# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _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' data_1 _database_code_depnum_ccdc_archive 'CCDC 864531' #TrackingRef 'Ir-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H120 Cl4 F12 Ir4 N12 O14 S4' _chemical_formula_weight 3052.98 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' Ir Ir -1.4442 7.9887 '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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 38.315(4) _cell_length_b 14.4214(14) _cell_length_c 22.307(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.0090(10) _cell_angle_gamma 90.00 _cell_volume 11959(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5269 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.17 _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 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6000 _exptl_absorpt_coefficient_mu 4.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5405 _exptl_absorpt_correction_T_max 0.6520 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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_% 5.21 _diffrn_reflns_number 33546 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.01 _reflns_number_total 12890 _reflns_number_gt 8061 _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. ; _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^)+(0.0910P)^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 12890 _refine_ls_number_parameters 683 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1740 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.064 _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 0.404897(11) 0.19035(2) 0.855682(18) 0.04315(13) Uani 1 1 d . . . Ir2 Ir 0.388063(10) 0.53673(2) 0.957572(18) 0.04152(13) Uani 1 1 d . . . N1 N 0.3825(2) 0.3270(5) 0.8294(4) 0.0422(19) Uani 1 1 d . . . N2 N 0.4285(2) 0.2717(5) 0.9375(3) 0.0412(18) Uani 1 1 d . . . N3 N 0.42053(19) 0.4119(5) 0.9782(3) 0.0389(17) Uani 1 1 d . . . N4 N 0.3756(2) 0.4685(5) 0.8685(4) 0.0396(18) Uani 1 1 d . . . N5 N 0.3610(2) 0.1786(5) 0.8980(4) 0.052(2) Uani 1 1 d . . . N6 N 0.1532(2) 0.0496(6) 1.0233(4) 0.054(2) Uani 1 1 d . . . S1 S 0.19611(9) 0.3211(2) 0.80133(17) 0.0732(9) Uani 1 1 d . . . S2 S 0.40953(16) 0.8969(4) 0.0537(2) 0.1213(18) Uani 1 1 d D . . F1 F 0.2272(3) 0.3451(12) 0.7125(6) 0.183(5) Uani 1 1 d U . . F2 F 0.2181(4) 0.4636(9) 0.7512(7) 0.193(6) Uani 1 1 d . . . F3 F 0.2604(2) 0.3745(8) 0.7983(5) 0.125(3) Uani 1 1 d . . . F4 F 0.4365(5) 0.9668(8) 0.1584(7) 0.218(8) Uani 1 1 d D . . F5 F 0.4402(7) 1.0382(14) 0.0798(11) 0.321(11) Uani 1 1 d DU . . F6 F 0.3944(5) 1.0452(11) 0.1030(8) 0.234(7) Uani 1 1 d DU . . O1 O 0.1621(3) 0.3280(8) 0.7594(6) 0.127(4) Uani 1 1 d . . . O2 O 0.2089(3) 0.2328(7) 0.8146(7) 0.140(5) Uani 1 1 d . . . O3 O 0.1991(4) 0.3737(10) 0.8552(6) 0.148(5) Uani 1 1 d . . . O4 O 0.3776(4) 0.8563(14) 0.0766(7) 0.217(9) Uani 1 1 d D . . O5 O 0.3886(6) 0.9243(14) -0.0041(8) 0.241(8) Uani 1 1 d U . . O6 O 0.4351(4) 0.8387(10) 0.0570(8) 0.175(6) Uani 1 1 d U . . C1 C 0.4464(3) 0.2693(6) 0.9989(5) 0.043(2) Uani 1 1 d . . . C2 C 0.4663(3) 0.2013(7) 1.0348(5) 0.052(3) Uani 1 1 d . . . H2 H 0.4695 0.1431 1.0179 0.062 Uiso 1 1 calc R . . C3 C 0.4818(3) 0.2209(9) 1.0976(5) 0.071(3) Uani 1 1 d . . . H3 H 0.4957 0.1752 1.1225 0.085 Uiso 1 1 calc R . . C4 C 0.4769(3) 0.3066(8) 1.1236(5) 0.063(3) Uani 1 1 d . . . H4 H 0.4869 0.3177 1.1658 0.075 Uiso 1 1 calc R . . C5 C 0.4572(3) 0.3752(8) 1.0867(5) 0.053(3) Uani 1 1 d . . . H5 H 0.4546 0.4335 1.1039 0.064 Uiso 1 1 calc R . . C6 C 0.4416(2) 0.3591(6) 1.0254(4) 0.040(2) Uani 1 1 d . . . C7 C 0.4145(2) 0.3574(6) 0.9304(4) 0.039(2) Uani 1 1 d . . . C8 C 0.3910(3) 0.3848(6) 0.8744(5) 0.042(2) Uani 1 1 d . . . C9 C 0.3535(3) 0.4655(6) 0.8096(5) 0.042(2) Uani 1 1 d . . . C10 C 0.3318(3) 0.5298(8) 0.7748(5) 0.063(3) Uani 1 1 d . . . H10 H 0.3295 0.5892 0.7908 0.075 Uiso 1 1 calc R . . C11 C 0.3130(3) 0.5067(9) 0.7154(6) 0.074(4) Uani 1 1 d . . . H11 H 0.2980 0.5510 0.6910 0.089 Uiso 1 1 calc R . . C12 C 0.3161(3) 0.4192(9) 0.6914(5) 0.068(3) Uani 1 1 d . . . H12 H 0.3030 0.4048 0.6511 0.082 Uiso 1 1 calc R . . C13 C 0.3380(3) 0.3536(8) 0.7255(5) 0.062(3) Uani 1 1 d . . . H13 H 0.3397 0.2942 0.7092 0.075 Uiso 1 1 calc R . . C14 C 0.3576(3) 0.3756(7) 0.7841(4) 0.046(2) Uani 1 1 d . . . C15 C 0.2737(4) 0.1436(11) 0.9858(7) 0.100(5) Uani 1 1 d . . . H15 H 0.2793 0.1213 1.0266 0.121 Uiso 1 1 calc R . . C16 C 0.2396(4) 0.1608(14) 0.9596(7) 0.124(7) Uani 1 1 d . . . H16 H 0.2341 0.1978 0.9239 0.149 Uiso 1 1 calc R . . C17 C 0.3661(3) 0.1492(8) 0.9566(5) 0.058(3) Uani 1 1 d . . . H17 H 0.3895 0.1340 0.9790 0.069 Uiso 1 1 calc R . . C18 C 0.3384(3) 0.1409(9) 0.9846(6) 0.078(4) Uani 1 1 d . . . H18 H 0.3432 0.1230 1.0263 0.093 Uiso 1 1 calc R . . C19 C 0.3048(3) 0.1572(8) 0.9546(5) 0.060(3) Uani 1 1 d . . . C20 C 0.2989(3) 0.1908(8) 0.8944(6) 0.067(3) Uani 1 1 d . . . H20 H 0.2756 0.2068 0.8720 0.080 Uiso 1 1 calc R . . C21 C 0.3274(3) 0.1998(7) 0.8685(5) 0.055(3) Uani 1 1 d . . . H21 H 0.3232 0.2222 0.8278 0.066 Uiso 1 1 calc R . . C22 C 0.1481(3) 0.0898(7) 0.9675(5) 0.056(3) Uani 1 1 d . . . H22 H 0.1247 0.0924 0.9418 0.067 Uiso 1 1 calc R . . C23 C 0.1753(3) 0.1260(7) 0.9475(6) 0.064(3) Uani 1 1 d . . . H23 H 0.1708 0.1531 0.9081 0.076 Uiso 1 1 calc R . . C24 C 0.2098(3) 0.1243(8) 0.9841(6) 0.060(3) Uani 1 1 d . . . C25 C 0.2145(3) 0.0901(8) 1.0424(5) 0.062(3) Uani 1 1 d . . . H25 H 0.2372 0.0934 1.0705 0.074 Uiso 1 1 calc R . . C26 C 0.1859(3) 0.0511(7) 1.0597(5) 0.056(3) Uani 1 1 d . . . H26 H 0.1898 0.0242 1.0991 0.068 Uiso 1 1 calc R . . C27 C 0.4038(4) 0.0444(7) 0.8298(6) 0.067(4) Uani 1 1 d . . . C28 C 0.3926(3) 0.0999(7) 0.7771(5) 0.061(3) Uani 1 1 d . . . C29 C 0.4235(3) 0.1635(7) 0.7733(5) 0.060(3) Uani 1 1 d . . . C30 C 0.4519(3) 0.1440(8) 0.8281(5) 0.059(3) Uani 1 1 d . . . C31 C 0.4404(4) 0.0707(8) 0.8622(5) 0.066(3) Uani 1 1 d . . . C32 C 0.3817(5) -0.0285(8) 0.8502(7) 0.097(5) Uani 1 1 d . . . H32A H 0.3565 -0.0109 0.8384 0.145 Uiso 1 1 calc R . . H32B H 0.3891 -0.0352 0.8948 0.145 Uiso 1 1 calc R . . H32C H 0.3849 -0.0870 0.8308 0.145 Uiso 1 1 calc R . . C33 C 0.3594(4) 0.0865(9) 0.7297(6) 0.086(4) Uani 1 1 d . . . H33A H 0.3603 0.0275 0.7092 0.130 Uiso 1 1 calc R . . H33B H 0.3566 0.1362 0.6996 0.130 Uiso 1 1 calc R . . H33C H 0.3391 0.0870 0.7487 0.130 Uiso 1 1 calc R . . C34 C 0.4239(4) 0.2300(8) 0.7246(5) 0.072(4) Uani 1 1 d . . . H34A H 0.4404 0.2801 0.7409 0.108 Uiso 1 1 calc R . . H34B H 0.3999 0.2549 0.7089 0.108 Uiso 1 1 calc R . . H34C H 0.4317 0.1995 0.6913 0.108 Uiso 1 1 calc R . . C35 C 0.4885(4) 0.1887(10) 0.8414(9) 0.108(6) Uani 1 1 d . . . H35A H 0.5068 0.1414 0.8436 0.162 Uiso 1 1 calc R . . H35B H 0.4928 0.2214 0.8806 0.162 Uiso 1 1 calc R . . H35C H 0.4896 0.2322 0.8087 0.162 Uiso 1 1 calc R . . C36 C 0.4638(4) 0.0244(9) 0.9173(7) 0.099(5) Uani 1 1 d . . . H36A H 0.4747 -0.0303 0.9042 0.148 Uiso 1 1 calc R . . H36B H 0.4494 0.0064 0.9457 0.148 Uiso 1 1 calc R . . H36C H 0.4825 0.0669 0.9378 0.148 Uiso 1 1 calc R . . C37 C 0.4289(3) 0.6400(7) 0.9888(5) 0.057(3) Uani 1 1 d . . . C38 C 0.4070(3) 0.6703(6) 0.9340(6) 0.052(3) Uani 1 1 d . . . C39 C 0.3711(3) 0.6796(7) 0.9404(6) 0.058(3) Uani 1 1 d . . . C40 C 0.3714(4) 0.6544(7) 1.0025(6) 0.069(4) Uani 1 1 d . . . C41 C 0.4076(4) 0.6299(8) 1.0336(5) 0.069(3) Uani 1 1 d . . . C42 C 0.4692(3) 0.6238(9) 1.0018(7) 0.089(4) Uani 1 1 d . . . H42A H 0.4770 0.6294 0.9637 0.133 Uiso 1 1 calc R . . H42B H 0.4748 0.5621 1.0188 0.133 Uiso 1 1 calc R . . H42C H 0.4816 0.6695 1.0313 0.133 Uiso 1 1 calc R . . C43 C 0.4178(5) 0.6923(9) 0.8738(6) 0.092(5) Uani 1 1 d . . . H43A H 0.4205 0.7588 0.8703 0.138 Uiso 1 1 calc R . . H43B H 0.3992 0.6703 0.8390 0.138 Uiso 1 1 calc R . . H43C H 0.4403 0.6618 0.8739 0.138 Uiso 1 1 calc R . . C44 C 0.3397(4) 0.7224(9) 0.8950(7) 0.088(4) Uani 1 1 d . . . H44A H 0.3177 0.6908 0.8975 0.132 Uiso 1 1 calc R . . H44B H 0.3431 0.7164 0.8535 0.132 Uiso 1 1 calc R . . H44C H 0.3379 0.7875 0.9048 0.132 Uiso 1 1 calc R . . C45 C 0.3396(5) 0.6540(10) 1.0311(9) 0.130(8) Uani 1 1 d . . . H45A H 0.3410 0.6004 1.0578 0.196 Uiso 1 1 calc R . . H45B H 0.3175 0.6511 0.9987 0.196 Uiso 1 1 calc R . . H45C H 0.3397 0.7101 1.0551 0.196 Uiso 1 1 calc R . . C46 C 0.4220(5) 0.6075(9) 1.1017(6) 0.117(6) Uani 1 1 d . . . H46A H 0.4371 0.6580 1.1218 0.175 Uiso 1 1 calc R . . H46B H 0.4360 0.5508 1.1060 0.175 Uiso 1 1 calc R . . H46C H 0.4020 0.5995 1.1209 0.175 Uiso 1 1 calc R . . C47 C 0.2264(4) 0.3768(11) 0.7653(7) 0.088(4) Uani 1 1 d . . . C48 C 0.4188(5) 0.9835(11) 0.1044(7) 0.123(6) Uiso 1 1 d D . . C49 C 0.5959(6) 0.2248(15) 0.3147(13) 0.186(12) Uani 1 1 d . . . H49A H 0.5914 0.2155 0.3557 0.224 Uiso 1 1 calc R . . H49B H 0.6174 0.1894 0.3123 0.224 Uiso 1 1 calc R . . Cl1 Cl 0.55511(19) 0.1850(5) 0.2514(3) 0.173(3) Uani 1 1 d . . . Cl2 Cl 0.60200(19) 0.3418(6) 0.3018(3) 0.181(3) Uani 1 1 d . . . C50 C 0.2702(15) 0.951(3) -0.0604(18) 0.47(4) Uiso 1 1 d D . . H50A H 0.2711 0.9122 -0.0955 0.698 Uiso 1 1 calc R . . H50B H 0.2895 0.9964 -0.0541 0.698 Uiso 1 1 calc R . . H50C H 0.2473 0.9829 -0.0684 0.698 Uiso 1 1 calc R . . C51 C 0.2747(6) 0.8910(15) -0.0025(10) 0.157(8) Uiso 1 1 d D . . H51A H 0.2527 0.8535 -0.0100 0.189 Uiso 1 1 calc R . . H51B H 0.2941 0.8477 -0.0046 0.189 Uiso 1 1 calc R . . C53 C 0.2605(14) 0.868(4) 0.1578(19) 0.45(3) Uiso 1 1 d D . . H53A H 0.2580 0.8095 0.1781 0.673 Uiso 1 1 calc R . . H53B H 0.2374 0.8986 0.1462 0.673 Uiso 1 1 calc R . . H53C H 0.2776 0.9069 0.1859 0.673 Uiso 1 1 calc R . . C52 C 0.2743(7) 0.8486(18) 0.0995(10) 0.185(10) Uiso 1 1 d D . . H52A H 0.2967 0.8135 0.1135 0.222 Uiso 1 1 calc R . . H52B H 0.2569 0.8058 0.0742 0.222 Uiso 1 1 calc R . . O7 O 0.2813(11) 0.915(2) 0.0591(14) 0.46(2) 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 0.0497(3) 0.0332(2) 0.0457(2) -0.00226(16) 0.00985(18) -0.00674(17) Ir2 0.0413(2) 0.0390(2) 0.0486(2) -0.00181(16) 0.01952(17) -0.00115(16) N1 0.048(5) 0.024(4) 0.053(5) -0.002(4) 0.010(4) -0.003(3) N2 0.040(5) 0.043(4) 0.041(5) -0.008(4) 0.011(3) -0.007(4) N3 0.036(4) 0.034(4) 0.047(5) 0.000(4) 0.011(3) -0.005(3) N4 0.040(5) 0.029(4) 0.054(5) -0.001(3) 0.018(4) 0.007(3) N5 0.052(6) 0.049(5) 0.052(5) 0.007(4) 0.008(4) -0.015(4) N6 0.037(5) 0.058(5) 0.073(6) 0.004(5) 0.025(4) -0.004(4) S1 0.058(2) 0.078(2) 0.076(2) 0.0224(18) 0.0023(16) -0.0022(16) S2 0.150(5) 0.134(4) 0.074(3) 0.019(3) 0.016(3) 0.066(4) F1 0.160(10) 0.291(14) 0.115(8) -0.037(9) 0.068(7) -0.040(10) F2 0.163(12) 0.153(12) 0.262(17) 0.112(11) 0.052(11) -0.008(9) F3 0.060(6) 0.186(10) 0.127(8) 0.018(7) 0.019(5) -0.025(6) F4 0.314(19) 0.111(9) 0.156(12) -0.002(8) -0.086(12) 0.024(10) F5 0.376(19) 0.264(16) 0.351(18) 0.056(13) 0.142(15) -0.153(14) F6 0.229(10) 0.224(10) 0.232(10) -0.042(8) 0.025(8) 0.099(8) O1 0.070(7) 0.164(11) 0.133(10) 0.070(8) -0.003(6) 0.005(7) O2 0.101(9) 0.072(7) 0.225(14) 0.058(8) -0.004(8) 0.009(6) O3 0.166(13) 0.187(13) 0.109(10) -0.048(9) 0.064(9) -0.020(10) O4 0.153(14) 0.36(3) 0.152(14) -0.130(15) 0.055(11) -0.059(15) O5 0.337(18) 0.216(14) 0.137(12) 0.018(12) -0.007(12) 0.053(14) O6 0.136(10) 0.133(10) 0.222(13) -0.086(9) -0.021(9) 0.031(8) C1 0.042(6) 0.042(5) 0.048(6) -0.001(5) 0.014(4) -0.002(4) C2 0.047(6) 0.038(6) 0.063(7) -0.004(5) -0.002(5) 0.000(5) C3 0.065(8) 0.082(9) 0.057(8) 0.000(7) -0.004(6) 0.008(7) C4 0.076(9) 0.064(7) 0.047(7) -0.009(6) 0.012(6) 0.000(6) C5 0.054(7) 0.061(7) 0.048(6) -0.002(5) 0.019(5) 0.010(5) C6 0.041(6) 0.044(5) 0.039(5) -0.004(4) 0.018(4) -0.001(4) C7 0.042(6) 0.035(5) 0.042(5) 0.002(4) 0.014(4) -0.001(4) C8 0.041(6) 0.030(5) 0.058(6) 0.003(5) 0.018(5) -0.008(4) C9 0.040(6) 0.042(5) 0.045(6) 0.005(4) 0.012(4) -0.004(4) C10 0.055(7) 0.067(8) 0.063(8) 0.013(6) 0.009(6) 0.002(6) C11 0.065(9) 0.075(9) 0.072(9) 0.022(7) -0.005(6) 0.020(7) C12 0.075(9) 0.076(9) 0.050(7) 0.005(6) 0.008(6) 0.008(7) C13 0.072(8) 0.058(7) 0.052(7) -0.007(6) 0.005(6) -0.012(6) C14 0.050(6) 0.046(6) 0.042(6) 0.004(5) 0.011(5) -0.009(5) C15 0.051(9) 0.130(13) 0.122(12) 0.060(10) 0.022(8) -0.021(8) C16 0.056(9) 0.219(19) 0.096(11) 0.081(12) 0.016(8) -0.030(11) C17 0.053(7) 0.066(7) 0.050(7) 0.014(5) 0.005(5) -0.012(6) C18 0.058(8) 0.105(10) 0.069(8) 0.031(7) 0.014(6) -0.027(7) C19 0.046(7) 0.080(8) 0.056(7) 0.015(6) 0.013(5) -0.015(6) C20 0.040(7) 0.071(8) 0.088(9) 0.013(7) 0.011(6) -0.007(5) C21 0.047(7) 0.054(6) 0.061(7) 0.007(5) 0.008(5) -0.007(5) C22 0.049(7) 0.066(7) 0.054(7) 0.025(6) 0.017(5) 0.000(5) C23 0.066(8) 0.057(7) 0.072(8) 0.013(6) 0.024(6) 0.003(6) C24 0.053(7) 0.057(7) 0.075(8) 0.013(6) 0.024(6) -0.004(5) C25 0.040(6) 0.071(8) 0.074(8) 0.012(6) 0.014(5) 0.002(5) C26 0.033(6) 0.072(7) 0.065(7) 0.010(6) 0.013(5) -0.006(5) C27 0.116(12) 0.036(6) 0.056(7) -0.010(5) 0.035(7) -0.011(6) C28 0.086(9) 0.046(6) 0.053(7) -0.014(5) 0.019(6) -0.007(6) C29 0.085(9) 0.048(6) 0.053(7) -0.015(5) 0.029(6) 0.005(6) C30 0.060(8) 0.059(7) 0.056(7) -0.011(6) 0.008(5) 0.012(6) C31 0.092(10) 0.054(7) 0.049(7) 0.003(6) 0.015(6) 0.016(7) C32 0.166(16) 0.035(7) 0.091(11) -0.007(6) 0.036(10) -0.032(8) C33 0.104(11) 0.059(8) 0.085(10) -0.036(7) 0.000(8) -0.011(7) C34 0.106(11) 0.063(7) 0.061(8) -0.003(6) 0.046(7) -0.004(7) C35 0.062(9) 0.096(11) 0.180(17) -0.026(11) 0.059(10) -0.004(8) C36 0.121(13) 0.075(10) 0.087(11) -0.002(8) -0.003(9) 0.056(9) C37 0.063(8) 0.047(6) 0.060(7) -0.015(5) 0.012(6) -0.011(5) C38 0.053(7) 0.032(5) 0.078(8) 0.005(5) 0.029(6) -0.003(5) C39 0.073(8) 0.035(6) 0.067(8) -0.002(5) 0.018(6) 0.008(5) C40 0.092(10) 0.039(6) 0.090(9) -0.009(6) 0.051(8) 0.010(6) C41 0.109(11) 0.048(7) 0.050(7) -0.012(5) 0.016(7) 0.015(7) C42 0.069(10) 0.060(8) 0.121(12) -0.011(8) -0.010(8) -0.021(7) C43 0.143(14) 0.067(9) 0.083(10) 0.016(7) 0.060(9) -0.002(8) C44 0.087(11) 0.067(8) 0.105(12) 0.014(8) 0.011(8) 0.012(8) C45 0.134(15) 0.086(10) 0.22(2) -0.005(12) 0.135(16) 0.026(10) C46 0.23(2) 0.063(9) 0.055(9) -0.029(7) 0.022(10) -0.002(10) C47 0.096(12) 0.089(11) 0.077(10) 0.020(8) 0.017(8) 0.014(9) C49 0.123(18) 0.151(18) 0.32(4) 0.10(2) 0.13(2) 0.027(15) Cl1 0.165(6) 0.230(8) 0.127(5) 0.011(4) 0.041(4) -0.023(5) Cl2 0.169(6) 0.254(8) 0.132(5) -0.011(5) 0.057(4) -0.019(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 Ir1 N5 2.125(8) . ? Ir1 C28 2.143(10) . ? Ir1 C30 2.147(11) . ? Ir1 C29 2.161(10) . ? Ir1 N1 2.172(7) . ? Ir1 N2 2.174(7) . ? Ir1 C31 2.179(11) . ? Ir1 C27 2.180(10) . ? Ir2 N6 2.135(8) 7_557 ? Ir2 C40 2.146(10) . ? Ir2 C37 2.149(11) . ? Ir2 C41 2.151(11) . ? Ir2 N4 2.164(8) . ? Ir2 C39 2.166(10) . ? Ir2 C38 2.167(9) . ? Ir2 N3 2.174(7) . ? N1 C8 1.284(12) . ? N1 C14 1.399(12) . ? N2 C7 1.342(11) . ? N2 C1 1.376(12) . ? N3 C7 1.298(11) . ? N3 C6 1.389(12) . ? N4 C8 1.335(11) . ? N4 C9 1.381(12) . ? N5 C21 1.332(13) . ? N5 C17 1.344(12) . ? N6 C26 1.318(13) . ? N6 C22 1.345(12) . ? N6 Ir2 2.135(8) 7_557 ? S1 O2 1.371(10) . ? S1 O3 1.401(11) . ? S1 O1 1.411(10) . ? S1 C47 1.757(16) . ? S2 O6 1.280(13) . ? S2 O5 1.399(17) . ? S2 O4 1.550(13) . ? S2 C48 1.664(14) . ? F1 C47 1.271(17) . ? F2 C47 1.310(17) . ? F3 C47 1.332(17) . ? F4 C48 1.255(15) . ? F5 C48 1.346(15) . ? F6 C48 1.285(15) . ? C1 C2 1.373(13) . ? C1 C6 1.455(12) . ? C2 C3 1.411(15) . ? C2 H2 0.9400 . ? C3 C4 1.397(15) . ? C3 H3 0.9400 . ? C4 C5 1.387(15) . ? C4 H4 0.9400 . ? C5 C6 1.373(13) . ? C5 H5 0.9400 . ? C7 C8 1.408(13) . ? C9 C10 1.358(14) . ? C9 C14 1.440(13) . ? C10 C11 1.388(17) . ? C10 H10 0.9400 . ? C11 C12 1.386(17) . ? C11 H11 0.9400 . ? C12 C13 1.368(16) . ? C12 H12 0.9400 . ? C13 C14 1.377(14) . ? C13 H13 0.9400 . ? C15 C16 1.318(18) . ? C15 C19 1.530(15) . ? C15 H15 0.9400 . ? C16 C24 1.477(15) . ? C16 H16 0.9400 . ? C17 C18 1.361(15) . ? C17 H17 0.9400 . ? C18 C19 1.319(16) . ? C18 H18 0.9400 . ? C19 C20 1.394(15) . ? C20 C21 1.359(14) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 C23 1.335(14) . ? C22 H22 0.9400 . ? C23 C24 1.375(16) . ? C23 H23 0.9400 . ? C24 C25 1.363(15) . ? C25 C26 1.367(13) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C27 C28 1.401(16) . ? C27 C31 1.462(18) . ? C27 C32 1.490(16) . ? C28 C33 1.459(17) . ? C28 C29 1.515(16) . ? C29 C30 1.453(16) . ? C29 C34 1.453(15) . ? C30 C31 1.433(16) . ? C30 C35 1.507(17) . ? C31 C36 1.494(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C38 1.375(15) . ? C37 C41 1.440(16) . ? C37 C42 1.521(16) . ? C38 C39 1.422(15) . ? C38 C43 1.532(15) . ? C39 C40 1.430(16) . ? C39 C44 1.507(17) . ? C40 C41 1.438(18) . ? C40 C45 1.504(16) . ? C41 C46 1.521(17) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C49 Cl2 1.74(2) . ? C49 Cl1 1.92(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.530(19) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 O7 1.382(19) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C53 C52 1.543(19) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C52 O7 1.387(19) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? 