d . . . H39A H 0.4500 0.5777 0.7854 0.275 Uiso 1 1 calc R . . H39B H 0.4021 0.5166 0.8158 0.275 Uiso 1 1 calc R . . H39C H 0.3603 0.5461 0.7481 0.275 Uiso 1 1 calc R . . C40 C 0.4567(6) 0.5352(7) 0.6570(6) 0.189(7) Uani 1 1 d . . . H40A H 0.3983 0.5360 0.6332 0.284 Uiso 1 1 calc R . . H40B H 0.4909 0.5300 0.6301 0.284 Uiso 1 1 calc R . . H40C H 0.4706 0.5849 0.6800 0.284 Uiso 1 1 calc R . . C41 C 0.8455(3) 0.9259(3) 0.6420(2) 0.0418(12) Uani 1 1 d . . . C42 C 0.9315(3) 0.9253(3) 0.6767(2) 0.0404(12) Uani 1 1 d . . . C43 C 0.9729(3) 0.8640(3) 0.6509(3) 0.0471(13) Uani 1 1 d . . . C44 C 0.9118(4) 0.8286(3) 0.6004(3) 0.0509(14) Uani 1 1 d . . . C45 C 0.8327(4) 0.8660(3) 0.5951(2) 0.0502(14) Uani 1 1 d . . . C46 C 0.7789(4) 0.9784(4) 0.6539(3) 0.0595(16) Uani 1 1 d . . . H46A H 0.7914 0.9874 0.6973 0.089 Uiso 1 1 calc R . . H46B H 0.7252 0.9520 0.6386 0.089 Uiso 1 1 calc R . . H46C H 0.7772 1.0297 0.6334 0.089 Uiso 1 1 calc R . . C47 C 0.9744(4) 0.9798(3) 0.7291(3) 0.0589(16) Uani 1 1 d . . . H47A H 1.0009 1.0240 0.7145 0.088 Uiso 1 1 calc R . . H47B H 1.0164 0.9495 0.7594 0.088 Uiso 1 1 calc R . . H47C H 0.9337 1.0010 0.7472 0.088 Uiso 1 1 calc R . . C48 C 1.0648(4) 0.8439(4) 0.6720(3) 0.0677(19) Uani 1 1 d . . . H48A H 1.0731 0.7900 0.6587 0.102 Uiso 1 1 calc R . . H48B H 1.0853 0.8465 0.7161 0.102 Uiso 1 1 calc R . . H48C H 1.0950 0.8822 0.6548 0.102 Uiso 1 1 calc R . . C49 C 0.9267(5) 0.7627(4) 0.5604(3) 0.074(2) Uani 1 1 d . . . H49A H 0.9520 0.7852 0.5314 0.112 Uiso 1 1 calc R . . H49B H 0.8740 0.7377 0.5387 0.112 Uiso 1 1 calc R . . H49C H 0.9637 0.7227 0.5852 0.112 Uiso 1 1 calc R . . C50 C 0.7494(5) 0.8497(5) 0.5459(3) 0.086(2) Uani 1 1 d . . . H50A H 0.7036 0.8656 0.5608 0.130 Uiso 1 1 calc R . . H50B H 0.7449 0.7928 0.5361 0.130 Uiso 1 1 calc R . . H50C H 0.7472 0.8805 0.5096 0.130 Uiso 1 1 calc R . . C51 C 0.8929(7) 0.0467(6) 0.9226(4) 0.100(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0358(2) 0.0402(2) 0.0374(2) 0.00428(18) 0.00641(17) -0.00996(18) Rh2 0.0367(2) 0.0311(2) 0.0380(2) 0.00764(17) 0.01162(17) -0.00113(17) N1 0.038(2) 0.050(3) 0.039(2) 0.005(2) 0.005(2) -0.008(2) N2 0.037(2) 0.031(2) 0.039(2) 0.0045(18) 0.0063(19) 0.0010(18) O1 0.045(2) 0.0320(18) 0.048(2) 0.0027(16) 0.0174(17) -0.0062(15) O2 0.0407(19) 0.042(2) 0.046(2) 0.0000(16) 0.0187(17) -0.0094(16) O3 0.0394(18) 0.0259(16) 0.049(2) 0.0052(15) 0.0180(16) 0.0042(14) O4 0.046(2) 0.0321(18) 0.055(2) -0.0001(16) 0.0230(17) -0.0056(16) O5 0.294(13) 0.162(8) 0.204(9) -0.030(7) 0.039(9) 0.121(9) O6 0.300(12) 0.143(7) 0.203(9) 0.004(6) 0.111(9) -0.129(8) O7 0.226(7) 0.076(4) 0.090(4) -0.032(3) 0.053(5) -0.050(4) F1 0.331(11) 0.237(9) 0.126(5) -0.025(5) 0.110(7) -0.162(8) F2 0.235(7) 0.115(4) 0.113(4) -0.042(4) 0.028(4) -0.037(5) F3 0.203(8) 0.256(9) 0.197(8) 0.025(7) 0.065(6) 0.134(7) S1 0.153(2) 0.0681(13) 0.0986(17) -0.0198(12) 0.0308(16) 0.0003(15) C1 0.031(3) 0.033(3) 0.032(3) 0.005(2) 0.004(2) 0.002(2) C2 0.026(2) 0.028(2) 0.031(2) 0.0025(19) 0.0060(19) -0.0041(19) C3 0.028(2) 0.040(3) 0.032(3) 0.001(2) 0.009(2) -0.006(2) C4 0.025(2) 0.037(3) 0.035(3) 0.002(2) 0.006(2) -0.001(2) C5 0.039(3) 0.049(3) 0.044(3) 0.004(2) 0.018(2) -0.005(2) C6 0.055(3) 0.055(3) 0.042(3) -0.006(3) 0.018(3) 0.008(3) C7 0.048(3) 0.037(3) 0.060(4) -0.003(3) 0.026(3) 0.004(2) C8 0.034(3) 0.035(3) 0.052(3) 0.001(2) 0.014(2) 0.003(2) C9 0.027(2) 0.038(3) 0.036(3) 0.002(2) 0.002(2) 0.004(2) C10 0.027(2) 0.033(3) 0.029(2) 0.005(2) 0.007(2) 0.0004(19) C11 0.028(2) 0.031(2) 0.028(2) 0.0015(19) 0.0060(19) -0.0016(19) C12 0.030(2) 0.032(2) 0.033(3) 0.004(2) 0.006(2) -0.002(2) C13 0.036(3) 0.033(2) 0.039(3) -0.001(2) 0.009(2) 0.003(2) C14 0.051(3) 0.037(3) 0.056(3) 0.006(2) 0.025(3) 0.001(2) C15 0.066(4) 0.047(3) 0.077(4) -0.013(3) 0.039(4) 0.009(3) C16 0.060(4) 0.036(3) 0.079(4) -0.007(3) 0.031(3) 0.003(3) C17 0.043(3) 0.038(3) 0.060(3) 0.002(3) 0.020(3) 0.007(2) C18 0.031(3) 0.030(2) 0.039(3) 0.004(2) 0.009(2) -0.002(2) C19 0.061(4) 0.053(3) 0.050(4) 0.001(3) 0.015(3) 0.004(3) C20 0.076(4) 0.058(4) 0.034(3) -0.005(3) 0.009(3) 0.007(3) C21 0.047(3) 0.044(3) 0.039(3) 0.003(2) 0.006(3) -0.008(3) C22 0.039(3) 0.051(3) 0.056(3) 0.004(3) 0.014(3) 0.002(3) C23 0.043(3) 0.053(3) 0.044(3) 0.002(3) 0.008(3) -0.001(3) C24 0.053(4) 0.058(4) 0.057(4) -0.001(3) 0.014(3) 0.005(3) C25 0.054(4) 0.055(4) 0.053(4) 0.004(3) 0.020(3) -0.011(3) C26 0.042(3) 0.039(3) 0.049(3) 0.011(3) 0.016(3) -0.002(2) C27 0.039(3) 0.062(4) 0.049(3) 0.005(3) 0.012(3) -0.005(3) C28 0.049(3) 0.047(3) 0.045(3) 0.009(3) 0.010(3) -0.014(3) C29 0.047(3) 0.035(3) 