# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Guo-Xin Jin' _publ_contact_author_email gxjin@fudan.edu.cn _publ_section_title ; ; _publ_author_name 'Guo-Xin Jin' # Attachment '- 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 790455' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H136 Ir4 N8 O30' _chemical_formula_weight 2747.01 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.202(3) _cell_length_b 18.202(3) _cell_length_c 45.641(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15121(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 3.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6168 _exptl_absorpt_correction_T_max 0.7169 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 9.10 _diffrn_reflns_number 50466 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8241 _reflns_number_gt 5253 _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. Two nitrate anions outside were strongly disordered and could not be refined properly. New data sets corresponding to omission of the disordered anions were generated with the SQUEEZE algorithm before the structures were refined to convergence. The largest differential peak of the data is 2.964. ; _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^)+(0.1169P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8241 _refine_ls_number_parameters 335 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.792292(17) 0.59151(2) 0.085246(7) 0.04792(16) Uani 1 1 d . . . N1 N 0.7349(3) 0.9603(3) 0.15293(14) 0.0396(14) Uani 1 1 d . . . N2 N 0.5000 0.2500 0.0955(3) 0.080(4) Uani 1 2 d S . . O1 O 0.7122(3) 0.6658(3) 0.09876(11) 0.0384(11) Uani 1 1 d . . . O2 O 0.8186(3) 0.5856(3) 0.12944(11) 0.0428(13) Uani 1 1 d . . . O3 O 0.7596(3) 0.6433(3) 0.21297(11) 0.0436(13) Uani 1 1 d . . . H3A H 0.7540 0.6563 0.2300 0.028(19) Uiso 1 1 calc R . . O4 O 0.7561(3) 0.8104(3) 0.22814(11) 0.0455(13) Uani 1 1 d . . . O5 O 0.4454(7) 0.2400(5) 0.0813(3) 0.155(5) Uani 1 1 d . . . O6 O 0.5000 0.2500 0.1202(3) 0.133(6) Uani 1 2 d S . . C1 C 0.6464(5) 0.7541(5) 0.1244(2) 0.060(3) Uani 1 1 d . . . H1A H 0.6177 0.7501 0.1069 0.08(3) Uiso 1 1 calc R . . H1B H 0.6630 0.8039 0.1267 0.122 Uiso 1 1 calc R . . H1C H 0.6170 0.7405 0.1410 0.09(4) Uiso 1 1 calc R . . C2 C 0.7119(4) 0.7038(4) 0.12243(16) 0.0392(17) Uani 1 1 d . . . C3 C 0.7639(4) 0.6982(4) 0.14550(15) 0.0355(16) Uani 1 1 d . . . C4 C 0.8076(4) 0.6363(4) 0.14843(16) 0.0352(16) Uani 1 1 d . . . C5 C 0.8484(4) 0.6205(4) 0.17616(16) 0.0423(18) Uani 1 1 d . . . H5A H 0.9005 0.6256 0.1722 0.07(3) Uiso 1 1 calc R . . H5B H 0.8397 0.5695 0.1813 0.032(19) Uiso 1 1 calc R . . C6 C 0.8297(4) 0.6677(4) 0.20267(15) 0.0400(17) Uani 1 1 d . . . C7 C 0.8263(4) 0.7471(4) 0.19166(16) 0.0395(17) Uani 1 1 d . . . H7 H 0.8732 0.7584 0.1821 0.035(19) Uiso 1 1 calc R . . C8 C 0.7623(3) 0.7610(3) 0.16853(12) 0.0173(11) Uiso 1 1 d . . . H8A H 0.7149 0.7604 0.1787 0.04(2) Uiso 1 1 calc R . . C9 C 0.7263(4) 0.8915(4) 0.16373(15) 0.0334(15) Uani 1 1 d . . . H9A H 0.6875 0.8816 0.1764 0.08(3) Uiso 1 1 calc R . . C10 C 0.7751(4) 0.8349(4) 0.15618(17) 0.0403(17) Uani 1 1 d . . . C11 C 0.8311(4) 0.8489(5) 0.13708(17) 0.048(2) Uani 1 1 d . . . H11A H 0.8631 0.8116 0.1315 0.071 Uiso 1 1 calc R . . C12 C 0.8396(5) 0.9199(5) 0.1260(2) 0.055(2) Uani 1 1 d . . . H12A H 0.8769 0.9307 0.1128 0.07(3) Uiso 1 1 calc R . . C13 C 0.7910(5) 0.9744(5) 0.1353(2) 0.051(2) Uani 1 1 d . . . H13A H 0.7982 1.0224 0.1289 0.06(3) Uiso 1 1 calc R . . C14 C 0.8886(5) 0.6562(5) 0.22603(17) 0.054(2) Uani 1 1 d . . . H14A H 0.8774 0.6858 0.2429 0.09(3) Uiso 1 1 calc R . . H14B H 0.9356 0.6703 0.2183 0.08(3) Uiso 1 1 calc R . . H14C H 0.8898 0.6054 0.2316 0.09(4) Uiso 1 1 calc R . . C15 C 0.8162(5) 0.8011(4) 0.21745(17) 0.0442(18) Uani 1 1 d . . . C16 C 0.8801(6) 0.8419(7) 0.2279(3) 0.079(3) Uani 1 1 d . . . H16A H 0.8659 0.8728 0.2440 0.030(18) Uiso 1 1 calc R . . H16B H 0.8992 0.8717 0.2123 0.11(5) Uiso 1 1 calc R . . H16C H 0.9172 0.8081 0.2343 0.12(5) Uiso 1 1 calc R . . C17 C 0.8079(6) 0.5567(8) 0.0414(2) 0.076(3) Uani 1 1 d . . . C18 C 0.8669(6) 0.5313(7) 0.0585(2) 0.079(3) Uani 1 1 d . . . C19 C 0.9048(5) 0.5943(7) 0.0699(2) 0.071(3) Uani 1 1 d . . . C20 C 0.8682(5) 0.6571(6) 0.0608(2) 0.061(3) Uani 1 1 d . . . C21 C 0.8086(5) 0.6345(7) 0.04248(19) 0.066(3) Uani 1 1 d . . . C22 C 0.7531(7) 0.5092(13) 0.0239(4) 0.136(7) Uani 1 1 d . . . H22A H 0.7721 0.5008 0.0045 0.18(7) Uiso 1 1 calc R . . H22B H 0.7069 0.5343 0.0225 0.264 Uiso 1 1 calc R . . H22C H 0.7463 0.4630 0.0336 0.19(10) Uiso 1 1 calc R . . C23 C 0.8879(8) 0.4522(8) 0.0620(4) 0.130(7) Uani 1 1 d . . . H23A H 0.9228 0.4390 0.0472 0.196 Uiso 1 1 calc R . . H23B H 0.8450 0.4220 0.0602 0.196 Uiso 1 1 calc R . . H23C H 0.9095 0.4450 0.0810 0.196 Uiso 1 1 calc R . . C24 C 0.9716(5) 0.5893(7) 0.0902(2) 0.080(3) Uani 1 1 d . . . H24A H 1.0158 0.5915 0.0788 0.119 Uiso 1 1 calc R . . H24B H 0.9701 0.5438 0.1008 0.119 Uiso 1 1 calc R . . H24C H 0.9708 0.6296 0.1038 0.119 Uiso 1 1 calc R . . C25 C 0.8920(7) 0.7370(7) 0.0665(3) 0.084(4) Uani 1 1 d . . . H25A H 0.9268 0.7519 0.0518 0.13(5) Uiso 1 1 calc R . . H25B H 0.9143 0.7404 0.0855 0.028(18) Uiso 1 1 calc R . . H25C H 0.8498 0.7686 0.0657 0.10(4) Uiso 1 1 calc R . . C26 C 0.7558(7) 0.6891(9) 0.0276(3) 0.097(5) Uani 1 1 d . . . H26A H 0.7737 0.7006 0.0083 0.06(3) Uiso 1 1 calc R . . H26B H 0.7530 0.7333 0.0390 0.13(6) Uiso 1 1 calc R . . H26C H 0.7079 0.6675 0.0261 0.191 Uiso 1 1 calc R . . O7 O 0.5000 0.7500 0.0490(7) 0.278(14) Uani 1 2 d SD . . H7A H 0.5000 0.7500 0.0669(8) 0.334 Uiso 1 2 d SD . . H7B H 0.47(4) 0.78(3) 0.0443(12) 0.334 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0428(2) 0.0686(3) 0.0323(2) -0.00807(14) -0.00053(13) -0.00581(15) N1 0.042(4) 0.039(3) 0.038(3) -0.003(3) 0.000(3) -0.001(3) N2 0.157(15) 0.051(7) 0.031(6) 0.000 0.000 0.013(8) O1 0.040(3) 0.036(3) 0.039(3) -0.003(2) -0.006(2) 0.000(2) O2 0.036(3) 0.058(3) 0.034(3) -0.010(2) -0.009(2) 0.010(2) O3 0.051(3) 0.052(3) 0.028(3) 0.000(2) 0.001(2) -0.004(3) O4 0.061(4) 0.050(3) 0.026(3) -0.003(2) 0.005(2) -0.002(3) O5 0.232(13) 0.074(6) 0.160(10) -0.018(7) -0.109(9) 0.050(8) O6 0.158(14) 0.171(15) 0.070(9) 0.000 0.000 -0.082(12) C1 0.065(6) 0.061(6) 0.053(6) -0.012(4) -0.025(5) 0.011(5) C2 0.033(4) 0.049(5) 0.036(4) 0.012(3) 0.001(3) -0.005(3) C3 0.035(4) 0.038(4) 0.033(4) 0.001(3) 0.000(3) 0.007(3) C4 0.033(4) 0.038(4) 0.035(4) -0.002(3) 0.001(3) 0.001(3) C5 0.050(5) 0.051(5) 0.027(4) 0.002(3) -0.002(3) 0.004(4) C6 0.050(5) 0.049(5) 0.021(3) 0.003(3) 0.001(3) 0.011(4) C7 0.032(4) 0.054(5) 0.033(4) -0.001(3) -0.006(3) 0.001(3) C9 0.044(4) 0.035(4) 0.022(3) 0.000(3) -0.006(3) -0.004(3) C10 0.041(4) 0.043(4) 0.037(4) 0.002(3) -0.003(3) 0.003(3) C11 0.046(5) 0.058(5) 0.039(4) 0.004(4) 0.004(4) 0.009(4) C12 0.055(5) 0.053(5) 0.057(6) 0.016(4) 0.010(4) -0.004(4) C13 0.053(5) 0.044(5) 0.056(5) 0.014(4) -0.002(4) -0.005(4) C14 0.071(6) 0.068(6) 0.023(4) 0.003(4) -0.011(4) 0.012(5) C15 0.054(5) 0.046(5) 0.033(4) 0.004(3) -0.006(4) 0.002(4) C16 0.068(7) 0.088(8) 0.082(8) -0.041(7) -0.002(6) -0.006(7) C17 0.071(7) 0.124(10) 0.033(5) -0.041(6) 0.011(5) -0.019(7) C18 0.056(6) 0.108(9) 0.072(7) -0.040(7) 0.020(5) 0.001(6) C19 0.051(6) 0.119(10) 