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 Ir1 C28 105.9(4) . . ? N5 Ir1 C30 155.8(4) . . ? C28 Ir1 C30 67.0(4) . . ? N5 Ir1 C29 145.4(4) . . ? C28 Ir1 C29 41.2(4) . . ? C30 Ir1 C29 39.4(4) . . ? N5 Ir1 N1 83.6(3) . . ? C28 Ir1 N1 109.7(4) . . ? C30 Ir1 N1 120.6(4) . . ? C29 Ir1 N1 97.1(4) . . ? N5 Ir1 N2 83.2(3) . . ? C28 Ir1 N2 168.3(4) . . ? C30 Ir1 N2 101.7(4) . . ? C29 Ir1 N2 130.9(4) . . ? N1 Ir1 N2 78.1(3) . . ? N5 Ir1 C31 117.1(4) . . ? C28 Ir1 C31 65.3(5) . . ? C30 Ir1 C31 38.7(4) . . ? C29 Ir1 C31 65.5(4) . . ? N1 Ir1 C31 159.3(4) . . ? N2 Ir1 C31 104.2(4) . . ? N5 Ir1 C27 94.3(4) . . ? C28 Ir1 C27 37.8(4) . . ? C30 Ir1 C27 65.6(5) . . ? C29 Ir1 C27 65.9(4) . . ? N1 Ir1 C27 145.4(4) . . ? N2 Ir1 C27 136.1(4) . . ? C31 Ir1 C27 39.2(5) . . ? N6 Ir2 C40 92.8(4) 7_557 . ? N6 Ir2 C37 148.8(4) 7_557 . ? C40 Ir2 C37 64.9(5) . . ? N6 Ir2 C41 109.9(4) 7_557 . ? C40 Ir2 C41 39.1(5) . . ? C37 Ir2 C41 39.1(4) . . ? N6 Ir2 N4 84.8(3) 7_557 . ? C40 Ir2 N4 139.8(4) . . ? C37 Ir2 N4 126.4(3) . . ? C41 Ir2 N4 164.8(4) . . ? N6 Ir2 C39 112.6(4) 7_557 . ? C40 Ir2 C39 38.7(4) . . ? C37 Ir2 C39 64.0(4) . . ? C41 Ir2 C39 65.0(5) . . ? N4 Ir2 C39 106.3(4) . . ? N6 Ir2 C38 150.9(4) 7_557 . ? C40 Ir2 C38 64.3(4) . . ? C37 Ir2 C38 37.1(4) . . ? C41 Ir2 C38 64.0(4) . . ? N4 Ir2 C38 101.2(4) . . ? C39 Ir2 C38 38.3(4) . . ? N6 Ir2 N3 83.6(3) 7_557 . ? C40 Ir2 N3 140.9(4) . . ? C37 Ir2 N3 99.9(4) . . ? C41 Ir2 N3 106.2(4) . . ? N4 Ir2 N3 78.7(3) . . ? C39 Ir2 N3 163.1(4) . . ? C38 Ir2 N3 125.4(3) . . ? C8 N1 C14 103.8(8) . . ? C8 N1 Ir1 111.7(7) . . ? C14 N1 Ir1 143.6(6) . . ? C7 N2 C1 103.3(7) . . ? C7 N2 Ir1 109.0(6) . . ? C1 N2 Ir1 145.9(7) . . ? C7 N3 C6 104.3(7) . . ? C7 N3 Ir2 110.4(6) . . ? C6 N3 Ir2 144.3(6) . . ? C8 N4 C9 102.7(8) . . ? C8 N4 Ir2 109.1(6) . . ? C9 N4 Ir2 146.7(6) . . ? C21 N5 C17 116.6(9) . . ? C21 N5 Ir1 122.4(7) . . ? C17 N5 Ir1 120.9(7) . . ? C26 N6 C22 117.8(9) . . ? C26 N6 Ir2 121.8(7) . 7_557 ? C22 N6 Ir2 119.1(7) . 7_557 ? O2 S1 O3 111.6(9) . . ? O2 S1 O1 115.7(8) . . ? O3 S1 O1 113.5(9) . . ? O2 S1 C47 106.3(8) . . ? O3 S1 C47 102.6(8) . . ? O1 S1 C47 105.7(7) . . ? O6 S2 O5 119.9(12) . . ? O6 S2 O4 112.8(12) . . ? O5 S2 O4 95.1(12) . . ? O6 S2 C48 114.7(9) . . ? O5 S2 C48 113.2(11) . . ? O4 S2 C48 96.6(9) . . ? C2 C1 N2 132.2(9) . . ? C2 C1 C6 120.4(9) . . ? N2 C1 C6 107.5(8) . . ? C1 C2 C3 118.5(10) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 121.5(11) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.5(11) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 120.9(10) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 N3 134.1(9) . . ? C5 C6 C1 119.2(9) . . ? N3 C6 C1 106.7(8) . . ? N3 C7 N2 118.3(8) . . ? N3 C7 C8 120.5(8) . . ? N2 C7 C8 121.0(8) . . ? N1 C8 N4 119.2(9) . . ? N1 C8 C7 119.8(8) . . ? N4 C8 C7 120.8(9) . . ? C10 C9 N4 132.3(9) . . ? C10 C9 C14 120.0(10) . . ? N4 C9 C14 107.7(8) . . ? C9 C10 C11 119.1(11) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 121.0(11) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 120.8(11) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.4(11) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 N1 133.7(10) . . ? C13 C14 C9 119.7(10) . . ? N1 C14 C9 106.6(8) . . ? C16 C15 C19 124.9(13) . . ? C16 C15 H15 117.6 . . ? C19 C15 H15 117.6 . . ? C15 C16 C24 122.8(13) . . ? C15 C16 H16 118.6 . . ? C24 C16 H16 118.6 . . ? N5 C17 C18 121.9(11) . . ? N5 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 121.7(11) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 117.4(10) . . ? C18 C19 C15 121.2(11) . . ? C20 C19 C15 121.4(11) . . ? C21 C20 C19 119.0(11) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N5 C21 C20 123.2(11) . . ? N5 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C23 C22 N6 121.8(11) . . ? C23 C22 H22 119.1 . . ? N6 C22 H22 119.1 . . ? C22 C23 C24 120.8(11) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 117.3(10) . . ? C25 C24 C16 123.0(12) . . ? C23 C24 C16 119.6(11) . . ? C24 C25 C26 119.2(11) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N6 C26 C25 122.8(11) . . ? N6 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C28 C27 C31 109.1(10) . . ? C28 C27 C32 125.4(13) . . ? C31 C27 C32 125.5(12) . . ? C28 C27 Ir1 69.7(6) . . ? C31 C27 Ir1 70.4(6) . . ? C32 C27 Ir1 125.2(9) . . ? C27 C28 C33 124.7(12) . . ? C27 C28 C29 108.0(11) . . ? C33 C28 C29 126.6(11) . . ? C27 C28 Ir1 72.5(6) . . ? C33 C28 Ir1 130.8(9) . . ? C29 C28 Ir1 70.0(5) . . ? C30 C29 C34 128.0(12) . . ? C30 C29 C28 105.8(10) . . ? C34 C29 C28 126.2(11) . . ? C30 C29 Ir1 69.8(6) . . ? C34 C29 Ir1 125.7(7) . . ? C28 C29 Ir1 68.8(5) . . ? C31 C30 C29 108.9(11) . . ? C31 C30 C35 127.1(12) . . ? C29 C30 C35 123.7(12) . . ? C31 C30 Ir1 71.8(7) . . ? C29 C30 Ir1 70.8(6) . . ? C35 C30 Ir1 128.0(8) . . ? C30 C31 C27 108.2(10) . . ? C30 C31 C36 124.4(13) . . ? C27 C31 C36 127.1(12) . . ? C30 C31 Ir1 69.5(6) . . ? C27 C31 Ir1 70.5(6) . . ? C36 C31 Ir1 130.6(8) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C41 108.8(11) . . ? C38 C37 C42 126.3(11) . . ? C41 C37 C42 124.8(12) . . ? C38 C37 Ir2 72.1(6) . . ? C41 C37 Ir2 70.5(6) . . ? C42 C37 Ir2 125.6(8) . . ? C37 C38 C39 109.7(10) . . ? C37 C38 C43 127.6(11) . . ? C39 C38 C43 122.7(12) . . ? C37 C38 Ir2 70.7(6) . . ? C39 C38 Ir2 70.8(5) . . ? C43 C38 Ir2 125.1(8) . . ? C38 C39 C40 107.1(10) . . ? C38 C39 C44 127.4(11) . . ? C40 C39 C44 124.8(11) . . ? C38 C39 Ir2 70.9(5) . . ? C40 C39 Ir2 69.9(6) . . ? C44 C39 Ir2 131.7(9) . . ? C39 C40 C41 107.9(10) . . ? C39 C40 C45 126.5(14) . . ? C41 C40 C45 125.6(13) . . ? C39 C40 Ir2 71.4(6) . . ? C41 C40 Ir2 70.6(6) . . ? C45 C40 Ir2 123.9(9) . . ? C40 C41 C37 106.5(10) . . ? C40 C41 C46 127.3(12) . . ? C37 C41 C46 125.9(13) . . ? C40 C41 Ir2 70.3(7) . . ? C37 C41 Ir2 70.4(6) . . ? C46 C41 Ir2 128.9(8) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F1 C47 F2 100.3(14) . . ? F1 C47 F3 105.3(14) . . ? F2 C47 F3 107.7(15) . . ? F1 C47 S1 115.2(13) . . ? F2 C47 S1 113.5(12) . . ? F3 C47 S1 113.7(10) . . ? F4 C48 F6 112.2(16) . . ? F4 C48 F5 105.1(19) . . ? F6 C48 F5 95.6(18) . . ? F4 C48 S2 119.0(13) . . ? F6 C48 S2 118.0(14) . . ? F5 C48 S2 102.3(14) . . ? Cl2 C49 Cl1 106.6(13) . . ? Cl2 C49 H49A 110.4 . . ? Cl1 C49 H49A 110.4 . . ? Cl2 C49 H49B 110.4 . . ? Cl1 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 C50 131(3) . . ? O7 C51 H51A 104.6 . . ? C50 C51 H51A 104.6 . . ? O7 C51 H51B 104.6 . . ? C50 C51 H51B 104.6 . . ? H51A C51 H51B 105.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O7 C52 C53 126(3) . . ? O7 C52 H52A 105.9 . . ? C53 C52 H52A 105.9 . . ? O7 C52 H52B 105.9 . . ? C53 C52 H52B 105.9 . . ? H52A C52 H52B 106.2 . . ? C51 O7 C52 117(2) . . ? 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 0.026 0.250 187.1 18.1 2 0.000 -0.027 0.750 187.1 15.5 3 0.500 0.009 0.250 29.1 0.7 4 0.500 -0.009 0.750 29.2 0.9 5 0.307 0.014 0.370 6.8 -0.2 6 0.693 0.014 0.130 6.8 -0.1 7 0.500 0.473 0.750 187.1 15.5 8 0.500 0.526 0.250 187.1 18.1 9 0.000 0.509 0.250 29.1 0.7 10 0.000 0.491 0.750 29.2 0.9 11 0.193 0.486 0.630 6.8 -0.1 12 0.807 0.486 0.870 6.8 -0.5 13 0.193 0.514 0.130 6.8 -0.1 14 0.807 0.514 0.370 6.8 -0.2 15 0.307 0.986 0.870 6.8 -0.5 16 0.693 0.986 0.630 6.8 -0.1 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.370 _refine_diff_density_min -2.071 _refine_diff_density_rms 0.176 # Attachment 'Ir-2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 864532' #TrackingRef 'Ir-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H112 F12 Ir4 N12 O16 S4' _chemical_formula_weight 2863.06 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 13.0767(9) _cell_length_b 23.9320(17) _cell_length_c 18.5594(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.0130(10) _cell_angle_gamma 90.00 _cell_volume 5751.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9079 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 4.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4807 _exptl_absorpt_correction_T_max 0.6471 _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_% 4.27 _diffrn_reflns_number 42266 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.81 _reflns_number_total 13510 _reflns_number_gt 10761 _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. ; _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^)+(0.0695P)^2^+9.7304P] 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 13510 _refine_ls_number_parameters 714 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.488698(14) 0.602161(8) 0.172459(12) 0.02663(7) Uani 1 1 d . . . Ir2 Ir 0.165610(16) 0.757606(8) 0.165987(12) 0.02832(7) Uani 1 1 d . . . N1 N 0.4293(3) 0.67632(17) 0.1149(3) 0.0269(9) Uani 1 1 d . . . N2 N 0.3702(3) 0.62765(18) 0.2371(3) 0.0290(9) Uani 1 1 d . . . N3 N 0.2369(4) 0.68970(18) 0.2327(3) 0.0311(10) Uani 1 1 d . . . N4 N 0.2952(3) 0.73789(17) 0.1105(3) 0.0265(9) Uani 1 1 d . . . N5 N 0.3613(3) 0.56160(18) 0.1095(3) 0.0261(9) Uani 1 1 d . . . N6 N 0.0919(3) 0.69174(17) 0.1028(3) 0.0277(9) Uani 1 1 d . . . S1 S 0.23348(16) 0.32163(11) 0.12753(13) 0.0669(6) Uani 1 1 d . . . O1 O 0.2379(5) 0.2840(3) 0.1875(4) 0.089(2) Uani 1 1 d . . . O2 O 0.3308(5) 0.3430(4) 0.1149(4) 0.099(2) Uani 1 1 d . . . O3 O 0.1546(5) 0.3625(2) 0.1222(4) 0.0752(17) Uani 1 1 d . . . F1 F 0.2635(6) 0.2352(3) 0.0448(5) 0.125(3) Uani 1 1 d . . . F2 F 0.1068(5) 0.2501(3) 0.0547(4) 0.0968(19) Uani 1 1 d . . . F3 F 0.1824(6) 0.3041(3) -0.0123(4) 0.113(2) Uani 1 1 d . . . F4 F 1.0666(4) 0.4992(3) 0.2332(3) 0.0890(18) Uani 1 1 d . A . F5 F 1.0187(6) 0.4947(6) 0.3356(4) 0.169(4) Uani 1 1 d U A . F6 F 1.0078(8) 0.4266(3) 0.2771(7) 0.171(4) Uani 1 1 d U A . S2 S 0.8662(3) 0.5098(3) 0.2421(3) 0.0500(14) Uani 0.568(11) 1 d PU A 1 O4 O 0.8101(13) 0.4885(8) 0.2928(9) 0.077(5) Uani 0.568(11) 1 d PU A 1 O5 O 0.8889(11) 0.5677(5) 0.2580(11) 0.108(6) Uani 0.568(11) 1 d P A 1 O6 O 0.8354(11) 0.5001(9) 0.1707(7) 0.101(5) Uani 0.568(11) 1 d PU A 1 S2' S 0.8737(3) 0.4800(3) 0.2215(3) 0.0401(16) Uani 0.432(11) 1 d PU A 2 O4' O 0.8033(15) 0.4660(6) 0.2711(10) 0.046(4) Uani 0.432(11) 1 d PU A 2 O5' O 0.8626(10) 0.5390(6) 0.1942(10) 0.060(4) Uani 0.432(11) 1 d PU A 2 O6' O 0.8824(16) 0.4371(6) 0.1705(7) 0.095(7) Uani 0.432(11) 1 d P A 2 C1 C 0.3512(4) 0.6974(2) 0.1444(3) 0.0269(10) Uani 1 1 d . . . C2 C 0.3208(4) 0.6727(2) 0.2078(3) 0.0292(11) Uani 1 1 d . . . C3 C 0.3084(5) 0.6120(2) 0.2896(3) 0.0316(12) Uani 1 1 d . . . C4 C 0.3191(5) 0.5671(3) 0.3386(4) 0.0426(14) Uani 1 1 d . . . H4 H 0.3750 0.5414 0.3406 0.051 Uiso 1 1 calc R . . C5 C 0.2452(6) 0.5621(3) 0.3833(4) 0.0548(18) Uani 1 1 d . . . H5 H 0.2502 0.5321 0.4171 0.066 Uiso 1 1 calc R . . C6 C 0.1623(7) 0.5993(3) 0.3814(4) 0.060(2) Uani 1 1 d . . . H6 H 0.1124 0.5942 0.4134 0.073 Uiso 1 1 calc R . . C7 C 0.1530(6) 0.6438(3) 0.3328(4) 0.0465(15) Uani 1 1 d . . . H7 H 0.0971 0.6693 0.3312 0.056 Uiso 1 1 calc R . . C8 C 0.2260(4) 0.6501(2) 0.2872(3) 0.0317(12) Uani 1 1 d . . . C9 C 0.3445(4) 0.7466(2) 0.0483(3) 0.0280(11) Uani 1 1 d . . . C10 C 0.3238(5) 0.7835(2) -0.0104(4) 0.0386(13) Uani 1 1 d . . . H10 H 0.2679 0.8090 -0.0130 0.046 Uiso 1 1 calc R . . C11 C 0.3851(5) 0.7819(3) -0.0635(4) 0.0499(17) Uani 1 1 d . . . H11 H 0.3718 0.8068 -0.1036 0.060 Uiso 1 1 calc R . . C12 C 0.4681(5) 0.7442(3) -0.0603(4) 0.0473(16) Uani 1 1 d . . . H12 H 0.5103 0.7445 -0.0980 0.057 Uiso 1 1 calc R . . C13 C 0.4898(5) 0.7067(3) -0.0036(4) 0.0392(13) Uani 1 1 d . . . H13 H 0.5451 0.6809 -0.0023 0.047 Uiso 1 1 calc R . . C14 C 0.4280(4) 0.7081(2) 0.0513(3) 0.0265(10) Uani 1 1 d . . . C15 C 0.3042(4) 0.5245(2) 0.1391(3) 0.0331(12) Uani 1 1 d . . . H15 H 0.3257 0.5133 0.1880 0.040 Uiso 1 1 calc R . . C16 C 0.2153(4) 0.5014(2) 0.1024(3) 0.0300(11) Uani 1 1 d . . . H16 H 0.1777 0.4746 0.1260 0.036 Uiso 1 1 calc R . . C17 C 0.1809(4) 0.5167(2) 0.0322(3) 0.0260(10) Uani 1 1 d . . . C18 C 0.2443(4) 0.5533(2) -0.0008(3) 0.0299(11) Uani 1 1 d . . . H18 H 0.2262 0.5636 -0.0504 0.036 Uiso 1 1 calc R . . C19 C 0.3332(4) 0.5743(2) 0.0389(3) 0.0284(11) Uani 1 1 d . . . H19 H 0.3758 0.5986 0.0157 0.034 Uiso 1 1 calc R . . C20 C 0.0439(5) 0.6508(2) 0.1339(3) 0.0347(12) Uani 1 1 d . . . H20 H 0.0355 0.6546 0.1837 0.042 Uiso 1 1 calc R . . C21 C 0.0058(5) 0.6030(2) 0.0970(3) 0.0330(12) Uani 1 1 d . . . H21 H -0.0259 0.5745 0.1219 0.040 Uiso 1 1 calc R . . C22 C 0.0142(4) 0.5971(2) 0.0239(3) 0.0265(11) Uani 1 1 d . . . C23 C 0.0592(4) 0.6415(2) -0.0096(3) 0.0325(12) Uani 1 1 d . . . H23 H 0.0636 0.6400 -0.0602 0.039 Uiso 1 1 calc R . . C24 C 0.0972(4) 0.6875(2) 0.0302(3) 0.0298(11) Uani 1 1 d . . . H24 H 0.1279 0.7170 0.0065 0.036 Uiso 1 1 calc R . . C25 C 0.0805(4) 0.4993(2) -0.0126(3) 0.0254(10) Uani 1 1 d . . . H25 H 0.0933 0.4872 -0.0622 0.030 Uiso 1 1 calc R . . C26 C -0.0113(4) 0.5439(2) -0.0193(3) 0.0255(10) Uani 1 1 d . . . H26 H -0.0377 0.5523 -0.0714 0.031 Uiso 1 1 calc R . . C27 C 0.6507(4) 0.6243(3) 0.1854(4) 0.0400(14) Uani 1 1 d . . . C28 C 0.6238(5) 0.6085(3) 0.2544(4) 0.0482(17) Uani 1 1 d . . . C29 C 0.5904(5) 0.5511(3) 0.2476(4) 0.0425(15) Uani 1 1 d . . . C30 C 0.5945(5) 0.5332(3) 0.1751(4) 0.0455(16) Uani 1 1 d . . . C31 C 0.6297(4) 0.5789(2) 0.1340(4) 0.0398(14) Uani 1 1 d . . . C32 C 0.6980(6) 0.6795(3) 0.1660(5) 0.060(2) Uani 1 1 d . . . H32A H 0.6750 0.7095 0.1960 0.091 Uiso 1 1 calc R . . H32B H 0.6760 0.6879 0.1145 0.091 Uiso 1 1 calc R . . H32C H 0.7735 0.6768 0.1751 0.091 Uiso 1 1 calc R . . C33 C 0.6335(7) 0.6432(4) 0.3219(5) 0.074(3) Uani 1 1 d . . . H33A H 0.6951 0.6317 0.3548 0.112 Uiso 1 1 calc R . . H33B H 0.5722 0.6380 0.3460 0.112 Uiso 1 1 calc R . . H33C H 0.6396 0.6827 0.3090 0.112 Uiso 1 1 calc R . . C34 C 0.5667(6) 0.5152(4) 0.3090(5) 0.079(3) Uani 1 1 d . . . H34A H 0.5148 0.4872 0.2905 0.118 Uiso 1 1 calc R . . H34B H 0.5399 0.5385 0.3456 0.118 Uiso 1 1 calc R . . H34C H 0.6298 0.4962 0.3312 0.118 Uiso 1 1 calc R . . C35 C 0.5698(6) 0.4756(3) 0.1445(5) 0.0558(19) Uani 1 1 d . . . H35A H 0.6342 0.4560 0.1395 0.084 Uiso 1 1 calc R . . H35B H 0.5276 0.4788 0.0967 0.084 Uiso 1 1 calc R . . H35C H 0.5316 0.4547 0.1775 0.084 Uiso 1 1 calc R . . C36 C 0.6577(6) 0.5766(3) 0.0592(4) 0.0555(19) Uani 1 1 d . . . H36A H 0.6614 0.6146 0.0401 0.083 Uiso 1 1 calc R . . H36B H 0.6052 0.5553 0.0277 0.083 Uiso 