# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email gxjin@fudan.edu.cn _publ_author_name 'Guo-Xin Jin' # Attachment '- 2a.cif' data_mo_2a _database_code_depnum_ccdc_archive 'CCDC 888409' #TrackingRef '- 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C160 H172 F24 Ir8 N24 O26 S8' _chemical_formula_weight 5097.30 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 C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 27.431(2) _cell_length_b 17.7844(14) _cell_length_c 20.7641(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.1960(10) _cell_angle_gamma 90.00 _cell_volume 9379.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8595 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.39 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 5.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5176 _exptl_absorpt_correction_T_max 0.7591 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.84 _diffrn_reflns_number 35364 _diffrn_reflns_av_R_equivalents 0.1387 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.53 _reflns_number_total 11142 _reflns_number_gt 7176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In asymmetric unit of this data, there was one disordered diethyl ether molecule which could not be restrained properly. Therefore, SQUEEZE algorithm was used to omit it. C35' and F7 were refined isotropically and other non-hydrogen atoms were refined anisotropically. 25 ISOR and 35 DFIX instructions were used to restrain the disordered anions and Cp* fragments so that there were 185 restraints in the data. There are several big residual density peaks in the structure but all of them are close to the heavy atoms. ; _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^)+(0.0915P)^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 11142 _refine_ls_number_parameters 756 _refine_ls_number_restraints 185 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 302.3 90.8 2 0.500 0.180 0.500 18.8 0.9 3 0.250 0.250 0.000 13.1 3.8 4 0.750 0.250 1.000 13.1 3.8 5 0.000 0.320 0.500 18.8 2.1 6 0.500 0.500 0.500 302.3 90.8 7 0.000 0.680 0.500 18.8 0.9 8 0.250 0.750 1.000 13.1 3.8 9 0.750 0.750 0.000 13.1 3.8 10 0.500 0.820 0.500 18.8 2.1 _platon_squeeze_details ; ; 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 0.904995(12) 0.803749(19) 0.88328(2) 0.04158(13) Uani 1 1 d . . . N1 N 0.9890(3) 0.7991(4) 0.9095(5) 0.042(2) Uani 1 1 d . . . N2 N 1.0673(3) 0.7985(4) 1.0058(5) 0.044(2) Uani 1 1 d . . . N3 N 0.9164(3) 0.9218(4) 0.8971(4) 0.0348(16) Uani 1 1 d . . . C1 C 1.0143(3) 0.7930(5) 0.9767(6) 0.044(3) Uani 1 1 d . . . C2 C 1.0307(4) 0.8071(5) 0.8852(6) 0.047(3) Uani 1 1 d . . . C3 C 1.0294(4) 0.8185(6) 0.8204(6) 0.052(3) Uani 1 1 d . . . H3 H 0.9970 0.8178 0.7814 0.062 Uiso 1 1 calc R . . C4 C 1.0767(5) 0.8313(7) 0.8121(8) 0.070(4) Uani 1 1 d . . . H4 H 1.0771 0.8390 0.7670 0.084 Uiso 1 1 calc R . . C5 C 1.1250(4) 0.8329(7) 0.8726(7) 0.070(4) Uani 1 1 d . . . H5 H 1.1570 0.8429 0.8664 0.084 Uiso 1 1 calc R . . C6 C 1.1269(4) 0.8205(6) 0.9391(7) 0.056(3) Uani 1 1 d . . . H6 H 1.1590 0.8204 0.9786 0.067 Uiso 1 1 calc R . . C7 C 1.0783(4) 0.8082(5) 0.9442(7) 0.054(3) Uani 1 1 d . . . C8 C 0.8945(3) 0.9607(5) 0.9352(5) 0.036(2) Uani 1 1 d . . . H8 H 0.8789 0.9343 0.9623 0.043 Uiso 1 1 calc R . . C9 C 0.9399(4) 0.9606(5) 0.8628(6) 0.046(2) Uani 1 1 d . . . H9 H 0.9572 0.9345 0.8375 0.055 Uiso 1 1 calc R . . C10 C 0.8296(4) 0.8135(7) 0.8000(8) 0.067(4) Uani 1 1 d . . . C11 C 0.8663(4) 0.7800(6) 0.7721(7) 0.065(4) Uani 1 1 d . . . C12 C 0.8829(4) 0.7103(6) 0.8133(9) 0.076(5) Uani 1 1 d . . . C13 C 0.8574(4) 0.7021(6) 0.8576(9) 0.074(4) Uani 1 1 d U . . C14 C 0.8227(4) 0.7681(8) 0.8487(9) 0.075(4) Uani 1 1 d . . . C15 C 0.8020(5) 0.8866(7) 0.7735(8) 0.083(5) Uani 1 1 d . . . H15A H 0.7649 0.8769 0.7452 0.125 Uiso 1 1 calc R . . H15B H 0.8186 0.9119 0.7450 0.125 Uiso 1 1 calc R . . H15C H 0.8046 0.9188 0.8129 0.125 Uiso 1 1 calc R . . C16 C 0.8788(6) 0.8045(8) 0.7141(8) 0.085(5) Uani 1 1 d . . . H16A H 0.8479 0.7982 0.6710 0.128 Uiso 1 1 calc R . . H16B H 0.9080 0.7743 0.7118 0.128 Uiso 1 1 calc R . . H16C H 0.8891 0.8576 0.7201 0.128 Uiso 1 1 calc R . . C17 C 0.9234(4) 0.6593(7) 0.7984(9) 0.084(5) Uani 1 1 d . . . H17A H 0.9355 0.6199 0.8339 0.126 Uiso 1 1 calc R . . H17B H 0.9535 0.6896 0.7994 0.126 Uiso 1 1 calc R . . H17C H 0.9067 0.6361 0.7524 0.126 Uiso 1 1 calc R . . C18 C 0.8610(5) 0.6400(8) 0.9078(10) 0.099(5) Uani 1 1 d U . . H18A H 0.8341 0.6020 0.8851 0.148 Uiso 1 1 calc R . . H18B H 0.8553 0.6605 0.9482 0.148 Uiso 1 1 calc R . . H18C H 0.8960 0.6170 0.9231 0.148 Uiso 1 1 calc R . . C19 C 0.7847(4) 0.7785(10) 0.8818(8) 0.090(5) Uani 1 1 d . . . H19A H 0.7790 0.8324 0.8861 0.136 Uiso 1 1 calc R . . H19B H 0.7983 0.7555 0.9281 0.136 Uiso 1 1 calc R . . H19C H 0.7512 0.7547 0.8533 0.136 Uiso 1 1 calc R . . Ir2 Ir 0.564955(15) 0.0000 0.72803(2) 0.02453(12) Uani 1 2 d S . . Ir3 Ir 0.351418(16) 0.0000 0.54998(2) 0.03245(14) Uani 1 2 d S . . N4 N 0.5005(2) 0.0778(4) 0.6785(4) 0.0318(16) Uani 1 1 d . . . N5 N 0.4138(2) 0.0775(4) 0.6077(4) 0.0323(16) Uani 1 1 d . . . N6 N 0.5754(3) 0.0000 0.6309(5) 0.0240(19) Uani 1 2 d S . . N7 N 0.6129(3) 0.0000 0.5250(5) 0.027(2) Uani 1 2 d S . . C20 C 0.4559(3) 0.0390(6) 0.6499(4) 0.034(2) Uani 1 1 d . . . C21 C 0.4867(3) 0.1499(5) 0.6534(5) 0.040(2) Uani 1 1 d . . . C22 C 0.5174(4) 0.2156(6) 0.6654(5) 0.046(2) Uani 1 1 d . . . H22 H 0.5532 0.2173 0.6967 0.055 Uiso 1 1 calc R . . C23 C 0.4903(4) 0.2801(7) 0.6264(7) 0.064(4) Uani 1 1 d . . . H23 H 0.5093 0.3256 0.6301 0.077 Uiso 1 1 calc R . . C24 C 0.4386(5) 0.2783(6) 0.5846(7) 0.064(4) Uani 1 1 d . . . H24 H 0.4224 0.3235 0.5624 0.076 Uiso 1 1 calc R . . C25 C 0.4092(4) 0.2158(6) 0.5730(6) 0.051(3) Uani 1 1 d . . . H25 H 0.3735 0.2159 0.5414 0.061 Uiso 1 1 calc R . . C26 C 0.4328(3) 0.1498(5) 0.6092(5) 0.039(2) Uani 1 1 d . . . C27 C 0.5840(3) -0.0639(5) 0.6020(5) 0.035(2) Uani 1 1 d . . . H27 H 0.5760 -0.1106 0.6179 0.043 Uiso 1 1 calc R . . C28 C 0.6037(3) -0.0641(5) 0.5513(4) 0.0342(19) Uani 1 1 d . . . H28 H 0.6110 -0.1106 0.5343 0.041 Uiso 1 1 calc R . . C29 C 0.5873(3) -0.0405(5) 0.8335(5) 0.0320(18) Uani 1 1 d . . . C30 C 0.6251(3) -0.0659(5) 0.8051(5) 0.037(2) Uani 1 1 d . . . C31 C 0.6481(4) 0.0000 0.7867(6) 0.037(3) Uani 1 2 d S . . C32 C 0.5553(4) -0.0903(6) 0.8593(5) 0.044(2) Uani 1 1 d . . . H32A H 0.5477 -0.1373 0.8327 0.066 Uiso 1 1 calc R . . H32B H 0.5222 -0.0651 0.8537 0.066 Uiso 1 1 calc R . . H32C H 0.5748 -0.1014 0.9086 0.066 Uiso 1 1 calc R . . C33 C 0.6426(4) -0.1441(6) 0.8035(6) 0.062(3) Uani 1 1 d . . . H33A H 0.6522 -0.1510 0.7630 0.092 Uiso 1 1 calc R . . H33B H 0.6139 -0.1786 0.8003 0.092 Uiso 1 1 calc R . . H33C H 0.6731 -0.1545 0.8461 0.092 Uiso 1 1 calc R . . C34 C 0.6907(5) 0.0000 0.7579(9) 0.065(5) Uani 1 2 d S . . H34A H 0.7252 0.0000 0.7963 0.098 Uiso 1 2 calc SR . . H34B H 0.6874 0.0450 0.7293 0.098 Uiso 0.50 1 calc PR . . H34C H 0.6874 -0.0450 0.7293 0.098 Uiso 0.50 1 calc PR . . C35 C 0.2932(15) 0.0000 0.5978(17) 0.028(9) Uani 0.46(2) 2 d SPDU . 1 C36 C 0.2877(14) 0.070(2) 0.5570(16) 0.058(10) Uani 0.46(2) 1 d PDU . 1 C37 C 0.2727(8) 0.0395(5) 0.4879(13) 0.040(6) Uani 0.46(2) 1 d PDU . 1 C38 C 0.306(2) 0.0000 0.6757(18) 0.111(18) Uani 0.46(2) 2 d SPDU . 1 H38A H 0.2733 0.0000 0.6842 0.167 Uiso 0.46(2) 2 calc SPR . 1 H38B H 0.3266 0.0450 0.6965 0.167 Uiso 0.229(12) 1 calc PR . 1 H38C H 0.3266 -0.0450 0.6965 0.167 Uiso 0.229(12) 1 calc PR . 1 C39 C 0.2867(15) 0.1472(16) 0.5798(15) 0.129(16) Uani 0.46(2) 1 d PDU . 1 H39A H 0.3027 0.1804 0.5557 0.194 Uiso 0.46(2) 1 calc PR . 1 H39B H 0.3065 0.1506 0.6301 0.194 Uiso 0.46(2) 1 calc PR . 1 H39C H 0.2502 0.1627 0.5691 0.194 Uiso 0.46(2) 1 calc PR . 1 C40 C 0.266(3) 0.0899(6) 0.4251(16) 0.28(5) Uani 0.46(2) 1 d PDU . 1 H40A H 0.2289 0.1037 0.4019 0.417 Uiso 0.46(2) 1 calc PR . 1 H40B H 0.2777 0.0626 0.3925 0.417 Uiso 0.46(2) 1 calc PR . 1 H40C H 0.2874 0.1354 0.4409 0.417 Uiso 0.46(2) 1 calc PR . 1 C35' C 0.2704(9) 0.0000 0.4721(12) 0.028(6) Uiso 0.54(2) 2 d SPD . 2 C36' C 0.2774(8) 0.0670(14) 0.5125(15) 0.050(6) Uani 0.54(2) 1 d PU . 2 C37' C 0.2914(8) 0.0406(14) 0.5851(12) 0.043(7) Uani 0.54(2) 1 d PD . 2 C38' C 0.248(2) 0.0000 0.3922(14) 0.15(2) Uani 0.54(2) 2 d SPDU . 2 H38D H 0.2090 0.0000 0.3752 0.228 Uiso 0.54(2) 2 calc SPR . 2 H38E H 0.2596 -0.0450 0.3752 0.228 Uiso 0.271(12) 1 calc PR . 2 H38F H 0.2596 0.0450 0.3752 0.228 Uiso 0.271(12) 1 calc PR . 2 C39' C 0.2671(10) 0.1482(13) 0.4862(14) 0.116(12) Uani 0.54(2) 1 d PDU . 2 H39D H 0.2291 0.1576 0.4663 0.175 Uiso 0.54(2) 1 calc PR . 2 H39E H 0.2818 0.1562 0.4504 0.175 Uiso 0.54(2) 1 calc PR . 2 H39F H 0.2838 0.1829 0.5250 0.175 Uiso 0.54(2) 1 calc PR . 2 C40' C 0.2987(15) 0.096(2) 0.6446(14) 0.151(16) Uani 0.54(2) 1 d PDU . 2 H40D H 0.2641 0.1111 0.6440 0.227 Uiso 0.54(2) 1 calc PR . 2 H40E H 0.3174 0.1409 0.6385 0.227 Uiso 0.54(2) 1 calc PR . 2 H40F H 0.3191 0.0723 0.6891 0.227 Uiso 0.54(2) 1 calc PR . 2 S1 S 0.4739(3) 0.0316(4) 0.9763(4) 0.0433(18) Uani 0.25 1 d P . . O1 O 0.4572(4) 0.0000 0.9050(5) 0.072(3) Uani 0.50 2 d SP . . O2 O 0.4889(13) 0.1028(7) 0.989(3) 0.070(8) Uani 0.25 1 d P . . O3 O 0.4322(5) 0.0000 0.9991(6) 0.104(5) Uani 0.50 2 d SP . . C41 C 0.4739(3) 0.0316(4) 0.9763(4) 0.0433(18) Uani 0.25 1 d P . . F1 F 0.4572(4) 0.0000 0.9050(5) 0.072(3) Uani 0.50 2 d SP . . F2 F 0.4889(13) 0.1028(7) 0.989(3) 0.070(8) Uani 0.25 1 d P . . F3 F 0.4322(5) 0.0000 0.9991(6) 0.104(5) Uani 0.50 2 d SP . . S2 S 0.9226(4) 0.0000 0.6756(6) 0.066(2) Uani 0.50 2 d SP . . O4 O 0.8806(7) 0.0000 0.6988(13) 0.056(5) Uani 0.50 2 d SPU . . O5 O 0.9522(8) 0.0679(9) 0.6849(10) 0.077(5) Uani 0.50 1 d P . . C42 C 0.8858(16) 0.0000 0.580(3) 0.083(12) Uani 0.50 2 d SPU . . F4 F 0.8554(6) 0.0629(10) 0.5660(12) 0.108(7) Uani 0.50 1 d P . . F5 F 0.9157(13) 0.0000 0.5464(16) 0.137(12) Uani 0.50 2 d SP . . S3 S 0.8065(3) 0.7551(3) 0.3540(3) 0.059(2) Uani 0.560(12) 1 d PD A 3 O6 O 0.7577(6) 0.7690(10) 0.3116(10) 0.086(6) Uani 0.560(12) 1 d PDU A 3 O7 O 0.8390(9) 0.6905(11) 0.3505(18) 0.104(5) Uani 0.560(12) 1 d PD A 3 O8 O 0.8127(13) 0.750(2) 0.4273(11) 0.162(13) Uani 0.560(12) 1 d PDU A 3 C43 C 0.8458(9) 0.8255(11) 0.3598(14) 0.137(14) Uani 0.560(12) 1 d PDU A 3 F6 F 0.8241(10) 0.8922(13) 0.359(2) 0.24(2) Uani 0.560(12) 1 d PD A 3 F7 F 0.8929(12) 0.832(2) 0.4184(14) 0.249(17) Uiso 0.560(12) 1 d PD A 3 F8 F 0.8671(11) 0.8285(16) 0.3119(14) 0.190(12) Uani 0.560(12) 1 d PDU A 3 S3' S 0.8400(5) 0.7587(8) 0.3712(7) 0.112(5) Uani 0.440(12) 1 d PD A 4 O6' O 0.8976(7) 0.763(2) 0.3995(17) 0.155(14) Uani 0.440(12) 1 d PDU A 4 O7' O 0.8231(8) 0.7913(12) 0.4231(10) 0.077(7) Uani 0.440(12) 1 d PDU A 4 O8' O 0.8204(11) 0.6894(15) 0.339(2) 0.104(5) Uani 0.440(12) 1 d PDU A 4 C43' C 0.8151(15) 0.824(2) 0.302(2) 0.086(10) Uani 0.440(12) 1 d PU A 4 F6' F 0.8168(14) 0.8926(10) 0.3197(15) 0.24(3) Uani 0.440(12) 1 d PD A 4 F7' F 0.8253(8) 0.8119(10) 0.2508(8) 0.086(6) Uani 0.440(12) 1 d PD A 4 F8' F 0.7583(8) 0.8134(16) 0.2755(12) 0.171(16) Uani 0.440(12) 1 d PD A 4 C131 C 0.7313(11) 0.9646(17) 1.0160(18) 0.079(9) Uani 0.50 1 d P . . F9 F 0.6822(6) 0.9632(13) 0.9813(13) 0.141(10) Uani 0.50 1 d P . . F10 F 0.7486(7) 0.8978(11) 1.0402(14) 0.134(9) Uani 0.50 1 d P . . F11 F 0.7343(6) 1.0000 1.0710(8) 0.137(6) Uani 1 2 d SU . . O9 O 0.8235(5) 1.0000 1.0246(8) 0.086(4) Uani 1 2 d S . . O10 O 0.7659(8) 0.9546(15) 0.9141(11) 0.099(7) Uani 0.50 1 d PU . . O12 O 0.9376(5) 0.0000 0.1047(7) 0.083(4) Uani 1 2 d S . . S4 S 0.76992(17) 1.0000 0.9724(3) 0.0569(10) Uani 1 2 d S . . O11 O 0.7489(8) 1.0755(12) 0.9460(13) 0.093(7) Uani 0.50 1 d PU . . 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 0.01723(16) 0.0298(2) 0.0655(3) -0.00873(17) 0.00175(16) 0.00029(12) N1 0.024(4) 0.029(4) 0.066(6) -0.005(4) 0.006(4) 0.002(3) N2 0.024(4) 0.039(4) 0.069(6) -0.008(4) 0.016(4) 0.004(3) N3 0.033(4) 0.026(4) 0.043(5) -0.004(3) 0.011(3) -0.003(3) C1 0.023(4) 0.030(5) 0.068(8) -0.009(4) 0.004(4) 0.000(3) C2 0.029(5) 0.033(5) 0.077(8) -0.023(5) 0.018(5) 0.001(4) C3 0.030(5) 0.062(7) 0.054(7) -0.028(6) 0.004(4) 0.003(4) C4 0.074(8) 0.069(8) 0.082(10) -0.043(7) 0.047(7) -0.012(6) C5 0.035(5) 0.080(8) 0.096(10) -0.062(8) 0.024(6) -0.016(5) C6 0.025(4) 0.068(7) 0.071(8) -0.044(6) 0.013(5) -0.001(4) C7 0.025(4) 0.030(5) 0.094(9) -0.028(5) 0.008(5) 0.002(4) C8 0.043(5) 0.037(5) 0.035(5) 0.003(4) 0.024(4) -0.006(4) C9 0.041(5) 0.036(5) 0.068(7) -0.011(5) 0.028(5) -0.006(4) C10 0.022(5) 0.058(7) 0.081(9) -0.039(7) -0.025(5) 0.020(5) C11 0.031(5) 0.056(7) 0.069(8) -0.042(6) -0.027(5) 0.006(5) C12 0.032(5) 0.032(5) 0.155(15) -0.039(7) 0.025(7) -0.010(4) C13 0.034(5) 0.041(6) 0.146(12) -0.031(7) 0.034(7) -0.018(4) C14 0.024(5) 0.070(8) 0.105(12) -0.039(8) -0.005(6) -0.006(5) C15 0.066(8) 0.071(8) 0.084(10) -0.028(7) -0.004(7) 0.037(7) C16 0.077(10) 0.085(10) 0.063(9) -0.031(8) -0.007(8) 0.008(7) C17 0.038(6) 0.068(8) 0.127(13) -0.046(8) 0.009(7) 0.012(6) C18 0.065(8) 0.066(8) 0.172(14) -0.022(9) 0.053(9) -0.027(6) C19 0.011(4) 0.141(13) 0.103(12) -0.049(10) 0.003(6) -0.009(6) Ir2 0.0177(2) 0.0338(2) 0.0214(2) 0.000 0.00656(16) 0.000 Ir3 0.0169(2) 0.0556(3) 0.0249(3) 0.000 0.00786(18) 0.000 N4 0.019(3) 0.031(4) 0.038(4) -0.002(3) 0.004(3) 0.007(3) N5 0.018(3) 0.043(4) 0.027(4) -0.010(3) -0.001(3) 0.007(3) N6 0.020(4) 0.037(5) 0.014(4) 0.000 0.006(4) 0.000 N7 0.023(4) 0.031(5) 0.022(5) 0.000 0.003(4) 0.000 C20 0.013(3) 0.063(5) 0.024(5) -0.004(4) 0.003(3) 0.005(3) C21 0.032(4) 0.045(5) 0.039(5) -0.014(4) 0.009(4) 0.007(4) C22 0.036(5) 0.050(6) 0.036(5) -0.013(5) -0.004(4) 0.009(4) C23 0.047(6) 0.050(6) 0.074(9) -0.041(6) 0.001(6) 0.005(5) C24 0.064(7) 0.036(6) 0.068(8) -0.018(6) -0.001(6) 0.024(5) C25 0.036(5) 0.054(6) 0.046(6) -0.016(5) -0.005(4) 0.019(5) C26 0.030(4) 0.039(5) 0.042(6) -0.012(4) 0.006(4) 0.011(4) C27 0.033(4) 0.034(5) 0.036(5) 0.001(4) 0.009(4) -0.006(4) C28 0.043(5) 0.032(4) 0.026(5) -0.003(4) 0.010(4) -0.001(4) C29 0.028(4) 0.033(4) 0.027(4) 0.000(4) 0.001(3) -0.005(3) C30 0.022(4) 0.047(5) 0.028(5) -0.001(4) -0.006(3) 0.008(4) C31 0.020(5) 0.062(8) 0.021(6) 0.000 0.001(5) 0.000 C32 0.051(5) 0.040(5) 0.046(6) 0.010(4) 0.023(5) -0.011(4) C33 0.050(6) 0.046(6) 0.058(7) -0.020(5) -0.015(5) 0.022(5) C34 0.023(7) 0.132(16) 0.046(9) 0.000 0.019(6) 0.000 C35 0.026(11) 0.035(13) 0.027(12) 0.000 0.016(8) 0.000 C36 0.031(12) 0.073(18) 0.073(19) -0.002(15) 0.020(14) 0.019(12) C37 0.019(8) 0.053(11) 0.045(10) -0.005(8) 0.008(7) 0.008(8) C38 0.11(2) 0.16(3) 0.09(2) 0.000 0.064(19) 0.000 C39 0.085(18) 0.13(2) 0.18(3) -0.022(18) 0.058(17) -0.009(16) C40 0.28(5) 0.30(5) 0.28(5) 0.03(2) 0.12(3) 0.00(2) C36' 0.030(9) 0.054(11) 0.072(15) -0.036(11) 0.027(10) -0.013(8) C37' 0.019(9) 0.07(2) 0.045(15) -0.026(15) 0.016(11) -0.001(14) C38' 0.16(3) 0.21(3) 0.11(3) 0.000 0.07(2) 0.000 C39' 0.047(12) 0.117(18) 0.16(2) 0.040(16) 0.009(13) 0.015(12) C40' 0.13(2) 0.19(2) 0.15(2) -0.070(17) 0.072(17) 0.021(17) S1 0.047(4) 0.040(4) 0.043(5) -0.008(3) 0.018(4) 0.003(3) O1 0.057(6) 0.118(9) 0.026(5) 0.000 -0.002(5) 0.000 O2 0.09(3) 0.035(6) 0.08(3) -0.003(9) 0.03(2) 0.009(8) O3 0.071(8) 0.207(16) 0.055(7) 0.000 0.048(7) 0.000 C41 0.047(4) 0.040(4) 0.043(5) -0.008(3) 0.018(4) 0.003(3) F1 0.057(6) 0.118(9) 0.026(5) 0.000 -0.002(5) 0.000 F2 0.09(3) 0.035(6) 0.08(3) -0.003(9) 0.03(2) 0.009(8) F3 0.071(8) 0.207(16) 0.055(7) 0.000 0.048(7) 0.000 S2 0.064(5) 0.038(4) 0.079(7) 0.000 0.010(5) 0.000 O4 0.036(9) 0.033(9) 0.085(14) 0.000 0.007(9) 0.000 O5 0.098(13) 0.049(9) 0.088(14) -0.012(9) 0.041(11) -0.033(9) C42 0.060(16) 0.093(19) 0.09(2) 0.000 0.026(15) 0.000 F4 0.046(8) 0.084(11) 0.19(2) 0.050(12) 0.045(11) 0.000(7) F5 0.15(3) 0.21(4) 0.10(2) 0.000 0.09(2) 0.000 S3 0.055(4) 0.059(3) 0.064(4) -0.007(3) 0.023(3) 0.014(3) O6 0.087(11) 0.073(11) 0.065(11) -0.030(9) -0.006(9) 0.004(9) O7 0.109(11) 0.092(7) 0.134(9) -0.001(6) 0.071(9) 0.029(7) O8 0.168(19) 0.22(2) 0.126(18) 0.034(15) 0.091(15) 0.002(16) C43 0.11(2) 0.13(2) 0.15(2) -0.014(18) 0.025(16) -0.030(17) F6 0.16(3) 0.11(2) 0.51(7) -0.04(3) 0.19(4) -0.05(2) F8 0.194(18) 0.202(19) 0.22(2) 0.061(15) 0.136(16) -0.021(14) S3' 0.088(9) 0.139(11) 0.121(11) -0.019(8) 0.053(8) 0.005(8) O6' 0.121(18) 0.20(2) 0.16(2) -0.013(17) 0.076(16) 0.010(16) O7' 0.052(10) 0.089(13) 0.079(13) 0.048(11) 0.011(9) 0.024(10) O8' 0.109(11) 0.092(7) 0.134(9) -0.001(6) 0.071(9) 0.029(7) C43' 0.075(16) 0.110(19) 0.082(18) -0.015(15) 0.039(14) 0.020(14) F6' 0.43(8) 0.06(2) 0.36(6) 0.09(3) 0.28(6) 0.04(3) F7' 0.104(15) 0.107(15) 0.063(12) -0.007(10) 0.051(12) -0.015(11) F8' 0.25(4) 0.17(3) 0.15(3) -0.08(2) 0.14(3) -0.07(3) C131 0.069(17) 0.10(2) 0.09(2) 0.040(16) 0.056(17) 0.017(13) F9 0.043(8) 0.19(2) 0.19(2) 0.048(16) 0.050(12) 0.005(10) F10 0.070(11) 0.097(13) 0.20(2) 0.082(15) 0.012(13) 0.008(10) F11 0.118(11) 0.240(16) 0.069(8) 0.000 0.052(8) 0.000 O9 0.059(8) 0.108(11) 0.093(11) 0.000 0.032(8) 0.000 O10 0.063(11) 0.152(16) 0.055(11) -0.007(11) -0.010(9) -0.018(10) O12 0.063(8) 0.096(10) 0.072(9) 0.000 0.004(7) 0.000 S4 0.055(2) 0.060(2) 0.062(3) 0.000 0.029(2) 0.000 O11 0.079(12) 0.087(12) 0.089(14) 0.039(11) 0.005(10) 0.000(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 N3 2.127(7) . ? Ir1 N2 2.137(10) 2_757 ? Ir1 C12 2.139(11) . ? Ir1 C10 2.143(9) . ? Ir1 N1 2.161(7) . ? Ir1 C13 2.175(10) . ? Ir1 C11 2.186(12) . ? Ir1 C14 2.189(11) . ? N1 C1 1.307(14) . ? N1 C2 1.422(13) . ? N2 C1 1.350(11) . ? N2 C7 1.432(16) . ? N2 Ir1 2.137(10) 2_757 ? N3 C9 1.321(12) . ? N3 C8 1.351(11) . ? C1 C1 1.46(2) 2_757 ? C2 C3 1.346(17) . ? C2 C7 1.412(15) . ? C3 C4 1.391(15) . ? C4 C5 1.441(18) . ? C5 C6 1.381(19) . ? C6 C7 1.394(14) . ? C8 C8 1.397(18) 6_575 ? C9 C9 1.400(19) 6_575 ? C10 C14 1.36(2) . ? C10 C11 1.463(18) . ? C10 C15 1.502(16) . ? C11 C16 1.44(2) . ? C11 C12 1.476(19) . ? C12 C13 1.36(2) . ? C12 C17 1.552(15) . ? C13 C14 1.479(17) . ? C13 C18 1.50(2) . ? C14 C19 1.46(2) . ? Ir2 N6 2.141(9) . ? Ir2 C31 2.141(11) . ? Ir2 C30 2.158(8) . ? Ir2 C30 2.159(8) 6 ? Ir2 C29 2.163(9) . ? Ir2 C29 2.163(9) 6 ? Ir2 N4 2.172(6) 6 ? Ir2 N4 2.172(6) . ? Ir3 N7 2.129(10) 5_656 ? Ir3 C37' 2.160(19) 6 ? Ir3 C37' 2.160(19) . ? Ir3 C37 2.17(2) 6 ? Ir3 C37 2.17(2) . ? Ir3 N5 2.171(7) 6 ? Ir3 N5 2.171(7) . ? Ir3 C35 2.18(4) . ? Ir3 C36 2.19(3) 6 ? Ir3 C36 2.19(3) . ? Ir3 C35' 2.20(2) . ? Ir3 C36' 2.23(2) 6 ? N4 C20 1.333(10) . ? N4 C21 1.383(12) . ? N5 C20 1.345(10) . ? N5 C26 1.383(12) . ? N6 C27 1.347(10) . ? N6 C27 1.347(10) 6 ? N7 C28 1.328(10) 6 ? N7 C28 1.328(10) . ? N7 Ir3 2.129(9) 5_656 ? C20 C20 1.39(2) 6 ? C21 C22 1.406(14) . ? C21 C26 1.415(12) . ? C22 C23 1.439(16) . ? C23 C24 1.354(15) . ? C24 C25 1.342(16) . ? C25 C26 1.413(14) . ? C27 C28 1.352(12) . ? C29 C29 1.442(17) 6 ? C29 C30 1.444(12) . ? C29 C32 1.482(12) . ? C30 C31 1.448(12) . ? C30 C33 1.476(13) . ? C31 C30 1.448(12) 6 ? C31 C34 1.502(17) . ? C35 C36 1.48(4) 6 ? C35 C36 1.48(4) . ? C35 C38 1.52(2) . ? C36 C37 1.44(3) . ? C36 C39 1.46(4) . ? C37 C37 1.405(19) 6 ? C37 C40 1.535(18) . ? C35' C36' 1.43(3) . ? C35' C36' 1.43(3) 6 ? C35' C38' 1.535(19) . ? C36' C37' 1.48(4) . ? C36' C39' 1.53(4) . ? C37' C37' 1.44(5) 6 ? C37' C40' 1.536(18) . ? S1 C41 1.125(16) 6 ? S1 S1 1.125(16) 6 ? S1 O2 1.326(16) . ? S1 C41 1.397(16) 2_657 ? S1 S1 1.397(16) 2_657 ? S1 O1 1.487(12) . ? S1 O3 1.502(12) . ? S1 F2 1.61(2) 2_657 ? S1 O2 1.61(2) 2_657 ? O1 C41 1.487(12) 6 ? O1 S1 1.487(12) 6 ? O2 F2 0.60(5) 2_657 ? O2 O2 0.60(5) 2_657 ? O2 S1 1.61(2) 2_657 ? O2 C41 1.61(2) 2_657 ? O3 C41 1.502(12) 6 ? O3 S1 1.502(12) 6 ? S2 O4 1.41(2) . ? S2 O5 1.428(15) . ? S2 O5 1.428(15) 6 ? S2 C42 1.85(5) . ? C42 F5 1.26(5) . ? C42 F4 1.36(3) 6 ? C42 F4 1.36(3) . ? S3 O6 1.317(14) . ? S3 O8 1.470(17) . ? S3 O7 1.473(16) . ? S3 C43 1.626(18) . ? C43 F6 1.323(18) . ? C43 F8 1.332(18) . ? C43 F7 1.407(18) . ? S3' O8' 1.409(16) . ? S3' O7' 1.446(15) . ? S3' O6' 1.466(16) . ? S3' C43' 1.78(4) . ? C43' F7' 1.22(4) . ? C43' F6' 1.26(4) . ? C43' F8' 1.46(4) . ? C131 C131 1.26(6) 6_575 ? C131 F9 1.26(3) . ? C131 F11 1.28(3) . ? C131 F10 1.31(3) . ? C131 S4 1.75(2) . ? C131 F9 1.80(3) 6_575 ? C131 O11 1.84(4) 6_575 ? F9 F9 1.31(4) 6_575 ? F9 C131 1.80(3) 6_575 ? F11 C131 1.28(3) 6_575 ? O9 S4 1.459(14) . ? O10 O11 1.09(3) 6_575 ? O10 S4 1.42(2) . ? O10 O10 1.61(5) 6_575 ? S4 O10 1.42(2) 6_575 ? S4 O11 1.48(2) 6_575 ? S4 O11 1.48(2) . ? S4 C131 1.75(2) 6_575 ? O11 O10 1.09(3) 6_575 ? O11 C131 1.84(4) 6_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ir1 N2 85.6(3) . 2_757 ? N3 Ir1 C12 148.0(5) . . ? N2 Ir1 C12 126.3(5) 2_757 . ? N3 Ir1 C10 94.5(4) . . ? N2 Ir1 C10 135.6(5) 2_757 . ? C12 Ir1 C10 64.9(4) . . ? N3 Ir1 N1 85.1(3) . . ? N2 Ir1 N1 79.3(3) 2_757 . ? C12 Ir1 N1 98.2(3) . . ? C10 Ir1 N1 145.0(5) . . ? N3 Ir1 C13 153.9(4) . . ? N2 Ir1 C13 99.4(5) 2_757 . ? C12 Ir1 C13 36.7(6) . . ? C10 Ir1 C13 64.1(5) . . ? N1 Ir1 C13 120.9(3) . . ? N3 Ir1 C11 108.8(4) . . ? N2 Ir1 C11 164.2(4) 2_757 . ? C12 Ir1 C11 39.9(5) . . ? C10 Ir1 C11 39.5(5) . . ? N1 Ir1 C11 107.8(4) . . ? C13 Ir1 C11 64.7(6) . . ? N3 Ir1 C14 114.3(4) . . ? N2 Ir1 C14 104.1(5) 2_757 . ? C12 Ir1 C14 63.9(5) . . ? C10 Ir1 C14 36.7(6) . . ? N1 Ir1 C14 160.3(4) . . ? C13 Ir1 C14 39.6(5) . . ? C11 Ir1 C14 64.5(6) . . ? C1 N1 C2 102.3(8) . . ? C1 N1 Ir1 111.0(7) . . ? C2 N1 Ir1 146.2(8) . . ? C1 N2 C7 99.4(9) . . ? C1 N2 Ir1 111.7(7) . 2_757 ? C7 N2 Ir1 148.1(6) . 2_757 ? C9 N3 C8 117.6(8) . . ? C9 N3 Ir1 121.4(6) . . ? C8 N3 Ir1 120.6(6) . . ? N1 C1 N2 121.3(10) . . ? N1 C1 C1 120.3(10) . 2_757 ? N2 C1 C1 117.5(12) . 2_757 ? C3 C2 C7 122.2(10) . . ? C3 C2 N1 130.4(10) . . ? C7 C2 N1 107.2(10) . . ? C2 C3 C4 118.3(10) . . ? C3 C4 C5 119.2(13) . . ? C6 C5 C4 122.9(10) . . ? C5 C6 C7 115.2(10) . . ? C6 C7 C2 122.2(12) . . ? C6 C7 N2 128.1(10) . . ? C2 C7 N2 109.7(9) . . ? N3 C8 C8 120.8(5) . 6_575 ? N3 C9 C9 121.5(5) . 6_575 ? C14 C10 C11 111.2(11) . . ? C14 C10 C15 126.4(13) . . ? C11 C10 C15 122.3(16) . . ? C14 C10 Ir1 73.5(7) . . ? C11 C10 Ir1 71.9(5) . . ? C15 C10 Ir1 124.4(8) . . ? C16 C11 C10 128.7(13) . . ? C16 C11 C12 128.3(12) . . ? C10 C11 C12 102.8(14) . . ? C16 C11 Ir1 130.6(9) . . ? C10 C11 Ir1 68.6(7) . . ? C12 C11 Ir1 68.3(7) . . ? C13 C12 C11 110.9(11) . . ? C13 C12 C17 131.5(13) . . ? C11 C12 C17 117.6(14) . . ? C13 C12 Ir1 73.1(8) . . ? C11 C12 Ir1 71.8(6) . . ? C17 C12 Ir1 123.3(8) . . ? C12 C13 C14 107.7(14) . . ? C12 C13 C18 129.6(11) . . ? C14 C13 C18 122.8(14) . . ? C12 C13 Ir1 70.2(6) . . ? C14 C13 Ir1 70.7(6) . . ? C18 C13 Ir1 124.5(11) . . ? C10 C14 C19 126.7(14) . . ? C10 C14 C13 107.3(13) . . ? C19 C14 C13 125.7(17) . . ? C10 C14 Ir1 69.8(7) . . ? C19 C14 Ir1 129.8(9) . . ? C13 C14 Ir1 69.7(6) . . ? N6 Ir2 C31 92.5(4) . . ? N6 Ir2 C30 111.2(3) . . ? C31 Ir2 C30 39.4(3) . . ? N6 Ir2 C30 111.2(3) . 6 ? C31 Ir2 C30 39.4(3) . 6 ? C30 Ir2 C30 65.7(5) . 6 ? N6 Ir2 C29 150.0(3) . . ? C31 Ir2 C29 65.8(4) . . ? C30 Ir2 C29 39.0(3) . . ? C30 Ir2 C29 65.5(3) 6 . ? N6 Ir2 C29 150.0(3) . 6 ? C31 Ir2 C29 65.8(4) . 6 ? C30 Ir2 C29 65.5(3) . 6 ? C30 Ir2 C29 39.0(3) 6 6 ? C29 Ir2 C29 39.0(5) . 6 ? N6 Ir2 N4 85.9(3) . 6 ? C31 Ir2 N4 140.38(18) . 6 ? C30 Ir2 N4 105.2(3) . 6 ? C30 Ir2 N4 162.5(3) 6 6 ? C29 Ir2 N4 97.8(3) . 6 ? C29 Ir2 N4 124.1(3) 6 6 ? N6 Ir2 N4 85.9(3) . . ? C31 Ir2 N4 140.38(18) . . ? C30 Ir2 N4 162.5(3) . . ? C30 Ir2 N4 105.2(3) 6 . ? C29 Ir2 N4 124.1(3) . . ? C29 Ir2 N4 97.8(3) 6 . ? N4 Ir2 N4 79.1(4) 6 . ? N7 Ir3 C37' 150.0(8) 5_656 6 ? N7 Ir3 C37' 150.0(7) 5_656 . ? C37' Ir3 C37' 39.1(14) 6 . ? N7 Ir3 C37 101.2(7) 5_656 6 ? C37' Ir3 C37 51.6(9) 6 6 ? C37' Ir3 C37 66.1(8) . 6 ? N7 Ir3 C37 101.2(7) 5_656 . ? C37' Ir3 C37 66.1(8) 6 . ? C37' Ir3 C37 51.6(9) . . ? C37 Ir3 C37 37.8(6) 6 . ? N7 Ir3 N5 85.4(3) 5_656 6 ? C37' Ir3 N5 98.2(6) 6 6 ? C37' Ir3 N5 124.6(7) . 6 ? C37 Ir3 N5 121.4(4) 6 6 ? C37 Ir3 N5 158.8(4) . 6 ? N7 Ir3 N5 85.4(3) 5_656 . ? C37' Ir3 N5 124.6(7) 6 . ? C37' Ir3 N5 98.2(6) . . ? C37 Ir3 N5 158.8(4) 6 . ? C37 Ir3 N5 121.4(4) . . ? N5 Ir3 N5 78.9(4) 6 . ? N7 Ir3 C35 162.4(10) 5_656 . ? C37' Ir3 C35 20.3(7) 6 . ? C37' Ir3 C35 20.3(7) . . ? C37 Ir3 C35 62.3(11) 6 . ? C37 Ir3 C35 62.3(11) . . ? N5 Ir3 C35 108.0(7) 6 . ? N5 Ir3 C35 108.0(7) . . ? N7 Ir3 C36 130.2(8) 5_656 6 ? C37' Ir3 C36 20.1(9) 6 6 ? C37' Ir3 C36 56.0(12) . 6 ? C37 Ir3 C36 38.5(9) 6 6 ? C37 Ir3 C36 65.5(11) . 6 ? N5 Ir3 C36 94.8(11) 6 6 ? N5 Ir3 C36 143.6(8) . 6 ? C35 Ir3 C36 39.6(9) . 6 ? N7 Ir3 C36 130.2(8) 5_656 . ? C37' Ir3 C36 56.0(12) 6 . ? C37' Ir3 C36 20.1(9) . . ? C37 Ir3 C36 65.5(11) 6 . ? C37 Ir3 C36 38.5(8) . . ? N5 Ir3 C36 143.6(8) 6 . ? N5 Ir3 C36 94.8(11) . . ? C35 Ir3 C36 39.6(9) . . ? C36 Ir3 C36 69(2) 6 . ? N7 Ir3 C35' 94.5(6) 5_656 . ? C37' Ir3 C35' 64.0(8) 6 . ? C37' Ir3 C35' 64.0(8) . . ? C37 Ir3 C35' 20.2(4) 6 . ? C37 Ir3 C35' 20.2(4) . . ? N5 Ir3 C35' 140.55(18) 6 . ? N5 Ir3 C35' 140.55(18) . . ? C35 Ir3 C35' 67.9(11) . . ? C36 Ir3 C35' 56.0(11) 6 . ? C36 Ir3 C35' 56.0(11) . . ? N7 Ir3 C36' 110.8(7) 5_656 6 ? C37' Ir3 C36' 39.5(10) 6 6 ? C37' Ir3 C36' 65.6(9) . 6 ? C37 Ir3 C36' 17.8(6) 6 6 ? C37 Ir3 C36' 52.7(6) . 6 ? N5 Ir3 C36' 106.1(6) 6 6 ? N5 Ir3 C36' 163.2(7) . 6 ? C35 Ir3 C36' 55.2(10) . 6 ? C36 Ir3 C36' 22.4(8) 6 6 ? C36 Ir3 C36' 71.5(11) . 6 ? C35' Ir3 C36' 37.6(6) . 6 ? C20 N4 C21 103.7(7) . . ? C20 N4 Ir2 109.1(5) . . ? C21 N4 Ir2 145.8(6) . . ? C20 N5 C26 103.5(7) . . ? C20 N5 Ir3 109.9(6) . . ? C26 N5 Ir3 144.6(6) . . ? C27 N6 C27 115.0(10) . 6 ? C27 N6 Ir2 121.9(5) . . ? C27 N6 Ir2 121.9(5) 6 . ? C28 N7 C28 118.1(10) 6 . ? C28 N7 Ir3 120.8(5) 6 5_656 ? C28 N7 Ir3 120.8(5) . 5_656 ? N4 C20 N5 116.5(8) . . ? N4 C20 C20 121.1(5) . 6 ? N5 C20 C20 120.6(5) . 6 ? N4 C21 C22 130.1(8) . . ? N4 C21 C26 108.2(8) . . ? C22 C21 C26 121.7(9) . . ? C21 C22 C23 114.5(9) . . ? C24 C23 C22 122.3(11) . . ? C25 C24 C23 123.3(11) . . ? C24 C25 C26 118.0(9) . . ? N5 C26 C25 131.7(8) . . ? N5 C26 C21 108.1(8) . . ? C25 C26 C21 120.0(9) . . ? N6 C27 C28 122.5(8) . . ? N7 C28 C27 120.8(8) . . ? C29 C29 C30 108.2(5) 6 . ? C29 C29 C32 126.6(5) 6 . ? C30 C29 C32 125.2(8) . . ? C29 C29 Ir2 70.5(2) 6 . ? C30 C29 Ir2 70.3(5) . . ? C32 C29 Ir2 125.8(6) . . ? C29 C30 C31 107.8(8) . . ? C29 C30 C33 126.3(10) . . ? C31 C30 C33 125.4(9) . . ? C29 C30 Ir2 70.6(5) . . ? C31 C30 Ir2 69.7(6) . . ? C33 C30 Ir2 131.2(7) . . ? C30 C31 C30 108.0(11) . 6 ? C30 C31 C34 125.9(5) . . ? C30 C31 C34 125.9(5) 6 . ? C30 C31 Ir2 71.0(5) . . ? C30 C31 Ir2 71.0(5) 6 . ? C34 C31 Ir2 126.5(10) . . ? C36 C35 C36 114(4) 6 . ? C36 C35 C38 122.8(19) 6 . ? C36 C35 C38 122.8(19) . . ? C36 C35 Ir3 71(2) 6 . ? C36 C35 Ir3 71(2) . . ? C38 C35 Ir3 125(3) . . ? C37 C36 C39 130(2) . . ? C37 C36 C35 101(3) . . ? C39 C36 C35 128(2) . . ? C37 C36 Ir3 69.8(16) . . ? C39 C36 Ir3 132(3) . . ? C35 C36 Ir3 69(2) . . ? C37 C37 C36 112.1(15) 6 . ? C37 C37 C40 125.7(7) 6 . ? C36 C37 C40 121.6(17) . . ? C37 C37 Ir3 71.1(3) 6 . ? C36 C37 Ir3 71.6(16) . . ? C40 C37 Ir3 118(3) . . ? C36' C35' C36' 113(3) . 6 ? C36' C35' C38' 123.0(15) . . ? C36' C35' C38' 123.0(15) 6 . ? C36' C35' Ir3 72.2(14) . . ? C36' C35' Ir3 72.2(14) 6 . ? C38' C35' Ir3 133(3) . . ? C35' C36' C37' 105(2) . . ? C35' C36' C39' 128(2) . . ? C37' C36' C39' 127(2) . . ? C35' C36' Ir3 70.2(13) . . ? C37' C36' Ir3 67.8(12) . . ? C39' C36' Ir3 130.5(16) . . ? C37' C37' C36' 108.4(12) 6 . ? C37' C37' C40' 130.1(17) 6 . ? C36' C37' C40' 121(2) . . ? C37' C37' Ir3 70.5(7) 6 . ? C36' C37' Ir3 72.7(11) . . ? C40' C37' Ir3 127.1(18) . . ? C41 S1 S1 0.0(15) 6 6 ? C41 S1 O2 162.6(11) 6 . ? S1 S1 O2 162.6(11) 6 . ? C41 S1 C41 89.999(2) 6 2_657 ? S1 S1 C41 89.999(2) 6 2_657 ? O2 S1 C41 72.6(11) . 2_657 ? C41 S1 S1 89.999(2) 6 2_657 ? S1 S1 S1 89.999(2) 6 2_657 ? O2 S1 S1 72.6(11) . 2_657 ? C41 S1 S1 0.0(11) 2_657 2_657 ? C41 S1 O1 67.8(3) 6 . ? S1 S1 O1 67.8(3) 6 . ? O2 S1 O1 121(3) . . ? C41 S1 O1 123.3(9) 2_657 . ? S1 S1 O1 123.3(9) 2_657 . ? C41 S1 O3 68.0(3) 6 . ? S1 S1 O3 68.0(3) 6 . ? O2 S1 O3 120(3) . . ? C41 S1 O3 118.6(9) 2_657 . ? S1 S1 O3 118.6(9) 2_657 . ? O1 S1 O3 100.8(8) . . ? C41 S1 F2 141.7(8) 6 2_657 ? S1 S1 F2 141.7(8) 6 2_657 ? O2 S1 F2 20.9(18) . 2_657 ? C41 S1 F2 51.7(8) 2_657 2_657 ? S1 S1 F2 51.7(8) 2_657 2_657 ? O1 S1 F2 130(2) . 2_657 ? O3 S1 F2 126(2) . 2_657 ? C41 S1 O2 141.7(8) 6 2_657 ? S1 S1 O2 141.7(8) 6 2_657 ? O2 S1 O2 20.9(18) . 2_657 ? C41 S1 O2 51.7(8) 2_657 2_657 ? S1 S1 O2 51.7(8) 2_657 2_657 ? O1 S1 O2 130(2) . 2_657 ? O3 S1 O2 126(2) . 2_657 ? F2 S1 O2 0(4) 2_657 2_657 ? S1 O1 C41 44.5(7) . 6 ? S1 O1 S1 44.5(7) . 6 ? C41 O1 S1 0.0(8) 6 6 ? F2 O2 O2 0(9) 2_657 2_657 ? F2 O2 S1 107.4(12) 2_657 . ? O2 O2 S1 107.4(12) 2_657 . ? F2 O2 S1 51.7(9) 2_657 2_657 ? O2 O2 S1 51.7(9) 2_657 2_657 ? S1 O2 S1 55.8(8) . 2_657 ? F2 O2 C41 51.7(9) 2_657 2_657 ? O2 O2 C41 51.7(9) 2_657 2_657 ? S1 O2 C41 55.8(8) . 2_657 ? S1 O2 C41 0.0(7) 2_657 2_657 ? C41 O3 S1 0.0(8) 6 6 ? C41 O3 S1 44.0(6) 6 . ? S1 O3 S1 44.0(6) 6 . ? O4 S2 O5 116.8(9) . . ? O4 S2 O5 116.8(9) . 6 ? O5 S2 O5 115.6(17) . 6 ? O4 S2 C42 100.4(17) . . ? O5 S2 C42 101.4(11) . . ? O5 S2 C42 101.4(11) 6 . ? F5 C42 F4 111(3) . 6 ? F5 C42 F4 111(3) . . ? F4 C42 F4 111(3) 6 . ? F5 C42 S2 113(3) . . ? F4 C42 S2 106(3) 6 . ? F4 C42 S2 106(3) . . ? O6 S3 O8 113.2(17) . . ? O6 S3 O7 126.4(15) . . ? O8 S3 O7 100(2) . . ? O6 S3 C43 112.6(11) . . ? O8 S3 C43 98.9(12) . . ? O7 S3 C43 102.0(12) . . ? F6 C43 F8 105.8(17) . . ? F6 C43 F7 101.3(17) . . ? F8 C43 F7 97.0(15) . . ? F6 C43 S3 114.1(18) . . ? F8 C43 S3 116.3(18) . . ? F7 C43 S3 120(2) . . ? O8' S3' O7' 122.4(16) . . ? O8' S3' O6' 113.3(15) . . ? O7' S3' O6' 106.3(13) . . ? O8' S3' C43' 103(2) . . ? O7' S3' C43' 101.8(15) . . ? O6' S3' C43' 109(2) . . ? F7' C43' F6' 116(4) . . ? F7' C43' F8' 102(3) . . ? F6' C43' F8' 99(3) . . ? F7' C43' S3' 116(3) . . ? F6' C43' S3' 116(3) . . ? F8' C43' S3' 104(3) . . ? C131 C131 F9 91.1(17) 6_575 . ? C131 C131 F11 60.5(12) 6_575 . ? F9 C131 F11 102(2) . . ? C131 C131 F10 155.3(19) 6_575 . ? F9 C131 F10 111(3) . . ? F11 C131 F10 102(2) . . ? C131 C131 S4 68.9(10) 6_575 . ? F9 C131 S4 116(2) . . ? F11 C131 S4 116(2) . . ? F10 C131 S4 108.8(19) . . ? C131 C131 F9 44.5(12) 6_575 6_575 ? F9 C131 F9 46.6(18) . 6_575 ? F11 C131 F9 78.0(17) . 6_575 ? F10 C131 F9 155(2) . 6_575 ? S4 C131 F9 92.5(14) . 6_575 ? C131 C131 O11 112.8(12) 6_575 6_575 ? F9 C131 O11 95(2) . 6_575 ? F11 C131 O11 161(2) . 6_575 ? F10 C131 O11 78(2) . 6_575 ? S4 C131 O11 48.7(10) . 6_575 ? F9 C131 O11 109.9(19) 6_575 6_575 ? C131 F9 F9 88.9(17) . 6_575 ? C131 F9 C131 44(2) . 6_575 ? F9 F9 C131 44.5(12) 6_575 6_575 ? C131 F11 C131 59(2) 6_575 . ? O11 O10 S4 70.9(18) 6_575 . ? O11 O10 O10 119.5(19) 6_575 6_575 ? S4 O10 O10 55.5(11) . 6_575 ? O10 S4 O10 69(2) . 6_575 ? O10 S4 O9 111.3(10) . . ? O10 S4 O9 111.3(10) 6_575 . ? O10 S4 O11 43.8(11) . 6_575 ? O10 S4 O11 107.7(16) 6_575 6_575 ? O9 S4 O11 114.7(8) . 6_575 ? O10 S4 O11 107.7(16) . . ? O10 S4 O11 43.8(11) 6_575 . ? O9 S4 O11 114.6(9) . . ? O11 S4 O11 129.8(18) 6_575 . ? O10 S4 C131 140.9(13) . 6_575 ? O10 S4 C131 111.6(15) 6_575 6_575 ? O9 S4 C131 104.7(12) . 6_575 ? O11 S4 C131 106.8(14) 6_575 6_575 ? O11 S4 C131 68.8(16) . 6_575 ? O10 S4 C131 111.6(16) . . ? O10 S4 C131 140.9(13) 6_575 . ? O9 S4 C131 104.7(12) . . ? O11 S4 C131 68.8(16) 6_575 . ? O11 S4 C131 106.8(14) . . ? C131 S4 C131 42(2) 6_575 . ? O10 O11 S4 65.3(19) 6_575 . ? O10 O11 C131 126(2) 6_575 6_575 ? S4 O11 C131 62.5(12) . 6_575 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.523 _refine_diff_density_min -2.563 _refine_diff_density_rms 0.276 # Attachment '- 2b.cif' data_mo_2b _database_code_depnum_ccdc_archive 'CCDC 888410' #TrackingRef '- 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95.60 H128.40 F12 N12 O18.60 Rh4 S4' _chemical_formula_weight 2511.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 13.3751(8) _cell_length_b 32.7892(18) _cell_length_c 14.0292(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.6330(10) _cell_angle_gamma 90.00 _cell_volume 5499.