0.043(5) -0.035(6) 0.009(4) -0.021(6) C20 0.046(5) 0.081(7) 0.057(6) 0.005(5) 0.004(4) -0.027(5) C21 0.044(5) 0.126(10) 0.029(4) -0.005(5) 0.004(4) -0.024(6) C22 0.083(10) 0.23(2) 0.093(10) -0.104(13) -0.001(8) -0.031(11) C23 0.088(9) 0.145(14) 0.158(15) -0.089(12) 0.062(10) -0.008(9) C24 0.039(5) 0.123(10) 0.077(7) -0.007(7) -0.005(5) -0.006(6) C25 0.071(8) 0.116(10) 0.065(7) 0.022(7) -0.011(6) -0.026(7) C26 0.084(9) 0.151(13) 0.056(7) 0.034(9) -0.017(6) -0.024(8) O7 0.20(3) 0.35(6) 0.28(3) 0.000 0.000 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O2 2.076(5) . ? Ir1 O1 2.082(5) . ? Ir1 N1 2.110(6) 15_565 ? Ir1 C17 2.119(8) . ? Ir1 C21 2.123(9) . ? Ir1 C18 2.129(9) . ? Ir1 C20 2.141(9) . ? Ir1 C19 2.164(9) . ? N1 C13 1.326(10) . ? N1 C9 1.355(9) . ? N1 Ir1 2.110(6) 12_766 ? N2 O6 1.127(16) . ? N2 O5 1.199(11) 6_554 ? N2 O5 1.199(11) . ? O1 C2 1.282(9) . ? O2 C4 1.282(9) . ? O3 C6 1.430(9) . ? O4 C15 1.210(10) . ? C1 C2 1.505(12) . ? C2 C3 1.420(10) . ? C3 C4 1.385(10) . ? C3 C8 1.553(9) . ? C4 C5 1.495(10) . ? C5 C6 1.523(10) . ? C6 C14 1.525(10) . ? C6 C7 1.532(11) . ? C7 C15 1.544(11) . ? C7 C8 1.593(9) . ? C8 C10 1.478(9) . ? C9 C10 1.403(10) . ? C10 C11 1.364(11) . ? C11 C12 1.397(12) . ? C12 C13 1.395(13) . ? C15 C16 1.460(13) . ? C17 C18 1.405(16) . ? C17 C21 1.417(17) . ? C17 C22 1.543(15) . ? C18 C19 1.435(15) . ? C18 C23 1.499(19) . ? C19 C20 1.387(15) . ? C19 C24 1.533(14) . ? C20 C21 1.429(12) . ? C20 C25 1.540(15) . ? C21 C26 1.541(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ir1 O1 84.7(2) . . ? O2 Ir1 N1 83.1(2) . 15_565 ? O1 Ir1 N1 81.8(2) . 15_565 ? O2 Ir1 C17 150.6(4) . . ? O1 Ir1 C17 124.6(4) . . ? N1 Ir1 C17 98.0(4) 15_565 . ? O2 Ir1 C21 151.6(3) . . ? O1 Ir1 C21 97.5(4) . . ? N1 Ir1 C21 125.2(3) 15_565 . ? C17 Ir1 C21 39.0(5) . . ? O2 Ir1 C18 112.6(4) . . ? O1 Ir1 C18 161.9(4) . . ? N1 Ir1 C18 105.0(4) 15_565 . ? C17 Ir1 C18 38.6(4) . . ? C21 Ir1 C18 64.7(5) . . ? O2 Ir1 C20 112.8(3) . . ? O1 Ir1 C20 104.1(3) . . ? N1 Ir1 C20 163.2(3) 15_565 . ? C17 Ir1 C20 65.6(4) . . ? C21 Ir1 C20 39.2(3) . . ? C18 Ir1 C20 64.9(5) . . ? O2 Ir1 C19 95.6(3) . . ? O1 Ir1 C19 138.0(4) . . ? N1 Ir1 C19 140.1(4) 15_565 . ? C17 Ir1 C19 64.8(4) . . ? C21 Ir1 C19 64.0(4) . . ? C18 Ir1 C19 39.0(4) . . ? C20 Ir1 C19 37.6(4) . . ? C13 N1 C9 119.2(7) . . ? C13 N1 Ir1 121.7(5) . 12_766 ? C9 N1 Ir1 119.0(5) . 12_766 ? O6 N2 O5 122.7(9) . 6_554 ? O6 N2 O5 122.7(9) . . ? O5 N2 O5 114.6(18) 6_554 . ? C2 O1 Ir1 127.1(5) . . ? C4 O2 Ir1 125.7(5) . . ? O1 C2 C3 125.7(7) . . ? O1 C2 C1 112.5(7) . . ? C3 C2 C1 121.7(7) . . ? C4 C3 C2 120.8(7) . . ? C4 C3 C8 123.0(6) . . ? C2 C3 C8 115.9(6) . . ? O2 C4 C3 127.6(7) . . ? O2 C4 C5 110.8(6) . . ? C3 C4 C5 121.6(7) . . ? C4 C5 C6 116.9(6) . . ? O3 C6 C5 106.5(6) . . ? O3 C6 C14 110.7(6) . . ? C5 C6 C14 108.8(6) . . ? O3 C6 C7 111.4(6) . . ? C5 C6 C7 106.3(6) . . ? C14 C6 C7 112.7(7) . . ? C6 C7 C15 110.8(6) . . ? C6 C7 C8 113.4(6) . . ? C15 C7 C8 108.5(6) . . ? C10 C8 C3 114.1(5) . . ? C10 C8 C7 106.4(5) . . ? C3 C8 C7 108.5(5) . . ? N1 C9 C10 121.1(7) . . ? C11 C10 C9 119.5(7) . . ? C11 C10 C8 122.1(7) . . ? C9 C10 C8 118.3(6) . . ? C10 C11 C12 119.1(8) . . ? C13 C12 C11 118.6(8) . . ? N1 C13 C12 122.3(8) . . ? O4 C15 C16 121.2(8) . . ? O4 C15 C7 120.2(7) . . ? C16 C15 C7 118.6(8) . . ? C18 C17 C21 107.5(9) . . ? C18 C17 C22 126.7(14) . . ? C21 C17 C22 125.7(14) . . ? C18 C17 Ir1 71.1(5) . . ? C21 C17 Ir1 70.7(5) . . ? C22 C17 Ir1 124.8(8) . . ? C17 C18 C19 107.8(11) . . ? C17 C18 C23 124.8(12) . . ? C19 C18 C23 127.2(12) . . ? C17 C18 Ir1 70.3(6) . . ? C19 C18 Ir1 71.8(6) . . ? C23 C18 Ir1 126.5(8) . . ? C20 C19 C18 108.6(10) . . ? C20 C19 C24 127.7(10) . . ? C18 C19 C24 123.6(12) . . ? C20 C19 Ir1 70.3(5) . . ? C18 C19 Ir1 69.2(5) . . ? C24 C19 Ir1 123.6(7) . . ? C19 C20 C21 107.5(9) . . ? C19 C20 C25 126.3(9) . . ? C21 C20 C25 125.9(11) . . ? C19 C20 Ir1 72.1(6) . . ? C21 C20 Ir1 69.8(5) . . ? C25 C20 Ir1 128.3(8) . . ? C17 C21 C20 108.4(10) . . ? C17 C21 C26 128.6(10) . . ? C20 C21 C26 123.0(11) . . ? C17 C21 Ir1 70.3(6) . . ? C20 C21 Ir1 71.1(5) . . ? C26 C21 Ir1 123.8(7) . . ? 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 -0.012 0.003 0.005 6387.6 477.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.964 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.185 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 790456' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H169 Ag2.50 Ir4 N10.50 O47.50' _chemical_formula_weight 3437.03 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' Ag Ag -0.8971 1.1015 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.876(5) _cell_length_b 36.814(5) _cell_length_c 22.468(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.009(2) _cell_angle_gamma 90.00 _cell_volume 30484(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.78 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13664 _exptl_absorpt_coefficient_mu 3.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4447 _exptl_absorpt_correction_T_max 0.5427 _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_% 7.82 _diffrn_reflns_number 81397 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 25.01 _reflns_number_total 26660 _reflns_number_gt 15735 _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. There were disordered solvent molecules which could not be refined properly so that the SQUEEZE algorithm was used to omit them. The hydrogen atoms in the solvents MeOH and water could not be found. The largest differential peak of the data is 5.610. ; _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26660 _refine_ls_number_parameters 1532 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1539 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.3193 _refine_ls_wR_factor_gt 0.2885 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.650304(17) 0.320442(17) 0.68082(3) 0.03218(19) Uani 1 1 d . . . Ir2 Ir 0.895291(19) 0.37374(2) 0.72118(3) 0.0416(2) Uani 1 1 d . . . Ir3 Ir 0.81669(2) 0.60139(2) 0.59431(3) 0.0480(2) Uani 1 1 d . . . Ir4 Ir 0.618391(18) 0.553536(19) 0.82229(3) 0.0371(2) Uani 1 1 d . . . Ag1 Ag 0.79450(11) 0.54396(9) 0.92869(16) 0.1470(12) Uani 1 1 d . . . Ag2 Ag 0.83797(6) 0.21308(6) 0.73050(10) 0.0837(6) Uani 1 1 d . . . Ag3 Ag 0.5000 0.62508(11) 0.2500 0.1292(14) Uani 1 2 d S . . N1 N 0.8501(4) 0.3388(3) 0.7197(6) 0.036(3) Uani 1 1 d . . . N2 N 0.8572(4) 0.5608(4) 0.6060(6) 0.037(3) Uani 1 1 d . . . N3 N 0.6550(3) 0.5873(3) 0.7830(5) 0.028(3) Uani 1 1 d . . . N4 N 0.6210(3) 0.3646(3) 0.7114(6) 0.028(3) Uani 1 1 d U . . N5 N 0.7604(9) 0.4818(10) 0.8544(13) 0.110(9) Uani 1 1 d . . . N6 N 0.7622(5) 0.2132(4) 0.7662(9) 0.051(4) Uani 1 1 d . . . N7 N 0.8671(10) 0.2083(7) 0.6120(14) 0.120(12) Uani 1 1 d . . . N8 N 0.8917(17) 0.2164(18) 0.817(3) 0.25(2) Uiso 1 1 d . . . N9 N 0.5000 0.5456(6) 0.2500 0.053(6) Uani 1 2 d S . . N10 N 0.513(2) 0.668(3) 0.368(2) 0.44(6) Uiso 1 1 d D . . N11 N 0.2909(7) 0.8735(9) 0.5644(14) 0.153(15) Uani 1 1 d D . . O1 O 0.6912(2) 0.3595(2) 0.6872(5) 0.025(2) Uani 1 1 d U . . O2 O 0.6639(3) 0.3126(3) 0.7689(5) 0.036(3) Uani 1 1 d . . . O3 O 0.7257(4) 0.3399(3) 0.9153(5) 0.052(4) Uani 1 1 d . . . H3 H 0.7357 0.3564 0.8959 0.079 Uiso 1 1 calc R . . O4 