1 1 calc R . . H36C H 0.7250 0.5583 0.0603 0.083 Uiso 1 1 calc R . . C37 C 0.1833(6) 0.8263(3) 0.2417(4) 0.0499(17) Uani 1 1 d . . . C38 C 0.1905(6) 0.8468(2) 0.1711(5) 0.055(2) Uani 1 1 d . . . C39 C 0.0944(6) 0.8338(3) 0.1258(4) 0.0482(17) Uani 1 1 d . . . C40 C 0.0305(5) 0.8084(3) 0.1696(4) 0.0420(15) Uani 1 1 d . . . C41 C 0.0843(5) 0.8023(3) 0.2408(4) 0.0442(15) Uani 1 1 d . . . C42 C 0.2652(8) 0.8305(4) 0.3091(6) 0.081(3) Uani 1 1 d . . . H42A H 0.2515 0.8636 0.3375 0.121 Uiso 1 1 calc R . . H42B H 0.3337 0.8338 0.2938 0.121 Uiso 1 1 calc R . . H42C H 0.2628 0.7970 0.3390 0.121 Uiso 1 1 calc R . . C43 C 0.2827(7) 0.8758(3) 0.1447(7) 0.086(3) Uani 1 1 d . . . H43A H 0.3388 0.8795 0.1853 0.129 Uiso 1 1 calc R . . H43B H 0.2619 0.9129 0.1258 0.129 Uiso 1 1 calc R . . H43C H 0.3066 0.8534 0.1060 0.129 Uiso 1 1 calc R . . C44 C 0.0643(9) 0.8527(4) 0.0486(5) 0.087(3) Uani 1 1 d . . . H44A H 0.0224 0.8237 0.0213 0.130 Uiso 1 1 calc R . . H44B H 0.1266 0.8594 0.0260 0.130 Uiso 1 1 calc R . . H44C H 0.0241 0.8873 0.0480 0.130 Uiso 1 1 calc R . . C45 C -0.0795(6) 0.7896(4) 0.1468(6) 0.070(2) Uani 1 1 d . . . H45A H -0.1259 0.8218 0.1463 0.105 Uiso 1 1 calc R . . H45B H -0.0980 0.7617 0.1814 0.105 Uiso 1 1 calc R . . H45C H -0.0858 0.7732 0.0981 0.105 Uiso 1 1 calc R . . C46 C 0.0379(7) 0.7809(3) 0.3068(5) 0.064(2) Uani 1 1 d . . . H46A H 0.0926 0.7647 0.3421 0.095 Uiso 1 1 calc R . . H46B H -0.0141 0.7523 0.2912 0.095 Uiso 1 1 calc R . . H46C H 0.0055 0.8120 0.3295 0.095 Uiso 1 1 calc R . . C47 C 0.1953(7) 0.2764(5) 0.0515(6) 0.080(3) Uani 1 1 d . . . C48 C 0.9973(6) 0.4776(3) 0.2691(5) 0.0559(19) Uani 1 1 d . . . C49 C 0.4832(10) 0.2976(5) 0.2721(9) 0.123(5) Uani 1 1 d . . . O7 O 0.4758(6) 0.3476(3) 0.2351(5) 0.104(3) Uani 1 1 d . . . C50 C 0.2708(11) 0.4096(8) 0.3026(14) 0.185(10) Uani 1 1 d D . . O8 O 0.3684(9) 0.4293(5) 0.2867(9) 0.179(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02171(10) 0.02081(10) 0.03524(12) 0.00069(8) -0.00352(8) 0.00016(7) Ir2 0.03029(11) 0.01652(10) 0.03735(13) -0.00750(8) 0.00192(9) 0.00048(7) N1 0.027(2) 0.021(2) 0.032(2) 0.0010(18) 0.0019(18) -0.0006(16) N2 0.032(2) 0.022(2) 0.031(2) -0.0011(18) -0.0004(19) 0.0014(17) N3 0.035(2) 0.023(2) 0.034(3) -0.0065(19) 0.003(2) -0.0009(18) N4 0.029(2) 0.0161(19) 0.034(2) -0.0010(17) 0.0028(19) 0.0007(16) N5 0.0222(19) 0.023(2) 0.032(2) 0.0003(18) 0.0017(17) -0.0002(16) N6 0.029(2) 0.0188(19) 0.035(2) -0.0038(18) 0.0064(19) -0.0013(16) S1 0.0488(11) 0.0813(15) 0.0687(14) 0.0157(12) 0.0016(9) 0.0077(10) O1 0.075(4) 0.101(5) 0.090(5) 0.039(4) 0.003(4) 0.022(4) O2 0.055(4) 0.133(7) 0.104(6) 0.015(5) -0.008(4) -0.010(4) O3 0.067(4) 0.057(3) 0.098(5) 0.011(3) 0.000(3) 0.011(3) F1 0.104(5) 0.125(6) 0.144(7) -0.028(5) 0.012(5) 0.048(4) F2 0.082(4) 0.102(5) 0.103(5) -0.016(4) 0.001(4) -0.001(3) F3 0.114(5) 0.154(7) 0.069(4) 0.002(4) 0.010(4) -0.009(5) F4 0.048(3) 0.106(4) 0.116(5) 0.036(4) 0.025(3) -0.008(3) F5 0.114(6) 0.311(12) 0.074(5) -0.004(6) -0.013(4) -0.061(7) F6 0.153(6) 0.084(5) 0.285(9) 0.042(6) 0.068(6) 0.001(4) S2 0.0400(16) 0.065(3) 0.046(2) 0.011(2) 0.0095(14) 0.0062(17) O4 0.055(7) 0.110(12) 0.070(9) 0.018(8) 0.023(6) -0.008(9) O5 0.086(9) 0.060(7) 0.184(18) -0.005(9) 0.037(10) 0.018(6) O6 0.084(8) 0.162(14) 0.054(7) 0.006(8) 0.000(6) -0.004(9) S2' 0.037(2) 0.044(3) 0.039(3) 0.013(2) 0.0055(17) -0.0059(19) O4' 0.043(7) 0.040(7) 0.061(10) 0.014(6) 0.023(7) -0.008(6) O5' 0.054(7) 0.046(7) 0.083(10) 0.033(7) 0.022(7) 0.006(6) O6' 0.166(17) 0.064(9) 0.042(8) -0.004(7) -0.035(9) -0.044(10) C1 0.025(2) 0.020(2) 0.034(3) 0.000(2) 0.000(2) -0.0040(19) C2 0.034(3) 0.023(2) 0.030(3) -0.001(2) -0.001(2) -0.001(2) C3 0.041(3) 0.030(3) 0.022(3) -0.005(2) -0.003(2) -0.002(2) C4 0.051(4) 0.039(3) 0.037(3) 0.009(3) 0.007(3) 0.003(3) C5 0.072(5) 0.055(4) 0.039(4) 0.009(3) 0.013(4) 0.001(4) C6 0.088(6) 0.051(4) 0.048(4) -0.002(3) 0.032(4) -0.004(4) C7 0.059(4) 0.042(3) 0.037(4) -0.003(3) 0.005(3) -0.009(3) C8 0.039(3) 0.025(3) 0.029(3) -0.009(2) 0.001(2) -0.005(2) C9 0.023(2) 0.027(3) 0.032(3) -0.001(2) 0.000(2) -0.0051(19) C10 0.036(3) 0.031(3) 0.047(4) 0.008(3) 0.000(3) 0.008(2) C11 0.046(4) 0.056(4) 0.047(4) 0.027(3) 0.008(3) 0.006(3) C12 0.041(3) 0.061(4) 0.042(4) 0.013(3) 0.011(3) 0.003(3) C13 0.035(3) 0.042(3) 0.041(3) 0.008(3) 0.005(3) 0.008(2) C14 0.025(2) 0.023(2) 0.030(3) 0.002(2) -0.001(2) -0.0021(19) C15 0.034(3) 0.029(3) 0.033(3) 0.002(2) -0.005(2) -0.006(2) C16 0.030(3) 0.025(2) 0.034(3) 0.000(2) 0.005(2) -0.007(2) C17 0.027(2) 0.022(2) 0.029(3) -0.006(2) 0.006(2) -0.0071(19) C18 0.028(3) 0.031(3) 0.030(3) -0.001(2) 0.004(2) -0.005(2) C19 0.028(3) 0.026(3) 0.030(3) -0.004(2) 0.001(2) -0.004(2) C20 0.042(3) 0.029(3) 0.034(3) -0.007(2) 0.007(2) -0.005(2) C21 0.040(3) 0.025(3) 0.034(3) -0.004(2) 0.007(2) -0.012(2) C22 0.026(2) 0.020(2) 0.030(3) -0.003(2) -0.006(2) -0.0032(19) C23 0.035(3) 0.029(3) 0.031(3) 0.001(2) -0.001(2) -0.007(2) C24 0.033(3) 0.022(2) 0.033(3) 0.002(2) -0.001(2) -0.003(2) C25 0.027(2) 0.021(2) 0.028(3) -0.007(2) 0.003(2) -0.0066(19) C26 0.025(2) 0.025(2) 0.027(3) -0.003(2) 0.002(2) -0.0038(19) C27 0.021(2) 0.040(3) 0.055(4) 0.001(3) -0.009(2) -0.006(2) C28 0.029(3) 0.059(4) 0.050(4) 0.001(3) -0.017(3) -0.002(3) C29 0.031(3) 0.043(3) 0.052(4) 0.012(3) 0.004(3) 0.009(3) C30 0.028(3) 0.031(3) 0.073(5) 0.004(3) -0.008(3) 0.010(2) C31 0.024(3) 0.032(3) 0.061(4) 0.011(3) 0.000(3) 0.009(2) C32 0.043(4) 0.052(4) 0.085(6) 0.006(4) 0.006(4) -0.019(3) C33 0.069(6) 0.095(7) 0.053(5) -0.010(5) -0.016(4) -0.005(5) C34 0.047(4) 0.105(7) 0.088(6) 0.067(6) 0.020(4) 0.035(4) C35 0.055(4) 0.030(3) 0.083(6) -0.003(3) 0.011(4) 0.011(3) C36 0.043(4) 0.064(5) 0.063(5) 0.008(4) 0.021(3) 0.022(3) C37 0.057(4) 0.032(3) 0.060(5) -0.021(3) 0.005(3) 0.002(3) C38 0.056(4) 0.017(3) 0.093(6) -0.019(3) 0.016(4) 0.000(3) C39 0.058(4) 0.027(3) 0.060(4) -0.002(3) 0.008(3) 0.018(3) C40 0.039(3) 0.033(3) 0.054(4) -0.016(3) 0.006(3) 0.013(3) C41 0.055(4) 0.031(3) 0.048(4) -0.016(3) 0.010(3) 0.009(3) C42 0.080(6) 0.072(6) 0.083(7) -0.050(5) -0.011(5) 0.000(5) C43 0.075(6) 0.031(4) 0.163(11) -0.017(5) 0.059(7) -0.019(4) C44 0.120(8) 0.071(6) 0.071(6) 0.026(5) 0.021(6) 0.062(6) C45 0.049(4) 0.064(5) 0.096(7) -0.026(5) 0.001(4) 0.015(4) C46 0.077(5) 0.057(5) 0.063(5) -0.013(4) 0.028(4) 0.015(4) C47 0.057(5) 0.110(8) 0.074(7) 0.004(6) 0.011(5) 0.011(5) C48 0.055(4) 0.049(4) 0.064(5) 0.013(4) 0.010(4) -0.008(3) C49 0.107(9) 0.081(8) 0.167(14) 0.041(9) -0.032(9) -0.003(7) O7 0.095(5) 0.091(5) 0.119(7) 0.033(5) -0.004(5) 0.011(4) C50 0.074(9) 0.146(15) 0.33(3) -0.039(17) 0.010(13) -0.021(9) O8 0.134(9) 0.128(9) 0.284(18) 0.004(10) 0.052(10) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N5 2.131(4) . ? Ir1 C31 2.141(6) . ? Ir1 C30 2.149(6) . ? Ir1 N1 2.159(4) . ? Ir1 C27 2.164(5) . ? Ir1 C29 2.166(6) . ? Ir1 C28 2.170(6) . ? Ir1 N2 2.175(5) . ? Ir2 N6 2.115(4) . ? Ir2 C39 2.135(6) . ? Ir2 C41 2.148(6) . ? Ir2 C40 2.154(6) . ? Ir2 C37 2.154(6) . ? Ir2 N4 2.155(5) . ? Ir2 C38 2.159(6) . ? Ir2 N3 2.173(5) . ? N1 C1 1.323(7) . ? N1 C14 1.403(7) . ? N2 C2 1.333(7) . ? N2 C3 1.401(8) . ? N3 C2 1.314(7) . ? N3 C8 1.407(7) . ? N4 C1 1.322(7) . ? N4 C9 1.412(7) . ? N5 C15 1.328(7) . ? N5 C19 1.344(7) . ? N6 C20 1.337(7) . ? N6 C24 1.363(7) . ? S1 O3 1.415(6) . ? S1 O2 1.421(7) . ? S1 O1 1.426(7) . ? S1 C47 1.794(12) . ? F1 C47 1.346(12) . ? F2 C47 1.325(12) . ? F3 C47 1.347(12) . ? F4 C48 1.304(9) . ? F5 C48 1.294(11) . ? F6 C48 1.235(10) . ? S2 O6 1.351(15) . ? S2 O4 1.369(17) . ? S2 O5 1.438(15) . ? S2 C48 1.884(9) . ? S2' O6' 1.413(18) . ? S2' O4' 1.429(18) . ? S2' O5' 1.500(13) . ? S2' C48 1.732(9) . ? C1 C2 1.421(8) . ? C3 C4 1.402(8) . ? C3 C8 1.407(8) . ? C4 C5 1.364(10) . ? C5 C6 1.399(12) . ? C6 C7 1.389(10) . ? C7 C8 1.370(9) . ? C9 C10 1.398(8) . ? C9 C14 1.424(7) . ? C10 C11 1.355(9) . ? C11 C12 1.407(10) . ? C12 C13 1.381(9) . ? C13 C14 1.386(8) . ? C15 C16 1.379(7) . ? C16 C17 1.367(8) . ? C17 C18 1.406(7) . ? C17 C25 1.511(7) . ? C18 C19 1.382(7) . ? C20 C21 1.390(7) . ? C21 C22 1.385(8) . ? C22 C23 1.401(7) . ? C22 C26 1.516(7) . ? C23 C24 1.379(8) . ? C25 C26 1.547(7) 3_565 ? C25 C26 1.599(7) . ? C26 C25 1.547(7) 3_565 ? C27 C28 1.426(10) . ? C27 C31 1.446(9) . ? C27 C32 1.524(9) . ? C28 C29 1.441(10) . ? C28 C33 1.493(11) . ? C29 C30 1.420(10) . ? C29 C34 1.495(10) . ? C30 C31 1.445(9) . ? C30 C35 1.508(9) . ? C31 C36 1.486(10) . ? C37 C41 1.414(10) . ? C37 C38 1.415(12) . ? C37 C42 1.531(11) . ? C38 C39 1.444(11) . ? C38 C43 1.531(11) . ? C39 C40 1.385(10) . ? C39 C44 1.502(12) . ? C40 C41 1.415(10) . ? C40 C45 1.510(10) . ? C41 C46 1.530(11) . ? C49 O7 1.378(14) . ? C50 O8 1.429(14) . ? 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 Ir1 C31 110.0(2) . . ? N5 Ir1 C30 96.5(2) . . ? C31 Ir1 C30 39.4(2) . . ? N5 Ir1 N1 84.44(16) . . ? C31 Ir1 N1 108.4(2) . . ? C30 Ir1 N1 145.9(2) . . ? N5 Ir1 C27 148.3(2) . . ? C31 Ir1 C27 39.2(3) . . ? C30 Ir1 C27 64.4(2) . . ? N1 Ir1 C27 97.6(2) . . ? N5 Ir1 C29 117.4(2) . . ? C31 Ir1 C29 65.7(2) . . ? C30 Ir1 C29 38.4(3) . . ? N1 Ir1 C29 158.2(2) . . ? C27 Ir1 C29 64.1(2) . . ? N5 Ir1 C28 156.1(2) . . ? C31 Ir1 C28 66.2(3) . . ? C30 Ir1 C28 65.1(3) . . ? N1 Ir1 C28 119.4(2) . . ? C27 Ir1 C28 38.4(3) . . ? C29 Ir1 C28 38.8(3) . . ? N5 Ir1 N2 82.41(17) . . ? C31 Ir1 N2 165.8(2) . . ? C30 Ir1 N2 135.1(2) . . ? N1 Ir1 N2 78.90(17) . . ? C27 Ir1 N2 129.2(2) . . ? C29 Ir1 N2 102.9(2) . . ? C28 Ir1 N2 99.6(2) . . ? N6 Ir2 C39 107.5(2) . . ? N6 Ir2 C41 120.1(2) . . ? C39 Ir2 C41 64.5(3) . . ? N6 Ir2 C40 97.2(2) . . ? C39 Ir2 C40 37.7(3) . . ? C41 Ir2 C40 38.4(3) . . ? N6 Ir2 C37 158.4(2) . . ? C39 Ir2 C37 65.0(3) . . ? C41 Ir2 C37 38.4(3) . . ? C40 Ir2 C37 64.1(3) . . ? N6 Ir2 N4 84.26(16) . . ? C39 Ir2 N4 110.7(2) . . ? C41 Ir2 N4 155.7(2) . . ? C40 Ir2 N4 147.3(2) . . ? C37 Ir2 N4 117.3(2) . . ? N6 Ir2 C38 144.6(3) . . ? C39 Ir2 C38 39.3(3) . . ? C41 Ir2 C38 64.2(3) . . ? C40 Ir2 C38 63.9(3) . . ? C37 Ir2 C38 38.3(3) . . ? N4 Ir2 C38 96.5(2) . . ? N6 Ir2 N3 83.37(17) . . ? C39 Ir2 N3 165.8(2) . . ? C41 Ir2 N3 102.4(2) . . ? C40 Ir2 N3 133.9(2) . . ? C37 Ir2 N3 101.5(2) . . ? N4 Ir2 N3 78.79(17) . . ? C38 Ir2 N3 131.6(3) . . ? C1 N1 C14 102.9(4) . . ? C1 N1 Ir1 110.7(3) . . ? C14 N1 Ir1 145.4(4) . . ? C2 N2 C3 101.9(5) . . ? C2 N2 Ir1 110.1(4) . . ? C3 N2 Ir1 146.4(4) . . ? C2 N3 C8 102.5(5) . . ? C2 N3 Ir2 110.1(4) . . ? C8 N3 Ir2 146.7(4) . . ? C1 N4 C9 102.3(4) . . ? C1 N4 Ir2 110.7(4) . . ? C9 N4 Ir2 146.8(4) . . ? C15 N5 C19 117.5(5) . . ? C15 N5 Ir1 121.3(4) . . ? C19 N5 Ir1 121.2(3) . . ? C20 N6 C24 117.7(5) . . ? C20 N6 Ir2 120.8(4) . . ? C24 N6 Ir2 121.4(3) . . ? O3 S1 O2 113.6(5) . . ? O3 S1 O1 116.2(4) . . ? O2 S1 O1 114.6(4) . . ? O3 S1 C47 104.0(4) . . ? O2 S1 C47 104.2(5) . . ? O1 S1 C47 102.1(5) . . ? O6 S2 O4 119.6(11) . . ? O6 S2 O5 113.1(13) . . ? O4 S2 O5 109.4(10) . . ? O6 S2 C48 109.0(8) . . ? O4 S2 C48 102.8(8) . . ? O5 S2 C48 100.7(7) . . ? O6' S2' O4' 112.4(10) . . ? O6' S2' O5' 118.1(10) . . ? O4' S2' O5' 113.4(9) . . ? O6' S2' C48 99.2(9) . . ? O4' S2' C48 107.7(9) . . ? O5' S2' C48 104.1(7) . . ? N4 C1 N1 119.3(5) . . ? N4 C1 C2 119.9(5) . . ? N1 C1 C2 120.4(5) . . ? N3 C2 N2 119.2(5) . . ? N3 C2 C1 120.5(5) . . ? N2 C2 C1 119.8(5) . . ? N2 C3 C4 129.9(5) . . ? N2 C3 C8 108.5(5) . . ? C4 C3 C8 121.6(6) . . ? C5 C4 C3 116.5(6) . . ? C4 C5 C6 122.8(7) . . ? C7 C6 C5 120.0(7) . . ? C8 C7 C6 118.7(7) . . ? C7 C8 C3 120.4(6) . . ? C7 C8 N3 131.8(6) . . ? C3 C8 N3 107.8(5) . . ? C10 C9 N4 132.0(5) . . ? C10 C9 C14 120.1(5) . . ? N4 C9 C14 107.9(5) . . ? C11 C10 C9 118.7(6) . . ? C10 C11 C12 121.2(6) . . ? C13 C12 C11 121.6(6) . . ? C12 C13 C14 117.8(6) . . ? C13 C14 N1 131.7(5) . . ? C13 C14 C9 120.6(5) . . ? N1 C14 C9 107.6(5) . . ? N5 C15 C16 123.2(5) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 116.5(5) . . ? C16 C17 C25 126.6(5) . . ? C18 C17 C25 116.8(5) . . ? C19 C18 C17 119.8(5) . . ? N5 C19 C18 122.2(5) . . ? N6 C20 C21 123.3(5) . . ? C22 C21 C20 119.6(5) . . ? C21 C22 C23 117.0(5) . . ? C21 C22 C26 124.2(5) . . ? C23 C22 C26 118.5(5) . . ? C24 C23 C22 120.7(5) . . ? N6 C24 C23 121.7(5) . . ? C17 C25 C26 118.8(4) . 3_565 ? C17 C25 C26 116.4(4) . . ? C26 C25 C26 90.2(4) 3_565 . ? C22 C26 C25 117.1(4) . 3_565 ? C22 C26 C25 114.4(4) . . ? C25 C26 C25 89.8(4) 3_565 . ? C28 C27 C31 110.2(6) . . ? C28 C27 C32 127.0(7) . . ? C31 C27 C32 122.8(7) . . ? C28 C27 Ir1 71.0(3) . . ? C31 C27 Ir1 69.5(3) . . ? C32 C27 Ir1 127.6(5) . . ? C27 C28 C29 106.5(6) . . ? C27 C28 C33 127.1(7) . . ? C29 C28 C33 126.4(7) . . ? C27 C28 Ir1 70.5(3) . . ? C29 C28 Ir1 70.4(4) . . ? C33 C28 Ir1 126.3(5) . . ? C30 C29 C28 108.7(6) . . ? C30 C29 C34 126.0(7) . . ? C28 C29 C34 125.0(8) . . ? C30 C29 Ir1 70.2(3) . . ? C28 C29 Ir1 70.8(3) . . ? C34 C29 Ir1 129.9(5) . . ? C29 C30 C31 109.1(6) . . ? C29 C30 C35 126.7(7) . . ? C31 C30 C35 124.1(7) . . ? C29 C30 Ir1 71.4(4) . . ? C31 C30 Ir1 70.0(3) . . ? C35 C30 Ir1 126.2(4) . . ? C30 C31 C27 105.4(6) . . ? C30 C31 C36 127.1(6) . . ? C27 C31 C36 126.6(6) . . ? C30 C31 Ir1 70.6(3) . . ? C27 C31 Ir1 71.2(3) . . ? C36 C31 Ir1 131.1(4) . . ? C41 C37 C38 107.9(7) . . ? C41 C37 C42 124.9(8) . . ? C38 C37 C42 127.1(8) . . ? C41 C37 Ir2 70.6(4) . . ? C38 C37 Ir2 71.0(4) . . ? C42 C37 Ir2 125.6(5) . . ? C37 C38 C39 107.5(6) . . ? C37 C38 C43 127.7(8) . . ? C39 C38 C43 124.8(9) . . ? C37 C38 Ir2 70.7(4) . . ? C39 C38 Ir2 69.5(3) . . ? C43 C38 Ir2 123.7(5) . . ? C40 C39 C38 107.4(7) . . ? C40 C39 C44 126.3(8) . . ? C38 C39 C44 125.7(8) . . ? C40 C39 Ir2 71.9(4) . . ? C38 C39 Ir2 71.2(4) . . ? C44 C39 Ir2 129.3(5) . . ? C39 C40 C41 109.3(6) . . ? C39 C40 C45 126.6(7) . . ? C41 C40 C45 124.1(7) . . ? C39 C40 Ir2 70.4(3) . . ? C41 C40 Ir2 70.5(3) . . ? C45 C40 Ir2 125.2(5) . . ? C37 C41 C40 107.8(6) . . ? C37 C41 C46 126.2(7) . . ? C40 C41 C46 125.5(7) . . ? C37 C41 Ir2 71.1(4) . . ? C40 C41 Ir2 71.0(3) . . ? C46 C41 Ir2 129.7(5) . . ? F2 C47 F1 104.5(10) . . ? F2 C47 F3 105.7(8) . . ? F1 C47 F3 106.5(9) . . ? F2 C47 S1 113.5(7) . . ? F1 C47 S1 113.5(7) . . ? F3 C47 S1 112.4(8) . . ? F6 C48 F5 101.0(10) . . ? F6 C48 F4 112.3(8) . . ? F5 C48 F4 106.9(8) . . ? F6 C48 S2' 100.1(8) . . ? F5 C48 S2' 122.5(7) . . ? F4 C48 S2' 113.1(6) . . ? F6 C48 S2 121.2(7) . . ? F5 C48 S2 101.0(7) . . ? F4 C48 S2 111.9(6) . . ? S2' C48 S2 25.9(2) . . ? 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 -0.019 0.000 0.000 457.3 128.0 2 -0.027 0.500 0.500 457.3 131.3 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.81 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.208 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.187 # Attachment 'Ir-tpt-guestincage-4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 864533' #TrackingRef 'Ir-tpt-guestincage-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C186 H180 F18 Ir6 N24 O24 S6' _chemical_formula_weight 4823.10 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 30.302(3) _cell_length_b 30.302(3) _cell_length_c 41.215(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 32774(6) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.92 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14256 _exptl_absorpt_coefficient_mu 3.