0.068(4) 0.007(3) 0.015(3) 0.005(2) C30 0.051(3) 0.035(3) 0.052(3) 0.009(2) 0.010(3) 0.003(2) C31 0.037(3) 0.101(5) 0.046(4) -0.028(4) 0.005(3) -0.023(3) C32 0.045(4) 0.024(3) 0.132(7) 0.001(4) -0.030(4) -0.010(3) C33 0.051(4) 0.096(6) 0.055(4) 0.002(4) 0.009(3) -0.044(4) C34 0.048(4) 0.087(6) 0.097(6) -0.023(5) 0.024(4) -0.023(4) C35 0.038(3) 0.063(4) 0.075(5) 0.017(4) -0.012(3) -0.003(3) C36 0.077(6) 0.47(3) 0.124(9) -0.179(13) 0.042(6) -0.076(10) C37 0.105(8) 0.046(5) 0.46(2) 0.012(9) -0.118(11) -0.025(5) C38 0.121(8) 0.37(2) 0.085(7) 0.030(9) 0.018(6) -0.156(11) C39 0.068(6) 0.191(12) 0.294(17) -0.142(12) 0.058(8) -0.026(7) C40 0.116(8) 0.157(11) 0.213(13) 0.110(10) -0.072(8) -0.047(7) C41 0.049(3) 0.035(3) 0.045(3) 0.018(2) 0.019(3) 0.002(2) C42 0.044(3) 0.034(3) 0.043(3) 0.012(2) 0.013(2) -0.002(2) C43 0.043(3) 0.046(3) 0.059(4) 0.019(3) 0.026(3) 0.004(2) C44 0.062(4) 0.043(3) 0.057(4) 0.015(3) 0.032(3) -0.003(3) C45 0.063(4) 0.045(3) 0.039(3) 0.014(3) 0.012(3) -0.003(3) C46 0.060(4) 0.052(3) 0.073(4) 0.021(3) 0.028(3) 0.018(3) C47 0.067(4) 0.038(3) 0.069(4) 0.005(3) 0.018(3) -0.014(3) C48 0.050(4) 0.060(4) 0.105(5) 0.023(4) 0.042(4) 0.005(3) C49 0.111(6) 0.059(4) 0.066(4) -0.005(3) 0.045(4) -0.002(4) C50 0.097(6) 0.077(5) 0.060(4) 0.012(4) -0.014(4) -0.011(4) C51 0.134(8) 0.088(6) 0.094(6) -0.027(5) 0.061(6) -0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.050(3) . ? Rh1 O2 2.063(3) . ? Rh1 C32 2.092(5) . ? Rh1 N1 2.102(4) . ? Rh1 C31 2.115(5) . ? Rh1 C35 2.119(6) . ? Rh1 C33 2.132(6) . ? Rh1 C34 2.160(7) . ? Rh2 O4 2.056(3) . ? Rh2 O3 2.066(3) . ? Rh2 C45 2.119(5) . ? Rh2 C41 2.125(5) . ? Rh2 C42 2.131(5) . ? Rh2 C43 2.133(5) . ? Rh2 N2 2.135(4) . ? Rh2 C44 2.137(5) . ? N1 C23 1.333(7) . ? N1 C19 1.342(7) . ? N2 C30 1.317(6) . ? N2 C26 1.336(6) . ? O1 C1 1.283(5) . ? O2 C3 1.273(5) . ? O3 C10 1.281(5) . ? O4 C12 1.272(5) . ? O5 S1 1.364(8) . ? O6 S1 1.478(8) . ? O7 S1 1.367(5) . ? F1 C51 1.285(10) . ? F2 C51 1.317(9) . ? F3 C51 1.243(10) . ? S1 C51 1.812(10) . ? C1 C2 1.409(6) . ? C1 C18 1.460(7) . ? C2 C3 1.418(6) . ? C2 C11 1.487(6) . ? C3 C4 1.450(7) . ? C4 C5 1.388(7) . ? C4 C9 1.402(7) . ? C5 C6 1.367(7) . ? C6 C7 1.403(8) . ? C7 C8 1.369(7) . ? C8 C9 1.391(7) . ? C9 C10 1.458(7) . ? C10 C11 1.421(6) . ? C11 C12 1.412(6) . ? C12 C13 1.477(6) . ? C13 C18 1.380(6) . ? C13 C14 1.388(7) . ? C14 C15 1.367(7) . ? C15 C16 1.389(8) . ? C16 C17 1.347(8) . ? C17 C18 1.390(7) . ? C19 C20 1.369(8) . ? C20 C21 1.358(8) . ? C21 C22 1.386(7) . ? C21 C24 1.473(8) . ? C22 C23 1.375(7) . ? C24 C25 1.250(8) . ? C25 C28 1.477(8) 3_767 ? C26 C27 1.371(7) . ? C27 C28 1.392(8) . ? C28 C29 1.371(8) . ? C28 C25 1.477(8) 3_767 ? C29 C30 1.397(8) . ? C31 C35 1.391(9) . ? C31 C36 1.435(10) . ? C31 C32 1.489(10) . ? C32 C33 1.416(10) . ? C32 C37 1.487(10) . ? C33 C34 1.317(10) . ? C33 C38 1.482(10) . ? C34 C35 1.339(10) . ? C34 C39 1.525(11) . ? C35 C40 1.553(11) . ? C41 C42 1.410(7) . ? C41 C45 1.422(8) . ? C41 C46 1.493(7) . ? C42 C43 1.443(7) . ? C42 C47 1.493(8) . ? C43 C44 1.411(8) . ? C43 C48 1.494(7) . ? C44 C45 1.425(8) . ? C44 C49 1.485(8) . ? C45 C50 1.521(8) . ? 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 Rh1 O2 83.85(13) . . ? O1 Rh1 C32 114.1(3) . . ? O2 Rh1 C32 160.8(2) . . ? O1 Rh1 N1 85.21(16) . . ? O2 Rh1 N1 84.96(15) . . ? C32 Rh1 N1 102.4(2) . . ? O1 Rh1 C31 93.46(19) . . ? O2 Rh1 C31 136.0(2) . . ? C32 Rh1 C31 41.4(3) . . ? N1 Rh1 C31 138.8(3) . . ? O1 Rh1 C35 112.7(2) . . ? O2 Rh1 C35 103.1(2) . . ? C32 Rh1 C35 64.9(2) . . ? N1 Rh1 C35 160.8(2) . . ? C31 Rh1 C35 38.4(3) . . ? O1 Rh1 C33 153.3(3) . . ? O2 Rh1 C33 122.6(3) . . ? C32 Rh1 C33 39.2(3) . . ? N1 Rh1 C33 99.8(2) . . ? C31 Rh1 C33 65.5(2) . . ? C35 Rh1 C33 61.2(3) . . ? O1 Rh1 C34 148.8(3) . . ? O2 Rh1 C34 97.4(2) . . ? C32 Rh1 C34 63.9(3) . . ? N1 Rh1 C34 126.0(3) . . ? C31 Rh1 C34 64.1(3) . . ? C35 Rh1 C34 36.5(3) . . ? C33 Rh1 C34 35.7(3) . . ? O4 Rh2 O3 85.39(12) . . ? O4 Rh2 C45 106.62(19) . . ? O3 Rh2 C45 110.14(19) . . ? O4 Rh2 C41 144.22(18) . . ? O3 Rh2 C41 97.00(16) . . ? C45 Rh2 C41 39.2(2) . . ? O4 Rh2 C42 156.05(17) . . ? O3 Rh2 C42 118.50(17) . . ? C45 Rh2 C42 65.4(2) . . ? C41 Rh2 C42 38.70(19) . . ? O4 Rh2 C43 116.57(18) . . ? O3 Rh2 C43 158.04(18) . . ? C45 Rh2 C43 65.4(2) . . ? C41 Rh2 C43 65.6(2) . . ? C42 Rh2 C43 39.6(2) . . ? O4 Rh2 N2 85.46(14) . . ? O3 Rh2 N2 82.55(15) . . ? C45 Rh2 N2 162.77(19) . . ? C41 Rh2 N2 130.31(18) . . ? C42 Rh2 N2 98.61(17) . . ? C43 Rh2 N2 98.40(19) . . ? O4 Rh2 C44 93.86(18) . . ? O3 Rh2 C44 147.43(19) . . ? C45 Rh2 C44 