O 0.8115(4) 0.3428(4) 0.8983(6) 0.059(4) Uani 1 1 d . . . O5 O 0.8550(3) 0.4130(3) 0.7100(5) 0.034(3) Uani 1 1 d . . . O6 O 0.8908(3) 0.3708(3) 0.6309(6) 0.042(3) Uani 1 1 d . . . O7 O 0.8498(4) 0.4091(4) 0.4732(6) 0.061(4) Uani 1 1 d . . . H7 H 0.8390 0.4278 0.4603 0.092 Uiso 1 1 calc R . . O8 O 0.8532(6) 0.4888(5) 0.4414(8) 0.100(6) Uani 1 1 d . . . O9 O 0.7853(3) 0.5628(3) 0.6364(4) 0.035(3) Uani 1 1 d . . . O10 O 0.8332(3) 0.6156(3) 0.6792(5) 0.042(3) Uani 1 1 d . . . O11 O 0.8262(4) 0.5940(3) 0.8551(6) 0.051(3) Uani 1 1 d . . . H11 H 0.8397 0.5974 0.8854 0.076 Uiso 1 1 calc R . . O12 O 0.7517(4) 0.5936(4) 0.9127(6) 0.071(4) Uani 1 1 d . . . O13 O 0.6517(3) 0.5141(3) 0.7892(4) 0.028(2) Uani 1 1 d . . . O14 O 0.5939(3) 0.5528(3) 0.7385(6) 0.045(3) Uani 1 1 d . . . O15 O 0.5987(3) 0.5162(3) 0.5717(6) 0.050(3) Uani 1 1 d . . . H15A H 0.5958 0.5370 0.5572 0.075 Uiso 1 1 calc R . . O16 O 0.6027(4) 0.4332(4) 0.5480(5) 0.051(3) Uani 1 1 d . . . O17 O 0.7840(9) 0.5063(9) 0.8436(12) 0.180(15) Uani 1 1 d . . . O18 O 0.7418(7) 0.4805(8) 0.8927(16) 0.146(10) Uani 1 1 d . . . O19 O 0.7561(7) 0.4553(6) 0.8211(10) 0.118(8) Uani 1 1 d . . . O20 O 0.7715(3) 0.2070(3) 0.7114(7) 0.053(4) Uani 1 1 d . . . O21 O 0.7862(4) 0.2164(4) 0.8079(7) 0.070(5) Uani 1 1 d . . . O22 O 0.7304(5) 0.2133(4) 0.7780(7) 0.077(5) Uani 1 1 d . . . O23 O 0.8471(9) 0.1874(9) 0.6386(18) 0.198(19) Uani 1 1 d . . . O24 O 0.8768(10) 0.2345(7) 0.6380(14) 0.182(13) Uani 1 1 d . . . O25 O 0.8804(7) 0.2010(5) 0.5649(11) 0.139(9) Uani 1 1 d D . . O26 O 0.8782(9) 0.2417(9) 0.8064(15) 0.166(11) Uiso 1 1 d . . . O27 O 0.8979(9) 0.1880(9) 0.7789(17) 0.179(12) Uiso 1 1 d . . . O28 O 0.9299(16) 0.2261(15) 0.835(3) 0.31(2) Uiso 1 1 d . . . O29 O 0.5017(4) 0.5633(4) 0.2978(6) 0.063(4) Uani 1 1 d . . . O30 O 0.5000 0.5103(9) 0.2500 0.103(9) Uani 1 2 d S . . O31 O 0.4881(10) 0.6458(11) 0.3506(18) 0.207(14) Uiso 1 1 d D . . O32 O 0.5233(12) 0.6771(12) 0.316(2) 0.26(2) Uiso 1 1 d D . . O33 O 0.5173(15) 0.6795(15) 0.421(2) 0.31(2) Uiso 1 1 d D . . O34 O 0.3159(6) 0.8615(6) 0.5320(11) 0.123(7) Uiso 1 1 d D . . O35 O 0.2668(11) 0.8508(12) 0.580(2) 0.31(3) Uiso 1 1 d D . . O36 O 0.293(2) 0.9048(14) 0.586(5) 0.66(9) Uiso 1 1 d D . . O37 O 0.7732(7) 0.5174(12) 1.0115(18) 0.25(2) Uani 1 1 d . . . C1 C 0.7445(4) 0.3892(4) 0.7145(7) 0.029(3) Uani 1 1 d . . . H1A H 0.7668 0.3799 0.6976 0.043 Uiso 1 1 calc R . . H1B H 0.7502 0.4008 0.7529 0.043 Uiso 1 1 calc R . . H1C H 0.7333 0.4071 0.6872 0.043 Uiso 1 1 calc R . . C2 C 0.7194(4) 0.3594(4) 0.7228(6) 0.029(4) Uani 1 1 d . . . C3 C 0.7260(4) 0.3349(4) 0.7709(6) 0.026(3) Uani 1 1 d . . . C4 C 0.6959(4) 0.3149(4) 0.7930(8) 0.037(4) Uani 1 1 d . . . C5 C 0.7003(4) 0.2938(4) 0.8506(7) 0.032(4) Uani 1 1 d . . . H5A H 0.7028 0.2677 0.8411 0.038 Uiso 1 1 calc R . . H5B H 0.6780 0.2969 0.8734 0.038 Uiso 1 1 calc R . . C6 C 0.7344(5) 0.3060(5) 0.8914(7) 0.038(4) Uani 1 1 d . . . C7 C 0.7647(4) 0.3054(4) 0.8523(6) 0.027(3) Uani 1 1 d . . . H7A H 0.7663 0.2805 0.8345 0.032 Uiso 1 1 calc R . . C8 C 0.7621(5) 0.3336(5) 0.8005(8) 0.042(5) Uani 1 1 d . . . H8 H 0.7669 0.3581 0.8183 0.051 Uiso 1 1 calc R . . C9 C 0.8233(4) 0.3457(4) 0.7556(6) 0.028(3) Uani 1 1 d . . . H9 H 0.8261 0.3660 0.7816 0.033 Uiso 1 1 calc R . . C10 C 0.7916(4) 0.3260(4) 0.7587(6) 0.031(4) Uani 1 1 d . . . C11 C 0.7891(6) 0.2954(5) 0.7176(9) 0.051(5) Uani 1 1 d . . . H11A H 0.7684 0.2801 0.7168 0.062 Uiso 1 1 calc R . . C12 C 0.8159(5) 0.2890(5) 0.6814(7) 0.040(4) Uani 1 1 d . . . H12 H 0.8139 0.2695 0.6538 0.048 Uiso 1 1 calc R . . C13 C 0.8466(4) 0.3101(4) 0.6833(7) 0.031(4) Uani 1 1 d . . . H13 H 0.8659 0.3043 0.6581 0.037 Uiso 1 1 calc R . . C14 C 0.7343(5) 0.2779(4) 0.9427(7) 0.039(4) Uani 1 1 d . . . H14A H 0.7491 0.2870 0.9766 0.059 Uiso 1 1 calc R . . H14B H 0.7444 0.2549 0.9290 0.059 Uiso 1 1 calc R . . H14C H 0.7094 0.2740 0.9550 0.059 Uiso 1 1 calc R . . C15 C 0.8009(5) 0.3132(6) 0.8876(8) 0.047(5) Uani 1 1 d . . . C16 C 0.8218(8) 0.2796(7) 0.9071(12) 0.100(11) Uani 1 1 d . . . H16A H 0.8288 0.2659 0.8719 0.150 Uiso 1 1 calc R . . H16B H 0.8065 0.2644 0.9317 0.150 Uiso 1 1 calc R . . H16C H 0.8436 0.2868 0.9303 0.150 Uiso 1 1 calc R . . C17 C 0.8188(5) 0.4593(5) 0.6704(9) 0.050(5) Uani 1 1 d . . . H17A H 0.8046 0.4530 0.7050 0.075 Uiso 1 1 calc R . . H17B H 0.8031 0.4583 0.6343 0.075 Uiso 1 1 calc R . . H17C H 0.8286 0.4839 0.6754 0.075 Uiso 1 1 calc R . . C18 C 0.8495(4) 0.4327(5) 0.6652(8) 0.040(4) Uani 1 1 d . . . C19 C 0.8693(4) 0.4306(4) 0.6109(7) 0.033(4) Uani 1 1 d . . . C20 C 0.8861(5) 0.3988(5) 0.5947(8) 0.043(5) Uani 1 1 d . . . C21 C 0.9014(6) 0.3915(5) 0.5360(8) 0.049(5) Uani 1 1 d . . . H21A H 0.8953 0.3663 0.5240 0.058 Uiso 1 1 calc R . . H21B H 0.9282 0.3932 0.5398 0.058 Uiso 1 1 calc R . . C22 C 0.8876(6) 0.4177(6) 0.4864(8) 0.053(5) Uani 1 1 d . . . C23 C 0.8902(5) 0.4567(5) 0.5127(9) 0.050(5) Uani 1 1 d . . . H23 H 0.9157 0.4602 0.5282 0.060 Uiso 1 1 calc R . . C24 C 0.8658(5) 0.4617(5) 0.5643(7) 0.037(4) Uani 1 1 d . . . H24 H 0.8402 0.4618 0.5481 0.044 Uiso 1 1 calc R . . C25 C 0.8496(5) 0.5267(5) 0.5847(7) 0.042(4) Uani 1 1 d . . . H25 H 0.8271 0.5226 0.5640 0.050 Uiso 1 1 calc R . . C26 C 0.8732(4) 0.4985(5) 0.5921(7) 0.035(4) Uani 1 1 d . . . C27 C 0.9076(5) 0.5045(5) 0.6207(7) 0.042(4) Uani 1 1 d . . . H27 H 0.9254 0.4860 0.6253 0.050 Uiso 1 1 calc R . . C28 C 0.9133(5) 0.5412(6) 0.6422(8) 0.053(5) Uani 1 1 d . . . H28 H 0.9353 0.5466 0.6636 0.063 Uiso 1 1 calc R . . C29 C 0.8895(5) 0.5671(5) 0.6334(8) 0.039(4) Uani 1 1 d . . . H29 H 0.8952 0.5910 0.6467 0.047 Uiso 1 1 calc R . . C30 C 0.9121(7) 0.4124(5) 0.4312(9) 0.064(6) Uani 1 1 d . . . H30A H 0.9085 0.3879 0.4150 0.096 Uiso 1 1 calc R . . H30B H 0.9376 0.4157 0.4436 0.096 Uiso 1 1 calc R . . H30C H 0.9054 0.4303 0.4005 0.096 Uiso 1 1 calc R . . C31 C 0.8836(7) 0.4836(6) 0.4649(9) 0.060(6) Uani 1 1 d . . . C32 C 0.9120(9) 0.5063(8) 0.4456(16) 0.124(14) Uani 1 1 d . . . H32A H 0.9094 0.5099 0.4024 0.185 Uiso 1 1 calc R . . H32B H 0.9354 0.4948 0.4553 0.185 Uiso 1 1 calc R . . H32C H 0.9108 0.5299 0.4657 0.185 Uiso 1 1 calc R . . C33 C 0.7493(5) 0.5333(4) 0.7060(7) 0.039(4) Uani 1 1 d . . . H33A H 0.7349 0.5408 0.7397 0.058 Uiso 1 1 calc R . . H33B H 0.7647 0.5126 0.7177 0.058 Uiso 1 1 calc R . . H33C H 0.7330 0.5262 0.6726 0.058 Uiso 1 1 calc R . . C34 C 0.7732(4) 0.5649(4) 0.6870(8) 0.034(4) Uani 1 1 d . . . C35 C 0.7823(4) 0.5939(4) 0.7310(7) 0.026(3) Uani 1 1 d . . . C36 C 0.8130(4) 0.6149(5) 0.7253(8) 0.038(4) Uani 1 1 d . . . C37 C 0.8268(5) 0.6377(4) 0.7747(7) 0.034(4) Uani 1 1 d . . . H37A H 0.8206 0.6634 0.7658 0.040 Uiso 1 1 calc R . . H37B H 0.8536 0.6358 0.7772 0.040 Uiso 1 1 calc R . . C38 C 0.8118(5) 0.6276(4) 0.8350(8) 0.040(4) Uani 1 1 d . . . C39 C 0.7708(4) 0.6267(4) 0.8288(7) 0.031(4) Uani 1 1 d . . . H39 H 0.7624 0.6501 0.8103 0.037 Uiso 1 1 calc R . . C40 C 0.7586(4) 0.5952(4) 0.7867(6) 0.031(4) Uani 1 1 d . . . H40 H 0.7611 0.5717 0.8087 0.037 Uiso 1 1 calc R . . C41 C 0.6921(4) 0.5817(4) 0.7945(7) 0.028(3) Uani 1 1 d . . . H41 H 0.6991 0.5628 0.8215 0.034 Uiso 1 1 calc R . . C42 C 0.7191(5) 0.6014(4) 0.7698(7) 0.033(4) Uani 1 1 d . . . C43 C 0.7092(5) 0.6273(4) 0.7272(8) 0.040(4) Uani 1 1 d . . . H43 H 0.7273 