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9221 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.86 _exptl_crystal_description rhombid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2571 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9217 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.47 _diffrn_reflns_number 42053 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.95 _reflns_number_total 13354 _reflns_number_gt 9161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In asymmetric unit of this data, there was one disordered diethyl ether molecule which could not be restrained properly. Therefore, the SQUEEZE algorithm was used to omit it. One ISOR and four DFIX instructions were used to restain the methanol molecules so that there were 10 restraints in the data. ; _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^)+(0.0701P)^2^+5.5807P] 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 SHELXL _refine_ls_extinction_coef 0.00024(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13354 _refine_ls_number_parameters 656 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.260 0.750 0.283 25.2 -2.4 2 0.500 0.000 0.000 380.7 100.4 3 0.500 0.500 0.000 380.8 102.1 4 0.740 0.250 0.717 25.2 -2.2 _platon_squeeze_details ; ; 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 0.32249(2) 0.642583(9) 0.51110(2) 0.01859(9) Uani 1 1 d . . . Rh2 Rh 0.07449(2) 0.642656(9) 0.06728(2) 0.01751(9) Uani 1 1 d . . . S1 S 0.10379(15) 0.46836(5) 0.27509(12) 0.0569(4) Uani 1 1 d . . . S2 S 0.25356(13) 0.2500 0.30798(14) 0.0341(4) Uani 1 2 d S . . S3 S 0.70985(14) 0.2500 0.16716(13) 0.0334(4) Uani 1 2 d S . . N1 N 0.3457(3) 0.65532(11) 0.3696(3) 0.0214(7) Uani 1 1 d . . . N2 N 0.1504(3) 0.64390(10) 0.3903(3) 0.0210(7) Uani 1 1 d . . . N3 N 0.0488(3) 0.64377(10) 0.2090(2) 0.0188(6) Uani 1 1 d . . . N4 N 0.2447(3) 0.65444(10) 0.1880(3) 0.0212(7) Uani 1 1 d . . . N5 N 0.3166(3) 0.70746(10) 0.5232(3) 0.0226(7) Uani 1 1 d . . . N6 N 0.0590(3) 0.70745(10) 0.0564(2) 0.0189(7) Uani 1 1 d . . . O1 O 0.1163(4) 0.51082(13) 0.3006(3) 0.0732(14) Uani 1 1 d . . . O2 O 0.1768(5) 0.45135(17) 0.2385(4) 0.0939(17) Uani 1 1 d . . . O3 O -0.0113(5) 0.4563(2) 0.2128(5) 0.120(2) Uani 1 1 d . . . O4 O 0.1555(4) 0.2500 0.2081(4) 0.0413(12) Uani 1 2 d S . . O5 O 0.3197(3) 0.28683(12) 0.3330(3) 0.0550(10) Uani 1 1 d . . . O6 O 0.6472(4) 0.2500 0.2291(4) 0.0467(13) Uani 1 2 d S . . O7 O 0.7047(3) 0.28712(11) 0.1098(3) 0.0513(10) Uani 1 1 d . . . F1 F 0.0776(7) 0.4551(2) 0.4453(5) 0.147(3) Uani 1 1 d . . . F2 F 0.1486(7) 0.40399(16) 0.3924(5) 0.157(3) Uani 1 1 d . . . F3 F 0.2473(6) 0.45564(19) 0.4695(4) 0.142(3) Uani 1 1 d . . . F4 F 0.2831(4) 0.2500 0.5042(3) 0.0608(13) Uani 1 2 d S . . F5 F 0.1376(3) 0.28257(11) 0.3975(3) 0.0580(9) Uani 1 1 d . . . F6 F 0.9257(3) 0.2500 0.2275(3) 0.0433(10) Uani 1 2 d S . . F7 F 0.8780(2) 0.28296(9) 0.3325(2) 0.0478(7) Uani 1 1 d . . . C1 C 0.4171(3) 0.66619(12) 0.3256(3) 0.0207(8) Uani 1 1 d . . . C2 C 0.5294(4) 0.67882(14) 0.3749(4) 0.0322(10) Uani 1 1 d . . . H2 H 0.5716 0.6796 0.4503 0.039 Uiso 1 1 calc R . . C3 C 0.5754(4) 0.69017(15) 0.3073(4) 0.0352(11) Uani 1 1 d . . . H3 H 0.6515 0.6985 0.3377 0.042 Uiso 1 1 calc R . . C4 C 0.5136(4) 0.68967(16) 0.1960(4) 0.0372(11) Uani 1 1 d . . . H4 H 0.5485 0.6976 0.1530 0.045 Uiso 1 1 calc R . . C5 C 0.4022(4) 0.67776(14) 0.1476(3) 0.0290(9) Uani 1 1 d . . . H5 H 0.3602 0.6777 0.0722 0.035 Uiso 1 1 calc R . . C6 C 0.3541(3) 0.66602(13) 0.2126(3) 0.0248(9) Uani 1 1 d . . . C7 C 0.2495(3) 0.64991(12) 0.2844(3) 0.0188(8) Uani 1 1 d . . . C8 C 0.1486(3) 0.64454(12) 0.2953(3) 0.0186(7) Uani 1 1 d . . . C9 C 0.0380(3) 0.64219(13) 0.3672(3) 0.0234(8) Uani 1 1 d . . . C10 C -0.0153(4) 0.64191(14) 0.4334(4) 0.0302(9) Uani 1 1 d . . . H10 H 0.0263 0.6424 0.5088 0.036 Uiso 1 1 calc R . . C11 C -0.1308(4) 0.64088(15) 0.3845(4) 0.0338(10) Uani 1 1 d . . . H11 H -0.1693 0.6402 0.4272 0.041 Uiso 1 1 calc R . . C12 C -0.1921(4) 0.64077(15) 0.2737(4) 0.0348(10) Uani 1 1 d . . . H12 H -0.2715 0.6403 0.2427 0.042 Uiso 1 1 calc R . . C13 C -0.1409(3) 0.64130(12) 0.2091(3) 0.0215(8) Uani 1 1 d . . . H13 H -0.1842 0.6412 0.1338 0.026 Uiso 1 1 calc R . . C14 C -0.0252(3) 0.64204(12) 0.2535(3) 0.0203(8) Uani 1 1 d . . . C15 C 0.2240(3) 0.72927(12) 0.5020(3) 0.0223(8) Uani 1 1 d . . . H15 H 0.1562 0.7153 0.4865 0.027 Uiso 1 1 calc R . . C16 C 0.4097(3) 0.72901(13) 0.5466(3) 0.0252(9) Uani 1 1 d . . . H16 H 0.4777 0.7149 0.5637 0.030 Uiso 1 1 calc R . . C17 C -0.0111(3) 0.72908(12) 0.0815(3) 0.0230(8) Uani 1 1 d . . . H17 H -0.0622 0.7150 0.0998 0.028 Uiso 1 1 calc R . . C18 C 0.1256(3) 0.72902(12) 0.0259(3) 0.0242(8) Uani 1 1 d . . . H18 H 0.1738 0.7149 0.0039 0.029 Uiso 1 1 calc R . . C19 C 0.3037(4) 0.58519(13) 0.5775(3) 0.0273(9) Uani 1 1 d . . . C20 C 0.3878(4) 0.58185(13) 0.5419(3) 0.0274(9) Uani 1 1 d . . . C21 C 0.4761(3) 0.61008(13) 0.6042(3) 0.0267(9) Uani 1 1 d . . . C22 C 0.4441(4) 0.63167(13) 0.6744(3) 0.0276(9) Uani 1 1 d . . . C23 C 0.3359(4) 0.61714(13) 0.6571(3) 0.0267(9) Uani 1 1 d . . . C24 C 0.1992(4) 0.56011(14) 0.5397(4) 0.0398(11) Uani 1 1 d . . . H24A H 0.1731 0.5532 0.4643 0.060 Uiso 1 1 calc R . . H24B H 0.1412 0.5757 0.5482 0.060 Uiso 1 1 calc R . . H24C H 0.2150 0.5350 0.5818 0.060 Uiso 1 1 calc R . . C25 C 0.3876(5) 0.55234(16) 0.4605(4) 0.0445(13) Uani 1 1 d . . . H25A H 0.4307 0.5280 0.4965 0.067 Uiso 1 1 calc R . . H25B H 0.4215 0.5652 0.4189 0.067 Uiso 1 1 calc R . . H25C H 0.3105 0.5445 0.4128 0.067 Uiso 1 1 calc R . . C26 C 0.5842(4) 0.61422(16) 0.5976(4) 0.0358(11) Uani 1 1 d . . . H26A H 0.6113 0.6423 0.6144 0.054 Uiso 1 1 calc R . . H26B H 0.5725 0.6074 0.5253 0.054 Uiso 1 1 calc R . . H26C H 0.6397 0.5956 0.6487 0.054 Uiso 1 1 calc R . . C27 C 0.5115(4) 0.66297(15) 0.7553(3) 0.0334(10) Uani 1 1 d . . . H27A H 0.5467 0.6504 0.8261 0.050 Uiso 1 1 calc R . . H27B H 0.4625 0.6852 0.7550 0.050 Uiso 1 1 calc R . . H27C H 0.5695 0.6738 0.7376 0.050 Uiso 1 1 calc R . . C28 C 0.2762(4) 0.62846(16) 0.7206(4) 0.0375(11) Uani 1 1 d . . . H28A H 0.3003 0.6105 0.7828 0.056 Uiso 1 1 calc R . . H28B H 0.1954 0.6255 0.6765 0.056 Uiso 1 1 calc R . . H28C H 0.2935 0.6568 0.7444 0.056 Uiso 1 1 calc R . . C29 C 0.0903(4) 0.58108(12) 0.0272(3) 0.0262(9) Uani 1 1 d . . . C30 C -0.0231(3) 0.58759(13) 0.0065(3) 0.0255(9) Uani 1 1 d . . . C31 C -0.0675(4) 0.62035(13) -0.0696(3) 0.0322(10) Uani 1 1 d . . . C32 C 0.0174(4) 0.63142(14) -0.1010(3) 0.0326(10) Uani 1 1 d . . . C33 C 0.1140(4) 0.60811(13) -0.0414(3) 0.0295(10) Uani 1 1 d . . . C34 C 0.1696(4) 0.54966(15) 0.0995(4) 0.0444(13) Uani 1 1 d . . . H34A H 0.1537 0.5450 0.1604 0.067 Uiso 1 1 calc R . . H34B H 0.2466 0.5594 0.1253 0.067 Uiso 1 1 calc R . . H34C H 0.1602 0.5241 0.0602 0.067 Uiso 1 1 calc R . . C35 C -0.0838(4) 0.56420(15) 0.0561(4) 0.0413(12) Uani 1 1 d . . . H35A H -0.1160 0.5394 0.0146 0.062 Uiso 1 1 calc R . . H35B H -0.1438 0.5811 0.0569 0.062 Uiso 1 1 calc R . . H35C H -0.0314 0.5567 0.1293 0.062 Uiso 1 1 calc R . . C36 C -0.1830(4) 0.63638(18) -0.1166(4) 0.0508(15) Uani 1 1 d . . . H36A H -0.1833 0.6647 -0.1387 0.076 Uiso 1 1 calc R . . H36B H -0.2117 0.6351 -0.0635 0.076 Uiso 1 1 calc R . . H36C H -0.2306 0.6199 -0.1788 0.076 Uiso 1 1 calc R . . C37 C 0.0040(6) 0.66208(17) -0.1852(4) 0.0520(15) Uani 1 1 d . . . H37A H 0.0778 0.6701 -0.1773 0.078 Uiso 1 1 calc R . . H37B H -0.0352 0.6861 -0.1774 0.078 Uiso 1 1 calc R . . H37C H -0.0395 0.6500 -0.2558 0.078 Uiso 1 1 calc R . . C38 C 0.2213(5) 0.60805(17) -0.0516(5) 0.0494(14) Uani 1 1 d . . . H38A H 0.2158 0.5882 -0.1060 0.074 Uiso 1 1 calc R . . H38B H 0.2835 0.6006 0.0170 0.074 Uiso 1 1 calc R . . H38C H 0.2344 0.6353 -0.0724 0.074 Uiso 1 1 calc R . . C39 C 0.1410(11) 0.4449(2) 0.3993(8) 0.105(3) Uani 1 1 d . . . C40 C 0.1985(6) 0.2500 0.4062(5) 0.0375(16) Uani 1 2 d S . . C41 C 0.8543(6) 0.2500 0.2689(5) 0.0324(14) Uani 1 2 d S . . C42 C 0.3239(7) 0.2500 1.0632(7) 0.066(3) Uani 1 2 d S . . H42A H 0.3995 0.2500 1.1196 0.099 Uiso 1 2 d SR . . H42B H 0.2860 0.2739 1.0713 0.099 Uiso 0.50 1 d PR . . C43 C 0.3242(7) 0.2500 0.9582(7) 0.061(2) Uani 1 2 d S . . H43A H 0.3644 0.2744 0.9521 0.073 Uiso 0.50 1 calc PR . . H43B H 0.3644 0.2256 0.9521 0.073 Uiso 0.50 1 calc PR . . C44 C 0.2105(6) 0.2500 0.7724(6) 0.0431(17) Uani 1 2 d S . . H44A H 0.2494 0.2256 0.7642 0.052 Uiso 0.50 1 calc PR . . H44B H 0.2494 0.2744 0.7642 0.052 Uiso 0.50 1 calc PR . . C45 C 0.0923(6) 0.2500 0.6887(6) 0.0445(18) Uani 1 2 d S . . H45A H 0.0906 0.2500 0.6181 0.067 Uiso 1 2 calc SR . . H45B H 0.0543 0.2744 0.6964 0.067 Uiso 0.50 1 calc PR . . H45C H 0.0543 0.2256 0.6964 0.067 Uiso 0.50 1 calc PR . . O8 O 0.2146(4) 0.2500 0.8749(4) 0.0355(11) Uani 1 2 d S . . C46 C 0.4669(8) 0.3854(4) -0.0099(8) 0.129(4) Uani 1 1 d D . . H46A H 0.5021 0.4089 -0.0262 0.194 Uiso 1 1 calc R . . H46B H 0.4339 0.3675 -0.0724 0.194 Uiso 1 1 calc R . . H46C H 0.5234 0.3703 0.0505 0.194 Uiso 1 1 calc R . . O9 O 0.3827(7) 0.3991(3) 0.0163(8) 0.150(3) Uani 1 1 d D . . H9' H 0.419(6) 0.418(4) 0.072(9) 0.226 Uiso 1 1 d D . . C47 C 0.8537(16) 0.5293(5) 0.2928(16) 0.171(7) Uani 0.80 1 d PDU . . H47A H 0.8858 0.5209 0.3677 0.256 Uiso 0.80 1 calc PR . . H47B H 0.7906 0.5477 0.2771 0.256 Uiso 0.80 1 calc PR . . H47C H 0.9108 0.5433 0.2794 0.256 Uiso 0.80 1 calc PR . . O10 O 0.8176(13) 0.4960(4) 0.2296(13) 0.194(6) Uani 0.80 1 d PD . . H10' H 0.751(10) 0.499(3) 0.174(11) 0.233 Uiso 0.80 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 0.01945(16) 0.02134(16) 0.01435(15) 0.00051(12) 0.00701(12) 0.00020(12) Rh2 0.02021(16) 0.01800(16) 0.01418(15) -0.00063(11) 0.00758(12) -0.00078(12) S1 0.0846(12) 0.0470(9) 0.0433(8) -0.0088(6) 0.0325(8) -0.0058(8) S2 0.0226(8) 0.0379(9) 0.0397(9) 0.000 0.0122(7) 0.000 S3 0.0400(9) 0.0347(9) 0.0264(8) 0.000 0.0156(7) 0.000 N1 0.0193(16) 0.0296(18) 0.0189(16) -0.0018(13) 0.0118(14) -0.0023(14) N2 0.0204(16) 0.0284(18) 0.0171(16) 0.0004(14) 0.0110(13) -0.0033(14) N3 0.0170(15) 0.0244(17) 0.0161(15) -0.0008(13) 0.0082(13) -0.0010(13) N4 0.0188(16) 0.0273(18) 0.0175(16) -0.0006(13) 0.0083(13) -0.0023(13) N5 0.0217(17) 0.0253(18) 0.0171(16) 0.0012(13) 0.0052(14) 0.0001(14) N6 0.0228(16) 0.0183(16) 0.0147(15) -0.0017(12) 0.0076(13) -0.0017(13) O1 0.123(4) 0.043(2) 0.051(3) -0.006(2) 0.036(3) -0.016(2) O2 0.127(5) 0.096(4) 0.073(3) -0.007(3) 0.058(3) 0.028(4) O3 0.094(4) 0.108(5) 0.112(5) -0.070(4) 0.007(4) -0.008(4) O4 0.030(2) 0.062(3) 0.029(2) 0.000 0.011(2) 0.000 O5 0.038(2) 0.049(2) 0.067(3) 0.002(2) 0.0146(19) -0.0132(17) O6 0.040(3) 0.059(3) 0.046(3) 0.000 0.023(2) 0.000 O7 0.064(3) 0.044(2) 0.040(2) 0.0140(17) 0.0184(19) 0.0073(19) F1 0.231(8) 0.135(5) 0.136(5) -0.008(4) 0.137(6) -0.034(5) F2 0.287(9) 0.062(3) 0.125(5) 0.018(3) 0.096(6) -0.020(4) F3 0.200(7) 0.109(4) 0.070(3) -0.003(3) 0.016(4) 0.029(4) F4 0.049(3) 0.082(4) 0.029(2) 0.000 -0.003(2) 0.000 F5 0.058(2) 0.068(2) 0.0479(19) -0.0020(17) 0.0237(16) 0.0190(17) F6 0.046(2) 0.048(2) 0.051(3) 0.000 0.035(2) 0.000 F7 0.0504(18) 0.0480(18) 0.0419(17) -0.0162(14) 0.0178(14) -0.0059(14) C1 0.0188(19) 0.028(2) 0.0186(19) 0.0000(16) 0.0110(16) -0.0011(16) C2 0.027(2) 0.044(3) 0.024(2) -0.0042(19) 0.0089(18) -0.005(2) C3 0.021(2) 0.047(3) 0.036(3) -0.005(2) 0.0119(19) -0.008(2) C4 0.030(2) 0.056(3) 0.035(3) -0.001(2) 0.023(2) -0.010(2) C5 0.028(2) 0.039(3) 0.023(2) -0.0012(18) 0.0145(18) 0.0006(19) C6 0.021(2) 0.027(2) 0.024(2) 0.0000(17) 0.0084(17) 0.0005(17) C7 0.0178(18) 0.024(2) 0.0181(18) 0.0014(15) 0.0114(15) 0.0003(15) C8 0.0162(17) 0.0238(19) 0.0152(17) 0.0016(15) 0.0065(14) -0.0008(15) C9 0.0219(19) 0.027(2) 0.022(2) 0.0009(17) 0.0103(16) -0.0010(17) C10 0.027(2) 0.038(2) 0.026(2) 0.0017(19) 0.0128(18) -0.0007(19) C11 0.026(2) 0.045(3) 0.038(3) 0.003(2) 0.022(2) -0.002(2) C12 0.022(2) 0.044(3) 0.044(3) 0.001(2) 0.020(2) -0.003(2) C13 0.0127(17) 0.027(2) 0.025(2) -0.0013(17) 0.0087(15) -0.0014(16) C14 0.0190(18) 0.0218(19) 0.0240(19) 0.0007(16) 0.0131(16) -0.0003(16) C15 0.0209(19) 0.025(2) 0.025(2) 0.0000(16) 0.0138(17) -0.0026(16) C16 0.0179(19) 0.030(2) 0.028(2) -0.0008(17) 0.0105(17) 0.0000(16) C17 0.0200(19) 0.024(2) 0.028(2) 0.0021(16) 0.0129(17) -0.0023(16) C18 0.023(2) 0.029(2) 0.026(2) -0.0036(17) 0.0162(17) -0.0015(16) C19 0.037(2) 0.025(2) 0.022(2) 0.0048(16) 0.0151(19) 0.0022(18) C20 0.030(2) 0.025(2) 0.027(2) 0.0000(17) 0.0129(19) 0.0059(17) C21 0.024(2) 0.031(2) 0.022(2) 0.0049(17) 0.0082(17) 0.0080(17) C22 0.027(2) 0.029(2) 0.0162(19) 0.0034(16) 0.0008(17) 0.0005(17) C23 0.037(2) 0.022(2) 0.0137(18) 0.0042(15) 0.0052(17) 0.0011(18) C24 0.047(3) 0.024(2) 0.049(3) 0.001(2) 0.022(2) -0.008(2) C25 0.054(3) 0.036(3) 0.044(3) -0.012(2) 0.023(3) 0.009(2) C26 0.025(2) 0.046(3) 0.030(2) 0.003(2) 0.0078(19) 0.009(2) C27 0.034(2) 0.037(3) 0.020(2) -0.0018(19) 0.0042(19) -0.005(2) C28 0.048(3) 0.043(3) 0.025(2) 0.007(2) 0.020(2) 0.006(2) C29 0.035(2) 0.019(2) 0.025(2) -0.0052(16) 0.0137(18) -0.0004(17) C30 0.029(2) 0.023(2) 0.022(2) -0.0083(16) 0.0100(18) -0.0070(17) C31 0.035(2) 0.024(2) 0.023(2) -0.0040(17) 0.0010(19) -0.0018(19) C32 0.050(3) 0.026(2) 0.015(2) -0.0046(16) 0.008(2) -0.004(2) C33 0.046(3) 0.026(2) 0.023(2) -0.0100(17) 0.021(2) -0.0074(19) C34 0.047(3) 0.031(3) 0.051(3) 0.004(2) 0.018(3) 0.014(2) C35 0.053(3) 0.032(3) 0.052(3) -0.011(2) 0.035(3) -0.017(2) C36 0.030(3) 0.058(4) 0.038(3) -0.009(3) -0.007(2) 0.004(2) C37 0.086(4) 0.042(3) 0.027(3) 0.002(2) 0.025(3) -0.005(3) C38 0.064(4) 0.047(3) 0.060(4) -0.022(3) 0.048(3) -0.011(3) C39 0.179(11) 0.045(4) 0.093(7) -0.007(4) 0.063(8) -0.010(5) C40 0.032(4) 0.051(4) 0.024(3) 0.000 0.008(3) 0.000 C41 0.046(4) 0.028(3) 0.034(4) 0.000 0.028(3) 0.000 C42 0.044(5) 0.104(8) 0.042(5) 0.000 0.012(4) 0.000 C43 0.040(5) 0.088(7) 0.063(6) 0.000 0.031(4) 0.000 C44 0.045(4) 0.053(5) 0.043(4) 0.000 0.030(4) 0.000 C45 0.053(5) 0.042(4) 0.036(4) 0.000 0.017(4) 0.000 O8 0.028(2) 0.049(3) 0.036(3) 0.000 0.020(2) 0.000 C46 0.095(7) 0.228(14) 0.080(6) -0.011(8) 0.053(6) 0.023(8) O9 0.147(7) 0.161(8) 0.153(8) 0.023(6) 0.076(6) 0.024(6) C47 0.241(15) 0.133(12) 0.212(15) 0.021(11) 0.168(13) 0.026(11) O10 0.264(17) 0.114(9) 0.219(16) -0.025(9) 0.119(13) 0.008(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 Rh1 N5 2.138(3) . ? Rh1 C20 2.140(4) . ? Rh1 C23 2.144(4) . ? Rh1 C21 2.158(4) . ? Rh1 N2 2.162(3) . ? Rh1 C22 2.164(4) . ? Rh1 C19 2.164(4) . ? Rh1 N1 2.182(3) . ? Rh2 C29 2.132(4) . ? Rh2 N6 2.133(3) . ? Rh2 C31 2.136(4) . ? Rh2 C33 2.147(4) . ? Rh2 C32 2.163(4) . ? Rh2 N3 2.165(3) . ? Rh2 C30 2.166(4) . ? Rh2 N4 2.178(3) . ? S1 O2 1.406(5) . ? S1 O1 1.429(4) . ? S1 O3 1.444(6) . ? S1 C39 1.761(10) . ? S2 O4 1.427(5) . ? S2 O5 1.444(4) 4_565 ? S2 O5 1.444(4) . ? S2 C40 1.830(7) . ? S3 O7 1.443(4) 4_565 ? S3 O7 1.444(4) . ? S3 O6 1.452(5) . ? S3 C41 1.816(7) . ? N1 C7 1.319(5) . ? N1 C1 1.396(5) . ? N2 C8 1.323(5) . ? N2 C9 1.389(5) . ? N3 C8 1.341(5) . ? N3 C14 1.387(5) . ? N4 C7 1.333(5) . ? N4 C6 1.397(5) . ? N5 C16 1.338(5) . ? N5 C15 1.343(5) . ? N6 C17 1.343(5) . ? N6 C18 1.348(5) . ? F1 C39 1.318(12) . ? F2 C39 1.352(9) . ? F3 C39 1.364(12) . ? F4 C40 1.333(8) . ? F5 C40 1.315(5) . ? F6 C41 1.322(7) . ? F7 C41 1.346(5) . ? C1 C2 1.405(6) . ? C1 C6 1.422(6) . ? C2 C3 1.394(6) . ? C3 C4 1.400(7) . ? C4 C5 1.388(6) . ? C5 C6 1.385(6) . ? C7 C8 1.435(5) . ? C9 C10 1.403(6) . ? C9 C14 1.432(6) . ? C10 C11 1.381(6) . ? C11 C12 1.394(7) . ? C12 C13 1.360(6) . ? C13 C14 1.385(5) . ? C15 C15 1.359(8) 4_575 ? C16 C16 1.376(8) 4_575 ? C17 C17 1.372(8) 4_575 ? C18 C18 1.376(8) 4_575 ? C19 C20 1.425(6) . ? C19 C23 1.449(6) . ? C19 C24 1.498(6) . ? C20 C21 1.445(6) . ? C20 C25 1.496(6) . ? C21 C22 1.426(6) . ? C21 C26 1.496(6) . ? C22 C23 1.437(6) . ? C22 C27 1.495(6) . ? C23 C28 1.486(6) . ? C29 C30 1.427(6) . ? C29 C33 1.444(6) . ? C29 C34 1.500(6) . ? C30 C31 1.441(6) . ? C30 C35 1.497(6) . ? C31 C32 1.437(7) . ? C31 C36 1.478(7) . ? C32 C33 1.409(7) . ? C32 C37 1.499(7) . ? C33 C38 1.504(7) . ? C40 F5 1.315(5) 4_565 ? C41 F7 1.346(5) 4_565 ? C42 C43 1.475(12) . ? C43 O8 1.407(9) . ? C44 O8 1.414(8) . ? C44 C45 1.487(10) . ? C46 O9 1.407(11) . ? C47 O10 1.35(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 N5 Rh1 C20 159.41(15) . . ? N5 Rh1 C23 107.55(14) . . ? C20 Rh1 C23 65.98(16) . . ? N5 Rh1 C21 120.14(15) . . ? C20 Rh1 C21 39.30(16) . . ? C23 Rh1 C21 65.19(17) . . ? N5 Rh1 N2 88.75(12) . . ? C20 Rh1 N2 111.84(15) . . ? C23 Rh1 N2 111.11(15) . . ? C21 Rh1 N2 150.98(15) . . ? N5 Rh1 C22 96.73(14) . . ? C20 Rh1 C22 65.61(16) . . ? C23 Rh1 C22 38.97(17) . . ? C21 Rh1 C22 38.54(16) . . ? N2 Rh1 C22 149.75(15) . . ? N5 Rh1 C19 144.63(14) . . ? C20 Rh1 C19 38.68(16) . . ? C23 Rh1 C19 39.31(16) . . ? C21 Rh1 C19 64.72(17) . . ? N2 Rh1 C19 93.80(15) . . ? C22 Rh1 C19 65.01(16) . . ? N5 Rh1 N1 84.68(13) . . ? C20 Rh1 N1 98.63(15) . . ? C23 Rh1 N1 163.43(15) . . ? C21 Rh1 N1 99.19(14) . . ? N2 Rh1 N1 79.59(12) . . ? C22 Rh1 N1 130.45(15) . . ? C19 Rh1 N1 130.49(15) . . ? C29 Rh2 N6 160.41(15) . . ? C29 Rh2 C31 65.91(17) . . ? N6 Rh2 C31 104.95(15) . . ? C29 Rh2 C33 39.45(16) . . ? N6 Rh2 C33 121.41(15) . . ? C31 Rh2 C33 65.40(18) . . ? C29 Rh2 C32 65.09(17) . . ? N6 Rh2 C32 96.65(15) . . ? C31 Rh2 C32 39.06(19) . . ? C33 Rh2 C32 38.15(18) . . ? C29 Rh2 N3 109.50(14) . . ? N6 Rh2 N3 89.94(12) . . ? C31 Rh2 N3 112.85(16) . . ? C33 Rh2 N3 148.46(15) . . ? C32 Rh2 N3 151.89(16) . . ? C29 Rh2 C30 38.77(16) . . ? N6 Rh2 C30 141.24(14) . . ? C31 Rh2 C30 39.14(16) . . ? C33 Rh2 C30 64.99(16) . . ? C32 Rh2 C30 64.69(17) . . ? N3 Rh2 C30 93.45(14) . . ? C29 Rh2 N4 100.39(15) . . ? N6 Rh2 N4 85.02(12) . . ? C31 Rh2 N4 163.42(16) . . ? C33 Rh2 N4 98.15(15) . . ? C32 Rh2 N4 127.86(16) . . ? N3 Rh2 N4 79.83(12) . . ? C30 Rh2 N4 133.57(15) . . ? O2 S1 O1 117.1(4) . . ? O2 S1 O3 113.4(4) . . ? O1 S1 O3 113.1(3) . . ? O2 S1 C39 104.7(5) . . ? O1 S1 C39 103.2(3) . . ? O3 S1 C39 103.3(5) . . ? O4 S2 O5 115.56(19) . 4_565 ? O4 S2 O5 115.56(19) . . ? O5 S2 O5 113.5(3) 4_565 . ? O4 S2 C40 103.7(3) . . ? O5 S2 C40 103.1(2) 4_565 . ? O5 S2 C40 103.1(2) . . ? O7 S3 O7 115.0(3) 4_565 . ? O7 S3 O6 115.91(19) 4_565 . ? O7 S3 O6 115.92(19) . . ? O7 S3 C41 101.9(2) 4_565 . ? O7 S3 C41 101.9(2) . . ? O6 S3 C41 103.1(3) . . ? C7 N1 C1 102.5(3) . . ? C7 N1 Rh1 108.7(2) . . ? C1 N1 Rh1 148.9(3) . . ? C8 N2 C9 103.7(3) . . ? C8 N2 Rh1 108.7(2) . . ? C9 N2 Rh1 147.4(3) . . ? C8 N3 C14 102.6(3) . . ? C8 N3 Rh2 109.0(2) . . ? C14 N3 Rh2 148.3(3) . . ? C7 N4 C6 102.2(3) . . ? C7 N4 Rh2 109.1(2) . . ? C6 N4 Rh2 148.7(3) . . ? C16 N5 C15 115.9(4) . . ? C16 N5 Rh1 118.8(3) . . ? C15 N5 Rh1 125.1(3) . . ? C17 N6 C18 116.4(3) . . ? C17 N6 Rh2 124.3(3) . . ? C18 N6 Rh2 119.2(3) . . ? N1 C1 C2 130.5(4) . . ? N1 C1 C6 108.2(3) . . ? C2 C1 C6 121.2(4) . . ? C3 C2 C1 116.4(4) . . ? C2 C3 C4 122.3(4) . . ? C5 C4 C3 121.1(4) . . ? C6 C5 C4 118.0(4) . . ? C5 C6 N4 131.1(4) . . ? C5 C6 C1 121.0(4) . . ? N4 C6 C1 107.9(3) . . ? N1 C7 N4 119.2(3) . . ? N1 C7 C8 120.1(3) . . ? N4 C7 C8 120.1(3) . . ? N2 C8 N3 118.0(3) . . ? N2 C8 C7 121.1(3) . . ? N3 C8 C7 120.6(3) . . ? N2 C9 C10 131.6(4) . . ? N2 C9 C14 107.3(3) . . ? C10 C9 C14 121.1(4) . . ? C11 C10 C9 117.3(4) . . ? C10 C11 C12 121.4(4) . . ? C13 C12 C11 121.5(4) . . ? C12 C13 C14 119.7(4) . . ? C13 C14 N3 132.6(4) . . ? C13 C14 C9 119.0(4) . . ? N3 C14 C9 108.4(3) . . ? N5 C15 C15 122.2(2) . 4_575 ? N5 C16 C16 121.9(2) . 4_575 ? N6 C17 C17 121.9(2) . 4_575 ? N6 C18 C18 121.6(2) . 4_575 ? C20 C19 C23 108.5(4) . . ? C20 C19 C24 126.2(4) . . ? C23 C19 C24 125.3(4) . . ? C20 C19 Rh1 69.7(2) . . ? C23 C19 Rh1 69.6(2) . . ? C24 C19 Rh1 126.5(3) . . ? C19 C20 C21 107.4(4) . . ? C19 C20 C25 125.8(4) . . ? C21 C20 C25 126.7(4) . . ? C19 C20 Rh1 71.6(2) . . ? C21 C20 Rh1 71.0(2) . . ? C25 C20 Rh1 125.9(3) . . ? C22 C21 C20 108.6(4) . . ? C22 C21 C26 126.6(4) . . ? C20 C21 C26 124.8(4) . . ? C22 C21 Rh1 71.0(2) . . ? C20 C21 Rh1 69.7(2) . . ? C26 C21 Rh1 127.0(3) . . ? C21 C22 C23 108.1(4) . . ? C21 C22 C27 126.8(4) . . ? C23 C22 C27 125.1(4) . . ? C21 C22 Rh1 70.5(2) . . ? C23 C22 Rh1 69.7(2) . . ? C27 C22 Rh1 127.0(3) . . ? C22 C23 C19 107.4(4) . . ? C22 C23 C28 125.9(4) . . ? C19 C23 C28 126.1(4) . . ? C22 C23 Rh1 71.3(2) . . ? C19 C23 Rh1 71.1(2) . . ? C28 C23 Rh1 129.7(3) . . ? C30 C29 C33 107.7(4) . . ? C30 C29 C34 127.2(4) . . ? C33 C29 C34 124.9(4) . . ? C30 C29 Rh2 71.9(2) . . ? C33 C29 Rh2 70.9(2) . . ? C34 C29 Rh2 126.5(3) . . ? C29 C30 C31 108.1(4) . . ? C29 C30 C35 125.3(4) . . ? C31 C30 C35 126.6(4) . . ? C29 C30 Rh2 69.3(2) . . ? C31 C30 Rh2 69.3(2) . . ? C35 C30 Rh2 126.9(3) . . ? C32 C31 C30 107.2(4) . . ? C32 C31 C36 125.8(5) . . ? C30 C31 C36 126.7(5) . . ? C32 C31 Rh2 71.5(2) . . ? C30 C31 Rh2 71.6(2) . . ? C36 C31 Rh2 127.6(3) . . ? C33 C32 C31 108.8(4) . . ? C33 C32 C37 125.8(5) . . ? C31 C32 C37 125.4(5) . . ? C33 C32 Rh2 70.3(2) . . ? C31 C32 Rh2 69.4(2) . . ? C37 C32 Rh2 127.2(3) . . ? C32 C33 C29 108.2(4) . . ? C32 C33 C38 127.2(4) . . ? C29 C33 C38 124.5(4) . . ? C32 C33 Rh2 71.5(2) . . ? C29 C33 Rh2 69.7(2) . . ? C38 C33 Rh2 128.1(3) . . ? F1 C39 F2 111.9(9) . . ? F1 C39 F3 105.8(8) . . ? F2 C39 F3 102.7(9) . . ? F1 C39 S1 114.6(8) . . ? F2 C39 S1 111.1(7) . . ? F3 C39 S1 110.0(7) . . ? F5 C40 F5 108.6(6) 4_565 . ? F5 C40 F4 107.4(4) 4_565 . ? F5 C40 F4 107.4(4) . . ? F5 C40 S2 111.8(4) 4_565 . ? F5 C40 S2 111.8(4) . . ? F4 C40 S2 109.5(5) . . ? F6 C41 F7 106.9(4) . . ? F6 C41 F7 106.9(4) . 4_565 ? F7 C41 F7 106.8(5) . 4_565 ? F6 C41 S3 112.2(5) . . ? F7 C41 S3 111.9(3) . . ? F7 C41 S3 111.9(3) 4_565 . ? O8 C43 C42 111.2(7) . . ? O8 C44 C45 110.2(6) . . ? C43 O8 C44 113.3(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.954 _refine_diff_density_min -2.030 _refine_diff_density_rms 0.117 # Attachment '- 2c_1.cif' data_mo_2c _database_code_depnum_ccdc_archive 'CCDC 888411' #TrackingRef '- 2c_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H126 F12 Ir4 N12 O19 S4' _chemical_formula_weight 2949.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8163(8) _cell_length_b 25.5882(14) _cell_length_c 17.7677(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.4360(10) _cell_angle_gamma 90.00 _cell_volume 5460.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.39 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2908 _exptl_absorpt_coefficient_mu 5.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6078 _exptl_absorpt_correction_T_max 0.7524 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.02 _diffrn_reflns_number 40168 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20032 _reflns_number_gt 16621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In asymmetric unit of this data, there was disordered solvent molecules (one disordered diethyl ether and two methanol) which could not be restrained properly. Therefore, SQUEEZE algorithm was used to omit them. O7-9, F1-3, F10-12, C82, C82', C85', C88', C95, C96 and O16 were refined isotropically and other non- hydrogen atoms were refined anisotropically. 37 ISOR, 29 DFIX, 3 SIMU and 2 DELU instructions were used to restrain the disordered anions and Cp* fragments so that there were 265 restraints in the data. There are several big residual density peaks in the structure but all of them are close to the heavy atoms. ; _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^)+(0.0879P)^2^+7.3679P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(8) _refine_ls_number_reflns 20032 _refine_ls_number_parameters 1191 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.290 0.528 0.639 164.8 40.4 2 0.213 0.873 0.865 108.2 28.3 3 0.487 0.886 0.779 8.9 1.0 4 0.525 0.388 0.216 10.6 1.7 5 0.710 0.028 0.360 164.8 40.9 6 0.790 0.373 0.134 106.5 25.0 _platon_squeeze_details ; ; 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 0.22058(4) 0.364203(18) -0.03163(3) 0.02997(12) Uani 1 1 d . . . Ir2 Ir 0.16979(4) 0.14919(2) -0.09272(3) 0.03180(12) Uani 1 1 d . . . Ir3 Ir 0.31659(5) 0.26432(2) 0.59908(3) 0.04028(14) Uani 1 1 d . . . Ir4 Ir 0.28411(4) 0.04857(2) 0.54244(3) 0.03790(14) Uani 1 1 d . . . N1 N 0.0891(9) 0.3070(5) -0.0812(6) 0.035(3) Uani 1 1 d . . . N2 N 0.3169(9) 0.2975(5) -0.0448(7) 0.039(3) Uani 1 1 d . . . N3 N 0.2960(10) 0.2093(6) -0.0670(8) 0.044(3) Uani 1 1 d . . . N4 N 0.0684(8) 0.2193(4) -0.1032(5) 0.024(2) Uani 1 1 d . . . N5 N 0.4206(10) 0.1972(5) 0.6120(6) 0.038(3) Uani 1 1 d . A . N6 N 0.1949(9) 0.2019(5) 0.5747(7) 0.035(3) Uani 1 1 d . . . N7 N 0.1836(9) 0.1134(5) 0.5527(7) 0.034(2) Uani 1 1 d . A . N8 N 0.4100(8) 0.1072(5) 0.5925(6) 0.032(2) Uani 1 1 d . A . N9 N 0.2296(8) 0.3286(4) 0.0794(6) 0.031(2) Uani 1 1 d . . . N10 N 0.2890(8) 0.2601(5) 0.4756(5) 0.030(2) Uani 1 1 d . . . N11 N 0.1994(8) 0.1539(6) 0.0321(7) 0.042(3) Uani 1 1 d . . . N12 N 0.2665(10) 0.0842(6) 0.4310(6) 0.045(3) Uani 1 1 d . A . O1 O 0.8473(15) 0.1526(10) 0.0724(14) 0.134(7) Uani 1 1 d . . . O2 O 0.9508(17) 0.0630(9) 0.1269(18) 0.200(14) Uani 1 1 d . . . O3 O 0.793(2) 0.0642(10) 0.0064(18) 0.218(16) Uani 1 1 d . . . O4 O 0.6372(11) 0.2653(6) 0.4205(10) 0.088(4) Uani 1 1 d . . . O5 O 0.745(2) 0.3403(9) 0.4947(8) 0.168(11) Uani 1 1 d . . . O6 O 0.568(2) 0.3494(12) 0.3945(19) 0.210(12) Uani 1 1 d U . . O7 O 0.955(3) 0.9322(12) 0.8252(13) 0.267(16) Uiso 1 1 d DU . . O8 O 0.951(2) 0.9032(8) 0.6904(14) 0.195(11) Uiso 1 1 d D . . O9 O 0.994(2) 0.9912(8) 0.7307(15) 0.186(11) Uiso 1 1 d D . . O10 O 0.439(3) 0.9126(14) 0.187(2) 0.289(18) Uani 1 1 d DU . . O11 O 0.250(3) 0.9288(15) 0.0738(16) 0.268(18) Uiso 1 1 d D . . O12 O 0.3923(16) 0.9898(7) 0.1061(13) 0.146(8) Uani 1 1 d DU . . S1 S 0.8416(7) 0.0909(4) 0.0774(6) 0.130(3) Uani 1 1 d D . . S2 S 0.6569(4) 0.3186(2) 0.4269(3) 0.0708(13) Uani 1 1 d . . . S3 S 0.9490(9) 0.9438(5) 0.7461(7) 0.168(4) Uani 1 1 d DU . . S4 S 0.3547(10) 0.9482(4) 0.1397(9) 0.206(6) Uani 1 1 d DU . . F1 F 0.763(3) 0.1068(12) 0.2036(18) 0.289(16) Uiso 1 1 d D . . F2 F 0.654(3) 0.0901(18) 0.083(2) 0.52(4) Uiso 1 1 d D . . F3 F 0.759(3) 0.0316(9) 0.1526(17) 0.242(13) Uiso 1 1 d D . . F4 F 0.667(2) 0.3096(7) 0.2837(9) 0.160(8) Uani 1 1 d DU . . F5 F 0.7346(17) 0.3797(6) 0.3433(12) 0.152(6) Uani 1 1 d DU . . F6 F 0.8298(18) 0.3043(8) 0.3845(14) 0.169(7) Uani 1 1 d DU . . F7 F 0.7459(14) 0.9097(6) 0.6781(11) 0.130(6) Uani 1 1 d . . . F8 F 0.7582(10) 0.9901(5) 0.7188(7) 0.091(4) Uani 1 1 d . . . F9 F 0.8095(16) 0.9725(6) 0.6092(7) 0.146(6) Uani 1 1 d U . . F10 F 0.2507(12) 0.9300(7) 0.2382(8) 0.122(5) Uiso 1 1 d D . . F11 F 0.368(3) 0.9938(16) 0.2730(17) 0.34(2) Uiso 1 1 d D . . F12 F 0.2131(13) 1.0042(7) 0.1794(10) 0.129(6) Uiso 1 1 d D . . C1 C -0.0233(10) 0.2943(6) -0.0945(6) 0.030(3) Uani 1 1 d . . . C2 C -0.1108(10) 0.3253(6) -0.0897(8) 0.037(3) Uani 1 1 d . . . H2 H -0.1029 0.3615 -0.0773 0.045 Uiso 1 1 calc R . . C3 C -0.2094(15) 0.2986(8) -0.1044(13) 0.069(6) Uani 1 1 d . . . H3 H -0.2739 0.3184 -0.1085 0.083 Uiso 1 1 calc R . . C4 C -0.2205(13) 0.2456(8) -0.1134(14) 0.073(6) Uani 1 1 d . . . H4 H -0.2892 0.2295 -0.1178 0.088 Uiso 1 1 calc R . . C5 C -0.1327(12) 0.2151(7) -0.1162(9) 0.045(3) Uani 1 1 d . . . H5 H -0.1413 0.1785 -0.1253 0.054 Uiso 1 1 calc R . . C6 C -0.0345(9) 0.2388(5) -0.1058(6) 0.025(3) Uani 1 1 d . . . C7 C 0.1326(9) 0.2607(6) -0.0892(6) 0.030(3) Uani 1 1 d . . . C8 C 0.2483(10) 0.2570(6) -0.0708(8) 0.036(3) Uani 1 1 d . . . C9 C 0.4240(11) 0.2737(6) -0.0229(8) 0.038(3) Uani 1 1 d . . . C10 C 0.5263(10) 0.2981(7) 0.0103(10) 0.052(4) Uani 1 1 d . . . H10 H 0.5344 0.3344 0.0218 0.062 Uiso 1 1 calc R . . C11 C 0.6136(13) 0.2651(10) 0.0248(11) 0.071(5) Uani 1 1 d . . . H11 H 0.6858 0.2803 0.0425 0.086 Uiso 1 1 calc R . . C12 C 0.6075(13) 0.2085(8) 0.0157(13) 0.067(5) Uani 1 1 d . . . H12 H 0.6720 0.1870 0.0331 0.080 Uiso 1 1 calc R . . C13 C 0.5005(12) 0.1878(7) -0.0203(10) 0.053(4) Uani 1 1 d . . . H13 H 0.4917 0.1518 -0.0346 0.064 Uiso 1 1 calc R . . C14 C 0.4065(10) 0.2195(6) -0.0356(8) 0.036(3) Uani 1 1 d . . . C15 C 0.5271(11) 0.1771(6) 0.6163(7) 0.035(3) Uani 1 1 d . A . C16 C 0.6271(11) 0.2038(7) 0.6266(8) 0.051(4) Uani 1 1 d . . . H16 H 0.6349 0.2405 0.6355 0.061 Uiso 1 1 calc R . . C17 C 0.7147(12) 0.1720(10) 0.6225(11) 0.068(5) Uani 1 1 d U . . H17 H 0.7840 0.1882 0.6292 0.081 Uiso 1 1 calc R . . C18 C 0.7059(11) 0.1190(9) 0.6096(10) 0.062(5) Uani 1 1 d U . . H18 H 0.7674 0.1000 0.6056 0.074 Uiso 1 1 calc R . . C19 C 0.6079(11) 0.0935(6) 0.6023(7) 0.039(3) Uani 1 1 d . A . H19 H 0.6042 0.0565 0.5976 0.047 Uiso 1 1 calc R . . C20 C 0.5158(11) 0.1212(6) 0.6019(7) 0.037(3) Uani 1 1 d . . . C21 C 0.3619(9) 0.1518(7) 0.5981(7) 0.036(3) Uani 1 1 d . . . C22 C 0.2428(9) 0.1561(6) 0.5769(8) 0.034(3) Uani 1 1 d . A . C23 C 0.0795(11) 0.1886(6) 0.5423(10) 0.046(4) Uani 1 1 d . A . C24 C -0.0129(14) 0.2200(8) 0.5246(12) 0.063(5) Uani 1 1 d . . . H24 H -0.0091 0.2567 0.5329 0.076 Uiso 1 1 calc R . . C25 C -0.1113(14) 0.1931(10) 0.4939(13) 0.084(8) Uani 1 1 d . . . H25 H -0.1776 0.2131 0.4822 0.101 Uiso 1 1 calc R . . C26 C -0.1240(12) 0.1418(10) 0.4784(13) 0.082(8) Uani 1 1 d . . . H26 H -0.1961 0.1269 0.4552 0.098 Uiso 1 1 calc R . . C27 C -0.0319(13) 0.1116(9) 0.4965(12) 0.072(6) Uani 1 1 d . A . H27 H -0.0401 0.0749 0.4883 0.086 Uiso 1 1 calc R . . C28 C 0.0770(12) 0.1333(7) 0.5277(10) 0.053(4) Uani 1 1 d . . . C29 C 0.1421(13) 0.3275(7) 0.1009(8) 0.049(4) Uani 1 1 d . . . H29 H 0.0734 0.3414 0.0664 0.058 Uiso 1 1 calc R . . C30 C 0.1498(12) 0.3054(9) 0.1759(8) 0.059(5) Uani 1 1 d . . . H30 H 0.0832 0.3006 0.1872 0.071 Uiso 1 1 calc R . . C31 C 0.2453(12) 0.2914(6) 0.2308(8) 0.040(3) Uani 1 1 d . . . C32 C 0.3433(17) 0.2975(10) 0.2113(13) 0.090(7) Uani 1 1 d U . . H32 H 0.4158 0.2937 0.2503 0.108 Uiso 1 1 calc R . . C33 C 0.3264(13) 0.3093(9) 0.1321(11) 0.073(6) Uani 1 1 d U . . H33 H 0.3862 0.3036 0.1132 0.088 Uiso 1 1 calc R . . C34 C 0.3730(11) 0.2540(7) 0.4489(7) 0.046(4) Uani 1 1 d . . . H34 H 0.4435 0.2435 0.4857 0.055 Uiso 1 1 calc R . . C35 C 0.3615(11) 0.2627(8) 0.3675(7) 0.052(4) Uani 1 1 d . . . H35 H 0.4239 0.2582 0.3510 0.062 Uiso 1 1 calc R . . C36 C 0.2620(12) 0.2772(6) 0.3133(8) 0.039(3) Uani 1 1 d . . . C37 C 0.1728(13) 0.2787(8) 0.3429(9) 0.059(5) Uani 1 1 d . . . H37 H 0.0991 0.2854 0.3074 0.071 Uiso 1 1 calc R . . C38 C 0.1931(13) 0.2703(11) 0.4228(9) 0.077(7) Uani 1 1 d . . . H38 H 0.1315 0.2722 0.4407 0.093 Uiso 1 1 calc R . . C39 C 0.1168(10) 0.1620(6) 0.0646(8) 0.042(3) Uani 1 1 d . . . H39 H 0.0471 0.1749 0.0301 0.050 Uiso 1 1 calc R . . C40 C 0.1285(11) 0.1530(7) 0.1392(8) 0.047(3) Uani 1 1 d . . . H40 H 0.0680 0.1582 0.1576 0.057 Uiso 1 1 calc R . . C41 C 0.2325(12) 0.1354(6) 0.1924(8) 0.048(4) Uani 1 1 d . A . C42 C 0.3169(13) 0.1264(8) 0.1633(9) 0.064(5) Uani 1 1 d . . . H42 H 0.3868 0.1134 0.1975 0.077 Uiso 1 1 calc R . . C43 C 0.2982(13) 0.1366(7) 0.0824(10) 0.056(5) Uani 1 1 d . . . H43 H 0.3570 0.1312 0.0624 0.067 Uiso 1 1 calc R . . C44 C 0.3555(11) 0.0988(6) 0.4117(8) 0.046(4) Uani 1 1 d . . . H44 H 0.4266 0.0997 0.4531 0.056 Uiso 1 1 calc R A . C45 C 0.3482(13) 0.1123(8) 0.3356(9) 0.056(4) Uani 1 1 d . A . H45 H 0.4134 0.1153 0.3221 0.068 Uiso 1 1 calc R . . C46 C 0.2450(11) 0.1214(6) 0.2787(8) 0.040(3) Uani 1 1 d . . . C47 C 0.1552(14) 0.1091(8) 0.2987(9) 0.070(6) Uani 1 1 d . A . H47 H 0.0824 0.1137 0.2604 0.084 Uiso 1 1 calc R . . C48 C 0.1683(10) 0.0894(6) 0.3756(7) 0.044(3) Uani 1 1 d . . . H48 H 0.1041 0.0796 0.3873 0.052 Uiso 1 1 calc R A . C49 C 0.1706(7) 0.4277(3) -0.1186(4) 0.046(4) Uani 1 1 d G . . C50 C 0.1364(7) 0.4401(3) -0.0537(5) 0.063(5) Uani 1 1 d G . . C51 C 0.2320(8) 0.4441(3) 0.0156(5) 0.082(6) Uani 1 1 d GU . . C52 C 0.3253(7) 0.4342(3) -0.0065(5) 0.080(6) Uani 1 1 d GU . . C53 C 0.2873(7) 0.4241(3) -0.0894(5) 0.065(5) Uani 1 1 d GU . . C54 C 0.0960(10) 0.4198(5) -0.2036(6) 0.137(13) Uani 1 1 d G . . H54A H 0.1404 0.4205 -0.2387 0.206 Uiso 1 1 calc R . . H54B H 0.0403 0.4477 -0.2192 0.206 Uiso 1 1 calc R . . H54C H 0.0585 0.3859 -0.2087 0.206 Uiso 1 1 calc R . . C55 C 0.0191(10) 0.4476(5) -0.0577(8) 0.118(9) Uani 1 1 d GU . . H55A H 0.0173 0.4507 -0.0032 0.177 Uiso 1 1 calc R . . H55B H -0.0260 0.4176 -0.0847 0.177 Uiso 1 1 calc R . . H55C H -0.0112 0.4795 -0.0879 0.177 Uiso 1 1 calc R . . C56 C 0.2341(13) 0.4567(5) 0.0981(7) 0.120(8) Uani 1 1 d GU . . H56A H 0.1851 0.4865 0.0957 0.180 Uiso 1 1 calc R . . H56B H 0.3103 0.4654 0.1325 0.180 Uiso 1 1 calc R . . H56C H 0.2082 0.4264 0.1204 0.180 Uiso 1 1 calc R . . C57 C 0.4439(10) 0.4345(6) 0.0486(8) 0.137(10) Uani 1 1 d GU . . H57A H 0.4855 0.4607 0.0303 0.206 Uiso 1 1 calc R . . H57B H 0.4767 0.3999 0.0483 0.206 Uiso 1 1 calc R . . H57C H 0.4474 0.4429 0.1032 0.206 Uiso 1 1 calc R . . C58 C 0.3586(11) 0.4117(5) -0.1379(8) 0.100(7) Uani 1 1 d GU . . H58A H 0.3427 0.3761 -0.1592 0.150 Uiso 1 1 calc R . . H58B H 0.4372 0.4143 -0.1039 0.150 Uiso 1 1 calc R . . H58C H 0.3427 0.4365 -0.1826 0.150 Uiso 1 1 calc R . . C59 C 0.2108(10) 0.1095(5) -0.1862(8) 0.037(3) Uani 1 1 d . . . C60 C 0.2392(12) 0.0760(6) -0.1138(9) 0.046(3) Uani 1 1 d . . . C61 C 0.1330(15) 0.0669(6) -0.1035(11) 0.054(4) Uani 1 1 d . . . C62 C 0.0490(14) 0.0920(6) -0.1589(12) 0.060(5) Uani 1 1 d . . . C63 C 0.0901(11) 0.1188(5) -0.2153(8) 0.038(3) Uani 1 1 d . . . C64 C 0.2869(12) 0.1288(5) -0.2261(9) 