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5834 _exptl_absorpt_correction_T_max 0.7040 _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_% 7.15 _diffrn_reflns_number 80769 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 27.59 _reflns_number_total 16790 _reflns_number_gt 10356 _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. ; _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^)+(0.1207P)^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 16790 _refine_ls_number_parameters 778 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1938 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.999 _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 0.619623(11) 0.850558(11) 1.065920(8) 0.04141(11) Uani 1 1 d . . . Ir2 Ir 0.618568(11) 0.858922(12) 0.930557(8) 0.04054(11) Uani 1 1 d . . . N1 N 0.5994(2) 0.8855(2) 1.02732(16) 0.0408(15) Uani 1 1 d . . . N2 N 0.6172(2) 0.8049(2) 1.02415(17) 0.0411(15) Uani 1 1 d . . . N3 N 0.6180(2) 0.8098(2) 0.96895(17) 0.0415(15) Uani 1 1 d . . . N4 N 0.5979(2) 0.8888(2) 0.97215(16) 0.0397(15) Uani 1 1 d . . . N5 N 0.5412(2) 0.7996(2) 1.07267(16) 0.0418(15) Uani 1 1 d . . . N6 N 0.3512(2) 0.7175(2) 1.08459(16) 0.0436(15) Uani 1 1 d . . . N7 N 0.5403(2) 0.8069(2) 0.92454(17) 0.0412(15) Uani 1 1 d . . . N8 N 0.3677(2) 0.6503(2) 0.91448(17) 0.0399(15) Uani 1 1 d . . . O1 O 0.5493(5) 0.6702(4) 0.1041(4) 0.167(6) Uani 1 1 d . . . O2 O 0.5393(6) 0.5994(6) 0.1339(3) 0.208(7) Uani 1 1 d U . . O3 O 0.5849(4) 0.6241(5) 0.0857(3) 0.144(4) Uani 1 1 d . . . O4 O 0.3516(4) 0.2896(5) 0.1354(3) 0.162(5) Uani 1 1 d . . . O5 O 0.4084(4) 0.3765(5) 0.1144(4) 0.178(7) Uani 1 1 d . . . O6 O 0.4417(4) 0.3144(4) 0.1215(2) 0.106(3) Uani 1 1 d . . . S1 S 0.54569(11) 0.62346(11) 0.10573(8) 0.0736(7) Uani 1 1 d . . . S2 S 0.40319(15) 0.32868(19) 0.12974(12) 0.1227(16) Uani 1 1 d . . . F1 F 0.4820(5) 0.5371(4) 0.0798(3) 0.169(5) Uani 1 1 d . . . F2 F 0.4509(4) 0.5824(6) 0.0921(4) 0.213(6) Uani 1 1 d U . . F3 F 0.4924(6) 0.5983(6) 0.0533(4) 0.230(7) Uani 1 1 d . . . F4 F 0.3908(3) 0.3752(4) 0.1773(2) 0.146(4) Uani 1 1 d D . . F5 F 0.4260(5) 0.3221(6) 0.1836(4) 0.245(8) Uani 1 1 d D . . F6 F 0.4723(4) 0.3939(5) 0.1670(3) 0.191(5) Uani 1 1 d DU . . C1 C 0.5817(3) 0.9183(3) 1.0186(2) 0.0403(18) Uani 1 1 d . . . C2 C 0.5656(3) 0.9463(3) 1.0377(2) 0.048(2) Uani 1 1 d . . . H2 H 0.5667 0.9461 1.0608 0.057 Uiso 1 1 calc R . . C3 C 0.5479(3) 0.9745(3) 1.0204(3) 0.053(2) Uani 1 1 d . . . H3 H 0.5356 0.9932 1.0322 0.064 Uiso 1 1 calc R . . C4 C 0.5479(3) 0.9759(3) 0.9871(3) 0.054(2) Uani 1 1 d . . . H4 H 0.5366 0.9964 0.9766 0.065 Uiso 1 1 calc R . . C5 C 0.5635(3) 0.9488(3) 0.9684(2) 0.0434(18) Uani 1 1 d . . . H5 H 0.5627 0.9500 0.9454 0.052 Uiso 1 1 calc R . . C6 C 0.5804(3) 0.9199(3) 0.9842(2) 0.0405(17) Uani 1 1 d . . . C7 C 0.6066(3) 0.8697(3) 0.9990(2) 0.0461(19) Uani 1 1 d . . . C8 C 0.6165(3) 0.8290(3) 0.9972(2) 0.0419(18) Uani 1 1 d . . . C9 C 0.6169(3) 0.7622(3) 1.0125(2) 0.0420(18) Uani 1 1 d . . . C10 C 0.6144(3) 0.7199(3) 1.0279(2) 0.051(2) Uani 1 1 d . . . H10 H 0.6145 0.7179 1.0509 0.062 Uiso 1 1 calc R . . C11 C 0.6118(4) 0.6808(3) 1.0088(2) 0.053(2) Uani 1 1 d . . . H11 H 0.6083 0.6510 1.0188 0.064 Uiso 1 1 calc R . . C12 C 0.6141(3) 0.6849(3) 0.9752(3) 0.056(2) Uani 1 1 d . . . H12 H 0.6142 0.6584 0.9629 0.067 Uiso 1 1 calc R . . C13 C 0.6163(3) 0.7273(3) 0.9582(2) 0.052(2) Uani 1 1 d . . . H13 H 0.6164 0.7293 0.9352 0.062 Uiso 1 1 calc R . . C14 C 0.6183(3) 0.7649(3) 0.9780(2) 0.0431(18) Uani 1 1 d . . . C15 C 0.5076(3) 0.8164(3) 1.0757(2) 0.048(2) Uani 1 1 d . . . H15 H 0.5203 0.8520 1.0745 0.057 Uiso 1 1 calc R . . C16 C 0.4568(3) 0.7853(3) 1.0803(2) 0.0449(18) Uani 1 1 d . . . H16 H 0.4347 0.7990 1.0824 0.054 Uiso 1 1 calc R . . C17 C 0.4380(3) 0.7334(3) 1.08201(19) 0.0429(18) Uani 1 1 d . . . C18 C 0.4714(3) 0.7153(3) 1.0803(2) 0.0433(18) Uani 1 1 d . . . H18 H 0.4593 0.6798 1.0823 0.052 Uiso 1 1 calc R . . C19 C 0.5229(3) 0.7492(3) 1.0756(2) 0.0456(19) Uani 1 1 d . . . H19 H 0.5459 0.7365 1.0744 0.055 Uiso 1 1 calc R . . C20 C 0.3827(3) 0.6983(3) 1.08454(18) 0.0375(16) Uani 1 1 d . . . C21 C 0.5053(3) 0.8224(3) 0.9225(2) 0.0415(18) Uani 1 1 d . . . H21 H 0.5168 0.8578 0.9242 0.050 Uiso 1 1 calc R . . C22 C 0.4551(3) 0.7899(3) 0.9181(2) 0.0467(19) Uani 1 1 d . . . H22 H 0.4322 0.8026 0.9163 0.056 Uiso 1 1 calc R . . C23 C 0.4367(3) 0.7371(3) 0.91620(19) 0.0377(16) Uani 1 1 d . . . C24 C 0.4719(3) 0.7204(3) 0.9166(2) 0.0465(19) Uani 1 1 d . . . H24 H 0.4615 0.6854 0.9140 0.056 Uiso 1 1 calc R . . C25 C 0.5232(3) 0.7570(3) 0.9211(2) 0.0417(18) Uani 1 1 d . . . H25 H 0.5473 0.7458 0.9218 0.050 Uiso 1 1 calc R . . C26 C 0.3818(3) 0.6993(3) 0.91460(19) 0.0382(16) Uani 1 1 d . . . C27 C 0.6414(3) 0.8944(3) 1.1105(2) 0.053(2) Uani 1 1 d . . . C28 C 0.6418(4) 0.8461(3) 1.1145(2) 0.054(2) Uani 1 1 d . . . C29 C 0.6778(3) 0.8463(3) 1.0932(2) 0.054(2) Uani 1 1 d . . . C30 C 0.7011(4) 0.8932(4) 1.0747(3) 0.058(2) Uani 1 1 d . . . C31 C 0.6783(3) 0.9212(3) 1.0864(2) 0.052(2) Uani 1 1 d . . . C32 C 0.6128(4) 0.9118(4) 1.1297(3) 0.070(3) Uani 1 1 d . . . H32A H 0.6315 0.9277 1.1497 0.105 Uiso 1 1 calc R . . H32B H 0.5794 0.8828 1.1351 0.105 Uiso 1 1 calc R . . H32C H 0.6083 0.9368 1.1172 0.105 Uiso 1 1 calc R . . C33 C 0.6099(4) 0.8057(3) 1.1390(2) 0.062(3) Uani 1 1 d . . . H33A H 0.6104 0.7743 1.1341 0.093 Uiso 1 1 calc R . . H33B H 0.5747 0.7990 1.1381 0.093 Uiso 1 1 calc R . . H33C H 0.6238 0.8175 1.1608 0.093 Uiso 1 1 calc R . . C34 C 0.6909(4) 0.8053(4) 1.0903(3) 0.069(3) Uani 1 1 d . . . H34A H 0.7271 0.8192 1.0953 0.104 Uiso 1 1 calc R . . H34B H 0.6841 0.7918 1.0681 0.104 Uiso 1 1 calc R . . H34C H 0.6702 0.7778 1.1056 0.104 Uiso 1 1 calc R . . C35 C 0.7418(4) 0.9099(4) 1.0501(3) 0.084(4) Uani 1 1 d . . . H35A H 0.7418 0.9363 1.0364 0.126 Uiso 1 1 calc R . . H35B H 0.7358 0.8807 1.0366 0.126 Uiso 1 1 calc R . . H35C H 0.7749 0.9237 1.0610 0.126 Uiso 1 1 calc R . . C36 C 0.6916(4) 0.9738(3) 1.0741(3) 0.062(3) Uani 1 1 d . . . H36A H 0.7254 0.9900 1.0639 0.093 Uiso 1 1 calc R . . H36B H 0.6918 0.9946 1.0923 0.093 Uiso 1 1 calc R . . H36C H 0.6662 0.9704 1.0580 0.093 Uiso 1 1 calc R . . C37 C 0.6767(3) 0.9339(3) 0.9133(3) 0.058(2) Uani 1 1 d . . . C38 C 0.6994(3) 0.9046(4) 0.9219(3) 0.061(3) Uani 1 1 d . . . C39 C 0.6788(3) 0.8611(4) 0.9010(2) 0.058(2) Uani 1 1 d . . . C40 C 0.6410(4) 0.8612(4) 0.8813(2) 0.062(3) Uani 1 1 d . . . C41 C 0.6399(3) 0.9085(4) 0.8895(3) 0.060(3) Uani 1 1 d . . . C42 C 0.6904(5) 0.9829(4) 0.9291(3) 0.090(4) Uani 1 1 d . . . H42A H 0.7217 1.0102 0.9193 0.135 Uiso 1 1 calc R . . H42B H 0.6960 0.9807 0.9523 0.135 Uiso 1 1 calc R . . H42C H 0.6628 0.9904 0.9261 0.135 Uiso 1 1 calc R . . C43 C 0.7419(4) 0.9181(5) 0.9467(3) 0.097(4) Uani 1 1 d . . . H43A H 0.7748 0.9337 0.9356 0.146 Uiso 1 1 calc R . . H43B H 0.7361 0.8870 0.9579 0.146 Uiso 1 1 calc R . . H43C H 0.7419 0.9421 0.9626 0.146 Uiso 1 1 calc R . . C44 C 0.6962(5) 0.8221(5) 0.9017(3) 0.089(4) Uani 1 1 d . . . H44A H 0.7093 0.8203 0.8803 0.134 Uiso 1 1 calc R . . H44B H 0.6674 0.7886 0.9073 0.134 Uiso 1 1 calc R . . H44C H 0.7232 0.8321 0.9179 0.134 Uiso 1 1 calc R . . C45 C 0.6095(5) 0.8252(5) 0.8553(3) 0.092(4) Uani 1 1 d . . . H45A H 0.6285 0.8352 0.8348 0.138 Uiso 1 1 calc R . . H45B H 0.5778 0.8261 0.8528 0.138 Uiso 1 1 calc R . . H45C H 0.6016 0.7906 0.8611 0.138 Uiso 1 1 calc R . . C46 C 0.6093(5) 0.9275(5) 0.8711(3) 0.091(4) Uani 1 1 d . . . H46A H 0.6053 0.9519 0.8845 0.136 Uiso 1 1 calc R . . H46B H 0.5756 0.8986 0.8658 0.136 Uiso 1 1 calc R . . H46C H 0.6271 0.9441 0.8510 0.136 Uiso 1 1 calc R . . C47 C 0.4928(5) 0.5830(6) 0.0833(4) 0.095(4) Uani 1 1 d . . . C48 C 0.4211(7) 0.3575(7) 0.1648(6) 0.178(9) Uiso 1 1 d D . . C49 C 0.4349(3) 0.6852(4) 0.9994(2) 0.055(2) Uani 1 1 d . . . C50 C 0.3839(3) 0.6763(3) 0.99950(19) 0.048(2) Uani 1 1 d . . . C51 C 0.3432(3) 0.6255(3) 0.99935(19) 0.0459(19) Uani 1 1 d . . . C52 C 0.3526(4) 0.5839(4) 0.9999(2) 0.057(2) Uani 1 1 d . . . C53 C 0.4032(5) 0.5944(5) 1.0009(2) 0.068(3) Uani 1 1 d . . . H53 H 0.4097 0.5669 1.0019 0.082 Uiso 1 1 calc R . . C54 C 0.4431(4) 0.6426(5) 1.0003(2) 0.066(3) Uani 1 1 d . . . H54 H 0.4769 0.6483 1.0005 0.079 Uiso 1 1 calc R . . C55 C 0.4756(4) 0.7385(5) 0.9993(2) 0.068(3) Uani 1 1 d . . . H55 H 0.5099 0.7458 0.9990 0.082 Uiso 1 1 calc R . . C56 C 0.4665(4) 0.7770(4) 0.9996(2) 0.057(2) Uani 1 1 d . . . H56 H 0.4944 0.8109 0.9997 0.069 Uiso 1 1 calc R . . C57 C 0.3318(6) 0.7605(5) 0.1660(3) 0.086(4) Uani 1 1 d . . . C58 C 0.3313(5) 0.7131(5) 0.1666(3) 0.074(3) Uani 1 1 d . . . C59 C 0.3735(7) 0.8049(6) 0.1655(4) 0.106(5) Uani 1 1 d . . . H59 H 0.3718 0.8354 0.1650 0.128 Uiso 1 1 calc R . . C60 C 0.2840(7) 0.7581(7) 0.1678(3) 0.112(5) Uani 1 1 d . . . H60 H 0.2825 0.7886 0.1689 0.134 Uiso 1 1 calc R . . C61 C 0.5126(6) 0.4154(6) 0.0647(4) 0.110(5) Uiso 1 1 d . . . C62 C 0.5082(9) 0.9432(10) 0.8765(6) 0.181(9) Uiso 1 1 d . . . O7 O 0.5311(5) 0.3984(5) 0.0917(3) 0.154(5) Uiso 1 1 d . . . O8 O 0.4787(8) 0.8891(9) 0.8650(5) 0.256(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.04329(18) 0.04061(18) 0.0401(2) 0.00450(13) 0.00493(13) 0.02080(14) Ir2 0.03432(16) 0.04295(18) 0.0402(2) 0.00730(13) 0.00935(13) 0.01620(13) N1 0.047(4) 0.040(3) 0.041(4) 0.003(3) 0.003(3) 0.025(3) N2 0.040(3) 0.040(3) 0.047(4) 0.003(3) 0.006(3) 0.023(3) N3 0.041(3) 0.040(3) 0.048(4) 0.003(3) 0.007(3) 0.024(3) N4 0.037(3) 0.036(3) 0.046(4) 0.010(3) 0.009(3) 0.019(3) N5 0.048(4) 0.039(3) 0.041(4) 0.007(3) 0.007(3) 0.023(3) N6 0.044(4) 0.043(4) 0.036(4) -0.001(3) 0.000(3) 0.016(3) N7 0.042(3) 0.040(3) 0.046(4) 0.005(3) 0.012(3) 0.024(3) N8 0.031(3) 0.043(3) 0.046(4) -0.004(3) 0.004(3) 0.019(3) O1 0.155(10) 0.101(8) 0.275(18) -0.035(9) -0.040(11) 0.086(8) O2 0.224(13) 0.188(12) 0.105(9) 0.029(9) -0.036(9) 0.024(10) O3 0.084(7) 0.178(11) 0.159(11) -0.024(9) 0.030(7) 0.057(7) O4 0.084(7) 0.189(12) 0.141(11) -0.050(9) -0.004(7) 0.014(8) O5 0.125(9) 0.173(11) 0.273(18) 0.134(12) 0.087(10) 0.103(9) O6 0.119(7) 0.127(7) 0.103(7) -0.014(6) 0.017(6) 0.087(6) S1 0.0739(17) 0.0752(18) 0.077(2) -0.0007(15) 0.0009(15) 0.0414(15) S2 0.090(3) 0.129(3) 0.131(4) -0.050(3) 0.012(2) 0.042(2) F1 0.183(11) 0.112(7) 0.186(11) -0.045(7) -0.080(9) 0.055(7) F2 0.102(7) 0.265(13) 0.276(14) -0.095(10) -0.008(8) 0.093(8) F3 0.209(14) 0.265(17) 0.238(17) 0.013(14) -0.102(13) 0.134(13) F4 0.111(6) 0.173(9) 0.151(9) -0.067(7) 0.016(6) 0.070(6) F5 0.156(11) 0.244(16) 0.30(2) 0.021(15) -0.086(12) 0.078(11) F6 0.125(6) 0.197(8) 0.147(7) -0.054(6) 0.006(6) 0.002(5) C1 0.035(4) 0.029(3) 0.057(5) 0.004(3) 0.002(4) 0.016(3) C2 0.047(4) 0.039(4) 0.056(5) -0.003(4) 0.013(4) 0.020(4) C3 0.045(5) 0.039(4) 0.079(7) 0.001(4) 0.008(5) 0.023(4) C4 0.045(5) 0.040(4) 0.081(7) 0.010(4) 0.003(5) 0.025(4) C5 0.039(4) 0.038(4) 0.052(5) 0.005(4) 0.006(4) 0.018(3) C6 0.033(4) 0.036(4) 0.047(5) 0.003(3) 0.002(3) 0.012(3) C7 0.055(5) 0.045(4) 0.043(5) 0.010(4) 0.011(4) 0.029(4) C8 0.042(4) 0.044(4) 0.044(5) 0.005(4) 0.008(4) 0.024(3) C9 0.048(4) 0.040(4) 0.049(5) 0.004(4) 0.001(4) 0.030(4) C10 0.052(5) 0.044(4) 0.064(6) 0.012(4) 0.005(4) 0.029(4) C11 0.072(6) 0.050(5) 0.052(6) 0.004(4) 0.007(5) 0.041(5) C12 0.049(5) 0.046(5) 0.082(7) 0.000(5) 0.007(5) 0.032(4) C13 0.051(5) 0.050(5) 0.056(6) -0.002(4) 0.012(4) 0.027(4) C14 0.046(4) 0.043(4) 0.049(5) 0.007(4) 0.008(4) 0.028(4) C15 0.042(4) 0.041(4) 0.055(6) 0.001(4) 0.004(4) 0.017(4) C16 0.050(5) 0.043(4) 0.042(5) 0.000(4) -0.003(4) 0.023(4) C17 0.056(5) 0.050(4) 0.033(4) -0.008(3) -0.009(4) 0.035(4) C18 0.055(5) 0.037(4) 0.040(5) 0.005(3) -0.002(4) 0.025(4) C19 0.054(5) 0.045(4) 0.048(5) 0.003(4) -0.002(4) 0.032(4) C20 0.050(4) 0.040(4) 0.025(4) 0.003(3) 0.006(3) 0.024(3) C21 0.048(4) 0.036(4) 0.040(5) 0.005(3) -0.001(4) 0.022(3) C22 0.053(5) 0.047(4) 0.052(5) 0.005(4) 0.004(4) 0.034(4) C23 0.038(4) 0.042(4) 0.033(4) 0.000(3) -0.006(3) 0.019(3) C24 0.055(5) 0.039(4) 0.050(5) -0.010(4) -0.006(4) 0.027(4) C25 0.035(4) 0.044(4) 0.048(5) -0.001(4) 0.008(3) 0.021(3) C26 0.038(4) 0.044(4) 0.034(4) 0.002(3) 0.002(3) 0.021(3) C27 0.061(5) 0.045(5) 0.042(5) -0.001(4) -0.009(4) 0.020(4) C28 0.061(5) 0.059(5) 0.046(5) -0.002(4) 0.000(4) 0.032(5) C29 0.055(5) 0.049(5) 0.066(6) -0.001(4) -0.008(5) 0.031(4) C30 0.054(5) 0.058(5) 0.061(6) 0.000(5) 0.005(5) 0.028(5) C31 0.048(5) 0.041(4) 0.050(5) -0.003(4) -0.008(4) 0.010(4) C32 0.095(8) 0.068(6) 0.061(7) 0.005(5) 0.003(6) 0.052(6) C33 0.092(7) 0.051(5) 0.049(6) 0.007(4) 0.005(5) 0.041(5) C34 0.068(6) 0.080(7) 0.080(8) -0.003(6) -0.012(6) 0.052(6) C35 0.060(6) 0.079(7) 0.092(9) -0.010(7) 0.019(6) 0.020(6) C36 0.061(6) 0.040(5) 0.084(8) 0.004(5) -0.009(5) 0.024(4) C37 0.042(5) 0.050(5) 0.069(7) 0.014(5) 0.021(5) 0.012(4) C38 0.034(4) 0.064(6) 0.069(7) 0.010(5) 0.004(4) 0.012(4) C39 0.052(5) 0.068(6) 0.061(6) 0.022(5) 0.026(5) 0.036(5) C40 0.047(5) 0.073(6) 0.047(6) 0.009(5) 0.027(4) 0.016(5) C41 0.049(5) 0.073(6) 0.061(6) 0.029(5) 0.029(5) 0.032(5) C42 0.071(7) 0.063(7) 0.105(10) 0.007(7) 0.022(7) 0.010(6) C43 0.050(6) 0.136(11) 0.088(10) 0.000(8) 0.003(6) 0.033(7) C44 0.081(8) 0.115(10) 0.093(10) 0.024(8) 0.034(7) 0.065(8) C45 0.101(9) 0.116(10) 0.042(6) -0.007(6) 0.029(6) 0.042(8) C46 0.095(8) 0.128(11) 0.079(9) 0.057(8) 0.032(7) 0.078(8) C47 0.071(8) 0.109(11) 0.116(13) -0.019(9) -0.012(8) 0.052(8) C49 0.054(5) 0.075(6) 0.034(5) 0.001(4) 0.001(4) 0.030(5) C50 0.059(5) 0.053(5) 0.026(4) 0.001(4) 0.003(4) 0.024(4) C51 0.054(5) 0.055(5) 0.029(4) -0.013(4) 0.001(4) 0.028(4) C52 0.077(6) 0.073(6) 0.028(5) -0.008(4) -0.005(4) 0.044(5) C53 0.099(8) 0.092(8) 0.041(6) 0.000(5) -0.002(5) 0.067(7) C54 0.066(6) 0.100(8) 0.045(6) -0.022(5) -0.005(5) 0.053(6) C55 0.048(5) 0.104(9) 0.049(6) 0.003(6) 0.007(4) 0.035(6) C56 0.057(5) 0.059(5) 0.038(5) 0.001(4) -0.003(4) 0.016(5) C57 0.110(10) 0.093(10) 0.063(8) -0.001(7) 0.004(7) 0.058(9) C58 0.076(6) 0.097(9) 0.045(6) 0.007(6) 0.010(5) 0.041(7) C59 0.150(14) 0.086(10) 0.086(10) 0.002(8) 0.011(10) 0.061(11) C60 0.129(12) 0.172(17) 0.079(10) 0.014(10) 0.015(9) 0.109(13) _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 N5 2.108(6) . ? Ir1 C28 2.139(10) . ? Ir1 C29 2.149(9) . ? Ir1 C31 2.155(8) . ? Ir1 N1 2.163(6) . ? Ir1 C27 2.167(9) . ? Ir1 C30 2.169(10) . ? Ir1 N2 2.186(7) . ? Ir2 N7 2.106(6) . ? Ir2 C40 2.130(9) . ? Ir2 C41 2.139(9) . ? Ir2 C38 2.157(8) . ? Ir2 N3 2.167(7) . ? Ir2 C39 2.167(8) . ? Ir2 N4 2.172(7) . ? Ir2 C37 2.184(8) . ? N1 C7 1.321(10) . ? N1 C1 1.391(9) . ? N2 C8 1.333(10) . ? N2 C9 1.376(9) . ? N3 C8 1.312(10) . ? N3 C14 1.417(9) . ? N4 C7 1.335(10) . ? N4 C6 1.383(10) . ? N5 C19 1.344(10) . ? N5 C15 1.350(10) . ? N6 C20 1.324(9) 2_665 ? N6 C20 1.344(9) . ? N7 C25 1.338(10) . ? N7 C21 1.359(10) . ? N8 C26 1.324(9) . ? N8 C26 1.334(9) 3_565 ? O1 S1 1.367(10) . ? O2 S1 1.333(14) . ? O3 S1 1.440(10) . ? O4 S2 1.432(11) . ? O5 S2 1.515(11) . ? O6 S2 1.474(9) . ? S1 C47 1.721(14) . ? S2 C48 1.63(2) . ? F1 C47 1.267(17) . ? F2 C47 1.313(16) . ? F3 C47 1.32(2) . ? F4 C48 1.377(16) . ? F5 C48 1.391(16) . ? F6 C48 1.385(16) . ? C1 C2 1.409(11) . ? C1 C6 1.421(12) . ? C2 C3 1.411(12) . ? C3 C4 1.374(13) . ? C4 C5 1.370(12) . ? C5 C6 1.381(11) . ? C7 C8 1.411(12) . ? C9 C10 1.401(10) . ? C9 C14 1.420(12) . ? C10 C11 1.391(12) . ? C11 C12 1.390(13) . ? C12 C13 1.433(12) . ? C13 C14 1.378(11) . ? C15 C16 1.358(11) . ? C16 C17 1.381(11) . ? C17 C18 1.372(11) . ? C17 C20 1.473(11) . ? C18 C19 1.389(11) . ? C20 N6 1.323(9) 3_565 ? C21 C22 1.349(11) . ? C22 C23 1.408(11) . ? C23 C24 1.392(11) . ? C23 C26 1.476(10) . ? C24 C25 1.397(11) . ? C26 N8 1.334(9) 2_665 ? C27 C31 1.410(13) . ? C27 C32 1.454(14) . ? C27 C28 1.479(12) . ? C28 C29 1.397(13) . ? C28 C33 1.507(13) . ? C29 C30 1.448(13) . ? C29 C34 1.488(12) . ? C30 C31 1.418(13) . ? C30 C35 1.478(14) . ? C31 C36 1.522(12) . ? C37 C41 1.394(14) . ? C37 C38 1.415(14) . ? C37 C42 1.478(15) . ? C38 C39 1.431(14) . ? C38 C43 1.531(15) . ? C39 C40 1.401(14) . ? C39 C44 1.519(14) . ? C40 C45 