0.6388 0.7049 0.048 Uiso 1 1 calc R . . C44 C 0.6738(4) 0.6361(4) 0.7175(7) 0.034(4) Uani 1 1 d . . . H44 H 0.6668 0.6565 0.6938 0.041 Uiso 1 1 calc R . . C45 C 0.6472(5) 0.6135(4) 0.7442(7) 0.036(4) Uani 1 1 d . . . H45 H 0.6224 0.6176 0.7334 0.043 Uiso 1 1 calc R . . C46 C 0.8230(6) 0.6581(5) 0.8806(9) 0.058(6) Uani 1 1 d . . . H46C H 0.8098 0.6548 0.9173 0.087 Uiso 1 1 calc R . . H46D H 0.8170 0.6820 0.8634 0.087 Uiso 1 1 calc R . . H46E H 0.8491 0.6568 0.8896 0.087 Uiso 1 1 calc R . . C47 C 0.7541(5) 0.6232(4) 0.8861(7) 0.030(4) Uani 1 1 d . . . C48 C 0.7347(6) 0.6551(5) 0.9122(10) 0.056(5) Uani 1 1 d . . . H48C H 0.7105 0.6575 0.8929 0.085 Uiso 1 1 calc R . . H48D H 0.7486 0.6773 0.9058 0.085 Uiso 1 1 calc R . . H48E H 0.7321 0.6513 0.9551 0.085 Uiso 1 1 calc R . . C49 C 0.6748(4) 0.4681(5) 0.7333(8) 0.040(4) Uani 1 1 d . . . H49A H 0.6945 0.4720 0.7630 0.060 Uiso 1 1 calc R . . H49B H 0.6838 0.4723 0.6934 0.060 Uiso 1 1 calc R . . H49C H 0.6659 0.4431 0.7363 0.060 Uiso 1 1 calc R . . C50 C 0.6455(4) 0.4932(4) 0.7440(6) 0.028(3) Uani 1 1 d . . . C51 C 0.6148(5) 0.4955(5) 0.7057(8) 0.044(4) Uani 1 1 d . . . C52 C 0.5910(4) 0.5244(5) 0.7044(8) 0.036(4) Uani 1 1 d . . . C53 C 0.5623(4) 0.5287(5) 0.6568(8) 0.039(4) Uani 1 1 d . . . H53A H 0.5606 0.5547 0.6457 0.047 Uiso 1 1 calc R . . H53B H 0.5387 0.5216 0.6731 0.047 Uiso 1 1 calc R . . C54 C 0.5685(5) 0.5063(4) 0.6007(8) 0.039(4) Uani 1 1 d . . . C55 C 0.5723(5) 0.4657(4) 0.6212(6) 0.032(4) Uani 1 1 d U . . H55 H 0.5507 0.4594 0.6448 0.039 Uiso 1 1 calc R . . C56 C 0.6076(4) 0.4632(4) 0.6641(6) 0.022(3) Uani 1 1 d . . . H56 H 0.6290 0.4607 0.6383 0.027 Uiso 1 1 calc R . . C57 C 0.6219(4) 0.3956(4) 0.6813(6) 0.023(3) Uani 1 1 d . . . H57 H 0.6354 0.3964 0.6461 0.028 Uiso 1 1 calc R . . C58 C 0.6039(4) 0.4271(4) 0.6989(7) 0.027(3) Uani 1 1 d . . . C59 C 0.5834(4) 0.4242(5) 0.7493(7) 0.032(4) Uani 1 1 d . . . H59 H 0.5704 0.4445 0.7632 0.038 Uiso 1 1 calc R . . C60 C 0.5822(5) 0.3924(5) 0.7781(8) 0.048(5) Uani 1 1 d . . . H60 H 0.5685 0.3908 0.8131 0.058 Uiso 1 1 calc R . . C61 C 0.5992(5) 0.3633(5) 0.7594(7) 0.038(4) Uani 1 1 d . . . H61 H 0.5963 0.3410 0.7798 0.045 Uiso 1 1 calc R . . C62 C 0.5326(4) 0.5078(5) 0.5595(8) 0.045(4) Uani 1 1 d . . . H62A H 0.5276 0.5330 0.5478 0.067 Uiso 1 1 calc R . . H62B H 0.5122 0.4983 0.5815 0.067 Uiso 1 1 calc R . . H62C H 0.5359 0.4930 0.5238 0.067 Uiso 1 1 calc R . . C63 C 0.5747(5) 0.4390(4) 0.5711(7) 0.034(4) Uani 1 1 d . . . C64 C 0.5403(6) 0.4229(6) 0.5509(11) 0.071(7) Uani 1 1 d . . . H64A H 0.5446 0.3986 0.5350 0.106 Uiso 1 1 calc R . . H64B H 0.5290 0.4382 0.5196 0.106 Uiso 1 1 calc R . . H64C H 0.5241 0.4212 0.5844 0.106 Uiso 1 1 calc R . . C65 C 0.6721(5) 0.2768(4) 0.6283(8) 0.036(4) Uani 1 1 d . . . C66 C 0.6408(5) 0.2636(5) 0.6633(7) 0.037(4) Uani 1 1 d . . . C67 C 0.6088(5) 0.2838(5) 0.6488(9) 0.046(5) Uani 1 1 d . . . C68 C 0.6204(5) 0.3093(4) 0.5994(8) 0.038(4) Uani 1 1 d . . . C69 C 0.6559(5) 0.3044(5) 0.5906(8) 0.046(5) Uani 1 1 d . . . C70 C 0.7077(5) 0.2613(5) 0.6325(8) 0.044(4) Uani 1 1 d . . . H70A H 0.7140 0.2515 0.5936 0.066 Uiso 1 1 calc R . . H70B H 0.7082 0.2417 0.6619 0.066 Uiso 1 1 calc R . . H70C H 0.7253 0.2800 0.6447 0.066 Uiso 1 1 calc R . . C71 C 0.6413(5) 0.2369(6) 0.7091(9) 0.058(6) Uani 1 1 d . . . H71A H 0.6272 0.2456 0.7425 0.087 Uiso 1 1 calc R . . H71B H 0.6664 0.2323 0.7229 0.087 Uiso 1 1 calc R . . H71C H 0.6305 0.2143 0.6935 0.087 Uiso 1 1 calc R . . C72 C 0.5742(6) 0.2796(7) 0.6636(12) 0.074(7) Uani 1 1 d . . . H72A H 0.5627 0.2611 0.6379 0.111 Uiso 1 1 calc R . . H72B H 0.5613 0.3027 0.6583 0.111 Uiso 1 1 calc R . . H72C H 0.5733 0.2719 0.7053 0.111 Uiso 1 1 calc R . . C73 C 0.5934(5) 0.3351(5) 0.5682(10) 0.056(5) Uani 1 1 d . . . H73A H 0.6059 0.3494 0.5383 0.085 Uiso 1 1 calc R . . H73B H 0.5832 0.3515 0.5976 0.085 Uiso 1 1 calc R . . H73C H 0.5739 0.3211 0.5486 0.085 Uiso 1 1 calc R . . C74 C 0.6788(6) 0.3252(5) 0.5474(9) 0.058(5) Uani 1 1 d . . . H74A H 0.6772 0.3134 0.5083 0.086 Uiso 1 1 calc R . . H74B H 0.7041 0.3255 0.5622 0.086 Uiso 1 1 calc R . . H74C H 0.6698 0.3502 0.5438 0.086 Uiso 1 1 calc R . . C75 C 0.9404(7) 0.3403(6) 0.7516(10) 0.066(6) Uani 1 1 d . . . C76 C 0.9526(6) 0.3743(9) 0.7226(10) 0.076(8) Uani 1 1 d . . . C77 C 0.9413(6) 0.4027(8) 0.7535(11) 0.073(7) Uani 1 1 d . . . C78 C 0.9214(5) 0.3907(7) 0.8045(9) 0.060(6) Uani 1 1 d . . . C79 C 0.9196(5) 0.3525(8) 0.8023(10) 0.071(7) Uani 1 1 d . . . C80 C 0.9463(12) 0.3062(11) 0.738(2) 0.22(3) Uani 1 1 d . . . H80A H 0.9686 0.2979 0.7587 0.337 Uiso 1 1 calc R . . H80B H 0.9488 0.3040 0.6949 0.337 Uiso 1 1 calc R . . H80C H 0.9258 0.2914 0.7503 0.337 Uiso 1 1 calc R . . C81 C 0.9738(7) 0.3781(15) 0.6705(16) 0.19(2) Uani 1 1 d . . . H81A H 0.9616 0.3949 0.6425 0.284 Uiso 1 1 calc R . . H81B H 0.9764 0.3543 0.6515 0.284 Uiso 1 1 calc R . . H81C H 0.9979 0.3876 0.6819 0.284 Uiso 1 1 calc R . . C82 C 0.9467(9) 0.4423(7) 0.7396(18) 0.139(17) Uani 1 1 d . . . H82A H 0.9552 0.4448 0.6989 0.208 Uiso 1 1 calc R . . H82B H 0.9649 0.4526 0.7678 0.208 Uiso 1 1 calc R . . H82C H 0.9237 0.4553 0.7430 0.208 Uiso 1 1 calc R . . C83 C 0.9034(9) 0.4156(11) 0.8494(16) 0.16(2) Uani 1 1 d . . . H83A H 0.8806 0.4251 0.8318 0.237 Uiso 1 1 calc R . . H83B H 0.9197 0.4358 0.8597 0.237 Uiso 1 1 calc R . . H83C H 0.8983 0.4018 0.8855 0.237 Uiso 1 1 calc R . . C84 C 0.9044(8) 0.3307(9) 0.8453(12) 0.111(12) Uani 1 1 d . . . H84A H 0.9238 0.3193 0.8697 0.167 Uiso 1 1 calc R . . H84B H 0.8895 0.3118 0.8257 0.167 Uiso 1 1 calc R . . H84C H 0.8892 0.3455 0.8706 0.167 Uiso 1 1 calc R . . C85 C 0.7799(5) 0.6423(5) 0.5572(8) 0.049(5) Uani 1 1 d . . . C86 C 0.8163(6) 0.6558(6) 0.5596(9) 0.057(5) Uani 1 1 d . . . C87 C 0.8390(6) 0.6333(6) 0.5246(12) 0.070(7) Uani 1 1 d . . . C88 C 0.8152(7) 0.6060(7) 0.5017(11) 0.070(7) Uani 1 1 d . . . C89 C 0.7784(10) 0.6104(8) 0.5167(11) 0.093(9) Uani 1 1 d . . . C90 C 0.7456(6) 0.6564(8) 0.5847(12) 0.089(9) Uani 1 1 d . . . H90A H 0.7520 0.6754 0.6137 0.133 Uiso 1 1 calc R . . H90B H 0.7335 0.6364 0.6049 0.133 Uiso 1 1 calc R . . H90C H 0.7294 0.6664 0.5535 0.133 Uiso 1 1 calc R . . C91 C 0.8257(11) 0.6884(7) 0.6004(16) 0.16(2) Uani 1 1 d . . . H91A H 0.8090 0.6890 0.6334 0.236 Uiso 1 1 calc R . . H91B H 0.8234 0.7110 0.5775 0.236 Uiso 1 1 calc R . . H91C H 0.8506 0.6859 0.6163 0.236 Uiso 1 1 calc R . . C92 C 0.8777(8) 0.6383(10) 0.5116(14) 0.119(12) Uani 1 1 d . . . H92A H 0.8804 0.6394 0.4684 0.178 Uiso 1 1 calc R . . H92B H 0.8918 0.6178 0.5280 0.178 Uiso 1 1 calc R . . H92C H 0.8866 0.6610 0.5297 0.178 Uiso 1 1 calc R . . C93 C 0.8224(10) 0.5754(8) 0.4559(11) 0.122(13) Uani 1 1 d . . . H93A H 0.8027 0.5750 0.4255 0.182 Uiso 1 1 calc R . . H93B H 0.8236 0.5519 0.4764 0.182 Uiso 1 1 calc R . . H93C H 0.8455 0.5800 0.4369 0.182 Uiso 1 1 calc R . . C94 C 0.7475(7) 0.5862(8) 0.5037(11) 0.085(8) Uani 1 1 d . . . H94A H 0.7489 0.5767 0.4630 0.128 Uiso 1 1 calc R . . H94B H 0.7248 0.5997 0.5074 0.128 Uiso 1 1 calc R . . H94C H 0.7481 0.5659 0.5319 0.128 Uiso 1 1 calc R . . C95 C 0.5859(5) 0.5255(6) 0.8854(9) 0.054(6) Uani 1 1 d . . . C96 C 0.6222(5) 0.5365(5) 0.9141(9) 0.047(5) Uani 1 1 d . . . C97 C 0.6224(4) 0.5754(5) 0.9086(8) 0.038(4) Uani 1 1 d . . . C98 C 