0.045(4) Uani 1 1 d . . . H64A H 0.2981 0.1015 -0.2611 0.068 Uiso 1 1 calc R . . H64B H 0.3587 0.1381 -0.1853 0.068 Uiso 1 1 calc R . . H64C H 0.2545 0.1598 -0.2582 0.068 Uiso 1 1 calc R . . C65 C 0.3478(14) 0.0493(6) -0.0748(10) 0.058(4) Uani 1 1 d U . . H65A H 0.3494 0.0169 -0.1036 0.086 Uiso 1 1 calc R . . H65B H 0.3572 0.0412 -0.0189 0.086 Uiso 1 1 calc R . . H65C H 0.4083 0.0723 -0.0762 0.086 Uiso 1 1 calc R . . C66 C 0.1276(19) 0.0317(7) -0.0357(12) 0.077(6) Uani 1 1 d . . . H66A H 0.0522 0.0325 -0.0337 0.115 Uiso 1 1 calc R . . H66B H 0.1807 0.0441 0.0155 0.115 Uiso 1 1 calc R . . H66C H 0.1465 -0.0042 -0.0454 0.115 Uiso 1 1 calc R . . C67 C -0.0784(15) 0.0872(9) -0.1747(14) 0.091(7) Uani 1 1 d U . . H67A H -0.1112 0.0614 -0.2170 0.136 Uiso 1 1 calc R . . H67B H -0.1142 0.1212 -0.1917 0.136 Uiso 1 1 calc R . . H67C H -0.0897 0.0761 -0.1253 0.136 Uiso 1 1 calc R . . C68 C 0.0226(12) 0.1497(9) -0.2851(9) 0.068(5) Uani 1 1 d . . . H68A H 0.0571 0.1840 -0.2838 0.101 Uiso 1 1 calc R . . H68B H -0.0525 0.1542 -0.2834 0.101 Uiso 1 1 calc R . . H68C H 0.0181 0.1314 -0.3346 0.101 Uiso 1 1 calc R . . C69 C 0.2723(6) 0.3046(2) 0.6909(4) 0.054(4) Uani 1 1 d G . . C70 C 0.3913(6) 0.2990(2) 0.7167(4) 0.074(6) Uani 1 1 d G . . C71 C 0.4293(7) 0.3261(3) 0.6603(5) 0.079(6) Uani 1 1 d GU . . C72 C 0.3339(8) 0.3486(2) 0.5996(5) 0.089(8) Uani 1 1 d G . . C73 C 0.2369(7) 0.3353(2) 0.6185(4) 0.072(6) Uani 1 1 d G . . C74 C 0.1968(7) 0.2820(2) 0.7330(5) 0.049(4) Uani 1 1 d G . . H74A H 0.2053 0.3025 0.7814 0.074 Uiso 1 1 calc R . . H74B H 0.2176 0.2456 0.7479 0.074 Uiso 1 1 calc R . . H74C H 0.1192 0.2835 0.6966 0.074 Uiso 1 1 calc R . . C75 C 0.4644(7) 0.2693(3) 0.7910(4) 0.065(5) Uani 1 1 d GU . . H75A H 0.5195 0.2485 0.7774 0.097 Uiso 1 1 calc R . . H75B H 0.4178 0.2461 0.8099 0.097 Uiso 1 1 calc R . . H75C H 0.5028 0.2943 0.8335 0.097 Uiso 1 1 calc R . . C76 C 0.5500(7) 0.3304(3) 0.6641(7) 0.113(9) Uani 1 1 d GU . . H76A H 0.5787 0.3653 0.6829 0.170 Uiso 1 1 calc R . . H76B H 0.5534 0.3245 0.6105 0.170 Uiso 1 1 calc R . . H76C H 0.5953 0.3041 0.7014 0.170 Uiso 1 1 calc R . . C77 C 0.3354(11) 0.3809(3) 0.5277(6) 0.19(2) Uani 1 1 d G . . H77A H 0.3440 0.4180 0.5424 0.278 Uiso 1 1 calc R . . H77B H 0.2653 0.3757 0.4828 0.278 Uiso 1 1 calc R . . H77C H 0.3977 0.3697 0.5117 0.278 Uiso 1 1 calc R . . C78 C 0.1171(8) 0.3510(3) 0.5702(5) 0.098(7) Uani 1 1 d GU . . H78A H 0.0658 0.3312 0.5893 0.147 Uiso 1 1 calc R . . H78B H 0.1013 0.3434 0.5132 0.147 Uiso 1 1 calc R . . H78C H 0.1074 0.3885 0.5771 0.147 Uiso 1 1 calc R . . C79 C 0.3563(7) -0.0276(3) 0.5407(5) 0.067(7) Uani 0.823(16) 1 d PG A 1 C80 C 0.3646(7) -0.0161(3) 0.6214(4) 0.036(4) Uani 0.823(16) 1 d PG A 1 C81 C 0.2542(7) -0.0103(3) 0.6226(5) 0.060(6) Uani 0.823(16) 1 d PG A 1 C82 C 0.1776(7) -0.0183(3) 0.5428(5) 0.098(9) Uiso 0.823(16) 1 d PG A 1 C83 C 0.2407(8) -0.0290(3) 0.4921(5) 0.090(8) Uani 0.823(16) 1 d PGU A 1 C84 C 0.4532(9) -0.0368(3) 0.5117(6) 0.109(9) Uani 0.823(16) 1 d PGU A 1 H84A H 0.4806 -0.0726 0.5247 0.163 Uiso 0.823(16) 1 calc PR A 1 H84B H 0.5132 -0.0121 0.5383 0.163 Uiso 0.823(16) 1 calc PR A 1 H84C H 0.4283 -0.0316 0.4534 0.163 Uiso 0.823(16) 1 calc PR A 1 C85 C 0.4719(7) -0.0108(3) 0.6932(5) 0.082(8) Uani 0.823(16) 1 d PG A 1 H85A H 0.4965 -0.0455 0.7159 0.123 Uiso 0.823(16) 1 calc PR A 1 H85B H 0.4589 0.0114 0.7339 0.123 Uiso 0.823(16) 1 calc PR A 1 H85C H 0.5295 0.0050 0.6759 0.123 Uiso 0.823(16) 1 calc PR A 1 C86 C 0.2236(8) 0.0021(3) 0.6960(5) 0.087(7) Uani 0.823(16) 1 d PGU A 1 H86A H 0.2856 -0.0074 0.7448 0.130 Uiso 0.823(16) 1 calc PR A 1 H86B H 0.1572 -0.0178 0.6936 0.130 Uiso 0.823(16) 1 calc PR A 1 H86C H 0.2083 0.0396 0.6970 0.130 Uiso 0.823(16) 1 calc PR A 1 C87 C 0.0514(7) -0.0158(3) 0.5163(7) 0.165(17) Uani 0.823(16) 1 d PGU A 1 H87A H 0.0222 -0.0505 0.5217 0.247 Uiso 0.823(16) 1 calc PR A 1 H87B H 0.0206 -0.0046 0.4601 0.247 Uiso 0.823(16) 1 calc PR A 1 H87C H 0.0300 0.0092 0.5501 0.247 Uiso 0.823(16) 1 calc PR A 1 C88 C 0.1933(10) -0.0399(3) 0.4024(5) 0.31(4) Uani 0.823(16) 1 d PGU A 1 H88A H 0.1801 -0.0775 0.3935 0.466 Uiso 0.823(16) 1 calc PR A 1 H88B H 0.2463 -0.0282 0.3773 0.466 Uiso 0.823(16) 1 calc PR A 1 H88C H 0.1229 -0.0210 0.3785 0.466 Uiso 0.823(16) 1 calc PR A 1 C79' C 0.3049(8) -0.0320(3) 0.5040(5) 0.067(7) Uani 0.177(16) 1 d PG A 2 C80' C 0.3792(7) -0.0231(3) 0.5827(5) 0.13(7) Uani 0.177(16) 1 d PGU A 2 C81' C 0.3160(7) -0.0113(3) 0.6313(4) 0.030(17) Uani 0.177(16) 1 d PGU A 2 C82' C 0.2027(7) -0.0129(3) 0.5827(5) 0.030(16) Uiso 0.177(16) 1 d PG A 2 C83' C 0.1958(8) -0.0256(3) 0.5040(5) 0.098(9) Uiso 0.177(16) 1 d PG A 2 C84' C 0.3364(10) -0.0457(3) 0.4329(6) 0.06(2) Uani 0.177(16) 1 d PGU A 2 H84D H 0.3399 -0.0838 0.4286 0.089 Uiso 0.177(16) 1 calc PR A 2 H84E H 0.4094 -0.0306 0.4395 0.089 Uiso 0.177(16) 1 calc PR A 2 H84F H 0.2806 -0.0317 0.3840 0.089 Uiso 0.177(16) 1 calc PR A 2 C85' C 0.5035(7) -0.0258(3) 0.6098(6) 0.24(10) Uiso 0.177(16) 1 d PGU A 2 H85D H 0.5280 -0.0618 0.6251 0.360 Uiso 0.177(16) 1 calc PR A 2 H85E H 0.5358 -0.0027 0.6562 0.360 Uiso 0.177(16) 1 calc PR A 2 H85F H 0.5282 -0.0146 0.5660 0.360 Uiso 0.177(16) 1 calc PR A 2 C86' C 0.3614(8) 0.0008(3) 0.7192(4) 0.082(8) Uani 0.177(16) 1 d PG A 2 H86D H 0.3703 -0.0318 0.7499 0.123 Uiso 0.177(16) 1 calc PR A 2 H86E H 0.3098 0.0240 0.7328 0.123 Uiso 0.177(16) 1 calc PR A 2 H86F H 0.4339 0.0180 0.7324 0.123 Uiso 0.177(16) 1 calc PR A 2 C87' C 0.1064(7) -0.0027(3) 0.6099(7) 0.09(4) Uani 0.177(16) 1 d PGU A 2 H87D H 0.0813 -0.0358 0.6257 0.141 Uiso 0.177(16) 1 calc PR A 2 H87E H 0.0452 0.0130 0.5658 0.141 Uiso 0.177(16) 1 calc PR A 2 H87F H 0.1295 0.0212 0.6558 0.141 Uiso 0.177(16) 1 calc PR A 2 C88' C 0.0910(9) -0.0315(3) 0.4329(6) 0.06(2) Uiso 0.177(16) 1 d PG A 2 H88D H 0.0672 -0.0681 0.4277 0.096 Uiso 0.177(16) 1 calc PR A 2 H88E H 0.1045 -0.0206 0.3842 0.096 Uiso 0.177(16) 1 calc PR A 2 H88F H 0.0325 -0.0096 0.4402 0.096 Uiso 0.177(16) 1 calc PR A 2 C89 C 0.7575(19) 0.0827(9) 0.1351(14) 0.130(3) Uani 1 1 d D . . C90 C 0.723(2) 0.3270(8) 0.3578(14) 0.166(12) Uani 1 1 d DU . . C91 C 0.798(2) 0.9499(9) 0.6858(12) 0.083(6) Uani 1 1 d . . . C92 C 0.2959(17) 0.9697(7) 0.2070(12) 0.128(10) Uani 1 1 d DU . . C93 C 0.3926(18) 0.6085(9) 0.1890(11) 0.080(6) Uani 1 1 d . . . C94 C 0.9107(17) 0.3322(14) 0.6275(13) 0.097(7) Uani 1 1 d U . . C95 C 0.620(4) 0.1729(19) 0.262(3) 0.204(18) Uiso 1 1 d . . . C96 C 0.912(3) 0.2090(15) 0.290(2) 0.157(13) Uiso 1 1 d D . . O13 O 0.4254(12) 0.5811(7) 0.1298(9) 0.088(4) Uani 1 1 d . . . O14 O 0.8698(16) 0.3023(13) 0.6726(19) 0.224(17) Uani 1 1 d . . . O15 O 0.5402(15) 0.1893(8) 0.2943(15) 0.152(10) Uani 1 1 d . . . O16 O 0.933(3) 0.2161(17) 0.217(2) 0.259(18) Uiso 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 Ir1 0.0313(2) 0.0225(3) 0.0360(2) -0.00055(19) 0.01152(18) -0.0025(2) Ir2 0.0291(2) 0.0226(3) 0.0469(3) -0.0014(2) 0.0173(2) -0.0028(2) Ir3 0.0616(3) 0.0223(3) 0.0511(3) -0.0004(2) 0.0374(3) -0.0041(2) Ir4 0.0363(3) 0.0235(3) 0.0425(3) -0.0010(2) -0.00045(19) 0.0002(2) N1 0.031(5) 0.035(7) 0.038(5) 0.006(5) 0.011(4) 0.007(5) N2 0.032(6) 0.038(8) 0.050(7) 0.008(5) 0.019(5) -0.004(5) N3 0.039(6) 0.040(8) 0.057(7) -0.003(6) 0.022(5) -0.006(6) N4 0.017(4) 0.024(6) 0.028(4) 0.004(4) 0.005(3) 0.001(4) N5 0.042(6) 0.040(8) 0.032(5) -0.001(5) 0.013(4) -0.008(5) N6 0.029(5) 0.023(6) 0.058(6) 0.006(5) 0.021(5) 0.006(5) N7 0.027(5) 0.022(6) 0.054(6) 0.001(5) 0.015(5) 0.002(5) N8 0.026(5) 0.032(7) 0.030(5) -0.006(4) 0.002(4) -0.003(5) N9 0.034(5) 0.025(6) 0.030(5) 0.002(4) 0.006(4) 0.005(4) N10 0.034(5) 0.038(7) 0.021(4) 0.007(4) 0.014(4) 0.013(5) N11 0.019(4) 0.040(8) 0.061(7) 0.008(6) 0.007(4) 0.002(5) N12 0.040(6) 0.045(9) 0.038(6) -0.003(5) 0.000(5) 0.001(6) O1 0.106(13) 0.110(17) 0.180(19) 0.060(14) 0.042(13) 0.015(13) O2 0.105(14) 0.094(16) 0.29(3) 0.028(17) -0.078(16) -0.007(12) O3 0.17(2) 0.114(19) 0.27(3) -0.13(2) -0.05(2) 0.004(16) O4 0.061(8) 0.043(8) 0.148(13) 0.003(8) 0.022(7) 0.014(7) O5 0.29(3) 0.126(19) 0.036(7) 0.004(8) -0.003(11) -0.010(17) O6 0.195(17) 0.147(17) 0.27(2) -0.019(14) 0.054(14) 0.108(14) O10 0.27(2) 0.30(3) 0.33(2) 0.122(18) 0.147(18) 0.011(18) O12 0.129(12) 0.122(13) 0.203(15) 0.091(11) 0.077(11) -0.012(10) S1 0.127(6) 0.088(6) 0.145(6) -0.020(5) 0.009(5) 0.059(5) S2 0.065(3) 0.049(3) 0.087(3) -0.016(2) 0.013(2) -0.006(2) S3 0.179(8) 0.160(9) 0.188(9) -0.010(7) 0.093(7) 0.049(7) S4 0.194(9) 0.169(9) 0.343(13) 0.177(9) 0.206(10) 0.098(7) F4 0.29(3) 0.109(13) 0.096(10) -0.011(9) 0.085(13) -0.015(14) F5 0.205(11) 0.076(8) 0.178(10) 0.024(7) 0.071(8) -0.025(7) F6 0.166(13) 0.147(14) 0.219(15) 0.022(12) 0.099(12) 0.054(11) F7 0.128(12) 0.053(8) 0.218(18) -0.025(9) 0.071(12) -0.036(8) F8 0.098(9) 0.090(10) 0.089(8) -0.015(7) 0.037(6) 0.019(7) F9 0.250(15) 0.069(9) 0.075(7) 0.022(6) 0.001(9) 0.045(10) C1 0.021(5) 0.042(9) 0.024(5) 0.008(5) 0.003(4) -0.003(5) C2 0.024(6) 0.040(9) 0.052(7) 0.005(6) 0.018(5) 0.006(6) C3 0.054(10) 0.049(12) 0.124(16) 0.018(10) 0.055(11) 0.024(9) C4 0.028(8) 0.043(10) 0.152(18) 0.007(11) 0.036(9) -0.012(7) C5 0.038(7) 0.037(9) 0.057(8) 0.007(7) 0.012(6) 0.001(6) C6 0.015(5) 0.036(8) 0.025(5) 0.009(5) 0.008(4) 0.000(5) C7 0.026(5) 0.029(8) 0.034(5) 0.013(5) 0.008(4) 0.004(6) C8 0.032(6) 0.029(9) 0.055(7) 0.002(6) 0.026(5) 0.008(6) C9 0.031(6) 0.035(9) 0.045(7) -0.005(6) 0.009(5) 0.013(6) C10 0.023(7) 0.045(10) 0.089(11) -0.005(8) 0.021(7) -0.014(7) C11 0.037(8) 0.090(17) 0.085(12) -0.005(11) 0.018(7) -0.012(10) C12 0.036(8) 0.056(11) 0.117(15) 0.028(10) 0.037(9) 0.009(8) C13 0.031(7) 0.049(10) 0.085(11) 0.004(8) 0.025(7) -0.005(7) C14 0.027(6) 0.035(8) 0.049(7) 0.002(6) 0.017(5) -0.004(5) C15 0.032(6) 0.048(9) 0.023(5) 0.004(5) 0.006(4) -0.007(6) C16 0.029(7) 0.065(12) 0.041(7) 0.010(7) -0.008(5) -0.018(7) C17 0.020(7) 0.094(14) 0.076(10) 0.026(9) 0.000(6) 0.000(8) C18 0.011(6) 0.081(13) 0.077(10) 0.020(9) -0.005(6) 0.011(7) C19 0.038(7) 0.035(8) 0.036(6) 0.007(5) 0.003(5) 0.013(6) C20 0.033(7) 0.042(9) 0.035(6) 0.002(6) 0.012(5) 0.011(6) C21 0.027(5) 0.050(9) 0.035(6) -0.011(6) 0.015(5) -0.011(7) C22 0.026(5) 0.027(8) 0.054(7) -0.007(6) 0.018(5) -0.008(6) C23 0.025(6) 0.034(8) 0.085(10) 0.019(7) 0.025(6) 0.009(6) C24 0.050(9) 0.052(11) 0.108(13) 0.044(10) 0.054(9) 0.031(8) C25 0.035(9) 0.12(2) 0.109(15) 0.070(15) 0.042(9) 0.040(11) C26 0.023(7) 0.085(17) 0.126(16) 0.065(14) 0.014(8) 0.013(9) C27 0.040(9) 0.080(15) 0.092(13) 0.058(11) 0.019(9) 0.004(9) C28 0.026(7) 0.041(10) 0.083(11) 0.029(8) 0.008(6) -0.004(6) C29 0.051(8) 0.062(11) 0.032(6) 0.009(6) 0.013(6) 0.011(7) C30 0.033(7) 0.101(16) 0.042(8) 0.008(8) 0.012(6) 0.011(8) C31 0.041(7) 0.038(9) 0.039(7) 0.001(6) 0.011(5) 0.001(6) C32 0.061(10) 0.129(16) 0.091(12) 0.048(11) 0.042(9) 0.055(10) C33 0.036(7) 0.119(14) 0.076(10) 0.050(9) 0.034(7) 0.014(8) C34 0.037(7) 0.069(12) 0.035(6) 0.011(7) 0.017(5) 0.014(7) C35 0.034(6) 0.098(14) 0.030(6) 0.011(7) 0.019(5) 0.016(8) C36 0.047(8) 0.024(8) 0.056(8) 0.008(6) 0.030(6) 0.006(6) C37 0.044(8) 0.091(15) 0.048(8) 0.032(8) 0.024(7) 0.023(9) C38 0.040(8) 0.16(2) 0.043(8) 0.000(11) 0.024(7) 0.014(11) C39 0.031(6) 0.040(9) 0.049(7) 0.000(6) 0.006(5) 0.008(6) C40 0.045(7) 0.043(9) 0.048(7) -0.001(6) 0.009(6) 0.022(7) C41 0.039(7) 0.043(11) 0.038(7) 0.001(6) -0.016(5) 0.000(6) C42 0.035(8) 0.092(15) 0.041(8) 0.020(8) -0.016(6) 0.009(8) C43 0.039(7) 0.061(12) 0.075(10) 0.036(9) 0.029(7) 0.021(7) C44 0.031(6) 0.055(10) 0.042(7) -0.009(6) -0.001(5) -0.026(6) C45 0.040(8) 0.063(12) 0.052(8) 0.015(7) -0.002(6) -0.014(8) C46 0.032(7) 0.032(9) 0.046(7) 0.006(6) 0.002(5) -0.003(6) C47 0.051(9) 0.089(15) 0.044(8) 0.028(8) -0.016(7) -0.008(9) C48 0.024(6) 0.068(11) 0.029(6) 0.012(6) -0.004(4) 0.006(6) C49 0.083(11) 0.013(7) 0.038(6) 0.016(5) 0.016(7) 0.009(6) C50 0.087(12) 0.013(7) 0.128(15) 0.005(8) 0.086(12) -0.002(7) C51 0.133(14) 0.034(10) 0.066(10) -0.004(8) 0.019(10) -0.026(10) C52 0.089(12) 0.021(8) 0.103(12) 0.013(8) 0.000(9) -0.022(8) C53 0.078(10) 0.027(8) 0.125(13) 0.019(8) 0.080(10) 0.007(7) C54 0.22(3) 0.049(14) 0.081(15) 0.012(11) -0.032(17) -0.006(16) C55 0.114(14) 0.093(15) 0.186(18) 0.020(13) 0.102(14) 0.017(12) C56 0.217(19) 0.058(12) 0.086(12) -0.029(10) 0.053(13) -0.023(13) C57 0.124(12) 0.113(13) 0.150(13) 0.002(9) 0.015(9) -0.030(9) C58 0.117(14) 0.059(11) 0.164(16) 0.018(11) 0.098(13) -0.015(10) C59 0.035(6) 0.028(8) 0.059(8) -0.013(6) 0.031(6) -0.012(5) C60 0.051(8) 0.029(8) 0.074(9) 0.008(7) 0.044(7) 0.006(6) C61 0.066(10) 0.021(8) 0.102(12) -0.012(7) 0.064(9) -0.007(7) C62 0.057(9) 0.034(9) 0.112(14) -0.031(9) 0.058(10) -0.029(8) C63 0.042(7) 0.026(7) 0.048(7) -0.016(6) 0.016(6) -0.010(6) C64 0.045(8) 0.029(8) 0.078(10) 0.010(7) 0.042(7) 0.009(6) C65 0.075(9) 0.016(6) 0.097(10) 0.019(7) 0.050(8) 0.012(7) C66 0.131(17) 0.032(10) 0.110(14) 0.001(9) 0.096(14) -0.018(10) C67 0.063(9) 0.088(13) 0.141(14) -0.068(11) 0.060(10) -0.045(9) C68 0.038(7) 0.099(16) 0.058(9) -0.020(10) 0.007(7) -0.017(10) C69 0.079(11) 0.030(9) 0.067(9) 0.005(7) 0.042(9) 0.019(8) C70 0.067(11) 0.060(14) 0.114(15) -0.038(11) 0.056(11) -0.021(10) C71 0.114(13) 0.040(10) 0.114(13) -0.038(9) 0.079(11) -0.035(9) C72 0.16(2) 0.024(10) 0.133(19) 0.002(9) 0.118(19) -0.003(11) C73 0.139(18) 0.015(8) 0.089(12) -0.008(8) 0.072(13) 0.003(9) C74 0.061(9) 0.042(10) 0.052(8) 0.004(7) 0.029(7) -0.013(7) C75 0.066(9) 0.049(9) 0.069(9) -0.043(8) 0.012(7) -0.001(8) C76 0.115(15) 0.100(16) 0.145(16) -0.051(13) 0.071(13) -0.051(12) C77 0.40(6) 0.060(18) 0.21(3) -0.047(19) 0.25(4) -0.08(3) C78 0.150(16) 0.057(12) 0.102(12) 0.012(9) 0.064(12) 0.049(12) C79 0.12(2) 0.043(13) 0.052(14) 0.015(10) 0.044(13) 0.044(13) C80 0.037(8) 0.033(9) 0.035(8) 0.009(6) 0.010(6) 0.000(7) C81 0.073(15) 0.031(10) 0.102(17) -0.011(10) 0.063(14) 0.008(9) C83 0.139(16) 0.022(10) 0.061(11) -0.012(8) -0.025(11) -0.014(11) C84 0.125(13) 0.107(13) 0.108(12) -0.017(9) 0.059(9) 0.028(9) C85 0.083(15) 0.070(17) 0.057(12) 0.030(11) -0.020(10) 0.007(12) C86 0.095(11) 0.090(12) 0.101(11) 0.016(8) 0.066(9) -0.012(8) C87 0.14(2) 0.12(2) 0.22(2) 0.002(17) 0.047(17) -0.007(17) C88 0.31(4) 0.30(4) 0.31(4) -0.004(10) 0.100(17) 0.002(10) C79' 0.12(2) 0.043(13) 0.052(14) 0.015(10) 0.044(13) 0.044(13) C80' 0.13(7) 0.13(7) 0.14(7) -0.001(10) 0.05(3) 0.002(10) C81' 0.03(2) 0.03(2) 0.028(19) -0.004(10) 0.010(11) 0.002(10) C84' 0.06(2) 0.06(2) 0.06(2) 0.003(10) 0.026(12) 0.003(10) C86' 0.083(15) 0.070(17) 0.057(12) 0.030(11) -0.020(10) 0.007(12) C87' 0.10(4) 0.09(4) 0.09(4) 0.005(10) 0.034(17) -0.002(10) C89 0.127(6) 0.088(6) 0.145(6) -0.020(5) 0.009(5) 0.059(5) C90 0.23(2) 0.129(19) 0.133(14) 0.048(13) 0.058(15) -0.055(16) C91 0.110(17) 0.049(12) 0.077(12) 0.013(10) 0.015(11) 0.005(12) C92 0.141(17) 0.094(16) 0.133(16) 0.065(13) 0.030(13) -0.027(13) C93 0.084(14) 0.073(14) 0.069(11) -0.011(9) 0.010(10) 0.036(11) C94 0.060(10) 0.157(18) 0.082(12) 0.008(12) 0.034(9) 0.002(12) O13 0.085(9) 0.098(12) 0.088(9) -0.014(8) 0.038(8) -0.010(9) O14 0.067(12) 0.23(3) 0.31(3) 0.13(3) -0.024(16) -0.048(15) O15 0.108(13) 0.136(17) 0.27(3) -0.115(17) 0.142(16) -0.066(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 Ir1 N9 2.139(10) . ? Ir1 N2 2.167(13) . ? Ir1 N1 2.173(12) . ? Ir1 C49 2.178(7) . ? Ir1 C53 2.179(7) . ? Ir1 C50 2.188(8) . ? Ir1 C52 2.189(8) . ? Ir1 C51 2.195(8) . ? Ir2 N11 2.119(12) . ? Ir2 C61 2.151(14) . ? Ir2 C62 2.156(14) . ? Ir2 C60 2.161(14) . ? Ir2 N3 2.161(13) . ? Ir2 C59 2.162(12) . ? Ir2 N4 2.185(10) . ? Ir2 C63 2.200(12) . ? Ir3 N10 2.099(8) . ? Ir3 N5 2.137(13) . ? Ir3 C70 2.161(6) . ? Ir3 C71 2.162(7) . ? Ir3 C69 2.166(5) . ? Ir3 C72 2.167(6) . ? Ir3 N6 2.167(12) . ? Ir3 C73 2.169(7) . ? Ir4 N12 2.120(12) . ? Ir4 C81' 2.134(7) . ? Ir4 C82' 2.143(8) . ? Ir4 N7 2.148(11) . ? Ir4 N8 2.155(11) . ? Ir4 C79 2.162(8) . ? Ir4 C83 2.168(8) . ? Ir4 C80' 2.180(7) . ? Ir4 C80 2.181(7) . ? Ir4 C82 2.190(8) . ? Ir4 C83' 2.194(8) . ? Ir4 C81 2.197(7) . ? N1 C7 1.338(18) . ? N1 C1 1.414(16) . ? N2 C8 1.333(18) . ? N2 C9 1.426(17) . ? N3 C14 1.354(17) . ? N3 C8 1.356(19) . ? N4 C7 1.310(17) . ? N4 C6 1.396(14) . ? N5 C21 1.358(19) . ? N5 C15 1.436(18) . ? N6 C22 1.317(18) . ? N6 C23 1.428(18) . ? N7 C22 1.314(17) . ? N7 C28 1.378(18) . ? N8 C21 1.32(2) . ? N8 C20 1.355(17) . ? N9 C29 1.304(18) . ? N9 C33 1.360(18) . ? N10 C38 1.286(19) . ? N10 C34 1.329(15) . ? N11 C43 1.344(18) . ? N11 C39 1.386(17) . ? N12 C48 1.306(15) . ? N12 C44 1.354(18) . ? O1 S1 1.59(3) . ? O2 S1 1.54(2) . ? O3 S1 1.38(2) . ? O4 S2 1.385(16) . ? O5 S2 1.45(2) . ? O6 S2 1.34(2) . ? O7 S3 1.414(15) . ? O8 S3 1.441(15) . ? O9 S3 1.410(15) . ? O10 S4 1.439(18) . ? O11 S4 1.524(18) . ? O12 S4 1.387(13) . ? S1 C89 1.739(17) . ? S2 C90 1.73(3) . ? S3 C91 1.87(3) . ? S4 C92 1.71(2) . ? F1 C89 1.343(18) . ? F2 C89 1.343(19) . ? F3 C89 1.342(18) . ? F4 C90 1.338(18) . ? F5 C90 1.390(17) . ? F6 C90 1.407(19) . ? F7 C91 1.20(2) . ? F8 C91 1.37(2) . ? F9 C91 1.54(3) . ? F10 C92 1.378(16) . ? F11 C92 1.363(18) . ? F12 C92 1.337(17) . ? C1 C2 1.401(18) . ? C1 C6 1.433(18) . ? C2 C3 1.38(2) . ? C3 C4 1.37(3) . ? C4 C5 1.38(2) . ? C5 C6 1.350(18) . ? C7 C8 1.406(16) . ? C9 C10 1.384(19) . ? C9 C14 1.41(2) . ? C10 C11 1.35(2) . ? C11 C12 1.46(3) . ? C12 C13 1.40(2) . ? C13 C14 1.40(2) . ? C15 C16 1.407(19) . ? C15 C20 1.45(2) . ? C16 C17 1.41(3) . ? C17 C18 1.37(3) . ? C18 C19 1.38(2) . ? C19 C20 1.376(18) . ? C21 C22 1.442(15) . ? C23 C24 1.37(2) . ? C23 C28 1.44(2) . ? C24 C25 1.37(3) . ? C25 C26 1.34(3) . ? C26 C27 1.35(2) . ? C27 C28 1.42(2) . ? C29 C30 1.42(2) . ? C30 C31 1.32(2) . ? C31 C32 1.42(2) . ? C31 C36 1.453(18) . ? C32 C33 1.38(2) . ? C34 C35 1.418(16) . ? C35 C36 1.356(19) . ? C36 C37 1.415(19) . ? C37 C38 1.37(2) . ? C39 C40 1.302(19) . ? C40 C41 1.412(17) . ? C41 C42 1.37(2) . ? C41 C46 1.53(2) . ? C42 C43 1.40(2) . ? C44 C45 1.37(2) . ? C45 C46 1.376(19) . ? C46 C47 1.36(2) . ? C47 C48 1.41(2) . ? C49 C50 1.404(4) . ? C49 C53 1.405(4) . ? C49 C54 1.493(5) . ? C50 C51 1.405(4) . ? C50 C55 1.493(5) . ? C51 C52 1.405(4) . ? C51 C56 1.493(5) . ? C52 C53 1.405(4) . ? C52 C57 1.493(5) . ? C53 C58 1.493(5) . ? C59 C63 1.469(18) . ? C59 C64 1.476(16) . ? C59 C60 1.483(19) . ? C60 C61 1.455(19) . ? C60 C65 1.49(2) . ? C61 C62 1.34(3) . ? C61 C66 1.52(2) . ? C62 C63 1.46(2) . ? C62 C67 1.56(2) . ? C63 C68 1.47(2) . ? C69 C73 1.4373(14) . ? C69 C70 1.4376(14) . ? C69 C74 1.5281(15) . ? C70 C71 1.4374(14) . ? C70 C75 1.5282(15) . ? C71 C72 1.4374(14) . ? C71 C76 1.5279(16) . ? C72 C73 1.4378(14) . ? C72 C77 1.5279(15) . ? C73 C78 1.5282(15) . ? C79 C83 1.4304(14) . ? C79 C80 1.4305(14) . ? C79 C84 1.5206(15) . ? C80 C81 1.4307(14) . ? C80 C85 1.5207(15) . ? C81 C82 1.4307(14) . ? C81 C86 1.5204(15) . ? C82 C83 1.4305(14) . ? C82 C87 1.5208(15) . ? C83 C88 1.5208(15) . ? C79' C80' 1.4078(14) . ? C79' C83' 1.4079(14) . ? C79' C84' 1.4968(15) . ? C80' C81' 1.4077(14) . ? C80' C85' 1.4963(15) . ? C81' C82' 1.4078(14) . ? C81' C86' 1.4963(15) . ? C82' C83' 1.4074(14) . ? C82' C87' 1.4966(15) . ? C83' C88' 1.4966(15) . ? C93 O13 1.44(2) . ? C94 O14 1.34(3) . ? C95 O15 1.39(5) . ? C96 O16 1.440(19) . ? 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 N9 Ir1 N2 85.1(4) . . ? N9 Ir1 N1 82.6(4) . . ? N2 Ir1 N1 79.4(4) . . ? N9 Ir1 C49 151.6(4) . . ? N2 Ir1 C49 123.3(4) . . ? N1 Ir1 C49 102.7(4) . . ? N9 Ir1 C53 146.1(4) . . ? N2 Ir1 C53 99.9(4) . . ? N1 Ir1 C53 131.3(4) . . ? C49 Ir1 C53 37.62(14) . . ? N9 Ir1 C50 114.1(4) . . ? N2 Ir1 C50 160.6(4) . . ? N1 Ir1 C50 105.1(4) . . ? C49 Ir1 C50 37.52(15) . . ? C53 Ir1 C50 62.7(2) . . ? N9 Ir1 C52 109.2(4) . . ? N2 Ir1 C52 109.6(4) . . ? N1 Ir1 C52 165.3(4) . . ? C49 Ir1 C52 62.7(2) . . ? C53 Ir1 C52 37.52(15) . . ? C50 Ir1 C52 62.6(2) . . ? N9 Ir1 C51 94.0(4) . . ? N2 Ir1 C51 144.2(4) . . ? N1 Ir1 C51 136.1(4) . . ? C49 Ir1 C51 62.6(2) . . ? C53 Ir1 C51 62.6(2) . . ? C50 Ir1 C51 37.38(15) . . ? C52 Ir1 C51 37.37(15) . . ? N11 Ir2 C61 95.8(6) . . ? N11 Ir2 C62 116.2(6) . . ? C61 Ir2 C62 36.3(7) . . ? N11 Ir2 C60 107.2(5) . . ? C61 Ir2 C60 39.4(5) . . ? C62 Ir2 C60 65.1(6) . . ? N11 Ir2 N3 83.7(5) . . ? C61 Ir2 N3 147.1(6) . . ? C62 Ir2 N3 160.0(5) . . ? C60 Ir2 N3 109.3(5) . . ? N11 Ir2 C59 145.9(5) . . ? C61 Ir2 C59 65.0(5) . . ? C62 Ir2 C59 65.4(5) . . ? C60 Ir2 C59 40.1(5) . . ? N3 Ir2 C59 97.6(4) . . ? N11 Ir2 N4 85.8(4) . . ? C61 Ir2 N4 133.7(5) . . ? C62 Ir2 N4 102.6(5) . . ? C60 Ir2 N4 164.9(5) . . ? N3 Ir2 N4 79.2(5) . . ? C59 Ir2 N4 128.1(5) . . ? N11 Ir2 C63 155.3(5) . . ? C61 Ir2 C63 63.6(6) . . ? C62 Ir2 C63 39.1(6) . . ? C60 Ir2 C63 66.4(6) . . ? N3 Ir2 C63 121.0(5) . . ? C59 Ir2 C63 39.3(5) . . ? N4 Ir2 C63 98.6(4) . . ? N10 Ir3 N5 86.7(4) . . ? N10 Ir3 C70 152.5(4) . . ? N5 Ir3 C70 100.2(3) . . ? N10 Ir3 C71 113.7(4) . . ? N5 Ir3 C71 104.6(4) . . ? C70 Ir3 C71 38.84(10) . . ? N10 Ir3 C69 144.9(4) . . ? N5 Ir3 C69 128.3(3) . . ? C70 Ir3 C69 38.81(9) . . ? C71 Ir3 C69 65.02(15) . . ? N10 Ir3 C72 92.0(4) . . ? N5 Ir3 C72 137.7(4) . . ? C70 Ir3 C72 65.01(15) . . ? C71 Ir3 C72 38.78(9) . . ? C69 Ir3 C72 64.93(14) . . ? N10 Ir3 N6 84.7(4) . . ? N5 Ir3 N6 78.9(5) . . ? C70 Ir3 N6 122.7(3) . . ? C71 Ir3 N6 161.3(4) . . ? C69 Ir3 N6 98.2(3) . . ? C72 Ir3 N6 143.1(4) . . ? N10 Ir3 C73 107.0(4) . . ? N5 Ir3 C73 165.1(4) . . ? C70 Ir3 C73 64.97(14) . . ? C71 Ir3 C73 64.96(14) . . ? C69 Ir3 C73 38.72(9) . . ? C72 Ir3 C73 38.73(9) . . ? N6 Ir3 C73 107.6(3) . . ? N12 Ir4 C81' 158.5(4) . . ? N12 Ir4 C82' 136.2(4) . . ? C81' Ir4 C82' 38.43(11) . . ? N12 Ir4 N7 82.8(5) . . ? C81' Ir4 N7 117.2(4) . . ? C82' Ir4 N7 99.3(4) . . ? N12 Ir4 N8 84.6(4) . . ? C81' Ir4 N8 105.8(4) . . ? C82' Ir4 N8 139.0(4) . . ? N7 Ir4 N8 79.1(4) . . ? N12 Ir4 C79 106.4(4) . . ? C81' Ir4 C79 52.49(14) . . ? C82' Ir4 C79 66.67(18) . . ? N7 Ir4 C79 166.0(4) . . ? N8 Ir4 C79 111.8(4) . . ? N12 Ir4 C83 94.6(4) . . ? C81' Ir4 C83 66.63(18) . . ? C82' Ir4 C83 51.79(15) . . ? N7 Ir4 C83 131.9(4) . . ? N8 Ir4 C83 148.8(4) . . ? C79 Ir4 C83 38.58(11) . . ? N12 Ir4 C80' 122.3(4) . . ? C81' Ir4 C80' 38.06(10) . . ? C82' Ir4 C80' 63.57(17) . . ? N7 Ir4 C80' 154.9(4) . . ? N8 Ir4 C80' 101.5(4) . . ? C79 Ir4 C80' 18.80(5) . . ? C83 Ir4 C80' 53.03(14) . . ? N12 Ir4 C80 143.1(4) . . ? C81' Ir4 C80 19.01(5) . . ? C82' Ir4 C80 53.50(14) . . ? N7 Ir4 C80 134.0(4) . . ? N8 Ir4 C80 98.3(4) . . ? C79 Ir4 C80 38.46(11) . . ? C83 Ir4 C80 64.32(17) . . ? C80' Ir4 C80 20.98(6) . . ? N12 Ir4 C82 118.4(4) . . ? C81' Ir4 C82 52.84(15) . . ? C82' Ir4 C82 18.10(6) . . ? N7 Ir4 C82 102.2(4) . . ? N8 Ir4 C82 157.0(4) . . ? C79 Ir4 C82 64.26(17) . . ? C83 Ir4 C82 38.32(11) . . ? C80' Ir4 C82 67.62(18) . . ? C80 Ir4 C82 63.96(17) . . ? N12 Ir4 C83' 101.9(4) . . ? C81' Ir4 C83' 63.49(17) . . ? C82' Ir4 C83' 37.85(12) . . ? N7 Ir4 C83' 115.8(4) . . ? N8 Ir4 C83' 164.1(4) . . ? C79 Ir4 C83' 52.56(14) . . ? C83 Ir4 C83' 18.05(5) . . ? C80' Ir4 C83' 62.77(17) . . ? C80 Ir4 C83' 67.69(18) . . ? C82 Ir4 C83' 21.60(7) . . ? N12 Ir4 C81 156.2(4) . . ? C81' Ir4 C81 19.96(6) . . ? C82' Ir4 C81 20.80(6) . . ? N7 Ir4 C81 103.2(4) . . ? N8 Ir4 C81 119.0(4) . . ? C79 Ir4 C81 64.14(17) . . ? C83 Ir4 C81 64.05(17) . . ? C80' Ir4 C81 54.18(14) . . ? C80 Ir4 C81 38.15(10) . . ? C82 Ir4 C81 38.07(11) . . ? C83' Ir4 C81 54.59(16) . . ? C7 N1 C1 102.5(11) . . ? C7 N1 Ir1 110.3(8) . . ? C1 N1 Ir1 145.4(10) . . ? C8 N2 C9 102.6(12) . . ? C8 N2 Ir1 108.6(8) . . ? C9 N2 Ir1 146.8(10) . . ? C14 N3 C8 103.7(12) . . ? C14 N3 Ir2 145.2(11) . . ? C8 N3 Ir2 109.8(9) . . ? C7 N4 C6 103.9(11) . . ? C7 N4 Ir2 109.4(8) . . ? C6 N4 Ir2 145.4(9) . . ? C21 N5 C15 99.2(12) . . ? C21 N5 Ir3 112.5(9) . . ? C15 N5 Ir3 147.1(10) . . ? C22 N6 C23 101.9(12) . . ? C22 N6 Ir3 110.7(8) . . ? C23 N6 Ir3 145.8(10) . . ? C22 N7 C28 101.2(12) . . ? C22 N7 Ir4 112.0(8) . . ? C28 N7 Ir4 144.5(11) . . ? C21 N8 C20 103.7(12) . . ? C21 N8 Ir4 109.4(8) . . ? C20 N8 Ir4 143.9(10) . . ? C29 N9 C33 117.5(11) . . ? C29 N9 Ir1 120.3(9) . . ? C33 N9 Ir1 122.1(9) . . ? C38 N10 C34 116.8(10) . . ? C38 N10 Ir3 121.4(8) . . ? C34 N10 Ir3 121.2(8) . . ? C43 N11 C39 116.8(12) . . ? C43 N11 Ir2 117.4(10) . . ? C39 N11 Ir2 124.1(8) . . ? C48 N12 C44 117.2(12) . . ? C48 N12 Ir4 120.6(10) . . ? C44 N12 Ir4 122.1(9) . . ? O3 S1 O2 108.9(16) . . ? O3 S1 O1 117.2(17) . . ? O2 S1 O1 116.2(12) . . ? O3 S1 C89 107.6(19) . . ? O2 S1 C89 103.6(16) . . ? O1 S1 C89 101.8(12) . . ? O6 S2 O4 116.2(16) . . ? O6 S2 O5 115.8(18) . . ? O4 S2 O5 120.9(11) . . ? O6 S2 C90 100.3(17) . . ? O4 S2 C90 100.6(11) . . ? O5 S2 C90 96.2(13) . . ? O9 S3 O7 119.3(15) . . ? O9 S3 O8 112.5(13) . . ? O7 S3 O8 121.7(15) . . ? O9 S3 C91 103.2(15) . . ? O7 S3 C91 105.6(19) . . ? O8 S3 C91 85.9(16) . . ? O12 S4 O10 115.7(19) . . ? O12 S4 O11 105(2) . . ? O10 S4 O11 121(3) . . ? O12 S4 C92 111.1(12) . . ? O10 S4 C92 102.8(13) . . ? O11 S4 C92 99.1(12) . . ? C2 C1 N1 130.5(14) . . ? C2 C1 C6 121.8(12) . . ? N1 C1 C6 107.3(11) . . ? C3 C2 C1 114.1(15) . . ? C4 C3 C2 124.4(16) . . ? C3 C4 C5 120.7(15) . . ? C6 C5 C4 118.2(16) . . ? C5 C6 N4 131.9(14) . . ? C5 C6 C1 120.5(12) . . ? N4 C6 C1 107.6(11) . . ? N4 C7 N1 118.6(10) . . ? N4 C7 C8 122.1(12) . . ? N1 C7 C8 118.7(12) . . ? N2 C8 N3 116.8(11) . . ? N2 C8 C7 122.9(13) . . ? N3 C8 C7 119.6(13) . . ? C10 C9 C14 125.9(13) . . ? C10 C9 N2 127.0(14) . . ? C14 C9 N2 106.9(12) . . ? C11 C10 C9 113.4(16) . . ? C10 C11 C12 126.2(16) . . ? C13 C12 C11 115.7(15) . . ? C14 C13 C12 120.7(17) . . ? N3 C14 C13 132.5(15) . . ? N3 C14 C9 109.9(13) . . ? C13 C14 C9 117.4(13) . . ? C16 C15 N5 129.7(15) . . ? C16 C15 C20 122.2(15) . . ? N5 C15 C20 108.0(12) . . ? C15 C16 C17 114.7(17) . . ? C18 C17 C16 124.0(17) . . ? C17 C18 C19 120.1(17) . . ? C20 C19 C18 120.4(16) . . ? N8 C20 C19 133.2(15) . . ? N8 C20 C15 108.4(12) . . ? C19 C20 C15 118.4(14) . . ? N8 C21 N5 120.6(10) . . ? N8 C21 C22 121.8(13) . . ? N5 C21 C22 116.8(14) . . ? N7 C22 N6 121.3(11) . . ? N7 C22 C21 117.4(13) . . ? N6 C22 C21 121.0(12) . . ? C24 C23 N6 130.0(16) . . ? C24 C23 C28 124.8(16) . . ? N6 C23 C28 105.2(12) . . ? C25 C24 C23 113.5(19) . . ? C26 C25 C24 127.0(16) . . ? C25 C26 C27 118.5(19) . . ? C26 C27 C28 122(2) . . ? N7 C28 C27 135.1(17) . . ? N7 C28 C23 110.4(13) . . ? C27 C28 C23 114.3(16) . . ? N9 C29 C30 119.9(13) . . ? C31 C30 C29 122.9(14) . . ? C30 C31 C32 117.4(15) . . ? C30 C31 C36 125.8(13) . . ? C32 C31 C36 116.2(14) . . ? C33 C32 C31 115.7(16) . . ? N9 C33 C32 124.2(14) . . ? N10 C34 C35 122.5(11) . . ? C36 C35 C34 120.3(11) . . ? C35 C36 C37 115.2(12) . . ? C35 C36 C31 123.8(12) . . ? C37 C36 C31 121.0(13) . . ? C38 C37 C36 119.7(14) . . ? N10 C38 C37 125.2(12) . . ? C40 C39 N11 124.4(12) . . ? C39 C40 C41 118.9(13) . . ? C42 C41 C40 119.1(13) . . ? C42 C41 C46 121.3(12) . . ? C40 C41 C46 119.3(14) . . ? C41 C42 C43 118.8(13) . . ? N11 C43 C42 122.0(14) . . ? N12 C44 C45 123.2(12) . . ? C44 C45 C46 119.1(15) . . ? C47 C46 C45 117.0(14) . . ? C47 C46 C41 121.1(12) . . ? C45 C46 C41 120.9(13) . . ? C46 C47 C48 120.8(13) . . ? N12 C48 C47 121.6(14) . . ? C50 C49 C53 108.0 . . ? C50 C49 C54 126.0 . . ? C53 C49 C54 126.0 . . ? C50 C49 Ir1 71.6(3) . . ? C53 C49 Ir1 71.2(3) . . ? C54 C49 Ir1 122.8(3) . . ? C49 C50 C51 108.0 . . ? C49 C50 C55 126.0 . . ? C51 C50 C55 126.0 . . ? C49 C50 Ir1 70.8(2) . . ? C51 C50 Ir1 71.6(3) . . ? C55 C50 Ir1 123.3(3) . . ? C52 C51 C50 108.0 . . ? C52 C51 C56 126.0 . . ? C50 C51 C56 126.0 . . ? C52 C51 Ir1 71.1(3) . . ? C50 C51 Ir1 71.1(3) . . ? C56 C51 Ir1 123.5(2) . . ? C51 C52 C53 108.0 . . ? C51 C52 C57 126.0 . . ? C53 C52 C57 126.0 . . ? C51 C52 Ir1 71.6(3) . . ? C53 C52 Ir1 70.8(2) . . ? C57 C52 Ir1 123.3(3) . . ? C52 C53 C49 108.0 . . ? C52 C53 C58 126.0 . . ? C49 C53 C58 126.0 . . ? C52 C53 Ir1 71.6(3) . . ? C49 C53 Ir1 71.2(3) . . ? C58 C53 Ir1 122.8(3) . . ? C63 C59 C64 124.6(13) . . ? C63 C59 C60 108.0(11) . . ? C64 C59 C60 127.4(12) . . ? C63 C59 Ir2 71.7(7) . . ? C64 C59 Ir2 126.2(9) . . ? C60 C59 Ir2 69.9(7) . . ? C61 C60 C59 104.2(13) . . ? C61 C60 C65 129.2(14) . . ? C59 C60 C65 125.2(12) . . ? C61 C60 Ir2 69.9(8) . . ? C59 C60 Ir2 70.0(7) . . ? C65 C60 Ir2 133.8(12) . . ? C62 C61 C60 112.2(14) . . ? C62 C61 C66 128.1(15) . . ? C60 C61 C66 119.7(17) . . ? C62 C61 Ir2 72.1(9) . . ? C60 C61 Ir2 70.6(8) . . ? C66 C61 Ir2 125.3(12) . . ? C61 C62 C63 109.9(13) . . ? C61 C62 C67 127.9(17) . . ? C63 C62 C67 121.3(18) . . ? C61 C62 Ir2 71.7(9) . . ? C63 C62 Ir2 72.1(7) . . ? C67 C62 Ir2 131.1(11) . . ? C62 C63 C68 125.8(14) . . ? C62 C63 C59 105.7(13) . . ? C68 C63 C59 128.5(13) . . ? C62 C63 Ir2 68.8(8) . . ? C68 C63 Ir2 125.4(11) . . ? C59 C63 Ir2 69.0(7) . . ? C73 C69 C70 108.0 . . ? C73 C69 C74 126.0 . . ? C70 C69 C74 126.0 . . ? C73 C69 Ir3 70.77(17) . . ? C70 C69 Ir3 70.4(2) . . ? C74 C69 Ir3 124.43(15) . . ? C71 C70 C69 108.0 . . ? C71 C70 C75 126.0 . . ? C69 C70 C75 126.0 . . ? C71 C70 Ir3 70.62(14) . . ? C69 C70 Ir3 70.78(18) . . ? C75 C70 Ir3 124.24(16) . . ? C72 C71 C70 108.0 . . ? C72 C71 C76 126.0 . . ? C70 C71 C76 126.0 . . ? C72 C71 Ir3 70.79(18) . . ? C70 C71 Ir3 70.54(14) . . ? C76 C71 Ir3 124.25(16) . . ? C71 C72 C73 108.0 . . ? C71 C72 C77 126.0 . . ? C73 C72 C77 126.0 . . ? C71 C72 Ir3 70.4(2) . . ? C73 C72 Ir3 70.73(17) . . ? C77 C72 Ir3 124.47(14) . . ? C69 C73 C72 108.0 . . ? C69 C73 C78 126.0 . . ? C72 C73 C78 126.0 . . ? C69 C73 Ir3 70.51(16) . . ? C72 C73 Ir3 70.54(15) . . ? C78 C73 Ir3 124.56(19) . . ? C83 C79 C80 108.0 . . ? C83 C79 C84 126.0 . . ? C80 C79 C84 126.0 . . ? C83 C79 Ir4 70.93(19) . . ? C80 C79 Ir4 71.46(17) . . ? C84 C79 Ir4 123.28(19) . . ? C79 C80 C81 108.0 . . ? C79 C80 C85 126.0 . . ? C81 C80 C85 126.0 . . ? C79 C80 Ir4 70.08(17) . . ? C81 C80 Ir4 71.6(2) . . ? C85 C80 Ir4 123.99(18) . . ? C82 C81 C80 108.0 . . ? C82 C81 C86 126.0 . . ? C80 C81 C86 126.0 . . ? C82 C81 Ir4 70.68(18) . . ? C80 C81 Ir4 70.29(19) . . ? C86 C81 Ir4 124.64(17) . . ? C83 C82 C81 108.0 . . ? C83 C82 C87 126.0 . . ? C81 C82 C87 126.0 . . ? C83 C82 Ir4 70.02(17) . . ? C81 C82 Ir4 71.26(17) . . ? C87 C82 Ir4 124.31(18) . . ? C79 C83 C82 108.0 . . ? C79 C83 C88 126.0 . . ? C82 C83 C88 126.0 . . ? C79 C83 Ir4 70.50(19) . . ? C82 C83 Ir4 71.66(19) . . ? C88 C83 Ir4 123.49(16) . . ? C80' C79' C83' 108.0 . . ? C80' C79' C84' 126.0 . . ? C83' C79' C84' 126.0 . . ? C80' C79' Ir4 69.96(17) . . ? C83' C79' Ir4 70.5(2) . . ? C84' C79' Ir4 125.13(17) . . ? C81' C80' C79' 108.0 . . ? C81' C80' C85' 126.0 . . ? C79' C80' C85' 126.0 . . ? C81' C80' Ir4 69.20(18) . . ? C79' C80' Ir4 72.70(17) . . ? C85' C80' Ir4 123.66(19) . . ? C80' C81' C82' 108.0 . . ? C80' C81' C86' 126.0 . . ? C82' C81' C86' 126.0 . . ? C80' C81' Ir4 72.74(19) . . ? C82' C81' Ir4 71.1(2) . . ? C86' C81' Ir4 121.87(17) . . ? C83' C82' C81' 108.0 . . ? C83' C82' C87' 126.0 . . ? C81' C82' C87' 126.0 . . ? C83' C82' Ir4 73.01(17) . . ? C81' C82' Ir4 70.44(18) . . ? C87' C82' Ir4 122.20(18) . . ? C82' C83' C79' 108.0 . . ? C82' C83' C88' 126.0 . . ? C79' C83' C88' 126.0 . . ? C82' C83' Ir4 69.14(17) . . ? C79' C83' Ir4 72.25(19) . . ? C88' C83' Ir4 124.25(17) . . ? F3 C89 F2 103.3(18) . . ? F3 C89 F1 104.2(17) . . ? F2 C89 F1 106.8(18) . . ? F3 C89 S1 106.9(18) . . ? F2 C89 S1 104(3) . . ? F1 C89 S1 129(2) . . ? F4 C90 F5 101.4(18) . . ? F4 C90 F6 109(3) . . ? F5 C90 F6 108(2) . . ? F4 C90 S2 115.2(19) . . ? F5 C90 S2 111.2(19) . . ? F6 C90 S2 111.6(17) . . ? F7 C91 F8 115(2) . . ? F7 C91 F9 116(2) . . ? F8 C91 F9 105.1(15) . . ? F7 C91 S3 114.5(17) . . ? F8 C91 S3 106.4(15) . . ? F9 C91 S3 97.7(15) . . ? F12 C92 F11 103(3) . . ? F12 C92 F10 104.1(17) . . ? F11 C92 F10 104(2) . . ? F12 C92 S4 116.3(13) . . ? F11 C92 S4 114.3(16) . . ? F10 C92 S4 113.3(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.473 _refine_diff_density_min -2.222 _refine_diff_density_rms 0.178 # Attachment '- 3a_1.cif' data_mo_3a _database_code_depnum_ccdc_archive 'CCDC 888412' #TrackingRef '- 3a_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C129 H136 Ag F15 Ir4 N16 O19 S5' _chemical_formula_weight 3536.51 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 33.945(2) _cell_length_b 25.8578(18) _cell_length_c 28.822(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25298(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.23 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13952 _exptl_absorpt_coefficient_mu 4.