1.487(16) . ? C40 C41 1.490(14) . ? C41 C46 1.516(14) . ? C49 C50 1.428(12) . ? C49 C54 1.430(14) . ? C49 C55 1.462(14) . ? C50 C51 1.411(11) . ? C50 C51 1.419(12) 2_665 ? C51 C50 1.419(12) 3_565 ? C51 C52 1.425(12) . ? C52 C53 1.403(14) . ? C52 C56 1.420(14) 3_565 ? C53 C54 1.352(16) . ? C55 C56 1.326(15) . ? C56 C52 1.420(14) 2_665 ? C57 C59 1.307(18) . ? C57 C60 1.414(19) . ? C57 C58 1.431(16) . ? C58 C58 1.438(12) 15 ? C58 C58 1.439(12) 14_455 ? C59 C60 1.52(2) 14_455 ? C60 C59 1.52(2) 15 ? C61 O7 1.454(19) . ? C62 O8 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 N5 Ir1 C28 96.0(3) . . ? N5 Ir1 C29 123.1(3) . . ? C28 Ir1 C29 38.0(3) . . ? N5 Ir1 C31 138.0(3) . . ? C28 Ir1 C31 64.4(4) . . ? C29 Ir1 C31 63.9(3) . . ? N5 Ir1 N1 87.9(2) . . ? C28 Ir1 N1 153.5(3) . . ? C29 Ir1 N1 148.9(3) . . ? C31 Ir1 N1 95.5(3) . . ? N5 Ir1 C27 102.9(3) . . ? C28 Ir1 C27 40.2(3) . . ? C29 Ir1 C27 65.5(3) . . ? C31 Ir1 C27 38.1(3) . . ? N1 Ir1 C27 113.4(3) . . ? N5 Ir1 C30 160.9(3) . . ? C28 Ir1 C30 65.2(4) . . ? C29 Ir1 C30 39.2(4) . . ? C31 Ir1 C30 38.3(3) . . ? N1 Ir1 C30 110.4(3) . . ? C27 Ir1 C30 65.6(4) . . ? N5 Ir1 N2 88.4(2) . . ? C28 Ir1 N2 127.6(3) . . ? C29 Ir1 N2 98.2(3) . . ? C31 Ir1 N2 133.3(3) . . ? N1 Ir1 N2 78.6(2) . . ? C27 Ir1 N2 163.5(3) . . ? C30 Ir1 N2 100.2(3) . . ? N7 Ir2 C40 97.7(3) . . ? N7 Ir2 C41 105.3(3) . . ? C40 Ir2 C41 40.9(4) . . ? N7 Ir2 C38 162.5(3) . . ? C40 Ir2 C38 65.2(4) . . ? C41 Ir2 C38 64.6(4) . . ? N7 Ir2 N3 87.3(2) . . ? C40 Ir2 N3 127.6(3) . . ? C41 Ir2 N3 163.1(3) . . ? C38 Ir2 N3 100.2(3) . . ? N7 Ir2 C39 124.9(3) . . ? C40 Ir2 C39 38.0(4) . . ? C41 Ir2 C39 65.1(3) . . ? C38 Ir2 C39 38.7(4) . . ? N3 Ir2 C39 98.6(3) . . ? N7 Ir2 N4 87.4(2) . . ? C40 Ir2 N4 153.2(3) . . ? C41 Ir2 N4 112.4(3) . . ? C38 Ir2 N4 109.5(3) . . ? N3 Ir2 N4 78.8(2) . . ? C39 Ir2 N4 147.6(3) . . ? N7 Ir2 C37 139.6(3) . . ? C40 Ir2 C37 65.0(4) . . ? C41 Ir2 C37 37.6(4) . . ? C38 Ir2 C37 38.0(4) . . ? N3 Ir2 C37 132.7(3) . . ? C39 Ir2 C37 63.6(4) . . ? N4 Ir2 C37 94.2(3) . . ? C7 N1 C1 103.0(7) . . ? C7 N1 Ir1 109.5(5) . . ? C1 N1 Ir1 147.6(6) . . ? C8 N2 C9 103.2(7) . . ? C8 N2 Ir1 108.3(5) . . ? C9 N2 Ir1 148.5(6) . . ? C8 N3 C14 102.0(7) . . ? C8 N3 Ir2 109.5(5) . . ? C14 N3 Ir2 148.4(6) . . ? C7 N4 C6 102.9(7) . . ? C7 N4 Ir2 108.3(5) . . ? C6 N4 Ir2 148.8(5) . . ? C19 N5 C15 117.4(7) . . ? C19 N5 Ir1 121.1(5) . . ? C15 N5 Ir1 121.5(5) . . ? C20 N6 C20 117.0(8) 2_665 . ? C25 N7 C21 117.1(7) . . ? C25 N7 Ir2 120.9(5) . . ? C21 N7 Ir2 121.9(5) . . ? C26 N8 C26 115.4(7) . 3_565 ? O2 S1 O1 121.7(11) . . ? O2 S1 O3 113.6(11) . . ? O1 S1 O3 108.7(9) . . ? O2 S1 C47 104.5(9) . . ? O1 S1 C47 105.9(8) . . ? O3 S1 C47 99.7(7) . . ? O4 S2 O6 119.5(8) . . ? O4 S2 O5 114.1(9) . . ? O6 S2 O5 117.8(7) . . ? O4 S2 C48 103.4(9) . . ? O6 S2 C48 105.0(8) . . ? O5 S2 C48 90.6(10) . . ? N1 C1 C2 131.1(8) . . ? N1 C1 C6 107.9(7) . . ? C2 C1 C6 121.0(7) . . ? C1 C2 C3 115.7(8) . . ? C4 C3 C2 121.9(8) . . ? C5 C4 C3 122.6(8) . . ? C4 C5 C6 117.8(8) . . ? C5 C6 N4 131.0(8) . . ? C5 C6 C1 121.0(7) . . ? N4 C6 C1 108.0(7) . . ? N1 C7 N4 118.1(7) . . ? N1 C7 C8 120.7(7) . . ? N4 C7 C8 120.7(8) . . ? N3 C8 N2 118.9(7) . . ? N3 C8 C7 120.2(8) . . ? N2 C8 C7 120.2(7) . . ? N2 C9 C10 132.4(8) . . ? N2 C9 C14 108.1(6) . . ? C10 C9 C14 119.5(7) . . ? C11 C10 C9 118.4(9) . . ? C12 C11 C10 120.7(8) . . ? C11 C12 C13 122.9(8) . . ? C14 C13 C12 114.5(9) . . ? C13 C14 N3 128.2(8) . . ? C13 C14 C9 123.9(7) . . ? N3 C14 C9 107.7(7) . . ? N5 C15 C16 124.0(8) . . ? C15 C16 C17 118.3(8) . . ? C18 C17 C16 119.1(8) . . ? C18 C17 C20 120.9(7) . . ? C16 C17 C20 119.9(7) . . ? C17 C18 C19 119.4(7) . . ? N5 C19 C18 121.7(7) . . ? N6 C20 N6 123.1(8) 3_565 . ? N6 C20 C17 117.9(7) 3_565 . ? N6 C20 C17 119.0(7) . . ? C22 C21 N7 123.0(7) . . ? C21 C22 C23 119.9(7) . . ? C24 C23 C22 118.2(7) . . ? C24 C23 C26 119.4(7) . . ? C22 C23 C26 122.4(7) . . ? C23 C24 C25 117.6(7) . . ? N7 C25 C24 124.0(7) . . ? N8 C26 N8 124.6(7) . 2_665 ? N8 C26 C23 118.5(7) . . ? N8 C26 C23 116.9(7) 2_665 . ? C31 C27 C32 128.2(8) . . ? C31 C27 C28 104.6(8) . . ? C32 C27 C28 126.9(8) . . ? C31 C27 Ir1 70.5(5) . . ? C32 C27 Ir1 129.1(7) . . ? C28 C27 Ir1 68.9(5) . . ? C29 C28 C27 108.5(8) . . ? C29 C28 C33 127.4(8) . . ? C27 C28 C33 124.0(8) . . ? C29 C28 Ir1 71.4(5) . . ? C27 C28 Ir1 70.9(5) . . ? C33 C28 Ir1 125.8(7) . . ? C28 C29 C30 109.4(8) . . ? C28 C29 C34 125.5(9) . . ? C30 C29 C34 125.1(9) . . ? C28 C29 Ir1 70.6(5) . . ? C30 C29 Ir1 71.2(5) . . ? C34 C29 Ir1 125.3(7) . . ? C31 C30 C29 105.3(8) . . ? C31 C30 C35 127.0(9) . . ? C29 C30 C35 127.6(9) . . ? C31 C30 Ir1 70.3(5) . . ? C29 C30 Ir1 69.7(5) . . ? C35 C30 Ir1 126.6(8) . . ? C27 C31 C30 112.2(8) . . ? C27 C31 C36 123.9(9) . . ? C30 C31 C36 124.0(9) . . ? C27 C31 Ir1 71.4(5) . . ? C30 C31 Ir1 71.4(5) . . ? C36 C31 Ir1 124.4(6) . . ? C41 C37 C38 109.7(9) . . ? C41 C37 C42 127.6(10) . . ? C38 C37 C42 122.6(11) . . ? C41 C37 Ir2 69.4(5) . . ? C38 C37 Ir2 70.0(5) . . ? C42 C37 Ir2 125.3(7) . . ? C37 C38 C39 107.4(9) . . ? C37 C38 C43 127.5(11) . . ? C39 C38 C43 124.9(10) . . ? C37 C38 Ir2 72.0(5) . . ? C39 C38 Ir2 71.1(5) . . ? C43 C38 Ir2 126.5(7) . . ? C40 C39 C38 109.2(8) . . ? C40 C39 C44 127.9(11) . . ? C38 C39 C44 122.8(10) . . ? C40 C39 Ir2 69.5(5) . . ? C38 C39 Ir2 70.3(5) . . ? C44 C39 Ir2 125.5(7) . . ? C39 C40 C45 129.8(11) . . ? C39 C40 C41 106.4(9) . . ? C45 C40 C41 123.6(11) . . ? C39 C40 Ir2 72.4(6) . . ? C45 C40 Ir2 125.9(7) . . ? C41 C40 Ir2 69.9(5) . . ? C37 C41 C40 107.0(9) . . ? C37 C41 C46 128.0(11) . . ? C40 C41 C46 124.4(11) . . ? C37 C41 Ir2 73.0(6) . . ? C40 C41 Ir2 69.3(5) . . ? C46 C41 Ir2 129.4(6) . . ? F1 C47 F2 107.4(14) . . ? F1 C47 F3 103.7(15) . . ? F2 C47 F3 95.0(14) . . ? F1 C47 S1 118.7(11) . . ? F2 C47 S1 114.2(12) . . ? F3 C47 S1 114.9(13) . . ? F4 C48 F6 111.4(16) . . ? F4 C48 F5 116.1(19) . . ? F6 C48 F5 93.9(16) . . ? F4 C48 S2 115.7(14) . . ? F6 C48 S2 115.2(15) . . ? F5 C48 S2 102.5(15) . . ? C50 C49 C54 119.2(9) . . ? C50 C49 C55 116.4(9) . . ? C54 C49 C55 124.4(9) . . ? C51 C50 C51 120.6(9) . 2_665 ? C51 C50 C49 118.8(8) . . ? C51 C50 C49 120.7(8) 2_665 . ? C50 C51 C50 119.4(8) . 3_565 ? C50 C51 C52 120.6(8) . . ? C50 C51 C52 119.9(8) 3_565 . ? C53 C52 C56 122.5(9) . 3_565 ? C53 C52 C51 118.7(9) . . ? C56 C52 C51 118.8(9) 3_565 . ? C54 C53 C52 122.0(10) . . ? C53 C54 C49 120.7(9) . . ? C56 C55 C49 122.7(9) . . ? C55 C56 C52 121.5(9) . 2_665 ? C59 C57 C60 119.6(13) . . ? C59 C57 C58 123.6(14) . . ? C60 C57 C58 116.7(13) . . ? C57 C58 C58 122.7(12) . 15 ? C57 C58 C58 117.3(12) . 14_455 ? C58 C58 C58 120.003(11) 15 14_455 ? C57 C59 C60 119.4(14) . 14_455 ? C57 C60 C59 120.1(15) . 15 ? 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 0.000 2571.6 587.5 2 0.667 0.333 0.333 2566.2 587.0 3 0.483 0.075 0.871 27.3 -2.1 4 0.258 0.074 0.538 26.7 -2.4 5 0.740 0.149 0.795 26.5 -2.3 6 0.926 0.184 0.538 26.6 -2.0 7 0.184 0.258 0.462 26.8 -2.3 8 0.409 0.259 0.795 26.4 -2.0 9 0.333 0.667 0.667 2566.2 586.8 10 0.149 0.409 0.205 26.6 -2.2 11 0.924 0.407 0.871 27.2 -2.5 12 0.407 0.483 0.129 27.0 -2.4 13 0.593 0.517 0.871 27.0 -2.2 14 0.851 0.591 0.795 26.6 -2.3 15 0.075 0.593 0.129 27.2 -2.1 16 0.816 0.742 0.538 26.8 -2.1 17 0.591 0.740 0.205 26.5 -2.5 18 0.074 0.816 0.462 26.6 -2.2 19 0.260 0.851 0.205 26.5 -2.1 20 0.517 0.924 0.129 27.3 -2.3 21 0.742 0.926 0.462 26.7 -1.9 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.854 _refine_diff_density_min -1.597 _refine_diff_density_rms 0.198 # Attachment 'Ir-tpt-hollowcage-3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 864534' #TrackingRef 'Ir-tpt-hollowcage-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H154 F18 Ir6 N24 O24 S6' _chemical_formula_weight 4316.49 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 20.861(3) _cell_length_b 33.223(5) _cell_length_c 28.731(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.195(2) _cell_angle_gamma 90.00 _cell_volume 19022(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9816 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.46 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8440 _exptl_absorpt_coefficient_mu 4.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2463 _exptl_absorpt_correction_T_max 0.6248 _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_% 7.33 _diffrn_reflns_number 103769 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1170 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 32977 _reflns_number_gt 16398 _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. ; _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^)+(0.1684P)^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 32977 _refine_ls_number_parameters 1515 _refine_ls_number_restraints 254 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2840 _refine_ls_wR_factor_gt 0.2510 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.84667(3) 0.742239(17) 0.78764(2) 0.05167(19) Uani 1 1 d . . . Ir2 Ir 0.71230(3) 0.743860(18) 0.58776(2) 0.0546(2) Uani 1 1 d . . . Ir3 Ir 0.34967(4) 0.56039(2) 0.86213(3) 0.0766(3) Uani 1 1 d . . . Ir4 Ir 0.21868(3) 0.53807(2) 0.66407(3) 0.0681(2) Uani 1 1 d . . . Ir5 Ir 0.86491(4) 0.342401(18) 0.83113(3) 0.0663(2) Uani 1 1 d D . . Ir6 Ir 0.73331(3) 0.341971(18) 0.63108(3) 0.0660(2) Uani 1 1 d . . . N1 N 0.7575(5) 0.7665(3) 0.7351(4) 0.041(3) Uani 1 1 d . . . N2 N 0.8652(6) 0.7308(3) 0.7200(5) 0.053(3) Uani 1 1 d . . . N3 N 0.8131(5) 0.7316(3) 0.6391(4) 0.040(3) Uani 1 1 d . . . N4 N 0.7064(7) 0.7684(3) 0.6578(4) 0.047(3) Uani 1 1 d . . . N5 N 0.3031(7) 0.5124(3) 0.8106(5) 0.059(4) Uani 1 1 d . A . N6 N 0.2985(6) 0.5942(4) 0.7972(7) 0.076(5) Uani 1 1 d . . . N7 N 0.2434(6) 0.5853(3) 0.7189(5) 0.051(3) Uani 1 1 d . A . N8 N 0.2503(6) 0.5034(4) 0.7314(5) 0.062(4) Uani 1 1 d . A . N9 N 0.8831(7) 0.3532(3) 0.7627(5) 0.053(3) Uani 1 1 d . . . N10 N 0.7724(6) 0.3191(3) 0.7775(4) 0.045(3) Uani 1 1 d . . . N11 N 0.7190(6) 0.3194(3) 0.6981(6) 0.063(4) Uani 1 1 d . . . N12 N 0.8227(7) 0.3539(4) 0.6782(4) 0.061(4) Uani 1 1 d U . . N13 N 0.7934(7) 0.6867(4) 0.7756(6) 0.066(4) Uani 1 1 d . . . N14 N 0.4285(8) 0.5532(4) 0.8297(6) 0.083(5) Uani 1 1 d . . . N15 N 0.8130(7) 0.3974(4) 0.8200(7) 0.087(5) Uani 1 1 d . . . N16 N 0.7363(7) 0.5423(4) 0.7852(6) 0.074(4) Uani 1 1 d . . . N17 N 0.6363(7) 0.5765(4) 0.7854(5) 0.062(4) Uani 1 1 d . . . N18 N 0.6435(7) 0.5072(4) 0.8017(6) 0.072(4) Uani 1 1 d . . . N19 N 0.6852(6) 0.6903(3) 0.6170(4) 0.047(3) Uani 1 1 d . . . N20 N 0.3231(6) 0.5416(4) 0.6715(6) 0.067(4) Uani 1 1 d . A . N21 N 0.7083(5) 0.3980(3) 0.6555(5) 0.055(3) Uani 1 1 d U . . N22 N 0.6482(6) 0.5457(4) 0.6567(5) 0.067(4) Uani 1 1 d . . . N23 N 0.5492(7) 0.5808(4) 0.6621(6) 0.075(4) Uani 1 1 d . . . N24 N 0.5580(7) 0.5101(4) 0.6729(6) 0.074(4) Uani 1 1 d . . . C1 C 0.6925(7) 0.7810(3) 0.7296(6) 0.042(4) Uani 1 1 d . . . C2 C 0.6573(8) 0.7941(4) 0.7630(7) 0.064(5) Uani 1 1 d . . . H2 H 0.6786 0.7930 0.7971 0.077 Uiso 1 1 calc R . . C3 C 0.5952(9) 0.8079(5) 0.7462(6) 0.064(4) Uiso 1 1 d . . . H3 H 0.5726 0.8180 0.7680 0.077 Uiso 1 1 calc R . . C4 C 0.5651(10) 0.8074(6) 0.6990(7) 0.083(6) Uiso 1 1 d . . . H4 H 0.5197 0.8163 0.6892 0.099 Uiso 1 1 calc R . . C5 C 0.5898(8) 0.7961(5) 0.6627(6) 0.055(4) Uani 1 1 d . . . H5 H 0.5649 0.7977 0.6292 0.066 Uiso 1 1 calc R . . C6 C 0.6569(7) 0.7817(4) 0.6794(6) 0.041(3) Uani 1 1 d . . . C7 C 0.7574(6) 0.7612(3) 0.6913(5) 0.028(3) Uani 1 1 d U . . C8 C 0.8128(7) 0.7419(3) 0.6838(5) 0.035(3) Uani 1 1 d U . . C9 C 0.9059(6) 0.7094(3) 0.6948(5) 0.031(3) Uani 1 1 d . . . C10 C 0.9660(9) 0.6930(4) 0.7108(7) 0.068(5) Uani 1 1 d . . . H10 H 0.9893 0.6942 0.7446 0.081 Uiso 1 1 calc R . . C11 C 0.9958(9) 0.6743(5) 0.6799(8) 0.076(6) Uani 1 1 d . . . H11 H 1.0375 0.6608 0.6920 0.092 Uiso 1 1 calc R . . C12 C 0.9629(9) 0.6759(5) 0.6304(7) 0.062(4) Uani 1 1 d . . . H12 H 0.9837 0.6636 0.6087 0.074 Uiso 1 1 calc R . . C13 C 0.9018(8) 0.6943(4) 0.6111(6) 0.051(4) Uani 1 1 d . . . H13 H 0.8808 0.6957 0.5770 0.061 Uiso 1 1 calc R . . C14 C 0.8716(7) 0.7110(4) 0.6451(5) 0.040(3) Uani 1 1 d . . . C15 C 0.3033(12) 0.4706(5) 0.7980(12) 0.101(9) Uani 1 1 d . A . C16 C 0.3380(10) 0.4415(5) 0.8325(8) 0.084(6) Uani 1 1 d . . . H16 H 0.3596 0.4471 0.8659 0.101 Uiso 1 1 calc R . . C17 C 0.3366(12) 0.4021(7) 0.8106(11) 0.118(8) Uani 1 1 d U . . H17 H 0.3596 0.3800 0.8290 0.142 Uiso 1 1 calc R . . C18 C 0.2974(11) 0.3975(6) 0.7576(9) 0.096(6) Uani 1 1 d U . . H18 H 0.2927 0.3712 0.7441 0.116 Uiso 1 1 calc R . . C19 C 0.2686(11) 0.4280(5) 0.7282(9) 0.091(7) Uani 1 1 d . A . H19 H 0.2466 0.4244 0.6945 0.109 Uiso 1 1 calc R . . C20 C 0.2736(12) 0.4658(5) 0.7514(10) 0.088(7) Uani 1 1 d . . . C21 C 0.2684(9) 0.5280(4) 0.7680(7) 0.061(5) Uani 1 1 d . . . C22 C 0.2670(8) 0.5707(4) 0.7642(8) 0.056(5) Uani 1 1 d . A . C23 C 0.2980(8) 0.6317(4) 0.7755(8) 0.066(5) Uani 1 1 d . A . C24 C 0.3266(10) 0.6687(5) 0.7933(10) 0.096(7) Uani 1 1 d . . . H24 H 0.3499 0.6730 0.8267 0.116 Uiso 1 1 calc R . . C25 C 0.3185(11) 0.6992(5) 0.7584(9) 0.087(6) Uani 1 1 d U . . H25 H 0.3357 0.7253 0.7686 0.105 Uiso 1 1 calc R . . C26 C 0.2869(10) 0.6928(6) 0.7104(10) 0.095(7) Uani 1 1 d . . . H26 H 0.2837 0.7146 0.6884 0.114 Uiso 1 1 calc R . . C27 C 0.2588(9) 0.6560(5) 0.6917(7) 0.072(5) Uani 1 1 d . A . H27 H 0.2383 0.6518 0.6579 0.086 Uiso 1 1 calc R . . C28 C 0.2631(8) 0.6260(4) 0.7260(7) 0.060(5) Uani 1 1 d . . . C29 C 0.9248(7) 0.3736(4) 0.7376(6) 0.044(4) Uani 1 1 d . . . C30 C 0.9850(8) 0.3914(5) 0.7577(7) 0.071(5) Uani 1 1 d . . . H30 H 1.0050 0.3918 0.7920 0.085 Uiso 1 1 calc R . . C31 C 1.0180(10) 0.4101(6) 0.7248(8) 0.088(6) Uani 1 1 d . . . H31 H 1.0613 0.4220 0.7363 0.106 Uiso 1 1 calc R . . C32 C 0.9805(11) 0.4094(6) 0.6735(10) 0.100(7) Uani 1 1 d . . . H32 H 0.9998 0.4215 0.6509 0.120 Uiso 1 1 calc R . . C33 C 0.9193(9) 0.3922(5) 0.6563(7) 0.075(5) Uani 1 1 d . . . H33 H 0.8959 0.3929 0.6225 0.090 Uiso 1 1 calc R . . C34 C 0.8906(8) 0.3732(4) 0.6895(7) 0.055(4) Uani 1 1 d U . . C35 C 0.8304(8) 0.3416(4) 0.7246(5) 0.042(3) Uani 1 1 d U . . C36 C 0.7759(7) 0.3279(4) 0.7347(6) 0.049(4) Uani 1 1 d . . . C37 C 0.7065(9) 0.3076(5) 0.7727(7) 0.060(5) Uani 1 1 d U . . C38 C 0.6696(10) 0.2963(4) 0.8046(7) 0.068(5) Uani 1 1 d . . . H38 H 0.6914 0.2936 0.8385 0.081 Uiso 1 1 calc R . . C39 C 0.6042(10) 0.2893(5) 0.7870(9) 0.075(6) Uani 1 1 d . . . H39 H 0.5781 0.2848 0.8086 0.090 Uiso 1 1 calc R . . C40 C 0.5740(12) 0.2885(5) 0.7369(10) 0.093(6) Uani 1 1 d U . . H40 H 0.5283 0.2805 0.7252 0.112 Uiso 1 1 calc R . . C41 C 0.6055(9) 0.2983(5) 0.7044(7) 0.071(5) Uani 1 1 d . . . H41 H 0.5838 0.2992 0.6704 0.085 Uiso 1 1 calc R . . C42 C 0.6755(8) 0.3074(4) 0.7257(8) 0.060(5) Uani 1 1 d . . . C43 C 0.7005(9) 0.5742(4) 0.7828(8) 0.077(6) Uani 1 1 d . . . C44 C 0.6113(8) 0.5435(4) 0.7966(7) 0.067(5) Uani 1 1 d . . . C45 C 0.7043(10) 0.5089(5) 0.7966(8) 0.081(6) Uani 1 1 d . . . C46 C 0.7323(9) 0.6844(4) 0.7779(6) 0.058(4) Uani 1 1 d . . . H46 H 0.7092 0.7088 0.7789 0.069 Uiso 1 1 calc R . . C47 C 0.6993(8) 0.6497(4) 0.7790(7) 0.069(5) Uani 1 1 d . . . H47 H 0.6552 0.6497 0.7822 0.083 Uiso 1 1 calc R . . C48 C 0.7329(8) 0.6125(4) 0.7752(6) 0.058(5) Uani 1 1 d . . . C49 C 0.7943(9) 0.6152(4) 0.7718(7) 0.070(5) Uani 1 1 d U . . H49 H 0.8191 0.5910 0.7729 0.084 Uiso 1 1 calc R . . C50 C 0.8254(8) 0.6522(4) 0.7666(7) 0.063(5) Uani 1 1 d . . . H50 H 0.8656 0.6533 0.7575 0.076 Uiso 1 1 calc R . . C51 C 0.4620(8) 0.5189(5) 0.8338(8) 0.076(6) Uani 1 1 d . . . H51 H 0.4442 0.4966 0.8465 0.091 Uiso 1 1 calc R . . C52 C 0.5191(9) 0.5127(5) 0.8219(7) 0.074(5) Uani 1 1 d . . . H52 