0.5883(5) 0.5895(5) 0.8764(9) 0.046(5) Uani 1 1 d . . . C99 C 0.5677(5) 0.5577(6) 0.8680(9) 0.052(5) Uani 1 1 d . . . C100 C 0.5721(7) 0.4888(6) 0.8839(10) 0.073(7) Uani 1 1 d . . . H10A H 0.5638 0.4821 0.9234 0.109 Uiso 1 1 calc R . . H10B H 0.5914 0.4722 0.8725 0.109 Uiso 1 1 calc R . . H10C H 0.5518 0.4872 0.8548 0.109 Uiso 1 1 calc R . . C101 C 0.6493(6) 0.5132(6) 0.9394(9) 0.063(6) Uani 1 1 d . . . H10D H 0.6691 0.5279 0.9568 0.095 Uiso 1 1 calc R . . H10E H 0.6586 0.4974 0.9084 0.095 Uiso 1 1 calc R . . H10F H 0.6387 0.4984 0.9706 0.095 Uiso 1 1 calc R . . C102 C 0.6526(6) 0.5985(6) 0.9330(10) 0.070(7) Uani 1 1 d . . . H10G H 0.6752 0.5845 0.9343 0.105 Uiso 1 1 calc R . . H10H H 0.6470 0.6064 0.9733 0.105 Uiso 1 1 calc R . . H10I H 0.6553 0.6198 0.9074 0.105 Uiso 1 1 calc R . . C103 C 0.5799(7) 0.6293(6) 0.8684(12) 0.078(8) Uani 1 1 d . . . H10J H 0.5597 0.6322 0.8391 0.117 Uiso 1 1 calc R . . H10K H 0.6013 0.6419 0.8542 0.117 Uiso 1 1 calc R . . H10L H 0.5731 0.6397 0.9065 0.117 Uiso 1 1 calc R . . C104 C 0.5320(6) 0.5611(7) 0.8335(11) 0.077(7) Uani 1 1 d . . . H10M H 0.5215 0.5369 0.8269 0.115 Uiso 1 1 calc R . . H10N H 0.5360 0.5727 0.7950 0.115 Uiso 1 1 calc R . . H10O H 0.5152 0.5759 0.8562 0.115 Uiso 1 1 calc R . . O38 O 0.5903(10) 0.5853(11) 0.5220(19) 0.227(16) Uiso 1 1 d D . . C105 C 0.5809(12) 0.6012(12) 0.465(2) 0.165(17) Uiso 1 1 d D . . O39 O 0.2767(7) 0.5334(6) 0.4139(15) 0.162(12) Uani 1 1 d . . . C106 C 0.2964(9) 0.5668(9) 0.4382(15) 0.110(11) Uani 1 1 d . . . O40 O 0.7074(5) 0.4035(4) 0.8543(6) 0.076(5) Uani 1 1 d . . . C107 C 0.6724(8) 0.4098(9) 0.8727(18) 0.118(12) Uani 1 1 d . . . O41 O 0.7723(10) 0.2814(10) 0.5129(18) 0.215(15) Uiso 1 1 d D . . C108 C 0.8094(11) 0.2770(13) 0.531(2) 0.178(18) Uiso 1 1 d D . . O42 O 0.8757(10) 0.4436(7) 0.2894(11) 0.164(12) Uani 1 1 d . . . C109 C 0.8568(13) 0.4755(11) 0.2777(15) 0.153(18) Uani 1 1 d . . . O43 O 0.6719(5) 0.5214(6) 0.5959(8) 0.098(6) Uani 1 1 d . . . C110 C 0.6733(8) 0.5575(7) 0.6081(19) 0.116(13) Uani 1 1 d . . . O44 O 0.0361(3) 0.4788(4) 0.5026(6) 0.057(4) Uani 1 1 d . . . O45 O 0.5988(11) 0.7277(11) 0.373(2) 0.30(3) Uani 1 1 d . . . O46 O 0.9656(7) 0.4682(7) 0.2966(11) 0.147(9) Uani 1 1 d . . . O47 O 0.8815(5) 0.2607(4) 0.5291(9) 0.093(6) Uani 1 1 d D . . O48 O 0.9726(8) 0.1177(8) 0.9158(18) 0.196(14) 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 0.0440(4) 0.0335(4) 0.0187(3) -0.0007(3) -0.0023(3) 0.0029(3) Ir2 0.0459(4) 0.0547(5) 0.0237(4) 0.0010(3) -0.0067(3) -0.0003(3) Ir3 0.0708(5) 0.0511(5) 0.0226(4) 0.0127(3) 0.0088(3) 0.0084(4) Ir4 0.0435(4) 0.0450(4) 0.0228(4) -0.0113(3) 0.0014(3) -0.0043(3) Ag1 0.201(3) 0.132(2) 0.108(3) 0.0242(19) 0.020(2) 0.026(2) Ag2 0.0821(13) 0.0959(15) 0.0733(14) 0.0071(11) 0.0047(11) 0.0050(11) Ag3 0.162(4) 0.112(3) 0.113(3) 0.000 -0.002(3) 0.000 N1 0.040(8) 0.026(7) 0.041(9) -0.005(6) -0.002(7) -0.024(6) N2 0.054(9) 0.033(8) 0.025(7) 0.007(6) 0.015(6) 0.034(7) N3 0.042(7) 0.031(7) 0.012(6) 0.001(5) 0.012(5) -0.015(6) N4 0.037(6) 0.026(6) 0.021(6) -0.009(5) 0.002(5) 0.020(5) N5 0.12(2) 0.15(3) 0.055(17) 0.012(18) -0.009(16) -0.03(2) N6 0.056(11) 0.023(8) 0.074(14) 0.000(8) 0.003(10) 0.010(7) N7 0.19(3) 0.066(17) 0.10(2) -0.060(17) -0.02(2) 0.050(19) N9 0.051(13) 0.027(12) 0.08(2) 0.000 -0.004(13) 0.000 N11 0.084(19) 0.26(4) 0.11(3) -0.04(3) -0.011(18) 0.05(2) O1 0.030(5) 0.010(4) 0.036(6) 0.005(4) -0.009(5) -0.016(4) O2 0.041(6) 0.034(6) 0.033(7) 0.004(5) 0.005(5) 0.005(5) O3 0.100(11) 0.032(7) 0.024(7) 0.002(5) -0.005(7) 0.010(7) O4 0.096(11) 0.054(9) 0.024(7) 0.002(6) -0.024(7) -0.032(8) O5 0.049(7) 0.030(6) 0.022(6) 0.007(5) -0.003(5) 0.008(5) O6 0.046(7) 0.034(7) 0.045(8) 0.001(5) -0.017(6) 0.001(5) O7 0.079(10) 0.072(10) 0.032(8) -0.014(7) -0.015(7) -0.014(8) O8 0.161(19) 0.092(13) 0.047(11) 0.018(9) -0.004(12) -0.023(13) O9 0.052(7) 0.046(7) 0.006(5) 0.005(5) -0.004(5) -0.015(5) O10 0.048(7) 0.045(7) 0.035(7) 0.008(6) 0.017(6) -0.025(6) O11 0.061(8) 0.052(8) 0.038(8) 0.000(6) -0.018(6) 0.003(6) O12 0.109(12) 0.079(11) 0.027(8) 0.001(7) 0.019(8) -0.017(9) O13 0.035(6) 0.031(6) 0.019(6) -0.013(4) 0.005(4) 0.011(5) O14 0.067(8) 0.031(6) 0.036(7) -0.007(5) -0.005(6) 0.000(6) O15 0.066(8) 0.044(7) 0.040(8) 0.015(6) -0.006(6) 0.009(6) O16 0.064(8) 0.066(9) 0.022(7) -0.008(6) -0.006(6) 0.020(7) O17 0.22(3) 0.23(3) 0.088(19) 0.046(19) -0.052(19) -0.14(3) O18 0.107(18) 0.17(2) 0.17(3) 0.00(2) 0.045(18) -0.012(16) O19 0.15(2) 0.122(18) 0.075(15) -0.015(13) -0.021(14) -0.026(15) O20 0.055(8) 0.020(6) 0.085(12) 0.020(7) 0.001(8) -0.020(6) O21 0.076(10) 0.060(9) 0.072(11) -0.023(8) -0.026(9) 0.015(8) O22 0.081(12) 0.091(12) 0.059(11) 0.026(9) 0.011(9) 0.005(9) O23 0.19(3) 0.17(3) 0.24(4) -0.08(3) 0.15(3) -0.08(2) O24 0.30(4) 0.101(19) 0.15(3) -0.025(18) 0.09(3) 0.03(2) O25 0.17(2) 0.15(2) 0.10(2) -0.051(17) 0.020(16) 0.047(17) O29 0.057(8) 0.097(11) 0.036(8) -0.028(8) 0.012(6) -0.005(8) O30 0.11(2) 0.14(3) 0.064(18) 0.000 0.001(15) 0.000 O37 0.105(19) 0.39(5) 0.25(4) 0.15(4) -0.03(2) 0.06(3) C1 0.019(7) 0.034(9) 0.033(9) 0.000(7) -0.002(6) 0.008(6) C2 0.048(9) 0.028(8) 0.011(7) 0.000(6) -0.006(7) 0.000(7) C3 0.040(9) 0.021(8) 0.015(7) -0.005(6) -0.007(6) 0.003(7) C4 0.043(10) 0.035(9) 0.031(9) 0.006(7) -0.008(8) 0.022(8) C5 0.041(9) 0.030(9) 0.024(9) 0.008(7) -0.001(7) 0.016(7) C6 0.058(11) 0.038(10) 0.018(8) 0.014(7) 0.003(8) -0.002(8) C7 0.043(9) 0.027(8) 0.011(7) -0.002(6) -0.008(6) 0.016(7) C8 0.060(11) 0.035(9) 0.030(10) -0.009(8) -0.026(9) 0.016(8) C9 0.031(8) 0.042(9) 0.009(7) 0.001(6) -0.011(6) 0.004(7) C10 0.056(10) 0.026(8) 0.010(7) 0.001(6) -0.012(7) -0.014(7) C11 0.061(12) 0.054(12) 0.037(11) -0.001(9) -0.025(10) 0.016(10) C12 0.061(11) 0.038(10) 0.020(9) 0.004(7) -0.010(8) 0.010(9) C13 0.032(8) 0.040(9) 0.020(8) -0.012(7) -0.009(7) 0.011(7) C14 0.069(12) 0.033(9) 0.015(8) 0.012(7) -0.012(8) -0.011(8) C15 0.058(11) 0.064(14) 0.019(9) 0.006(9) -0.008(8) 0.020(10) C16 0.12(2) 0.10(2) 0.076(19) 0.032(15) -0.067(17) -0.048(17) C17 0.073(13) 0.028(9) 0.050(12) 0.006(8) 0.008(10) 0.000(9) C18 0.025(8) 0.064(12) 0.031(10) 0.007(9) -0.006(7) -0.014(8) C19 0.042(9) 0.040(10) 0.017(8) -0.006(7) -0.014(7) 0.010(8) C20 0.046(10) 0.059(12) 0.023(9) 0.019(8) -0.010(8) -0.019(9) C21 0.091(14) 0.029(9) 0.025(10) -0.005(7) -0.016(9) -0.005(9) C22 0.076(14) 0.061(13) 0.022(10) -0.007(9) 0.000(9) 0.013(11) C23 0.044(10) 0.059(12) 0.047(12) -0.003(10) -0.005(9) -0.011(9) C24 0.043(9) 0.051(11) 0.016(8) 0.004(7) -0.006(7) 0.012(8) C25 0.037(9) 0.071(13) 0.018(8) 0.006(8) 0.013(7) 0.011(9) C26 0.044(9) 0.053(11) 0.008(7) 0.007(7) 0.002(7) -0.005(8) C27 0.063(11) 0.043(10) 0.021(9) 0.000(8) 0.008(8) -0.004(9) C28 0.046(11) 0.087(16) 0.025(10) 0.015(10) -0.014(8) -0.009(11) C29 0.057(11) 0.027(9) 0.034(10) 0.000(7) 0.005(8) -0.006(8) C30 0.114(18) 0.049(12) 0.030(11) -0.008(9) 0.027(11) -0.034(12) C31 0.076(15) 0.075(16) 0.031(11) 0.022(10) 0.022(11) 0.003(12) C32 0.15(3) 0.09(2) 0.13(3) 0.06(2) -0.06(2) -0.03(2) C33 0.062(11) 0.036(10) 0.018(8) -0.009(7) 0.008(8) -0.010(8) C34 0.050(10) 0.015(7) 0.036(10) -0.004(7) -0.025(8) 0.013(7) C35 0.029(8) 0.024(8) 0.026(8) 0.003(6) -0.001(6) 0.008(6) C36 0.037(9) 0.043(10) 0.036(10) 0.001(8) 0.002(8) 0.003(8) C37 0.057(10) 