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6604 _exptl_absorpt_correction_T_max 0.8397 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.08 _diffrn_reflns_number 148971 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.01 _reflns_number_total 22279 _reflns_number_gt 12100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In asymmetric unit of this data, there were three disordered diethyl ether molecules which could not be restrained properly. Therefore, SQUEEZE algorithm was used to omit them. F12, O8-10, F7-9, O8'-10', F7'-9' and C115 were refined isotropically and other non-hydrogen atoms were refined anisotropically. 15 ISOR, 33 DFIX and 2 SIMU instructions were used to restrain the disordered anions and Cp* fragments so that there were 130 restraints in the data. There are several big residual density peaks in the structure but all of them are close to the heavy atoms. ; _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^)+(0.1175P)^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 22279 _refine_ls_number_parameters 1522 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.071 0.429 -0.118 4221.5 1033.5 2 0.250 0.250 0.027 16.2 -2.9 3 0.750 0.750 0.059 8.9 -2.1 4 0.608 0.511 0.165 47.2 1.9 5 0.892 -0.011 0.165 47.1 -0.7 6 0.592 0.619 0.225 13.1 -1.0 7 0.908 0.881 0.225 12.9 -0.6 8 0.045 0.509 0.239 13.1 0.5 9 0.455 -0.009 0.239 13.6 0.1 10 0.542 0.492 0.264 12.2 -1.3 11 0.958 0.008 0.264 12.6 -0.6 12 0.093 0.382 0.277 13.1 -0.4 13 0.407 0.118 0.277 13.7 -0.9 14 0.109 0.489 0.337 46.4 0.0 15 0.391 1.011 0.337 45.3 -0.6 16 0.250 0.250 0.441 8.3 -2.0 17 0.750 0.750 0.473 15.7 -3.4 18 0.250 0.250 0.529 15.7 -3.1 19 0.750 0.750 0.562 8.3 -2.1 20 0.608 -0.011 0.665 47.6 0.6 21 0.892 0.511 0.665 46.8 -0.2 22 0.592 0.881 0.725 12.7 -0.8 23 0.908 0.619 0.725 13.2 -1.0 24 0.045 -0.009 0.739 13.1 0.8 25 0.455 0.509 0.739 13.6 1.3 26 0.542 0.008 0.764 12.2 -1.0 27 0.958 0.492 0.764 12.6 -0.2 28 0.093 0.118 0.777 13.5 -0.6 29 0.407 0.382 0.777 13.3 -0.7 30 0.109 1.011 0.837 45.9 1.4 31 0.391 0.489 0.837 45.7 -0.1 32 0.250 0.250 0.938 7.8 -2.1 33 0.750 0.750 0.971 15.1 -3.5 _platon_squeeze_details ; ; 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 0.053465(18) 0.23353(2) 0.359504(18) 0.05473(18) Uani 1 1 d . . . Ir2 Ir -0.017896(19) 0.27971(2) 0.18893(2) 0.0637(2) Uani 1 1 d . . . Ir3 Ir 0.310839(18) -0.01545(2) 0.177237(18) 0.05538(18) Uani 1 1 d . . . Ir4 Ir 0.250462(18) 0.045804(19) 0.004856(16) 0.05125(17) Uani 1 1 d . . . Ag1 Ag 0.11521(3) 0.06823(4) 0.18254(3) 0.0566(3) Uani 1 1 d . . . N1 N 0.0686(3) 0.2599(4) 0.2907(4) 0.053(3) Uani 1 1 d . . . N2 N -0.0032(4) 0.2504(5) 0.3327(4) 0.070(4) Uani 1 1 d . . . N3 N -0.0326(4) 0.2679(5) 0.2606(4) 0.063(3) Uani 1 1 d . . . N4 N 0.0394(3) 0.2795(4) 0.2212(4) 0.051(3) Uani 1 1 d . . . N5 N 0.2863(3) 0.0524(4) 0.1433(3) 0.051(3) Uani 1 1 d . B . N6 N 0.3103(4) -0.0413(4) 0.1051(4) 0.058(3) Uani 1 1 d . B . N7 N 0.2846(3) -0.0154(4) 0.0349(3) 0.051(3) Uani 1 1 d . . . N8 N 0.2605(3) 0.0749(4) 0.0731(3) 0.049(3) Uani 1 1 d . B . N9 N 0.0450(4) 0.1614(4) 0.3276(4) 0.058(3) Uani 1 1 d . . . N10 N 0.2525(3) -0.0410(4) 0.1774(4) 0.060(3) Uani 1 1 d . B . N11 N 0.0988(3) 0.0598(4) 0.2668(4) 0.055(3) Uani 1 1 d . . . N12 N 0.1553(3) 0.0027(4) 0.2202(3) 0.048(3) Uani 1 1 d . . . N13 N -0.0132(3) 0.1972(5) 0.1886(3) 0.049(3) Uani 1 1 d . . . N14 N 0.2013(4) 0.0081(4) 0.0357(4) 0.060(3) Uani 1 1 d . . . N15 N 0.0525(3) 0.0974(4) 0.1448(4) 0.054(3) Uani 1 1 d . . . N16 N 0.1144(4) 0.0419(4) 0.1026(4) 0.056(3) Uani 1 1 d . . . O1 O 0.1276(3) 0.1570(4) 0.2002(3) 0.077(3) Uani 1 1 d . . . O2 O 0.1809(3) 0.3984(5) 0.8501(4) 0.090(4) Uani 1 1 d . . . O3 O 0.2170(3) 0.4231(4) 0.7834(4) 0.085(3) Uani 1 1 d . . . O4 O 0.1771(3) 0.3455(4) 0.7836(4) 0.087(3) Uani 1 1 d . . . O5 O 0.1246(5) 0.3466(5) 0.5386(5) 0.143(7) Uani 1 1 d . . . O6 O 0.0674(5) 0.2965(9) 0.5437(8) 0.200(9) Uani 1 1 d . . . O7 O 0.1063(5) 0.3046(6) 0.6077(4) 0.144(6) Uani 1 1 d . . . O11 O 0.0398(4) 0.9743(5) 0.1343(4) 0.108(5) Uani 1 1 d . . . O12 O 0.0379(9) 0.9724(7) 0.2175(6) 0.233(13) Uani 1 1 d . . . O13 O 0.0741(7) 0.9141(14) 0.1787(9) 0.293(18) Uani 1 1 d . . . S1 S 0.19960(11) 0.38348(14) 0.80959(12) 0.0570(9) Uani 1 1 d . . . S2 S 0.10500(17) 0.30513(19) 0.55943(16) 0.0862(14) Uani 1 1 d . . . S3 S 0.1465(2) 0.8799(3) 0.9040(3) 0.180(4) Uani 1 1 d DU . . S4 S 0.04285(17) 0.9487(2) 0.17568(17) 0.0906(15) Uani 1 1 d . . . F1 F 0.2618(3) 0.3243(4) 0.7967(3) 0.087(3) Uani 1 1 d . . . F2 F 0.2682(3) 0.3774(5) 0.8515(3) 0.105(3) Uani 1 1 d . . . F3 F 0.2337(3) 0.3127(4) 0.8619(3) 0.113(4) Uani 1 1 d . . . F4 F 0.1694(4) 0.2524(4) 0.5573(4) 0.122(4) Uani 1 1 d . . . F5 F 0.1189(5) 0.2074(4) 0.5563(5) 0.173(7) Uani 1 1 d . . . F6 F 0.1369(5) 0.2491(5) 0.4965(4) 0.138(5) Uani 1 1 d . . . F10 F -0.0078(6) 0.8840(5) 0.1472(5) 0.182(7) Uani 1 1 d . . . F11 F 0.0060(5) 0.8733(5) 0.2145(5) 0.195(8) Uani 1 1 d . . . F12 F -0.0303(8) 0.9404(10) 0.1869(8) 0.256(10) Uiso 1 1 d . . . C1 C 0.0988(4) 0.2701(5) 0.2585(4) 0.051(3) Uani 1 1 d . . . C2 C 0.1395(4) 0.2696(5) 0.2604(5) 0.050(3) Uani 1 1 d . . . H2 H 0.1524 0.2613 0.2887 0.060 Uiso 1 1 calc R . . C3 C 0.1609(5) 0.2807(5) 0.2231(5) 0.061(4) Uani 1 1 d . . . H3 H 0.1888 0.2809 0.2256 0.073 Uiso 1 1 calc R . . C4 C 0.1438(6) 0.2921(6) 0.1807(5) 0.068(4) Uani 1 1 d . . . H4 H 0.1598 0.2997 0.1546 0.081 Uiso 1 1 calc R . . C5 C 0.1047(5) 0.2924(5) 0.1766(5) 0.065(4) Uani 1 1 d . . . H5 H 0.0931 0.3003 0.1474 0.078 Uiso 1 1 calc R . . C6 C 0.0800(4) 0.2811(5) 0.2148(4) 0.054(4) Uani 1 1 d . . . C7 C 0.0362(4) 0.2664(5) 0.2646(4) 0.054(4) Uani 1 1 d . . . C8 C -0.0003(4) 0.2619(6) 0.2870(4) 0.053(4) Uani 1 1 d . . . C9 C -0.0435(4) 0.2478(6) 0.3366(5) 0.065(4) Uani 1 1 d . . . C10 C -0.0676(6) 0.2371(7) 0.3757(8) 0.104(7) Uani 1 1 d . . . H10 H -0.0562 0.2297 0.4051 0.125 Uiso 1 1 calc R . . C11 C -0.1081(5) 0.2377(8) 0.3700(8) 0.103(6) Uani 1 1 d . . . H11 H -0.1244 0.2310 0.3962 0.123 Uiso 1 1 calc R . . C12 C -0.1267(8) 0.2480(8) 0.3258(9) 0.113(7) Uani 1 1 d . . . H12 H -0.1546 0.2477 0.3231 0.135 Uiso 1 1 calc R . . C13 C -0.1047(6) 0.2577(7) 0.2893(8) 0.088(5) Uani 1 1 d . . . H13 H -0.1169 0.2640 0.2602 0.106 Uiso 1 1 calc R . . C14 C -0.0619(5) 0.2591(6) 0.2928(7) 0.071(5) Uani 1 1 d . . . C15 C 0.2657(4) 0.0985(5) 0.1489(4) 0.048(3) Uani 1 1 d . . . C16 C 0.2581(4) 0.1285(6) 0.1881(4) 0.061(4) Uani 1 1 d . B . H16 H 0.2686 0.1192 0.2175 0.073 Uiso 1 1 calc R . . C17 C 0.2350(5) 0.1719(5) 0.1830(5) 0.067(4) Uani 1 1 d . . . H17 H 0.2282 0.1914 0.2098 0.081 Uiso 1 1 calc R B . C18 C 0.2211(5) 0.1883(6) 0.1398(5) 0.068(4) Uani 1 1 d . B . H18 H 0.2077 0.2205 0.1372 0.081 Uiso 1 1 calc R . . C19 C 0.2268(4) 0.1585(5) 0.1015(5) 0.059(4) Uani 1 1 d . . . H19 H 0.2151 0.1676 0.0727 0.071 Uiso 1 1 calc R B . C20 C 0.2507(4) 0.1135(4) 0.1055(4) 0.038(3) Uani 1 1 d . B . C21 C 0.2811(4) 0.0429(5) 0.0987(4) 0.045(3) Uani 1 1 d . . . C22 C 0.2921(4) -0.0052(5) 0.0799(5) 0.055(3) Uani 1 1 d . B . C23 C 0.3121(4) -0.0833(5) 0.0755(4) 0.053(4) Uani 1 1 d . . . C24 C 0.3256(5) -0.1339(7) 0.0821(5) 0.080(5) Uani 1 1 d . B . H24 H 0.3378 -0.1442 0.1103 0.096 Uiso 1 1 calc R . . C25 C 0.3205(6) -0.1680(7) 0.0463(6) 0.096(6) Uani 1 1 d . . . H25 H 0.3276 -0.2032 0.0507 0.115 Uiso 1 1 calc R B . C26 C 0.3043(5) -0.1519(6) 0.0012(5) 0.080(5) Uani 1 1 d . B . H26 H 0.3019 -0.1763 -0.0233 0.096 Uiso 1 1 calc R . . C27 C 0.2930(5) -0.1030(5) -0.0052(5) 0.067(4) Uani 1 1 d . . . H27 H 0.2827 -0.0921 -0.0342 0.081 Uiso 1 1 calc R B . C28 C 0.2967(4) -0.0674(5) 0.0324(4) 0.056(4) Uani 1 1 d . B . C29 C 0.1107(5) -0.0009(5) 0.3345(5) 0.060(4) Uani 1 1 d . . . C30 C 0.0842(5) 0.0065(6) 0.3698(5) 0.066(4) Uani 1 1 d . . . H30 H 0.0655 0.0339 0.3702 0.080 Uiso 1 1 calc R . . C31 C 0.0875(6) -0.0322(10) 0.4066(6) 0.106(7) Uani 1 1 d . . . H31 H 0.0690 -0.0302 0.4312 0.127 Uiso 1 1 calc R . . C32 C 0.1145(7) -0.0703(7) 0.4090(7) 0.096(6) Uani 1 1 d . . . H32 H 0.1152 -0.0928 0.4350 0.115 Uiso 1 1 calc R . . C33 C 0.1409(5) -0.0763(6) 0.3731(5) 0.057(4) Uani 1 1 d . . . C34 C 0.1707(6) -0.1144(6) 0.3720(5) 0.080(5) Uani 1 1 d . . . H34 H 0.1750 -0.1367 0.3977 0.096 Uiso 1 1 calc R . . C35 C 0.1929(5) -0.1180(6) 0.3334(6) 0.077(5) Uani 1 1 d . . . H35 H 0.2122 -0.1447 0.3320 0.092 Uiso 1 1 calc R . . C36 C 0.1893(5) -0.0845(6) 0.2946(5) 0.073(5) Uani 1 1 d . . . H36 H 0.2053 -0.0891 0.2678 0.087 Uiso 1 1 calc R . . C37 C 0.1626(4) -0.0458(4) 0.2967(4) 0.049(3) Uani 1 1 d . . . C38 C 0.1393(4) -0.0413(5) 0.3349(4) 0.050(3) Uani 1 1 d . . . C39 C 0.1152(4) 0.0227(5) 0.2866(4) 0.051(3) Uani 1 1 d . . . C40 C 0.1483(4) -0.0068(4) 0.2629(4) 0.045(3) Uani 1 1 d . . . C41 C 0.0722(4) 0.1361(5) 0.3047(4) 0.048(3) Uani 1 1 d . . . H41 H 0.0966 0.1531 0.2993 0.058 Uiso 1 1 calc R . . C42 C 0.0679(4) 0.0859(6) 0.2875(5) 0.056(4) Uani 1 1 d . . . C43 C 0.0311(5) 0.0640(7) 0.2921(6) 0.083(5) Uani 1 1 d . . . H43 H 0.0260 0.0306 0.2798 0.099 Uiso 1 1 calc R . . C44 C 0.0017(4) 0.0913(6) 0.3147(7) 0.086(6) Uani 1 1 d . . . H44 H -0.0238 0.0766 0.3176 0.103 Uiso 1 1 calc R . . C45 C 0.0088(6) 0.1371(8) 0.3322(7) 0.104(7) Uani 1 1 d . . . H45 H -0.0116 0.1543 0.3486 0.125 Uiso 1 1 calc R . . C46 C 0.2227(4) -0.0132(4) 0.1958(4) 0.039(3) Uani 1 1 d . . . H46 H 0.2288 0.0200 0.2079 0.047 Uiso 1 1 calc R B . C47 C 0.1858(4) -0.0283(5) 0.1981(5) 0.058(4) Uani 1 1 d . B . C48 C 0.1764(5) -0.0759(5) 0.1798(5) 0.065(4) Uani 1 1 d . . . H48 H 0.1499 -0.0876 0.1805 0.078 Uiso 1 1 calc R B . C49 C 0.2043(5) -0.1057(6) 0.1613(5) 0.063(4) Uani 1 1 d . B . H49 H 0.1977 -0.1386 0.1489 0.075 Uiso 1 1 calc R . . C50 C 0.2407(5) -0.0895(5) 0.1604(5) 0.068(4) Uani 1 1 d . . . H50 H 0.2602 -0.1116 0.1476 0.081 Uiso 1 1 calc R B . C51 C 0.0188(4) 0.0857(4) 0.0675(5) 0.053(4) Uani 1 1 d . . . C52 C -0.0185(5) 0.1063(5) 0.0649(6) 0.079(5) Uani 1 1 d . . . H52 H -0.0300 0.1212 0.0918 0.094 Uiso 1 1 calc R . . C53 C -0.0395(5) 0.1055(6) 0.0241(8) 0.084(5) Uani 1 1 d . . . H53 H -0.0649 0.1210 0.0229 0.101 Uiso 1 1 calc R . . C54 C -0.0249(8) 0.0834(8) -0.0131(8) 0.110(9) Uani 1 1 d . . . H54 H -0.0409 0.0819 -0.0402 0.132 Uiso 1 1 calc R . . C55 C 0.0132(6) 0.0620(6) -0.0151(6) 0.071(5) Uani 1 1 d . . . C56 C 0.0336(7) 0.0351(6) -0.0526(6) 0.079(5) Uani 1 1 d . . . H56 H 0.0202 0.0304 -0.0812 0.095 Uiso 1 1 calc R . . C57 C 0.0694(6) 0.0173(6) -0.0484(6) 0.079(5) Uani 1 1 d . . . H57 H 0.0821 0.0021 -0.0744 0.094 Uiso 1 1 calc R . . C58 C 0.0890(5) 0.0207(5) -0.0062(5) 0.060(4) Uani 1 1 d . . . H58 H 0.1145 0.0061 -0.0032 0.071 Uiso 1 1 calc R . . C59 C 0.0717(4) 0.0449(4) 0.0315(4) 0.050(3) Uani 1 1 d . . . C60 C 0.0321(5) 0.0657(5) 0.0263(5) 0.062(4) Uani 1 1 d . . . C61 C 0.0505(4) 0.0831(5) 0.1034(5) 0.047(3) Uani 1 1 d . . . C62 C 0.0835(4) 0.0545(5) 0.0796(4) 0.049(3) Uani 1 1 d . . . C63 C 0.0188(4) 0.1736(6) 0.1680(5) 0.056(4) Uani 1 1 d . . . H63 H 0.0397 0.1936 0.1555 0.068 Uiso 1 1 calc R . . C64 C 0.0199(4) 0.1202(5) 0.1657(5) 0.057(4) Uani 1 1 d . . . C65 C -0.0116(7) 0.0920(9) 0.1825(7) 0.117(7) Uani 1 1 d . . . H65 H -0.0113 0.0553 0.1805 0.141 Uiso 1 1 calc R . . C66 C -0.0432(4) 0.1169(7) 0.2022(7) 0.087(5) Uani 1 1 d . . . H66 H -0.0644 0.0976 0.2148 0.104 Uiso 1 1 calc R . . C67 C -0.0437(5) 0.1710(7) 0.2036(6) 0.084(5) Uani 1 1 d . . . H67 H -0.0662 0.1887 0.2153 0.101 Uiso 1 1 calc R . . C68 C 0.1753(4) 0.0356(5) 0.0598(4) 0.045(3) Uani 1 1 d . . . H68 H 0.1796 0.0716 0.0640 0.054 Uiso 1 1 calc R . . C69 C 0.1416(4) 0.0122(5) 0.0793(4) 0.050(3) Uani 1 1 d . . . C70 C 0.1385(5) -0.0406(6) 0.0750(5) 0.065(4) Uani 1 1 d . . . H70 H 0.1170 -0.0577 0.0894 0.078 Uiso 1 1 calc R . . C71 C 0.1650(5) -0.0690(5) 0.0513(5) 0.070(4) Uani 1 1 d . . . H71 H 0.1623 -0.1055 0.0487 0.084 Uiso 1 1 calc R . . C72 C 0.1972(5) -0.0427(5) 0.0301(5) 0.062(4) Uani 1 1 d . . . H72 H 0.2157 -0.0614 0.0120 0.075 Uiso 1 1 calc R . . C73 C 0.0463(5) 0.2692(7) 0.4283(5) 0.077(5) Uani 1 1 d . . . C74 C 0.0474(6) 0.2167(7) 0.4336(6) 0.082(5) Uani 1 1 d . . . C75 C 0.0852(5) 0.2002(6) 0.4151(5) 0.066(4) Uani 1 1 d . . . C76 C 0.1070(5) 0.2410(6) 0.3996(5) 0.060(4) Uani 1 1 d . . . C77 C 0.0834(5) 0.2890(6) 0.4040(5) 0.067(4) Uani 1 1 d . . . C78 C 0.0140(6) 0.3041(8) 0.4432(6) 0.119(8) Uani 1 1 d . . . H78A H -0.0114 0.2888 0.4348 0.178 Uiso 1 1 calc R . . H78B H 0.0169 0.3376 0.4276 0.178 Uiso 1 1 calc R . . H78C H 0.0153 0.3090 0.4768 0.178 Uiso 1 1 calc R . . C79 C 0.0163(5) 0.1841(8) 0.4571(6) 0.107(7) Uani 1 1 d . . . H79A H -0.0026 0.2067 0.4730 0.161 Uiso 1 1 calc R . . H79B H 0.0288 0.1612 0.4797 0.161 Uiso 1 1 calc R . . H79C H 0.0024 0.1634 0.4338 0.161 Uiso 1 1 calc R . . C80 C 0.0999(5) 0.1443(6) 0.4188(5) 0.075(5) Uani 1 1 d . . . H80A H 0.1172 0.1366 0.3925 0.113 Uiso 1 1 calc R . . H80B H 0.0773 0.1207 0.4184 0.113 Uiso 1 1 calc R . . H80C H 0.1144 0.1399 0.4479 0.113 Uiso 1 1 calc R . . C81 C 0.1495(5) 0.2396(6) 0.3827(5) 0.078(5) Uani 1 1 d . . . H81A H 0.1669 0.2298 0.4085 0.117 Uiso 1 1 calc R . . H81B H 0.1571 0.2738 0.3712 0.117 Uiso 1 1 calc R . . H81C H 0.1520 0.2142 0.3577 0.117 Uiso 1 1 calc R . . C82 C 0.0961(6) 0.3402(7) 0.3961(7) 0.117(8) Uani 1 1 d . . . H82A H 0.1109 0.3525 0.4231 0.175 Uiso 1 1 calc R . . H82B H 0.0732 0.3625 0.3910 0.175 Uiso 1 1 calc R . . H82C H 0.1131 0.3411 0.3686 0.175 Uiso 1 1 calc R . . C83 C -0.0705(6) 0.2964(6) 0.1508(6) 0.078(5) Uani 1 1 d . . . C84 C -0.0602(5) 0.3413(6) 0.1774(6) 0.076(5) Uani 1 1 d . . . C85 C -0.0214(6) 0.3589(6) 0.1619(5) 0.080(5) Uani 1 1 d . . . C86 C -0.0093(6) 0.3243(7) 0.1257(6) 0.084(6) Uani 1 1 d . . . C87 C -0.0394(8) 0.2877(8) 0.1184(6) 0.104(7) Uani 1 1 d . . . C88 C -0.1101(6) 0.2709(8) 0.1529(9) 0.137(10) Uani 1 1 d . . . H88A H -0.1236 0.2754 0.1231 0.206 Uiso 1 1 calc R . . H88B H -0.1258 0.2868 0.1776 0.206 Uiso 1 1 calc R . . H88C H -0.1068 0.2339 0.1593 0.206 Uiso 1 1 calc R . . C89 C -0.0847(5) 0.3654(7) 0.2144(6) 0.087(5) Uani 1 1 d . . . H89A H -0.1126 0.3626 0.2061 0.130 Uiso 1 1 calc R . . H89B H -0.0775 0.4020 0.2175 0.130 Uiso 1 1 calc R . . H89C H -0.0800 0.3476 0.2439 0.130 Uiso 1 1 calc R . . C90 C -0.0016(6) 0.4074(7) 0.1786(6) 0.095(6) Uani 1 1 d . . . H90A H 0.0225 0.3984 0.1955 0.143 Uiso 1 1 calc R . . H90B H -0.0194 0.4263 0.1993 0.143 Uiso 1 1 calc R . . H90C H 0.0051 0.4292 0.1519 0.143 Uiso 1 1 calc R . . C91 C 0.0267(7) 0.3302(8) 0.0972(6) 0.120(8) Uani 1 1 d . . . H91A H 0.0372 0.2959 0.0894 0.181 Uiso 1 1 calc R . . H91B H 0.0466 0.3496 0.1148 0.181 Uiso 1 1 calc R . . H91C H 0.0203 0.3489 0.0687 0.181 Uiso 1 1 calc R . . C92 C -0.0410(6) 0.2428(6) 0.0824(5) 0.144(11) Uani 1 1 d . . . H92A H -0.0421 0.2572 0.0510 0.217 Uiso 1 1 calc R . . H92B H -0.0645 0.2217 0.0880 0.217 Uiso 1 1 calc R . . H92C H -0.0174 0.2213 0.0856 0.217 Uiso 1 1 calc R . . O8 O 0.1560(3) 0.9213(4) 0.9321(3) 0.236(16) Uiso 0.708(18) 1 d PRD A 1 O9 O 0.1506(3) 0.8914(4) 0.8533(4) 0.40(2) Uiso 0.708(18) 1 d PRDU A 1 O10 O 0.1128(3) 0.8504(4) 0.9143(3) 0.187(12) Uiso 0.708(18) 1 d PRD A 1 F7 F 0.1862(3) 0.7912(4) 0.8982(3) 0.182(9) Uiso 0.708(18) 1 d PRD A 1 F8 F 0.2120(3) 0.8573(4) 0.8669(4) 0.227(13) Uiso 0.708(18) 1 d PRD A 1 F9 F 0.2062(3) 0.8532(4) 0.9394(4) 0.314(19) Uiso 0.708(18) 1 d PRDU A 1 C93 C 0.3434(4) 0.0190(4) 0.2334(4) 0.088(10) Uani 0.64(2) 1 d PG B 1 C94 C 0.3206(3) -0.0226(5) 0.2522(3) 0.057(8) Uani 0.64(2) 1 d PGU B 1 C95 C 0.3339(3) -0.0698(4) 0.2314(4) 0.073(8) Uani 0.64(2) 1 d PG B 1 C96 C 0.3650(3) -0.0573(6) 0.1997(4) 0.064(8) Uani 0.64(2) 1 d PG B 1 C97 C 0.3708(3) -0.0025(6) 0.2009(3) 0.070(9) Uani 0.64(2) 1 d PG B 1 C98 C 0.3392(7) 0.0760(6) 0.2457(7) 0.140(14) Uani 0.64(2) 1 d PGU B 1 H98A H 0.3135 0.0886 0.2351 0.210 Uiso 0.64(2) 1 calc PR B 1 H98B H 0.3601 0.0958 0.2304 0.210 Uiso 0.64(2) 1 calc PR B 1 H98C H 0.3412 0.0803 0.2794 0.210 Uiso 0.64(2) 1 calc PR B 1 C99 C 0.2878(5) -0.0176(9) 0.2881(5) 0.141(15) Uani 0.64(2) 1 d PGU B 1 H99A H 0.2978 0.0012 0.3153 0.211 Uiso 0.64(2) 1 calc PR B 1 H99B H 0.2791 -0.0521 0.2976 0.211 Uiso 0.64(2) 1 calc PR B 1 H99C H 0.2657 0.0014 0.2746 0.211 Uiso 0.64(2) 1 calc PR B 1 C100 C 0.3179(6) -0.1237(6) 0.2413(7) 0.145(18) Uani 0.64(2) 1 d PG B 1 H10G H 0.3206 -0.1452 0.2135 0.218 Uiso 0.64(2) 1 calc PR B 1 H10H H 0.2900 -0.1212 0.2499 0.218 Uiso 0.64(2) 1 calc PR B 1 H10I H 0.3328 -0.1393 0.2669 0.218 Uiso 0.64(2) 1 calc PR B 1 C101 C 0.3878(5) -0.0957(10) 0.1699(6) 0.132(14) Uani 0.64(2) 1 d PGU B 1 H10J H 0.3699 -0.1225 0.1586 0.198 Uiso 0.64(2) 1 calc PR B 1 H10K H 0.4087 -0.1116 0.1885 0.198 Uiso 0.64(2) 1 calc PR B 1 H10L H 0.3995 -0.0775 0.1435 0.198 Uiso 0.64(2) 1 calc PR B 1 C102 C 0.4009(5) 0.0277(10) 0.1726(6) 0.22(3) Uani 0.64(2) 1 d PG B 1 H10M H 0.4259 0.0292 0.1896 0.325 Uiso 0.64(2) 1 calc PR B 1 H10N H 0.3912 0.0629 0.1673 0.325 Uiso 0.64(2) 1 calc PR B 1 H10O H 0.4051 0.0105 0.1427 0.325 Uiso 0.64(2) 1 calc PR B 1 C93' C 0.3312(4) 0.0174(4) 0.2430(4) 0.053(13) Uani 0.36(2) 1 d PGU B 2 C94' C 0.3217(3) -0.0359(5) 0.2485(3) 0.11(3) Uani 0.36(2) 1 d PGU B 2 C95' C 0.3461(3) -0.0648(4) 0.2180(4) 0.044(12) Uani 0.36(2) 1 d PGU B 2 C96' C 0.3708(3) -0.0295(6) 0.1937(3) 0.054(14) Uani 0.36(2) 1 d PGU B 2 C97' C 0.3615(4) 0.0213(5) 0.2092(4) 0.053(13) Uani 0.36(2) 1 d PGU B 2 C98' C 0.3123(6) 0.0620(7) 0.2687(6) 0.072(13) Uani 0.36(2) 1 d PGU B 2 H98D H 0.2938 0.0485 0.2919 0.108 Uiso 0.36(2) 1 calc PR B 2 H98E H 0.2981 0.0840 0.2466 0.108 Uiso 0.36(2) 1 calc PR B 2 H98F H 0.3328 0.0823 0.2843 0.108 Uiso 0.36(2) 1 calc PR B 2 C99' C 0.2909(5) -0.0578(9) 0.2810(5) 0.12(2) Uani 0.36(2) 1 d PGU B 2 H99D H 0.3023 -0.0616 0.3121 0.187 Uiso 0.36(2) 1 calc PR B 2 H99E H 0.2824 -0.0917 0.2696 0.187 Uiso 0.36(2) 1 calc PR B 2 H99F H 0.2683 -0.0344 0.2824 0.187 Uiso 0.36(2) 1 calc PR B 2 C10A C 0.3460(6) -0.1230(6) 0.2124(7) 0.096(17) Uani 0.36(2) 1 d PGU B 2 H10P H 0.3645 -0.1384 0.2346 0.144 Uiso 0.36(2) 1 calc PR B 2 H10Q H 0.3541 -0.1320 0.1808 0.144 Uiso 0.36(2) 1 calc PR B 2 H10R H 0.3195 -0.1363 0.2182 0.144 Uiso 0.36(2) 1 calc PR B 2 C10B C 0.4014(4) -0.0435(11) 0.1577(5) 0.087(16) Uani 0.36(2) 1 d PGU B 2 H10S H 0.3900 -0.0399 0.1266 0.130 Uiso 0.36(2) 1 calc PR B 2 H10T H 0.4100 -0.0793 0.1625 0.130 Uiso 0.36(2) 1 calc PR B 2 H10U H 0.4241 -0.0203 0.1607 0.130 Uiso 0.36(2) 1 calc PR B 2 C10C C 0.3806(6) 0.0708(8) 0.1925(7) 0.12(2) Uani 0.36(2) 1 d PGU B 2 H10V H 0.3867 0.0679 0.1594 0.180 Uiso 0.36(2) 1 calc PR B 2 H10W H 0.4049 0.0769 0.2100 0.180 Uiso 0.36(2) 1 calc PR B 2 H10X H 0.3625 0.0998 0.1974 0.180 Uiso 0.36(2) 1 calc PR B 2 O8' O 0.1599(10) 0.9293(8) 0.8909(16) 0.20(3) Uiso 0.292(18) 1 d PD A 2 O9' O 0.1193(8) 0.8562(13) 0.8731(12) 0.14(2) Uiso 0.292(18) 1 d PD A 2 O10' O 0.1349(11) 0.8754(18) 0.9520(8) 0.23(4) Uiso 0.292(18) 1 d PD A 2 F7' F 0.1795(15) 0.8030(15) 0.9336(11) 0.182(9) Uiso 0.292(18) 1 d PD A 2 F8' F 0.1872(13) 0.8131(15) 0.8618(9) 0.146(19) Uiso 0.292(18) 1 d PD A 2 F9' F 0.2225(5) 0.8561(14) 0.9089(18) 0.27(4) Uiso 0.292(18) 1 d PD A 2 C103 C 0.2897(4) 0.0623(5) -0.0524(5) 0.055(4) Uani 1 1 d . . . C104 C 0.2564(5) 0.0331(5) -0.0683(4) 0.056(4) Uani 1 1 d . . . C105 C 0.2215(5) 0.0646(6) -0.0602(5) 0.066(4) Uani 1 1 d . . . C106 C 0.2338(5) 0.1103(5) -0.0365(4) 0.065(4) Uani 1 1 d . . . C107 C 0.2765(4) 0.1092(5) -0.0314(4) 0.053(3) Uani 1 1 d . . . C108 C 0.3311(5) 0.0417(6) -0.0545(5) 0.069(4) Uani 1 1 d . . . H10A H 0.3308 0.0043 -0.0491 0.104 Uiso 1 1 calc R . . H10B H 0.3472 0.0586 -0.0306 0.104 Uiso 1 1 calc R . . H10C H 0.3424 0.0489 -0.0851 0.104 Uiso 1 1 calc R . . C109 C 0.2560(5) -0.0151(5) -0.0976(4) 0.063(4) Uani 1 1 d . . . H10D H 0.2714 -0.0092 -0.1259 0.095 Uiso 1 1 calc R . . H10E H 0.2288 -0.0236 -0.1060 0.095 Uiso 1 1 calc R . . H10F H 0.2675 -0.0438 -0.0800 0.095 Uiso 1 1 calc R . . C110 C 0.1824(6) 0.0520(7) -0.0723(5) 0.088(6) Uani 1 1 d . . . H11A H 0.1641 0.0714 -0.0526 0.132 Uiso 1 1 calc R . . H11B H 0.1781 0.0148 -0.0678 0.132 Uiso 1 1 calc R . . H11C H 0.1778 0.0608 -0.1049 0.132 Uiso 1 1 calc R . . C111 C 0.2081(6) 0.1572(6) -0.0265(5) 0.098(7) Uani 1 1 d . . . H11D H 0.1981 0.1714 -0.0557 0.146 Uiso 1 1 calc R . . H11E H 0.2238 0.1836 -0.0105 0.146 Uiso 1 1 calc R . . H11F H 0.1860 0.1469 -0.0068 0.146 Uiso 1 1 calc R . . C112 C 0.3014(6) 0.1517(6) -0.0134(5) 0.092(6) Uani 1 1 d . . . H11G H 0.3233 0.1371 0.0046 0.138 Uiso 1 1 calc R . . H11H H 0.2856 0.1742 0.0066 0.138 Uiso 1 1 calc R . . H11I H 0.3120 0.1718 -0.0394 0.138 Uiso 1 1 calc R . . C113 C 0.2409(5) 0.3475(7) 0.8299(5) 0.069(4) Uani 1 1 d . . . C114 C 0.1312(4) 0.2494(5) 0.5396(4) 0.036(3) Uani 1 1 d . . . C115 C 0.1875(4) 0.8393(6) 0.9023(6) 0.252(18) Uiso 1 1 d DU A . C116 C 0.0067(9) 0.9083(12) 0.1821(9) 0.151(9) Uani 1 1 d U . . 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 0.0629(4) 0.0552(3) 0.0461(3) -0.0087(2) -0.0060(3) 0.0160(3) Ir2 0.0666(4) 0.0584(4) 0.0662(4) -0.0085(3) -0.0261(3) 0.0153(3) Ir3 0.0605(4) 0.0634(4) 0.0423(3) -0.0032(2) -0.0007(3) 0.0011(3) Ir4 0.0772(4) 0.0454(3) 0.0311(3) -0.0002(2) 0.0102(2) 0.0031(3) Ag1 0.0691(7) 0.0541(6) 0.0465(6) -0.0048(5) -0.0067(5) -0.0006(6) N1 0.057(7) 0.051(7) 0.050(7) -0.011(5) -0.016(6) 0.005(6) N2 0.093(11) 0.064(8) 0.052(8) 0.004(6) 0.006(7) 0.006(8) N3 0.062(8) 0.068(8) 0.058(7) -0.012(6) -0.015(7) 0.014(7) N4 0.045(7) 0.065(7) 0.043(7) 0.003(5) -0.007(5) 0.008(6) N5 0.073(8) 0.054(7) 0.025(5) -0.004(5) -0.001(5) -0.004(6) N6 0.078(9) 0.050(7) 0.046(6) 0.003(5) -0.009(6) 0.016(6) N7 0.069(8) 0.051(7) 0.031(6) -0.010(5) 0.005(5) 0.000(6) N8 0.044(7) 0.058(7) 0.047(6) 0.002(5) 0.008(5) -0.007(6) N9 0.063(8) 0.030(6) 0.081(8) -0.006(5) 0.002(6) 0.001(6) N10 0.061(8) 0.062(7) 0.057(7) 0.002(6) 0.020(6) 0.004(7) N11 0.060(8) 0.041(6) 0.063(7) 0.000(5) -0.022(6) 0.010(6) N12 0.065(8) 0.037(6) 0.041(6) -0.004(5) 0.001(5) -0.009(5) N13 0.036(6) 0.081(8) 0.030(5) 0.001(5) -0.008(5) -0.001(6) N14 0.084(9) 0.059(7) 0.038(6) 0.005(5) -0.007(6) 0.014(7) N15 0.066(8) 0.045(6) 0.051(7) -0.003(5) 0.001(6) -0.006(6) N16 0.070(8) 0.051(7) 0.046(6) -0.004(5) 0.010(6) -0.016(6) O1 0.088(8) 0.071(7) 0.071(7) -0.007(5) 0.010(6) -0.030(6) O2 0.069(7) 0.116(9) 0.086(8) -0.027(7) 0.013(6) 0.009(7) O3 0.077(8) 0.060(6) 0.118(9) 0.028(6) 0.013(7) 0.014(6) O4 0.097(9) 0.083(7) 0.081(7) -0.006(6) -0.034(6) -0.028(7) O5 0.203(17) 0.073(8) 0.153(13) 0.045(8) 0.084(12) 0.075(10) O6 0.077(11) 0.23(2) 0.30(3) -0.083(19) -0.030(14) 0.052(13) O7 0.251(19) 0.127(11) 0.054(8) -0.024(7) 0.026(9) 0.058(12) O11 0.149(12) 0.094(9) 0.081(8) 0.039(7) -0.032(8) -0.050(8) O12 0.48(4) 0.109(12) 0.113(13) -0.043(11) 0.035(18) -0.062(18) O13 0.132(17) 0.44(5) 0.30(3) 0.20(3) 0.039(18) 0.09(2) S1 0.066(2) 0.058(2) 0.047(2) -0.0012(17) 0.0004(17) 0.0055(19) S2 0.110(4) 0.079(3) 0.070(3) -0.010(2) -0.002(3) 0.023(3) S3 0.159(7) 0.196(8) 0.184(7) -0.096(6) 0.075(6) -0.064(6) S4 0.104(4) 0.086(3) 0.081(3) 0.003(3) -0.023(3) -0.020(3) F1 0.098(7) 0.093(6) 0.072(6) -0.004(5) 0.004(5) 0.037(6) F2 0.087(7) 0.141(9) 0.086(7) -0.015(6) -0.018(6) -0.001(7) F3 0.122(9) 0.130(9) 0.085(7) 0.065(6) 0.007(6) 0.021(7) F4 0.150(11) 0.091(7) 0.124(9) -0.018(6) -0.031(8) 0.032(7) F5 0.244(17) 0.070(7) 0.204(14) -0.036(8) 0.123(13) -0.017(9) F6 0.209(15) 0.129(9) 0.076(8) -0.040(6) -0.032(8) 0.063(9) F10 0.29(2) 0.122(11) 0.131(11) 0.028(9) -0.043(12) -0.099(13) F11 0.285(19) 0.148(11) 0.152(11) 0.103(10) -0.129(12) -0.135(12) C1 0.065(10) 0.045(7) 0.042(7) -0.003(6) -0.019(7) 0.001(7) C2 0.037(8) 0.053(8) 0.060(9) -0.004(6) 0.003(7) -0.002(7) C3 0.058(9) 0.062(9) 0.063(10) -0.004(7) -0.006(8) -0.004(8) C4 0.090(13) 0.066(10) 0.048(9) -0.007(7) -0.011(8) 0.012(9) C5 0.100(14) 0.033(7) 0.063(9) -0.012(6) 0.022(9) 0.000(8) C6 0.063(10) 0.057(8) 0.041(8) -0.021(6) -0.007(7) -0.011(7) C7 0.059(9) 0.068(9) 0.035(7) 0.000(6) -0.016(7) 0.014(8) C8 0.030(7) 0.082(10) 0.048(8) -0.012(7) -0.003(6) 0.020(7) C9 0.043(9) 0.086(11) 0.065(10) -0.010(8) -0.008(8) 0.016(8) C10 0.093(15) 0.079(12) 0.141(18) 0.044(12) 0.046(13) 0.035(11) C11 0.050(11) 0.127(17) 0.131(18) 0.017(13) 0.024(11) -0.002(11) C12 0.120(19) 0.100(15) 0.118(18) 0.008(14) -0.003(16) 0.001(14) C13 0.084(14) 0.081(12) 0.100(15) -0.008(10) -0.010(12) -0.013(11) C14 0.048(10) 0.057(9) 0.109(14) -0.016(9) -0.016(10) 0.003(8) C15 0.057(9) 0.039(7) 0.047(8) 0.000(6) -0.002(6) -0.007(7) C16 0.065(10) 0.084(11) 0.033(7) -0.010(7) -0.015(6) -0.019(9) C17 0.100(13) 0.048(8) 0.054(9) -0.021(7) 0.011(8) -0.010(9) C18 0.081(11) 0.067(10) 0.055(9) -0.011(7) -0.022(8) 0.014(9) C19 0.072(10) 0.053(8) 0.053(8) -0.006(7) -0.003(7) -0.020(8) C20 0.052(8) 0.032(6) 0.032(6) -0.004(5) 0.004(6) -0.017(6) C21 0.056(9) 0.042(7) 0.037(7) 0.002(6) 0.004(6) 0.001(7) C22 0.057(9) 0.058(8) 0.049(8) -0.010(7) 0.000(7) -0.004(7) C23 0.070(10) 0.042(7) 0.048(8) -0.003(6) 0.009(7) 0.021(7) C24 0.104(14) 0.101(13) 0.033(8) 0.000(8) -0.002(8) 0.028(11) C25 0.145(18) 0.071(11) 0.072(11) -0.013(9) -0.022(11) 0.018(11) C26 0.111(15) 0.068(11) 0.061(10) -0.008(8) -0.004(9) 0.028(10) C27 0.100(12) 0.043(8) 0.058(9) 0.007(7) 0.018(8) 0.014(8) C28 0.070(10) 0.068(9) 0.030(7) 0.009(6) 0.020(6) 0.013(8) C29 0.074(11) 0.047(8) 0.058(9) -0.012(6) 0.009(8) -0.023(8) C30 0.093(12) 0.059(9) 0.047(8) -0.003(7) 0.009(8) -0.008(9) C31 0.096(15) 0.17(2) 0.054(11) 0.024(12) 0.016(10) -0.052(15) C32 0.123(18) 0.073(12) 0.091(14) 0.011(10) 0.000(13) -0.018(12) C33 0.061(10) 0.061(9) 0.049(8) -0.005(7) 0.002(7) -0.003(8) C34 0.125(16) 0.072(11) 0.043(9) -0.004(8) -0.007(10) -0.029(12) C35 0.079(12) 0.044(8) 0.108(14) 0.008(9) -0.053(11) -0.013(8) C36 0.107(14) 0.059(10) 0.052(9) -0.006(7) -0.010(8) -0.036(10) C37 0.082(10) 0.027(6) 0.037(7) 0.005(5) 0.010(7) 0.013(7) C38 0.054(9) 0.048(8) 0.049(8) 0.005(6) 0.000(7) -0.015(7) C39 0.052(9) 0.052(8) 0.051(8) -0.020(7) -0.011(7) -0.004(7) C40 0.059(9) 0.036(7) 0.040(7) 0.008(5) -0.011(6) -0.024(6) C41 0.056(9) 0.053(8) 0.036(7) -0.005(6) -0.001(6) 0.014(7) C42 0.045(9) 0.064(9) 0.057(9) 0.012(7) -0.006(7) -0.001(8) C43 0.062(11) 0.071(11) 0.116(14) -0.015(10) 0.016(10) -0.022(9) C44 0.024(8) 0.066(11) 0.167(18) -0.009(11) 0.036(10) 0.002(8) C45 0.073(13) 0.080(13) 0.160(19) -0.031(13) 0.039(12) -0.002(11) C46 0.036(7) 0.038(7) 0.044(7) -0.004(5) -0.012(6) -0.014(6) C47 0.054(9) 0.061(9) 0.059(9) -0.031(7) -0.015(7) 0.011(8) C48 0.091(12) 0.050(8) 0.055(9) 0.000(7) -0.006(8) -0.012(9) C49 0.067(11) 0.048(8) 0.074(10) -0.012(7) 0.010(8) -0.006(8) C50 0.094(13) 0.054(9) 0.056(9) -0.016(7) 0.035(8) -0.011(9) C51 0.045(9) 0.024(6) 0.090(11) -0.009(7) -0.001(8) -0.010(6) C52 0.087(13) 0.043(9) 0.106(13) 0.012(8) -0.028(11) -0.025(9) C53 0.072(12) 0.057(11) 0.124(16) 0.007(11) -0.022(12) -0.025(9) C54 0.16(2) 0.071(13) 0.101(16) 0.027(11) -0.074(16) -0.065(15) C55 0.077(12) 0.040(8) 0.096(13) 0.020(8) -0.016(11) -0.027(9) C56 0.115(16) 0.060(11) 0.062(11) 0.018(8) -0.016(11) -0.015(11) C57 0.115(16) 0.050(9) 0.071(11) 0.010(8) 0.007(11) -0.031(10) C58 0.071(10) 0.064(9) 0.044(8) 0.016(7) -0.014(7) -0.017(8) C59 0.075(10) 0.036(7) 0.040(7) 0.011(6) -0.011(7) -0.028(7) C60 0.073(11) 0.043(8) 0.070(10) 0.001(7) -0.031(9) -0.018(8) C61 0.039(8) 0.037(7) 0.066(9) 0.002(6) 0.000(7) -0.008(6) C62 0.066(10) 0.037(7) 0.044(7) 0.002(6) 0.001(7) -0.032(7) C63 0.046(9) 0.066(9) 0.058(9) 0.015(7) -0.015(7) 0.000(8) C64 0.046(9) 0.051(9) 0.074(10) -0.011(7) -0.003(7) -0.026(8) C65 0.120(19) 0.112(17) 0.121(17) -0.035(13) 0.016(14) 0.022(15) C66 0.041(9) 0.074(11) 0.146(16) -0.007(11) 0.030(10) -0.005(9) C67 0.075(12) 0.077(12) 0.101(13) -0.025(10) 0.032(10) -0.001(10) C68 0.058(9) 0.047(7) 0.031(6) -0.003(6) -0.005(6) -0.004(7) C69 0.080(10) 0.038(7) 0.031(6) -0.009(5) 0.006(7) 0.007(7) C70 0.067(10) 0.069(10) 0.058(9) 0.005(8) 0.008(8) -0.001(9) C71 0.095(13) 0.039(8) 0.078(11) 0.008(7) 0.009(9) -0.001(9) C72 0.093(12) 0.044(8) 0.050(8) 0.002(6) -0.002(8) 0.021(8) C73 0.075(12) 0.093(13) 0.063(10) -0.006(9) -0.023(9) 0.030(10) C74 0.095(14) 0.088(13) 0.062(10) -0.024(9) -0.012(9) 0.021(11) C75 0.081(12) 0.068(10) 0.048(8) -0.010(7) 0.002(8) 0.014(9) C76 0.074(11) 0.066(10) 0.041(8) -0.013(7) -0.010(7) 0.022(9) C77 0.077(12) 0.061(10) 0.062(9) -0.028(8) -0.018(8) 0.018(9) C78 0.129(18) 0.139(18) 0.089(13) -0.045(12) -0.045(12) 0.080(15) C79 0.075(13) 0.149(19) 0.098(14) 0.038(13) 0.015(11) -0.009(13) C80 0.096(13) 0.074(10) 0.055(9) 0.002(8) -0.008(8) 0.017(10) C81 0.089(13) 0.097(12) 0.048(9) -0.015(8) -0.007(8) 0.003(10) C82 0.143(19) 0.080(13) 0.127(17) -0.046(12) -0.065(14) 0.037(13) C83 0.095(13) 0.053(9) 0.085(12) -0.020(8) -0.064(11) 0.036(9) C84 0.056(10) 0.065(10) 0.106(13) -0.016(9) -0.043(10) 0.008(9) C85 0.095(14) 0.075(11) 0.070(10) -0.004(9) -0.051(10) 0.028(11) C86 0.072(12) 0.094(13) 0.086(13) -0.027(10) -0.052(11) 0.029(11) C87 0.16(2) 0.101(15) 0.051(10) -0.006(10) -0.049(13) 0.054(16) C88 0.107(18) 0.102(16) 0.20(3) -0.035(16) -0.091(18) 0.001(14) C89 0.062(11) 0.091(12) 0.109(14) -0.002(11) -0.017(10) 0.029(10) C90 0.089(13) 0.101(14) 0.096(13) 0.014(11) -0.026(11) -0.024(12) C91 0.16(2) 0.130(17) 0.075(12) 0.030(12) -0.016(13) 0.077(16) C92 0.21(3) 0.16(2) 0.064(12) -0.029(13) -0.039(14) 0.11(2) C93 0.09(2) 0.09(3) 0.08(2) -0.025(18) -0.02(2) 0.008(19) C94 0.052(13) 0.083(14) 0.036(11) 0.005(10) 0.014(9) 0.027(11) C95 0.041(14) 0.12(3) 0.061(16) 0.010(16) -0.011(13) -0.025(16) C96 0.065(17) 0.083(19) 0.044(14) -0.026(13) 0.022(12) -0.027(15) C97 0.048(16) 0.06(2) 0.10(2) -0.007(16) -0.051(15) 0.000(15) C98 0.16(2) 0.110(19) 0.15(2) -0.015(16) -0.029(17) -0.009(17) C99 0.15(2) 0.16(2) 0.12(2) 0.021(16) -0.012(16) 0.011(17) C100 0.14(3) 0.13(3) 0.17(4) 0.06(3) -0.08(3) -0.01(3) C101 0.114(19) 0.14(2) 0.140(19) -0.059(16) -0.026(15) 0.033(16) C102 0.10(3) 0.33(8) 0.22(5) 0.05(5) 0.01(3) -0.10(4) C93' 0.07(2) 0.05(2) 0.044(18) 0.006(15) -0.013(15) 0.005(16) C94' 0.12(3) 0.11(3) 0.10(3) 0.005(19) 0.000(19) 0.003(19) C95' 0.046(15) 0.048(14) 0.038(14) 0.013(9) -0.005(9) 0.003(9) C96' 0.045(19) 0.07(2) 0.045(18) -0.014(16) 0.009(15) -0.003(17) C97' 0.06(2) 0.044(19) 0.058(19) 0.025(15) -0.005(15) 0.019(15) C98' 0.09(2) 0.070(19) 0.058(18) 0.009(15) -0.006(16) 0.022(16) C99' 0.14(3) 0.12(3) 0.12(3) 0.019(18) 0.001(19) -0.004(19) C10A 0.13(3) 0.06(2) 0.10(2) 0.006(16) -0.023(18) 0.007(17) C10B 0.080(18) 0.092(18) 0.089(18) -0.004(10) 0.016(10) 0.000(10) C10C 0.09(3) 0.14(3) 0.12(3) 0.006(19) -0.026(18) -0.016(19) C103 0.056(10) 0.054(8) 0.054(8) 0.015(7) 0.017(7) -0.005(8) C104 0.079(11) 0.065(9) 0.025(6) 0.013(6) 0.006(6) 0.012(8) C105 0.083(13) 0.064(10) 0.052(9) 0.010(7) 0.011(8) 0.006(9) C106 0.118(14) 0.045(8) 0.033(7) 0.007(6) 0.034(8) 0.017(9) C107 0.061(10) 0.050(8) 0.048(8) 0.005(6) 0.021(7) -0.007(8) C108 0.080(12) 0.080(11) 0.047(8) 0.019(7) 0.005(8) -0.020(9) C109 0.087(11) 0.082(10) 0.022(6) -0.013(6) 0.003(6) 0.019(9) C110 0.105(15) 0.120(15) 0.039(9) 0.021(9) -0.001(9) 0.023(12) C111 0.173(19) 0.058(10) 0.062(10) 0.023(8) 0.041(11) 0.053(11) C112 0.145(18) 0.065(10) 0.066(10) 0.011(8) 0.026(11) -0.020(11) C113 0.067(11) 0.087(11) 0.052(9) 0.005(8) 0.006(8) 0.021(10) C114 0.042(7) 0.047(7) 0.021(6) -0.018(5) 0.002(5) 0.001(6) C116 0.163(17) 0.164(17) 0.126(14) 0.076(13) -0.070(13) -0.057(14) _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 N9 2.099(10) . ? Ir1 C75 2.114(15) . ? Ir1 N2 2.119(14) . ? Ir1 N1 2.160(11) . ? Ir1 C76 2.162(15) . ? Ir1 C77 2.176(14) . ? Ir1 C74 2.189(17) . ? Ir1 C73 2.200(16) . ? Ir2 C83 2.139(14) . ? Ir2 N13 2.140(12) . ? Ir2 N3 2.146(12) . ? Ir2 N4 2.155(10) . ? Ir2 C87 2.169(15) . ? Ir2 C84 2.170(15) . ? Ir2 C86 2.17(2) . ? Ir2 C85 2.193(16) . ? Ir3 N10 2.088(12) . ? Ir3 C95' 2.109(9) . ? Ir3 C96' 2.120(9) . ? Ir3 C93 2.151(9) . ? Ir3 C94' 2.152(9) . ? Ir3 C97' 2.170(10) . ? Ir3 C97 2.173(9) . ? Ir3 N5 2.174(10) . ? Ir3 N6 2.183(11) . ? Ir3 C93' 2.189(10) . ? Ir3 C94 2.194(9) . ? Ir3 C96 2.229(9) . ? Ir4 C106 2.126(13) . ? Ir4 N14 2.128(12) . ? Ir4 N8 2.135(10) . ? Ir4 C107 2.136(12) . ? Ir4 C104 2.145(12) . ? Ir4 N7 2.145(11) . ? Ir4 C103 2.163(12) . ? Ir4 C105 2.172(16) . ? Ag1 O1 2.388(10) . ? Ag1 N16 2.403(10) . ? Ag1 N12 2.430(10) . ? Ag1 N11 2.501(11) . ? Ag1 N15 2.506(11) . ? N1 C7 1.343(16) . ? N1 C1 1.407(18) . ? N2 C8 1.354(17) . ? N2 C9 1.372(19) . ? N3 C8 1.347(16) . ? N3 C14 1.38(2) . ? N4 C7 1.300(15) . ? N4 C6 1.393(17) . ? N5 C21 1.320(14) . ? N5 C15 1.394(16) . ? N6 C22 1.335(16) . ? N6 C23 1.384(15) . ? N7 C22 1.348(15) . ? N7 C28 1.409(16) . ? N8 C21 1.312(15) . ? N8 C20 1.406(14) . ? N9 C41 1.311(16) . ? N9 C45 1.39(2) . ? N10 C46 1.350(15) . ? N10 C50 1.404(17) . ? N11 C39 1.246(16) . ? N11 C42 1.385(17) . ? N12 C40 1.278(14) . ? N12 C47 1.456(16) . ? N13 C67 1.311(18) . ? N13 C63 1.381(17) . ? N14 C68 1.329(16) . ? N14 C72 1.330(16) . ? N15 C61 1.251(15) . ? N15 C64 1.392(17) . ? N16 C62 1.284(17) . ? N16 C69 1.375(16) . ? O2 S1 