39.1(2) . . ? C41 Rh2 C44 65.4(2) . . ? C42 Rh2 C44 65.4(2) . . ? C43 Rh2 C44 38.6(2) . . ? N2 Rh2 C44 129.9(2) . . ? C23 N1 C19 118.9(5) . . ? C23 N1 Rh1 120.9(4) . . ? C19 N1 Rh1 120.2(4) . . ? C30 N2 C26 116.9(5) . . ? C30 N2 Rh2 121.6(4) . . ? C26 N2 Rh2 121.5(3) . . ? C1 O1 Rh1 127.5(3) . . ? C3 O2 Rh1 129.8(3) . . ? C10 O3 Rh2 127.7(3) . . ? C12 O4 Rh2 129.4(3) . . ? O5 S1 O7 118.8(6) . . ? O5 S1 O6 111.8(7) . . ? O7 S1 O6 113.2(5) . . ? O5 S1 C51 106.5(6) . . ? O7 S1 C51 104.0(4) . . ? O6 S1 C51 100.0(5) . . ? O1 C1 C2 125.7(4) . . ? O1 C1 C18 114.0(4) . . ? C2 C1 C18 120.3(4) . . ? C1 C2 C3 121.2(4) . . ? C1 C2 C11 119.1(4) . . ? C3 C2 C11 119.6(4) . . ? O2 C3 C2 125.1(4) . . ? O2 C3 C4 115.5(4) . . ? C2 C3 C4 119.4(4) . . ? C5 C4 C9 119.8(5) . . ? C5 C4 C3 120.2(4) . . ? C9 C4 C3 120.1(4) . . ? C6 C5 C4 120.5(5) . . ? C5 C6 C7 120.3(5) . . ? C8 C7 C6 119.2(5) . . ? C7 C8 C9 121.5(5) . . ? C8 C9 C4 118.7(5) . . ? C8 C9 C10 120.3(4) . . ? C4 C9 C10 120.8(4) . . ? O3 C10 C11 125.9(4) . . ? O3 C10 C9 115.0(4) . . ? C11 C10 C9 119.1(4) . . ? C12 C11 C10 121.2(4) . . ? C12 C11 C2 120.0(4) . . ? C10 C11 C2 118.9(4) . . ? O4 C12 C11 127.0(4) . . ? O4 C12 C13 113.7(4) . . ? C11 C12 C13 119.3(4) . . ? C18 C13 C14 120.0(5) . . ? C18 C13 C12 120.4(4) . . ? C14 C13 C12 119.6(4) . . ? C15 C14 C13 120.3(5) . . ? C14 C15 C16 119.1(5) . . ? C17 C16 C15 121.1(5) . . ? C16 C17 C18 120.4(5) . . ? C13 C18 C17 119.1(5) . . ? C13 C18 C1 120.9(4) . . ? C17 C18 C1 120.0(4) . . ? N1 C19 C20 121.5(5) . . ? C21 C20 C19 121.4(6) . . ? C20 C21 C22 116.2(5) . . ? C20 C21 C24 120.1(5) . . ? C22 C21 C24 123.6(5) . . ? C23 C22 C21 121.2(5) . . ? N1 C23 C22 120.8(5) . . ? C25 C24 C21 128.7(6) . . ? C24 C25 C28 125.4(6) . 3_767 ? N2 C26 C27 124.3(5) . . ? C26 C27 C28 119.0(6) . . ? C29 C28 C27 116.9(5) . . ? C29 C28 C25 122.8(5) . 3_767 ? C27 C28 C25 120.3(6) . 3_767 ? C28 C29 C30 120.3(5) . . ? N2 C30 C29 122.7(5) . . ? C35 C31 C36 127.4(10) . . ? C35 C31 C32 103.2(6) . . ? C36 C31 C32 129.3(10) . . ? C35 C31 Rh1 71.0(3) . . ? C36 C31 Rh1 122.5(5) . . ? C32 C31 Rh1 68.5(3) . . ? C33 C32 C37 125.7(11) . . ? C33 C32 C31 104.5(5) . . ? C37 C32 C31 129.6(11) . . ? C33 C32 Rh1 71.9(3) . . ? C37 C32 Rh1 125.5(5) . . ? C31 C32 Rh1 70.1(3) . . ? C34 C33 C32 110.8(7) . . ? C34 C33 C38 124.5(10) . . ? C32 C33 C38 124.7(10) . . ? C34 C33 Rh1 73.3(4) . . ? C32 C33 Rh1 68.9(3) . . ? C38 C33 Rh1 125.7(5) . . ? C33 C34 C35 109.1(7) . . ? C33 C34 C39 126.8(10) . . ? C35 C34 C39 124.1(10) . . ? C33 C34 Rh1 71.0(4) . . ? C35 C34 Rh1 70.1(4) . . ? C39 C34 Rh1 123.9(5) . . ? C34 C35 C31 112.3(7) . . ? C34 C35 C40 124.1(9) . . ? C31 C35 C40 123.6(9) . . ? C34 C35 Rh1 73.4(4) . . ? C31 C35 Rh1 70.7(3) . . ? C40 C35 Rh1 124.2(5) . . ? C42 C41 C45 108.3(5) . . ? C42 C41 C46 125.9(5) . . ? C45 C41 C46 125.8(5) . . ? C42 C41 Rh2 70.9(3) . . ? C45 C41 Rh2 70.2(3) . . ? C46 C41 Rh2 123.1(4) . . ? C41 C42 C43 107.8(5) . . ? C41 C42 C47 127.2(5) . . ? C43 C42 C47 125.0(5) . . ? C41 C42 Rh2 70.4(3) . . ? C43 C42 Rh2 70.3(3) . . ? C47 C42 Rh2 126.8(4) . . ? C44 C43 C42 107.7(5) . . ? C44 C43 C48 125.9(6) . . ? C42 C43 C48 126.3(6) . . ? C44 C43 Rh2 70.9(3) . . ? C42 C43 Rh2 70.2(3) . . ? C48 C43 Rh2 126.3(4) . . ? C43 C44 C45 108.2(5) . . ? C43 C44 C49 126.1(6) . . ? C45 C44 C49 125.7(6) . . ? C43 C44 Rh2 70.5(3) . . ? C45 C44 Rh2 69.8(3) . . ? C49 C44 Rh2 124.5(4) . . ? C41 C45 C44 108.0(5) . . ? C41 C45 C50 125.1(6) . . ? C44 C45 C50 126.8(6) . . ? C41 C45 Rh2 70.6(3) . . ? C44 C45 Rh2 71.1(3) . . ? C50 C45 Rh2 126.8(4) . . ? F3 C51 F1 109.0(10) . . ? F3 C51 F2 113.5(11) . . ? F1 C51 F2 103.6(8) . . ? F3 C51 S1 109.5(7) . . ? F1 C51 S1 109.7(8) . . ? F2 C51 S1 111.3(7) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.195 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.109 # Attachment 'Complex 5a.cif' data_complex_5a _database_code_depnum_ccdc_archive 'CCDC 712025' #TrackingRef 'Complex 5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H96 F12 Ir4 N4 O20 S4' _chemical_formula_weight 2846.89 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.741(7) _cell_length_b 16.323(7) _cell_length_c 22.861(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.395(6) _cell_angle_gamma 90.00 _cell_volume 5962(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 895 _cell_measurement_theta_min 2.496 _cell_measurement_theta_max 21.924 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 4.