0.021(8) 0.022(8) 0.000(6) -0.002(7) -0.026(7) C38 0.058(11) 0.025(9) 0.036(10) -0.010(7) -0.001(8) 0.005(8) C39 0.046(9) 0.018(8) 0.029(9) 0.007(6) 0.007(7) 0.003(7) C40 0.051(10) 0.034(9) 0.009(7) -0.005(6) 0.010(7) -0.008(7) C41 0.034(8) 0.030(8) 0.021(8) -0.004(6) 0.002(6) 0.011(7) C42 0.057(10) 0.026(8) 0.015(8) -0.004(6) -0.017(7) 0.006(7) C43 0.062(11) 0.032(9) 0.027(9) -0.006(7) -0.002(8) -0.003(8) C44 0.051(10) 0.022(8) 0.031(9) 0.009(7) 0.009(8) 0.003(7) C45 0.048(10) 0.040(10) 0.021(9) -0.011(7) -0.003(7) 0.020(8) C46 0.100(16) 0.035(10) 0.037(11) -0.011(8) -0.023(11) -0.008(10) C47 0.057(10) 0.022(8) 0.012(7) -0.005(6) 0.005(7) -0.011(7) C48 0.086(15) 0.030(10) 0.054(13) -0.015(9) 0.025(11) -0.004(10) C49 0.039(9) 0.052(11) 0.029(10) -0.012(8) -0.005(7) 0.008(8) C50 0.055(10) 0.024(8) 0.004(7) -0.001(6) -0.003(6) -0.011(7) C51 0.052(10) 0.059(12) 0.023(9) -0.010(8) 0.003(8) -0.010(9) C52 0.019(7) 0.044(10) 0.044(11) 0.005(8) -0.003(7) 0.015(7) C53 0.043(9) 0.037(10) 0.037(10) 0.000(8) -0.023(8) 0.022(8) C54 0.051(10) 0.028(9) 0.037(10) 0.015(7) -0.019(9) 0.004(8) C55 0.050(9) 0.040(9) 0.006(7) -0.007(6) -0.009(6) 0.003(7) C56 0.018(7) 0.035(8) 0.013(7) -0.001(6) -0.007(6) 0.010(6) C57 0.027(7) 0.033(8) 0.010(7) -0.003(6) 0.005(6) -0.003(6) C58 0.031(8) 0.024(8) 0.025(8) 0.004(6) -0.014(7) 0.014(6) C59 0.038(9) 0.042(10) 0.016(8) -0.008(7) 0.002(6) -0.006(7) C60 0.065(12) 0.061(13) 0.018(9) -0.001(9) 0.000(8) -0.009(10) C61 0.060(11) 0.033(9) 0.020(9) 0.007(7) -0.010(8) -0.003(8) C62 0.039(9) 0.068(13) 0.027(10) 0.004(9) -0.007(8) 0.007(9) C63 0.046(10) 0.030(9) 0.025(9) -0.001(7) -0.005(8) 0.000(7) C64 0.064(13) 0.064(14) 0.082(17) -0.007(12) -0.043(13) -0.001(11) C65 0.050(10) 0.027(9) 0.031(9) 0.010(7) 0.013(8) 0.010(7) C66 0.053(10) 0.042(10) 0.016(8) -0.006(7) -0.013(7) 0.019(8) C67 0.043(10) 0.037(10) 0.056(13) -0.038(9) -0.006(9) 0.000(8) C68 0.041(10) 0.035(9) 0.038(10) -0.008(8) -0.009(8) 0.014(8) C69 0.051(11) 0.047(11) 0.037(11) -0.015(8) -0.025(9) 0.022(9) C70 0.059(11) 0.047(11) 0.027(10) -0.002(8) 0.010(8) 0.015(9) C71 0.060(12) 0.064(13) 0.050(13) -0.015(10) -0.004(10) 0.026(11) C72 0.058(14) 0.093(18) 0.070(17) -0.011(14) 0.000(12) -0.001(12) C73 0.063(13) 0.048(12) 0.057(14) -0.007(10) -0.015(11) -0.003(10) C74 0.090(15) 0.049(12) 0.034(11) 0.017(9) 0.004(10) 0.010(11) C75 0.101(18) 0.053(13) 0.043(13) 0.013(10) -0.009(12) 0.033(13) C76 0.057(14) 0.14(2) 0.031(12) 0.009(14) 0.001(10) 0.016(15) C77 0.040(11) 0.12(2) 0.055(15) 0.026(15) -0.017(11) -0.001(13) C78 0.032(10) 0.114(19) 0.034(11) 0.011(12) 0.003(8) -0.036(11) C79 0.045(12) 0.13(2) 0.039(12) -0.010(13) 0.005(9) -0.043(13) C80 0.22(5) 0.13(3) 0.30(7) 0.00(4) -0.21(5) 0.07(3) C81 0.040(15) 0.44(8) 0.08(3) -0.02(4) -0.025(16) 0.01(3) C82 0.15(3) 0.061(17) 0.20(4) 0.04(2) -0.09(3) -0.068(18) C83 0.12(3) 0.23(4) 0.12(3) -0.09(3) -0.08(2) 0.11(3) C84 0.11(2) 0.17(3) 0.056(18) 0.056(19) -0.017(16) -0.04(2) C85 0.063(12) 0.059(12) 0.025(10) 0.011(9) 0.004(9) 0.027(10) C86 0.081(15) 0.052(12) 0.039(12) 0.008(9) 0.022(11) 0.012(11) C87 0.052(12) 0.068(15) 0.091(19) 0.050(14) 0.023(12) 0.004(11) C88 0.075(15) 0.072(16) 0.061(16) 0.041(13) -0.017(13) 0.018(13) C89 0.16(3) 0.09(2) 0.034(14) 0.018(13) -0.002(16) 0.02(2) C90 0.084(17) 0.11(2) 0.074(18) 0.054(16) 0.021(14) 0.038(15) C91 0.24(4) 0.056(17) 0.17(4) 0.08(2) -0.12(3) -0.08(2) C92 0.12(3) 0.16(3) 0.08(2) 0.02(2) -0.034(19) -0.01(2) C93 0.23(4) 0.11(2) 0.028(14) 0.018(15) -0.025(19) -0.02(2) C94 0.105(19) 0.10(2) 0.046(15) 0.008(13) -0.029(14) -0.009(17) C95 0.037(10) 0.078(15) 0.048(12) -0.028(11) 0.026(9) -0.025(10) C96 0.044(10) 0.056(12) 0.043(12) -0.002(9) 0.022(9) -0.007(9) C97 0.026(8) 0.040(10) 0.049(11) -0.011(8) 0.002(7) 0.007(7) C98 0.045(10) 0.041(10) 0.054(13) -0.026(9) 0.013(9) 0.015(9) C99 0.030(9) 0.086(16) 0.042(12) -0.019(10) 0.010(8) -0.001(10) C100 0.13(2) 0.055(13) 0.038(13) -0.002(10) 0.022(13) -0.024(14) C101 0.079(14) 0.089(16) 0.024(10) 0.016(10) 0.017(10) 0.000(13) C102 0.078(15) 0.086(16) 0.050(14) -0.017(12) 0.046(12) -0.007(13) C103 0.078(16) 0.082(17) 0.074(18) -0.044(14) -0.004(13) 0.015(13) C104 0.058(13) 0.105(19) 0.070(17) -0.015(14) 0.033(12) -0.015(13) O39 0.16(2) 0.081(15) 0.24(4) -0.030(18) -0.07(2) -0.005(15) C106 0.14(3) 0.10(2) 0.08(2) 0.026(18) -0.02(2) -0.01(2) O40 0.137(15) 0.058(9) 0.033(8) 0.016(7) 0.012(9) -0.010(9) C107 0.09(2) 0.12(3) 0.15(3) 0.01(2) 0.05(2) 0.024(19) O42 0.28(4) 0.13(2) 0.073(17) -0.017(14) 0.00(2) -0.01(2) C109 0.25(5) 0.15(3) 0.06(2) 0.03(2) 0.05(3) 0.10(3) O43 0.077(11) 0.161(19) 0.056(11) -0.019(12) -0.008(9) 0.025(12) C110 0.080(18) 0.057(16) 0.21(4) -0.05(2) 0.00(2) -0.031(14) O44 0.059(8) 0.084(10) 0.029(7) 0.019(7) 0.018(6) 0.001(7) O45 0.26(4) 0.25(4) 0.41(7) 0.05(4) 0.24(5) 0.07(3) O46 0.17(2) 0.18(2) 0.095(18) -0.027(16) 0.079(16) -0.004(19) O47 0.098(12) 0.039(9) 0.140(18) 0.005(9) 0.001(12) 0.020(8) O48 0.16(2) 0.16(3) 0.26(5) -0.02(3) 0.06(3) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O2 2.046(11) . ? Ir1 N4 2.083(11) . ? Ir1 O1 2.084(8) . ? Ir1 C69 2.129(18) . ? Ir1 C68 2.144(16) . ? Ir1 C67 2.145(16) . ? Ir1 C66 2.154(17) . ? Ir1 C65 2.166(16) . ? Ir2 O6 2.033(13) . ? Ir2 O5 2.082(10) . ? Ir2 N1 2.104(11) . ? Ir2 C77 2.11(2) . ? Ir2 C76 2.11(2) . ? Ir2 C79 2.15(2) . ? Ir2 C75 2.16(2) . ? Ir2 C78 2.17(2) . ? Ir3 O10 2.050(12) . ? Ir3 O9 2.081(10) . ? Ir3 C88 2.09(2) . ? Ir3 N2 2.124(12) . ? Ir3 C87 2.14(2) . ? Ir3 C86 2.15(2) . ? Ir3 C85 2.174(17) . ? Ir3 C89 2.23(3) . ? Ir4 N3 2.056(11) . ? Ir4 O13 2.058(9) . ? Ir4 O14 2.059(12) . ? Ir4 C97 2.098(18) . ? Ir4 C98 2.135(16) . ? Ir4 C95 2.152(19) . ? Ir4 C96 2.16(2) . ? Ir4 C99 2.171(18) . ? Ag1 O37 2.27(4) . ? Ag1 O17 2.38(3) . ? Ag1 O12 2.431(17) . ? Ag1 O8 2.49(2) 6_566 ? Ag2 O23 2.31(3) . ? Ag2 O26 2.46(3) . ? Ag2 O20 2.483(12) . ? Ag2 O27 2.60(3) . ? Ag3 O31 2.44(4) . ? Ag3 O31 2.44(4) 2_655 ? Ag3 O29 2.516(17) 2_655 ? Ag3 O29 2.516(17) . ? Ag3 O32 2.56(5) . ? Ag3 O32 2.56(5) 2_655 ? N1 C9 1.32(2) . ? N1 C13 1.339(19) . ? N2 C29 1.34(2) . ? N2 C25 1.37(2) . ? N3 C45 1.33(2) . ? N3 C41 1.400(19) . ? N4 C57 1.325(19) . ? N4 C61 1.37(2) . ? N5 O18 1.12(3) . ? N5 O19 1.24(3) . ? N5 O17 1.28(3) . ? N6 O22 1.21(2) . ? N6 O21 1.27(2) . ? N6 O20 1.31(2) . ? N7 O24 1.18(3) . ? N7 O25 1.21(4) . ? N7 O23 1.23(4) . ? N8 O26 1.08(6) . ? N8 O27 1.37(6) . ? N8 O28 1.49(6) . ? N9 O29 1.255(16) . ? N9 O29 1.255(16) 2_655 ? N9 O30 1.30(3) . ? N10 O33 1.27(2) . ? N10 O32 1.28(2) . ? N10 O31 1.28(2) . ? N11 O36 1.248(17) . ? N11 O34 1.274(16) . ? N11 O35 1.280(17) . ? O1 C2 1.290(17) . ? O2 C4 1.284(19) . ? O3 C6 1.40(2) . ? O4 C15 1.18(2) . ? O5 C18 1.25(2) . ? O6 C20 1.318(19) . ? O7 C22 1.45(2) . ? O8 C31 1.24(3) . ? O8 Ag1 2.49(2) 6_565 ? O9 C34 1.24(2) . ? O10 C36 1.30(2) . ? O11 C38 1.41(2) . ? O12 C47 1.25(2) . ? O13 C50 1.286(16) . ? O14 C52 1.30(2) . ? O15 C54 1.36(2) . ? O16 C63 1.19(2) . ? C1 C2 1.45(2) . ? C2 C3 1.42(2) . ? C3 C4 1.43(2) . ? C3 C8 1.47(2) . ? C4 C5 1.51(2) . ? C5 C6 1.59(2) . ? C6 C7 1.45(2) . ? C6 C14 1.55(2) . ? C7 C15 1.56(2) . ? C7 C8 1.56(2) . ? C8 C10 1.49(2) . ? C9 C10 1.38(2) . ? C10 C11 1.46(2) . ? C11 C12 1.32(3) . ? C12 C13 1.37(2) . ? C15 C16 1.51(3) . ? C17 C18 