1.384(10) . ? O3 S1 1.404(10) . ? O4 S1 1.452(10) . ? O5 S2 1.397(14) . ? O6 S2 1.373(17) . ? O7 S2 1.392(12) . ? O11 S4 1.368(11) . ? O12 S4 1.362(16) . ? O13 S4 1.39(2) . ? S1 C113 1.781(15) . ? S2 C114 1.786(12) . ? S3 O8 1.381(10) . ? S3 O8' 1.406(17) . ? S3 O10 1.407(11) . ? S3 O9' 1.420(16) . ? S3 O10' 1.445(17) . ? S3 O9 1.497(12) . ? S3 C115 1.746(12) . ? S4 C116 1.62(3) . ? F1 C113 1.334(16) . ? F2 C113 1.358(18) . ? F3 C113 1.313(16) . ? F4 C114 1.396(16) . ? F5 C114 1.259(15) . ? F6 C114 1.258(14) . ? F10 C116 1.29(3) . ? F11 C116 1.30(2) . ? F12 C116 1.51(4) . ? C1 C2 1.383(19) . ? C1 C6 1.442(17) . ? C2 C3 1.327(18) . ? C3 C4 1.385(19) . ? C4 C5 1.33(2) . ? C5 C6 1.413(19) . ? C7 C8 1.401(19) . ? C9 C10 1.42(2) . ? C9 C14 1.44(2) . ? C10 C11 1.38(3) . ? C11 C12 1.45(3) . ? C12 C13 1.31(3) . ? C13 C14 1.46(2) . ? C15 C16 1.392(17) . ? C15 C20 1.407(16) . ? C16 C17 1.38(2) . ? C17 C18 1.396(19) . ? C18 C19 1.361(17) . ? C19 C20 1.423(18) . ? C21 C22 1.405(17) . ? C23 C24 1.399(19) . ? C23 C28 1.411(17) . ? C24 C25 1.37(2) . ? C25 C26 1.47(2) . ? C26 C27 1.336(19) . ? C27 C28 1.424(19) . ? C29 C30 1.372(19) . ? C29 C38 1.426(19) . ? C29 C39 1.519(19) . ? C30 C31 1.46(2) . ? C31 C32 1.35(3) . ? C32 C33 1.38(2) . ? C33 C34 1.41(2) . ? C33 C38 1.424(18) . ? C34 C35 1.35(2) . ? C35 C36 1.42(2) . ? C36 C37 1.35(2) . ? C37 C38 1.361(17) . ? C37 C40 1.483(16) . ? C39 C40 1.521(19) . ? C41 C42 1.398(18) . ? C42 C43 1.375(19) . ? C43 C44 1.38(2) . ? C44 C45 1.31(2) . ? C46 C47 1.312(17) . ? C47 C48 1.376(18) . ? C48 C49 1.33(2) . ? C49 C50 1.31(2) . ? C51 C60 1.371(19) . ? C51 C52 1.38(2) . ? C51 C61 1.494(19) . ? C52 C53 1.37(2) . ? C53 C54 1.31(3) . ? C54 C55 1.41(3) . ? C55 C60 1.36(2) . ? C55 C56 1.46(2) . ? C56 C57 1.30(2) . ? C57 C58 1.39(2) . ? C58 C59 1.384(19) . ? C59 C60 1.46(2) . ? C59 C62 1.466(17) . ? C61 C62 1.505(19) . ? C63 C64 1.382(19) . ? C64 C65 1.38(2) . ? C65 C66 1.37(2) . ? C66 C67 1.40(2) . ? C68 C69 1.412(18) . ? C69 C70 1.374(18) . ? C70 C71 1.35(2) . ? C71 C72 1.42(2) . ? C73 C74 1.36(2) . ? C73 C78 1.48(2) . ? C73 C77 1.53(2) . ? C74 C75 1.45(2) . ? C74 C79 1.51(2) . ? C75 C76 1.36(2) . ? C75 C80 1.53(2) . ? C76 C77 1.484(19) . ? C76 C81 1.52(2) . ? C77 C82 1.41(2) . ? C83 C87 1.43(3) . ? C83 C84 1.43(2) . ? C83 C88 1.50(3) . ? C84 C85 1.46(2) . ? C84 C89 1.49(2) . ? C85 C86 1.43(2) . ? C85 C90 1.50(2) . ? C86 C87 1.41(3) . ? C86 C91 1.48(3) . ? C87 C92 1.56(2) . ? F7 C115 1.250(13) . ? F8 C115 1.396(14) . ? F9 C115 1.294(14) . ? C93 C97 1.432(5) . ? C93 C94 1.433(5) . ? C93 C98 1.523(6) . ? C94 C95 1.432(5) . ? C94 C99 1.523(6) . ? C95 C96 1.433(5) . ? C95 C100 1.523(6) . ? C96 C97 1.433(5) . ? C96 C101 1.523(6) . ? C97 C102 1.523(6) . ? C93' C94' 1.422(5) . ? C93' C97' 1.423(5) . ? C93' C98' 1.512(6) . ? C94' C95' 1.423(5) . ? C94' C99' 1.512(6) . ? C95' C96' 1.423(5) . ? C95' C10A 1.513(6) . ? C96' C97' 1.423(5) . ? C96' C10B 1.512(6) . ? C97' C10C 1.512(6) . ? F7' C115 1.330(18) . ? F8' C115 1.350(18) . ? F9' C115 1.278(16) . ? C103 C107 1.428(18) . ? C103 C104 1.437(19) . ? C103 C108 1.50(2) . ? C104 C105 1.46(2) . ? C104 C109 1.505(18) . ? C105 C110 1.41(2) . ? C105 C106 1.42(2) . ? C106 C107 1.46(2) . ? C106 C111 1.521(18) . ? C107 C112 1.48(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 N9 Ir1 C75 92.3(5) . . ? N9 Ir1 N2 84.2(5) . . ? C75 Ir1 N2 145.3(6) . . ? N9 Ir1 N1 84.9(4) . . ? C75 Ir1 N1 134.7(5) . . ? N2 Ir1 N1 79.5(4) . . ? N9 Ir1 C76 115.3(5) . . ? C75 Ir1 C76 37.2(5) . . ? N2 Ir1 C76 160.0(5) . . ? N1 Ir1 C76 105.2(5) . . ? N9 Ir1 C77 155.2(5) . . ? C75 Ir1 C77 65.4(6) . . ? N2 Ir1 C77 120.2(5) . . ? N1 Ir1 C77 102.8(5) . . ? C76 Ir1 C77 40.0(5) . . ? N9 Ir1 C74 103.7(6) . . ? C75 Ir1 C74 39.5(6) . . ? N2 Ir1 C74 108.1(6) . . ? N1 Ir1 C74 168.9(6) . . ? C76 Ir1 C74 64.9(6) . . ? C77 Ir1 C74 66.4(7) . . ? N9 Ir1 C73 138.7(6) . . ? C75 Ir1 C73 62.9(6) . . ? N2 Ir1 C73 98.1(5) . . ? N1 Ir1 C73 136.2(6) . . ? C76 Ir1 C73 64.8(6) . . ? C77 Ir1 C73 40.9(6) . . ? C74 Ir1 C73 36.2(6) . . ? C83 Ir2 N13 105.1(5) . . ? C83 Ir2 N3 109.1(7) . . ? N13 Ir2 N3 83.1(4) . . ? C83 Ir2 N4 167.1(6) . . ? N13 Ir2 N4 86.1(4) . . ? N3 Ir2 N4 78.2(4) . . ? C83 Ir2 C87 38.6(7) . . ? N13 Ir2 C87 96.6(6) . . ? N3 Ir2 C87 146.7(8) . . ? N4 Ir2 C87 135.1(8) . . ? C83 Ir2 C84 38.9(5) . . ? N13 Ir2 C84 141.3(5) . . ? N3 Ir2 C84 95.5(6) . . ? N4 Ir2 C84 131.7(5) . . ? C87 Ir2 C84 64.2(7) . . ? C83 Ir2 C86 64.9(7) . . ? N13 Ir2 C86 121.0(5) . . ? N3 Ir2 C86 155.8(6) . . ? N4 Ir2 C86 104.0(6) . . ? C87 Ir2 C86 37.9(7) . . ? C84 Ir2 C86 64.7(7) . . ? C83 Ir2 C85 65.4(6) . . ? N13 Ir2 C85 158.9(5) . . ? N3 Ir2 C85 117.5(6) . . ? N4 Ir2 C85 101.8(5) . . ? C87 Ir2 C85 63.9(7) . . ? C84 Ir2 C85 39.2(6) . . ? C86 Ir2 C85 38.3(6) . . ? N10 Ir3 C95' 110.2(5) . . ? N10 Ir3 C96' 148.8(5) . . ? C95' Ir3 C96' 39.32(18) . . ? N10 Ir3 C93 128.0(5) . . ? C95' Ir3 C93 62.6(2) . . ? C96' Ir3 C93 53.9(2) . . ? N10 Ir3 C94' 94.7(4) . . ? C95' Ir3 C94' 38.99(17) . . ? C96' Ir3 C94' 65.2(3) . . ? C93 Ir3 C94' 45.3(2) . . ? N10 Ir3 C97' 152.8(5) . . ? C95' Ir3 C97' 65.1(3) . . ? C96' Ir3 C97' 38.71(18) . . ? C93 Ir3 C97' 24.91(12) . . ? C94' Ir3 C97' 64.4(3) . . ? N10 Ir3 C97 159.5(4) . . ? C95' Ir3 C97 52.2(2) . . ? C96' Ir3 C97 19.51(9) . . ? C93 Ir3 C97 38.68(17) . . ? C94' Ir3 C97 65.1(3) . . ? C97' Ir3 C97 19.38(9) . . ? N10 Ir3 N5 83.8(4) . . ? C95' Ir3 N5 163.1(4) . . ? C96' Ir3 N5 127.4(5) . . ? C93 Ir3 N5 101.6(4) . . ? C94' Ir3 N5 133.9(4) . . ? C97' Ir3 N5 98.1(4) . . ? C97 Ir3 N5 112.1(5) . . ? N10 Ir3 N6 84.1(4) . . ? C95' Ir3 N6 110.5(4) . . ? C96' Ir3 N6 99.7(4) . . ? C93 Ir3 N6 147.8(5) . . ? C94' Ir3 N6 146.6(4) . . ? C97' Ir3 N6 123.0(5) . . ? C97 Ir3 N6 110.7(5) . . ? N5 Ir3 N6 79.3(4) . . ? N10 Ir3 C93' 114.8(5) . . ? C95' Ir3 C93' 64.7(3) . . ? C96' Ir3 C93' 64.6(3) . . ? C93 Ir3 C93' 13.23(6) . . ? C94' Ir3 C93' 38.24(17) . . ? C97' Ir3 C93' 38.11(18) . . ? C97 Ir3 C93' 51.2(2) . . ? N5 Ir3 C93' 101.4(4) . . ? N6 Ir3 C93' 161.1(5) . . ? N10 Ir3 C94 96.5(4) . . ? C95' Ir3 C94 46.8(2) . . ? C96' Ir3 C94 67.7(3) . . ? C93 Ir3 C94 38.48(17) . . ? C94' Ir3 C94 9.5 . . ? C97' Ir3 C94 60.0(2) . . ? C97 Ir3 C94 64.1(2) . . ? N5 Ir3 C94 124.7(4) . . ? N6 Ir3 C94 156.0(4) . . ? C93' Ir3 C94 29.77(14) . . ? N10 Ir3 C96 128.9(5) . . ? C95' Ir3 C96 22.42(11) . . ? C96' Ir3 C96 20.07(10) . . ? C93 Ir3 C96 63.9(3) . . ? C94' Ir3 C96 57.5(2) . . ? C97' Ir3 C96 55.7(2) . . ? C97 Ir3 C96 37.96(17) . . ? N5 Ir3 C96 147.0(5) . . ? N6 Ir3 C96 97.7(4) . . ? C93' Ir3 C96 71.2(3) . . ? C94 Ir3 C96 63.2(2) . . ? C106 Ir4 N14 112.6(5) . . ? C106 Ir4 N8 106.4(5) . . ? N14 Ir4 N8 84.4(4) . . ? C106 Ir4 C107 40.0(6) . . ? N14 Ir4 C107 151.7(5) . . ? N8 Ir4 C107 96.5(5) . . ? C106 Ir4 C104 66.0(5) . . ? N14 Ir4 C104 114.4(5) . . ? N8 Ir4 C104 161.1(5) . . ? C107 Ir4 C104 66.3(5) . . ? C106 Ir4 N7 161.6(5) . . ? N14 Ir4 N7 85.3(4) . . ? N8 Ir4 N7 78.6(4) . . ? C107 Ir4 N7 122.7(5) . . ? C104 Ir4 N7 103.5(4) . . ? C106 Ir4 C103 65.3(5) . . ? N14 Ir4 C103 153.1(5) . . ? N8 Ir4 C103 122.3(5) . . ? C107 Ir4 C103 38.8(5) . . ? C104 Ir4 C103 39.0(5) . . ? N7 Ir4 C103 96.9(5) . . ? C106 Ir4 C105 38.7(5) . . ? N14 Ir4 C105 96.2(5) . . ? N8 Ir4 C105 142.1(5) . . ? C107 Ir4 C105 66.0(6) . . ? C104 Ir4 C105 39.5(5) . . ? N7 Ir4 C105 139.4(5) . . ? C103 Ir4 C105 65.0(6) . . ? O1 Ag1 N16 118.6(3) . . ? O1 Ag1 N12 118.5(4) . . ? N16 Ag1 N12 103.7(4) . . ? O1 Ag1 N11 85.2(3) . . ? N16 Ag1 N11 154.7(3) . . ? N12 Ag1 N11 68.3(3) . . ? O1 Ag1 N15 87.3(4) . . ? N16 Ag1 N15 70.1(4) . . ? N12 Ag1 N15 151.6(3) . . ? N11 Ag1 N15 105.0(4) . . ? C7 N1 C1 101.9(11) . . ? C7 N1 Ir1 111.0(9) . . ? C1 N1 Ir1 146.8(9) . . ? C8 N2 C9 99.4(12) . . ? C8 N2 Ir1 109.3(10) . . ? C9 N2 Ir1 149.9(10) . . ? C8 N3 C14 100.8(12) . . ? C8 N3 Ir2 111.8(10) . . ? C14 N3 Ir2 147.1(10) . . ? C7 N4 C6 102.6(11) . . ? C7 N4 Ir2 109.9(9) . . ? C6 N4 Ir2 146.8(8) . . ? C21 N5 C15 101.9(10) . . ? C21 N5 Ir3 109.8(8) . . ? C15 N5 Ir3 146.2(8) . . ? C22 N6 C23 103.6(11) . . ? C22 N6 Ir3 107.9(8) . . ? C23 N6 Ir3 145.8(9) . . ? C22 N7 C28 100.6(10) . . ? C22 N7 Ir4 110.2(8) . . ? C28 N7 Ir4 147.2(9) . . ? C21 N8 C20 101.8(10) . . ? C21 N8 Ir4 112.3(8) . . ? C20 N8 Ir4 145.4(9) . . ? C41 N9 C45 116.6(12) . . ? C41 N9 Ir1 124.6(10) . . ? C45 N9 Ir1 118.8(10) . . ? C46 N10 C50 113.5(12) . . ? C46 N10 Ir3 122.9(9) . . ? C50 N10 Ir3 123.5(10) . . ? C39 N11 C42 121.2(12) . . ? C39 N11 Ag1 114.3(9) . . ? C42 N11 Ag1 123.0(8) . . ? C40 N12 C47 116.6(11) . . ? C40 N12 Ag1 117.4(9) . . ? C47 N12 Ag1 126.0(8) . . ? C67 N13 C63 122.4(13) . . ? C67 N13 Ir2 117.0(10) . . ? C63 N13 Ir2 120.1(9) . . ? C68 N14 C72 121.5(13) . . ? C68 N14 Ir4 119.6(9) . . ? C72 N14 Ir4 119.0(10) . . ? C61 N15 C64 119.7(12) . . ? C61 N15 Ag1 111.8(9) . . ? C64 N15 Ag1 127.9(9) . . ? C62 N16 C69 116.0(11) . . ? C62 N16 Ag1 115.6(9) . . ? C69 N16 Ag1 128.3(9) . . ? O2 S1 O3 116.4(7) . . ? O2 S1 O4 112.4(7) . . ? O3 S1 O4 116.0(7) . . ? O2 S1 C113 103.2(7) . . ? O3 S1 C113 103.1(7) . . ? O4 S1 C113 103.3(8) . . ? O6 S2 O7 110.9(13) . . ? O6 S2 O5 115.2(13) . . ? O7 S2 O5 115.0(11) . . ? O6 S2 C114 103.1(9) . . ? O7 S2 C114 107.2(7) . . ? O5 S2 C114 104.1(7) . . ? O8 S3 O8' 52(2) . . ? O8 S3 O10 119.1(7) . . ? O8' S3 O10 144.4(16) . . ? O8 S3 O9' 148.7(15) . . ? O8' S3 O9' 115.8(16) . . ? O10 S3 O9' 50.9(17) . . ? O8 S3 O10' 64(2) . . ? O8' S3 O10' 114.7(16) . . ? O10 S3 O10' 62(2) . . ? O9' S3 O10' 112.8(16) . . ? O8 S3 O9 113.5(7) . . ? O8' S3 O9 62(2) . . ? O10 S3 O9 113.0(7) . . ? O9' S3 O9 62.4(18) . . ? O10' S3 O9 167.7(15) . . ? O8 S3 C115 107.2(8) . . ? O8' S3 C115 106.2(14) . . ? O10 S3 C115 109.1(8) . . ? O9' S3 C115 104.0(12) . . ? O10' S3 C115 101.3(13) . . ? O9 S3 C115 91.0(7) . . ? O12 S4 O11 122.9(11) . . ? O12 S4 O13 109.1(17) . . ? O11 S4 O13 115.1(12) . . ? O12 S4 C116 95.5(16) . . ? O11 S4 C116 110.8(10) . . ? O13 S4 C116 99.0(18) . . ? C2 C1 N1 134.5(12) . . ? C2 C1 C6 118.6(13) . . ? N1 C1 C6 106.9(12) . . ? C3 C2 C1 120.7(14) . . ? C2 C3 C4 122.2(15) . . ? C5 C4 C3 119.8(16) . . ? C4 C5 C6 121.3(16) . . ? N4 C6 C5 134.1(14) . . ? N4 C6 C1 108.5(12) . . ? C5 C6 C1 117.4(14) . . ? N4 C7 N1 120.2(13) . . ? N4 C7 C8 122.6(12) . . ? N1 C7 C8 117.0(12) . . ? N3 C8 N2 121.0(13) . . ? N3 C8 C7 116.7(12) . . ? N2 C8 C7 122.3(12) . . ? N2 C9 C10 130.4(16) . . ? N2 C9 C14 110.7(14) . . ? C10 C9 C14 119.0(16) . . ? C11 C10 C9 118(2) . . ? C10 C11 C12 123(2) . . ? C13 C12 C11 119(2) . . ? C12 C13 C14 121(2) . . ? N3 C14 C9 108.1(13) . . ? N3 C14 C13 132.5(17) . . ? C9 C14 C13 119.3(17) . . ? C16 C15 N5 131.5(12) . . ? C16 C15 C20 120.1(12) . . ? N5 C15 C20 108.3(10) . . ? C17 C16 C15 118.1(12) . . ? C16 C17 C18 122.3(13) . . ? C19 C18 C17 120.3(14) . . ? C18 C19 C20 118.6(13) . . ? N8 C20 C15 107.9(11) . . ? N8 C20 C19 131.5(11) . . ? C15 C20 C19 120.2(11) . . ? N8 C21 N5 120.0(11) . . ? N8 C21 C22 119.0(12) . . ? N5 C21 C22 120.3(12) . . ? N6 C22 N7 118.3(12) . . ? N6 C22 C21 122.1(12) . . ? N7 C22 C21 119.6(12) . . ? N6 C23 C24 131.7(12) . . ? N6 C23 C28 107.4(11) . . ? C24 C23 C28 120.9(12) . . ? C25 C24 C23 117.3(14) . . ? C24 C25 C26 122.2(15) . . ? C27 C26 C25 119.7(14) . . ? C26 C27 C28 118.8(14) . . ? N7 C28 C23 109.8(11) . . ? N7 C28 C27 129.1(12) . . ? C23 C28 C27 120.9(12) . . ? C30 C29 C38 122.9(14) . . ? C30 C29 C39 133.1(15) . . ? C38 C29 C39 103.5(11) . . ? C29 C30 C31 113.0(16) . . ? C32 C31 C30 126.1(18) . . ? C31 C32 C33 119.1(18) . . ? C32 C33 C34 124.1(16) . . ? C32 C33 C38 118.9(15) . . ? C34 C33 C38 117.0(13) . . ? C35 C34 C33 117.9(15) . . ? C34 C35 C36 123.9(17) . . ? C37 C36 C35 118.3(15) . . ? C36 C37 C38 119.3(12) . . ? C36 C37 C40 133.8(12) . . ? C38 C37 C40 106.5(12) . . ? C37 C38 C33 123.2(13) . . ? C37 C38 C29 116.8(12) . . ? C33 C38 C29 119.8(13) . . ? N11 C39 C29 132.9(13) . . ? N11 C39 C40 120.8(12) . . ? C29 C39 C40 106.2(11) . . ? N12 C40 C37 134.7(13) . . ? N12 C40 C39 118.2(11) . . ? C37 C40 C39 106.8(11) . . ? N9 C41 C42 124.5(13) . . ? C43 C42 N11 121.9(14) . . ? C43 C42 C41 116.4(14) . . ? N11 C42 C41 121.7(13) . . ? C42 C43 C44 119.4(15) . . ? C45 C44 C43 120.5(15) . . ? C44 C45 N9 122.5(16) . . ? C47 C46 N10 125.1(11) . . ? C46 C47 C48 117.9(13) . . ? C46 C47 N12 122.4(12) . . ? C48 C47 N12 119.6(14) . . ? C49 C48 C47 120.4(16) . . ? C50 C49 C48 119.6(14) . . ? C49 C50 N10 123.3(14) . . ? C60 C51 C52 113.6(15) . . ? C60 C51 C61 110.3(13) . . ? C52 C51 C61 135.9(14) . . ? C53 C52 C51 121.2(18) . . ? C54 C53 C52 121(2) . . ? C53 C54 C55 123.4(18) . . ? C60 C55 C54 111.8(18) . . ? C60 C55 C56 117.3(18) . . ? C54 C55 C56 130.8(19) . . ? C57 C56 C55 122.9(17) . . ? C56 C57 C58 120.2(17) . . ? C59 C58 C57 120.9(16) . . ? C58 C59 C60 118.5(12) . . ? C58 C59 C62 134.9(14) . . ? C60 C59 C62 106.6(13) . . ? C55 C60 C51 129.2(17) . . ? C55 C60 C59 120.1(16) . . ? C51 C60 C59 110.7(12) . . ? N15 C61 C51 133.3(13) . . ? N15 C61 C62 122.6(12) . . ? C51 C61 C62 104.0(11) . . ? N16 C62 C59 131.9(14) . . ? N16 C62 C61 119.9(12) . . ? C59 C62 C61 108.2(13) . . ? N13 C63 C64 118.9(13) . . ? C63 C64 C65 119.3(16) . . ? C63 C64 N15 117.7(13) . . ? C65 C64 N15 123.0(14) . . ? C66 C65 C64 120(2) . . ? C65 C66 C67 119.4(17) . . ? N13 C67 C66 119.7(15) . . ? N14 C68 C69 121.2(12) . . ? C70 C69 N16 123.3(13) . . ? C70 C69 C68 116.7(13) . . ? N16 C69 C68 120.0(11) . . ? C71 C70 C69 122.5(14) . . ? C70 C71 C72 117.9(13) . . ? N14 C72 C71 120.0(13) . . ? C74 C73 C78 126(2) . . ? C74 C73 C77 111.2(15) . . ? C78 C73 C77 122.4(17) . . ? C74 C73 Ir1 71.4(10) . . ? C78 C73 Ir1 126.7(11) . . ? C77 C73 Ir1 68.7(8) . . ? C73 C74 C75 105.9(17) . . ? C73 C74 C79 125.8(17) . . ? C75 C74 C79 128.2(17) . . ? C73 C74 Ir1 72.3(10) . . ? C75 C74 Ir1 67.5(9) . . ? C79 C74 Ir1 127.9(12) . . ? C76 C75 C74 111.9(14) . . ? C76 C75 C80 125.2(15) . . ? C74 C75 C80 122.5(16) . . ? C76 C75 Ir1 73.3(9) . . ? C74 C75 Ir1 73.0(9) . . ? C80 C75 Ir1 127.0(10) . . ? C75 C76 C77 109.0(14) . . ? C75 C76 C81 126.9(14) . . ? C77 C76 C81 124.0(15) . . ? C75 C76 Ir1 69.5(9) . . ? C77 C76 Ir1 70.5(8) . . ? C81 C76 Ir1 128.6(9) . . ? C82 C77 C76 127.3(17) . . ? C82 C77 C73 129.9(15) . . ? C76 C77 C73 101.7(14) . . ? C82 C77 Ir1 131.8(12) . . ? C76 C77 Ir1 69.5(8) . . ? C73 C77 Ir1 70.4(9) . . ? C87 C83 C84 107.4(18) . . ? C87 C83 C88 128.2(17) . . ? C84 C83 C88 123.6(19) . . ? C87 C83 Ir2 71.8(9) . . ? C84 C83 Ir2 71.7(8) . . ? C88 C83 Ir2 129.8(13) . . ? C83 C84 C85 107.8(16) . . ? C83 C84 C89 125.9(17) . . ? C85 C84 C89 126.2(14) . . ? C83 C84 Ir2 69.4(8) . . ? C85 C84 Ir2 71.3(9) . . ? C89 C84 Ir2 124.6(12) . . ? C86 C85 C84 106.7(16) . . ? C86 C85 C90 128.6(19) . . ? C84 C85 C90 124.3(16) . . ? C86 C85 Ir2 70.2(10) . . ? C84 C85 Ir2 69.6(9) . . ? C90 C85 Ir2 129.9(10) . . ? C87 C86 C85 108.6(18) . . ? C87 C86 C91 125.9(19) . . ? C85 C86 C91 125.2(19) . . ? C87 C86 Ir2 70.8(11) . . ? C85 C86 Ir2 71.5(11) . . ? C91 C86 Ir2 129.1(11) . . ? C86 C87 C83 109.4(16) . . ? C86 C87 C92 129(2) . . ? C83 C87 C92 122(2) . . ? C86 C87 Ir2 71.3(10) . . ? C83 C87 Ir2 69.5(8) . . ? C92 C87 Ir2 124.4(11) . . ? C97 C93 C94 108.0 . . ? C97 C93 C98 126.0 . . ? C94 C93 C98 126.0 . . ? C97 C93 Ir3 71.5(3) . . ? C94 C93 Ir3 72.4(3) . . ? C98 C93 Ir3 121.8(3) . . ? C95 C94 C93 108.0 . . ? C95 C94 C99 126.0 . . ? C93 C94 C99 126.0 . . ? C95 C94 Ir3 73.0(3) . . ? C93 C94 Ir3 69.1(3) . . ? C99 C94 Ir3 123.5(3) . . ? C94 C95 C96 108.0 . . ? C94 C95 C100 126.0 . . ? C96 C95 C100 126.0 . . ? C94 C95 Ir3 69.4(3) . . ? C96 C95 Ir3 70.8(3) . . ? C100 C95 Ir3 125.4(3) . . ? C97 C96 C95 108.0 . . ? C97 C96 C101 126.0 . . ? C95 C96 C101 126.0 . . ? C97 C96 Ir3 68.9(3) . . ? C95 C96 Ir3 71.8(3) . . ? C101 C96 Ir3 124.9(3) . . ? C93 C97 C96 108.0 . . ? C93 C97 C102 126.0 . . ? C96 C97 C102 126.0 . . ? C93 C97 Ir3 69.8(3) . . ? C96 C97 Ir3 73.1(3) . . ? C102 C97 Ir3 122.7(3) . . ? C94' C93' C97' 108.0 . . ? C94' C93' C98' 126.0 . . ? C97' C93' C98' 126.0 . . ? C94' C93' Ir3 69.5(3) . . ? C97' C93' Ir3 70.2(3) . . ? C98' C93' Ir3 125.9(3) . . ? C93' C94' C95' 108.0 . . ? C93' C94' C99' 126.0 . . ? C95' C94' C99' 126.0 . . ? C93' C94' Ir3 72.3(3) . . ? C95' C94' Ir3 68.9(3) . . ? C99' C94' Ir3 124.4(3) . . ? C94' C95' C96' 108.0 . . ? C94' C95' C10A 126.0 . . ? C96' C95' C10A 126.0 . . ? C94' C95' Ir3 72.1(3) . . ? C96' C95' Ir3 70.8(3) . . ? C10A C95' Ir3 122.8(3) . . ? C97' C96' C95' 108.0 . . ? C97' C96' C10B 126.0 . . ? C95' C96' C10B 126.0 . . ? C97' C96' Ir3 72.5(3) . . ? C95' C96' Ir3 69.9(3) . . ? C10B C96' Ir3 123.2(3) . . ? C96' C97' C93' 108.0 . . ? C96' C97' C10C 126.0 . . ? C93' C97' C10C 126.0 . . ? C96' C97' Ir3 68.8(3) . . ? C93' C97' Ir3 71.7(3) . . ? C10C C97' Ir3 125.1(3) . . ? C107 C103 C104 109.5(13) . . ? C107 C103 C108 127.7(14) . . ? C104 C103 C108 122.5(13) . . ? C107 C103 Ir4 69.6(7) . . ? C104 C103 Ir4 69.8(7) . . ? C108 C103 Ir4 122.5(9) . . ? C103 C104 C105 107.1(13) . . ? C103 C104 C109 128.5(13) . . ? C105 C104 C109 123.1(14) . . ? C103 C104 Ir4 71.2(7) . . ? C105 C104 Ir4 71.3(8) . . ? C109 C104 Ir4 132.7(9) . . ? C110 C105 C106 125.9(16) . . ? C110 C105 C104 126.5(15) . . ? C106 C105 C104 107.7(15) . . ? C110 C105 Ir4 126.0(10) . . ? C106 C105 Ir4 68.9(8) . . ? C104 C105 Ir4 69.3(8) . . ? C105 C106 C107 108.9(13) . . ? C105 C106 C111 125.8(17) . . ? C107 C106 C111 124.4(15) . . ? C105 C106 Ir4 72.4(8) . . ? C107 C106 Ir4 70.3(8) . . ? C111 C106 Ir4 132.2(9) . . ? C103 C107 C106 106.6(12) . . ? C103 C107 C112 126.8(14) . . ? C106 C107 C112 126.2(13) . . ? C103 C107 Ir4 71.6(7) . . ? C106 C107 Ir4 69.6(7) . . ? C112 C107 Ir4 129.4(10) . . ? F3 C113 F1 107.0(13) . . ? F3 C113 F2 101.3(12) . . ? F1 C113 F2 102.8(13) . . ? F3 C113 S1 116.3(12) . . ? F1 C113 S1 114.7(11) . . ? F2 C113 S1 113.1(11) . . ? F6 C114 F5 114.9(12) . . ? F6 C114 F4 102.5(12) . . ? F5 C114 F4 102.5(13) . . ? F6 C114 S2 113.4(10) . . ? F5 C114 S2 114.2(9) . . ? F4 C114 S2 107.6(8) . . ? F7 C115 F9' 112.8(18) . . ? F7 C115 F9 111.9(10) . . ? F9' C115 F9 48(2) . . ? F7 C115 F7' 49.8(19) . . ? F9' C115 F7' 109.2(18) . . ? F9 C115 F7' 75(2) . . ? F7 C115 F8' 54.4(18) . . ? F9' C115 F8' 108.0(18) . . ? F9 C115 F8' 149(2) . . ? F7' C115 F8' 103.3(17) . . ? F7 C115 F8 106.5(9) . . ? F9' C115 F8 56(2) . . ? F9 C115 F8 102.8(9) . . ? F7' C115 F8 149(2) . . ? F8' C115 F8 62.6(18) . . ? F7 C115 S3 124.9(10) . . ? F9' C115 S3 122.1(17) . . ? F9 C115 S3 101.5(8) . . ? F7' C115 S3 104(2) . . ? F8' C115 S3 109(2) . . ? F8 C115 S3 107.1(8) . . ? F10 C116 F11 102(2) . . ? F10 C116 F12 91.2(19) . . ? F11 C116 F12 107(3) . . ? F10 C116 S4 121(2) . . ? F11 C116 S4 123.1(18) . . ? F12 C116 S4 107(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.433 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.186 # Attachment '- 3b_1.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 888413' #TrackingRef '- 3b_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C117 H106 Ag F15 N16 O16 Rh4 S5' _chemical_formula_weight 2956.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 34.2162(8) _cell_length_b 25.9800(5) _cell_length_c 28.8348(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25632.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6059 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 67.93 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11920 _exptl_absorpt_coefficient_mu 6.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8484 _exptl_absorpt_correction_T_max 0.8760 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.17 _diffrn_reflns_number 124155 _diffrn_reflns_av_R_equivalents 0.1029 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 67.50 _reflns_number_total 22619 _reflns_number_gt 12878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In this data, 3 DFIX and 17 ISOR instructions were used to refine disordered Cp* and triflate groups so that there were 105 restraints. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.063 0.436 -0.042 7353.3 1916.8 2 0.250 0.250 -0.011 29.6 3.5 3 0.750 0.750 0.011 29.6 2.8 4 0.250 0.250 0.489 29.6 3.3 5 0.750 0.750 0.511 29.6 2.0 _platon_squeeze_details ; ; _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^)+(0.2000P)^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 constral _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22619 _refine_ls_number_parameters 1351 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.2919 _refine_ls_wR_factor_gt 0.2603 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.05306(2) 0.26735(3) 0.86023(2) 0.0491(2) Uani 1 1 d . . . Rh2 Rh -0.01687(2) 0.22007(3) 0.68944(3) 0.0542(2) Uani 1 1 d . . . Rh3 Rh 0.30966(2) 0.51226(3) 0.67634(2) 0.0511(2) Uani 1 1 d . . . Rh4 Rh 0.24985(2) 0.45248(2) 0.50362(2) 0.0465(2) Uani 1 1 d . . . Ag1 Ag 0.11567(4) 0.43021(5) 0.68167(4) 0.0967(4) Uani 1 1 d . . . N1 N 0.0687(4) 0.2384(5) 0.7911(4) 0.082(3) Uani 1 1 d . . . N2 N -0.0045(5) 0.2491(5) 0.8315(5) 0.109(5) Uani 1 1 d . . . N3 N -0.0321(4) 0.2347(6) 0.7607(5) 0.095(4) Uani 1 1 d . . . N4 N 0.0404(4) 0.2211(5) 0.7224(4) 0.085(3) Uani 1 1 d . . . N5 N 0.3099(4) 0.5384(5) 0.6047(5) 0.097(4) Uani 1 1 d . . . N6 N 0.2844(5) 0.4429(5) 0.6416(4) 0.095(4) Uani 1 1 d . . . N7 N 0.2594(4) 0.4222(5) 0.5722(4) 0.088(3) Uani 1 1 d . . . N8 N 0.2832(4) 0.5145(5) 0.5358(4) 0.093(4) Uani 1 1 d . . . N9 N 0.0445(5) 0.3391(5) 0.8272(5) 0.104(4) Uani 1 1 d . . . N10 N 0.2526(4) 0.5386(5) 0.6762(5) 0.096(4) Uani 1 1 d . . . N11 N 0.0987(4) 0.4391(5) 0.7638(5) 0.098(4) Uani 1 1 d . . . N12 N 0.1554(4) 0.4947(5) 0.7196(5) 0.096(4) Uani 1 1 d . . . N13 N -0.0130(5) 0.3035(7) 0.6891(4) 0.114(5) Uani 1 1 d . . . N14 N 0.2002(4) 0.4886(5) 0.5348(4) 0.095(4) Uani 1 1 d . . . N15 N 0.0540(4) 0.4025(5) 0.6455(5) 0.095(4) Uani 1 1 d . . . N16 N 0.1138(4) 0.4567(5) 0.6017(4) 0.093(4) Uani 1 1 d . . . O1 O 0.1277(5) 0.3424(5) 0.6997(5) 0.093(6) Uani 0.72(3) 1 d P . . O1' O 0.168(4) 0.371(4) 0.675(4) 0.27(6) Uani 0.28(3) 1 d PU . . O2 O 0.1815(6) 0.3958(10) 0.8497(7) 0.204(10) Uani 1 1 d . . . O3 O 0.2158(6) 0.4224(5) 0.7834(7) 0.165(7) Uani 1 1 d . . . O4 O 0.1754(5) 0.3461(6) 0.7838(6) 0.160(6) Uani 1 1 d . . . O5 O 0.1079(8) 0.3021(8) 0.6087(7) 0.219(11) Uani 1 1 d . . . O6 O 0.1273(8) 0.3458(7) 0.5380(8) 0.223(11) Uani 1 1 d . . . O7 O 0.0663(7) 0.2969(16) 0.5456(13) 0.36(2) Uani 1 1 d . . . S1 S 0.19947(15) 0.38284(17) 0.80832(15) 0.0996(12) Uani 1 1 d . . . S2 S 0.1054(2) 0.3041(2) 0.5593(2) 0.1293(18) Uani 1 1 d . . . F1 F 0.2613(4) 0.3232(6) 0.7954(5) 0.152(5) Uani 1 1 d . . . F2 F 0.2667(5) 0.3747(6) 0.8493(5) 0.166(5) Uani 1 1 d . . . F3 F 0.2317(6) 0.3127(7) 0.8613(5) 0.197(7) Uani 1 1 d . . . F4 F 0.1345(8) 0.2491(8) 0.4946(5) 0.238(10) Uani 1 1 d . . . F5 F 0.1693(6) 0.2487(6) 0.5547(7) 0.199(7) Uani 1 1 d . . . F6 F 0.1155(6) 0.2080(7) 0.5548(8) 0.221(8) Uani 1 1 d U . . C1 C 0.0976(5) 0.2310(6) 0.7584(5) 0.085(4) Uani 1 1 d . . . C2 C 0.1387(5) 0.2300(6) 0.7626(6) 0.089(4) Uani 1 1 d . . . H2 H 0.1506 0.2382 0.7914 0.106 Uiso 1 1 calc R . . C3 C 0.1620(7) 0.2167(7) 0.7241(7) 0.122(7) Uani 1 1 d . . . H3 H 0.1896 0.2144 0.7274 0.147 Uiso 1 1 calc R . . C4 C 0.1448(6) 0.2070(7) 0.6813(6) 0.105(5) Uani 1 1 d . . . H4 H 0.1607 0.1990 0.6552 0.126 Uiso 1 1 calc R . . C5 C 0.1030(6) 0.2092(6) 0.6765(6) 0.099(5) Uani 1 1 d . . . H5 H 0.0913 0.2036 0.6470 0.119 Uiso 1 1 calc R . . C6 C 0.0798(5) 0.2193(5) 0.7147(5) 0.081(4) Uani 1 1 d . . . C7 C 0.0388(5) 0.2341(6) 0.7663(5) 0.089(4) Uani 1 1 d . . . C8 C 0.0005(5) 0.2390(6) 0.7857(5) 0.085(4) Uani 1 1 d . . . C9 C -0.0453(5) 0.2556(8) 0.8373(6) 0.109(6) Uani 1 1 d . . . C10 C -0.0635(7) 0.2678(9) 0.8764(9) 0.141(8) Uani 1 1 d . . . H10 H -0.0507 0.2764 0.9045 0.169 Uiso 1 1 calc R . . C11 C -0.1078(10) 0.2663(12) 0.8702(11) 0.184(12) Uani 1 1 d DU . . H11 H -0.1240 0.2733 0.8962 0.221 Uiso 1 1 calc R . . C12 C -0.1260(10) 0.2545(14) 0.8264(11) 0.192(12) Uani 1 1 d DU . . H12 H -0.1537 0.2525 0.8252 0.230 Uiso 1 1 calc R . . C13 C -0.1032(7) 0.2453(9) 0.7826(9) 0.137(8) Uani 1 1 d . . . H13 H -0.1144 0.2403 0.7528 0.164 Uiso 1 1 calc R . . C14 C -0.0615(5) 0.2453(8) 0.7929(8) 0.112(6) Uani 1 1 d . . . C15 C 0.3116(5) 0.5812(6) 0.5748(6) 0.094(4) Uani 1 1 d . . . C16 C 0.3236(7) 0.6293(8) 0.5826(6) 0.135(8) Uani 1 1 d . . . H16 H 0.3343 0.6389 0.6117 0.161 Uiso 1 1 calc R . . C17 C 0.3196(8) 0.6651(8) 0.5466(7) 0.148(9) Uani 1 1 d . . . H17 H 0.3244 0.7006 0.5521 0.178 Uiso 1 1 calc R . . C18 C 0.3084(9) 0.6479(8) 0.5015(8) 0.154(10) Uani 1 1 d . . . H18 H 0.3115 0.6706 0.4760 0.185 Uiso 1 1 calc R . . C19 C 0.2929(7) 0.5989(7) 0.4934(7) 0.128(7) Uani 1 1 d . . . H19 H 0.2828 0.5884 0.4643 0.153 Uiso 1 1 calc R . . C20 C 0.2937(5) 0.5670(6) 0.5321(5) 0.093(4) Uani 1 1 d . . . C21 C 0.2943(6) 0.5025(6) 0.5794(5) 0.098(5) Uani 1 1 d . . . C22 C 0.2809(5) 0.4550(5) 0.5983(5) 0.082(4) Uani 1 1 d . . . C23 C 0.2649(5) 0.4001(6) 0.6488(5) 0.089(4) Uani 1 1 d . . . C24 C 0.2584(5) 0.3684(6) 0.6842(6) 0.096(5) Uani 1 1 d . . . H24 H 0.2707 0.3761 0.7129 0.116 Uiso 1 1 calc R . . C25 C 0.2351(6) 0.3252(7) 0.6822(7) 0.119(6) Uani 1 1 d . . . H25 H 0.2279 0.3063 0.7091 0.142 Uiso 1 1 calc R . . C26 C 0.2232(6) 0.3115(7) 0.6383(6) 0.103(5) Uani 1 1 d . . . H26 H 0.2102 0.2794 0.6352 0.123 Uiso 1 1 calc R . . C27 C 0.2282(6) 0.3397(6) 0.5985(6) 0.104(5) Uani 1 1 d . . . H27 H 0.2174 0.3296 0.5696 0.124 Uiso 1 1 calc R . . C28 C 0.2498(4) 0.3834(5) 0.6038(4) 0.072(3) Uani 1 1 d . . . C29 C 0.1403(5) 0.5419(6) 0.8332(6) 0.092(4) Uani 1 1 d . . . C30 C 0.1627(6) 0.5450(5) 0.7941(6) 0.094(5) Uani 1 1 d . . . C31 C 0.1890(7) 0.5827(8) 0.7924(7) 0.125(7) Uani 1 1 d . . . H31 H 0.2049 0.5864 0.7655 0.150 Uiso 1 1 calc R . . C32 C 0.1938(6) 0.6178(7) 0.8301(8) 0.120(6) Uani 1 1 d U . . H32 H 0.2127 0.6446 0.8282 0.144 Uiso 1 1 calc R . . C33 C 0.1695(8) 0.6124(8) 0.8717(7) 0.128(7) Uani 1 1 d . . . H33 H 0.1727 0.6353 0.8971 0.154 Uiso 1 1 calc R . . C34 C 0.1423(6) 0.5744(7) 0.8735(6) 0.100(5) Uani 1 1 d . . . C35 C 0.1137(8) 0.5675(10) 0.9098(8) 0.139(8) Uani 1 1 d U . . H35 H 0.1129 0.5902 0.9355 0.167 Uiso 1 1 calc R . . C36 C 0.0887(7) 0.5289(9) 0.9065(7) 0.123(6) Uani 1 1 d U . . H36 H 0.0711 0.5246 0.9318 0.147 Uiso 1 1 calc R . . C37 C 0.0849(7) 0.4918(8) 0.8679(7) 0.125(7) Uani 1 1 d . . . H37 H 0.0665 0.4645 0.8691 0.150 Uiso 1 1 calc R . . C38 C 0.1095(5) 0.4982(6) 0.8298(6) 0.099(5) Uani 1 1 d . . . C39 C 0.1160(5) 0.4750(6) 0.7854(6) 0.091(4) Uani 1 1 d . . . C40 C 0.1481(6) 0.5051(6) 0.7626(5) 0.094(5) Uani 1 1 d . . . C41 C 0.0721(5) 0.3640(6) 0.8054(6) 0.091(4) Uani 1 1 d . . . H41 H 0.0966 0.3474 0.8015 0.110 Uiso 1 1 calc R . . C42 C 0.0677(5) 0.4136(7) 0.7874(7) 0.109(5) Uani 1 1 d . . . C43 C 0.0298(6) 0.4380(9) 0.7924(10) 0.146(9) Uani 1 1 d . . . H43 H 0.0242 0.4709 0.7795 0.175 Uiso 1 1 calc R . . C44 C 0.0035(6) 0.4111(7) 0.8162(9) 0.127(7) Uani 1 1 d . . . H44 H -0.0209 0.4274 0.8218 0.153 Uiso 1 1 calc R . . C45 C 0.0076(7) 0.3638(8) 0.8331(9) 0.142(9) Uani 1 1 d . . . H45 H -0.0133 0.3470 0.8485 0.170 Uiso 1 1 calc R . . C46 C 0.2428(6) 0.5844(7) 0.6606(6) 0.105(6) Uani 1 1 d . . . H46 H 0.2629 0.6057 0.6485 0.126 Uiso 1 1 calc R . . C47 C 0.2032(6) 0.6046(7) 0.6606(7) 0.120(6) Uani 1 1 d . . . H47 H 0.1971 0.6377 0.6486 0.143 Uiso 1 1 calc R . . C48 C 0.1742(7) 0.5716(7) 0.6800(7) 0.117(6) Uani 1 1 d . . . H48 H 0.1475 0.5814 0.6792 0.140 Uiso 1 1 calc R . . C49 C 0.1845(5) 0.5271(5) 0.6990(6) 0.089(4) Uani 1 1 d . . . C50 C 0.2221(5) 0.5092(5) 0.6950(5) 0.082(4) Uani 1 1 d . . . H50 H 0.2277 0.4753 0.7055 0.099 Uiso 1 1 calc R . . C51 C 0.0326(6) 0.4328(7) 0.5262(6) 0.103(5) Uani 1 1 d . . . C52 C 0.0718(5) 0.4555(6) 0.5313(6) 0.094(4) Uani 1 1 d . . . C53 C 0.0893(7) 0.4757(8) 0.4931(6) 0.116(6) Uani 1 1 d . . . H53 H 0.1154 0.4881 0.4954 0.139 Uiso 1 1 calc R . . C54 C 0.0702(7) 0.4785(9) 0.4510(6) 0.125(7) Uani 1 1 d . . . H54 H 0.0842 0.4914 0.4251 0.150 Uiso 1 1 calc R . . C55 C 0.0323(9) 0.4640(7) 0.4445(7) 0.132(8) Uani 1 1 d . . . H55 H 0.0194 0.4701 0.4158 0.159 Uiso 1 1 calc R . . C56 C 0.0111(7) 0.4378(6) 0.4844(8) 0.117(6) Uani 1 1 d . . . C57 C -0.0247(8) 0.4176(10) 0.4895(10) 0.144(8) Uani 1 1 d U . . H57 H -0.0414 0.4214 0.4634 0.172 Uiso 1 1 calc R . . C58 C -0.0404(7) 0.3934(9) 0.5250(8) 0.127(7) Uani 1 1 d U . . H58 H -0.0653 0.3772 0.5234 0.153 Uiso 1 1 calc R . . C59 C -0.0186(7) 0.3933(7) 0.5637(8) 0.124(7) Uani 1 1 d . . . H59 H -0.0300 0.3788 0.5907 0.149 Uiso 1 1 calc R . . C60 C 0.0197(6) 0.4126(6) 0.5679(8) 0.110(6) Uani 1 1 d . . . C61 C 0.0497(5) 0.4166(7) 0.6027(6) 0.095(4) Uani 1 1 d . . . C62 C 0.0840(5) 0.4441(5) 0.5796(5) 0.088(4) Uani 1 1 d . . . C63 C -0.0442(6) 0.3306(8) 0.7052(8) 0.130(8) Uani 1 1 d . . . H63 H -0.0662 0.3148 0.7192 0.155 Uiso 1 1 calc R . . C64 C -0.0408(7) 0.3838(10) 0.6994(11) 0.159(10) Uani 1 1 d . . . H64 H -0.0626 0.4037 0.7091 0.190 Uiso 1 1 calc R . . C65 C -0.0105(9) 0.4102(8) 0.6818(10) 0.167(12) Uani 1 1 d . . . H65 H -0.0099 0.4468 0.6806 0.201 Uiso 1 1 calc R . . C66 C 0.0210(5) 0.3792(7) 0.6649(7) 0.102(5) Uani 1 1 d . . . C67 C 0.0205(6) 0.3256(8) 0.6677(6) 0.110(6) Uani 1 1 d . . . H67 H 0.0413 0.3051 0.6560 0.132 Uiso 1 1 calc R . . C68 C 0.1757(5) 0.4623(7) 0.5600(5) 0.089(4) Uani 1 1 d . . . H68 H 0.1805 0.4269 0.5660 0.107 Uiso 1 1 calc R . . C69 C 0.1430(5) 0.4853(6) 0.5781(6) 0.093(4) Uani 1 1 d . . . C70 C 0.1373(6) 0.5375(7) 0.5737(7) 0.116(6) Uani 1 1 d . . . H70 H 0.1146 0.5532 0.5862 0.139 Uiso 1 1 calc R . . C71 C 0.1661(6) 0.5681(7) 0.5498(7) 0.112(6) Uani 1 1 d . . . H71 H 0.1644 0.6045 0.5478 0.135 Uiso 1 1 calc R . . C72 C 0.1960(6) 0.5407(6) 0.5303(6) 0.111(6) Uani 1 1 d . . . H72 H 0.2149 0.5590 0.5127 0.133 Uiso 1 1 calc R . . C73 C 0.0447(8) 0.2313(10) 0.9281(8) 0.131(8) Uani 1 1 d . . . C74 C 0.0827(8) 0.2140(7) 0.9079(7) 0.121(7) Uani 1 1 d . . . C75 C 0.1058(5) 0.2598(7) 0.8995(5) 0.098(5) Uani 1 1 d . . . C76 C 0.0854(6) 0.3014(7) 0.9169(6) 0.106(5) Uani 1 1 d . . . C77 C 0.0475(6) 0.2831(9) 0.9343(5) 0.109(6) Uani 1 1 d . . . C78 C 0.0163(7) 0.2013(10) 0.9452(9) 0.156(10) Uani 1 1 d . . . H78A H 0.0189 0.1990 0.9789 0.233 Uiso 1 1 calc R . . H78B H 0.0183 0.1668 0.9316 0.233 Uiso 1 1 calc R . . H78C H -0.0092 0.2162 0.9374 0.233 Uiso 1 1 calc R . . C79 C 0.0961(10) 0.1591(8) 0.8940(11) 0.220(18) Uani 1 1 d . . . H79A H 0.1085 0.1424 0.9206 0.330 Uiso 1 1 calc R . . H79B H 0.1149 0.1614 0.8684 0.330 Uiso 1 1 calc R . . H79C H 0.0734 0.1389 0.8841 0.330 Uiso 1 1 calc R . . C80 C 0.1502(6) 0.2574(8) 0.8828(7) 0.125(7) Uani 1 1 d . . . H80A H 0.1603 0.2925 0.8792 0.187 Uiso 1 1 calc R . . H80B H 0.1517 0.2394 0.8530 0.187 Uiso 1 1 calc R . . H80C H 0.1658 0.2389 0.9059 0.187 Uiso 1 1 calc R . . C81 C 0.1017(7) 0.3555(7) 0.9201(8) 0.135(8) Uani 1 1 d . . . H81A H 0.1260 0.3550 0.9380 0.202 Uiso 1 1 calc R . . H81B H 0.0827 0.3779 0.9356 0.202 Uiso 1 1 calc R . . H81C H 0.1069 0.3686 0.8888 0.202 Uiso 1 1 calc R . . C82 C 0.0153(9) 0.3193(12) 0.9584(11) 0.193(12) Uani 1 1 d U . . H82A H 0.0196 0.3197 0.9920 0.289 Uiso 1 1 calc R . . H82B H -0.0108 0.3059 0.9517 0.289 Uiso 1 1 calc R . . H82C H 0.0177 0.3543 0.9462 0.289 Uiso 1 1 calc R . . C83 C -0.0342(9) 0.2129(10) 0.6134(10) 0.149(10) Uani 1 1 d . . . C84 C -0.0079(7) 0.1793(9) 0.6258(7) 0.118(6) Uani 1 1 d . . . C85 C -0.0194(6) 0.1414(9) 0.6639(7) 0.127(7) Uani 1 1 d D . . C86 C -0.0571(7) 0.1619(9) 0.6790(8) 0.139(8) Uani 1 1 d DU . . C87 C -0.0688(7) 0.2055(7) 0.6502(7) 0.113(6) Uani 1 1 d . . . C88 C -0.0350(9) 0.2577(10) 0.5840(8) 0.174(12) Uani 1 1 d . . . H88A H -0.0308 0.2886 0.6028 0.261 Uiso 1 1 calc R . . H88B H -0.0605 0.2600 0.5685 0.261 Uiso 1 1 calc R . . H88C H -0.0143 0.2550 0.5606 0.261 Uiso 1 1 calc R . . C89 C 0.0307(8) 0.1685(10) 0.5963(7) 0.148(9) Uani 1 1 d . . . H89A H 0.0242 0.1464 0.5698 0.221 Uiso 1 1 calc R . . H89B H 0.0501 0.1512 0.6158 0.221 Uiso 1 1 calc R . . H89C H 0.0413 0.2012 0.5850 0.221 Uiso 1 1 calc R . . C90 C 0.0001(7) 0.0946(8) 0.6785(8) 0.132(7) Uani 1 1 d . . . H90A H 0.0015 0.0705 0.6524 0.198 Uiso 1 1 calc R . . H90B H -0.0145 0.0788 0.7040 0.198 Uiso 1 1 calc R . . H90C H 0.0267 0.1028 0.6890 0.198 Uiso 1 1 calc R . . C91 C -0.0849(7) 0.1344(9) 0.7097(7) 0.140(8) Uani 1 1 d D . . H91A H -0.0892 0.1547 0.7379 0.210 Uiso 1 1 calc R . . H91B H -0.0740 0.1008 0.7181 0.210 Uiso 1 1 calc R . . H91C H -0.1098 0.1296 0.6935 0.210 Uiso 1 1 calc R . . C92 C -0.1048(9) 0.2317(11) 0.6470(10) 0.186(13) Uani 1 1 d . . . H92A H -0.1117 0.2366 0.6143 0.279 Uiso 1 1 calc R . . H92B H -0.1026 0.2654 0.6622 0.279 Uiso 1 1 calc R . . H92C H -0.1252 0.2115 0.6624 0.279 Uiso 