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4597 _exptl_absorpt_correction_T_max 0.6562 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.03 _diffrn_reflns_number 28370 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.1433 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.15 _reflns_number_total 12799 _reflns_number_gt 6484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12799 _refine_ls_number_parameters 632 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.773 _refine_ls_restrained_S_all 0.773 _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 Ir1 Ir 0.380061(17) 0.694077(18) 0.682643(12) 0.03718(9) Uani 1 1 d . . . Ir2 Ir 0.086094(18) 1.062389(19) 0.772959(12) 0.04062(9) Uani 1 1 d . . . N1 N 0.4532(4) 0.7280(4) 0.7719(3) 0.0403(15) Uani 1 1 d . . . N2 N 0.1697(4) 1.0942(4) 0.8579(2) 0.0442(16) Uani 1 1 d . A . O1 O 0.2867(3) 0.7025(3) 0.72497(19) 0.0396(12) Uani 1 1 d . . . O2 O 0.3632(3) 0.8189(3) 0.66964(19) 0.0399(12) Uani 1 1 d . . . O3 O 0.1916(3) 1.0594(3) 0.74431(19) 0.0406(11) Uani 1 1 d . A . O4 O 0.1225(3) 0.9448(3) 0.80318(18) 0.0387(12) Uani 1 1 d . A . O5 O 0.3208(4) 0.0074(4) 0.3124(3) 0.102(2) Uani 1 1 d . . . O6 O 0.2819(7) 0.1325(7) 0.3502(4) 0.201(5) Uani 1 1 d . . . O7 O 0.4166(6) 0.1199(5) 0.3327(4) 0.151(4) Uani 1 1 d . . . S1 S 0.3452(2) 0.08041(19) 0.34506(13) 0.0906(9) Uani 1 1 d . . . F1 F 0.3397(6) 0.0038(5) 0.4422(3) 0.167(3) Uani 1 1 d . . . F2 F 0.4188(4) 0.1077(5) 0.4606(3) 0.137(3) Uani 1 1 d . . . F3 F 0.4554(5) -0.0036(5) 0.4239(4) 0.173(4) Uani 1 1 d . . . C1 C 0.2588(4) 0.7663(4) 0.7450(3) 0.0332(17) Uani 1 1 d . A . C2 C 0.2664(4) 0.8481(4) 0.7267(3) 0.0313(16) Uani 1 1 d . . . C3 C 0.3156(4) 0.8677(4) 0.6876(3) 0.0346(17) Uani 1 1 d . . . C4 C 0.3180(4) 0.9519(4) 0.6656(3) 0.0311(16) Uani 1 1 d . . . C5 C 0.3610(4) 0.9711(4) 0.6253(3) 0.0424(19) Uani 1 1 d . . . H5 H 0.3914 0.9294 0.6121 0.051 Uiso 1 1 calc R . . C6 C 0.3614(5) 1.0488(5) 0.6036(4) 0.058(2) Uani 1 1 d . . . H6 H 0.3911 1.0603 0.5750 0.069 Uiso 1 1 calc R . . C7 C 0.3191(5) 1.1109(5) 0.6227(4) 0.054(2) Uani 1 1 d . . . H7 H 0.3197 1.1649 0.6073 0.064 Uiso 1 1 calc R . . C8 C 0.2762(4) 1.0943(4) 0.6641(3) 0.0455(19) Uani 1 1 d . . . H8 H 0.2475 1.1369 0.6777 0.055 Uiso 1 1 calc R . . C9 C 0.2750(4) 1.0147(4) 0.6861(3) 0.0344(17) Uani 1 1 d . A . C10 C 0.2244(4) 0.9960(4) 0.7271(3) 0.0318(16) Uani 1 1 d . . . C11 C 0.2202(4) 0.9150(4) 0.7463(3) 0.0307(16) Uani 1 1 d . A . C12 C 0.1741(4) 0.8958(4) 0.7874(3) 0.0363(17) Uani 1 1 d . . . C13 C 0.1799(4) 0.8145(4) 0.8146(3) 0.0340(16) Uani 1 1 d . A . C14 C 0.1504(4) 0.8008(5) 0.8652(3) 0.0465(19) Uani 1 1 d . . . H14 H 0.1247 0.8439 0.8810 0.056 Uiso 1 1 calc R A . C15 C 0.1594(5) 0.7229(5) 0.8923(3) 0.051(2) Uani 1 1 d . A . H15 H 0.1397 0.7130 0.9265 0.061 Uiso 1 1 calc R . . C16 C 0.1970(4) 0.6606(5) 0.8692(3) 0.046(2) Uani 1 1 d . . . H16 H 0.2025 0.6079 0.8876 0.055 Uiso 1 1 calc R A . C17 C 0.2265(4) 0.6737(4) 0.8199(3) 0.0404(18) Uani 1 1 d . A . H17 H 0.2521 0.6301 0.8046 0.049 Uiso 1 1 calc R . . C18 C 0.2191(4) 0.7505(4) 0.7921(3) 0.0316(16) Uani 1 1 d . . . C19 C 0.4461(4) 0.6912(5) 0.8225(3) 0.051(2) Uani 1 1 d . . . H19 H 0.4057 0.6489 0.8172 0.061 Uiso 1 1 calc R . . C20 C 0.4917(5) 0.7095(5) 0.8804(3) 0.051(2) Uani 1 1 d . . . H20 H 0.4829 0.6807 0.9141 0.061 Uiso 1 1 calc R . . C21 C 0.5523(5) 0.7716(5) 0.8903(3) 0.050(2) Uani 1 1 d . . . C22 C 0.5616(5) 0.8104(5) 0.8405(4) 0.057(2) Uani 1 1 d . . . H22 H 0.6021 0.8527 0.8456 0.069 Uiso 1 1 calc R . . C23 C 0.5111(5) 0.7886(4) 0.7804(4) 0.050(2) Uani 1 1 d . . . H23 H 0.5181 0.8169 0.7460 0.060 Uiso 1 1 calc R . . C24 C 0.6048(5) 0.7905(5) 0.9545(4) 0.059(2) Uani 1 1 d . . . H24 H 0.5909 0.7660 0.9879 0.071 Uiso 1 1 calc R . . C25 C 0.1676(5) 1.0594(5) 0.9095(3) 0.057(2) Uani 1 1 d . . . H25 H 0.1279 1.0170 0.9073 0.068 Uiso 1 1 calc R A . C26 C 0.2183(5) 1.0804(5) 0.9650(3) 0.061(2) Uani 1 1 d . A . H26 H 0.2135 1.0532 1.0006 0.073 Uiso 1 1 calc R . . C27 C 0.2767(5) 1.1406(5) 0.9705(3) 0.053(2) Uani 1 1 d . . . C28 C 0.2788(4) 1.1790(5) 0.9167(3) 0.051(2) Uani 1 1 d . A . H28 H 0.3172 1.2225 0.9184 0.061 Uiso 1 1 calc R . . C29 C 0.2267(5) 1.1549(5) 0.8618(3) 0.049(2) Uani 1 1 d . . . H29 H 0.2299 1.1809 0.8254 0.059 Uiso 1 1 calc R A . C30 C 0.3327(5) 1.1617(5) 1.0348(4) 0.063(2) Uani 1 1 d . . . H30 H 0.3201 1.1375 1.0688 0.076 Uiso 1 1 calc R . . C31 C 0.3487(4) 0.5763(4) 0.6427(3) 0.0411(19) Uani 1 1 d . . . C32 C 0.4345(4) 0.5766(4) 0.6771(3) 0.0410(19) Uani 1 1 d . . . C33 C 0.4737(5) 0.6365(5) 0.6509(3) 0.045(2) Uani 1 1 d . . . C34 C 0.4141(5) 0.6730(5) 0.6002(3) 0.048(2) Uani 1 1 d . . . C35 C 0.3349(5) 0.6370(5) 0.5952(3) 0.048(2) Uani 