H 0.5405 0.4872 0.8261 0.089 Uiso 1 1 calc R . . C53 C 0.5445(9) 0.5443(5) 0.8035(7) 0.072(5) Uani 1 1 d . . . C54 C 0.5108(8) 0.5814(5) 0.7998(8) 0.090(7) Uani 1 1 d . . . H54 H 0.5275 0.6045 0.7878 0.108 Uiso 1 1 calc R . . C55 C 0.4561(10) 0.5836(5) 0.8132(9) 0.099(8) Uani 1 1 d . . . H55 H 0.4346 0.6091 0.8108 0.119 Uiso 1 1 calc R . . C56 C 0.8358(9) 0.4285(5) 0.7999(7) 0.078(5) Uani 1 1 d U . . H56 H 0.8754 0.4258 0.7902 0.094 Uiso 1 1 calc R . . C57 C 0.7990(9) 0.4670(5) 0.7929(7) 0.076(5) Uani 1 1 d U . . H57 H 0.8174 0.4899 0.7817 0.091 Uiso 1 1 calc R . . C58 C 0.7399(8) 0.4699(5) 0.8022(8) 0.083(7) Uani 1 1 d . . . C59 C 0.7161(7) 0.4353(4) 0.8185(7) 0.064(5) Uani 1 1 d . . . H59 H 0.6738 0.4348 0.8247 0.076 Uiso 1 1 calc R . . C60 C 0.7561(10) 0.4023(5) 0.8251(9) 0.096(7) Uani 1 1 d . . . H60 H 0.7377 0.3789 0.8354 0.115 Uiso 1 1 calc R . . C61 C 0.6118(9) 0.5786(5) 0.6534(7) 0.072(5) Uani 1 1 d . . . C62 C 0.5242(9) 0.5462(5) 0.6678(8) 0.077(6) Uani 1 1 d . A . C63 C 0.6175(8) 0.5121(5) 0.6642(7) 0.072(5) Uani 1 1 d . . . C64 C 0.6290(8) 0.6879(5) 0.6330(7) 0.067(5) Uani 1 1 d . . . H64 H 0.6077 0.7121 0.6380 0.080 Uiso 1 1 calc R . . C65 C 0.6036(9) 0.6528(5) 0.6418(7) 0.077(6) Uani 1 1 d . . . H65 H 0.5611 0.6512 0.6476 0.092 Uiso 1 1 calc R . . C66 C 0.6427(6) 0.6188(4) 0.6419(5) 0.043(4) Uani 1 1 d . . . C67 C 0.6966(9) 0.6183(5) 0.6308(7) 0.078(5) Uani 1 1 d U . . H67 H 0.7201 0.5938 0.6306 0.093 Uiso 1 1 calc R . . C68 C 0.7214(8) 0.6561(5) 0.6181(6) 0.057(4) Uani 1 1 d . . . H68 H 0.7629 0.6570 0.6107 0.068 Uiso 1 1 calc R . . C69 C 0.3591(10) 0.5086(6) 0.6792(8) 0.088(7) Uani 1 1 d . . . H69 H 0.3379 0.4839 0.6826 0.105 Uiso 1 1 calc R A . C70 C 0.4293(10) 0.5082(6) 0.6828(9) 0.100(7) Uani 1 1 d . A . H70 H 0.4555 0.4845 0.6919 0.119 Uiso 1 1 calc R . . C71 C 0.4584(8) 0.5448(4) 0.6721(6) 0.057(4) Uani 1 1 d . . . C72 C 0.4170(9) 0.5781(5) 0.6616(7) 0.074(5) Uani 1 1 d . A . H72 H 0.4344 0.6031 0.6546 0.089 Uiso 1 1 calc R . . C73 C 0.3473(10) 0.5754(5) 0.6609(8) 0.090(6) Uani 1 1 d . . . H73 H 0.3191 0.5984 0.6527 0.107 Uiso 1 1 calc R A . C74 C 0.7431(8) 0.4319(4) 0.6538(7) 0.062(5) Uani 1 1 d . . . H74 H 0.7870 0.4306 0.6504 0.075 Uiso 1 1 calc R . . C75 C 0.7111(8) 0.4713(5) 0.6575(7) 0.068(5) Uani 1 1 d . . . H75 H 0.7330 0.4955 0.6532 0.081 Uiso 1 1 calc R . . C76 C 0.6538(9) 0.4731(5) 0.6664(7) 0.076(6) Uani 1 1 d . . . C77 C 0.6210(9) 0.4374(6) 0.6751(8) 0.092(6) Uani 1 1 d U . . H77 H 0.5828 0.4378 0.6867 0.110 Uiso 1 1 calc R . . C78 C 0.6498(10) 0.4020(6) 0.6652(9) 0.104(7) Uani 1 1 d U . . H78 H 0.6252 0.3780 0.6654 0.125 Uiso 1 1 calc R . . C79 C 0.8531(11) 0.7647(6) 0.8584(6) 0.079(6) Uani 1 1 d . . . C80 C 0.8891(10) 0.7292(6) 0.8646(7) 0.076(5) Uani 1 1 d U . . C81 C 0.9419(9) 0.7321(6) 0.8445(6) 0.070(5) Uani 1 1 d . . . C82 C 0.9410(10) 0.7738(5) 0.8265(8) 0.091(7) Uani 1 1 d . . . C83 C 0.8807(8) 0.7939(5) 0.8337(6) 0.058(4) Uani 1 1 d U . . C84 C 0.7941(11) 0.7760(10) 0.8779(8) 0.144(12) Uani 1 1 d . . . H84A H 0.7540 0.7611 0.8598 0.216 Uiso 1 1 calc R . . H84B H 0.7854 0.8050 0.8738 0.216 Uiso 1 1 calc R . . H84C H 0.8055 0.7691 0.9126 0.216 Uiso 1 1 calc R . . C85 C 0.8667(14) 0.6948(9) 0.8890(10) 0.165(13) Uani 1 1 d . . . H85A H 0.8923 0.6944 0.9236 0.247 Uiso 1 1 calc R . . H85B H 0.8741 0.6695 0.8737 0.247 Uiso 1 1 calc R . . H85C H 0.8188 0.6977 0.8857 0.247 Uiso 1 1 calc R . . C86 C 0.9935(12) 0.7031(7) 0.8546(9) 0.136(11) Uani 1 1 d . . . H86A H 1.0297 0.7113 0.8835 0.204 Uiso 1 1 calc R . . H86B H 1.0112 0.7008 0.8267 0.204 Uiso 1 1 calc R . . H86C H 0.9756 0.6770 0.8607 0.204 Uiso 1 1 calc R . . C87 C 0.9879(10) 0.7884(8) 0.7977(9) 0.117(9) Uani 1 1 d . . . H87A H 1.0299 0.7731 0.8077 0.176 Uiso 1 1 calc R . . H87B H 0.9976 0.8171 0.8042 0.176 Uiso 1 1 calc R . . H87C H 0.9662 0.7844 0.7628 0.176 Uiso 1 1 calc R . . C88 C 0.8668(10) 0.8361(6) 0.8183(9) 0.118(9) Uani 1 1 d . . . H88A H 0.8325 0.8370 0.7865 0.177 Uiso 1 1 calc R . . H88B H 0.9081 0.8488 0.8159 0.177 Uiso 1 1 calc R . . H88C H 0.8506 0.8506 0.8424 0.177 Uiso 1 1 calc R . . C89 C 0.7189(9) 0.7369(5) 0.5144(7) 0.067(5) Uiso 1 1 d . . . C90 C 0.6521(10) 0.7314(7) 0.5150(7) 0.084(6) Uani 1 1 d U . . C91 C 0.6308(11) 0.7682(6) 0.5340(7) 0.082(6) Uani 1 1 d . . . C92 C 0.6795(15) 0.7952(7) 0.5383(7) 0.109(8) Uani 1 1 d . . . C93 C 0.7359(11) 0.7781(6) 0.5309(8) 0.086(6) Uani 1 1 d U . . C94 C 0.7639(12) 0.7060(7) 0.4950(8) 0.113(8) Uani 1 1 d . . . H94A H 0.7480 0.6785 0.4971 0.169 Uiso 1 1 calc R . . H94B H 0.8108 0.7083 0.5149 0.169 Uiso 1 1 calc R . . H94C H 0.7604 0.7123 0.4610 0.169 Uiso 1 1 calc R . . C95 C 0.6132(12) 0.6940(8) 0.4976(12) 0.155(12) Uani 1 1 d . . . H95A H 0.6051 0.6799 0.5253 0.232 Uiso 1 1 calc R . . H95B H 0.6387 0.6765 0.4820 0.232 Uiso 1 1 calc R . . H95C H 0.5701 0.7009 0.4739 0.232 Uiso 1 1 calc R . . C96 C 0.5552(11) 0.7726(7) 0.5301(8) 0.111(8) Uani 1 1 d . . . H96A H 0.5502 0.7919 0.5546 0.167 Uiso 1 1 calc R . . H96B H 0.5373 0.7464 0.5359 0.167 Uiso 1 1 calc R . . H96C H 0.5306 0.7823 0.4975 0.167 Uiso 1 1 calc R . . C97 C 0.6745(16) 0.8379(8) 0.5558(12) 0.179(15) Uani 1 1 d . . . H97A H 0.6673 0.8565 0.5283 0.268 Uiso 1 1 calc R . . H97B H 0.7161 0.8449 0.5809 0.268 Uiso 1 1 calc R . . H97C H 0.6367 0.8397 0.5694 0.268 Uiso 1 1 calc R . . C98 C 0.8070(11) 0.7930(9) 0.5338(9) 0.149(12) Uani 1 1 d . . . H98A H 0.8054 0.8083 0.5043 0.224 Uiso 1 1 calc R . . H98B H 0.8369 0.7698 0.5364 0.224 Uiso 1 1 calc R . . H98C H 0.8238 0.8103 0.5624 0.224 Uiso 1 1 calc R . . C99 C 0.3601(5) 0.5348(3) 0.9331(3) 0.138(10) Uiso 1 1 d G . . C100 C 0.4157(5) 0.5610(3) 0.9352(3) 0.137(10) Uiso 1 1 d G . . C101 C 0.3896(5) 0.6010(3) 0.9226(3) 0.102(7) Uani 1 1 d G . . C102 C 0.3179(5) 0.5994(3) 0.9128(3) 0.120(9) Uani 1 1 d G . . C103 C 0.2997(5) 0.5585(3) 0.9192(3) 0.108(8) Uani 1 1 d G . . C104 C 0.3644(7) 0.4896(3) 0.9438(3) 0.180(15) Uani 1 1 d G . . H10A H 0.3549 0.4746 0.9131 0.270 Uiso 1 1 calc R . . H10B H 0.3315 0.4823 0.9606 0.270 Uiso 1 1 calc R . . H10C H 0.4096 0.4829 0.9645 0.270 Uiso 1 1 calc R . . C105 C 0.4895(6) 0.5487(4) 0.9485(3) 0.122(9) Uani 1 1 d G . . H10D H 0.4955 0.5226 0.9651 0.182 Uiso 1 1 calc R . . H10E H 0.5171 0.5690 0.9700 0.182 Uiso 1 1 calc R . . H10F H 0.5032 0.5465 0.9187 0.182 Uiso 1 1 calc R . . C106 C 0.4309(6) 0.6385(4) 0.9202(3) 0.209(18) Uani 1 1 d G . . H10G H 0.4007 0.6614 0.9086 0.313 Uiso 1 1 calc R . . H10H H 0.4574 0.6337 0.8976 0.313 Uiso 1 1 calc R . . H10I H 0.4611 0.6445 0.9527 0.313 Uiso 1 1 calc R . . C107 C 0.2696(6) 0.6349(3) 0.8980(3) 0.165(11) Uani 1 1 d GU . . H10J H 0.2639 0.6477 0.9272 0.247 Uiso 1 1 calc R . . H10K H 0.2261 0.6253 0.8774 0.247 Uiso 1 1 calc R . . H10L H 0.2880 0.6546 0.8799 0.247 Uiso 1 1 calc R . . C108 C 0.2285(5) 0.5429(4) 0.9126(3) 0.135(10) Uani 1 1 d G . . H10M H 0.2220 0.5383 0.9446 0.202 Uiso 1 1 calc R . . H10N H 0.2220 0.5176 0.8942 0.202 Uiso 1 1 calc R . . H10O H 0.1959 0.5629 0.8946 0.202 Uiso 1 1 calc R . . C109 C 0.1806(5) 0.5084(3) 0.5922(3) 0.089(18) Uiso 0.530(17) 1 d PG A 1 C110 C 0.1435(5) 0.4905(3) 0.6230(3) 0.133(18) Uiso 0.530(17) 1 d PG A 1 C111 C 0.1073(4) 0.5227(3) 0.6393(3) 0.076(10) Uani 0.530(17) 1 d PGU A 1 C112 C 0.1221(4) 0.5607(3) 0.6185(3) 0.093(7) Uani 0.530(17) 1 d PGU A 1 C113 C 0.1674(4) 0.5518(3) 0.5894(3) 0.074(11) Uani 0.530(17) 1 d PGU A 1 C114 C 0.2262(5) 0.4855(4) 0.5668(4) 0.096(13) Uani 0.530(17) 1 d PGU A 1 H11A H 0.1986 0.4749 0.5354 0.145 Uiso 0.530(17) 1 calc PR A 1 H11B H 0.2486 0.4631 0.5876 0.145 Uiso 0.530(17) 1 calc PR A 1 H11C H 0.2599 0.5039 0.5615 0.145 Uiso 0.530(17) 1 calc PR A 1 C115 C 0.1426(7) 0.4450(3) 0.6362(4) 0.18(2) Uani 0.530(17) 1 d PGU A 1 H11D H 0.1839 0.4322 0.6339 0.264 Uiso 0.530(17) 1 calc PR A 1 H11E H 0.1037 0.4320 0.6134 0.264 Uiso 0.530(17) 1 calc PR A 1 H11F H 0.1396 0.4423 0.6694 0.264 Uiso 0.530(17) 1 calc PR A 1 C116 C 0.0612(4) 0.5176(4) 0.6728(3) 0.137(18) Uani 0.530(17) 1 d PGU A 1 H11G H 0.0890 0.5147 0.7067 0.205 Uiso 0.530(17) 1 calc PR A 1 H11H H 0.0332 0.4936 0.6629 0.205 Uiso 0.530(17) 1 calc PR A 1 H11I H 0.0324 0.5414 0.6699 0.205 Uiso 0.530(17) 1 calc PR A 1 C117 C 0.0945(5) 0.6029(3) 0.6261(3) 0.15(3) Uani 0.530(17) 1 d PG A 1 H11J H 0.0606 0.6000 0.6433 0.232 Uiso 0.530(17) 1 calc PR A 1 H11K H 0.0741 0.6156 0.5943 0.232 Uiso 0.530(17) 1 calc PR A 1 H11L H 0.1314 0.6198 0.6454 0.232 Uiso 0.530(17) 1 calc PR A 1 C118 C 0.1964(6) 0.5831(4) 0.5606(3) 0.087(13) Uani 0.530(17) 1 d PG A 1 H11M H 0.1599 0.5996 0.5403 0.130 Uiso 0.530(17) 1 calc PR A 1 H11N H 0.2188 0.5689 0.5399 0.130 Uiso 0.530(17) 1 calc PR A 1 H11O H 0.2289 0.6004 0.5836 0.130 Uiso 0.530(17) 1 calc PR A 1 C10A C 0.1136(4) 0.5529(3) 0.6244(3) 0.093(7) Uani 0.470(17) 1 d PGU A 2 C11A C 0.1523(5) 0.5729(3) 0.5971(3) 0.076(12) Uani 0.470(17) 1 d PGU A 2 C11B C 0.1918(5) 0.5429(4) 0.5818(3) 0.073(12) Uani 0.470(17) 1 d PGU A 2 C11C C 0.1776(5) 0.5044(3) 0.5997(3) 0.069(15) Uani 0.470(17) 1 d PGU A 2 C11D C 0.1293(4) 0.5105(3) 0.6260(3) 0.087(14) Uani 0.470(17) 1 d PGU A 2 C11E C 0.0646(4) 0.5731(4) 0.6476(3) 0.111(16) Uani 0.470(17) 1 d PGU A 2 H11P H 0.0859 0.5760 0.6828 0.167 Uiso 0.470(17) 1 calc PR A 2 H11Q H 0.0242 0.5565 0.6420 0.167 Uiso 0.470(17) 1 calc PR A 2 H11R H 0.0523 0.5997 0.6331 0.167 Uiso 0.470(17) 1 calc PR A 2 C11F C 0.1515(7) 0.6180(3) 0.5863(3) 0.090(14) Uani 0.470(17) 1 d PGU A 2 H11S H 0.1107 0.6248 0.5602 0.134 Uiso 0.470(17) 1 calc PR A 2 H11T H 0.1909 0.6250 0.5760 0.134 Uiso 0.470(17) 1 calc PR A 2 H11U H 0.1524 0.6332 0.6157 0.134 Uiso 0.470(17) 1 calc PR A 2 C11G C 0.2404(5) 0.5506(5) 0.5519(3) 0.15(2) Uani 0.470(17) 1 d PGU A 2 H11V H 0.2153 0.5512 0.5172 0.222 Uiso 0.470(17) 1 calc PR A 2 H11W H 0.2738 0.5290 0.5579 0.222 Uiso 0.470(17) 1 calc PR A 2 H11X H 0.2630 0.5765 0.5615 0.222 Uiso 0.470(17) 1 calc PR A 2 C11H C 0.2084(6) 0.4640(4) 0.5920(4) 0.104(16) Uani 0.470(17) 1 d PGU A 2 H11Y H 0.1830 0.4527 0.5604 0.157 Uiso 0.470(17) 1 calc PR A 2 H11Z H 0.2066 0.4453 0.6180 0.157 Uiso 0.470(17) 1 calc PR A 2 H12P H 0.2552 0.4680 0.5927 0.157 Uiso 0.470(17) 1 calc PR A 2 C11I C 0.0997(5) 0.4778(3) 0.6512(3) 0.14(2) Uiso 0.470(17) 1 d PG A 2 H12Q H 0.0578 0.4678 0.6286 0.205 Uiso 0.470(17) 1 calc PR A 2 H12R H 0.0907 0.4892 0.6801 0.205 Uiso 0.470(17) 1 calc PR A 2 H12S H 0.1318 0.4556 0.6609 0.205 Uiso 0.470(17) 1 calc PR A 2 C119 C 0.9066(12) 0.3488(7) 0.9076(9) 0.098(7) Uiso 1 1 d . . . C120 C 0.8651(12) 0.3159(9) 0.8998(10) 0.123(10) Uani 1 1 d . . . C121 C 0.9020(10) 0.2890(6) 0.8759(6) 0.073(5) Uani 1 1 d . . . C122 C 0.9547(11) 0.3092(6) 0.8661(8) 0.090(6) Uani 1 1 d . . . C123 C 0.9563(9) 0.3509(8) 0.8854(7) 0.117(8) Uani 1 1 d DU . . C124 C 0.8954(16) 0.3891(10) 0.9353(12) 0.176(13) Uiso 1 1 d . . . H12A H 0.8647 0.3835 0.9545 0.264 Uiso 1 1 calc R . . H12B H 0.8762 0.4101 0.9113 0.264 Uiso 1 1 calc R . . H12C H 0.9386 0.3983 0.9570 0.264 Uiso 1 1 calc R . . C125 C 0.8061(11) 0.3016(10) 0.9215(10) 0.168(15) Uani 1 1 d . . . H12D H 0.8185 0.2760 0.9387 0.251 Uiso 1 1 calc R . . H12E H 0.7645 0.2982 0.8948 0.251 Uiso 1 1 calc R . . H12F H 0.7993 0.3220 0.9442 0.251 Uiso 1 1 calc R . . C126 C 0.8823(12) 0.2444(5) 0.8585(8) 0.107(8) Uani 1 1 d . . . H12G H 0.8612 0.2441 0.8231 0.160 Uiso 1 1 calc R . . H12H H 0.8508 0.2339 0.8748 0.160 Uiso 1 1 calc R . . H12I H 0.9227 0.2276 0.8667 0.160 Uiso 1 1 calc R . . C127 C 1.0031(11) 0.2930(7) 0.8362(9) 0.123(10) Uani 1 1 d . . . H12J H 1.0499 0.2977 0.8551 0.185 Uiso 1 1 calc R . . H12K H 0.9933 0.3073 0.8050 0.185 Uiso 1 1 calc R . . H12L H 0.9957 0.2641 0.8302 0.185 Uiso 1 1 calc R . . C128 C 1.0135(12) 0.3807(7) 0.8960(11) 0.148(11) Uani 1 1 d D . . H12M H 0.9980 0.4069 0.9041 0.222 Uiso 1 1 calc R . . H12N H 1.0294 0.3835 0.8673 0.222 Uiso 1 1 calc R . . H12O H 1.0504 0.3710 0.9236 0.222 Uiso 1 1 calc R . . C129 C 0.7004(5) 0.2885(3) 0.5859(4) 0.086(6) Uani 1 1 d GU . . C130 C 0.6510(6) 0.3196(3) 0.5704(4) 0.105(7) Uiso 1 1 d G . . C131 C 0.6818(6) 0.3529(3) 0.5536(4) 0.110(8) Uiso 1 1 d G . . C132 C 0.7501(5) 0.3424(3) 0.5587(4) 0.108(9) Uani 1 1 d G . . C133 C 0.7616(5) 0.3026(3) 0.5786(4) 0.093(7) Uani 1 1 d G . . C134 C 0.6896(8) 0.2476(4) 0.6064(6) 0.143(10) Uani 1 1 d GU . . H13A H 0.6462 0.2475 0.6132 0.215 Uiso 1 1 calc R . . H13B H 0.7256 0.2426 0.6367 0.215 Uiso 1 1 calc R . . H13C H 0.6900 0.2266 0.5827 0.215 Uiso 1 1 calc R . . C135 C 0.5786(8) 0.3176(5) 0.5716(7) 0.179(13) Uiso 1 1 d G . . H13D H 0.5771 0.3223 0.6049 0.269 Uiso 1 1 calc R . . H13E H 0.5600 0.2909 0.5608 0.269 Uiso 1 1 calc R . . H13F H 0.5520 0.3382 0.5499 0.269 Uiso 1 1 calc R . . C136 C 0.6478(9) 0.3925(5) 0.5338(7) 0.26(2) Uiso 1 1 d G . . H13G H 0.6675 0.4143 0.5565 0.387 Uiso 1 1 calc R . . H13H H 0.5997 0.3906 0.5301 0.387 Uiso 1 1 calc R . . H13I H 0.6544 0.3981 0.5020 0.387 Uiso 1 1 calc R . . C137 C 0.8016(8) 0.3689(5) 0.5452(6) 0.169(12) Uani 1 1 d GU . . H13J H 0.8087 0.3935 0.5649 0.254 Uiso 1 1 calc R . . H13K H 0.7850 0.3760 0.5106 0.254 Uiso 1 1 calc R . . H13L H 0.8441 0.3542 0.5515 0.254 Uiso 1 1 calc R . . C138 C 0.8274(7) 0.2793(5) 0.5901(6) 0.157(13) Uani 1 1 d G . . H13M H 0.8421 0.2776 0.5608 0.236 Uiso 1 1 calc R . . H13N H 0.8208 0.2522 0.6011 0.236 Uiso 1 1 calc R . . H13O H 0.8617 0.2933 0.6159 0.236 Uiso 1 1 calc R . . C139 C 0.1486(17) 0.7941(8) 0.3249(10) 0.137(12) Uani 1 1 d . . . C140 C 0.1198(14) 0.6001(10) 0.7797(11) 0.158(12) Uani 1 1 d . . . O3 O 0.1665(10) 0.5214(6) 0.4119(7) 0.163(8) Uani 1 1 d . . . O1 O 0.1528(11) 0.7786(9) 0.2794(13) 0.231(13) Uani 1 1 d . . . O4 O 0.9770(16) 0.5943(11) 0.8179(12) 0.272(14) Uiso 1 1 d . . . O2 O 0.0913(9) 0.6314(6) 0.8043(7) 0.137(6) Uani 1 1 d . . . O5 O 0.5288(19) 0.5964(13) 0.5375(14) 0.331(19) Uiso 1 1 d . . . O6 O 0.9138(6) 0.0360(4) 0.0341(4) 0.080(4) 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 0.0619(4) 0.0374(3) 0.0579(4) -0.0014(3) 0.0212(3) -0.0064(3) Ir2 0.0632(4) 0.0416(3) 0.0584(4) 0.0022(3) 0.0168(4) -0.0104(3) Ir3 0.0746(5) 0.0619(5) 0.0982(6) 0.0092(4) 0.0331(5) 0.0218(4) Ir4 0.0538(4) 0.0536(4) 0.1081(6) -0.0113(4) 0.0412(4) -0.0003(3) Ir5 0.0740(5) 0.0354(3) 0.0992(6) 0.0069(3) 0.0408(4) 0.0163(3) Ir6 0.0616(4) 0.0384(3) 0.0995(6) 0.0298(3) 0.0265(4) 0.0069(3) N1 0.044(7) 0.029(6) 0.050(8) -0.004(5) 0.014(6) 0.009(5) N2 0.047(8) 0.028(6) 0.094(11) -0.010(6) 0.035(8) -0.009(5) N3 0.043(7) 0.042(6) 0.032(7) 0.001(5) 0.010(6) -0.003(5) N4 0.073(9) 0.018(5) 0.048(8) -0.015(5) 0.017(8) -0.002(5) N5 0.081(10) 0.021(6) 0.071(10) 0.002(6) 0.016(8) 0.005(6) N6 0.035(8) 0.045(8) 0.155(16) -0.006(10) 0.036(9) -0.010(6) N7 0.076(9) 0.016(5) 0.070(9) -0.008(6) 0.038(8) -0.005(6) N8 0.066(9) 0.029(7) 0.091(11) 0.005(7) 0.020(8) -0.009(6) N9 0.079(9) 0.022(6) 0.068(9) 0.001(6) 0.036(8) 0.014(6) N10 0.049(8) 0.046(7) 0.048(8) 0.004(6) 0.026(7) 0.014(6) N11 0.030(7) 0.027(6) 0.132(13) 0.022(7) 0.023(8) 0.002(5) N12 0.110(8) 0.049(6) 0.038(6) 0.012(5) 0.045(6) -0.007(6) N13 0.074(10) 0.039(7) 0.098(12) 0.019(7) 0.045(9) 0.009(7) N14 0.107(13) 0.039(8) 0.114(13) 0.004(8) 0.048(11) 0.017(8) N15 0.070(10) 0.041(8) 0.172(17) -0.001(9) 0.071(11) 0.005(7) N16 0.061(9) 0.028(7) 0.141(14) -0.003(8) 0.039(9) 0.001(6) N17 0.059(9) 0.040(7) 0.088(11) 0.002(7) 0.024(8) 0.009(6) N18 0.065(9) 0.031(7) 0.129(14) 0.015(7) 0.044(9) -0.007(6) N19 0.037(7) 0.039(7) 0.061(9) -0.001(6) 0.009(6) -0.011(5) N20 0.057(9) 0.039(7) 0.119(13) 0.021(8) 0.048(9) 0.023(6) N21 0.018(6) 0.043(7) 0.102(10) 0.038(6) 0.015(6) 0.009(5) N22 0.049(8) 0.056(9) 0.104(12) 0.023(8) 0.035(8) 0.013(7) N23 0.059(9) 0.049(8) 0.121(13) 