1.51(3) . ? C18 C19 1.44(2) . ? C19 C20 1.38(2) . ? C19 C24 1.55(2) . ? C20 C21 1.48(3) . ? C21 C22 1.55(2) . ? C22 C23 1.56(3) . ? C22 C30 1.57(3) . ? C23 C31 1.47(3) . ? C23 C24 1.50(3) . ? C24 C26 1.51(2) . ? C25 C26 1.36(2) . ? C26 C27 1.42(2) . ? C27 C28 1.45(3) . ? C28 C29 1.31(3) . ? C31 C32 1.42(4) . ? C33 C34 1.53(2) . ? C34 C35 1.48(2) . ? C35 C36 1.38(2) . ? C35 C40 1.55(2) . ? C36 C37 1.47(2) . ? C37 C38 1.53(2) . ? C38 C39 1.51(2) . ? C38 C46 1.57(2) . ? C39 C47 1.45(2) . ? C39 C40 1.55(2) . ? C40 C42 1.51(2) . ? C41 C42 1.36(2) . ? C42 C43 1.39(2) . ? C43 C44 1.36(2) . ? C44 C45 1.43(2) . ? C47 C48 1.51(2) . ? C49 C50 1.45(2) . ? C50 C51 1.40(2) . ? C51 C52 1.38(2) . ? C51 C56 1.53(2) . ? C52 C53 1.49(2) . ? C53 C54 1.53(2) . ? C54 C55 1.57(2) . ? C54 C62 1.59(2) . ? C55 C63 1.50(2) . ? C55 C56 1.594(18) . ? C56 C58 1.55(2) . ? C57 C58 1.40(2) . ? C58 C59 1.39(2) . ? C59 C60 1.34(2) . ? C60 C61 1.32(3) . ? C63 C64 1.46(2) . ? C65 C70 1.43(2) . ? C65 C69 1.44(2) . ? C65 C66 1.50(2) . ? C66 C67 1.42(2) . ? C66 C71 1.43(3) . ? C67 C72 1.34(3) . ? C67 C68 1.53(3) . ? C68 C69 1.34(2) . ? C68 C73 1.53(2) . ? C69 C74 1.52(3) . ? C75 C80 1.31(4) . ? C75 C79 1.47(3) . ? C75 C76 1.49(3) . ? C76 C77 1.33(4) . ? C76 C81 1.44(4) . ? C77 C78 1.45(3) . ? C77 C82 1.51(3) . ? C78 C79 1.41(3) . ? C78 C83 1.53(4) . ? C79 C84 1.39(3) . ? C85 C86 1.43(3) . ? C85 C89 1.49(3) . ? C85 C90 1.52(3) . ? C86 C87 1.43(3) . ? C86 C91 1.54(4) . ? C87 C88 1.42(3) . ? C87 C92 1.48(4) . ? C88 C89 1.42(4) . ? C88 C93 1.56(4) . ? C89 C94 1.47(4) . ? C95 C99 1.41(3) . ? C95 C100 1.45(3) . ? C95 C96 1.52(3) . ? C96 C101 1.42(3) . ? C96 C97 1.44(3) . ? C97 C102 1.49(3) . ? C97 C98 1.52(2) . ? C98 C99 1.41(3) . ? C98 C103 1.51(3) . ? C99 C104 1.51(3) . ? O38 C105 1.447(19) . ? O39 C106 1.52(4) . ? O40 C107 1.39(3) . ? O41 C108 1.419(19) . ? O42 C109 1.38(4) . ? O43 C110 1.36(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ir1 N4 84.5(5) . . ? O2 Ir1 O1 83.0(4) . . ? N4 Ir1 O1 79.7(5) . . ? O2 Ir1 C69 148.5(5) . . ? N4 Ir1 C69 126.9(6) . . ? O1 Ir1 C69 99.4(6) . . ? O2 Ir1 C68 154.2(6) . . ? N4 Ir1 C68 100.0(5) . . ? O1 Ir1 C68 122.7(6) . . ? C69 Ir1 C68 36.7(7) . . ? O2 Ir1 C67 112.5(7) . . ? N4 Ir1 C67 103.2(6) . . ? O1 Ir1 C67 164.3(6) . . ? C69 Ir1 C67 66.3(8) . . ? C68 Ir1 C67 41.7(7) . . ? O2 Ir1 C66 94.1(5) . . ? N4 Ir1 C66 137.3(6) . . ? O1 Ir1 C66 142.6(5) . . ? C69 Ir1 C66 65.0(7) . . ? C68 Ir1 C66 65.3(6) . . ? C67 Ir1 C66 38.6(6) . . ? O2 Ir1 C65 109.8(5) . . ? N4 Ir1 C65 165.1(6) . . ? O1 Ir1 C65 105.6(5) . . ? C69 Ir1 C65 39.2(6) . . ? C68 Ir1 C65 65.3(6) . . ? C67 Ir1 C65 68.0(6) . . ? C66 Ir1 C65 40.6(6) . . ? O6 Ir2 O5 83.3(4) . . ? O6 Ir2 N1 85.1(5) . . ? O5 Ir2 N1 82.0(5) . . ? O6 Ir2 C77 114.0(8) . . ? O5 Ir2 C77 104.6(8) . . ? N1 Ir2 C77 160.2(8) . . ? O6 Ir2 C76 93.6(7) . . ? O5 Ir2 C76 134.7(9) . . ? N1 Ir2 C76 142.9(9) . . ? C77 Ir2 C76 36.7(10) . . ? O6 Ir2 C79 147.6(8) . . ? O5 Ir2 C79 129.0(8) . . ? N1 Ir2 C79 95.6(7) . . ? C77 Ir2 C79 65.5(8) . . ? C76 Ir2 C79 66.7(8) . . ? O6 Ir2 C75 108.7(7) . . ? O5 Ir2 C75 166.4(7) . . ? N1 Ir2 C75 104.9(8) . . ? C77 Ir2 C75 65.0(10) . . ? C76 Ir2 C75 40.8(10) . . ? C79 Ir2 C75 39.8(9) . . ? O6 Ir2 C78 153.6(6) . . ? O5 Ir2 C78 101.4(8) . . ? N1 Ir2 C78 121.2(6) . . ? C77 Ir2 C78 39.6(8) . . ? C76 Ir2 C78 64.5(8) . . ? C79 Ir2 C78 38.0(9) . . ? C75 Ir2 C78 64.9(9) . . ? O10 Ir3 O9 84.5(4) . . ? O10 Ir3 C88 154.6(8) . . ? O9 Ir3 C88 120.9(8) . . ? O10 Ir3 N2 83.1(5) . . ? O9 Ir3 N2 82.1(5) . . ? C88 Ir3 N2 100.1(8) . . ? O10 Ir3 C87 115.5(8) . . ? O9 Ir3 C87 160.0(8) . . ? C88 Ir3 C87 39.1(10) . . ? N2 Ir3 C87 100.9(7) . . ? O10 Ir3 C86 95.6(7) . . ? O9 Ir3 C86 143.6(7) . . ? C88 Ir3 C86 64.0(9) . . ? N2 Ir3 C86 134.2(7) . . ? C87 Ir3 C86 39.0(8) . . ? O10 Ir3 C85 109.9(6) . . ? O9 Ir3 C85 107.4(6) . . ? C88 Ir3 C85 64.3(8) . . ? N2 Ir3 C85 164.2(6) . . ? C87 Ir3 C85 65.8(8) . . ? C86 Ir3 C85 38.7(8) . . ? O10 Ir3 C89 148.1(9) . . ? O9 Ir3 C89 96.3(9) . . ? C88 Ir3 C89 38.2(10) . . ? N2 Ir3 C89 128.6(9) . . ? C87 Ir3 C89 66.1(11) . . ? C86 Ir3 C89 65.3(10) . . ? C85 Ir3 C89 39.4(9) . . ? N3 Ir4 O13 82.1(5) . . ? N3 Ir4 O14 83.6(5) . . ? O13 Ir4 O14 84.8(4) . . ? N3 Ir4 C97 98.0(6) . . ? O13 Ir4 C97 125.5(5) . . ? O14 Ir4 C97 149.7(5) . . ? N3 Ir4 C98 103.4(7) . . ? O13 Ir4 C98 166.5(6) . . ? O14 Ir4 C98 108.0(6) . . ? C97 Ir4 C98 42.1(7) . . ? N3 Ir4 C95 164.1(6) . . ? O13 Ir4 C95 104.7(7) . . ? O14 Ir4 C95 111.1(6) . . ? C97 Ir4 C95 66.3(7) . . ? C98 Ir4 C95 66.9(8) . . ? N3 Ir4 C96 124.4(6) . . ? O13 Ir4 C96 96.9(6) . . ? O14 Ir4 C96 152.0(6) . . ? C97 Ir4 C96 39.4(7) . . ? C98 Ir4 C96 69.7(8) . . ? C95 Ir4 C96 41.3(7) . . ? N3 Ir4 C99 138.6(7) . . ? O13 Ir4 C99 139.0(7) . . ? O14 Ir4 C99 94.4(6) . . ? C97 Ir4 C99 64.5(7) . . ? C98 Ir4 C99 38.1(7) . . ? C95 Ir4 C99 38.0(8) . . ? C96 Ir4 C99 66.2(7) . . ? O37 Ag1 O17 110.8(14) . . ? O37 Ag1 O12 101.8(9) . . ? O17 Ag1 O12 103.5(9) . . ? O37 Ag1 O8 91.2(8) . 6_566 ? O17 Ag1 O8 85.8(9) . 6_566 ? O12 Ag1 O8 159.9(6) . 6_566 ? O23 Ag2 O26 133.9(11) . . ? O23 Ag2 O20 89.0(9) . . ? O26 Ag2 O20 136.6(9) . . ? O23 Ag2 O27 94.6(14) . . ? O26 Ag2 O27 51.6(11) . . ? O20 Ag2 O27 149.3(8) . . ? O31 Ag3 O31 143.6(18) . 2_655 ? O31 Ag3 O29 132.5(10) . 2_655 ? O31 Ag3 O29 83.7(10) 2_655 2_655 ? O31 Ag3 O29 83.7(10) . . ? O31 Ag3 O29 132.5(10) 2_655 . ? O29 Ag3 O29 50.5(6) 2_655 . ? O31 Ag3 O32 45.1(14) . . ? O31 Ag3 O32 103.7(14) 2_655 . ? O29 Ag3 O32 158.3(11) 2_655 . ? O29 Ag3 O32 115.3(11) . . ? O31 Ag3 O32 103.7(14) . 2_655 ? O31 Ag3 O32 45.1(14) 2_655 2_655 ? O29 Ag3 O32 115.3(11) 2_655 2_655 ? O29 Ag3 O32 158.3(11) . 2_655 ? O32 Ag3 O32 83(2) . 2_655 ? C9 N1 C13 117.9(13) . . ? C9 N1 Ir2 118.8(10) . . ? C13 N1 Ir2 123.4(12) . . ? C29 N2 C25 119.3(13) . . ? C29 N2 Ir3 122.9(11) . . ? C25 N2 Ir3 117.9(11) . . ? C45 N3 C41 114.6(13) . . ? C45 N3 Ir4 126.3(11) . . ? C41 N3 Ir4 119.0(10) . . ? C57 N4 C61 117.3(12) . . ? C57 N4 Ir1 118.7(10) . . ? C61 N4 Ir1 124.0(11) . . ? O18 N5 O19 111(4) . . ? O18 N5 O17 128(4) . . ? O19 N5 O17 121(3) . . ? O22 N6 O21 120(2) . . ? O22 N6 O20 119.6(18) . . ? O21 N6 O20 120.5(17) . . ? O24 N7 O25 119(4) . . ? O24 N7 O23 117(4) . . ? O25 N7 O23 124(3) . . ? O26 N8 O27 127(7) . . ? O26 N8 O28 106(6) . . ? O27 N8 O28 100(5) . . ? O29 N9 O29 117(2) . 2_655 ? O29 N9 O30 121.3(12) . . ? O29 N9 O30 121.3(12) 2_655 . ? O33 N10 O32 137(6) . . ? O33 N10 O31 124(6) . . ? O32 N10 O31 97(4) . . ? O36 N11 O34 121(2) . . ? O36 N11 O35 121(2) . . ? O34 N11 O35 117.2(19) . . ? C2 O1 Ir1 127.3(9) . . ? C4 O2 Ir1 126.1(11) . . ? C18 O5 Ir2 126.4(12) . . ? C20 O6 Ir2 125.3(11) . . ? C31 O8 Ag1 138.4(16) . 