1 1 d . . . C36 C 0.2821(5) 0.5229(5) 0.6543(4) 0.059(2) Uani 1 1 d . . . H36A H 0.2808 0.4703 0.6334 0.088 Uiso 1 1 calc R . . H36B H 0.2277 0.5500 0.6386 0.088 Uiso 1 1 calc R . . H36C H 0.2944 0.5136 0.6984 0.088 Uiso 1 1 calc R . . C37 C 0.4764(5) 0.5226(4) 0.7298(3) 0.055(2) Uani 1 1 d . . . H37A H 0.5082 0.4800 0.7163 0.083 Uiso 1 1 calc R . . H37B H 0.4341 0.4970 0.7456 0.083 Uiso 1 1 calc R . . H37C H 0.5146 0.5553 0.7623 0.083 Uiso 1 1 calc R . . C38 C 0.5670(5) 0.6576(5) 0.6719(4) 0.074(3) Uani 1 1 d . . . H38A H 0.5872 0.6585 0.7168 0.111 Uiso 1 1 calc R . . H38B H 0.5755 0.7115 0.6559 0.111 Uiso 1 1 calc R . . H38C H 0.5980 0.6162 0.6564 0.111 Uiso 1 1 calc R . . C39 C 0.4293(6) 0.7394(5) 0.5610(4) 0.076(3) Uani 1 1 d . . . H39A H 0.4513 0.7162 0.5294 0.115 Uiso 1 1 calc R . . H39B H 0.4701 0.7781 0.5862 0.115 Uiso 1 1 calc R . . H39C H 0.3767 0.7681 0.5415 0.115 Uiso 1 1 calc R . . C40 C 0.2539(5) 0.6533(6) 0.5443(3) 0.082(3) Uani 1 1 d . . . H40A H 0.2508 0.7114 0.5331 0.124 Uiso 1 1 calc R . . H40B H 0.2060 0.6390 0.5586 0.124 Uiso 1 1 calc R . . H40C H 0.2527 0.6200 0.5084 0.124 Uiso 1 1 calc R . . C41 C 0.0118(3) 1.1266(5) 0.6957(3) 0.072(5) Uani 0.728(12) 1 d PG A 1 C42 C 0.0083(3) 1.1670(3) 0.7495(3) 0.065(5) Uani 0.728(12) 1 d PG A 1 C43 C -0.0302(3) 1.1137(4) 0.7816(2) 0.051(3) Uani 0.728(12) 1 d PG A 1 C44 C -0.0506(3) 1.0404(4) 0.7476(3) 0.068(4) Uani 0.728(12) 1 d PGU A 1 C45 C -0.0246(3) 1.0483(4) 0.6946(3) 0.079(6) Uani 0.728(12) 1 d PG A 1 C46 C 0.0479(5) 1.1608(8) 0.6482(5) 0.208(16) Uani 0.728(12) 1 d PG A 1 H46A H 0.0036 1.1883 0.6162 0.312 Uiso 0.728(12) 1 calc PR A 1 H46B H 0.0715 1.1162 0.6299 0.312 Uiso 0.728(12) 1 calc PR A 1 H46C H 0.0920 1.2003 0.6674 0.312 Uiso 0.728(12) 1 calc PR A 1 C47 C 0.0400(5) 1.2517(4) 0.7692(6) 0.172(13) Uani 0.728(12) 1 d PG A 1 H47A H 0.0824 1.2491 0.8094 0.258 Uiso 0.728(12) 1 calc PR A 1 H47B H -0.0066 1.2863 0.7718 0.258 Uiso 0.728(12) 1 calc PR A 1 H47C H 0.0649 1.2749 0.7391 0.258 Uiso 0.728(12) 1 calc PR A 1 C48 C -0.0467(6) 1.1318(8) 0.8413(3) 0.141(10) Uani 0.728(12) 1 d PG A 1 H48A H -0.1065 1.1250 0.8365 0.211 Uiso 0.728(12) 1 calc PR A 1 H48B H -0.0300 1.1883 0.8537 0.211 Uiso 0.728(12) 1 calc PR A 1 H48C H -0.0143 1.0941 0.8729 0.211 Uiso 0.728(12) 1 calc PR A 1 C49 C -0.0925(4) 0.9669(6) 0.7649(6) 0.235(17) Uani 0.728(12) 1 d PG A 1 H49A H -0.1531 0.9711 0.7461 0.353 Uiso 0.728(12) 1 calc PR A 1 H49B H -0.0797 0.9645 0.8096 0.353 Uiso 0.728(12) 1 calc PR A 1 H49C H -0.0718 0.9171 0.7503 0.353 Uiso 0.728(12) 1 calc PR A 1 C50 C -0.0340(6) 0.9848(7) 0.6455(4) 0.182(12) Uani 0.728(12) 1 d PG A 1 H50A H -0.0552 0.9339 0.6581 0.273 Uiso 0.728(12) 1 calc PR A 1 H50B H 0.0205 0.9745 0.6392 0.273 Uiso 0.728(12) 1 calc PR A 1 H50C H -0.0734 1.0045 0.6072 0.273 Uiso 0.728(12) 1 calc PR A 1 C41' C 0.0062(3) 1.0976(5) 0.6855(2) 0.006(6) Uiso 0.272(12) 1 d PG A 2 C42' C 0.0266(3) 1.1692(4) 0.7205(4) 0.038(11) Uani 0.272(12) 1 d PG A 2 C43' C -0.0002(3) 1.1599(4) 0.7725(3) 0.031(9) Uani 0.272(12) 1 d PGU A 2 C44' C -0.0372(3) 1.0825(4) 0.7697(3) 0.034(9) Uiso 0.272(12) 1 d PG A 2 C45' C -0.0333(3) 1.0440(4) 0.7160(3) 0.012(7) Uani 0.272(12) 1 d PGU A 2 C46' C 0.0234(6) 1.0813(9) 0.6264(3) 0.14(2) Uiso 0.272(12) 1 d PG A 2 H46D H 0.0222 1.0221 0.6190 0.209 Uiso 0.272(12) 1 calc PR A 2 H46E H 0.0787 1.1029 0.6283 0.209 Uiso 0.272(12) 1 calc PR A 2 H46F H -0.0193 1.1081 0.5930 0.209 Uiso 0.272(12) 1 calc PR A 2 C47' C 0.0693(5) 1.2424(6) 0.7051(6) 0.098(16) Uani 0.272(12) 1 d PG A 2 H47D H 0.0275 1.2802 0.6800 0.147 Uiso 0.272(12) 1 calc PR A 2 H47E H 0.1075 1.2252 0.6821 0.147 Uiso 0.272(12) 1 calc PR A 2 H47F H 0.1012 1.2700 0.7429 0.147 Uiso 0.272(12) 1 calc PR A 2 C48' C 0.0090(6) 1.2214(6) 0.8221(5) 0.063(10) Uani 0.272(12) 1 d PGU A 2 H48D H 0.0368 1.2704 0.8128 0.095 Uiso 0.272(12) 1 calc PR A 2 H48E H 0.0426 1.1981 0.8612 0.095 Uiso 0.272(12) 1 calc PR A 2 H48F H -0.0465 1.2363 0.8250 0.095 Uiso 0.272(12) 1 calc PR A 2 C49' C -0.0743(5) 1.0474(7) 0.8158(4) 0.067(11) Uani 0.272(12) 1 d PGU A 2 H49D H -0.1314 1.0681 0.8082 0.100 Uiso 0.272(12) 1 calc PR A 2 H49E H -0.0403 1.0634 0.8570 0.100 Uiso 0.272(12) 1 calc PR A 2 H49F H -0.0755 0.9875 0.8125 0.100 Uiso 0.272(12) 1 calc PR A 2 C50' C -0.0654(5) 0.9608(5) 0.6948(5) 0.064(12) Uani 0.272(12) 1 d PG A 2 H50D H -0.0743 0.9562 0.6506 0.095 Uiso 0.272(12) 1 calc PR A 2 H50E H -0.1184 0.9516 0.7037 0.095 Uiso 0.272(12) 1 calc PR A 2 H50F H -0.0244 0.9196 0.7163 0.095 Uiso 0.272(12) 1 calc PR A 2 C51 C 0.3929(9) 0.0458(8) 0.4205(6) 0.106(4) 