1 1 calc R . . C93 C 0.3365(4) 0.4775(5) 0.7387(4) 0.130(7) Uani 1 1 d GU . . C94 C 0.3655(4) 0.4870(6) 0.7044(5) 0.149(10) Uani 1 1 d G . . C95 C 0.3660(4) 0.5408(6) 0.6953(4) 0.158(9) Uani 1 1 d GU . . C96 C 0.3374(4) 0.5644(5) 0.7239(4) 0.128(7) Uani 1 1 d GU . . C97 C 0.3191(4) 0.5253(5) 0.7507(4) 0.113(6) Uani 1 1 d GU . . C98 C 0.3261(7) 0.4256(7) 0.7588(7) 0.30(2) Uani 1 1 d GU . . H98A H 0.3421 0.4190 0.7863 0.443 Uiso 1 1 calc R . . H98B H 0.3309 0.3987 0.7356 0.443 Uiso 1 1 calc R . . H98C H 0.2984 0.4254 0.7675 0.443 Uiso 1 1 calc R . . C99 C 0.3912(6) 0.4470(9) 0.6817(8) 0.39(4) Uani 1 1 d GU . . H99A H 0.3766 0.4148 0.6784 0.583 Uiso 1 1 calc R . . H99B H 0.4144 0.4412 0.7010 0.583 Uiso 1 1 calc R . . H99C H 0.3993 0.4592 0.6510 0.583 Uiso 1 1 calc R . . C100 C 0.3924(6) 0.5679(10) 0.6612(6) 0.81(12) Uani 1 1 d G . . H10A H 0.4168 0.5776 0.6766 1.208 Uiso 1 1 calc R . . H10B H 0.3793 0.5989 0.6496 1.208 Uiso 1 1 calc R . . H10C H 0.3982 0.5449 0.6352 1.208 Uiso 1 1 calc R . . C101 C 0.3280(7) 0.6212(6) 0.7255(8) 0.33(3) Uani 1 1 d G . . H10D H 0.3007 0.6259 0.7350 0.497 Uiso 1 1 calc R . . H10E H 0.3319 0.6363 0.6947 0.497 Uiso 1 1 calc R . . H10F H 0.3452 0.6382 0.7479 0.497 Uiso 1 1 calc R . . C102 C 0.2869(6) 0.5332(9) 0.7858(6) 0.30(3) Uani 1 1 d G . . H10G H 0.2984 0.5379 0.8167 0.448 Uiso 1 1 calc R . . H10H H 0.2698 0.5030 0.7861 0.448 Uiso 1 1 calc R . . H10I H 0.2717 0.5638 0.7775 0.448 Uiso 1 1 calc R . . C103 C 0.2561(6) 0.4640(7) 0.4306(5) 0.103(6) Uani 1 1 d . . . C104 C 0.2881(5) 0.4357(6) 0.4480(6) 0.093(4) Uani 1 1 d . . . C105 C 0.2754(6) 0.3896(6) 0.4656(6) 0.096(5) Uani 1 1 d . . . C106 C 0.2335(6) 0.3878(7) 0.4624(5) 0.101(5) Uani 1 1 d . . . C107 C 0.2227(6) 0.4331(8) 0.4400(6) 0.109(5) Uani 1 1 d . . . C108 C 0.3286(6) 0.4579(11) 0.4458(8) 0.157(10) Uani 1 1 d . . . H10J H 0.3475 0.4320 0.4561 0.235 Uiso 1 1 calc R . . H10K H 0.3301 0.4881 0.4661 0.235 Uiso 1 1 calc R . . H10L H 0.3345 0.4681 0.4139 0.235 Uiso 1 1 calc R . . C109 C 0.3024(7) 0.3476(8) 0.4847(8) 0.141(8) Uani 1 1 d . . . H10M H 0.3241 0.3636 0.5014 0.211 Uiso 1 1 calc R . . H10N H 0.3126 0.3270 0.4589 0.211 Uiso 1 1 calc R . . H10O H 0.2876 0.3254 0.5059 0.211 Uiso 1 1 calc R . . C110 C 0.2052(8) 0.3432(7) 0.4715(7) 0.143(9) Uani 1 1 d . . . H11A H 0.1863 0.3533 0.4954 0.214 Uiso 1 1 calc R . . H11B H 0.2199 0.3130 0.4821 0.214 Uiso 1 1 calc R . . H11C H 0.1912 0.3348 0.4428 0.214 Uiso 1 1 calc R . . C111 C 0.1800(7) 0.4493(10) 0.4260(6) 0.144(9) Uani 1 1 d . . . H11D H 0.1802 0.4635 0.3945 0.217 Uiso 1 1 calc R . . H11E H 0.1704 0.4754 0.4477 0.217 Uiso 1 1 calc R . . H11F H 0.1628 0.4191 0.4270 0.217 Uiso 1 1 calc R . . C112 C 0.2582(7) 0.5143(8) 0.4021(6) 0.132(8) Uani 1 1 d . . . H11G H 0.2843 0.5295 0.4053 0.198 Uiso 1 1 calc R . . H11H H 0.2386 0.5387 0.4137 0.198 Uiso 1 1 calc R . . H11I H 0.2530 0.5068 0.3694 0.198 Uiso 1 1 calc R . . C113 C 0.2407(6) 0.3463(8) 0.8280(5) 0.107(5) Uani 1 1 d . . . C114 C 0.1312(5) 0.2490(5) 0.5377(5) 0.076(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 0.0597(5) 0.0475(4) 0.0401(3) 0.0078(3) -0.0041(3) -0.0126(3) Rh2 0.0602(5) 0.0514(4) 0.0511(4) 0.0082(3) -0.0150(3) -0.0138(3) Rh3 0.0607(5) 0.0538(4) 0.0389(3) 0.0009(3) -0.0021(3) -0.0074(3) Rh4 0.0693(5) 0.0405(3) 0.0297(3) -0.0014(3) 0.0085(3) -0.0067(3) Ag1 0.1216(10) 0.0830(7) 0.0856(7) 0.0050(6) -0.0051(6) -0.0042(6) N1 0.086(8) 0.084(7) 0.076(7) 0.004(6) -0.002(6) -0.005(6) N2 0.151(14) 0.083(8) 0.092(9) 0.000(7) 0.020(9) -0.037(8) N3 0.089(9) 0.110(10) 0.085(8) 0.007(7) -0.006(7) -0.018(7) N4 0.082(9) 0.095(8) 0.078(7) 0.008(6) -0.011(6) -0.011(6) N5 0.122(11) 0.081(8) 0.089(8) 0.001(7) -0.010(7) -0.024(7) N6 0.132(12) 0.080(8) 0.073(7) 0.010(6) -0.006(7) 0.002(7) N7 0.118(10) 0.084(8) 0.062(6) 0.001(6) 0.000(6) 0.005(6) N8 0.121(11) 0.083(8) 0.075(7) 0.003(6) 0.001(7) -0.026(7) N9 0.111(11) 0.091(9) 0.109(10) 0.011(8) 0.021(8) -0.014(7) N10 0.104(10) 0.102(9) 0.083(8) 0.010(7) 0.000(7) -0.010(7) N11 0.105(10) 0.092(9) 0.096(9) 0.009(7) -0.014(8) -0.014(7) N12 0.127(11) 0.076(7) 0.085(8) 0.006(6) -0.001(8) -0.005(7) N13 0.110(12) 0.178(16) 0.054(6) 0.031(8) -0.017(7) -0.018(10) N14 0.118(11) 0.088(8) 0.078(7) 0.003(6) 0.010(7) -0.006(7) N15 0.116(11) 0.086(8) 0.084(8) 0.005(6) 0.000(7) -0.004(7) N16 0.121(11) 0.073(7) 0.085(8) 0.002(6) -0.002(7) -0.013(7) O1 0.126(14) 0.071(8) 0.082(9) 0.014(7) -0.001(8) 0.015(7) O1' 0.27(6) 0.27(6) 0.27(6) 0.00(2) 0.00(2) 0.01(2) O2 0.181(19) 0.29(3) 0.144(15) -0.073(16) 0.001(13) 0.057(17) O3 0.203(17) 0.089(9) 0.203(18) 0.023(10) 0.042(14) -0.011(9) O4 0.187(16) 0.138(12) 0.155(14) -0.020(10) -0.052(12) -0.017(11) O5 0.35(3) 0.181(18) 0.128(14) -0.047(13) 0.076(17) -0.014(19) O6 0.32(3) 0.098(11) 0.26(3) 0.039(14) 0.06(2) 0.005(14) O7 0.13(2) 0.52(6) 0.43(5) -0.17(4) -0.11(3) 0.10(3) S1 0.116(3) 0.092(3) 0.091(2) -0.009(2) 0.007(2) -0.002(2) S2 0.167(6) 0.110(4) 0.111(4) -0.012(3) 0.012(3) 0.017(3) F1 0.168(12) 0.164(12) 0.123(9) 0.002(8) 0.007(8) 0.031(9) F2 0.165(13) 0.193(14) 0.140(11) -0.016(10) -0.026(9) -0.012(10) F3 0.26(2) 0.216(16) 0.119(10) 0.059(11) -0.019(11) 0.023(14) F4 0.36(3) 0.25(2) 0.105(10) -0.052(12) -0.025(13) 0.110(19) F5 0.207(17) 0.162(13) 0.230(19) -0.038(13) -0.073(15) 0.023(11) F6 0.242(15) 0.153(11) 0.268(16) -0.029(12) 0.062(13) -0.006(11) C1 0.092(11) 0.078(9) 0.085(9) 0.000(7) -0.007(8) -0.001(7) C2 0.089(11) 0.082(9) 0.095(10) -0.003(8) -0.011(8) -0.004(7) C3 0.155(19) 0.104(13) 0.108(14) 0.012(11) 0.030(13) 0.011(12) C4 0.115(15) 0.126(14) 0.075(10) 0.011(9) -0.010(9) -0.030(11) C5 0.120(14) 0.094(11) 0.083(10) 0.009(8) 0.023(9) -0.015(9) C6 0.085(10) 0.072(8) 0.085(9) 0.008(7) 0.014(7) 0.001(6) C7 0.108(13) 0.085(9) 0.072(9) 0.006(7) -0.008(8) -0.016(8) C8 0.100(11) 0.084(9) 0.072(8) 0.009(7) -0.012(8) -0.015(7) C9 0.090(12) 0.148(16) 0.088(11) -0.027(10) 0.035(9) -0.047(10) C10 0.120(18) 0.15(2) 0.15(2) -0.033(16) 0.014(15) 0.009(13) C11 0.173(18) 0.188(18) 0.190(19) -0.032(16) 0.002(16) 0.004(15) C12 0.177(19) 0.22(2) 0.183(19) -0.004(16) 0.010(16) 0.026(16) C13 0.14(2) 0.123(16) 0.15(2) 0.022(15) 0.008(15) 0.011(13) C14 0.075(12) 0.116(13) 0.145(17) 0.016(12) -0.003(11) -0.017(9) C15 0.117(13) 0.072(9) 0.092(10) -0.006(8) -0.006(9) -0.012(8) C16 0.19(2) 0.126(15) 0.083(11) 0.006(11) -0.014(12) -0.078(15) C17 0.23(3) 0.105(14) 0.107(14) 0.009(12) -0.053(16) -0.037(15) C18 0.25(3) 0.095(14) 0.119(16) 0.040(12) 0.001(17) -0.027(16) C19 0.19(2) 0.070(10) 0.121(15) -0.007(10) 0.020(14) 0.019(11) C20 0.131(14) 0.075(9) 0.072(8) -0.003(7) 0.016(9) -0.008(8) C21 0.148(15) 0.094(10) 0.053(7) 0.005(7) -0.001(8) -0.023(10) C22 0.105(11) 0.069(8) 0.072(8) -0.002(7) 0.004(7) -0.010(7) C23 0.092(11) 0.092(10) 0.081(9) 0.019(8) 0.008(8) 0.001(8) C24 0.128(14) 0.073(9) 0.088(10) 0.012(8) -0.020(9) -0.001(8) C25 0.145(18) 0.102(13) 0.109(14) -0.004(11) -0.009(12) -0.025(11) C26 0.129(15) 0.088(10) 0.092(11) 0.011(9) -0.012(10) -0.016(9) C27 0.132(15) 0.086(10) 0.092(11) 0.012(9) 0.007(10) -0.015(9) C28 0.089(9) 0.065(7) 0.064(7) 0.003(6) 0.001(6) 0.006(6) C29 0.096(11) 0.096(11) 0.084(9) -0.004(8) -0.009(8) 0.016(8) C30 0.138(14) 0.055(7) 0.089(10) 0.002(7) 0.002(9) -0.018(8) C31 0.17(2) 0.116(15) 0.092(11) -0.026(11) -0.041(12) 0.036(13) C32 0.142(14) 0.079(9) 0.139(13) -0.009(10) -0.024(11) 0.020(9) C33 0.20(2) 0.094(13) 0.093(12) -0.003(10) -0.014(14) -0.014(14) C34 0.128(15) 0.093(11) 0.080(10) -0.020(8) -0.014(9) 0.018(10) C35 0.169(16) 0.137(14) 0.112(13) -0.028(11) -0.001(12) -0.006(12) C36 0.143(14) 0.133(13) 0.093(10) -0.021(10) 0.012(10) 0.028(11) C37 0.139(18) 0.111(14) 0.125(15) 0.006(12) 0.045(13) 0.016(11) C38 0.113(13) 0.076(9) 0.108(12) 0.009(9) 0.035(10) 0.014(8) C39 0.106(12) 0.075(9) 0.090(10) 0.007(8) -0.013(9) -0.005(8) C40 0.135(14) 0.095(10) 0.054(7) 0.002(7) 0.012(8) 0.022(9) C41 0.092(11) 0.076(9) 0.106(11) 0.017(8) -0.008(9) -0.005(7) C42 0.090(12) 0.105(12) 0.133(15) 0.001(11) 0.011(10) -0.001(9) C43 0.081(13) 0.119(15) 0.24(3) 0.040(17) 0.017(15) 0.009(10) C44 0.104(15) 0.088(12) 0.19(2) 0.008(13) 0.012(14) 0.014(10) C45 0.142(19) 0.102(14) 0.18(2) 0.035(15) 0.043(16) 0.027(12) C46 0.124(15) 0.096(11) 0.094(11) 0.024(9) 0.044(10) 0.017(10) C47 0.132(17) 0.098(12) 0.129(15) 0.037(11) 0.003(13) -0.006(11) C48 0.142(17) 0.092(12) 0.117(14) 0.021(10) 0.029(12) 0.007(10) C49 0.099(12) 0.062(7) 0.106(11) 0.012(7) -0.017(9) -0.006(7) C50 0.104(12) 0.065(7) 0.078(8) 0.012(6) -0.028(8) 0.001(7) C51 0.143(16) 0.085(10) 0.080(10) 0.005(8) -0.007(10) 0.001(10) C52 0.115(13) 0.081(9) 0.086(10) -0.007(8) 0.005(9) 0.020(8) C53 0.150(18) 0.111(13) 0.086(11) -0.025(10) -0.008(11) 0.021(12) C54 0.142(19) 0.16(2) 0.073(10) -0.005(11) -0.023(11) 0.009(14) C55 0.22(3) 0.084(12) 0.092(12) -0.007(10) -0.013(15) 0.052(14) C56 0.145(18) 0.067(9) 0.138(17) -0.015(10) -0.030(14) 0.010(9) C57 0.145(15) 0.133(14) 0.153(15) -0.019(13) -0.026(13) 0.021(12) C58 0.133(14) 0.119(13) 0.130(13) -0.015(11) -0.023(12) -0.002(10) C59 0.16(2) 0.082(11) 0.133(17) 0.003(11) -0.024(14) 0.004(11) C60 0.104(13) 0.066(9) 0.161(18) 0.009(10) -0.007(12) -0.005(8) C61 0.095(12) 0.107(12) 0.084(10) 0.002(9) -0.008(8) -0.007(8) C62 0.108(12) 0.068(8) 0.088(9) -0.019(7) -0.006(9) 0.006(7) C63 0.117(16) 0.107(14) 0.16(2) -0.021(14) 0.049(14) -0.002(11) C64 0.112(18) 0.127(18) 0.24(3) 0.005(19) 0.053(18) 0.009(13) C65 0.21(3) 0.081(12) 0.21(3) 0.007(14) 0.11(2) 0.007(14) C66 0.098(13) 0.098(12) 0.111(13) 0.019(10) 0.002(10) -0.012(9) C67 0.115(14) 0.129(15) 0.085(10) 0.007(10) -0.011(9) -0.033(11) C68 0.097(11) 0.102(11) 0.068(8) -0.004(8) 0.010(8) -0.001(8) C69 0.122(13) 0.069(8) 0.089(10) -0.017(7) 0.016(9) -0.001(8) C70 0.115(15) 0.089(11) 0.143(16) -0.018(11) 0.034(12) -0.022(9) C71 0.139(17) 0.078(10) 0.120(14) 0.002(10) 0.022(12) 0.016(10) C72 0.153(18) 0.080(10) 0.100(12) 0.000(9) 0.012(11) -0.026(10) C73 0.14(2) 0.15(2) 0.102(14) 0.030(13) -0.007(13) -0.040(15) C74 0.17(2) 0.094(12) 0.094(12) 0.030(10) -0.024(13) -0.027(12) C75 0.099(12) 0.122(13) 0.073(9) 0.008(9) 0.022(8) -0.018(9) C76 0.112(14) 0.112(13) 0.093(11) -0.001(10) -0.028(10) 0.008(10) C77 0.129(16) 0.134(16) 0.064(8) 0.008(9) 0.021(9) -0.005(12) C78 0.15(2) 0.17(2) 0.15(2) 0.049(18) -0.049(16) -0.046(17) C79 0.30(4) 0.093(15) 0.27(4) 0.047(19) -0.17(3) -0.062(19) C80 0.144(19) 0.140(17) 0.090(12) -0.001(11) -0.028(12) -0.012(13) C81 0.18(2) 0.094(12) 0.132(16) -0.009(12) -0.010(15) -0.035(13) C82 0.197(19) 0.204(19) 0.178(18) 0.014(16) -0.005(15) 0.003(16) C83 0.17(2) 0.125(17) 0.16(2) 0.038(16) -0.066(19) -0.034(16) C84 0.119(16) 0.123(15) 0.111(14) 0.001(12) -0.008(12) -0.019(12) C85 0.131(18) 0.150(19) 0.100(13) 0.020(13) -0.013(12) -0.010(14) C86 0.153(15) 0.136(14) 0.129(14) 0.013(12) 0.000(12) 0.005(12) C87 0.131(16) 0.084(10) 0.124(14) 0.024(10) -0.057(12) 0.004(10) C88 0.27(4) 0.15(2) 0.100(15) 0.035(15) -0.040(19) -0.06(2) C89 0.19(3) 0.15(2) 0.101(14) -0.017(14) -0.014(15) -0.028(17) C90 0.131(17) 0.129(17) 0.136(17) 0.001(14) -0.013(14) 0.024(13) C91 0.17(2) 0.136(17) 0.116(15) 0.010(13) 0.034(14) -0.038(15) C92 0.20(3) 0.18(3) 0.18(3) -0.03(2) -0.07(2) 0.03(2) C93 0.163(15) 0.097(11) 0.130(13) -0.001(10) -0.033(12) -0.023(11) C94 0.17(2) 0.15(2) 0.122(17) -0.059(16) -0.028(16) 0.059(17) C95 0.145(16) 0.188(17) 0.142(15) -0.011(14) 0.011(13) -0.032(14) C96 0.154(15) 0.115(12) 0.114(12) -0.002(10) -0.042(11) -0.003(11) C97 0.112(12) 0.143(13) 0.086(9) -0.024(10) -0.013(9) -0.002(10) C98 0.30(3) 0.28(3) 0.30(3) 0.021(19) -0.022(19) -0.005(19) C99 0.39(4) 0.39(4) 0.38(4) 0.00(2) -0.02(2) 0.01(2) C100 0.69(12) 1.6(3) 0.09(2) 0.19(7) -0.08(4) -0.88(17) C101 0.40(7) 0.11(2) 0.48(8) 0.05(4) -0.18(6) -0.02(3) C102 0.25(5) 0.51(9) 0.14(3) -0.01(4) 0.02(3) 0.06(5) C103 0.150(17) 0.109(12) 0.051(7) -0.010(7) 0.013(9) -0.024(11) C104 0.106(13) 0.079(9) 0.093(10) 0.001(8) 0.016(9) -0.008(8) C105 0.121(14) 0.079(9) 0.089(10) 0.001(8) 0.014(9) -0.005(8) C106 0.133(15) 0.102(12) 0.067(8) -0.007(8) 0.038(9) -0.037(10) C107 0.128(16) 0.132(15) 0.065(9) -0.003(9) 0.003(9) -0.014(12) C108 0.105(16) 0.23(3) 0.132(18) -0.058(19) 0.020(13) -0.023(16) C109 0.19(2) 0.109(15) 0.126(16) 0.003(13) -0.002(15) 0.040(14) C110 0.22(3) 0.093(13) 0.113(14) -0.022(11) 0.046(16) -0.041(14) C111 0.18(2) 0.19(2) 0.070(10) -0.005(12) 0.004(12) -0.030(18) C112 0.18(2) 0.152(18) 0.060(9) 0.015(10) 0.025(11) 0.000(15) C113 0.140(17) 0.123(14) 0.058(8) -0.005(9) -0.003(9) -0.003(12) C114 0.097(10) 0.060(7) 0.071(8) -0.005(6) 0.003(7) -0.005(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 N9 2.112(14) . ? Rh1 C75 2.140(19) . ? Rh1 C76 2.162(17) . ? Rh1 C77 2.182(16) . ? Rh1 C73 2.19(2) . ? Rh1 N2 2.188(17) . ? Rh1 N1 2.196(12) . ? Rh1 C74 2.200(19) . ? Rh2 C86 2.07(2) . ? Rh2 C84 2.14(2) . ? Rh2 C87 2.141(18) . ? Rh2 N3 2.154(14) . ? Rh2 N13 2.171(19) . ? Rh2 C85 2.17(2) . ? Rh2 N4 2.177(12) . ? Rh2 C83 2.28(3) . ? Rh3 N10 2.068(15) . ? Rh3 C95 2.137(13) . ? Rh3 C96 2.149(11) . ? Rh3 N5 2.174(13) . ? Rh3 C94 2.176(13) . ? Rh3 C97 2.195(11) . ? Rh3 C93 2.212(12) . ? Rh3 N6 2.236(13) . ? Rh4 C104 2.115(16) . ? Rh4 C107 2.117(17) . ? Rh4 C106 2.132(16) . ? Rh4 N14 2.138(14) . ? Rh4 C103 2.138(14) . ? Rh4 C105 2.152(16) . ? Rh4 N7 2.154(11) . ? Rh4 N8 2.182(12) . ? Ag1 O1' 2.37(11) . ? Ag1 O1 2.375(13) . ? Ag1 N16 2.408(13) . ? Ag1 N12 2.420(14) . ? Ag1 N11 2.450(15) . ? Ag1 N15 2.462(14) . ? N1 C7 1.254(19) . ? N1 C1 1.38(2) . ? N2 C8 1.36(2) . ? N2 C9 1.42(2) . ? N3 C8 1.33(2) . ? N3 C14 1.40(2) . ? N4 C7 1.313(19) . ? N4 C6 1.367(19) . ? N5 C21 1.297(19) . ? N5 C15 1.41(2) . ? N6 C22 1.296(18) . ? N6 C23 1.31(2) . ? N7 C22 1.351(18) . ? N7 C28 1.397(17) . ? N8 C21 1.352(19) . ? N8 C20 1.415(18) . ? N9 C41 1.31(2) . ? N9 C45 1.43(2) . ? N10 C46 1.32(2) . ? N10 C50 1.40(2) . ? N11 C39 1.27(2) . ? N11 C42 1.42(2) . ? N12 C40 1.295(18) . ? N12 C49 1.43(2) . ? N13 C63 1.36(2) . ? N13 C67 1.42(2) . ? N14 C68 1.304(19) . ? N14 C72 1.37(2) . ? N15 C61 1.30(2) . ? N15 C66 1.40(2) . ? N16 C62 1.25(2) . ? N16 C69 1.42(2) . ? O1 O1' 1.72(12) . ? O2 S1 1.383(18) . ? O3 S1 1.373(15) . ? O4 S1 1.446(16) . ? O5 S2 1.43(2) . ? O6 S2 1.46(2) . ? O7 S2 1.41(2) . ? S1 C113 1.79(2) . ? S2 C114 1.794(15) . ? F1 C113 1.32(2) . ? F2 C113 1.31(2) . ? F3 C113 1.33(2) . ? F4 C114 1.25(2) . ? F5 C114 1.39(2) . ? F6 C114 1.29(2) . ? C1 C2 1.41(2) . ? C1 C6 1.43(2) . ? C2 C3 1.41(2) . ? C3 C4 1.39(3) . ? C4 C5 1.44(3) . ? C5 C6 1.38(2) . ? C7 C8 1.43(2) . ? C9 C10 1.32(3) . ? C9 C14 1.42(3) . ? C10 C11 1.53(4) . ? C11 C12 1.440(19) . ? C12 C13 1.50(4) . ? C13 C14 1.46(3) . ? C15 C16 1.33(2) . ? C15 C20 1.42(2) . ? C16 C17 1.40(3) . ? C17 C18 1.43(3) . ? C18 C19 1.40(3) . ? C19 C20 1.39(2) . ? C21 C22 1.42(2) . ? C23 C24 1.33(2) . ? C23 C28 1.46(2) . ? C24 C25 1.38(2) . ? C25 C26 1.38(2) . ? C26 C27 1.37(2) . ? C27 C28 1.36(2) . ? C29 C30 1.36(2) . ? C29 C34 1.44(2) . ? C29 C38 1.55(2) . ? C30 C31 1.33(3) . ? C30 C40 1.46(2) . ? C31 C32 1.43(2) . ? C32 C33 1.47(3) . ? C33 C34 1.36(3) . ? C34 C35 1.44(3) . ? C35 C36 1.32(3) . ? C36 C37 1.48(3) . ? C37 C38 1.39(2) . ? C38 C39 1.43(2) . ? C39 C40 1.50(2) . ? C41 C42 1.40(2) . ? C42 C43 1.45(3) . ? C43 C44 1.33(3) . ? C44 C45 1.33(3) . ? C46 C47 1.45(3) . ? C47 C48 1.43(3) . ? C48 C49 1.33(2) . ? C49 C50 1.37(2) . ? C51 C60 1.38(3) . ? C51 C56 1.42(3) . ? C51 C52 1.47(3) . ? C52 C53 1.36(3) . ? C52 C62 1.48(2) . ? C53 C54 1.38(2) . ? C54 C55 1.36(3) . ? C55 C56 1.52(3) . ? C56 C57 1.34(3) . ? C57 C58 1.32(3) . ? C58 C59 1.34(3) . ? C59 C60 1.41(3) . ? C60 C61 1.44(2) . ? C61 C62 1.52(2) . ? C63 C64 1.40(3) . ? C64 C65 1.34(3) . ? C65 C66 1.43(3) . ? C66 C67 1.40(3) . ? C68 C69 1.37(2) . ? C69 C70 1.37(2) . ? C70 C71 1.44(2) . ? C71 C72 1.37(3) . ? C73 C78 1.34(3) . ? C73 C77 1.36(3) . ? C73 C74 1.49(3) . ? C74 C75 1.45(2) . ? C74 C79 1.55(3) . ? C75 C76 1.38(3) . ? C75 C80 1.59(3) . ? C76 C77 1.47(3) . ? C76 C81 1.52(2) . ? C77 C82 1.60(3) . ? C83 C84 1.30(3) . ? C83 C88 1.44(3) . ? C83 C87 1.60(4) . ? C84 C85 1.52(3) . ? C84 C89 1.59(3) . ? C85 C90 1.45(3) . ? C85 C86 1.464(17) . ? C86 C87 1.46(3) . ? C86 C91 1.481(17) . ? C87 C92 1.41(3) . ? C93 C94 1.421(7) . ? C93 C97 1.421(7) . ? C93 C98 1.510(8) . ? C94 C95 1.421(7) . ? C94 C99 1.511(8) . ? C95 C96 1.421(7) . ? C95 C100 1.510(8) . ? C96 C97 1.421(7) . ? C96 C101 1.510(8) . ? C97 C102 1.510(8) . ? C103 C104 1.41(3) . ? C103 C107 1.43(3) . ? C103 C112 1.54(3) . ? C104 C105 1.37(2) . ? C104 C108 1.50(3) . ? C105 C106 1.44(3) . ? C105 C109 1.53(3) . ? C106 C107 1.39(3) . ? C106 C110 1.53(2) . ? C107 C111 1.57(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 N9 Rh1 C75 115.9(6) . . ? N9 Rh1 C76 92.9(7) . . ? C75 Rh1 C76 37.5(7) . . ? N9 Rh1 C77 105.3(7) . . ? C75 Rh1 C77 64.8(7) . . ? C76 Rh1 C77 39.5(7) . . ? N9 Rh1 C73 139.6(9) . . ? C75 Rh1 C73 66.3(8) . . ? C76 Rh1 C73 64.2(8) . . ? C77 Rh1 C73 36.2(8) . . ? N9 Rh1 N2 84.0(6) . . ? C75 Rh1 N2 160.0(6) . . ? C76 Rh1 N2 146.6(7) . . ? C77 Rh1 N2 109.4(7) . . ? C73 Rh1 N2 97.4(7) . . ? N9 Rh1 N1 85.8(5) . . ? C75 Rh1 N1 104.0(6) . . ? C76 Rh1 N1 134.5(7) . . ? C77 Rh1 N1 166.7(7) . . ? C73 Rh1 N1 134.2(8) . . ? N2 Rh1 N1 78.6(5) . . ? N9 Rh1 C74 154.3(7) . . ? C75 Rh1 C74 39.0(7) . . ? C76 Rh1 C74 63.2(7) . . ? C77 Rh1 C74 63.0(8) . . ? C73 Rh1 C74 39.7(9) . . ? N2 Rh1 C74 121.0(7) . . ? N1 Rh1 C74 103.8(7) . . ? C86 Rh2 C84 67.0(8) . . ? C86 Rh2 C87 40.6(7) . . ? C84 Rh2 C87 65.1(9) . . ? C86 Rh2 N3 96.1(7) . . ? C84 Rh2 N3 160.0(7) . . ? C87 Rh2 N3 109.6(8) . . ? C86 Rh2 N13 140.3(8) . . ? C84 Rh2 N13 118.8(7) . . ? C87 Rh2 N13 103.0(6) . . ? N3 Rh2 N13 81.0(5) . . ? C86 Rh2 C85 40.3(5) . . ? C84 Rh2 C85 41.4(7) . . ? C87 Rh2 C85 67.8(7) . . ? N3 Rh2 C85 118.6(7) . . ? N13 Rh2 C85 159.9(6) . . ? C86 Rh2 N4 132.2(7) . . ? C84 Rh2 N4 104.5(7) . . ? C87 Rh2 N4 168.4(7) . . ? N3 Rh2 N4 78.4(5) . . ? N13 Rh2 N4 86.3(5) . . ? C85 Rh2 N4 101.2(6) . . ? C86 Rh2 C83 68.1(9) . . ? C84 Rh2 C83 34.2(9) . . ? C87 Rh2 C83 42.3(9) . . ? N3 Rh2 C83 150.4(9) . . ? N13 Rh2 C83 95.3(7) . . ? C85 Rh2 C83 65.6(8) . . ? N4 Rh2 C83 130.9(9) . . ? N10 Rh3 C95 137.5(6) . . ? N10 Rh3 C96 102.0(6) . . ? C95 Rh3 C96 38.7(2) . . ? N10 Rh3 N5 84.2(5) . . ? C95 Rh3 N5 97.6(5) . . ? C96 Rh3 N5 114.1(5) . . ? N10 Rh3 C94 158.3(5) . . ? C95 Rh3 C94 38.4(2) . . ? C96 Rh3 C94 64.2(3) . . ? N5 Rh3 C94 116.4(6) . . ? N10 Rh3 C97 95.2(5) . . ? C95 Rh3 C97 64.1(3) . . ? C96 Rh3 C97 38.2(2) . . ? N5 Rh3 C97 151.6(5) . . ? C94 Rh3 C97 63.5(3) . . ? N10 Rh3 C93 122.0(5) . . ? C95 Rh3 C93 63.8(3) . . ? C96 Rh3 C93 63.6(3) . . ? N5 Rh3 C93 153.9(6) . . ? C94 Rh3 C93 37.8(2) . . ? C97 Rh3 C93 37.6(2) . . ? N10 Rh3 N6 84.3(6) . . ? C95 Rh3 N6 138.0(6) . . ? C96 Rh3 N6 164.8(4) . . ? N5 Rh3 N6 80.1(4) . . ? C94 Rh3 N6 105.3(5) . . ? C97 Rh3 N6 128.2(5) . . ? C93 Rh3 N6 101.2(5) . . ? C104 Rh4 C107 64.3(8) . . ? C104 Rh4 C106 65.0(6) . . ? C107 Rh4 C106 38.2(7) . . ? C104 Rh4 N14 154.2(6) . . ? C107 Rh4 N14 96.9(7) . . ? C106 Rh4 N14 111.8(6) . . ? C104 Rh4 C103 38.8(7) . . ? C107 Rh4 C103 39.1(7) . . ? C106 Rh4 C103 65.7(6) . . ? N14 Rh4 C103 115.6(7) . . ? C104 Rh4 C105 37.5(6) . . ? C107 Rh4 C105 63.7(8) . . ? C106 Rh4 C105 39.2(7) . . ? N14 Rh4 C105 150.4(6) . . ? C103 Rh4 C105 64.2(7) . . ? C104 Rh4 N7 121.8(6) . . ? C107 Rh4 N7 140.8(7) . . ? C106 Rh4 N7 105.3(6) . . ? N14 Rh4 N7 84.0(5) . . ? C103 Rh4 N7 160.2(7) . . ? C105 Rh4 N7 97.4(6) . . ? C104 Rh4 N8 98.7(6) . . ? C107 Rh4 N8 140.7(6) . . ? C106 Rh4 N8 163.0(6) . . ? N14 Rh4 N8 85.0(5) . . ? C103 Rh4 N8 105.2(6) . . ? C105 Rh4 N8 124.4(6) . . ? N7 Rh4 N8 78.4(5) . . ? O1' Ag1 O1 42(3) . . ? O1' Ag1 N16 97(3) . . ? O1 Ag1 N16 119.3(5) . . ? O1' Ag1 N12 94(3) . . ? O1 Ag1 N12 117.9(5) . . ? N16 Ag1 N12 104.5(4) . . ? O1' Ag1 N11 109(3) . . ? O1 Ag1 N11 85.4(5) . . ? N16 Ag1 N11 153.3(5) . . ? N12 Ag1 N11 68.3(4) . . ? O1' Ag1 N15 115(3) . . ? O1 Ag1 N15 87.7(5) . . ? N16 Ag1 N15 69.8(5) . . ? N12 Ag1 N15 151.2(5) . . ? N11 Ag1 N15 103.6(5) . . ? C7 N1 C1 100.5(13) . . ? C7 N1 Rh1 110.4(11) . . ? C1 N1 Rh1 147.5(10) . . ? C8 N2 C9 105.2(15) . . ? C8 N2 Rh1 107.3(12) . . ? C9 N2 Rh1 144.7(11) . . ? C8 N3 C14 103.2(15) . . ? C8 N3 Rh2 109.1(11) . . ? C14 N3 Rh2 147.5(13) . . ? C7 N4 C6 101.8(13) . . ? C7 N4 Rh2 112.8(11) . . ? C6 N4 Rh2 144.8(10) . . ? C21 N5 C15 103.9(13) . . ? C21 N5 Rh3 107.9(10) . . ? C15 N5 Rh3 145.9(11) . . ? C22 N6 C23 108.1(14) . . ? C22 N6 Rh3 105.7(10) . . ? C23 N6 Rh3 144.0(11) . . ? C22 N7 C28 102.8(11) . . ? C22 N7 Rh4 111.3(9) . . ? C28 N7 Rh4 145.6(10) . . ? C21 N8 C20 102.8(12) . . ? C21 N8 Rh4 111.9(10) . . ? C20 N8 Rh4 144.4(11) . . ? C41 N9 C45 118.3(16) . . ? C41 N9 Rh1 123.6(13) . . ? C45 N9 Rh1 117.9(12) . . ? C46 N10 C50 115.6(15) . . ? C46 N10 Rh3 122.9(12) . . ? C50 N10 Rh3 121.5(11) . . ? C39 N11 C42 117.1(16) . . ? C39 N11 Ag1 115.6(12) . . ? C42 N11 Ag1 126.5(12) . . ? C40 N12 C49 114.1(15) . . ? C40 N12 Ag1 117.9(12) . . ? C49 N12 Ag1 127.7(10) . . ? C63 N13 C67 125(2) . . ? C63 N13 Rh2 117.9(13) . . ? C67 N13 Rh2 117.0(15) . . ? C68 N14 C72 120.2(16) . . ? C68 N14 Rh4 121.0(12) . . ? C72 N14 Rh4 118.6(12) . . ? C61 N15 C66 114.4(15) . . ? C61 N15 Ag1 114.6(11) . . ? C66 N15 Ag1 130.5(11) . . ? C62 N16 C69 118.0(15) . . ? C62 N16 Ag1 115.8(11) . . ? C69 N16 Ag1 126.2(11) . . ? O1' O1 Ag1 69(4) . . ? O1 O1' Ag1 69(4) . . ? O3 S1 O2 116.7(13) . . ? O3 S1 O4 118.2(12) . . ? O2 S1 O4 109.2(13) . . ? O3 S1 C113 104.0(11) . . ? O2 S1 C113 101.8(11) . . ? O4 S1 C113 104.6(10) . . ? O7 S2 O5 109(2) . . ? O7 S2 O6 118(2) . . ? O5 S2 O6 114.8(15) . . ? O7 S2 C114 105.4(15) . . ? O5 S2 C114 106.7(11) . . ? O6 S2 C114 101.2(10) . . ? N1 C1 C2 131.0(15) . . ? N1 C1 C6 109.0(13) . . ? C2 C1 C6 119.8(15) . . ? C3 C2 C1 120.0(17) . . ? C4 C3 C2 120(2) . . ? C3 C4 C5 119.9(19) . . ? C6 C5 C4 120.1(17) . . ? N4 C6 C5 134.5(16) . . ? N4 C6 C1 105.8(13) . . ? C5 C6 C1 119.7(16) . . ? N1 C7 N4 122.7(17) . . ? N1 C7 C8 121.2(14) . . ? N4 C7 C8 115.9(14) . . ? N3 C8 N2 115.8(16) . . ? N3 C8 C7 123.4(14) . . ? N2 C8 C7 120.8(15) . . ? C10 C9 N2 126(2) . . ? C10 C9 C14 129(2) . . ? N2 C9 C14 104.8(14) . . ? C9 C10 C11 111(2) . . ? C12 C11 C10 122(3) . . ? C11 C12 C13 123(3) . . ? C14 C13 C12 110(2) . . ? N3 C14 C9 110.8(15) . . ? N3 C14 C13 125(2) . . ? C9 C14 C13 124(2) . . ? C16 C15 N5 130.4(16) . . ? C16 C15 C20 121.4(16) . . ? N5 C15 C20 107.9(13) . . ? C15 C16 C17 117.8(18) . . ? C16 C17 C18 119.5(19) . . ? C19 C18 C17 122.6(19) . . ? C20 C19 C18 114(2) . . ? C19 C20 N8 129.1(15) . . ? C19 C20 C15 123.2(16) . . ? N8 C20 C15 107.1(13) . . ? N5 C21 N8 118.2(14) . . ? N5 C21 C22 122.8(13) . . ? N8 C21 C22 117.6(14) . . ? N6 C22 N7 115.6(13) . . ? N6 C22 C21 123.3(14) . . ? N7 C22 C21 120.7(13) . . ? N6 C23 C24 136.8(17) . . ? N6 C23 C28 106.9(12) . . ? C24 C23 C28 116.1(15) . . ? C23 C24 C25 124.7(17) . . ? C24 C25 C26 114.9(18) . . ? C27 C26 C25 126.4(17) . . ? C28 C27 C26 114.9(16) . . ? C27 C28 N7 131.1(14) . . ? C27 C28 C23 122.4(13) . . ? N7 C28 C23 106.3(12) . . ? C30 C29 C34 127.4(17) . . ? C30 C29 C38 111.8(14) . . ? C34 C29 C38 120.7(16) . . ? C31 C30 C29 116.9(17) . . ? C31 C30 C40 136.6(17) . . ? C29 C30 C40 106.3(14) . . ? C30 C31 C32 121(2) . . ? C31 C32 C33 120(2) . . ? C34 C33 C32 119.3(18) . . ? C33 C34 C29 115.3(18) . . ? C33 C34 C35 125.7(18) . . ? C29 C34 C35 118.8(19) . . ? C36 C35 C34 119(2) . . ? C35 C36 C37 127(2) . . ? C38 C37 C36 118(2) . . ? C37 C38 C39 138.5(19) . . ? C37 C38 C29 116.6(17) . . ? C39 C38 C29 104.9(13) . . ? N11 C39 C38 132.4(17) . . ? N11 C39 C40 120.8(16) . . ? C38 C39 C40 106.6(13) . . ? N12 C40 C30 132.5(17) . . ? N12 C40 C39 116.9(16) . . ? C30 C40 C39 110.3(12) . . ? N9 C41 C42 123.9(17) . . ? C41 C42 N11 121.7(16) . . ? C41 C42 C43 117.6(17) . . ? N11 C42 C43 120.6(18) . . ? C44 C43 C42 115(2) . . ? C45 C44 C43 127(2) . . ? C44 C45 N9 118(2) . . ? N10 C46 C47 124.5(16) . . ? C48 C47 C46 115.5(17) . . ? C49 C48 C47 120(2) . . ? C48 C49 C50 120.6(16) . . ? C48 C49 N12 119.9(17) . . ? C50 C49 N12 119.1(13) . . ? C49 C50 N10 123.1(13) . . ? C60 C51 C56 127(2) . . ? C60 C51 C52 110.8(16) . . ? C56 C51 C52 121.4(18) . . ? C53 C52 C51 118.3(17) . . ? C53 C52 C62 135.7(19) . . ? C51 C52 C62 105.6(15) . . ? C52 C53 C54 122(2) . . ? C55 C54 C53 124(2) . . ? C54 C55 C56 118(2) . . ? C57 C56 C51 110(2) . . ? C57 C56 C55 134(2) . . ? C51 C56 C55 116(2) . . ? C58 C57 C56 130(3) . . ? C57 C58 C59 115(2) . . ? C58 C59 C60 126(2) . . ? C51 C60 C59 111(2) . . ? C51 C60 C61 110.5(17) . . ? C59 C60 C61 138(2) . . ? N15 C61 C60 136.4(17) . . ? N15 C61 C62 117.5(15) . . ? C60 C61 C62 106.1(15) . . ? N16 C62 C52 130.9(17) . . ? N16 C62 C61 122.0(15) . . ? C52 C62 C61 106.8(15) . . ? N13 C63 C64 114(2) . . ? C65 C64 C63 128(2) . . ? C64 C65 C66 115(2) . . ? C67 C66 N15 117.6(18) . . ? C67 C66 C65 122.4(18) . . ? N15 C66 C65 120.0(17) . . ? C66 C67 N13 116(2) . . ? N14 C68 C69 120.5(16) . . ? C68 C69 C70 120.7(16) . . ? C68 C69 N16 121.8(14) . . ? C70 C69 N16 117.4(15) . . ? C69 C70 C71 119.5(18) . . ? C72 C71 C70 114.9(17) . . ? C71 C72 N14 123.7(17) . . ? C78 C73 C77 125(3) . . ? C78 C73 C74 127(3) . . ? C77 C73 C74 106.8(18) . . ? C78 C73 Rh1 132.1(18) . . ? C77 C73 Rh1 71.7(11) . . ? C74 C73 Rh1 70.6(11) . . ? C75 C74 C73 107.1(19) . . ? C75 C74 C79 123(2) . . ? C73 C74 C79 130(2) . . ? C75 C74 Rh1 68.3(10) . . ? C73 C74 Rh1 69.7(12) . . ? C79 C74 Rh1 123.6(15) . . ? C76 C75 C74 107.6(18) . . ? C76 C75 C80 128.5(17) . . ? C74 C75 C80 122.7(19) . . ? C76 C75 Rh1 72.1(11) . . ? C74 C75 Rh1 72.7(11) . . ? C80 C75 Rh1 130.3(11) . . ? C75 C76 C77 108.5(17) . . ? C75 C76 C81 124(2) . . ? C77 C76 C81 127.2(19) . . ? C75 C76 Rh1 70.4(11) . . ? C77 C76 Rh1 71.0(10) . . ? C81 C76 Rh1 127.9(13) . . ? C73 C77 C76 109.7(19) . . ? C73 C77 C82 126(2) . . ? C76 C77 C82 124(2) . . ? C73 C77 Rh1 72.1(12) . . ? C76 C77 Rh1 69.5(9) . . ? C82 C77 Rh1 126.4(16) . . ? C84 C83 C88 136(3) . . ? C84 C83 C87 104(2) . . ? C88 C83 C87 118(3) . . ? C84 C83 Rh2 67.1(14) . . ? C88 C83 Rh2 120.3(18) . . ? C87 C83 Rh2 64.2(12) . . ? C83 C84 C85 117(2) . . ? C83 C84 C89 123(2) . . ? C85 C84 C89 119(2) . . ? C83 C84 Rh2 78.8(17) . . ? C85 C84 Rh2 70.5(12) . . ? C89 C84 Rh2 131.6(14) . . ? C90 C85 C86 129(2) . . ? C90 C85 C84 129(2) . . ? C86 C85 C84 102.0(18) . . ? C90 C85 Rh2 132.2(16) . . ? C86 C85 Rh2 66.0(13) . . ? C84 C85 Rh2 68.1(13) . . ? C87 C86 C85 110.6(18) . . ? C87 C86 C91 123(2) . . ? C85 C86 C91 125(2) . . ? C87 C86 Rh2 72.4(12) . . ? C85 C86 Rh2 73.7(14) . . ? C91 C86 Rh2 133.8(18) . . ? C92 C87 C86 131(2) . . ? C92 C87 C83 123(2) . . ? C86 C87 C83 105.6(18) . . ? C92 C87 Rh2 132.3(17) . . ? C86 C87 Rh2 67.0(12) . . ? C83 C87 Rh2 73.5(12) . . ? C94 C93 C97 108.0 . . ? C94 C93 C98 126.0 . . ? C97 C93 C98 126.0 . . ? C94 C93 Rh3 69.8(4) . . ? C97 C93 Rh3 70.6(4) . . ? C98 C93 Rh3 125.3(4) . . ? C93 C94 C95 108.0 . . ? C93 C94 C99 126.0 . . ? C95 C94 C99 126.0 . . ? C93 C94 Rh3 72.5(4) . . ? C95 C94 Rh3 69.3(4) . . ? C99 C94 Rh3 123.9(4) . . ? C94 C95 C96 108.0 . . ? C94 C95 C100 126.0 . . ? C96 C95 C100 126.0 . . ? C94 C95 Rh3 72.3(4) . . ? C96 C95 Rh3 71.1(5) . . ? C100 C95 Rh3 122.3(4) . . ? C97 C96 C95 108.0 . . ? C97 C96 C101 126.0 . . ? C95 C96 C101 126.0 . . ? C97 C96 Rh3 72.7(4) . . ? C95 C96 Rh3 70.2(5) . . ? C101 C96 Rh3 122.8(4) . . ? C93 C97 C96 108.0 . . ? C93 C97 C102 126.0 . . ? C96 C97 C102 126.0 . . ? C93 C97 Rh3 71.8(4) . . ? C96 C97 Rh3 69.2(4) . . ? C102 C97 Rh3 124.6(4) . . ? C104 C103 C107 105.1(17) . . ? C104 C103 C112 126.4(18) . . ? C107 C103 C112 128(2) . . ? C104 C103 Rh4 69.7(9) . . ? C107 C103 Rh4 69.6(9) . . ? C112 C103 Rh4 130.3(12) . . ? C105 C104 C103 109.8(17) . . ? C105 C104 C108 130(2) . . ? C103 C104 C108 120.0(18) . . ? C105 C104 Rh4 72.7(10) . . ? C103 C104 Rh4 71.5(9) . . ? C108 C104 Rh4 121.6(13) . . ? C104 C105 C106 108.8(16) . . ? C104 C105 C109 124.3(19) . . ? C106 C105 C109 126.9(17) . . ? C104 C105 Rh4 69.8(10) . . ? C106 C105 Rh4 69.7(9) . . ? C109 C105 Rh4 127.1(13) . . ? C107 C106 C105 105.6(14) . . ? C107 C106 C110 123(2) . . ? C105 C106 C110 130.1(19) . . ? C107 C106 Rh4 70.3(10) . . ? C105 C106 Rh4 71.2(9) . . ? C110 C106 Rh4 131.8(11) . . ? C106 C107 C103 110.6(19) . . ? C106 C107 C111 126.5(19) . . ? C103 C107 C111 122.9(19) . . ? C106 C107 Rh4 71.5(10) . . ? C103 C107 Rh4 71.3(10) . . ? C111 C107 Rh4 124.5(13) . . ? F2 C113 F1 103.0(19) . . ? F2 C113 F3 101.0(15) . . ? F1 C113 F3 109.7(18) . . ? F2 C113 S1 112.7(15) . . ? F1 C113 S1 115.9(12) . . ? F3 C113 S1 113.2(16) . . ? F4 C114 F6 114.9(18) . . ? F4 C114 F5 105.3(18) . . ? F6 C114 F5 104.6(16) . . ? F4 C114 S2 112.8(13) . . ? F6 C114 S2 108.7(13) . . ? F5 C114 S2 110.1(11) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.463 _refine_diff_density_min -2.784 _refine_diff_density_rms 0.194 # Attachment '- 4a_1.cif' data_mo_4a _database_code_depnum_ccdc_archive 'CCDC 888414' #TrackingRef '- 4a_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C202 H219 F18 Ir6 N24 O27 S6' _chemical_formula_weight 5102.57 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 22.1957(19) _cell_length_b 33.541(3) _cell_length_c 29.504(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.164(2) _cell_angle_gamma 90.00 _cell_volume 20618(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9836 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.10 _exptl_crystal_description sheet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10140 _exptl_absorpt_coefficient_mu 4.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5665 _exptl_absorpt_correction_T_max 0.7399 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.17 _diffrn_reflns_number 134029 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 26.01 _reflns_number_total 40344 _reflns_number_gt 19523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. In asymmetric unit of this data, there were disordered anions and solvent molecules (3 triflate anions, 3 diethyl ether and 4 MeOH) which could not be restrained properly. Hence, the SQUEEZE algorithm was used to omit them. F7-9, C125, C136, C139 -C141, C16A, C169, C172-174, C179 and C184 were refined isotropically and other non-hydrogen atoms were refined anisotropically. 