6_565 ? C34 O9 Ir3 126.7(10) . . ? C36 O10 Ir3 125.3(10) . . ? C47 O12 Ag1 132.1(13) . . ? C50 O13 Ir4 128.0(10) . . ? C52 O14 Ir4 125.0(10) . . ? N5 O17 Ag1 110(2) . . ? N6 O20 Ag2 96.4(11) . . ? N7 O23 Ag2 107(2) . . ? N8 O26 Ag2 93(4) . . ? N8 O27 Ag2 80(3) . . ? N9 O29 Ag3 96.0(12) . . ? N10 O31 Ag3 109(4) . . ? N10 O32 Ag3 103(4) . . ? O1 C2 C3 125.9(14) . . ? O1 C2 C1 114.9(13) . . ? C3 C2 C1 119.0(13) . . ? C2 C3 C4 118.4(13) . . ? C2 C3 C8 119.5(15) . . ? C4 C3 C8 121.7(14) . . ? O2 C4 C3 126.8(14) . . ? O2 C4 C5 113.3(15) . . ? C3 C4 C5 120.0(13) . . ? C4 C5 C6 114.0(13) . . ? O3 C6 C7 116.1(14) . . ? O3 C6 C14 107.7(14) . . ? C7 C6 C14 117.4(15) . . ? O3 C6 C5 106.6(13) . . ? C7 C6 C5 104.9(13) . . ? C14 C6 C5 102.6(13) . . ? C6 C7 C15 110.8(13) . . ? C6 C7 C8 114.3(13) . . ? C15 C7 C8 106.7(14) . . ? C3 C8 C10 113.0(13) . . ? C3 C8 C7 113.0(15) . . ? C10 C8 C7 108.5(12) . . ? N1 C9 C10 125.6(14) . . ? C9 C10 C11 114.1(16) . . ? C9 C10 C8 124.9(14) . . ? C11 C10 C8 121.0(15) . . ? C12 C11 C10 119.7(19) . . ? C11 C12 C13 120.9(17) . . ? N1 C13 C12 121.7(15) . . ? O4 C15 C16 122.3(17) . . ? O4 C15 C7 123.2(15) . . ? C16 C15 C7 114.5(17) . . ? O5 C18 C19 125.2(16) . . ? O5 C18 C17 114.5(16) . . ? C19 C18 C17 120.3(15) . . ? C20 C19 C18 120.8(16) . . ? C20 C19 C24 118.3(15) . . ? C18 C19 C24 119.9(14) . . ? O6 C20 C19 123.5(17) . . ? O6 C20 C21 111.1(17) . . ? C19 C20 C21 125.4(15) . . ? C20 C21 C22 113.7(16) . . ? O7 C22 C21 107.5(17) . . ? O7 C22 C23 109.1(15) . . ? C21 C22 C23 106.7(14) . . ? O7 C22 C30 112.7(15) . . ? C21 C22 C30 107.8(17) . . ? C23 C22 C30 112.6(17) . . ? C31 C23 C24 113.0(16) . . ? C31 C23 C22 109.7(17) . . ? C24 C23 C22 112.0(16) . . ? C23 C24 C26 108.8(15) . . ? C23 C24 C19 113.2(14) . . ? C26 C24 C19 111.8(12) . . ? C26 C25 N2 122.3(16) . . ? C25 C26 C27 119.5(16) . . ? C25 C26 C24 121.8(14) . . ? C27 C26 C24 118.3(15) . . ? C26 C27 C28 114.6(16) . . ? C29 C28 C27 122.7(17) . . ? C28 C29 N2 121.4(16) . . ? O8 C31 C32 117(2) . . ? O8 C31 C23 123(2) . . ? C32 C31 C23 121(2) . . ? O9 C34 C35 125.1(15) . . ? O9 C34 C33 115.9(13) . . ? C35 C34 C33 118.8(15) . . ? C36 C35 C34 120.7(15) . . ? C36 C35 C40 122.8(14) . . ? C34 C35 C40 115.9(13) . . ? O10 C36 C35 125.4(16) . . ? O10 C36 C37 113.4(14) . . ? C35 C36 C37 121.1(16) . . ? C36 C37 C38 113.8(13) . . ? O11 C38 C39 111.9(14) . . ? O11 C38 C37 110.6(14) . . ? C39 C38 C37 108.4(14) . . ? O11 C38 C46 109.5(14) . . ? C39 C38 C46 108.4(15) . . ? C37 C38 C46 108.0(14) . . ? C47 C39 C38 111.8(14) . . ? C47 C39 C40 110.6(12) . . ? C38 C39 C40 109.8(13) . . ? C42 C40 C39 107.3(12) . . ? C42 C40 C35 111.5(12) . . ? C39 C40 C35 110.9(12) . . ? C42 C41 N3 124.6(14) . . ? C41 C42 C43 117.9(15) . . ? C41 C42 C40 121.8(13) . . ? C43 C42 C40 120.3(16) . . ? C44 C43 C42 120.3(18) . . ? C43 C44 C45 117.5(15) . . ? N3 C45 C44 124.3(15) . . ? O12 C47 C39 122.8(15) . . ? O12 C47 C48 116.9(16) . . ? C39 C47 C48 119.8(14) . . ? O13 C50 C51 124.5(15) . . ? O13 C50 C49 113.6(13) . . ? C51 C50 C49 121.8(14) . . ? C52 C51 C50 123.9(16) . . ? C52 C51 C56 119.4(14) . . ? C50 C51 C56 116.7(15) . . ? O14 C52 C51 124.7(14) . . ? O14 C52 C53 112.4(13) . . ? C51 C52 C53 122.3(16) . . ? C52 C53 C54 114.3(13) . . ? O15 C54 C53 113.6(15) . . ? O15 C54 C55 109.1(14) . . ? C53 C54 C55 106.6(13) . . ? O15 C54 C62 113.0(14) . . ? C53 C54 C62 108.4(14) . . ? C55 C54 C62 105.6(13) . . ? C63 C55 C54 114.4(13) . . ? C63 C55 C56 110.4(13) . . ? C54 C55 C56 107.2(12) . . ? C51 C56 C58 111.9(12) . . ? C51 C56 C55 116.4(12) . . ? C58 C56 C55 105.8(11) . . ? N4 C57 C58 123.2(14) . . ? C59 C58 C57 116.3(14) . . ? C59 C58 C56 122.6(13) . . ? C57 C58 C56 121.2(14) . . ? C60 C59 C58 119.5(16) . . ? C61 C60 C59 122.0(18) . . ? C60 C61 N4 121.6(16) . . ? O16 C63 C64 123.3(18) . . ? O16 C63 C55 121.2(15) . . ? C64 C63 C55 115.3(17) . . ? C70 C65 C69 132.9(16) . . ? C70 C65 C66 124.0(14) . . ? C69 C65 C66 103.0(14) . . ? C70 C65 Ir1 128.2(13) . . ? C69 C65 Ir1 69.0(9) . . ? C66 C65 Ir1 69.2(9) . . ? C67 C66 C71 121.0(18) . . ? C67 C66 C65 111.1(15) . . ? C71 C66 C65 127.7(15) . . ? C67 C66 Ir1 70.3(9) . . ? C71 C66 Ir1 122.8(12) . . ? C65 C66 Ir1 70.1(9) . . ? C72 C67 C66 132(2) . . ? C72 C67 C68 123.0(19) . . ? C66 C67 C68 103.7(15) . . ? C72 C67 Ir1 131.7(15) . . ? C66 C67 Ir1 71.0(10) . . ? C68 C67 Ir1 69.1(9) . . ? C69 C68 C67 108.8(15) . . ? C69 C68 C73 129.7(19) . . ? C67 C68 C73 121.5(16) . . ? C69 C68 Ir1 71.0(10) . . ? C67 C68 Ir1 69.2(9) . . ? C73 C68 Ir1 125.4(12) . . ? C68 C69 C65 113.3(19) . . ? C68 C69 C74 126.3(17) . . ? C65 C69 C74 120.4(16) . . ? C68 C69 Ir1 72.3(11) . . ? C65 C69 Ir1 71.8(10) . . ? C74 C69 Ir1 122.9(13) . . ? C80 C75 C79 125(4) . . ? C80 C75 C76 130(4) . . ? C79 C75 C76 105(2) . . ? C80 C75 Ir2 127(2) . . ? C79 C75 Ir2 69.7(13) . . ? C76 C75 Ir2 67.9(11) . . ? C77 C76 C81 123(3) . . ? C77 C76 C75 109(2) . . ? C81 C76 C75 128(3) . . ? C77 C76 Ir2 71.5(14) . . ? C81 C76 Ir2 124.1(17) . . ? C75 C76 Ir2 71.3(13) . . ? C76 C77 C78 111(2) . . ? C76 C77 C82 127(3) . . ? C78 C77 C82 122(3) . . ? C76 C77 Ir2 71.8(16) . . ? C78 C77 Ir2 72.3(12) . . ? C82 C77 Ir2 122.0(16) . . ? C79 C78 C77 108(2) . . ? C79 C78 C83 127(2) . . ? C77 C78 C83 126(3) . . ? C79 C78 Ir2 70.3(12) . . ? C77 C78 Ir2 68.0(12) . . ? C83 C78 Ir2 123.5(15) . . ? C84 C79 C78 125(3) . . ? C84 C79 C75 127(3) . . ? C78 C79 C75 107.9(19) . . ? C84 C79 Ir2 129.3(16) . . ? C78 C79 Ir2 71.6(14) . . ? C75 C79 Ir2 70.5(12) . . ? C86 C85 C89 108(2) . . ? C86 C85 C90 131(2) . . ? C89 C85 C90 121(2) . . ? C86 C85 Ir3 69.8(10) . . ? C89 C85 Ir3 72.3(13) . . ? C90 C85 Ir3 126.7(14) . . ? C85 C86 C87 110.0(19) . . ? C85 C86 C91 119(2) . . ? C87 C86 C91 131(3) . . ? C85 C86 Ir3 71.6(11) . . ? C87 C86 Ir3 70.2(11) . . ? C91 C86 Ir3 120.7(15) . . ? C88 C87 C86 104(2) . . ? C88 C87 C92 127(3) . . ? C86 C87 C92 129(3) . . ? C88 C87 Ir3 68.3(12) . . ? C86 C87 Ir3 70.8(12) . . ? C92 C87 Ir3 127.6(17) . . ? C87 C88 C89 115(3) . . ? C87 C88 C93 130(3) . . ? C89 C88 C93 115(3) . . ? C87 C88 Ir3 72.6(14) . . ? C89 C88 Ir3 76.4(16) . . ? C93 C88 Ir3 126.9(15) . . ? C88 C89 C94 129(3) . . ? C88 C89 C85 103(3) . . ? C94 C89 C85 128(3) . . ? C88 C89 Ir3 65.4(15) . . ? C94 C89 Ir3 122.1(17) . . ? C85 C89 Ir3 68.3(12) . . ? C99 C95 C100 128.0(19) . . ? C99 C95 C96 107.5(16) . . ? C100 C95 C96 124(2) . . ? C99 C95 Ir4 71.7(12) . . ? C100 C95 Ir4 129.5(14) . . ? C96 C95 Ir4 69.5(10) . . ? C101 C96 C97 129.1(18) . . ? C101 C96 C95 127.4(19) . . ? C97 C96 C95 103.5(17) . . ? C101 C96 Ir4 125.5(13) . . ? C97 C96 Ir4 68.1(11) . . ? C95 C96 Ir4 69.2(11) . . ? C96 C97 C102 122.9(17) . . ? C96 C97 C98 112.0(15) . . ? C102 C97 C98 125.1(17) . . ? C96 C97 Ir4 72.4(10) . . ? C102 C97 Ir4 125.9(13) . . ? C98 C97 Ir4 70.2(9) . . ? C99 C98 C103 133.3(18) . . ? C99 C98 C97 102.3(16) . . ? C103 C98 C97 123.5(17) . . ? C99 C98 Ir4 72.3(10) . . ? C103 C98 Ir4 130.0(16) . . ? C97 C98 Ir4 67.7(9) . . ? C98 C99 C95 114.3(16) . . ? C98 C99 C104 117(2) . . ? C95 C99 C104 127.7(19) . . ? C98 C99 Ir4 69.6(10) . . ? C95 C99 Ir4 70.2(10) . . ? C104 C99 Ir4 120.9(14) . . ? 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 0.500 0.000 0.055 3326.2 996.2 2 0.333 0.047 0.315 7.8 -0.6 3 0.667 0.047 0.185 7.8 -0.3 4 0.320 0.089 0.326 5.6 -1.3 5 0.680 0.089 0.174 5.5 -0.9 6 0.000 0.500 0.738 3326.1 996.2 7 0.178 0.417 0.676 6.7 0.6 8 0.822 0.417 0.824 6.7 -0.6 9 0.165 0.459 0.687 6.6 0.8 10 0.835 0.459 0.813 6.7 0.3 11 0.167 0.547 0.185 7.8 -0.3 12 0.833 0.547 0.315 7.8 -0.6 13 0.180 0.589 0.174 5.5 -0.9 14 0.820 0.589 0.326 5.6 -1.3 15 0.322 0.917 0.824 6.7 -0.6 16 0.678 0.917 0.676 6.7 0.6 17 0.335 0.959 0.813 6.7 0.3 18 0.665 0.959 0.687 6.6 0.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 5.610 _refine_diff_density_min -3.090 _refine_diff_density_rms 0.356