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 Ir1 0.03633(17) 0.03106(17) 0.04304(17) -0.00788(14) 0.01017(12) 0.00279(14) Ir2 0.03937(18) 0.0403(2) 0.03964(16) -0.00326(15) 0.00790(13) 0.01313(15) N1 0.041(4) 0.033(4) 0.046(4) -0.012(3) 0.012(3) 0.004(3) N2 0.038(4) 0.065(5) 0.031(3) -0.007(3) 0.012(3) 0.013(3) O1 0.039(3) 0.028(3) 0.052(3) -0.008(2) 0.014(2) 0.000(2) O2 0.038(3) 0.029(3) 0.055(3) 0.000(2) 0.019(2) 0.006(2) O3 0.048(3) 0.028(3) 0.046(3) -0.002(2) 0.014(2) 0.005(2) O4 0.033(3) 0.044(3) 0.042(3) 0.001(2) 0.016(2) 0.007(2) O5 0.142(6) 0.082(5) 0.093(5) -0.031(4) 0.050(4) -0.051(5) O6 0.209(11) 0.201(11) 0.168(9) -0.062(8) 0.019(7) 0.108(9) O7 0.199(9) 0.113(7) 0.152(7) -0.018(6) 0.069(7) -0.084(7) S1 0.122(3) 0.067(2) 0.086(2) -0.0173(16) 0.0358(18) -0.0120(19) F1 0.234(9) 0.173(8) 0.125(6) -0.023(5) 0.101(6) -0.085(7) F2 0.167(7) 0.126(6) 0.124(5) -0.047(5) 0.050(5) -0.041(5) F3 0.163(8) 0.173(9) 0.194(8) 0.026(6) 0.070(6) 0.072(7) C1 0.029(4) 0.030(4) 0.033(4) -0.006(3) -0.002(3) 0.007(3) C2 0.024(4) 0.031(4) 0.041(4) 0.000(3) 0.013(3) 0.007(3) C3 0.027(4) 0.033(5) 0.039(4) -0.002(3) 0.002(3) 0.000(3) C4 0.032(4) 0.026(4) 0.035(4) -0.003(3) 0.008(3) -0.006(3) C5 0.050(5) 0.030(5) 0.054(5) -0.002(4) 0.027(4) 0.002(4) C6 0.064(6) 0.046(6) 0.076(6) -0.007(5) 0.040(5) -0.016(5) C7 0.054(5) 0.032(5) 0.085(6) -0.007(4) 0.035(5) -0.009(4) C8 0.043(5) 0.027(5) 0.071(5) -0.006(4) 0.022(4) -0.003(4) C9 0.036(4) 0.023(4) 0.040(4) -0.010(3) 0.005(3) 0.004(3) C10 0.037(4) 0.025(4) 0.032(4) -0.004(3) 0.008(3) 0.006(3) C11 0.039(4) 0.025(4) 0.029(4) -0.005(3) 0.012(3) 0.004(3) C12 0.032(4) 0.031(4) 0.042(4) -0.006(4) 0.005(3) 0.004(3) C13 0.032(4) 0.030(4) 0.037(4) -0.004(3) 0.007(3) -0.001(3) C14 0.042(4) 0.051(5) 0.053(5) -0.006(4) 0.024(4) -0.011(4) C15 0.048(5) 0.056(6) 0.051(5) 0.013(4) 0.018(4) -0.004(4) C16 0.045(5) 0.029(5) 0.067(5) 0.000(4) 0.022(4) -0.005(4) C17 0.036(4) 0.032(5) 0.051(5) -0.005(4) 0.009(4) -0.007(3) C18 0.030(4) 0.028(4) 0.036(4) -0.002(3) 0.008(3) 0.000(3) C19 0.039(5) 0.055(6) 0.056(5) -0.023(5) 0.008(4) 0.004(4) C20 0.048(5) 0.059(6) 0.044(5) -0.007(4) 0.012(4) 0.008(4) C21 0.048(5) 0.048(6) 0.046(5) -0.008(4) 0.004(4) 0.017(4) C22 0.051(5) 0.042(5) 0.076(6) -0.014(5) 0.014(5) -0.005(4) C23 0.059(5) 0.026(5) 0.063(5) -0.011(4) 0.016(4) 0.007(4) C24 0.071(6) 0.052(6) 0.061(6) -0.007(4) 0.030(5) 0.006(5) C25 0.073(6) 0.044(5) 0.049(5) -0.013(4) 0.011(4) -0.006(5) C26 0.076(6) 0.064(7) 0.037(5) 0.004(4) 0.008(4) -0.020(5) C27 0.051(5) 0.062(6) 0.037(5) 0.002(4) -0.001(4) 0.016(5) C28 0.041(5) 0.047(5) 0.064(5) -0.010(5) 0.014(4) 0.005(4) C29 0.040(5) 0.061(6) 0.042(5) -0.006(4) 0.007(4) 0.004(4) C30 0.059(6) 0.050(6) 0.078(6) -0.004(5) 0.016(5) -0.002(5) C31 0.038(5) 0.041(5) 0.045(4) -0.009(4) 0.014(4) 0.013(4) C32 0.045(5) 0.029(5) 0.048(4) -0.012(4) 0.013(4) 0.008(4) C33 0.052(5) 0.036(5) 0.050(5) -0.012(4) 0.019(4) 0.007(4) C34 0.067(6) 0.038(5) 0.045(5) -0.009(4) 0.026(4) 0.001(4) C35 0.044(5) 0.046(5) 0.048(5) -0.013(4) 0.007(4) 0.006(4) C36 0.043(5) 0.047(6) 0.081(6) -0.014(5) 0.012(4) -0.010(4) C37 0.053(5) 0.035(5) 0.081(6) -0.011(5) 0.024(4) 0.000(4) C38 0.047(6) 0.058(6) 0.132(8) -0.015(6) 0.049(5) -0.005(5) C39 0.110(8) 0.058(7) 0.070(6) -0.004(5) 0.040(6) 0.008(6) C40 0.096(8) 0.079(8) 0.055(5) -0.012(5) -0.002(5) 0.029(6) C41 0.063(11) 0.074(13) 0.088(11) 0.019(11) 0.035(8) 0.025(9) C42 0.042(9) 0.059(12) 0.077(12) 0.011(8) -0.008(8) 0.007(7) C43 0.047(8) 0.046(9) 0.054(8) 0.005(7) 0.008(6) 0.009(6) C44 0.045(6) 0.064(8) 0.092(8) -0.017(7) 0.017(6) 0.008(6) C45 0.049(9) 0.120(16) 0.048(8) -0.046(9) -0.014(6) 0.031(9) C46 0.152(18) 0.39(5) 0.096(14) 0.14(2) 0.062(13) 0.12(2) C47 0.091(13) 0.041(10) 0.30(3) -0.016(15) -0.068(16) 0.022(9) C48 0.124(15) 0.22(2) 0.092(11) 0.019(12) 0.053(10) 0.114(16) C49 0.065(12) 0.086(15) 0.53(5) 0.11(2) 0.054(19) -0.006(10) C50 0.074(13) 0.28(3) 0.143(17) -0.129(18) -0.037(11) 0.056(15) C42' 0.034(19) 0.005(16) 0.07(3) -0.007(15) 0.004(18) 0.010(13) C43' 0.033(12) 0.035(12) 0.022(11) -0.010(8) 0.006(8) 0.006(9) C45' 0.016(10) 0.013(10) 0.007(9) 0.003(7) 0.003(7) -0.011(7) C47' 0.07(3) 0.05(3) 0.11(3) -0.01(2) -0.06(2) 0.03(2) C48' 0.066(13) 0.064(13) 0.056(12) -0.025(9) 0.012(9) 0.021(9) C49' 0.054(13) 0.084(14) 0.070(13) 0.006(9) 0.029(9) 0.004(9) C50' 0.025(17) 0.06(2) 0.08(2) 0.054(19) -0.019(15) -0.031(15) C51 0.127(11) 0.097(11) 0.117(10) -0.031(8) 0.075(9) -0.045(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O2 2.066(5) . ? Ir1 O1 2.075(4) . ? Ir1 N1 2.115(6) . ? Ir1 C31 