0.025(8) 0.032(9) 0.015(7) N24 0.063(9) 0.062(9) 0.112(13) 0.038(8) 0.050(9) 0.020(7) C1 0.063(10) 0.020(6) 0.059(10) 0.002(6) 0.042(9) 0.009(6) C2 0.061(11) 0.038(8) 0.104(14) -0.026(9) 0.041(11) -0.003(7) C5 0.064(11) 0.057(10) 0.041(10) 0.004(7) 0.013(9) -0.005(8) C6 0.036(8) 0.023(7) 0.060(11) 0.011(6) 0.011(8) 0.012(6) C7 0.023(6) 0.027(5) 0.033(7) -0.022(5) 0.006(5) -0.003(5) C8 0.034(6) 0.013(5) 0.049(7) -0.004(5) 0.000(6) -0.004(5) C9 0.043(8) 0.014(6) 0.043(9) -0.007(5) 0.023(7) 0.003(5) C10 0.071(12) 0.039(9) 0.093(14) -0.019(9) 0.025(11) 0.008(8) C11 0.048(11) 0.066(12) 0.123(19) -0.008(12) 0.037(12) 0.008(9) C12 0.059(11) 0.067(11) 0.069(13) 0.000(9) 0.034(10) 0.009(9) C13 0.062(10) 0.039(8) 0.055(10) -0.002(7) 0.020(9) 0.001(7) C14 0.044(9) 0.035(7) 0.051(10) -0.010(7) 0.029(8) -0.008(6) C15 0.107(18) 0.039(11) 0.20(3) 0.005(15) 0.11(2) 0.008(11) C16 0.089(14) 0.043(10) 0.124(18) 0.037(11) 0.036(13) 0.037(10) C17 0.125(15) 0.069(12) 0.170(17) 0.046(12) 0.058(13) 0.005(11) C18 0.120(14) 0.043(10) 0.136(15) -0.019(10) 0.054(12) -0.020(10) C19 0.127(18) 0.028(9) 0.142(19) -0.016(11) 0.078(16) -0.003(10) C20 0.13(2) 0.030(10) 0.126(19) -0.012(12) 0.074(17) -0.016(10) C21 0.083(13) 0.035(8) 0.085(14) 0.000(9) 0.055(12) -0.007(8) C22 0.044(9) 0.029(8) 0.109(15) 0.016(9) 0.043(10) 0.004(7) C23 0.031(9) 0.037(9) 0.109(16) 0.006(9) -0.011(10) 0.011(7) C24 0.094(15) 0.052(11) 0.17(2) -0.027(13) 0.083(16) -0.007(10) C25 0.112(14) 0.040(9) 0.112(14) 0.005(10) 0.035(12) -0.004(9) C26 0.075(14) 0.070(14) 0.16(2) 0.039(15) 0.059(16) 0.030(11) C27 0.089(14) 0.040(10) 0.092(14) 0.017(9) 0.034(12) 0.003(9) C28 0.053(10) 0.020(7) 0.111(16) 0.004(8) 0.028(11) 0.009(7) C29 0.025(8) 0.046(8) 0.064(11) 0.005(7) 0.020(8) 0.003(6) C30 0.052(11) 0.060(11) 0.095(15) -0.007(10) 0.011(10) 0.023(9) C31 0.069(13) 0.101(16) 0.098(17) 0.032(13) 0.031(13) -0.005(11) C32 0.084(15) 0.085(15) 0.14(2) 0.035(14) 0.054(16) -0.021(12) C33 0.066(12) 0.074(12) 0.101(15) 0.017(11) 0.049(12) -0.004(10) C34 0.048(9) 0.036(7) 0.084(11) 0.032(7) 0.025(9) 0.017(6) C35 0.060(7) 0.047(7) 0.017(6) -0.011(5) 0.006(6) 0.011(6) C36 0.039(9) 0.042(8) 0.073(12) -0.009(8) 0.029(9) -0.009(7) C37 0.081(11) 0.050(9) 0.063(10) 0.029(8) 0.040(9) -0.007(8) C38 0.088(14) 0.036(9) 0.095(14) 0.015(9) 0.050(12) -0.002(8) C39 0.065(13) 0.048(10) 0.128(19) 0.007(11) 0.054(13) 0.011(9) C40 0.095(13) 0.049(10) 0.148(16) 0.009(11) 0.055(13) -0.002(9) C41 0.074(13) 0.044(9) 0.092(14) 0.034(9) 0.018(11) -0.009(8) C42 0.043(10) 0.026(7) 0.127(17) 0.011(9) 0.049(11) 0.010(6) C43 0.085(13) 0.022(8) 0.142(18) 0.003(9) 0.061(13) 0.010(8) C44 0.065(11) 0.020(7) 0.127(16) 0.019(8) 0.042(11) 0.016(7) C45 0.087(14) 0.051(11) 0.120(17) -0.003(10) 0.052(13) 0.023(10) C46 0.080(12) 0.019(7) 0.077(12) 0.013(7) 0.029(10) 0.005(7) C47 0.044(9) 0.036(9) 0.134(17) 0.003(9) 0.038(11) 0.002(7) C48 0.074(11) 0.021(7) 0.097(13) -0.010(7) 0.052(10) -0.018(7) C49 0.075(11) 0.030(7) 0.107(12) -0.001(8) 0.031(10) 0.014(7) C50 0.073(11) 0.033(8) 0.099(14) 0.006(8) 0.047(11) 0.014(8) C51 0.046(10) 0.039(9) 0.145(19) -0.004(10) 0.033(11) 0.014(8) C52 0.076(13) 0.037(9) 0.093(14) 0.001(9) 0.000(11) 0.023(9) C53 0.091(14) 0.032(9) 0.103(15) -0.012(9) 0.045(12) -0.002(8) C54 0.042(10) 0.054(11) 0.17(2) 0.018(12) 0.019(12) 0.012(8) C55 0.095(16) 0.030(9) 0.19(2) 0.034(12) 0.062(16) 0.019(9) C56 0.077(11) 0.064(10) 0.111(13) 0.000(9) 0.053(10) 0.033(9) C57 0.084(11) 0.033(8) 0.122(13) 0.003(8) 0.047(10) 0.015(8) C58 0.046(10) 0.042(9) 0.17(2) -0.035(11) 0.045(12) 0.000(8) C59 0.032(8) 0.039(9) 0.128(16) 0.019(9) 0.035(10) 0.003(7) C60 0.096(15) 0.041(10) 0.17(2) 0.031(12) 0.077(16) 0.015(10) C61 0.067(12) 0.037(9) 0.126(17) 0.015(9) 0.050(12) 0.009(8) C62 0.082(13) 0.040(10) 0.129(17) 0.018(10) 0.061(13) 0.009(9) C63 0.052(10) 0.052(10) 0.119(16) 0.037(10) 0.039(11) 0.026(8) C64 0.059(11) 0.043(9) 0.093(14) 0.003(9) 0.014(10) 0.008(8) C65 0.060(11) 0.064(12) 0.125(17) -0.017(11) 0.057(12) -0.017(9) C66 0.022(7) 0.039(8) 0.068(11) -0.010(7) 0.013(7) 0.002(6) C67 0.067(11) 0.030(8) 0.130(14) 0.006(9) 0.019(10) -0.002(7) C68 0.045(9) 0.056(10) 0.069(12) -0.001(8) 0.016(9) -0.004(8) C69 0.103(16) 0.072(13) 0.120(18) 0.026(12) 0.082(14) -0.001(11) C70 0.099(16) 0.054(11) 0.16(2) 0.030(13) 0.065(16) 0.011(11) C71 0.065(11) 0.031(8) 0.092(13) 0.022(8) 0.050(10) 0.014(7) C72 0.072(12) 0.045(10) 0.125(17) 0.014(10) 0.057(12) 0.010(8) C73 0.078(14) 0.044(11) 0.14(2) 0.001(11) 0.026(14) 0.004(9) C74 0.040(9) 0.037(8) 0.102(14) 0.013(8) 0.008(9) 0.004(7) C75 0.052(10) 0.048(9) 0.107(15) 0.022(9) 0.029(10) 0.006(8) C76 0.084(13) 0.061(11) 0.116(16) 0.038(10) 0.081(12) 0.027(9) C77 0.070(11) 0.086(12) 0.148(15) 0.022(11) 0.076(11) 0.008(9) C78 0.058(11) 0.073(12) 0.175(17) 0.006(12) 0.026(11) 0.010(9) C79 0.126(17) 0.098(15) 0.028(10) -0.006(9) 0.044(11) 0.005(13) C80 0.095(9) 0.067(8) 0.058(8) -0.016(7) 0.010(7) -0.007(7) C81 0.079(13) 0.078(13) 0.051(11) -0.021(9) 0.016(10) -0.009(10) C82 0.086(14) 0.049(11) 0.127(19) -0.036(12) 0.016(14) -0.008(10) C83 0.063(9) 0.052(9) 0.047(9) -0.037(7) -0.002(8) 0.015(7) C84 0.099(18) 0.26(4) 0.070(16) -0.069(19) 0.012(14) 0.02(2) C85 0.15(3) 0.18(3) 0.14(3) 0.09(2) 0.00(2) -0.02(2) C86 0.15(2) 0.094(17) 0.11(2) -0.022(14) -0.053(16) 0.072(16) C87 0.065(14) 0.15(2) 0.14(2) -0.038(18) 0.042(15) -0.027(14) C88 0.083(15) 0.097(17) 0.15(2) -0.097(16) 0.004(15) -0.015(12) C90 0.093(12) 0.102(13) 0.053(10) -0.038(9) 0.016(9) -0.028(11) C91 0.107(17) 0.075(13) 0.084(15) 0.008(11) 0.057(13) -0.018(12) C92 0.18(3) 0.085(16) 0.055(14) 0.023(11) 0.021(16) -0.011(18) C93 0.099(10) 0.077(9) 0.080(9) 0.035(7) 0.021(8) -0.004(8) C94 0.14(2) 0.14(2) 0.089(17) -0.026(15) 0.071(16) 0.009(16) C95 0.079(17) 0.14(2) 0.26(4) -0.02(2) 0.07(2) -0.005(16) C96 0.088(17) 0.113(18) 0.104(18) -0.009(14) -0.016(14) 0.027(14) C97 0.19(3) 0.10(2) 0.19(3) 0.01(2) -0.04(2) 0.07(2) C98 0.101(19) 0.21(3) 0.11(2) 0.01(2) -0.003(16) -0.09(2) C101 0.14(2) 0.086(16) 0.077(15) 0.007(12) 0.034(15) 0.023(15) C102 0.12(2) 0.12(2) 0.14(2) -0.031(17) 0.069(19) 0.000(17) C103 0.15(2) 0.078(15) 0.12(2) -0.010(13) 0.078(18) 0.032(15) C104 0.35(5) 0.088(19) 0.12(2) 0.011(16) 0.09(3) 0.04(2) C105 0.13(2) 0.14(2) 0.086(17) 0.016(14) 0.018(15) 0.090(17) C106 0.32(5) 0.23(4) 0.09(2) -0.04(2) 0.08(3) -0.10(4) C107 0.178(19) 0.123(16) 0.192(19) -0.054(15) 0.054(15) 0.036(14) C108 0.15(2) 0.18(3) 0.084(17) 0.001(17) 0.052(17) -0.07(2) C111 0.039(14) 0.067(16) 0.13(2) -0.035(15) 0.033(14) -0.010(12) C112 0.070(11) 0.107(13) 0.107(12) 0.018(10) 0.034(10) 0.037(10) C113 0.067(13) 0.078(14) 0.085(14) 0.011(9) 0.036(10) 0.000(9) C114 0.10(2) 0.11(2) 0.085(19) -0.030(15) 0.036(16) -0.009(15) C115 0.17(3) 0.16(3) 0.20(3) -0.021(19) 0.055(19) -0.007(19) C116 0.13(2) 0.14(3) 0.14(2) 0.021(17) 0.055(18) -0.027(17) C117 0.27(7) 0.06(3) 0.20(5) 0.02(3) 0.16(5) 0.07(3) C118 0.10(3) 0.11(3) 0.05(2) 0.01(2) 0.02(2) -0.05(2) C10A 0.070(11) 0.107(13) 0.107(12) 0.018(10) 0.034(10) 0.037(10) C11A 0.073(18) 0.09(2) 0.070(19) 0.022(15) 0.032(15) 0.006(15) C11B 0.078(14) 0.069(14) 0.074(14) -0.010(9) 0.024(10) 0.004(9) C11C 0.06(2) 0.09(2) 0.08(2) -0.008(14) 0.047(16) -0.004(14) C11D 0.087(16) 0.080(16) 0.092(16) -0.006(9) 0.023(10) -0.018(10) C11E 0.11(2) 0.10(2) 0.12(2) -0.033(17) 0.025(17) 0.022(17) C11F 0.071(19) 0.09(2) 0.09(2) -0.012(16) 0.003(15) -0.015(16) C11G 0.15(3) 0.16(3) 0.14(3) -0.003(18) 0.06(2) 0.021(18) C11H 0.12(2) 0.11(2) 0.10(2) -0.013(17) 0.055(17) 0.021(17) C120 0.095(17) 0.16(3) 0.14(2) 0.042(19) 0.076(17) 0.045(17) C121 0.078(13) 0.091(14) 0.047(11) 0.025(10) 0.013(10) 0.030(11) C122 0.091(15) 0.073(13) 0.117(18) 0.018(12) 0.048(14) 0.026(11) C123 0.141(16) 0.121(15) 0.108(14) -0.020(12) 0.068(13) 0.007(13) C125 0.076(16) 0.28(4) 0.15(3) 0.15(3) 0.042(17) 0.03(2) C126 0.15(2) 0.034(10) 0.13(2) 0.028(11) 0.028(17) 0.004(11) C127 0.093(16) 0.12(2) 0.18(3) 0.060(18) 0.078(18) 0.060(14) C128 0.13(2) 0.10(2) 0.22(3) 0.03(2) 0.06(2) -0.015(17) C129 0.104(13) 0.054(9) 0.118(14) 0.037(9) 0.060(11) 0.004(9) C132 0.125(19) 0.15(2) 0.046(12) -0.028(12) 0.020(13) -0.083(17) C133 0.092(15) 0.105(17) 0.085(15) 0.032(13) 0.029(13) -0.021(13) C134 0.171(18) 0.075(13) 0.169(18) 0.020(13) 0.026(15) -0.005(13) C137 0.196(19) 0.186(19) 0.140(17) 0.040(15) 0.073(15) -0.063(15) C138 0.104(19) 0.23(3) 0.15(3) -0.01(2) 0.061(19) 0.09(2) C139 0.22(3) 0.106(19) 0.092(19) -0.013(15) 0.06(2) 0.05(2) C140 0.13(2) 0.19(3) 0.16(3) -0.06(2) 0.06(2) 0.03(2) O3 0.173(18) 0.170(19) 0.140(16) 0.039(14) 0.039(14) -0.026(15) O1 0.122(18) 0.23(3) 0.34(4) 0.06(3) 0.07(2) 0.008(18) O2 0.133(14) 0.130(15) 0.167(17) -0.008(12) 0.072(13) 0.004(11) O6 0.078(7) 0.129(8) 0.048(6) -0.010(6) 0.043(5) 0.004(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 Ir1 N2 2.125(12) . ? Ir1 N13 2.129(13) . ? Ir1 C79 2.133(15) . ? Ir1 C83 2.154(13) . ? Ir1 C80 2.167(19) . ? Ir1 N1 2.174(11) . ? Ir1 C81 2.193(19) . ? Ir1 C82 2.217(19) . ? Ir2 C91 2.09(2) . ? Ir2 N19 2.115(11) . ? Ir2 C90 2.138(18) . ? Ir2 C93 2.164(18) . ? Ir2 C89 2.165(17) . ? Ir2 C92 2.20(2) . ? Ir2 N4 2.207(11) . ? Ir2 N3 2.221(11) . ? Ir3 N14 2.130(15) . ? Ir3 C100 2.143(8) . ? Ir3 C99 2.161(8) . ? Ir3 C101 2.162(8) . ? Ir3 N6 2.170(17) . ? Ir3 C103 2.190(7) . ? Ir3 C102 2.191(7) . ? Ir3 N5 2.198(12) . ? Ir4 C11D 2.075(8) . ? Ir4 C11C 2.116(8) . ? Ir4 N20 2.128(12) . ? Ir4 C113 2.144(9) . ? Ir4 N7 2.175(11) . ? Ir4 N8 2.179(14) . ? Ir4 C112 2.185(8) . ? Ir4 C10A 2.206(7) . ? Ir4 C109 2.213(8) . ? Ir4 C11B 2.267(9) . ? Ir4 C111 2.278(8) . ? Ir4 C110 2.294(8) . ? Ir5 C123 2.094(16) . ? Ir5 N15 2.100(14) . ? Ir5 C119 2.12(2) . ? Ir5 N9 2.141(12) . ? Ir5 C122 2.150(19) . ? Ir5 C120 2.16(2) . ? Ir5 C121 2.194(17) . ? Ir5 N10 2.222(13) . ? Ir6 N12 1.994(15) . ? Ir6 N21 2.108(12) . ? Ir6 N11 2.168(14) . ? Ir6 C130 2.184(11) . ? Ir6 C129 2.188(10) . ? Ir6 C131 2.198(11) . ? Ir6 C133 2.204(10) . ? Ir6 C132 2.210(9) . ? N1 C7 1.270(15) . ? N1 C1 1.404(16) . ? N2 C8 1.320(17) . ? N2 C9 1.454(15) . ? N3 C8 1.329(16) . ? N3 C14 1.364(16) . ? N4 C7 1.230(16) . ? N4 C6 1.423(17) . ? N5 C21 1.33(2) . ? N5 C15 1.43(2) . ? N6 C22 1.25(2) . ? N6 C23 1.39(2) . ? N7 C22 1.34(2) . ? N7 C28 1.409(17) . ? N8 C21 1.30(2) . ? N8 C20 1.40(2) . ? N9 C35 1.358(18) . ? N9 C29 1.452(17) . ? N10 C36 1.288(18) . ? N10 C37 1.394(19) . ? N11 C36 1.36(2) . ? N11 C42 1.428(18) . ? N12 C35 1.358(17) . ? N12 C34 1.50(2) . ? N13 C46 1.297(19) . ? N13 C50 1.390(18) . ? N14 C55 1.32(2) . ? N14 C51 1.322(19) . ? N15 C60 1.25(2) . ? N15 C56 1.34(2) . ? N16 C43 1.284(18) . ? N16 C45 1.38(2) . ? N17 C44 1.294(18) . ? N17 C43 1.366(19) . ? N18 C45 1.32(2) . ? N18 C44 1.368(18) . ? N19 C68 1.360(18) . ? N19 C64 1.383(19) . ? N20 C73 1.30(2) . ? N20 C69 1.31(2) . ? N21 C78 1.34(2) . ? N21 C74 1.348(17) . ? N22 C61 1.320(19) . ? N22 C63 1.335(19) . ? N23 C62 1.295(19) . ? N23 C61 1.401(19) . ? N24 C63 1.337(18) . ? N24 C62 1.375(19) . ? C1 C6 1.41(2) . ? C1 C2 1.436(18) . ? C2 C3 1.32(2) . ? C3 C4 1.32(2) . ? C4 C5 1.35(2) . ? C5 C6 1.423(19) . ? C7 C8 1.395(17) . ? C9 C10 1.32(2) . ? C9 C14 1.396(19) . ? C10 C11 1.37(2) . ? C11 C12 1.39(2) . ? C12 C13 1.37(2) . ? C13 C14 1.423(18) . ? C15 C20 1.31(3) . ? C15 C16 1.42(3) . ? C16 C17 1.45(3) . ? C17 C18 1.51(3) . ? C18 C19 1.34(3) . ? C19 C20 1.41(2) . ? C21 C22 1.42(2) . ? C23 C24 1.40(2) . ? C23 C28 1.41(2) . ? C24 C25 1.40(3) . ? C25 C26 1.36(3) . ? C26 C27 1.39(3) . ? C27 C28 1.39(2) . ? C29 C30 1.35(2) . ? C29 C34 1.35(2) . ? C30 C31 1.46(2) . ? C31 C32 1.45(3) . ? C32 C33 1.35(3) . ? C33 C34 1.42(2) . ? C35 C36 1.334(19) . ? C37 C42 1.31(2) . ? C37 C38 1.41(2) . ? C38 C39 1.33(2) . ? C39 C40 1.39(3) . ? C40 C41 1.33(2) . ? C41 C42 1.44(2) . ? C43 C48 1.488(19) . ? C44 C53 1.46(2) . ? C45 C58 1.48(2) . ? C46 C47 1.347(19) . ? C47 C48 1.440(19) . ? C48 C49 1.31(2) . ? C49 C50 1.42(2) . ? C51 C52 1.35(2) . ? C52 C53 1.35(2) . ? C53 C54 1.41(2) . ? C54 C55 1.31(2) . ? C56 C57 1.47(2) . ? C57 C58 1.34(2) . ? C58 C59 1.39(2) . ? C59 C60 1.36(2) . ? C61 C66 1.56(2) . ? C62 C71 1.41(2) . ? C63 C76 1.49(2) . ? C64 C65 1.33(2) . ? C65 C66 1.39(2) . ? C66 C67 1.26(2) . ? C67 C68 1.45(2) . ? C69 C70 1.44(2) . ? C70 C71 1.43(2) . ? C71 C72 1.38(2) . ? C72 C73 1.45(2) . ? C74 C75 1.49(2) . ? C75 C76 1.30(2) . ? C76 C77 1.43(2) . ? C77 C78 1.39(3) . ? C79 C80 1.38(3) . ? C79 C83 1.42(2) . ? C79 C84 1.54(3) . ? C80 C81 1.39(2) . ? C80 C85 1.49(3) . ? C81 C86 1.41(2) . ? C81 C82 1.48(3) . ? C82 C83 1.49(2) . ? C82 C87 1.54(3) . ? C83 C88 1.47(3) . ? C89 C90 1.41(2) . ? C89 C93 1.46(3) . ? C89 C94 1.60(2) . ? C90 C91 1.46(3) . ? C90 C95 1.49(3) . ? C91 C92 1.33(3) . ? C91 C96 1.55(3) . ? C92 C93 1.38(3) . ? C92 C97 1.52(3) . ? C93 C98 1.54(3) . ? C99 C103 1.4386(17) . ? C99 C100 1.4389(17) . ? C99 C104 1.5290(18) . ? C100 C101 1.4385(17) . ? C100 C105 1.5292(18) . ? C101 C102 1.4386(17) . ? C101 C106 1.5293(18) . ? C102 C103 1.4384(17) . ? C102 C107 1.5292(18) . ? C103 C108 1.5292(18) . ? C109 C113 1.4653(17) . ? C109 C110 1.4655(17) . ? C109 C114 1.5576(18) . ? C110 C111 1.4651(17) . ? C110 C115 1.5575(18) . ? C111 C112 1.4651(17) . ? C111 C116 1.5576(18) . ? C112 C113 1.4653(17) . ? C112 C117 1.5575(18) . ? C113 C118 1.5572(18) . ? C10A C11D 1.4415(17) . ? C10A C11A 1.4416(17) . ? C10A C11E 1.5322(18) . ? C11A C11B 1.4416(17) . ? C11A C11F 1.5321(18) . ? C11B C11C 1.4412(17) . ? C11B C11G 1.5322(18) . ? C11C C11D 1.4412(17) . ? C11C C11H 1.5322(18) . ? C11D C11I 1.5324(18) . ? C119 C120 1.37(3) . ? C119 C123 1.37(3) . ? C119 C124 1.61(3) . ? C120 C121 1.48(3) . ? C120 C125 1.61(3) . ? C121 C122 1.39(3) . ? C121 C126 1.58(3) . ? C122 C123 1.49(3) . ? C122 C127 1.60(3) . ? C123 C128 1.512(17) . ? C129 C133 1.433(6) . ? C129 C130 1.433(6) . ? C129 C134 1.523(6) . ? C130 C131 1.433(6) . ? C130 C135 1.523(6) . ? C131 C132 1.433(6) . ? C131 C136 1.523(6) . ? C132 C133 1.433(6) . ? C132 C137 1.523(6) . ? C133 C138 1.523(6) . ? C139 O1 1.43(3) . ? C140 O2 1.48(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 N2 Ir1 N13 85.6(5) . . ? N2 Ir1 C79 163.2(7) . . ? N13 Ir1 C79 109.9(7) . . ? N2 Ir1 C83 126.0(6) . . ? N13 Ir1 C83 148.3(6) . . ? C79 Ir1 C83 38.7(7) . . ? N2 Ir1 C80 140.1(7) . . ? N13 Ir1 C80 91.7(6) . . ? C79 Ir1 C80 37.4(7) . . ? C83 Ir1 C80 64.6(7) . . ? N2 Ir1 N1 77.4(5) . . ? N13 Ir1 N1 84.8(5) . . ? C79 Ir1 N1 109.4(6) . . ? C83 Ir1 N1 101.0(5) . . ? C80 Ir1 N1 142.1(6) . . ? N2 Ir1 C81 106.5(6) . . ? N13 Ir1 C81 107.6(6) . . ? C79 Ir1 C81 63.6(7) . . ? C83 Ir1 C81 66.7(6) . . ? C80 Ir1 C81 37.2(6) . . ? N1 Ir1 C81 167.1(6) . . ? N2 Ir1 C82 99.8(7) . . ? N13 Ir1 C82 146.6(7) . . ? C79 Ir1 C82 63.8(8) . . ? C83 Ir1 C82 39.9(6) . . ? C80 Ir1 C82 63.1(8) . . ? N1 Ir1 C82 128.6(6) . . ? C81 Ir1 C82 39.1(7) . . ? C91 Ir2 N19 111.3(6) . . ? C91 Ir2 C90 40.4(8) . . ? N19 Ir2 C90 94.4(7) . . ? C91 Ir2 C93 63.6(7) . . ? N19 Ir2 C93 152.8(7) . . ? C90 Ir2 C93 64.0(8) . . ? C91 Ir2 C89 66.0(7) . . ? N19 Ir2 C89 113.4(6) . . ? C90 Ir2 C89 38.3(7) . . ? C93 Ir2 C89 39.4(7) . . ? C91 Ir2 C92 36.2(8) . . ? N19 Ir2 C92 147.3(8) . . ? C90 Ir2 C92 62.4(8) . . ? C93 Ir2 C92 36.9(8) . . ? C89 Ir2 C92 63.3(8) . . ? C91 Ir2 N4 106.2(6) . . ? N19 Ir2 N4 81.7(4) . . ? C90 Ir2 N4 142.0(7) . . ? C93 Ir2 N4 125.5(7) . . ? C89 Ir2 N4 164.5(5) . . ? C92 Ir2 N4 102.2(7) . . ? C91 Ir2 N3 164.7(6) . . ? N19 Ir2 N3 83.9(4) . . ? C90 Ir2 N3 141.4(6) . . ? C93 Ir2 N3 102.5(7) . . ? C89 Ir2 N3 107.9(6) . . ? C92 Ir2 N3 128.7(8) . . ? N4 Ir2 N3 76.1(4) . . ? N14 Ir3 C100 94.3(5) . . ? N14 Ir3 C99 119.6(5) . . ? C100 Ir3 C99 39.06(11) . . ? N14 