59 ISOR, 46 DFIX and 1 DELU instructions were used to restrain pyrene molecules so that there were 395 restraints in the data. There are several big residual density peaks in the structure but all of them are close to the iridium atoms. ; _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^)+(0.1419P)^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 40344 _refine_ls_number_parameters 2061 _refine_ls_number_restraints 401 _refine_ls_R_factor_all 0.1456 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2423 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.444 0.500 0.000 3011.1 824.7 2 0.387 0.000 0.500 3010.8 827.9 _platon_squeeze_details ; ; 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 0.75743(2) 1.151534(14) 0.977037(19) 0.04300(14) Uani 1 1 d . . . Ir2 Ir 0.83670(2) 1.150557(15) 0.81695(2) 0.04784(15) Uani 1 1 d . . . Ir3 Ir 0.21756(2) 0.962578(14) 0.71697(2) 0.04709(15) Uani 1 1 d . . . Ir4 Ir 0.30822(3) 0.963487(15) 0.56127(2) 0.05073(15) Uani 1 1 d . . . Ir5 Ir 0.71541(3) 0.755181(15) 0.98084(2) 0.05538(17) Uani 1 1 d . . . Ir6 Ir 0.82331(3) 0.761721(17) 0.83493(2) 0.05462(17) Uani 1 1 d . . . N1 N 0.7194(5) 1.1649(3) 0.9006(4) 0.047(3) Uani 1 1 d . . . N2 N 0.8271(5) 1.1212(3) 0.9527(4) 0.046(3) Uani 1 1 d . . . N3 N 0.8614(4) 1.1211(3) 0.8875(4) 0.043(2) Uani 1 1 d . . . N4 N 0.7537(5) 1.1670(3) 0.8354(4) 0.053(3) Uani 1 1 d . . . N5 N 0.2512(5) 0.9233(3) 0.6729(4) 0.049(3) Uani 1 1 d . . . N6 N 0.2520(5) 1.0042(3) 0.6754(4) 0.046(3) Uani 1 1 d . . . N7 N 0.2882(5) 1.0046(3) 0.6114(4) 0.046(3) Uani 1 1 d . . . N8 N 0.2829(5) 0.9234(3) 0.6073(4) 0.056(3) Uani 1 1 d . . . N9 N 0.7921(5) 0.7820(3) 0.9653(4) 0.058(3) Uani 1 1 d . . . N10 N 0.6900(6) 0.7418(3) 0.9049(4) 0.065(3) Uani 1 1 d . . . N11 N 0.7360(5) 0.7433(3) 0.8465(4) 0.046(3) Uani 1 1 d . . . N12 N 0.8375(6) 0.7858(3) 0.9064(4) 0.060(3) Uani 1 1 d . . . N13 N 0.6175(5) 0.9593(3) 0.9413(4) 0.043(2) Uani 1 1 d . . . N14 N 0.5277(5) 0.9963(3) 0.8934(4) 0.039(2) Uani 1 1 d . . . N15 N 0.5223(5) 0.9253(3) 0.8923(4) 0.046(3) Uani 1 1 d . . . N16 N 0.7010(5) 1.0996(3) 0.9607(4) 0.046(3) Uani 1 1 d . . . N17 N 0.3125(4) 0.9624(3) 0.7685(4) 0.036(2) Uani 1 1 d . . . N18 N 0.6697(5) 0.8119(3) 0.9606(5) 0.060(3) Uani 1 1 d . . . N19 N 0.7242(5) 0.9543(3) 0.7509(4) 0.048(3) Uani 1 1 d . . . N20 N 0.6298(5) 0.9907(3) 0.7069(4) 0.048(3) Uani 1 1 d . . . N21 N 0.6277(5) 0.9205(3) 0.7092(4) 0.051(3) Uani 1 1 d . . . N22 N 0.7887(5) 1.0979(3) 0.7900(4) 0.058(3) Uani 1 1 d . . . N23 N 0.4025(5) 0.9607(3) 0.6108(5) 0.059(3) Uani 1 1 d . . . N24 N 0.7769(4) 0.8150(3) 0.8063(4) 0.050(3) Uani 1 1 d . . . O1 O 0.0514(7) 0.1085(4) 0.1412(6) 0.139(6) Uani 1 1 d . . . O2 O 0.0804(7) 0.0442(4) 0.1819(7) 0.141(6) Uani 1 1 d . . . O3 O -0.0303(7) 0.0569(5) 0.1351(6) 0.161(7) Uani 1 1 d . . . O4 O 0.3067(9) 0.7806(6) 0.8740(6) 0.167(7) Uani 1 1 d U . . O5 O 0.3128(9) 0.8398(5) 0.8283(8) 0.167(7) Uani 1 1 d U . . O6 O 0.3138(11) 0.7745(6) 0.7932(7) 0.187(8) Uani 1 1 d U . . O7 O 0.1452(11) 0.4099(8) 0.3341(10) 0.259(11) Uani 1 1 d DU . . O8 O 0.1608(9) 0.3457(4) 0.3610(9) 0.185(9) Uani 1 1 d D . . O9 O 0.2284(17) 0.3910(10) 0.4138(8) 0.332(17) Uani 1 1 d DU . . S1 S 0.0300(3) 0.07288(19) 0.1599(2) 0.1112(18) Uani 1 1 d . . . S2 S 0.3275(4) 0.80089(19) 0.8332(3) 0.137(3) Uani 1 1 d D . . S3 S 0.1879(4) 0.38355(18) 0.3647(3) 0.130(2) Uani 1 1 d D . . F1 F -0.0032(9) 0.0636(5) 0.2368(7) 0.195(7) Uani 1 1 d . . . F2 F 0.0713(9) 0.1117(5) 0.2426(6) 0.188(7) Uani 1 1 d . . . F3 F -0.0283(8) 0.1229(4) 0.2004(7) 0.179(7) Uani 1 1 d . . . F4 F 0.4186(11) 0.8232(7) 0.8948(7) 0.261(10) Uani 1 1 d DU . . F5 F 0.4350(11) 0.7646(5) 0.8766(8) 0.255(10) Uani 1 1 d DU . . F6 F 0.4324(9) 0.8127(6) 0.8265(6) 0.260(11) Uani 1 1 d D . . F7 F 0.2878(12) 0.3550(6) 0.3489(9) 0.273(11) Uiso 1 1 d D . . F8 F 0.2266(15) 0.3837(9) 0.2884(10) 0.43(2) Uiso 1 1 d D . . F9 F 0.2922(11) 0.4177(6) 0.3419(8) 0.249(9) Uiso 1 1 d D . . C1 C 0.6759(5) 1.1861(3) 0.8624(5) 0.043(3) Uani 1 1 d . . . C2 C 0.6182(6) 1.2041(4) 0.8614(6) 0.060(4) Uani 1 1 d . . . H2 H 0.6044 1.2041 0.8885 0.072 Uiso 1 1 calc R . . C3 C 0.5820(7) 1.2224(4) 0.8165(6) 0.070(4) Uani 1 1 d . . . H3 H 0.5413 1.2336 0.8127 0.084 Uiso 1 1 calc R . . C4 C 0.6048(8) 1.2241(4) 0.7788(6) 0.067(4) Uani 1 1 d . . . H4 H 0.5814 1.2388 0.7507 0.080 Uiso 1 1 calc R . . C5 C 0.6586(6) 1.2059(4) 0.7804(6) 0.060(4) Uani 1 1 d . . . H5 H 0.6720 1.2055 0.7530 0.072 Uiso 1 1 calc R . . C6 C 0.6956(6) 1.1870(3) 0.8241(5) 0.042(3) Uani 1 1 d . . . C7 C 0.7649(6) 1.1559(3) 0.8818(5) 0.043(3) Uani 1 1 d . . . C8 C 0.8181(6) 1.1325(4) 0.9084(6) 0.052(4) Uani 1 1 d . . . C9 C 0.8791(7) 1.0965(4) 0.9620(6) 0.062(4) Uani 1 1 d . . . C10 C 0.9115(7) 1.0728(4) 1.0025(6) 0.061(4) Uani 1 1 d . . . H10 H 0.8969 1.0723 1.0292 0.074 Uiso 1 1 calc R . . C11 C 0.9650(8) 1.0499(4) 1.0039(7) 0.079(5) Uani 1 1 d . . . H11 H 0.9880 1.0350 1.0320 0.094 Uiso 1 1 calc R . . C12 C 0.9839(7) 1.0493(4) 0.9628(8) 0.078(5) Uani 1 1 d . . . H12 H 1.0193 1.0332 0.9634 0.094 Uiso 1 1 calc R . . C13 C 0.9518(7) 1.0720(5) 0.9205(7) 0.074(5) Uani 1 1 d . . . H13 H 0.9640 1.0712 0.8927 0.089 Uiso 1 1 calc R . . C14 C 0.9007(6) 1.0955(4) 0.9230(5) 0.052(3) Uani 1 1 d . . . C15 C 0.2655(6) 0.8834(3) 0.6659(5) 0.055(4) Uani 1 1 d . . . C16 C 0.2704(7) 0.8491(4) 0.6939(6) 0.073(5) Uani 1 1 d . . . H16 H 0.2581 0.8492 0.7217 0.088 Uiso 1 1 calc R . . C17 C 0.2943(8) 0.8141(4) 0.6792(7) 0.086(6) Uani 1 1 d . . . H17 H 0.2965 0.7899 0.6965 0.103 Uiso 1 1 calc R . . C18 C 0.3153(7) 0.8148(4) 0.6378(6) 0.062(4) Uani 1 1 d . . . H18 H 0.3341 0.7918 0.6294 0.074 Uiso 1 1 calc R . . C19 C 0.3084(7) 0.8469(4) 0.6125(6) 0.062(4) Uani 1 1 d . . . H19 H 0.3186 0.8461 0.5838 0.074 Uiso 1 1 calc R . . C20 C 0.2861(6) 0.8835(3) 0.6257(5) 0.051(3) Uani 1 1 d . . . C21 C 0.2623(6) 0.9432(3) 0.6382(5) 0.043(3) Uani 1 1 d . . . C22 C 0.2621(6) 0.9843(4) 0.6393(5) 0.046(3) Uani 1 1 d . . . C23 C 0.2730(7) 1.0421(3) 0.6708(5) 0.059(4) Uani 1 1 d . . . C24 C 0.2806(7) 1.0772(4) 0.7007(6) 0.069(4) Uani 1 1 d . . . H24 H 0.2678 1.0775 0.7282 0.083 Uiso 1 1 calc R . . C25 C 0.3061(6) 1.1086(4) 0.6878(6) 0.062(4) Uani 1 1 d . . . H25 H 0.3083 1.1329 0.7048 0.074 Uiso 1 1 calc R . . C26 C 0.3301(7) 1.1072(4) 0.6498(7) 0.075(5) Uani 1 1 d . . . H26 H 0.3508 1.1304 0.6438 0.090 Uiso 1 1 calc R . . C27 C 0.3260(7) 1.0759(4) 0.6217(5) 0.059(4) Uani 1 1 d . . . H27 H 0.3412 1.0767 0.5953 0.071 Uiso 1 1 calc R . . C28 C 0.2995(6) 1.0432(3) 0.6321(5) 0.046(3) Uani 1 1 d . . . C29 C 0.8475(6) 0.8084(4) 0.9824(6) 0.061(4) Uani 1 1 d . . . C30 C 0.8741(7) 0.8304(5) 1.0219(6) 0.073(4) Uani 1 1 d . . . H30 H 0.8571 0.8289 1.0474 0.088 Uiso 1 1 calc R . . C31 C 0.9250(8) 0.8550(5) 1.0270(7) 0.075(5) Uani 1 1 d . . . H31 H 0.9420 0.8714 1.0547 0.090 Uiso 1 1 calc R . . C32 C 0.9515(8) 0.8553(5) 0.9904(7) 0.076(5) Uani 1 1 d . . . H32 H 0.9892 0.8707 0.9952 0.092 Uiso 1 1 calc R . . C33 C 0.9265(8) 0.8350(5) 0.9487(6) 0.076(5) Uani 1 1 d . . . H33 H 0.9435 0.8378 0.9234 0.091 Uiso 1 1 calc R . . C34 C 0.8764(6) 0.8105(4) 0.9443(5) 0.062(4) Uani 1 1 d . . . C35 C 0.7911(6) 0.7721(4) 0.9201(6) 0.056(4) Uani 1 1 d . . . C36 C 0.7401(7) 0.7504(4) 0.8916(5) 0.054(4) Uani 1 1 d . . . C37 C 0.6458(5) 0.7264(4) 0.8610(5) 0.047(3) Uani 1 1 d . . . C38 C 0.5845(7) 0.7113(4) 0.8527(6) 0.065(4) Uani 1 1 d . . . H38 H 0.5661 0.7104 0.8774 0.077 Uiso 1 1 calc R . . C39 C 0.5529(8) 0.6981(5) 0.8075(7) 0.078(5) Uani 1 1 d . . . H39 H 0.5113 0.6871 0.8006 0.094 Uiso 1 1 calc R . . C40 C 0.5784(8) 0.7000(4) 0.7705(6) 0.075(5) Uani 1 1 d . . . H40 H 0.5532 0.6920 0.7387 0.090 Uiso 1 1 calc R . . C41 C 0.6409(7) 0.7134(4) 0.7800(6) 0.060(4) Uani 1 1 d . . . H41 H 0.6602 0.7131 0.7559 0.072 Uiso 1 1 calc R . . C42 C 0.6732(5) 0.7272(3) 0.8258(5) 0.042(3) Uani 1 1 d . . . C43 C 0.5886(6) 0.9928(4) 0.9249(4) 0.040(3) Uani 1 1 d . . . C44 C 0.4979(5) 0.9617(3) 0.8775(4) 0.037(3) Uani 1 1 d . . . C45 C 0.5811(6) 0.9266(3) 0.9242(4) 0.039(3) Uani 1 1 d . . . C46 C 0.6381(6) 1.1000(4) 0.9325(5) 0.053(4) Uani 1 1 d . . . H46 H 0.6194 1.1248 0.9196 0.064 Uiso 1 1 calc R . . C47 C 0.6000(5) 1.0666(3) 0.9216(5) 0.047(3) Uani 1 1 d . . . H47 H 0.5565 1.0686 0.9010 0.056 Uiso 1 1 calc R . . C48 C 0.6251(5) 1.0306(4) 0.9404(4) 0.037(3) Uani 1 1 d . . . C49 C 0.6912(6) 1.0284(4) 0.9719(5) 0.051(3) Uani 1 1 d . . . H49 H 0.7105 1.0040 0.9859 0.061 Uiso 1 1 calc R . . C50 C 0.7237(6) 1.0629(4) 0.9802(4) 0.044(3) Uani 1 1 d . . . H50 H 0.7669 1.0620 1.0018 0.053 Uiso 1 1 calc R . . C51 C 0.3422(6) 0.9281(3) 0.7872(5) 0.047(3) Uani 1 1 d . . . H51 H 0.3220 0.9037 0.7740 0.056 Uiso 1 1 calc R . . C52 C 0.3974(7) 0.9267(3) 0.8224(5) 0.052(3) Uani 1 1 d . . . H52 H 0.4145 0.9017 0.8361 0.063 Uiso 1 1 calc R . . C53 C 0.4319(5) 0.9626(3) 0.8403(5) 0.041(3) Uani 1 1 d . . . C54 C 0.4029(6) 0.9982(3) 0.8232(4) 0.042(3) Uani 1 1 d . . . H54 H 0.4229 1.0229 0.8356 0.050 Uiso 1 1 calc R . . C55 C 0.3432(7) 0.9968(4) 0.7869(5) 0.051(3) Uani 1 1 d . . . H55 H 0.3228 1.0213 0.7744 0.061 Uiso 1 1 calc R . . C56 C 0.6997(7) 0.8447(4) 0.9830(7) 0.080(5) Uani 1 1 d . . . H56 H 0.7419 0.8420 1.0057 0.096 Uiso 1 1 calc R . . C57 C 0.6725(6) 0.8825(3) 0.9749(5) 0.048(3) Uani 1 1 d . . . H57 H 0.6938 0.9050 0.9929 0.058 Uiso 1 1 calc R . . C58 C 0.6121(5) 0.8857(3) 0.9388(5) 0.043(3) Uani 1 1 d . . . C59 C 0.5807(7) 0.8514(4) 0.9161(6) 0.071(4) Uani 1 1 d . . . H59 H 0.5385 0.8526 0.8930 0.085 Uiso 1 1 calc R . . C60 C 0.6127(8) 0.8155(4) 0.9283(7) 0.073(5) Uani 1 1 d . . . H60 H 0.5920 0.7921 0.9122 0.088 Uiso 1 1 calc R . . C61 C 0.6927(7) 0.9892(4) 0.7343(5) 0.058(4) Uani 1 1 d . . . C62 C 0.6004(6) 0.9563(4) 0.6945(5) 0.059(4) Uani 1 1 d . . . C63 C 0.6897(6) 0.9228(4) 0.7383(4) 0.046(3) Uani 1 1 d . . . C64 C 0.7273(6) 1.0978(3) 0.7599(5) 0.049(3) Uani 1 1 d . . . H64 H 0.7050 1.1225 0.7529 0.059 Uiso 1 1 calc R . . C65 C 0.6955(7) 1.0641(5) 0.7389(6) 0.071(4) Uani 1 1 d . . . H65 H 0.6531 1.0657 0.7163 0.085 Uiso 1 1 calc R . . C66 C 0.7255(5) 1.0282(4) 0.7509(4) 0.037(3) Uani 1 1 d . . . C67 C 0.7895(4) 1.0290(4) 0.7805(5) 0.044(3) Uani 1 1 d U . . H67 H 0.8134 1.0049 0.7882 0.052 Uiso 1 1 calc R . . C68 C 0.8167(6) 1.0626(3) 0.7976(5) 0.051(4) Uani 1 1 d . . . H68 H 0.8607 1.0618 0.8173 0.061 Uiso 1 1 calc R . . C69 C 0.4341(7) 0.9260(4) 0.6270(6) 0.062(4) Uani 1 1 d . . . H69 H 0.4098 0.9021 0.6191 0.074 Uiso 1 1 calc R . . C70 C 0.4958(7) 0.9226(4) 0.6528(6) 0.069(4) Uani 1 1 d . . . H70 H 0.5150 0.8974 0.6635 0.083 Uiso 1 1 calc R . . C71 C 0.5312(6) 0.9578(4) 0.6634(5) 0.052(3) Uani 1 1 d . . . C72 C 0.5020(7) 0.9936(4) 0.6501(6) 0.070(4) Uani 1 1 d . . . H72 H 0.5253 1.0179 0.6579 0.084 Uiso 1 1 calc R . . C73 C 0.4364(8) 0.9931(5) 0.6246(6) 0.075(5) Uani 1 1 d . . . H73 H 0.4148 1.0180 0.6166 0.090 Uiso 1 1 calc R . . C74 C 0.8069(5) 0.8494(3) 0.8142(5) 0.045(3) Uani 1 1 d . . . H74 H 0.8496 0.8497 0.8367 0.054 Uiso 1 1 calc R . . C75 C 0.7817(7) 0.8852(4) 0.7926(6) 0.066(4) Uani 1 1 d . . . H75 H 0.8053 0.9094 0.8009 0.079 Uiso 1 1 calc R . . C76 C 0.7225(5) 0.8843(3) 0.7596(5) 0.041(3) Uani 1 1 d . . . C77 C 0.6861(6) 0.8464(4) 0.7469(5) 0.056(4) Uani 1 1 d . . . H77 H 0.6440 0.8449 0.7237 0.067 Uiso 1 1 calc R . . C78 C 0.7180(7) 0.8139(4) 0.7712(5) 0.054(4) Uani 1 1 d . . . H78 H 0.6977 0.7887 0.7632 0.065 Uiso 1 1 calc R . . C79 C 0.7561(7) 1.2111(4) 1.0021(5) 0.051(3) Uani 1 1 d . . . C80 C 0.7159(8) 1.1896(4) 1.0173(6) 0.068(4) Uani 1 1 d . . . C81 C 0.7551(8) 1.1599(4) 1.0504(5) 0.062(4) Uani 1 1 d . . . C82 C 0.8218(6) 1.1658(4) 1.0507(5) 0.047(3) Uani 1 1 d . . . C83 C 0.8183(7) 1.1992(4) 1.0166(6) 0.061(4) Uani 1 1 d . . . C84 C 0.7325(10) 1.2472(4) 0.9631(8) 0.107(7) Uani 1 1 d . . . H84A H 0.6936 1.2390 0.9368 0.161 Uiso 1 1 calc R . . H84B H 0.7664 1.2534 0.9500 0.161 Uiso 1 1 calc R . . H84C H 0.7233 1.2708 0.9791 0.161 Uiso 1 1 calc R . . C85 C 0.6446(8) 1.1953(5) 1.0084(6) 0.076(5) Uani 1 1 d . . . H85A H 0.6393 1.2105 1.0352 0.115 Uiso 1 1 calc R . . H85B H 0.6240 1.1692 1.0063 0.115 Uiso 1 1 calc R . . H85C H 0.6247 1.2098 0.9781 0.115 Uiso 1 1 calc R . . C86 C 0.7343(10) 1.1280(5) 1.0769(7) 0.103(7) Uani 1 1 d . . . H86A H 0.7388 1.1375 1.1093 0.154 Uiso 1 1 calc R . . H86B H 0.7612 1.1043 1.0794 0.154 Uiso 1 1 calc R . . H86C H 0.6893 1.1212 1.0593 0.154 Uiso 1 1 calc R . . C87 C 0.8787(8) 1.1439(4) 1.0788(6) 0.078(5) Uani 1 1 d . . . H87A H 0.9004 1.1581 1.1091 0.117 Uiso 1 1 calc R . . H87B H 0.9078 1.1417 1.0604 0.117 Uiso 1 1 calc R . . H87C H 0.8665 1.1172 1.0859 0.117 Uiso 1 1 calc R . . C88 C 0.8798(8) 1.2152(5) 1.0092(7) 0.094(6) Uani 1 1 d . . . H88A H 0.8679 1.2312 0.9797 0.142 Uiso 1 1 calc R . . H88B H 0.9066 1.1927 1.0065 0.142 Uiso 1 1 calc R . . H88C H 0.9039 1.2318 1.0369 0.142 Uiso 1 1 calc R . . C89 C 0.8570(6) 1.2094(4) 0.7977(6) 0.061(4) Uani 1 1 d . . . C90 C 0.9133(6) 1.1938(5) 0.8324(5) 0.063(4) Uani 1 1 d . . . C91 C 0.9283(8) 1.1582(4) 0.8099(6) 0.064(4) Uani 1 1 d . . . C92 C 0.8844(7) 1.1537(5) 0.7634(6) 0.061(4) Uani 1 1 d . . . C93 C 0.8384(7) 1.1843(5) 0.7553(6) 0.066(4) Uani 1 1 d . . . C94 C 0.8262(7) 1.2477(4) 0.8048(5) 0.064(4) Uani 1 1 d . . . H94A H 0.8306 1.2504 0.8389 0.095 Uiso 1 1 calc R . . H94B H 0.7806 1.2474 0.7849 0.095 Uiso 1 1 calc R . . H94C H 0.8474 1.2702 0.7954 0.095 Uiso 1 1 calc R . . C95 C 0.9502(8) 1.2117(5) 0.8830(7) 0.091(6) Uani 1 1 d . . . H95A H 0.9948 1.2169 0.8858 0.137 Uiso 1 1 calc R . . H95B H 0.9493 1.1927 0.9080 0.137 Uiso 1 1 calc R . . H95C H 0.9297 1.2367 0.8871 0.137 Uiso 1 1 calc R . . C96 C 0.9891(8) 1.1347(5) 0.8331(7) 0.087(5) Uani 1 1 d . . . H96A H 0.9829 1.1073 0.8209 0.130 Uiso 1 1 calc R . . H96B H 0.9996 1.1345 0.8682 0.130 Uiso 1 1 calc R . . H96C H 1.0243 1.1471 0.8253 0.130 Uiso 1 1 calc R . . C97 C 0.8836(8) 1.1201(5) 0.7304(6) 0.083(5) Uani 1 1 d . . . H97A H 0.9130 1.1260 0.7129 0.124 Uiso 1 1 calc R . . H97B H 0.8400 1.1166 0.7072 0.124 Uiso 1 1 calc R . . H97C H 0.8974 1.0956 0.7492 0.124 Uiso 1 1 calc R . . C98 C 0.7812(7) 1.1915(5) 0.7079(6) 0.075(5) Uani 1 1 d . . . H98A H 0.7973 1.2016 0.6830 0.113 Uiso 1 1 calc R . . H98B H 0.7519 1.2111 0.7137 0.113 Uiso 1 1 calc R . . H98C H 0.7583 1.1664 0.6970 0.113 Uiso 1 1 calc R . . C99 C 0.1159(7) 0.9689(5) 0.6824(7) 0.071(4) Uani 1 1 d . . . C100 C 0.1279(8) 0.9317(5) 0.7040(8) 0.093(6) Uani 1 1 d . . . C101 C 0.1643(7) 0.9375(5) 0.7586(8) 0.084(6) Uani 1 1 d . . . C102 C 0.1676(7) 0.9773(5) 0.7671(6) 0.068(4) Uani 1 1 d . . . C103 C 0.1383(9) 0.9961(5) 0.7208(8) 0.086(5) Uani 1 1 d . . . C104 C 0.0774(10) 0.9780(9) 0.6320(8) 0.161(12) Uani 1 1 d . . . H10A H 0.0810 0.9560 0.6112 0.242 Uiso 1 1 calc R . . H10B H 0.0931 1.0026 0.6221 0.242 Uiso 1 1 calc R . . H10C H 0.0324 0.9813 0.6291 0.242 Uiso 1 1 calc R . . C105 C 0.1119(10) 0.8905(6) 0.6818(9) 0.140(8) Uani 1 1 d U . . H10D H 0.0679 0.8834 0.6790 0.211 Uiso 1 1 calc R . . H10E H 0.1418 0.8710 0.7023 0.211 Uiso 1 1 calc R . . H10F H 0.1156 0.8905 0.6496 0.211 Uiso 1 1 calc R . . C106 C 0.1874(11) 0.9039(8) 0.7949(10) 0.158(12) Uani 1 1 d . . . H10G H 0.1941 0.9140 0.8274 0.236 Uiso 1 1 calc R . . H10H H 0.2279 0.8933 0.7935 0.236 Uiso 1 1 calc R . . H10I H 0.1551 0.8827 0.7871 0.236 Uiso 1 1 calc R . . C107 C 0.1942(10) 0.9964(8) 0.8132(9) 0.134(9) Uani 1 1 d . . . H10J H 0.1643 0.9937 0.8309 0.201 Uiso 1 1 calc R . . H10K H 0.2013 1.0247 0.8085 0.201 Uiso 1 1 calc R . . H10L H 0.2351 0.9837 0.8316 0.201 Uiso 1 1 calc R . . C108 C 0.1298(10) 1.0430(5) 0.7166(9) 0.119(8) Uani 1 1 d . . . H10M H 0.1408 1.0525 0.6890 0.178 Uiso 1 1 calc R . . H10N H 0.1582 1.0555 0.7462 0.178 Uiso 1 1 calc R . . H10O H 0.0852 1.0499 0.7118 0.178 Uiso 1 1 calc R . . C109 C 0.2471(10) 0.9401(6) 0.4914(5) 0.086(5) Uani 1 1 d . . . C110 C 0.2330(11) 0.9807(7) 0.4964(6) 0.093(6) Uani 1 1 d . . . C111 C 0.2862(10) 1.0010(6) 0.4983(5) 0.077(5) Uani 1 1 d . . . C112 C 0.3424(11) 0.9747(8) 0.5003(8) 0.108(7) Uani 1 1 d . . . C113 C 0.3147(13) 0.9347(6) 0.4986(6) 0.099(7) Uani 1 1 d . . . C114 C 0.2070(10) 0.9033(7) 0.4909(7) 0.127(8) Uani 1 1 d . . . H11A H 0.1760 0.9094 0.5069 0.191 Uiso 1 1 calc R . . H11B H 0.2352 0.8816 0.5081 0.191 Uiso 1 1 calc R . . H11C H 0.1841 0.8952 0.4575 0.191 Uiso 1 1 calc R . . C115 C 0.1655(17) 0.9976(11) 0.4903(10) 0.225(18) Uani 1 1 d . . . H11D H 0.1415 1.0022 0.4560 0.338 Uiso 1 1 calc R . . H11E H 0.1701 1.0229 0.5079 0.338 Uiso 1 1 calc R . . H11F H 0.1422 0.9785 0.5032 0.338 Uiso 1 1 calc R . . C116 C 0.2983(13) 1.0457(6) 0.4992(9) 0.144(9) Uani 1 1 d . . . H11G H 0.2592 1.0593 0.4790 0.216 Uiso 1 1 calc R . . H11H H 0.3331 1.0511 0.4867 0.216 Uiso 1 1 calc R . . H11I H 0.3105 1.0554 0.5325 0.216 Uiso 1 1 calc R . . C117 C 0.4037(13) 0.9857(10) 0.5024(10) 0.191(14) Uani 1 1 d . . . H11J H 0.4034 1.0136 0.4925 0.287 Uiso 1 1 calc R . . H11K H 0.4172 0.9687 0.4807 0.287 Uiso 1 1 calc R . . H11L H 0.4337 0.9825 0.5355 0.287 Uiso 1 1 calc R . . C118 C 0.3546(14) 0.8983(8) 0.4945(9) 0.162(10) Uani 1 1 d U . . H11M H 0.3302 0.8739 0.4942 0.242 Uiso 1 1 calc R . . H11N H 0.3948 0.8978 0.5221 0.242 Uiso 1 1 calc R . . H11O H 0.3641 0.9001 0.4645 0.242 Uiso 1 1 calc R . . C119 C 0.6901(4) 0.6960(2) 0.9994(3) 0.083(5) Uani 1 1 d GU . . C120 C 0.7575(4) 0.70192(19) 1.0223(2) 0.112(7) Uani 1 1 d GU . . C121 C 0.7667(4) 0.7353(2) 1.0540(2) 0.094(6) Uani 1 1 d GU . . C122 C 0.7050(5) 0.7501(2) 1.0507(3) 0.091(6) Uani 1 1 d GU . . C123 C 0.6576(5) 0.7258(2) 1.0169(3) 0.091(5) Uani 1 1 d GU . . C124 C 0.6584(5) 0.6638(3) 0.9629(3) 0.181(12) Uani 1 1 d GU . . H12A H 0.6347 0.6762 0.9317 0.271 Uiso 1 1 calc R . . H12B H 0.6287 0.6485 0.9741 0.271 Uiso 1 1 calc R . . H12C H 0.6914 0.6460 0.9591 0.271 Uiso 1 1 calc R . . C125 C 0.8101(4) 0.6770(2) 1.0144(3) 0.27(2) Uiso 1 1 d G . . H12D H 0.8025 0.6488 1.0190 0.412 Uiso 1 1 calc R . . H12E H 0.8518 0.6850 1.0376 0.412 Uiso 1 1 calc R . . H12F H 0.8099 0.6812 0.9815 0.412 Uiso 1 1 calc R . . C126 C 0.8309(5) 0.7521(3) 1.0857(3) 0.167(11) Uani 1 1 d GU . . H12G H 0.8253 0.7671 1.1125 0.251 Uiso 1 1 calc R . . H12H H 0.8476 0.7700 1.0664 0.251 Uiso 1 1 calc R . . H12I H 0.8613 0.7303 1.0985 0.251 Uiso 1 1 calc R . . C127 C 0.6921(6) 0.7854(3) 1.0782(3) 0.176(11) Uani 1 1 d GU . . H12J H 0.6890 0.7762 1.1088 0.264 Uiso 1 1 calc R . . H12K H 0.6516 0.7981 1.0589 0.264 Uiso 1 1 calc R . . H12L H 0.7272 0.8046 1.0846 0.264 Uiso 1 1 calc R . . C128 C 0.5854(5) 0.7308(3) 1.0022(3) 0.185(11) Uani 1 1 d GU . . H12M H 0.5656 0.7047 1.0026 0.278 Uiso 1 1 calc R . . H12N H 0.5685 0.7421 0.9697 0.278 Uiso 1 1 calc R . . H12O H 0.5757 0.7487 1.0250 0.278 Uiso 1 1 calc R . . C129 C 0.8411(4) 0.7280(3) 0.7799(3) 0.098(6) Uani 1 1 d GU . . C130 C 0.8785(4) 0.7610(3) 0.7847(4) 0.098(7) Uani 1 1 d G . . C131 C 0.9214(4) 0.7616(3) 0.8305(4) 0.096(6) Uani 1 1 d G . . C132 C 0.9106(3) 0.7290(2) 0.8540(3) 0.078(5) Uani 1 1 d G . . C133 C 0.8610(4) 0.7083(2) 0.8228(3) 0.098(7) Uani 1 1 d G . . C134 C 0.7894(5) 0.7160(4) 0.7368(4) 0.195(12) Uani 1 1 d GU . . H13A H 0.8068 0.7008 0.7158 0.293 Uiso 1 1 calc R . . H13B H 0.7674 0.7398 0.7196 0.293 Uiso 1 1 calc R . . H13C H 0.7589 0.6994 0.7457 0.293 Uiso 1 1 calc R . . C135 C 0.8734(6) 0.7902(3) 0.7475(4) 0.261(19) Uani 1 1 d GU . . H13D H 0.9026 0.7830 0.7304 0.392 Uiso 1 1 calc R . . H13E H 0.8850 0.8165 0.7623 0.392 Uiso 1 1 calc R . . H13F H 0.8292 0.7908 0.7247 0.392 Uiso 1 1 calc R . . C136 C 0.9700(5) 0.7916(3) 0.8506(4) 0.192(13) Uiso 1 1 d G . . H13G H 0.9970 0.7838 0.8833 0.288 Uiso 1 1 calc R . . H13H H 0.9494 0.8172 0.8519 0.288 Uiso 1 1 calc R . . H13I H 0.9967 0.7943 0.8303 0.288 Uiso 1 1 calc R . . C137 C 0.9457(3) 0.7183(3) 0.9036(3) 0.173(13) Uani 1 1 d G . . H13J H 0.9912 0.7248 0.9114 0.260 Uiso 1 1 calc R . . H13K H 0.9410 0.6897 0.9081 0.260 Uiso 1 1 calc R . . H13L H 0.9287 0.7333 0.9251 0.260 Uiso 1 1 calc R . . C138 C 0.8341(5) 0.6716(2) 0.8333(4) 0.189(12) Uani 1 1 d GU . . H13M H 0.7874 0.6744 0.8239 0.283 Uiso 1 1 calc R . . H13N H 0.8526 0.6660 0.8679 0.283 Uiso 1 1 calc R . . H13O H 0.8440 0.6497 0.8151 0.283 Uiso 1 1 calc R . . C139 C 0.0130(13) 0.0922(8) 0.2127(10) 0.119(7) Uiso 1 1 d . . . C140 C 0.4098(9) 0.7981(7) 0.8591(8) 0.236(19) Uiso 1 1 d D . . C141 C 0.2500(12) 0.3881(8) 0.3380(11) 0.26(2) Uiso 1 1 d D . . C145 C 0.8353(11) 0.9400(7) 0.9272(8) 0.092(14) Uani 0.401(11) 1 d PGU A 1 H145 H 0.8754 0.9299 0.9477 0.111 Uiso 0.401(11) 1 calc PR A 1 C146 C 0.8276(10) 0.9813(7) 0.9182(8) 0.057(9) Uani 0.401(11) 1 d PGU A 1 H146 H 0.8624 0.9990 0.9325 0.068 Uiso 0.401(11) 1 calc PR A 1 C147 C 0.7681(9) 0.9964(5) 0.8878(7) 0.089(18) Uani 0.401(11) 1 d PGD A 1 C148 C 0.7164(7) 0.9702(4) 0.8664(5) 0.107(8) Uani 0.401(11) 1 d PG A 1 C149 C 0.7242(9) 0.9290(5) 0.8754(7) 0.093(8) Uani 0.401(11) 1 d PGD A 1 C150 C 0.7836(10) 0.9138(7) 0.9058(9) 0.081(12) Uani 0.401(11) 1 d PGU A 1 H150 H 0.7889 0.8860 0.9119 0.098 Uiso 0.401(11) 1 calc PR A 1 C151 C 0.6494(8) 0.9801(5) 0.8353(6) 0.049(9) Uani 0.401(11) 1 d PGU A 1 C152 C 0.6359(10) 1.0210(6) 0.8261(8) 0.064(11) Uani 0.401(11) 1 d PGDU A 1 C153 C 0.5751(13) 1.0331(8) 0.7946(10) 0.120(8) Uani 0.401(11) 1 d PGU A 1 H153 H 0.5660 1.0606 0.7884 0.144 Uiso 0.401(11) 1 calc PR A 1 C154 C 0.5277(14) 1.0044(9) 0.7723(10) 0.144(11) Uani 0.401(11) 1 d PGU A 1 H154 H 0.4867 1.0125 0.7511 0.173 Uiso 0.401(11) 1 calc PR A 1 C155 C 0.5413(13) 0.9635(8) 0.7815(10) 0.074(12) Uani 0.401(11) 1 d PGU A 1 H155 H 0.5094 0.9441 0.7665 0.089 Uiso 0.401(11) 1 calc PR A 1 C156 C 0.6021(10) 0.9513(6) 0.8131(8) 0.062(5) Uani 0.401(11) 1 d PGD A 1 C157 C 0.750(3) 1.0352(10) 0.872(2) 0.13(2) Uani 0.401(11) 1 d PDU A 1 H157 H 0.7831 1.0549 0.8804 0.161 Uiso 0.401(11) 1 calc PR A 1 C158 C 0.688(2) 1.0474(16) 0.846(2) 0.093(9) Uani 0.401(11) 1 d PD A 1 H158 H 0.6801 1.0751 0.8405 0.111 Uiso 0.401(11) 1 calc PR A 1 C159 C 0.6737(18) 0.9011(14) 0.8538(15) 0.098(15) Uani 0.401(11) 1 d PDU A 1 H159 H 0.6827 0.8739 0.8621 0.117 Uiso 0.401(11) 1 calc PR A 1 C160 C 0.612(2) 0.9103(9) 0.8213(18) 0.115(19) Uani 0.401(11) 1 d PDU A 1 H160 H 0.5803 0.8907 0.8065 0.138 Uiso 0.401(11) 1 calc PR A 1 C14A C 0.4919(8) 1.0911(5) 0.7489(6) 0.129(15) Uani 0.599(11) 1 d PG A 2 H14A H 0.4607 1.1103 0.7323 0.155 Uiso 0.599(11) 1 calc PR A 2 C14B C 0.4757(7) 1.0501(4) 0.7458(6) 0.102(12) Uani 0.599(11) 1 d PG A 2 H14B H 0.4335 1.0418 0.7270 0.123 Uiso 0.599(11) 1 calc PR A 2 C14C C 0.5223(6) 1.0215(3) 0.7706(5) 0.144(11) Uani 0.599(11) 1 d PGD A 2 C14D C 0.5851(5) 1.0338(3) 0.7987(4) 0.120(8) Uani 0.599(11) 1 d PGU A 2 C14E C 0.6013(6) 1.0748(4) 0.8018(5) 0.19(2) Uani 0.599(11) 1 d PGU A 2 C15A C 0.5548(8) 1.1034(4) 0.7770(6) 0.058(7) Uani 0.599(11) 1 d PG A 2 H15A H 0.5656 1.1309 0.7791 0.069 Uiso 0.599(11) 1 calc PR A 2 C15B C 0.6260(6) 0.9978(3) 0.8205(4) 0.066(8) Uani 0.599(11) 1 d PGU A 2 C15C C 0.6060(7) 0.9595(4) 0.8136(5) 0.062(5) Uani 0.599(11) 1 d PGDU A 2 C15D C 0.6462(8) 0.9297(5) 0.8360(6) 0.070(8) Uani 0.599(11) 1 d PG A 2 H15D H 0.6321 0.9028 0.8312 0.085 Uiso 0.599(11) 1 calc PR A 2 C15E C 0.7066(9) 0.9382(6) 0.8655(6) 0.093(8) Uani 0.599(11) 1 d PG A 2 H15E H 0.7350 0.9173 0.8812 0.111 Uiso 0.599(11) 1 calc PR A 2 C15F C 0.7267(8) 0.9765(5) 0.8724(6) 0.107(8) Uani 0.599(11) 1 d PG A 2 H15F H 0.7691 0.9825 0.8930 0.129 Uiso 0.599(11) 1 calc PR A 2 C15G C 0.6864(7) 1.0063(4) 0.8499(5) 0.095(11) Uani 0.599(11) 1 d PG A 2 C15H C 0.6638(18) 1.0788(12) 0.8399(14) 0.117(12) Uani 0.599(11) 1 d PU A 2 H15H H 0.6772 1.1052 0.8504 0.141 Uiso 0.599(11) 1 calc PR A 2 C15I C 0.7100(19) 1.0455(11) 0.8646(16) 0.093(9) Uani 0.599(11) 1 d PU A 2 H15I H 0.7511 1.0504 0.8879 0.111 Uiso 0.599(11) 1 calc PR A 2 C15J C 0.5005(18) 0.9736(9) 0.7590(15) 0.113(12) Uani 0.599(11) 1 d PDU A 2 H15J H 0.4598 0.9666 0.7363 0.136 Uiso 0.599(11) 1 calc PR A 2 C16A C 0.542(2) 0.9457(16) 0.7825(19) 0.17(2) Uiso 0.599(11) 1 d PD A 2 H16A H 0.5307 0.9182 0.7794 0.208 Uiso 0.599(11) 1 calc PR A 2 C161 C 0.9618(8) 0.2644(6) 0.2265(7) 0.138(9) Uani 1 1 d GDU . . C162 C 0.9313(9) 0.2809(5) 0.1800(7) 0.179(12) Uani 1 1 d GU . . C163 C 0.8761(8) 0.2624(6) 0.1474(7) 0.179(13) Uani 1 1 d GDU . . C164 C 0.8513(9) 0.2273(6) 0.1612(9) 0.203(15) Uani 1 1 d GDU . . H164 H 0.8143 0.2149 0.1393 0.244 Uiso 1 1 calc R . . C165 C 0.8819(11) 0.2108(5) 0.2076(9) 0.168(12) Uani 1 1 d G . . H165 H 0.8653 0.1873 0.2169 0.202 Uiso 1 1 calc R . . C166 C 0.9371(11) 0.2294(6) 0.2403(7) 0.153(10) Uani 1 1 d GU . . C167 C 0.9754(15) 0.2134(10) 0.2896(12) 0.181(12) Uani 1 1 d DU . . H167 H 0.9630 0.1896 0.3016 0.218 Uiso 1 1 calc R . . C168 C 1.0303(17) 0.2348(9) 0.3174(9) 0.236(17) Uani 1 1 d DU . . H168 H 1.0540 0.2244 0.3484 0.283 Uiso 1 1 calc R . . C169 C 1.053(2) 0.2700(13) 0.3037(14) 0.36(3) Uiso 1 1 d D . . H169 H 1.0915 0.2821 0.3245 0.430 Uiso 1 1 calc R . . C170 C 1.0201(11) 0.2868(6) 0.2599(9) 0.119(7) Uani 1 1 d DU . . C171 C 1.0445(10) 0.3274(8) 0.2424(8) 0.155(10) Uani 1 1 d DU . . H171 H 1.0797 0.3421 0.2633 0.186 Uiso 1 1 calc R . . C172 C 1.0118(12) 0.3397(8) 0.1955(9) 0.180(12) Uiso 1 1 d D . . H172 H 1.0238 0.3622 0.1809 0.216 Uiso 1 1 calc R . . C173 C 0.9572(12) 0.3144(8) 0.1711(9) 0.166(11) Uiso 1 1 d D . . C174 C 0.9226(13) 0.3308(9) 0.1253(10) 0.193(13) Uiso 1 1 d D . . H174 H 0.9361 0.3553 0.1156 0.231 Uiso 1 1 calc R . . C175 C 0.8705(14) 0.3118(8) 0.0953(10) 0.195(13) Uani 1 1 d DU . . H175 H 0.8517 0.3231 0.0641 0.234 Uiso 1 1 calc R . . C176 C 0.8418(13) 0.2786(8) 0.1040(9) 0.192(13) Uani 1 1 d DU . . H176 H 0.8027 0.2680 0.0825 0.230 Uiso 1 1 calc R . . C177 C 0.4819(9) 0.9833(4) 0.9913(7) 0.152(10) Uani 1 1 d GDU . . C178 C 0.5208(9) 0.9531(7) 1.0117(6) 0.136(9) Uani 1 1 d GDU . . C179 C 0.5014(12) 0.9156(7) 1.0002(8) 0.28(3) Uiso 1 1 d G . . H179 H 0.5291 0.8940 1.0147 0.336 Uiso 1 1 calc R . . C180 C 0.4431(14) 0.9083(6) 0.9682(9) 0.212(17) Uani 1 1 d G . . H180 H 0.4294 0.8817 0.9600 0.255 Uiso 1 1 calc R . . C181 C 0.4042(11) 0.9386(7) 0.9478(7) 0.160(11) Uani 1 1 d GU . . H181 H 0.3627 0.9335 0.9250 0.192 Uiso 1 1 calc R . . C182 C 0.4236(9) 0.9761(5) 0.9593(7) 0.139(9) Uani 1 1 d GU . . C183 C 0.3942(13) 1.0111(9) 0.9427(9) 0.144(9) Uani 1 1 d DU . . H183 H 0.3530 1.0095 0.9184 0.173 Uiso 1 1 calc R . . C184 C 0.4177(13) 1.0496(9) 0.9571(13) 0.239(18) Uiso 1 1 d D . . H184 H 0.3943 1.0736 0.9468 0.287 Uiso 1 1 calc R . . C185 C 0.1596(16) 0.0441(10) 0.9729(13) 0.187(13) Uani 1 1 d U . . O20 O 0.1582(7) 0.9571(4) 0.9054(7) 0.144(7) Uani 1 1 d . . . C187 C -0.0227(11) 0.9712(8) 0.2060(14) 0.181(14) Uani 1 1 d . . . O19 O 0.2012(9) 0.0314(5) 0.9464(8) 0.169(7) Uani 1 1 d . . . O21 O 0.0364(7) 0.9673(4) 0.1925(8) 0.158(7) 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 0.0428(3) 0.0372(3) 0.0508(3) -0.0054(2) 0.0184(2) -0.0066(2) Ir2 0.0444(3) 0.0460(3) 0.0590(4) 0.0017(2) 0.0254(3) -0.0073(2) Ir3 0.0424(3) 0.0420(3) 0.0531(4) -0.0025(2) 0.0116(2) 0.0007(2) Ir4 0.0510(3) 0.0484(3) 0.0474(3) -0.0046(2) 0.0101(3) 0.0036(2) Ir5 0.0702(4) 0.0423(3) 0.0610(4) 0.0093(3) 0.0320(3) 0.0078(3) Ir6 0.0450(3) 0.0645(4) 0.0576(4) 0.0043(3) 0.0218(3) 0.0168(3) N1 0.035(6) 0.046(6) 0.063(8) -0.009(5) 0.020(6) -0.006(5) N2 0.066(7) 0.032(5) 0.049(7) 0.001(5) 0.029(6) -0.004(5) N3 0.031(5) 0.053(6) 0.045(6) 0.013(5) 0.013(5) 0.005(4) N4 0.046(6) 0.045(6) 0.075(9) 0.007(6) 0.029(6) -0.005(5) N5 0.057(7) 0.033(6) 0.055(7) -0.002(5) 0.019(6) -0.006(5) N6 0.052(6) 0.042(6) 0.040(6) -0.009(5) 0.010(5) 0.006(5) N7 0.040(6) 0.043(6) 0.051(7) 0.010(5) 0.010(5) 0.013(5) N8 0.045(6) 0.044(6) 0.066(8) -0.018(6) 0.003(6) 0.002(5) N9 0.061(8) 0.061(7) 0.053(8) 0.020(6) 0.020(6) 0.018(6) N10 0.084(9) 0.061(8) 0.054(8) 0.012(6) 0.028(7) 0.004(7) N11 0.045(6) 0.042(6) 0.059(8) -0.001(5) 0.026(6) 0.006(5) N12 0.058(8) 0.070(8) 0.050(8) 0.007(6) 0.016(6) 0.020(6) N13 0.048(6) 0.040(6) 0.045(7) 0.001(5) 0.024(5) -0.005(5) N14 0.048(6) 0.029(5) 0.057(7) 0.000(4) 0.039(6) 0.001(4) N15 0.037(6) 0.039(6) 0.058(7) -0.004(5) 0.014(5) -0.003(5) N16 0.041(6) 0.054(7) 0.040(6) -0.007(5) 0.010(5) -0.004(5) N17 0.024(5) 0.038(5) 0.047(6) -0.010(5) 0.012(4) 0.000(4) N18 0.047(7) 0.040(6) 0.095(10) 0.014(6) 0.026(7) -0.004(5) N19 0.036(6) 0.052(7) 0.062(8) 0.015(5) 0.026(5) 0.011(5) N20 0.049(7) 0.042(6) 0.049(7) -0.005(5) 0.012(6) -0.004(5) N21 0.052(7) 0.054(7) 0.041(7) 0.006(5) 0.007(5) 0.009(5) N22 0.062(8) 0.053(7) 0.067(8) -0.021(6) 0.030(7) -0.024(6) N23 0.040(6) 0.039(6) 0.087(9) -0.012(6) 0.009(6) 0.000(5) N24 0.023(5) 0.065(7) 0.053(7) -0.004(6) 0.002(5) 0.000(5) O1 0.136(13) 0.101(10) 0.169(15) 0.049(10) 0.037(11) -0.034(9) O2 0.100(11) 0.123(12) 0.211(18) 0.052(11) 0.070(12) 0.040(9) O3 0.093(11) 0.166(14) 0.167(16) 0.025(12) -0.027(10) -0.069(10) O4 0.203(14) 0.208(14) 0.123(12) 0.003(11) 0.097(11) -0.058(12) O5 0.180(13) 0.103(10) 0.250(16) 0.042(10) 0.113(12) 0.037(10) O6 0.221(16) 0.194(14) 0.154(13) -0.059(12) 0.074(12) -0.062(13) O7 0.226(18) 0.258(18) 0.295(19) 0.119(15) 0.091(15) 0.026(15) O8 0.173(18) 0.090(12) 0.29(3) 0.019(13) 0.085(18) -0.002(11) O9 0.36(2) 0.32(2) 0.28(2) -0.029(17) 0.066(17) -0.058(17) S1 0.072(3) 0.130(5) 0.119(5) 0.025(4) 0.018(3) -0.014(3) S2 0.168(6) 0.094(4) 0.116(5) -0.022(4) 0.008(5) 0.046(4) S3 0.164(6) 0.079(4) 0.125(5) 0.015(3) 0.020(5) -0.006(4) F1 0.237(18) 0.158(13) 0.210(18) 0.042(12) 0.105(15) -0.048(12) F2 0.23(2) 0.186(15) 0.149(14) -0.013(12) 0.072(14) -0.012(14) F3 0.160(13) 0.124(11) 0.29(2) 0.007(12) 0.128(15) 0.000(10) F4 0.258(17) 0.333(18) 0.220(16) -0.028(14) 0.120(14) -0.058(14) F5 0.235(16) 0.215(15) 0.286(17) 0.095(13) 0.051(13) 0.053(13) F6 0.24(2) 0.37(3) 0.24(2) -0.05(2) 0.170(19) -0.11(2) C1 0.037(7) 0.030(6) 0.070(10) 0.003(6) 0.026(7) -0.001(5) C2 0.036(7) 0.048(8) 0.096(12) -0.007(8) 0.022(8) -0.008(6) C3 0.046(8) 0.059(9) 0.091(13) 0.004(9) 0.006(9) 0.006(7) C4 0.080(11) 0.057(9) 0.054(10) -0.004(7) 0.012(9) 0.002(8) C5 0.035(7) 0.054(8) 0.081(11) 0.007(8) 0.006(7) -0.004(6) C6 0.040(7) 0.029(6) 0.064(9) 0.007(6) 0.025(7) -0.008(5) C7 0.046(7) 0.041(7) 0.042(8) 0.000(6) 0.015(6) 0.001(6) C8 0.054(8) 0.039(7) 0.081(11) 0.016(7) 0.045(8) -0.006(6) C9 0.070(10) 0.026(7) 0.090(12) 0.005(7) 0.027(9) -0.008(6) C10 0.057(9) 0.055(8) 0.066(10) 0.012(7) 0.014(8) -0.014(7) C11 0.073(11) 0.058(10) 0.103(15) -0.012(9) 0.027(11) 0.003(8) C12 0.055(10) 0.060(10) 0.128(17) 0.010(10) 0.041(11) 0.002(8) C13 0.064(10) 0.068(10) 0.092(13) -0.031(9) 0.029(9) 0.007(8) C14 0.047(8) 0.044(7) 0.073(10) -0.006(7) 0.029(8) -0.005(6) C15 0.048(8) 0.032(7) 0.059(10) -0.003(6) -0.016(7) 0.000(6) C16 0.061(9) 0.048(9) 0.096(13) 0.007(8) 0.007(9) -0.017(7) C17 0.070(11) 0.034(8) 0.121(16) -0.002(9) -0.006(11) 0.000(7) C18 0.083(11) 0.042(8) 0.055(10) -0.014(7) 0.017(9) 0.004(7) C19 0.060(9) 0.069(10) 0.055(10) -0.021(8) 0.017(8) 0.001(7) C20 0.046(7) 0.025(6) 0.066(10) 0.006(6) 0.000(7) -0.002(5) C21 0.049(7) 0.031(6) 0.043(8) -0.011(6) 0.008(6) -0.007(5) C22 0.043(7) 0.049(8) 0.041(8) 0.012(6) 0.009(6) 0.003(6) C23 0.070(9) 0.025(6) 0.059(10) -0.008(6) -0.007(8) 0.015(6) C24 0.072(10) 0.054(9) 0.080(12) -0.005(8) 0.026(9) 0.018(8) C25 0.050(8) 0.030(7) 0.087(12) 0.004(7) -0.001(8) -0.001(6) C26 0.060(10) 0.051(9) 0.099(14) 0.022(9) 0.007(10) -0.003(7) C27 0.067(9) 0.045(8) 0.060(10) 0.001(7) 0.014(8) -0.003(7) C28 0.067(9) 0.025(6) 0.041(8) 0.002(5) 0.012(7) 0.004(6) C29 0.041(8) 0.071(10) 0.069(11) 0.010(8) 0.015(8) 0.009(7) C30 0.067(10) 0.083(11) 0.066(11) -0.024(9) 0.019(9) -0.012(9) C31 0.064(10) 0.067(10) 0.080(13) -0.001(9) 0.006(9) -0.009(8) C32 0.058(10) 0.073(11) 0.090(14) -0.021(9) 0.016(10) -0.029(8) C33 0.063(10) 0.097(13) 0.070(12) 0.013(10) 0.026(9) 0.016(9) C34 0.036(8) 0.077(10) 0.054(10) 0.002(8) -0.011(7) -0.009(7) C35 0.040(7) 0.068(9) 0.059(10) 0.005(7) 0.018(7) -0.020(7) C36 0.067(10) 0.048(8) 0.051(9) 0.025(7) 0.024(8) 0.015(7) C37 0.028(6) 0.048(7) 0.051(9) -0.009(6) -0.006(6) -0.003(5) C38 0.053(9) 0.052(8) 0.080(12) 0.002(8) 0.012(8) -0.001(7) C39 0.065(11) 0.076(11) 0.073(13) -0.004(9) -0.003(10) -0.006(8) C40 0.088(13) 0.056(9) 0.059(11) -0.011(8) -0.004(10) 0.014(8) C41 0.064(10) 0.050(8) 0.066(11) -0.005(7) 0.021(8) 0.019(7) C42 0.038(7) 0.039(7) 0.057(9) -0.005(6) 0.027(7) 0.003(5) C43 0.042(7) 0.047(7) 0.037(7) -0.014(6) 0.024(6) -0.011(6) C44 0.024(6) 0.045(7) 0.042(7) -0.003(5) 0.012(5) -0.003(5) C45 0.047(7) 0.032(6) 0.047(8) 0.000(5) 0.025(6) -0.014(5) C46 0.054(8) 0.036(7) 0.078(11) -0.002(7) 0.033(8) -0.003(6) C47 0.023(6) 0.041(7) 0.074(10) -0.013(6) 0.014(6) -0.009(5) C48 0.023(6) 0.064(8) 0.032(7) -0.004(6) 0.018(5) -0.001(5) C49 0.056(8) 0.045(7) 0.063(9) 0.011(6) 0.036(7) 0.002(6) C50 0.038(7) 0.068(9) 0.022(7) 0.005(6) 0.004(5) -0.011(6) C51 0.042(7) 0.031(6) 0.069(10) -0.010(6) 0.020(7) -0.010(5) C52 0.076(10) 0.020(6) 0.061(9) 0.003(6) 0.025(8) -0.001(6) C53 0.017(5) 0.051(7) 0.049(8) -0.002(6) 0.003(5) -0.001(5) C54 0.055(8) 0.029(6) 0.037(7) -0.003(5) 0.012(6) -0.001(5) C55 0.066(9) 0.036(7) 0.057(9) 0.003(6) 0.031(8) 0.002(6) C56 0.049(9) 0.029(7) 0.136(16) -0.013(8) -0.002(9) -0.008(6) C57 0.037(7) 0.039(7) 0.067(9) -0.005(6) 0.015(7) -0.007(5) C58 0.026(6) 0.037(7) 0.069(9) 0.004(6) 0.019(6) -0.001(5) C59 0.044(8) 0.070(10) 0.094(13) 0.009(9) 0.019(8) 0.000(7) C60 0.068(11) 0.032(7) 0.121(15) 0.000(8) 0.033(11) -0.015(7) C61 0.082(11) 0.053(8) 0.050(9) -0.010(7) 0.036(8) 0.015(8) C62 0.039(7) 0.066(10) 0.055(9) -0.002(7) -0.005(7) 0.010(7) C63 0.064(9) 0.053(8) 0.032(7) 0.002(6) 0.032(7) 0.000(7) C64 0.044(8) 0.031(6) 0.069(10) -0.001(6) 0.015(7) -0.014(5) C65 0.060(9) 0.080(11) 0.085(12) -0.016(9) 0.041(9) 0.000(8) C66 0.029(6) 0.070(8) 0.017(6) -0.003(5) 0.014(5) 0.009(5) C67 0.006(5) 0.058(7) 0.065(8) 0.010(6) 0.010(5) -0.007(5) C68 0.032(7) 0.028(6) 0.088(11) -0.001(6) 0.014(7) 0.009(5) C69 0.060(9) 0.046(8) 0.078(11) 0.002(7) 0.022(8) -0.012(7) C70 0.057(9) 0.051(9) 0.085(12) 0.014(8) 0.007(9) -0.005(7) C71 0.046(8) 0.053(8) 0.054(9) -0.008(6) 0.013(7) -0.001(6) C72 0.068(10) 0.046(8) 0.083(12) -0.009(8) 0.008(9) -0.005(7) C73 0.067(11) 0.081(11) 0.065(11) -0.008(9) 0.005(9) 0.016(9) C74 0.028(6) 0.038(7) 0.066(9) -0.018(6) 0.013(6) 0.002(5) C75 0.063(9) 0.041(8) 0.088(12) -0.020(7) 0.018(9) -0.030(7) C76 0.031(6) 0.037(6) 0.058(8) 0.004(6) 0.018(6) -0.007(5) C77 0.035(7) 0.064(9) 0.063(10) 0.006(7) 0.009(7) 0.002(6) C78 0.067(9) 0.053(8) 0.058(9) -0.014(7) 0.041(8) -0.019(7) C79 0.066(9) 0.054(8) 0.033(8) -0.011(6) 0.017(7) 0.006(7) C80 0.081(11) 0.053(9) 0.072(11) -0.010(8) 0.029(10) -0.001(8) C81 0.114(13) 0.040(8) 0.053(9) -0.011(7) 0.053(9) -0.008(8) C82 0.038(7) 0.044(7) 0.051(8) -0.013(6) 0.008(6) 0.003(6) C83 0.052(9) 0.041(8) 0.084(12) -0.017(7) 0.014(8) -0.016(6) C84 0.135(18) 0.040(9) 0.143(19) 0.013(10) 0.043(15) -0.018(10) C85 0.084(12) 0.093(12) 0.064(11) 0.010(9) 0.041(10) 0.015(9) C86 0.142(18) 0.063(11) 0.113(16) -0.029(10) 0.057(14) -0.037(11) C87 0.079(11) 0.068(10) 0.080(12) -0.008(9) 0.017(10) 