2.126(7) . ? Ir1 C35 2.130(7) . ? Ir1 C33 2.133(7) . ? Ir1 C32 2.143(7) . ? Ir1 C34 2.154(7) . ? Ir2 C45' 2.055(4) . ? Ir2 O3 2.060(4) . ? Ir2 O4 2.069(5) . ? Ir2 C44' 2.070(4) . ? Ir2 N2 2.092(6) . ? Ir2 C41 2.109(4) . ? Ir2 C42 2.117(4) . ? Ir2 C41' 2.125(5) . ? Ir2 C43' 2.148(5) . ? Ir2 C45 2.171(5) . ? Ir2 C42' 2.181(5) . ? Ir2 C43 2.183(5) . ? N1 C19 1.340(9) . ? N1 C23 1.358(9) . ? N2 C25 1.320(9) . ? N2 C29 1.359(9) . ? O1 C1 1.280(7) . ? O2 C3 1.279(7) . ? O3 C10 1.287(7) . ? O4 C12 1.304(7) . ? O5 S1 1.401(6) . ? O6 S1 1.391(9) . ? O7 S1 1.457(8) . ? S1 C51 1.763(13) . ? F1 C51 1.331(11) . ? F2 C51 1.345(11) . ? F3 C51 1.304(13) . ? C1 C2 1.416(9) . ? C1 C18 1.449(9) . ? C2 C3 1.421(9) . ? C2 C11 1.482(8) . ? C3 C4 1.468(9) . ? C4 C5 1.364(8) . ? C4 C9 1.412(8) . ? C5 C6 1.363(9) . ? C6 C7 1.380(10) . ? C7 C8 1.375(9) . ? C8 C9 1.396(9) . ? C9 C10 1.470(9) . ? C10 C11 1.402(9) . ? C11 C12 1.418(9) . ? C12 C13 1.456(9) . ? C13 C14 1.406(8) . ? C13 C18 1.409(9) . ? C14 C15 1.402(10) . ? C15 C16 1.382(10) . ? C16 C17 1.376(9) . ? C17 C18 1.394(9) . ? C19 C20 1.349(9) . ? C20 C21 1.404(10) . ? C21 C22 1.351(10) . ? C21 C24 1.500(10) . ? C22 C23 1.426(10) . ? C24 C30 1.270(10) 3_677 ? C25 C26 1.342(9) . ? C26 C27 1.365(10) . ? C27 C28 1.392(9) . ? C27 C30 1.527(10) . ? C28 C29 1.355(9) . ? C30 C24 1.270(10) 3_677 ? C31 C32 1.416(9) . ? C31 C35 1.438(9) . ? C31 C36 1.499(9) . ? C32 C33 1.407(10) . ? C32 C37 1.490(9) . ? C33 C34 1.415(10) . ? C33 C38 1.529(10) . ? C34 C35 1.425(10) . ? C34 C39 1.476(10) . ? C35 C40 1.523(10) . ? C41 C42 1.412(3) . ? C41 C45 1.412(3) . ? C41 C46 1.501(3) . ? C42 C43 1.412(3) . ? C42 C47 1.501(3) . ? C43 C44 1.412(3) . ? C43 C48 1.501(3) . ? C44 C45 1.412(3) . ? C44 C49 1.501(3) . ? C45 C50 1.501(3) . ? C41' C42' 1.400(3) . ? C41' C45' 1.400(3) . ? C41' C46' 1.488(3) . ? C42' C43' 1.400(3) . ? C42' C47' 1.488(3) . ? C43' C44' 1.400(3) . ? C43' C48' 1.488(3) . ? C44' C45' 1.400(3) . ? C44' C49' 1.488(3) . ? C45' C50' 1.488(3) . ? 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 O2 Ir1 O1 84.93(17) . . ? O2 Ir1 N1 84.0(2) . . ? O1 Ir1 N1 80.4(2) . . ? O2 Ir1 C31 145.6(2) . . ? O1 Ir1 C31 97.9(2) . . ? N1 Ir1 C31 130.4(2) . . ? O2 Ir1 C35 107.6(2) . . ? O1 Ir1 C35 111.2(2) . . ? N1 Ir1 C35 163.9(2) . . ? C31 Ir1 C35 39.5(3) . . ? O2 Ir1 C33 117.9(3) . . ? O1 Ir1 C33 157.1(3) . . ? N1 Ir1 C33 99.8(2) . . ? C31 Ir1 C33 64.4(3) . . ? C35 Ir1 C33 65.1(3) . . ? O2 Ir1 C32 156.4(2) . . ? O1 Ir1 C32 118.7(2) . . ? N1 Ir1 C32 99.0(2) . . ? C31 Ir1 C32 38.7(2) . . ? C35 Ir1 C32 65.8(3) . . ? C33 Ir1 C32 38.4(3) . . ? O2 Ir1 C34 95.3(2) . . ? O1 Ir1 C34 148.5(3) . . ? N1 Ir1 C34 131.1(3) . . ? C31 Ir1 C34 64.9(3) . . ? C35 Ir1 C34 38.8(3) . . ? C33 Ir1 C34 38.5(3) . . ? C32 Ir1 C34 64.9(3) . . ? C45' Ir2 O3 124.0(2) . . ? C45' Ir2 O4 102.1(2) . . ? O3 Ir2 O4 83.62(17) . . ? C45' Ir2 C44' 39.67(9) . . ? O3 Ir2 C44' 158.96(19) . . ? O4 Ir2 C44' 110.5(2) . . ? C45' Ir2 N2 151.5(2) . . ? O3 Ir2 N2 84.3(2) . . ? O4 Ir2 N2 82.6(2) . . ? C44' Ir2 N2 112.2(2) . . ? C45' Ir2 C41 47.43(11) . . ? O3 Ir2 C41 95.33(19) . . ? O4 Ir2 C41 141.4(3) . . ? C44' Ir2 C41 63.82(13) . . ? N2 Ir2 C41 135.8(3) . . ? C45' Ir2 C42 63.21(13) . . ? O3 Ir2 C42 117.4(2) . . ? O4 Ir2 C42 158.5(2) . . ? C44' Ir2 C42 48.03(11) . . ? N2 Ir2 C42 103.0(2) . . ? C41 Ir2 C42 39.04(9) . . ? C45' Ir2 C41' 39.08(9) . . ? O3 Ir2 C41' 93.78(19) . . ? O4 Ir2 C41' 127.2(3) . . ? C44' Ir2 C41' 65.34(13) . . ? N2 Ir2 C41' 149.8(3) . . ? C41 Ir2 C41' 14.2 . . ? C42 Ir2 C41' 51.48(11) . . ? C45' Ir2 C43' 65.16(13) . . ? O3 Ir2 C43' 131.0(3) . . ? O4 Ir2 C43' 145.1(2) . . ? C44' Ir2 C43' 38.70(9) . . ? N2 Ir2 C43' 94.8(2) . . ? C41 Ir2 C43' 53.16(12) . . ? C42 Ir2 C43' 16.0 . . ? C41' Ir2 C43' 64.01(13) . . ? C45' Ir2 C45 14.7 . . ? O3 Ir2 C45 109.7(2) . . ? O4 Ir2 C45 105.7(2) . . ? C44' Ir2 C45 52.49(12) . . ? N2 Ir2 C45 164.1(2) . . ? C41 Ir2 C45 38.49(9) . . ? C42 Ir2 C45 64.38(13) . . ? C41' Ir2 C45 27.15(7) . . ? C43' Ir2 C45 70.58(14) . . ? C45' Ir2 C42' 64.56(13) . . ? O3 Ir2 C42' 97.9(2) . . ? O4 Ir2 C42' 165.0(2) . . ? C44' Ir2 C42' 64.32(13) . . ? N2 Ir2 C42' 112.4(3) . . ? C41 Ir2 C42' 23.72(6) . . ? C42 Ir2 C42' 21.68(5) . . ? C41' Ir2 C42' 37.91(9) . . ? C43' Ir2 C42' 37.72(9) . . ? C45 Ir2 C42' 59.59(13) . . ? C45' Ir2 C43 52.31(12) . . ? O3 Ir2 C43 155.7(2) . . ? O4 Ir2 C43 120.5(2) . . ? C44' Ir2 C43 15.2 . . ? N2 Ir2 C43 100.9(2) . . ? C41 Ir2 C43 64.29(13) . . ? C42 Ir2 C43 38.30(9) . . ? C41' Ir2 C43 69.73(14) . . ? C43' Ir2 C43 25.67(6) . . ? C45 Ir2 C43 