Ir3 C101 104.9(5) . . ? C100 Ir3 C101 39.03(12) . . ? C99 Ir3 C101 65.15(17) . . ? N14 Ir3 N6 85.9(5) . . ? C100 Ir3 N6 148.0(5) . . ? C99 Ir3 N6 154.5(4) . . ? C101 Ir3 N6 110.1(5) . . ? N14 Ir3 C103 157.7(5) . . ? C100 Ir3 C103 64.97(17) . . ? C99 Ir3 C103 38.61(12) . . ? C101 Ir3 C103 64.65(17) . . ? N6 Ir3 C103 116.0(4) . . ? N14 Ir3 C102 141.3(5) . . ? C100 Ir3 C102 64.95(17) . . ? C99 Ir3 C102 64.66(17) . . ? C101 Ir3 C102 38.58(12) . . ? N6 Ir3 C102 95.6(5) . . ? C103 Ir3 C102 38.33(11) . . ? N14 Ir3 N5 82.4(6) . . ? C100 Ir3 N5 134.0(4) . . ? C99 Ir3 N5 104.5(4) . . ? C101 Ir3 N5 169.3(4) . . ? N6 Ir3 N5 77.8(5) . . ? C103 Ir3 N5 105.6(4) . . ? C102 Ir3 N5 135.7(4) . . ? C11D Ir4 C11C 40.21(13) . . ? C11D Ir4 N20 144.2(5) . . ? C11C Ir4 N20 104.8(5) . . ? C11D Ir4 C113 57.40(16) . . ? C11C Ir4 C113 44.30(13) . . ? N20 Ir4 C113 106.4(5) . . ? C11D Ir4 N7 133.2(4) . . ? C11C Ir4 N7 164.5(4) . . ? N20 Ir4 N7 82.6(5) . . ? C113 Ir4 N7 120.8(4) . . ? C11D Ir4 N8 103.0(4) . . ? C11C Ir4 N8 115.7(5) . . ? N20 Ir4 N8 84.7(5) . . ? C113 Ir4 N8 158.6(4) . . ? N7 Ir4 N8 78.2(5) . . ? C11D Ir4 C112 46.35(14) . . ? C11C Ir4 C112 66.07(18) . . ? N20 Ir4 C112 140.9(5) . . ? C113 Ir4 C112 39.55(12) . . ? N7 Ir4 C112 99.5(4) . . ? N8 Ir4 C112 134.2(4) . . ? C11D Ir4 C10A 39.20(12) . . ? C11C Ir4 C10A 65.29(18) . . ? N20 Ir4 C10A 150.5(5) . . ? C113 Ir4 C10A 46.36(14) . . ? N7 Ir4 C10A 101.5(4) . . ? N8 Ir4 C10A 124.8(4) . . ? C112 Ir4 C10A 9.9 . . ? C11D Ir4 C109 44.99(13) . . ? C11C Ir4 C109 6.9 . . ? N20 Ir4 C109 101.1(5) . . ? C113 Ir4 C109 39.27(12) . . ? N7 Ir4 C109 160.0(4) . . ? N8 Ir4 C109 121.6(5) . . ? C112 Ir4 C109 65.23(18) . . ? C10A Ir4 C109 65.75(17) . . ? C11D Ir4 C11B 64.79(18) . . ? C11C Ir4 C11B 38.20(12) . . ? N20 Ir4 C11B 91.8(5) . . ? C113 Ir4 C11B 17.40(6) . . ? N7 Ir4 C11B 129.5(4) . . ? N8 Ir4 C11B 151.5(5) . . ? C112 Ir4 C11B 56.74(17) . . ? C10A Ir4 C11B 62.85(18) . . ? C109 Ir4 C11B 31.63(10) . . ? C11D Ir4 C111 20.25(7) . . ? C11C Ir4 C111 59.72(17) . . ? N20 Ir4 C111 164.4(5) . . ? C113 Ir4 C111 64.76(18) . . ? N7 Ir4 C111 112.9(4) . . ? N8 Ir4 C111 99.9(4) . . ? C112 Ir4 C111 38.26(12) . . ? C10A Ir4 C111 28.66(9) . . ? C109 Ir4 C111 63.72(18) . . ? C11B Ir4 C111 76.97(19) . . ? C11D Ir4 C110 18.78(7) . . ? C11C Ir4 C110 31.38(10) . . ? N20 Ir4 C110 127.9(5) . . ? C113 Ir4 C110 64.49(17) . . ? N7 Ir4 C110 148.2(4) . . ? N8 Ir4 C110 94.2(4) . . ? C112 Ir4 C110 63.86(18) . . ? C10A Ir4 C110 57.59(17) . . ? C109 Ir4 C110 37.90(11) . . ? C11B Ir4 C110 65.89(18) . . ? C111 Ir4 C110 37.38(12) . . ? C123 Ir5 N15 108.2(8) . . ? C123 Ir5 C119 37.9(8) . . ? N15 Ir5 C119 96.1(8) . . ? C123 Ir5 N9 106.9(7) . . ? N15 Ir5 N9 86.4(5) . . ? C119 Ir5 N9 143.6(8) . . ? C123 Ir5 C122 41.0(8) . . ? N15 Ir5 C122 148.9(8) . . ? C119 Ir5 C122 62.2(9) . . ? N9 Ir5 C122 98.5(6) . . ? C123 Ir5 C120 67.6(10) . . ? N15 Ir5 C120 110.8(8) . . ? C119 Ir5 C120 37.3(9) . . ? N9 Ir5 C120 162.8(7) . . ? C122 Ir5 C120 66.3(8) . . ? C123 Ir5 C121 65.6(9) . . ? N15 Ir5 C121 150.4(7) . . ? C119 Ir5 C121 60.6(8) . . ? N9 Ir5 C121 123.1(5) . . ? C122 Ir5 C121 37.3(7) . . ? C120 Ir5 C121 39.6(8) . . ? C123 Ir5 N10 167.3(8) . . ? N15 Ir5 N10 84.0(5) . . ? C119 Ir5 N10 139.4(7) . . ? N9 Ir5 N10 77.0(5) . . ? C122 Ir5 N10 127.1(7) . . ? C120 Ir5 N10 104.9(9) . . ? C121 Ir5 N10 102.0(6) . . ? N12 Ir6 N21 82.6(5) . . ? N12 Ir6 N11 79.2(5) . . ? N21 Ir6 N11 84.1(4) . . ? N12 Ir6 C130 165.1(5) . . ? N21 Ir6 C130 110.7(4) . . ? N11 Ir6 C130 108.0(4) . . ? N12 Ir6 C129 129.2(4) . . ? N21 Ir6 C129 148.1(4) . . ? N11 Ir6 C129 98.4(4) . . ? C130 Ir6 C129 38.3(2) . . ? N12 Ir6 C131 137.3(4) . . ? N21 Ir6 C131 95.5(5) . . ? N11 Ir6 C131 143.4(4) . . ? C130 Ir6 C131 38.17(19) . . ? C129 Ir6 C131 63.8(3) . . ? N12 Ir6 C133 101.4(4) . . ? N21 Ir6 C133 153.4(4) . . ? N11 Ir6 C133 122.5(4) . . ? C130 Ir6 C133 63.8(3) . . ? C129 Ir6 C133 38.1(2) . . ? C131 Ir6 C133 63.6(3) . . ? N12 Ir6 C132 105.1(4) . . ? N21 Ir6 C132 115.6(4) . . ? N11 Ir6 C132 160.1(4) . . ? C130 Ir6 C132 63.7(3) . . ? C129 Ir6 C132 63.6(3) . . ? C131 Ir6 C132 37.94(19) . . ? C133 Ir6 C132 37.9(2) . . ? C7 N1 C1 102.5(11) . . ? C7 N1 Ir1 112.8(9) . . ? C1 N1 Ir1 143.7(9) . . ? C8 N2 C9 102.4(12) . . ? C8 N2 Ir1 109.8(9) . . ? C9 N2 Ir1 146.4(10) . . ? C8 N3 C14 105.4(11) . . ? C8 N3 Ir2 108.7(9) . . ? C14 N3 Ir2 144.3(9) . . ? C7 N4 C6 106.8(11) . . ? C7 N4 Ir2 112.0(9) . . ? C6 N4 Ir2 139.1(10) . . ? C21 N5 C15 100.8(17) . . ? C21 N5 Ir3 110.4(10) . . ? C15 N5 Ir3 147.0(16) . . ? C22 N6 C23 106.7(17) . . ? C22 N6 Ir3 110.0(12) . . ? C23 N6 Ir3 141.7(13) . . ? C22 N7 C28 101.4(13) . . ? C22 N7 Ir4 112.5(9) . . ? C28 N7 Ir4 142.6(12) . . ? C21 N8 C20 104.3(16) . . ? C21 N8 Ir4 108.9(11) . . ? C20 N8 Ir4 144.5(14) . . ? C35 N9 C29 101.2(12) . . ? C35 N9 Ir5 111.8(9) . . ? C29 N9 Ir5 146.1(11) . . ? C36 N10 C37 107.3(13) . . ? C36 N10 Ir5 107.5(10) . . ? C37 N10 Ir5 142.5(11) . . ? C36 N11 C42 100.4(14) . . ? C36 N11 Ir6 107.3(9) . . ? C42 N11 Ir6 150.2(12) . . ? C35 N12 C34 94.9(13) . . ? C35 N12 Ir6 115.0(10) . . ? C34 N12 Ir6 150.0(10) . . ? C46 N13 C50 119.5(13) . . ? C46 N13 Ir1 121.2(10) . . ? C50 N13 Ir1 119.3(10) . . ? C55 N14 C51 114.7(16) . . ? C55 N14 Ir3 123.1(12) . . ? C51 N14 Ir3 120.9(13) . . ? C60 N15 C56 115.0(15) . . ? C60 N15 Ir5 124.1(12) . . ? C56 N15 Ir5 120.3(10) . . ? C43 N16 C45 111.1(14) . . ? C44 N17 C43 116.1(13) . . ? C45 N18 C44 114.1(13) . . ? C68 N19 C64 117.6(12) . . ? C68 N19 Ir2 120.1(9) . . ? C64 N19 Ir2 122.2(10) . . ? C73 N20 C69 121.1(15) . . ? C73 N20 Ir4 118.7(11) . . ? C69 N20 Ir4 119.3(12) . . ? C78 N21 C74 117.3(14) . . ? C78 N21 Ir6 119.3(12) . . ? C74 N21 Ir6 122.5(10) . . ? C61 N22 C63 114.2(13) . . ? C62 N23 C61 114.1(14) . . ? C63 N24 C62 114.4(13) . . ? N1 C1 C6 108.6(11) . . ? N1 C1 C2 134.2(15) . . ? C6 C1 C2 117.3(14) . . ? C3 C2 C1 120.0(18) . . ? C4 C3 C2 119.4(18) . . ? C3 C4 C5 129(2) . . ? C4 C5 C6 113.5(16) . . ? C1 C6 N4 102.2(11) . . ? C1 C6 C5 121.1(13) . . ? N4 C6 C5 136.6(14) . . ? N4 C7 N1 119.9(11) . . ? N4 C7 C8 122.2(12) . . ? N1 C7 C8 117.3(13) . . ? N2 C8 N3 116.7(12) . . ? N2 C8 C7 122.5(13) . . ? N3 C8 C7 120.6(13) . . ? C10 C9 C14 121.3(13) . . ? C10 C9 N2 131.7(15) . . ? C14 C9 N2 106.9(11) . . ? C9 C10 C11 121.8(18) . . ? C10 C11 C12 117.8(17) . . ? C13 C12 C11 123.3(15) . . ? C12 C13 C14 116.3(15) . . ? N3 C14 C9 108.6(11) . . ? N3 C14 C13 132.0(14) . . ? C9 C14 C13 119.3(13) . . ? C20 C15 C16 128(2) . . ? C20 C15 N5 110(2) . . ? C16 C15 N5 121(3) . . ? C15 C16 C17 112(2) . . ? C16 C17 C18 117.8(19) . . ? C19 C18 C17 124.5(19) . . ? C18 C19 C20 115(2) . . ? C15 C20 N8 108.3(17) . . ? C15 C20 C19 123(2) . . ? N8 C20 C19 129(2) . . ? N8 C21 N5 116.6(14) . . ? N8 C21 C22 124.9(18) . . ? N5 C21 C22 117.0(17) . . ? N6 C22 N7 118.0(14) . . ? N6 C22 C21 124.7(19) . . ? N7 C22 C21 115.4(17) . . ? N6 C23 C24 133(2) . . ? N6 C23 C28 105.4(14) . . ? C24 C23 C28 121.7(18) . . ? C23 C24 C25 115(2) . . ? C26 C25 C24 122(2) . . ? C25 C26 C27 123.5(19) . . ? C28 C27 C26 115(2) . . ? C27 C28 C23 121.9(16) . . ? C27 C28 N7 129.2(18) . . ? C23 C28 N7 108.5(14) . . ? C30 C29 C34 125.8(15) . . ? C30 C29 N9 127.4(16) . . ? C34 C29 N9 106.7(13) . . ? C29 C30 C31 117.6(18) . . ? C32 C31 C30 115.6(18) . . ? C33 C32 C31 123.2(19) . . ? C32 C33 C34 119(2) . . ? C29 C34 C33 118.7(16) . . ? C29 C34 N12 114.0(12) . . ? C33 C34 N12 127.2(16) . . ? C36 C35 N9 117.5(13) . . ? C36 C35 N12 117.0(15) . . ? N9 C35 N12 122.5(14) . . ? N10 C36 C35 125.2(15) . . ? N10 C36 N11 114.2(12) . . ? C35 C36 N11 120.5(15) . . ? C42 C37 N10 106.1(13) . . ? C42 C37 C38 117.9(18) . . ? N10 C37 C38 136.0(18) . . ? C39 C38 C37 119.7(19) . . ? C38 C39 C40 119.9(19) . . ? C41 C40 C39 124(2) . . ? C40 C41 C42 114(2) . . ? C37 C42 N11 111.6(15) . . ? C37 C42 C41 124.7(16) . . ? N11 C42 C41 123.6(18) . . ? N16 C43 N17 127.4(14) . . ? N16 C43 C48 115.5(14) . . ? N17 C43 C48 117.0(13) . . ? N17 C44 N18 123.4(14) . . ? N17 C44 C53 119.3(13) . . ? N18 C44 C53 117.3(13) . . ? N18 C45 N16 127.3(14) . . ? N18 C45 C58 114.8(16) . . ? N16 C45 C58 117.9(15) . . ? N13 C46 C47 124.7(14) . . ? C46 C47 C48 117.8(13) . . ? C49 C48 C47 117.0(12) . . ? C49 C48 C43 124.2(14) . . ? C47 C48 C43 118.1(13) . . ? C48 C49 C50 123.5(14) . . ? N13 C50 C49 115.8(13) . . ? N14 C51 C52 126.3(17) . . ? C51 C52 C53 117.3(15) . . ? C52 C53 C54 117.6(17) . . ? C52 C53 C44 122.6(15) . . ? C54 C53 C44 118.7(15) . . ? C55 C54 C53 119.2(18) . . ? C54 C55 N14 124.9(17) . . ? N15 C56 C57 119.4(15) . . ? C58 C57 C56 120.6(17) . . ? C57 C58 C59 116.7(15) . . ? C57 C58 C45 120.3(17) . . ? C59 C58 C45 123.0(14) . . ? C60 C59 C58 116.8(14) . . ? N15 C60 C59 130.9(17) . . ? N22 C61 N23 125.3(14) . . ? N22 C61 C66 117.3(13) . . ? N23 C61 C66 117.3(12) . . ? N23 C62 N24 125.0(15) . . ? N23 C62 C71 118.5(14) . . ? N24 C62 C71 116.4(14) . . ? N22 C63 N24 126.0(14) . . ? N22 C63 C76 118.0(13) . . ? N24 C63 C76 116.0(14) . . ? C65 C64 N19 122.4(15) . . ? C64 C65 C66 116.4(14) . . ? C67 C66 C65 125.2(15) . . ? C67 C66 C61 120.0(13) . . ? C65 C66 C61 114.6(12) . . ? C66 C67 C68 117.8(15) . . ? N19 C68 C67 119.6(14) . . ? N20 C69 C70 122.7(16) . . ? C71 C70 C69 117.6(16) . . ? C72 C71 C62 121.0(13) . . ? C72 C71 C70 116.8(14) . . ? C62 C71 C70 121.9(14) . . ? C71 C72 C73 120.8(15) . . ? N20 C73 C72 120.4(16) . . ? N21 C74 C75 118.4(13) . . ? C76 C75 C74 120.9(15) . . ? C75 C76 C77 120.9(15) . . ? C75 C76 C63 121.3(15) . . ? C77 C76 C63 117.7(14) . . ? C78 C77 C76 114.2(15) . . ? N21 C78 C77 127.2(19) . . ? C80 C79 C83 111.2(17) . . ? C80 C79 C84 129(2) . . ? C83 C79 C84 120(2) . . ? C80 C79 Ir1 72.7(10) . . ? C83 C79 Ir1 71.5(8) . . ? C84 C79 Ir1 126.8(15) . . ? C79 C80 C81 110.9(18) . . ? C79 C80 C85 119(2) . . ? C81 C80 C85 130(2) . . ? C79 C80 Ir1 69.9(10) . . ? C81 C80 Ir1 72.4(11) . . ? C85 C80 Ir1 122.9(16) . . ? C80 C81 C86 121(2) . . ? C80 C81 C82 106.2(17) . . ? C86 C81 C82 130(2) . . ? C80 C81 Ir1 70.4(11) . . ? C86 C81 Ir1 136.7(14) . . ? C82 C81 Ir1 71.3(11) . . ? C81 C82 C83 107.2(17) . . ? C81 C82 C87 122.8(18) . . ? C83 C82 C87 129.1(19) . . ? C81 C82 Ir1 69.6(10) . . ? C83 C82 Ir1 67.8(9) . . ? C87 C82 Ir1 119.4(15) . . ? C79 C83 C88 136.6(17) . . ? C79 C83 C82 104.3(15) . . ? C88 C83 C82 118.9(18) . . ? C79 C83 Ir1 69.8(9) . . ? C88 C83 Ir1 125.1(12) . . ? C82 C83 Ir1 72.3(9) . . ? C90 C89 C93 105.3(17) . . ? C90 C89 C94 127.3(17) . . ? C93 C89 C94 127.2(18) . . ? C90 C89 Ir2 69.8(10) . . ? C93 C89 Ir2 70.3(10) . . ? C94 C89 Ir2 128.5(13) . . ? C89 C90 C91 107.9(16) . . ? C89 C90 C95 123.1(19) . . ? C91 C90 C95 129.0(19) . . ? C89 C90 Ir2 71.9(11) . . ? C91 C90 Ir2 68.2(11) . . ? C95 C90 Ir2 126.6(19) . . ? C92 C91 C90 107(2) . . ? C92 C91 C96 132(2) . . ? C90 C91 C96 117.9(18) . . ? C92 C91 Ir2 76.2(15) . . ? C90 C91 Ir2 71.5(12) . . ? C96 C91 Ir2 132.4(13) . . ? C91 C92 C93 112(2) . . ? C91 C92 C97 122(3) . . ? C93 C92 C97 126(3) . . ? C91 C92 Ir2 67.7(13) . . ? C93 C92 Ir2 70.3(13) . . ? C97 C92 Ir2 123.4(17) . . ? C92 C93 C89 107.5(19) . . ? C92 C93 C98 135(2) . . ? C89 C93 C98 117(2) . . ? C92 C93 Ir2 72.8(12) . . ? C89 C93 Ir2 70.3(10) . . ? C98 C93 Ir2 123.9(15) . . ? C103 C99 C100 108.0 . . ? C103 C99 C104 126.0 . . ? C100 C99 C104 126.0 . . ? C103 C99 Ir3 71.8(2) . . ? C100 C99 Ir3 69.8(2) . . ? C104 C99 Ir3 124.0(2) . . ? C101 C100 C99 108.0 . . ? C101 C100 C105 126.0 . . ? C99 C100 C105 126.0 . . ? C101 C100 Ir3 71.2(2) . . ? C99 C100 Ir3 71.1(2) . . ? C105 C100 Ir3 123.3(2) . . ? C100 C101 C102 108.0 . . ? C100 C101 C106 126.0 . . ? C102 C101 C106 126.0 . . ? C100 C101 Ir3 69.8(2) . . ? C102 C101 Ir3 71.8(2) . . ? C106 C101 Ir3 124.0(2) . . ? C103 C102 C101 108.0 . . ? C103 C102 C107 126.0 . . ? C101 C102 C107 126.0 . . ? C103 C102 Ir3 70.8(2) . . ? C101 C102 Ir3 69.6(2) . . ? C107 C102 Ir3 125.16(19) . . ? C102 C103 C99 108.0 . . ? C102 C103 C108 126.0 . . ? C99 C103 C108 126.0 . . ? C102 C103 Ir3 70.9(2) . . ? C99 C103 Ir3 69.6(2) . . ? C108 C103 Ir3 125.1(2) . . ? C113 C109 C110 108.0 . . ? C113 C109 C114 126.0 . . ? C110 C109 C114 126.0 . . ? C113 C109 Ir4 67.8(2) . . ? C110 C109 Ir4 74.1(2) . . ? C114 C109 Ir4 123.7(2) . . ? C111 C110 C109 108.0 . . ? C111 C110 C115 126.0 . . ? C109 C110 C115 126.0 . . ? C111 C110 Ir4 70.7(2) . . ? C109 C110 Ir4 68.0(2) . . ? C115 C110 Ir4 126.8(2) . . ? C112 C111 C110 108.0 . . ? C112 C111 C116 126.0 . . ? C110 C111 C116 126.0 . . ? C112 C111 Ir4 67.5(2) . . ? C110 C111 Ir4 71.9(2) . . ? C116 C111 Ir4 126.18(19) . . ? C111 C112 C113 108.0 . . ? C111 C112 C117 126.0 . . ? C113 C112 C117 126.0 . . ? C111 C112 Ir4 74.3(2) . . ? C113 C112 Ir4 68.7(2) . . ? C117 C112 Ir4 122.7(2) . . ? C109 C113 C112 108.0 . . ? C109 C113 C118 126.0 . . ? C112 C113 C118 126.0 . . ? C109 C113 Ir4 72.9(2) . . ? C112 C113 Ir4 71.8(2) . . ? C118 C113 Ir4 121.1(2) . . ? C11D C10A C11A 108.0 . . ? C11D C10A C11E 126.0 . . ? C11A C10A C11E 126.0 . . ? C11D C10A Ir4 65.5(2) . . ? C11A C10A Ir4 75.8(2) . . ? C11E C10A Ir4 124.2(2) . . ? C10A C11A C11B 108.0 . . ? C10A C11A C11F 126.0 . . ? C11B C11A C11F 126.0 . . ? C10A C11A Ir4 67.2(2) . . ? C11B C11A Ir4 69.7(2) . . ? C11F C11A Ir4 128.7(2) . . ? C11C C11B C11A 108.0 . . ? C11C C11B C11G 126.0 . . ? C11A C11B C11G 126.0 . . ? C11C C11B Ir4 65.2(2) . . ? C11A C11B Ir4 73.7(2) . . ? C11G C11B Ir4 126.6(2) . . ? C11B C11C C11D 108.0 . . ? C11B C11C C11H 126.0 . . ? C11D C11C C11H 126.0 . . ? C11B C11C Ir4 76.6(2) . . ? C11D C11C Ir4 68.4(2) . . ? C11H C11C Ir4 120.7(2) . . ? C11C C11D C10A 108.0 . . ? C11C C11D C11I 126.0 . . ? C10A C11D C11I 126.0 . . ? C11C C11D Ir4 71.4(2) . . ? C10A C11D Ir4 75.3(2) . . ? C11I C11D Ir4 119.2(2) . . ? C120 C119 C123 120(2) . . ? C120 C119 C124 125(2) . . ? C123 C119 C124 115(2) . . ? C120 C119 Ir5 72.9(15) . . ? C123 C119 Ir5 70.0(12) . . ? C124 C119 Ir5 121.4(18) . . ? C119 C120 C121 99.7(18) . . ? C119 C120 C125 134(3) . . ? C121 C120 C125 124(3) . . ? C119 C120 Ir5 69.8(14) . . ? C121 C120 Ir5 71.5(11) . . ? C125 C120 Ir5 132.8(17) . . ? C122 C121 C120 111(2) . . ? C122 C121 C126 122.5(18) . . ? C120 C121 C126 126(2) . . ? C122 C121 Ir5 69.7(11) . . ? C120 C121 Ir5 68.9(12) . . ? C126 C121 Ir5 124.1(13) . . ? C121 C122 C123 107.8(17) . . ? C121 C122 C127 128(2) . . ? C123 C122 C127 124.5(19) . . ? C121 C122 Ir5 73.1(11) . . ? C123 C122 Ir5 67.5(10) . . ? C127 C122 Ir5 121.6(15) . . ? C119 C123 C122 101(2) . . ? C119 C123 C128 127(2) . . ? C122 C123 C128 128(2) . . ? C119 C123 Ir5 72.1(12) . . ? C122 C123 Ir5 71.5(11) . . ? C128 C123 Ir5 137(2) . . ? C133 C129 C130 108.0 . . ? C133 C129 C134 126.0 . . ? C130 C129 C134 126.0 . . ? C133 C129 Ir6 71.6(4) . . ? C130 C129 Ir6 70.7(4) . . ? C134 C129 Ir6 123.4(3) . . ? C131 C130 C129 108.0 . . ? C131 C130 C135 126.0 . . ? C129 C130 C135 126.0 . . ? C131 C130 Ir6 71.4(3) . . ? C129 C130 Ir6 71.0(4) . . ? C135 C130 Ir6 123.2(3) . . ? C132 C131 C130 108.0 . . ? C132 C131 C136 126.0 . . ? C130 C131 C136 126.0 . . ? C132 C131 Ir6 71.5(4) . . ? C130 C131 Ir6 70.4(3) . . ? C136 C131 Ir6 123.7(4) . . ? C131 C132 C133 108.0 . . ? C131 C132 C137 126.0 . . ? C133 C132 C137 126.0 . . ? C131 C132 Ir6 70.6(4) . . ? C133 C132 Ir6 70.8(4) . . ? C137 C132 Ir6 124.2(3) . . ? C132 C133 C129 108.0 . . ? C132 C133 C138 126.0 . . ? C129 C133 C138 126.0 . . ? C132 C133 Ir6 71.3(3) . . ? C129 C133 Ir6 70.4(3) . . ? C138 C133 Ir6 124.0(3) . . ? 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 0.300 0.085 -0.074 8533.4 1887.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.639 _refine_diff_density_min -2.235 _refine_diff_density_rms 0.222