0.004(8) C88 0.074(12) 0.095(13) 0.105(15) -0.029(11) 0.019(11) -0.048(10) C89 0.042(8) 0.062(9) 0.083(12) 0.011(8) 0.029(8) 0.001(7) C90 0.035(7) 0.084(11) 0.059(10) 0.007(8) 0.001(7) -0.017(7) C91 0.076(11) 0.049(8) 0.075(12) -0.010(8) 0.036(9) -0.005(7) C92 0.046(8) 0.078(10) 0.071(11) -0.007(8) 0.037(8) -0.012(7) C93 0.070(10) 0.070(10) 0.069(11) 0.002(8) 0.036(9) -0.008(8) C94 0.073(10) 0.037(7) 0.059(10) -0.018(6) -0.005(8) 0.002(7) C95 0.071(11) 0.076(11) 0.102(15) 0.006(10) -0.001(10) -0.016(9) C96 0.078(12) 0.084(12) 0.115(16) 0.025(11) 0.055(12) 0.003(9) C97 0.079(12) 0.100(13) 0.083(13) 0.000(10) 0.046(10) -0.014(10) C98 0.059(10) 0.095(12) 0.065(11) 0.028(9) 0.012(8) -0.009(8) C99 0.046(9) 0.084(12) 0.081(13) -0.006(10) 0.019(9) 0.008(8) C100 0.050(10) 0.067(11) 0.145(18) -0.042(12) 0.014(11) -0.036(8) C101 0.035(8) 0.073(11) 0.144(18) 0.018(11) 0.030(10) -0.005(7) C102 0.042(8) 0.098(13) 0.065(11) -0.009(10) 0.021(8) -0.013(8) C103 0.091(13) 0.086(13) 0.103(16) 0.010(11) 0.061(12) 0.024(10) C104 0.068(13) 0.27(3) 0.101(18) 0.058(19) -0.032(12) -0.034(17) C105 0.082(12) 0.135(15) 0.184(17) -0.053(13) 0.019(12) -0.039(11) C106 0.106(17) 0.19(2) 0.20(3) 0.11(2) 0.072(19) 0.022(17) C107 0.084(15) 0.21(3) 0.13(2) -0.043(19) 0.065(15) -0.018(15) C108 0.120(17) 0.093(15) 0.17(2) -0.017(14) 0.083(17) 0.034(12) C109 0.106(15) 0.116(16) 0.020(8) -0.027(9) 0.002(9) -0.015(13) C110 0.104(16) 0.104(15) 0.047(11) 0.007(10) -0.006(10) 0.001(13) C111 0.108(15) 0.096(13) 0.029(9) 0.010(8) 0.025(9) 0.013(12) C112 0.104(16) 0.15(2) 0.088(16) 0.037(14) 0.050(13) 0.020(15) C113 0.16(2) 0.099(15) 0.034(10) -0.016(9) 0.035(12) 0.027(15) C114 0.111(17) 0.16(2) 0.073(14) -0.017(14) -0.011(12) -0.031(16) C115 0.26(4) 0.27(4) 0.11(2) 0.02(2) 0.03(2) 0.15(3) C116 0.20(3) 0.111(19) 0.13(2) 0.026(15) 0.07(2) -0.002(18) C117 0.16(2) 0.33(4) 0.14(2) -0.05(3) 0.13(2) -0.06(3) C118 0.195(18) 0.155(16) 0.126(16) -0.033(13) 0.043(14) 0.054(14) C119 0.145(14) 0.046(8) 0.048(9) -0.005(7) 0.020(9) -0.009(9) C120 0.169(16) 0.085(11) 0.090(13) 0.040(10) 0.054(12) 0.033(11) C121 0.123(13) 0.082(11) 0.055(10) 0.000(8) 0.002(9) -0.047(10) C122 0.163(15) 0.077(10) 0.063(10) 0.010(8) 0.075(11) 0.017(10) C123 0.096(10) 0.086(11) 0.105(13) 0.032(10) 0.053(10) -0.010(9) C124 0.23(2) 0.162(17) 0.147(18) 0.002(14) 0.066(15) -0.038(15) C126 0.165(18) 0.189(18) 0.125(16) 0.045(14) 0.021(14) -0.018(14) C127 0.24(2) 0.146(17) 0.162(18) -0.012(14) 0.100(16) 0.000(15) C128 0.143(14) 0.22(2) 0.22(2) 0.058(16) 0.094(15) -0.017(14) C129 0.097(12) 0.125(13) 0.079(12) -0.038(10) 0.037(10) 0.046(10) C130 0.117(17) 0.088(14) 0.119(18) 0.031(13) 0.078(15) 0.053(12) C131 0.086(14) 0.090(14) 0.121(18) -0.014(13) 0.048(13) -0.021(11) C132 0.082(12) 0.064(10) 0.080(13) -0.023(9) 0.020(10) 0.003(9) C133 0.133(17) 0.051(10) 0.16(2) -0.016(11) 0.113(17) -0.003(10) C134 0.180(19) 0.23(2) 0.191(19) -0.097(15) 0.084(15) 0.031(15) C135 0.28(3) 0.27(3) 0.26(2) 0.023(18) 0.127(19) 0.025(18) C137 0.17(3) 0.25(3) 0.11(2) 0.01(2) 0.064(19) 0.12(2) C138 0.169(17) 0.188(19) 0.25(2) -0.045(16) 0.131(16) 0.018(14) C145 0.062(18) 0.12(2) 0.08(2) -0.004(17) 0.009(15) 0.021(16) C146 0.063(16) 0.074(17) 0.041(16) -0.023(13) 0.028(13) -0.014(14) C147 0.19(5) 0.030(19) 0.11(4) 0.00(2) 0.13(4) -0.01(2) C148 0.11(2) 0.15(2) 0.095(18) 0.018(18) 0.077(17) 0.016(18) C149 0.13(2) 0.11(2) 0.059(16) 0.003(15) 0.053(16) 0.027(18) C150 0.089(19) 0.084(19) 0.10(2) -0.014(15) 0.063(16) 0.007(15) C151 0.054(16) 0.059(17) 0.043(16) 0.012(13) 0.028(13) 0.010(13) C152 0.060(17) 0.087(19) 0.052(17) 0.013(15) 0.029(14) -0.005(15) C153 0.097(12) 0.121(12) 0.140(14) 0.008(10) 0.039(11) -0.008(10) C154 0.179(18) 0.17(2) 0.138(17) 0.000(15) 0.121(15) -0.043(16) C155 0.10(2) 0.09(2) 0.051(18) 0.013(15) 0.061(16) 0.013(16) C156 0.092(11) 0.060(10) 0.054(9) 0.009(8) 0.051(9) -0.004(9) C157 0.13(3) 0.15(3) 0.12(3) -0.003(18) 0.05(2) 0.005(19) C158 0.079(17) 0.097(13) 0.10(2) -0.017(14) 0.024(15) -0.012(14) C159 0.11(2) 0.12(2) 0.08(2) -0.015(17) 0.050(17) -0.011(17) C160 0.12(2) 0.15(3) 0.11(2) -0.010(17) 0.09(2) 0.024(18) C14A 0.07(2) 0.09(2) 0.19(4) 0.04(2) 0.01(2) -0.036(18) C14B 0.16(3) 0.047(16) 0.08(2) 0.016(14) 0.03(2) 0.051(18) C14C 0.179(18) 0.17(2) 0.138(17) 0.000(15) 0.121(15) -0.043(16) C14D 0.097(12) 0.121(12) 0.140(14) 0.008(10) 0.039(11) -0.008(10) C14E 0.19(3) 0.20(3) 0.19(3) -0.015(18) 0.078(19) -0.019(19) C15A 0.049(13) 0.074(16) 0.062(16) 0.019(13) 0.036(13) 0.023(12) C15B 0.082(15) 0.050(13) 0.071(15) 0.000(12) 0.035(12) -0.014(12) C15C 0.092(11) 0.060(10) 0.054(9) 0.009(8) 0.051(9) -0.004(9) C15D 0.052(16) 0.11(2) 0.07(2) 0.023(18) 0.043(15) 0.041(17) C15E 0.13(2) 0.11(2) 0.059(16) 0.003(15) 0.053(16) 0.027(18) C15F 0.11(2) 0.15(2) 0.095(18) 0.018(18) 0.077(17) 0.016(18) C15G 0.12(3) 0.12(3) 0.07(2) -0.01(2) 0.07(2) 0.01(2) C15H 0.114(19) 0.119(19) 0.13(2) 0.009(16) 0.050(16) -0.029(15) C15I 0.079(17) 0.097(13) 0.10(2) -0.017(14) 0.024(15) -0.012(14) C15J 0.106(18) 0.124(19) 0.13(2) -0.003(15) 0.072(16) -0.004(15) C161 0.145(16) 0.125(15) 0.173(18) -0.050(13) 0.093(14) 0.043(12) C162 0.176(19) 0.21(2) 0.179(19) -0.053(16) 0.094(16) 0.043(15) C163 0.166(19) 0.20(2) 0.20(2) -0.051(16) 0.096(16) 0.049(15) C164 0.23(2) 0.20(2) 0.21(2) -0.085(16) 0.104(17) 0.052(16) C165 0.16(3) 0.17(3) 0.23(4) 0.00(3) 0.13(3) -0.02(2) C166 0.134(16) 0.171(18) 0.183(19) -0.032(15) 0.093(15) 0.033(14) C167 0.166(18) 0.22(2) 0.18(2) -0.029(16) 0.088(16) 0.011(15) C168 0.27(2) 0.24(2) 0.20(2) -0.057(17) 0.080(18) 0.014(18) C170 0.107(11) 0.127(12) 0.122(13) -0.045(10) 0.038(10) 0.045(10) C171 0.145(15) 0.180(17) 0.175(18) -0.049(13) 0.101(14) 0.072(13) C175 0.22(2) 0.20(2) 0.19(2) -0.023(16) 0.094(17) 0.054(16) C176 0.18(2) 0.19(2) 0.20(2) -0.036(16) 0.056(16) 0.042(16) C177 0.146(17) 0.22(2) 0.121(16) -0.015(15) 0.090(15) -0.030(15) C178 0.137(16) 0.213(19) 0.082(13) -0.012(13) 0.070(12) -0.001(14) C180 0.23(4) 0.34(5) 0.13(3) 0.07(3) 0.14(3) 0.05(4) C181 0.182(18) 0.21(2) 0.145(17) -0.001(15) 0.124(15) -0.035(15) C182 0.131(15) 0.180(17) 0.122(16) -0.009(14) 0.065(13) -0.085(14) C183 0.160(16) 0.207(19) 0.105(14) 0.004(13) 0.098(13) -0.010(14) C185 0.162(18) 0.21(2) 0.21(2) -0.015(16) 0.088(16) 0.037(15) O20 0.146(12) 0.079(8) 0.29(2) -0.037(10) 0.181(15) -0.035(8) C187 0.089(17) 0.15(2) 0.31(4) -0.05(2) 0.07(2) 0.016(15) O19 0.145(15) 0.123(13) 0.22(2) 0.005(13) 0.034(15) -0.005(11) O21 0.106(11) 0.120(12) 0.27(2) 0.002(13) 0.100(14) 0.011(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 N16 2.100(10) . ? Ir1 C79 2.133(12) . ? Ir1 C80 2.154(15) . ? Ir1 C83 2.158(12) . ? Ir1 N1 2.165(11) . ? Ir1 N2 2.168(10) . ? Ir1 C81 2.201(13) . ? Ir1 C82 2.203(13) . ? Ir2 N22 2.074(10) . ? Ir2 C91 2.129(15) . ? Ir2 C89 2.143(14) . ? Ir2 C93 2.154(15) . ? Ir2 C90 2.161(13) . ? Ir2 N4 2.165(10) . ? Ir2 C92 2.186(13) . ? Ir2 N3 2.197(10) . ? Ir3 C103 2.123(16) . ? Ir3 N17 2.130(9) . ? Ir3 C99 2.143(15) . ? Ir3 C101 2.148(17) . ? Ir3 N5 2.156(10) . ? Ir3 C100 2.158(14) . ? Ir3 N6 2.164(11) . ? Ir3 C102 2.189(16) . ? Ir4 N23 2.102(11) . ? Ir4 N8 2.120(12) . ? Ir4 C113 2.133(15) . ? Ir4 C110 2.141(18) . ? Ir4 C111 2.157(16) . ? Ir4 N7 2.177(10) . ? Ir4 C109 2.187(14) . ? Ir4 C112 2.21(2) . ? Ir5 N9 2.109(12) . ? Ir5 N18 2.141(11) . ? Ir5 C122 2.158(7) . ? Ir5 N10 2.162(12) . ? Ir5 C123 2.166(7) . ? Ir5 C121 2.170(7) . ? Ir5 C119 2.183(6) . ? Ir5 C120 2.185(6) . ? Ir6 C133 2.062(6) . ? Ir6 N24 2.090(10) . ? Ir6 C129 2.125(7) . ? Ir6 C132 2.127(6) . ? Ir6 N11 2.171(10) . ? Ir6 N12 2.177(12) . ? Ir6 C130 2.225(7) . ? Ir6 C131 2.226(7) . ? N1 C7 1.344(15) . ? N1 C1 1.400(16) . ? N2 C8 1.309(16) . ? N2 C9 1.372(16) . ? N3 C8 1.361(15) . ? N3 C14 1.401(16) . ? N4 C7 1.354(16) . ? N4 C6 1.390(15) . ? N5 C21 1.316(16) . ? N5 C15 1.405(15) . ? N6 C22 1.339(16) . ? N6 C23 1.379(16) . ? N7 C22 1.344(15) . ? N7 C28 1.414(15) . ? N8 C21 1.330(15) . ? N8 C20 1.437(15) . ? N9 C35 1.369(18) . ? N9 C29 1.458(18) . ? N10 C36 1.334(18) . ? N10 C37 1.425(16) . ? N11 C36 1.322(17) . ? N11 C42 1.421(15) . ? N12 C35 1.312(16) . ? N12 C34 1.419(17) . ? N13 C43 1.302(15) . ? N13 C45 1.351(14) . ? N14 C44 1.341(14) . ? N14 C43 1.357(15) . ? N15 C45 1.321(15) . ? N15 C44 1.347(14) . ? N16 C46 1.357(16) . ? N16 C50 1.378(15) . ? N17 C51 1.345(14) . ? N17 C55 1.357(15) . ? N18 C60 1.301(18) . ? N18 C56 1.336(17) . ? N19 C63 1.281(15) . ? N19 C61 1.365(16) . ? N20 C62 1.316(16) . ? N20 C61 1.351(17) . ? N21 C62 1.347(16) . ? N21 C63 1.351(16) . ? N22 C68 1.319(15) . ? N22 C64 1.347(16) . ? N23 C73 1.306(18) . ? N23 C69 1.356(16) . ? N24 C74 1.311(14) . ? N24 C78 1.360(16) . ? O1 S1 1.462(13) . ? O2 S1 1.449(14) . ? O3 S1 1.392(13) . ? O4 S2 1.584(16) . ? O5 S2 1.340(15) . ? O6 S2 1.420(18) . ? O7 S3 1.381(16) . ? O8 S3 1.393(13) . ? O9 S3 1.440(18) . ? S1 C139 1.84(3) . ? S2 C140 1.723(18) . ? S3 C141 1.814(17) . ? F1 C139 1.31(3) . ? F2 C139 1.45(3) . ? F3 C139 1.34(3) . ? F4 C140 1.308(18) . ? F5 C140 1.281(17) . ? F6 C140 1.323(18) . ? F7 C141 1.361(18) . ? F8 C141 1.381(19) . ? F9 C141 1.342(17) . ? C1 C6 1.345(17) . ? C1 C2 1.407(16) . ? C2 C3 1.43(2) . ? C3 C4 1.37(2) . ? C4 C5 1.328(19) . ? C5 C6 1.416(18) . ? C7 C8 1.410(18) . ? C9 C14 1.391(19) . ? C9 C10 1.407(19) . ? C10 C11 1.40(2) . ? C11 C12 1.41(2) . ? C12 C13 1.42(2) . ? C13 C14 1.404(18) . ? C15 C16 1.399(19) . ? C15 C20 1.41(2) . ? C16 C17 1.42(2) . ? C17 C18 1.45(2) . ? C18 C19 1.288(19) . ? C19 C20 1.428(18) . ? C21 C22 1.379(17) . ? C23 C24 1.444(18) . ? C23 C28 1.454(19) . ? C24 C25 1.311(19) . ? C25 C26 1.40(2) . ? C26 C27 1.32(2) . ? C27 C28 1.331(17) . ? C29 C30 1.33(2) . ? C29 C34 1.47(2) . ? C30 C31 1.37(2) . ? C31 C32 1.40(2) . ? C32 C33 1.35(2) . ? C33 C34 1.35(2) . ? C35 C36 1.36(2) . ? C37 C42 1.374(17) . ? C37 C38 1.390(17) . ? C38 C39 1.35(2) . ? C39 C40 1.39(2) . ? C40 C41 1.39(2) . ? C41 C42 1.372(18) . ? C43 C48 1.489(16) . ? C44 C53 1.497(15) . ? C45 C58 1.529(15) . ? C46 C47 1.372(16) . ? C47 C48 1.367(16) . ? C48 C49 1.443(17) . ? C49 C50 1.341(16) . ? C51 C52 1.306(17) . ? C52 C53 1.428(16) . ? C53 C54 1.368(15) . ? C54 C55 1.387(17) . ? C56 C57 1.388(17) . ? C57 C58 1.399(17) . ? C58 C59 1.391(18) . ? C59 C60 1.382(19) . ? C61 C66 1.495(18) . ? C62 C71 1.494(17) . ? C63 C76 1.511(16) . ? C64 C65 1.361(18) . ? C65 C66 1.365(18) . ? C66 C67 1.386(14) . ? C67 C68 1.296(16) . ? C69 C70 1.323(19) . ? C70 C71 1.394(18) . ? C71 C72 1.357(18) . ? C72 C73 1.39(2) . ? C74 C75 1.386(18) . ? C75 C76 1.339(17) . ? C76 C77 1.483(17) . ? C77 C78 1.362(18) . ? C79 C80 1.34(2) . ? C79 C83 1.357(18) . ? C79 C84 1.63(2) . ? C80 C81 1.45(2) . ? C80 C85 1.52(2) . ? C81 C86 1.49(2) . ? C81 C82 1.490(19) . ? C82 C87 1.449(18) . ? C82 C83 1.489(19) . ? C83 C88 1.55(2) . ? C89 C90 1.414(19) . ? C89 C93 1.44(2) . ? C89 C94 1.504(18) . ? C90 C91 1.46(2) . ? C90 C95 1.55(2) . ? C91 C92 1.39(2) . ? C91 C96 1.51(2) . ? C92 C93 1.41(2) . ? C92 C97 1.49(2) . ? C93 C98 1.55(2) . ? C99 C100 1.38(2) . ? C99 C103 1.41(2) . ? C99 C104 1.47(2) . ? C100 C105 1.52(2) . ? C100 C101 1.55(3) . ? C101 C102 1.35(2) . ? C101 C106 1.52(2) . ? C102 C107 1.43(2) . ? C102 C103 1.44(2) . ? C103 C108 1.58(2) . ? C109 C110 1.42(3) . ? C109 C113 1.45(3) . ? C109 C114 1.52(3) . ? C110 C111 1.35(2) . ? C110 C115 1.55(3) . ? C111 C112 1.51(3) . ? C111 C116 1.52(3) . ? C112 C117 1.39(3) . ? C112 C113 1.47(3) . ? C113 C118 1.54(3) . ? C119 C120 1.4278(16) . ? C119 C123 1.4280(16) . ? C119 C124 1.5173(18) . ? C120 C121 1.4275(17) . ? C120 C125 1.5178(17) . ? C121 C122 1.4281(17) . ? C121 C126 1.5178(18) . ? C122 C123 1.4277(17) . ? C122 C127 1.5173(18) . ? C123 C128 1.5179(18) . ? C129 C133 1.3600(16) . ? C129 C130 1.3602(16) . ? C129 C134 1.4452(17) . ? C130 C131 1.3597(16) . ? C130 C135 1.4452(17) . ? C131 C132 1.3600(16) . ? C131 C136 1.4452(17) . ? C132 C133 1.3600(16) . ? C132 C137 1.4457(17) . ? C133 C138 1.4451(17) . ? C145 C150 1.410(8) . ? C145 C146 1.410(8) . ? C146 C147 1.409(8) . ? C147 C157 1.39(2) . ? C147 C148 1.410(8) . ? C148 C149 1.409(8) . ? C148 C151 1.489(9) . ? C149 C150 1.409(8) . ? C149 C159 1.427(19) . ? C151 C156 1.410(8) . ? C151 C152 1.411(8) . ? C152 C153 1.410(8) . ? C152 C158 1.41(2) . ? C153 C154 1.410(8) . ? C154 C155 1.410(8) . ? C155 C156 1.411(8) . ? C156 C160 1.40(2) . ? C157 C158 1.40(2) . ? C159 C160 1.41(2) . ? C14A C15A 1.416(5) . ? C14A C14B 1.417(5) . ? C14B C14C 1.416(5) . ? C14C C14D 1.417(5) . ? C14C C15J 1.68(3) . ? C14D C14E 1.416(5) . ? C14D C15B 1.515(6) . ? C14E C15A 1.416(5) . ? C14E C15H 1.46(4) . ? C15B C15C 1.352(5) . ? C15B C15G 1.353(5) . ? C15C C15D 1.352(5) . ? C15C C16A 1.48(4) . ? C15D C15E 1.353(5) . ? C15E C15F 1.352(5) . ? C15F C15G 1.352(5) . ? C15G C15I 1.42(4) . ? C15H C15I 1.52(5) . ? C15J C16A 1.32(4) . ? C161 C166 1.415(10) . ? C161 C162 1.416(10) . ? C161 C170 1.53(3) . ? C162 C173 1.33(2) . ? C162 C163 1.416(10) . ? C163 C176 1.357(16) . ? C163 C164 1.415(10) . ? C164 C165 1.415(10) . ? C165 C166 1.416(10) . ? C166 C167 1.51(3) . ? C167 C168 1.409(18) . ? C168 C169 1.40(2) . ? C169 C170 1.37(2) . ? C170 C171 1.61(3) . ? C171 C172 1.386(17) . ? C172 C173 1.452(17) . ? C173 C174 1.418(18) . ? C174 C175 1.350(18) . ? C175 C176 1.350(18) . ? C177 C178 1.334(10) . ? C177 C182 1.335(10) . ? C177 C177 1.370(17) 3_677 ? C178 C179 1.335(10) . ? C178 C184 1.361(16) 3_677 ? C179 C180 1.335(10) . ? C180 C181 1.334(10) . ? C181 C182 1.335(10) . ? C182 C183 1.35(3) . ? C183 C184 1.400(18) . ? C184 C178 1.36(4) 3_677 ? C185 O19 1.46(3) . ? C187 O21 1.50(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 N16 Ir1 C79 141.0(5) . . ? N16 Ir1 C80 106.4(5) . . ? C79 Ir1 C80 36.4(5) . . ? N16 Ir1 C83 161.8(5) . . ? C79 Ir1 C83 36.9(5) . . ? C80 Ir1 C83 64.6(6) . . ? N16 Ir1 N1 86.9(4) . . ? C79 Ir1 N1 96.9(4) . . ? C80 Ir1 N1 111.4(5) . . ? C83 Ir1 N1 110.9(5) . . ? N16 Ir1 N2 88.4(4) . . ? C79 Ir1 N2 130.5(5) . . ? C80 Ir1 N2 161.6(5) . . ? C83 Ir1 N2 98.1(5) . . ? N1 Ir1 N2 79.6(4) . . ? N16 Ir1 C81 96.7(5) . . ? C79 Ir1 C81 62.1(5) . . ? C80 Ir1 C81 39.0(6) . . ? C83 Ir1 C81 66.1(6) . . ? N1 Ir1 C81 149.9(5) . . ? N2 Ir1 C81 130.3(5) . . ? N16 Ir1 C82 122.6(5) . . ? C79 Ir1 C82 62.4(5) . . ? C80 Ir1 C82 65.3(5) . . ? C83 Ir1 C82 39.9(5) . . ? N1 Ir1 C82 150.5(4) . . ? N2 Ir1 C82 97.7(4) . . ? C81 Ir1 C82 39.6(5) . . ? N22 Ir2 C91 116.5(5) . . ? N22 Ir2 C89 144.0(6) . . ? C91 Ir2 C89 64.5(5) . . ? N22 Ir2 C93 106.3(5) . . ? C91 Ir2 C93 63.8(6) . . ? C89 Ir2 C93 39.2(6) . . ? N22 Ir2 C90 156.3(5) . . ? C91 Ir2 C90 39.9(5) . . ? C89 Ir2 C90 38.4(5) . . ? C93 Ir2 C90 65.4(6) . . ? N22 Ir2 N4 86.8(4) . . ? C91 Ir2 N4 156.7(5) . . ? C89 Ir2 N4 96.1(4) . . ? C93 Ir2 N4 110.1(5) . . ? C90 Ir2 N4 116.8(5) . . ? N22 Ir2 C92 94.4(5) . . ? C91 Ir2 C92 37.5(5) . . ? C89 Ir2 C92 64.3(6) . . ? C93 Ir2 C92 37.9(5) . . ? C90 Ir2 C92 65.1(6) . . ? N4 Ir2 C92 146.7(5) . . ? N22 Ir2 N3 84.7(4) . . ? C91 Ir2 N3 102.3(5) . . ? C89 Ir2 N3 131.2(5) . . ? C93 Ir2 N3 164.9(5) . . ? C90 Ir2 N3 100.4(5) . . ? N4 Ir2 N3 80.3(4) . . ? C92 Ir2 N3 133.0(5) . . ? C103 Ir3 N17 126.7(6) . . ? C103 Ir3 C99 38.5(7) . . ? N17 Ir3 C99 163.7(5) . . ? C103 Ir3 C101 63.0(6) . . ? N17 Ir3 C101 101.2(5) . . ? C99 Ir3 C101 67.3(7) . . ? C103 Ir3 N5 145.1(7) . . ? N17 Ir3 N5 88.0(4) . . ? C99 Ir3 N5 107.4(5) . . ? C101 Ir3 N5 118.6(6) . . ? C103 Ir3 C100 62.1(7) . . ? N17 Ir3 C100 138.6(7) . . ? C99 Ir3 C100 37.6(6) . . ? C101 Ir3 C100 42.1(7) . . ? N5 Ir3 C100 95.2(6) . . ? C103 Ir3 N6 98.6(6) . . ? N17 Ir3 N6 87.2(4) . . ? C99 Ir3 N6 100.7(5) . . ? C101 Ir3 N6 161.4(5) . . ? N5 Ir3 N6 77.8(4) . . ? C100 Ir3 N6 133.9(7) . . ? C103 Ir3 C102 39.0(6) . . ? N17 Ir3 C102 97.2(5) . . ? C99 Ir3 C102 66.7(6) . . ? C101 Ir3 C102 36.4(6) . . ? N5 Ir3 C102 155.0(5) . . ? C100 Ir3 C102 64.9(7) . . ? N6 Ir3 C102 126.7(5) . . ? N23 Ir4 N8 86.9(4) . . ? N23 Ir4 C113 103.5(8) . . ? N8 Ir4 C113 112.4(7) . . ? N23 Ir4 C110 156.4(7) . . ? N8 Ir4 C110 116.6(7) . . ? C113 Ir4 C110 67.1(8) . . ? N23 Ir4 C111 120.0(7) . . ? N8 Ir4 C111 153.0(6) . . ? C113 Ir4 C111 65.2(7) . . ? C110 Ir4 C111 36.5(7) . . ? N23 Ir4 N7 86.8(4) . . ? N8 Ir4 N7 78.8(4) . . ? C113 Ir4 N7 164.9(6) . . ? C110 Ir4 N7 99.1(7) . . ? C111 Ir4 N7 100.2(5) . . ? N23 Ir4 C109 141.7(7) . . ? N8 Ir4 C109 99.3(6) . . ? C113 Ir4 C109 39.2(7) . . ? C110 Ir4 C109 38.2(7) . . ? C111 Ir4 C109 60.9(7) . . ? N7 Ir4 C109 131.5(7) . . ? N23 Ir4 C112 91.9(7) . . ? N8 Ir4 C112 150.5(7) . . ? C113 Ir4 C112 39.5(8) . . ? C110 Ir4 C112 66.8(8) . . ? C111 Ir4 C112 40.4(7) . . ? N7 Ir4 C112 130.6(7) . . ? C109 Ir4 C112 64.5(8) . . ? N9 Ir5 N18 84.3(4) . . ? N9 Ir5 C122 126.9(4) . . ? N18 Ir5 C122 98.0(4) . . ? N9 Ir5 N10 78.8(5) . . ? N18 Ir5 N10 88.1(5) . . ? C122 Ir5 N10 153.9(4) . . ? N9 Ir5 C123 163.6(4) . . ? N18 Ir5 C123 103.7(4) . . ? C122 Ir5 C123 38.57(9) . . ? N10 Ir5 C123 115.3(4) . . ? N9 Ir5 C121 99.3(4) . . ? N18 Ir5 C121 125.9(4) . . ? C122 Ir5 C121 38.54(10) . . ? N10 Ir5 C121 145.9(4) . . ? C123 Ir5 C121 64.39(14) . . ? N9 Ir5 C119 137.6(4) . . ? N18 Ir5 C119 137.6(4) . . ? C122 Ir5 C119 64.33(14) . . ? N10 Ir5 C119 94.2(4) . . ? C123 Ir5 C119 38.34(10) . . ? C121 Ir5 C119 64.11(15) . . ? N9 Ir5 C120 104.4(4) . . ? N18 Ir5 C120 162.2(4) . . ? C122 Ir5 C120 64.28(15) . . ? N10 Ir5 C120 108.6(4) . . ? C123 Ir5 C120 64.14(15) . . ? C121 Ir5 C120 38.27(11) . . ? C119 Ir5 C120 38.16(10) . . ? C133 Ir6 N24 147.8(4) . . ? C133 Ir6 C129 37.87(10) . . ? N24 Ir6 C129 110.0(4) . . ? C133 Ir6 C132 37.85(11) . . ? N24 Ir6 C132 145.6(4) . . ? C129 Ir6 C132 62.33(14) . . ? C133 Ir6 N11 102.5(3) . . ? N24 Ir6 N11 88.0(4) . . ? C129 Ir6 N11 112.3(4) . . ? C132 Ir6 N11 126.3(4) . . ? C133 Ir6 N12 124.0(4) . . ? N24 Ir6 N12 87.8(4) . . ? C129 Ir6 N12 159.2(4) . . ? C132 Ir6 N12 96.9(4) . . ? N11 Ir6 N12 78.0(4) . . ? C133 Ir6 C130 61.63(13) . . ? N24 Ir6 C130 92.8(4) . . ? C129 Ir6 C130 36.35(9) . . ? C132 Ir6 C130 60.68(14) . . ? N11 Ir6 C130 145.9(4) . . ? N12 Ir6 C130 136.1(4) . . ? C133 Ir6 C131 61.61(14) . . ? N24 Ir6 C131 109.5(4) . . ? C129 Ir6 C131 60.71(13) . . ? C132 Ir6 C131 36.32(11) . . ? N11 Ir6 C131 162.4(4) . . ? N12 Ir6 C131 103.9(4) . . ? C130 Ir6 C131 35.57(9) . . ? C7 N1 C1 100.9(10) . . ? C7 N1 Ir1 107.8(8) . . ? C1 N1 Ir1 149.0(8) . . ? C8 N2 C9 101.7(11) . . ? C8 N2 Ir1 108.4(8) . . ? C9 N2 Ir1 149.9(10) . . ? C8 N3 C14 101.0(10) . . ? C8 N3 Ir2 108.5(8) . . ? C14 N3 Ir2 150.5(8) . . ? C7 N4 C6 102.0(10) . . ? C7 N4 Ir2 108.0(8) . . ? C6 N4 Ir2 149.6(9) . . ? C21 N5 C15 104.8(11) . . ? C21 N5 Ir3 110.8(8) . . ? C15 N5 Ir3 144.3(10) . . ? C22 N6 C23 103.1(11) . . ? C22 N6 Ir3 108.6(8) . . ? C23 N6 Ir3 148.0(9) . . ? C22 N7 C28 104.3(11) . . ? C22 N7 Ir4 109.0(8) . . ? C28 N7 Ir4 145.7(9) . . ? C21 N8 C20 101.0(12) . . ? C21 N8 Ir4 110.6(8) . . ? C20 N8 Ir4 147.5(10) . . ? C35 N9 C29 102.2(11) . . ? C35 N9 Ir5 111.4(9) . . ? C29 N9 Ir5 146.4(10) . . ? C36 N10 C37 101.3(12) . . ? C36 N10 Ir5 108.2(11) . . ? C37 N10 Ir5 150.4(10) . . ? C36 N11 C42 102.8(11) . . ? C36 N11 Ir6 110.5(9) . . ? C42 N11 Ir6 146.7(9) . . ? C35 N12 C34 106.9(12) . . ? C35 N12 Ir6 107.5(10) . . ? C34 N12 Ir6 145.6(10) . . ? C43 N13 C45 114.1(11) . . ? C44 N14 C43 114.7(9) . . ? C45 N15 C44 112.9(10) . . ? C46 N16 C50 114.5(10) . . ? C46 N16 Ir1 122.6(8) . . ? C50 N16 Ir1 122.8(8) . . ? C51 N17 C55 117.0(10) . . ? C51 N17 Ir3 121.3(8) . . ? C55 N17 Ir3 121.4(8) . . ? C60 N18 C56 118.5(12) . . ? C60 N18 Ir5 122.3(9) . . ? C56 N18 Ir5 119.2(10) . . ? C63 N19 C61 114.9(12) . . ? C62 N20 C61 116.4(11) . . ? C62 N21 C63 113.6(11) . . ? C68 N22 C64 114.8(11) . . ? C68 N22 Ir2 123.3(9) . . ? C64 N22 Ir2 121.6(9) . . ? C73 N23 C69 115.6(12) . . ? C73 N23 Ir4 120.5(10) . . ? C69 N23 Ir4 123.6(9) . . ? C74 N24 C78 117.1(11) . . ? C74 N24 Ir6 122.0(8) . . ? C78 N24 Ir6 119.6(9) . . ? O3 S1 O2 115.8(11) . . ? O3 S1 O1 119.7(10) . . ? O2 S1 O1 114.3(9) . . ? O3 S1 C139 98.0(13) . . ? O2 S1 C139 101.8(12) . . ? O1 S1 C139 102.7(12) . . ? O5 S2 O6 122.9(14) . . ? O5 S2 O4 111.9(12) . . ? O6 S2 O4 109.2(12) . . ? O5 S2 C140 106.4(13) . . ? O6 S2 C140 103.1(13) . . ? O4 S2 C140 100.5(11) . . ? O7 S3 O8 110.7(16) . . ? O7 S3 O9 127(2) . . ? O8 S3 O9 109.8(17) . . ? O7 S3 C141 96.6(15) . . ? O8 S3 C141 114.5(13) . . ? O9 S3 C141 96.8(19) . . ? C6 C1 N1 110.8(10) . . ? C6 C1 C2 122.0(13) . . ? N1 C1 C2 127.2(13) . . ? C1 C2 C3 114.8(14) . . ? C4 C3 C2 121.5(14) . . ? C5 C4 C3 122.0(15) . . ? C4 C5 C6 118.0(15) . . ? C1 C6 N4 109.3(11) . . ? C1 C6 C5 121.4(12) . . ? N4 C6 C5 129.3(12) . . ? N1 C7 N4 117.0(11) . . ? N1 C7 C8 120.0(12) . . ? N4 C7 C8 122.8(12) . . ? N2 C8 N3 118.8(12) . . ? N2 C8 C7 121.8(12) . . ? N3 C8 C7 119.4(12) . . ? N2 C9 C14 110.7(13) . . ? N2 C9 C10 131.3(15) . . ? C14 C9 C10 117.9(14) . . ? C11 C10 C9 121.0(16) . . ? C10 C11 C12 118.6(16) . . ? C11 C12 C13 122.5(15) . . ? C14 C13 C12 115.1(16) . . ? C9 C14 N3 107.5(11) . . ? C9 C14 C13 124.7(15) . . ? N3 C14 C13 127.7(14) . . ? C16 C15 N5 132.3(15) . . ? C16 C15 C20 120.9(13) . . ? N5 C15 C20 106.1(11) . . ? C15 C16 C17 117.7(17) . . ? C16 C17 C18 120.4(15) . . ? C19 C18 C17 119.7(14) . . ? C18 C19 C20 122.9(15) . . ? C15 C20 C19 118.2(12) . . ? C15 C20 N8 109.3(11) . . ? C19 C20 N8 132.4(15) . . ? N5 C21 N8 118.8(11) . . ? N5 C21 C22 119.1(12) . . ? N8 C21 C22 121.3(12) . . ? N6 C22 N7 117.5(11) . . ? N6 C22 C21 121.2(12) . . ? N7 C22 C21 119.1(12) . . ? N6 C23 C24 131.7(15) . . ? N6 C23 C28 109.9(10) . . ? C24 C23 C28 117.8(13) . . ? C25 C24 C23 116.6(16) . . ? C24 C25 C26 121.9(15) . . ? C27 C26 C25 124.5(15) . . ? C26 C27 C28 116.7(15) . . ? C27 C28 N7 132.8(13) . . ? C27 C28 C23 122.2(12) . . ? N7 C28 C23 105.0(10) . . ? C30 C29 N9 134.7(15) . . ? C30 C29 C34 117.6(14) . . ? N9 C29 C34 107.7(12) . . ? C29 C30 C31 121.9(17) . . ? C30 C31 C32 118.4(15) . . ? C33 C32 C31 123.4(15) . . ? C32 C33 C34 117.5(16) . . ? C33 C34 N12 133.4(16) . . ? C33 C34 C29 120.9(14) . . ? N12 C34 C29 105.4(12) . . ? N12 C35 C36 124.8(14) . . ? N12 C35 N9 117.7(13) . . ? C36 C35 N9 117.4(12) . . ? N11 C36 N10 118.7(14) . . ? N11 C36 C35 118.2(13) . . ? N10 C36 C35 122.3(14) . . ? C42 C37 C38 122.5(13) . . ? C42 C37 N10 109.5(11) . . ? C38 C37 N10 128.0(14) . . ? C39 C38 C37 115.8(16) . . ? C38 C39 C40 123.1(16) . . ? C41 C40 C39 120.1(15) . . ? C42 C41 C40 117.0(14) . . ? C41 C42 C37 121.2(12) . . ? C41 C42 N11 130.9(12) . . ? C37 C42 N11 107.8(11) . . ? N13 C43 N14 125.3(10) . . ? N13 C43 C48 118.4(11) . . ? N14 C43 C48 116.3(11) . . ? N14 C44 N15 125.3(10) . . ? N14 C44 C53 118.6(10) . . ? N15 C44 C53 116.1(10) . . ? N15 C45 N13 127.5(11) . . ? N15 C45 C58 114.1(10) . . ? N13 C45 C58 118.0(11) . . ? N16 C46 C47 123.9(12) . . ? C48 C47 C46 119.6(12) . . ? C47 C48 C49 119.2(11) . . ? C47 C48 C43 121.8(11) . . ? C49 C48 C43 118.7(11) . . ? C50 C49 C48 116.0(12) . . ? C49 C50 N16 126.7(12) . . ? C52 C51 N17 123.5(11) . . ? C51 C52 C53 119.9(11) . . ? C54 C53 C52 118.5(11) . . ? C54 C53 C44 120.3(10) . . ? C52 C53 C44 121.2(11) . . ? C53 C54 C55 117.2(11) . . ? N17 C55 C54 123.6(11) . . ? N18 C56 C57 123.7(13) . . ? C56 C57 C58 116.5(12) . . ? C59 C58 C57 119.5(11) . . ? C59 C58 C45 120.2(11) . . ? C57 C58 C45 120.2(10) . . ? C60 C59 C58 117.8(14) . . ? N18 C60 C59 123.7(14) . . ? N20 C61 N19 122.9(13) . . ? N20 C61 C66 116.7(11) . . ? N19 C61 C66 120.0(13) . . ? N20 C62 N21 124.6(12) . . ? N20 C62 C71 116.6(12) . . ? N21 C62 C71 118.8(12) . . ? N19 C63 N21 127.5(12) . . ? N19 C63 C76 115.5(12) . . ? N21 C63 C76 117.0(11) . . ? N22 C64 C65 123.4(13) . . ? C64 C65 C66 119.1(14) . . ? C65 C66 C67 116.5(13) . . ? C65 C66 C61 123.3(12) . . ? C67 C66 C61 120.2(11) . . ? C68 C67 C66 120.1(12) . . ? C67 C68 N22 125.9(12) . . ? C70 C69 N23 125.8(13) . . ? C69 C70 C71 116.5(13) . . ? C72 C71 C70 120.7(13) . . ? C72 C71 C62 119.7(12) . . ? C70 C71 C62 119.3(12) . . ? C71 C72 C73 116.9(14) . . ? N23 C73 C72 124.2(15) . . ? N24 C74 C75 125.5(12) . . ? C76 C75 C74 117.0(11) . . ? C75 C76 C77 121.1(11) . . ? C75 C76 C63 119.6(11) . . ? C77 C76 C63 119.1(11) . . ? C78 C77 C76 114.3(12) . . ? N24 C78 C77 124.7(12) . . ? C80 C79 C83 117.2(14) . . ? C80 C79 C84 123.2(14) . . ? C83 C79 C84 119.2(14) . . ? C80 C79 Ir1 72.6(8) . . ? C83 C79 Ir1 72.6(7) . . ? C84 C79 Ir1 119.5(10) . . ? C79 C80 C81 106.3(14) . . ? C79 C80 C85 130.3(15) . . ? C81 C80 C85 123.1(14) . . ? C79 C80 Ir1 70.9(9) . . ? C81 C80 Ir1 72.3(8) . . ? C85 C80 Ir1 126.6(11) . . ? C80 C81 C86 128.5(16) . . ? C80 C81 C82 106.1(12) . . ? C86 C81 C82 125.3(15) . . ? C80 C81 Ir1 68.7(8) . . ? C86 C81 Ir1 122.7(10) . . ? C82 C81 Ir1 70.3(7) . . ? C87 C82 C83 126.7(13) . . ? C87 C82 C81 127.3(13) . . ? C83 C82 C81 106.0(11) . . ? C87 C82 Ir1 126.6(9) . . ? C83 C82 Ir1 68.4(7) . . ? C81 C82 Ir1 70.2(7) . . ? C79 C83 C82 104.2(12) . . ? C79 C83 C88 134.6(15) . . ? C82 C83 C88 120.9(13) . . ? C79 C83 Ir1 70.6(8) . . ? C82 C83 Ir1 71.7(7) . . ? C88 C83 Ir1 126.7(11) . . ? C90 C89 C93 109.3(13) . . ? C90 C89 C94 122.9(14) . . ? C93 C89 C94 127.7(14) . . ? C90 C89 Ir2 71.5(8) . . ? C93 C89 Ir2 70.8(8) . . ? C94 C89 Ir2 127.0(10) . . ? C89 C90 C91 104.8(13) . . ? C89 C90 C95 126.6(15) . . ? C91 C90 C95 128.6(14) . . ? C89 C90 Ir2 70.1(7) . . ? C91 C90 Ir2 68.9(8) . . ? C95 C90 Ir2 125.3(11) . . ? C92 C91 C90 110.2(14) . . ? C92 C91 C96 127.3(14) . . ? C90 C91 C96 122.0(15) . . ? C92 C91 Ir2 73.4(8) . . ? C90 C91 Ir2 71.3(8) . . ? C96 C91 Ir2 128.9(10) . . ? C91 C92 C93 108.0(14) . . ? C91 C92 C97 125.1(15) . . ? C93 C92 C97 126.7(15) . . ? C91 C92 Ir2 69.0(9) . . ? C93 C92 Ir2 69.8(8) . . ? C97 C92 Ir2 122.6(10) . . ? C92 C93 C89 107.7(14) . . ? C92 C93 C98 125.9(15) . . ? C89 C93 C98 126.3(14) . . ? C92 C93 Ir2 72.3(9) . . ? C89 C93 Ir2 70.0(8) . . ? C98 C93 Ir2 126.6(10) . . ? C100 C99 C103 104.7(16) . . ? C100 C99 C104 127.3(19) . . ? C103 C99 C104 127.1(19) . . ? C100 C99 Ir3 71.8(9) . . ? C103 C99 Ir3 70.0(10) . . ? C104 C99 Ir3 130.7(14) . . ? C99 C100 C105 130(2) . . ? C99 C100 C101 108.4(14) . . ? C105 C100 C101 121.7(19) . . ? C99 C100 Ir3 70.6(9) . . ? C105 C100 Ir3 125.2(14) . . ? C101 C100 Ir3 68.6(7) . . ? C102 C101 C106 128(2) . . ? C102 C101 C100 107.0(15) . . ? C106 C101 C100 124.7(19) . . ? C102 C101 Ir3 73.5(9) . . ? C106 C101 Ir3 125.1(12) . . ? C100 C101 Ir3 69.3(10) . . ? C101 C102 C107 126(2) . . ? C101 C102 C103 106.1(16) . . ? C107 C102 C103 127(2) . . ? C101 C102 Ir3 70.2(10) . . ? C107 C102 Ir3 127.1(11) . . ? C103 C102 Ir3 68.1(9) . . ? C99 C103 C102 113.6(16) . . ? C99 C103 C108 125.5(19) . . ? C102 C103 C108 120.8(19) . . ? C99 C103 Ir3 71.5(9) . . ? C102 C103 Ir3 73.0(9) . . ? C108 C103 Ir3 126.8(12) . . ? C110 C109 C113 110.9(18) . . ? C110 C109 C114 129(2) . . ? C113 C109 C114 118(2) . . ? C110 C109 Ir4 69.1(9) . . ? C113 C109 Ir4 68.4(9) . . ? C114 C109 Ir4 118.1(12) . . ? C111 C110 C109 106(2) . . ? C111 C110 C115 128(2) . . ? C109 C110 C115 125(2) . . ? C111 C110 Ir4 72.4(11) . . ? C109 C110 Ir4 72.6(10) . . ? C115 C110 Ir4 128.7(16) . . ? C110 C111 C112 113.9(19) . . ? C110 C111 C116 130(2) . . ? C112 C111 C116 116(2) . . ? C110 C111 Ir4 71.1(10) . . ? C112 C111 Ir4 71.7(10) . . ? C116 C111 Ir4 125.0(14) . . ? C117 C112 C113 129(3) . . ? C117 C112 C111 129(3) . . ? C113 C112 C111 101.6(18) . . ? C117 C112 Ir4 127.9(18) . . ? C113 C112 Ir4 67.4(10) . . ? C111 C112 Ir4 67.9(9) . . ? C109 C113 C112 107.0(17) . . ? C109 C113 C118 133(2) . . ? C112 C113 C118 119(2) . . ? C109 C113 Ir4 72.4(9) . . ? C112 C113 Ir4 73.1(11) . . ? C118 C113 Ir4 129.9(15) . . ? C120 C119 C123 108.0 . . ? C120 C119 C124 126.0 . . ? C123 C119 C124 126.0 . . ? C120 C119 Ir5 71.0(2) . . ? C123 C119 Ir5 70.19(18) . . ? C124 C119 Ir5 124.43(18) . . ? C121 C120 C119 108.0 . . ? C121 C120 C125 126.0 . . ? C119 C120 C125 126.0 . . ? C121 C120 Ir5 70.29(19) . . ? C119 C120 Ir5 70.8(2) . . ? C125 C120 Ir5 124.51(16) . . ? C120 C121 C122 108.0 . . ? C120 C121 C126 126.0 . . ? C122 C121 C126 126.0 . . ? C120 C121 Ir5 71.44(19) . . ? C122 C121 Ir5 70.27(18) . . ? C126 C121 Ir5 123.85(19) . . ? C123 C122 C121 108.0 . . ? C123 C122 C127 126.0 . . ? C121 C122 C127 126.0 . . ? C123 C122 Ir5 71.0(2) . . ? C121 C122 Ir5 71.2(2) . . ? C127 C122 Ir5 123.46(18) . . ? C122 C123 C119 108.0 . . ? C122 C123 C128 126.0 . . ? C119 C123 C128 126.0 . . ? C122 C123 Ir5 70.4(2) . . ? C119 C123 Ir5 71.47(19) . . ? C128 C123 Ir5 123.7(2) . . ? C133 C129 C130 108.0 . . ? C133 C129 C134 126.0 . . ? C130 C129 C134 126.0 . . ? C133 C129 Ir6 68.5(2) . . ? C130 C129 Ir6 75.8(2) . . ? C134 C129 Ir6 121.3(2) . . ? C131 C130 C129 108.0 . . ? C131 C130 C135 126.0 . . ? C129 C130 C135 126.0 . . ? C131 C130 Ir6 72.3(2) . . ? C129 C130 Ir6 67.8(2) . . ? C135 C130 Ir6 125.51(19) . . ? C130 C131 C132 108.0 . . ? C130 C131 C136 126.0 . . ? C132 C131 C136 126.0 . . ? C130 C131 Ir6 72.2(2) . . ? C132 C131 Ir6 67.8(2) . . ? C136 C131 Ir6 125.5(2) . . ? C133 C132 C131 108.0 . . ? C133 C132 C137 126.0 . . ? C131 C132 C137 126.0 . . ? C133 C132 Ir6 68.5(2) . . ? C131 C132 Ir6 75.8(2) . . ? C137 C132 Ir6 121.32(19) . . ? C132 C133 C129 108.0 . . ? C132 C133 C138 126.0 . . ? C129 C133 C138 126.0 . . ? C132 C133 Ir6 73.7(2) . . ? C129 C133 Ir6 73.6(2) . . ? C138 C133 Ir6 118.7(2) . . ? F1 C139 F3 115(2) . . ? F1 C139 F2 111(2) . . ? F3 C139 F2 102(2) . . ? F1 C139 S1 112.0(19) . . ? F3 C139 S1 111.2(19) . . ? F2 C139 S1 105.9(17) . . ? F5 C140 F4 108.4(17) . . ? F5 C140 F6 113.1(18) . . ? F4 C140 F6 111.2(18) . . ? F5 C140 S2 118.4(19) . . ? F4 C140 S2 99.5(17) . . ? F6 C140 S2 105.5(16) . . ? F9 C141 F7 103.2(16) . . ? F9 C141 F8 99.6(16) . . ? F7 C141 F8 98.0(16) . . ? F9 C141 S3 129(2) . . ? F7 C141 S3 109.2(19) . . ? F8 C141 S3 113(3) . . ? C150 C145 C146 120.0 . . ? C147 C146 C145 120.0 . . ? C157 C147 C146 130(3) . . ? C157 C147 C148 110(3) . . ? C146 C147 C148 120.0 . . ? C149 C148 C147 120.0 . . ? C149 C148 C151 111.4 . . ? C147 C148 C151 128.5 . . ? C148 C149 C150 120.0 . . ? C148 C149 C159 122(2) . . ? C150 C149 C159 118(2) . . ? C149 C150 C145 120.0 . . ? C156 C151 C152 120.0 . . ? C156 C151 C148 124.1 . . ? C152 C151 C148 115.8 . . ? C153 C152 C151 120.0 . . ? C153 C152 C158 124(3) . . ? C151 C152 C158 116(3) . . ? C152 C153 C154 120.0 . . ? C155 C154 C153 120.0 . . ? C154 C155 C156 120.0 . . ? C160 C156 C151 123(2) . . ? C160 C156 C155 117(2) . . ? C151 C156 C155 120.0 . . ? C147 C157 C158 125(5) . . ? C157 C158 C152 124(5) . . ? C160 C159 C149 126(5) . . ? C156 C160 C159 113(4) . . ? C15A C14A C14B 120.0 . . ? C14C C14B C14A 120.0 . . ? C14B C14C C14D 120.0 . . ? C14B C14C C15J 115.8(15) . . ? C14D C14C C15J 123.8(15) . . ? C14E C14D C14C 120.0 . . ? C14E C14D C15B 130.1 . . ? C14C C14D C15B 109.9 . . ? C15A C14E C14D 120.0 . . ? C15A C14E C15H 131.9(18) . . ? C14D C14E C15H 107.0(17) . . ? C14E C15A C14A 120.0 . . ? C15C C15B C15G 120.0 . . ? C15C C15B C14D 125.1 . . ? C15G C15B C14D 114.9 . . ? C15B C15C C15D 120.0 . . ? C15B C15C C16A 126(2) . . ? C15D C15C C16A 114(2) . . ? C15C C15D C15E 120.0 . . ? C15F C15E C15D 120.0 . . ? C15E C15F C15G 120.0 . . ? C15F C15G C15B 120.0 . . ? C15F C15G C15I 114.9(18) . . ? C15B C15G C15I 124.6(18) . . ? C14E C15H C15I 127(3) . . ? C15G C15I C15H 115(3) . . ? C16A C15J C14C 118(4) . . ? C15J C16A C15C 117(4) . . ? C166 C161 C162 120.0 . . ? C166 C161 C170 123.3(16) . . ? C162 C161 C170 116.7(15) . . ? C173 C162 C161 115.2(16) . . ? C173 C162 C163 124.7(16) . . ? C161 C162 C163 120.0 . . ? C176 C163 C164 117.3(14) . . ? C176 C163 C162 122.5(14) . . ? C164 C163 C162 120.0 . . ? C163 C164 C165 120.0 . . ? C164 C165 C166 120.0 . . ? C161 C166 C165 120.0 . . ? C161 C166 C167 115(2) . . ? C165 C166 C167 125(2) . . ? C168 C167 C166 118(3) . . ? C169 C168 C167 126(2) . . ? C170 C169 C168 119(2) . . ? C169 C170 C161 118(2) . . ? C169 C170 C171 121(2) . . ? C161 C170 C171 120.8(19) . . ? C172 C171 C170 117(2) . . ? C171 C172 C173 112.3(18) . . ? C162 C173 C174 112.9(18) . . ? C162 C173 C172 138(2) . . ? C174 C173 C172 109.2(16) . . ? C175 C174 C173 120(2) . . ? C174 C175 C176 128(2) . . ? C175 C176 C163 111(2) . . ? C178 C177 C182 120.0 . . ? C178 C177 C177 104(3) . 3_677 ? C182 C177 C177 136(3) . 3_677 ? C177 C178 C179 120.0 . . ? C177 C178 C184 134.2(19) . 3_677 ? C179 C178 C184 105.7(19) . 3_677 ? C178 C179 C180 120.0 . . ? C181 C180 C179 120.0 . . ? C180 C181 C182 120.0 . . ? C177 C182 C181 120.0 . . ? C177 C182 C183 109.1(19) . . ? C181 C182 C183 130.9(19) . . ? C182 C183 C184 127(2) . . ? C178 C184 C183 109(2) 3_677 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.592 _refine_diff_density_min -2.231 _refine_diff_density_rms 0.205