63.30(13) . . ? C42' Ir2 C43 57.99(12) . . ? C19 N1 C23 116.4(6) . . ? C19 N1 Ir1 122.8(5) . . ? C23 N1 Ir1 120.8(5) . . ? C25 N2 C29 117.5(6) . . ? C25 N2 Ir2 122.2(6) . . ? C29 N2 Ir2 120.2(5) . . ? C1 O1 Ir1 128.8(4) . . ? C3 O2 Ir1 129.8(4) . . ? C10 O3 Ir2 126.9(4) . . ? C12 O4 Ir2 129.1(4) . . ? O6 S1 O5 117.2(6) . . ? O6 S1 O7 115.8(7) . . ? O5 S1 O7 113.5(5) . . ? O6 S1 C51 104.3(6) . . ? O5 S1 C51 102.9(5) . . ? O7 S1 C51 100.0(6) . . ? O1 C1 C2 126.0(6) . . ? O1 C1 C18 114.7(6) . . ? C2 C1 C18 119.2(6) . . ? C1 C2 C3 121.1(6) . . ? C1 C2 C11 120.4(6) . . ? C3 C2 C11 118.5(6) . . ? O2 C3 C2 126.6(6) . . ? O2 C3 C4 112.9(6) . . ? C2 C3 C4 120.5(6) . . ? C5 C4 C9 118.9(6) . . ? C5 C4 C3 121.4(6) . . ? C9 C4 C3 119.7(6) . . ? C6 C5 C4 121.4(7) . . ? C5 C6 C7 120.6(7) . . ? C8 C7 C6 119.7(7) . . ? C7 C8 C9 119.9(7) . . ? C8 C9 C4 119.4(6) . . ? C8 C9 C10 119.8(6) . . ? C4 C9 C10 120.6(6) . . ? O3 C10 C11 126.6(6) . . ? O3 C10 C9 114.0(6) . . ? C11 C10 C9 119.2(6) . . ? C10 C11 C12 120.3(6) . . ? C10 C11 C2 121.4(6) . . ? C12 C11 C2 118.3(6) . . ? O4 C12 C11 125.7(6) . . ? O4 C12 C13 114.0(6) . . ? C11 C12 C13 120.2(6) . . ? C14 C13 C18 119.9(7) . . ? C14 C13 C12 120.0(6) . . ? C18 C13 C12 120.0(6) . . ? C15 C14 C13 119.3(7) . . ? C16 C15 C14 120.0(7) . . ? C17 C16 C15 121.0(7) . . ? C16 C17 C18 120.6(7) . . ? C17 C18 C13 119.2(6) . . ? C17 C18 C1 120.1(6) . . ? C13 C18 C1 120.4(6) . . ? N1 C19 C20 125.4(8) . . ? C19 C20 C21 119.1(8) . . ? C22 C21 C20 117.6(7) . . ? C22 C21 C24 123.1(8) . . ? C20 C21 C24 119.3(8) . . ? C21 C22 C23 120.7(8) . . ? N1 C23 C22 120.8(7) . . ? C30 C24 C21 121.5(8) 3_677 . ? N2 C25 C26 123.8(8) . . ? C25 C26 C27 120.3(8) . . ? C26 C27 C28 116.7(7) . . ? C26 C27 C30 117.9(7) . . ? C28 C27 C30 125.3(8) . . ? C29 C28 C27 120.5(8) . . ? C28 C29 N2 121.2(7) . . ? C24 C30 C27 124.0(8) 3_677 . ? C32 C31 C35 108.9(7) . . ? C32 C31 C36 126.1(7) . . ? C35 C31 C36 125.0(7) . . ? C32 C31 Ir1 71.3(4) . . ? C35 C31 Ir1 70.4(4) . . ? C36 C31 Ir1 123.4(5) . . ? C33 C32 C31 107.0(7) . . ? C33 C32 C37 126.1(7) . . ? C31 C32 C37 126.9(7) . . ? C33 C32 Ir1 70.4(4) . . ? C31 C32 Ir1 70.0(4) . . ? C37 C32 Ir1 126.0(5) . . ? C32 C33 C34 109.7(7) . . ? C32 C33 C38 125.8(7) . . ? C34 C33 C38 124.5(7) . . ? C32 C33 Ir1 71.2(4) . . ? C34 C33 Ir1 71.6(4) . . ? C38 C33 Ir1 125.4(5) . . ? C33 C34 C35 107.7(7) . . ? C33 C34 C39 126.8(8) . . ? C35 C34 C39 125.4(8) . . ? C33 C34 Ir1 69.9(4) . . ? C35 C34 Ir1 69.7(4) . . ? C39 C34 Ir1 123.5(5) . . ? C34 C35 C31 106.7(6) . . ? C34 C35 C40 125.8(8) . . ? C31 C35 C40 127.1(7) . . ? C34 C35 Ir1 71.5(4) . . ? C31 C35 Ir1 70.1(4) . . ? C40 C35 Ir1 128.7(5) . . ? C42 C41 C45 108.0 . . ? C42 C41 C46 126.0 . . ? C45 C41 C46 126.0 . . ? C42 C41 Ir2 70.77(18) . . ? C45 C41 Ir2 73.11(17) . . ? C46 C41 Ir2 121.81(17) . . ? C41 C42 C43 108.0 . . ? C41 C42 C47 126.0 . . ? C43 C42 C47 126.0 . . ? C41 C42 Ir2 70.19(18) . . ? C43 C42 Ir2 73.38(18) . . ? C47 C42 Ir2 122.12(16) . . ? C44 C43 C42 108.0 . . ? C44 C43 C48 126.0 . . ? C42 C43 C48 126.0 . . ? C44 C43 Ir2 72.53(17) . . ? C42 C43 Ir2 68.32(17) . . ? C48 C43 Ir2 124.73(16) . . ? C45 C44 C43 108.0 . . ? C45 C44 C49 126.0 . . ? C43 C44 C49 126.0 . . ? C45 C44 Ir2 69.52(17) . . ? C43 C44 Ir2 70.03(17) . . ? C49 C44 Ir2 126.02(15) . . ? C44 C45 C41 108.0 . . ? C44 C45 C50 126.0 . . ? C41 C45 C50 126.0 . . ? C44 C45 Ir2 72.94(18) . . ? C41 C45 Ir2 68.39(17) . . ? C50 C45 Ir2 124.24(16) . . ? C42' C41' C45' 108.0 . . ? C42' C41' C46' 126.0 . . ? C45' C41' C46' 126.0 . . ? C42' C41' Ir2 73.21(17) . . ? C45' C41' Ir2 67.77(17) . . ? C46' C41' Ir2 124.58(17) . . ? C41' C42' C43' 108.0 . . ? C41' C42' C47' 126.0 . . ? C43' C42' C47' 126.0 . . ? C41' C42' Ir2 68.88(17) . . ? C43' C42' Ir2 69.87(17) . . ? C47' C42' Ir2 126.83(15) . . ? C44' C43' C42' 108.0 . . ? C44' C43' C48' 126.0 . . ? C42' C43' C48' 126.0 . . ? C44' C43' Ir2 67.63(17) . . ? C42' C43' Ir2 72.41(18) . . ? C48' C43' Ir2 125.50(16) . . ? C43' C44' C45' 108.0 . . ? C43' C44' C49' 126.0 . . ? C45' C44' C49' 126.0 . . ? C43' C44' Ir2 73.67(18) . . ? C45' C44' Ir2 69.60(18) . . ? C49' C44' Ir2 122.40(17) . . ? C41' C45' C44' 108.0 . . ? C41' C45' C50' 126.0 . . ? C44' C45' C50' 126.0 . . ? C41' C45' Ir2 73.15(18) . . ? C44' C45' Ir2 70.73(18) . . ? C50' C45' Ir2 121.82(17) . . ? F3 C51 F1 105.9(12) . . ? F3 C51 F2 109.6(12) . . ? F1 C51 F2 104.3(9) . . ? F3 C51 S1 112.1(8) . . ? F1 C51 S1 111.8(10) . . ? F2 C51 S1 112.6(10) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.421 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.130