# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Takahiko Kojima' _publ_contact_author_email KOJIMA@CHEM.TSUKUBA.AC.JP _publ_section_title ; A Tetranuclear Iridium(III) Complex Having a Flavin Analog as Bridging Ligands in Different Coordination Modes and Exchangeable Anion Encapsulation in a Supramolecular Cage ; loop_ _publ_author_name 'Takahiko Kojima' 'Shunichi Fukuzumi' 'Yuji Inui' 'Soushi Miyazaki' 'Motoo Shiro' # Attachment '726570.cif' data_Ir-complex _database_code_depnum_ccdc_archive 'CCDC 726570' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C74.5 H82.5 Cl15.5 F12 Ir4 N12 O8 P2 ' _chemical_formula_moiety 'C70 H74 Cl2 Ir4 N12 O6, 4.5(C H Cl3), 2(H2 O), 2(F6 P)' _chemical_formula_weight 2882.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 31.4226(7) _cell_length_b 24.4702(5) _cell_length_c 34.0543(8) _cell_angle_alpha 90.0000 _cell_angle_beta 122.6940(7) _cell_angle_gamma 90.0000 _cell_volume 22036.3(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 67831 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 123.15 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11096.00 _exptl_absorpt_coefficient_mu 5.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.473 _exptl_absorpt_correction_T_max 0.588 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku SATURN' _diffrn_reflns_number 92718 _diffrn_reflns_av_R_equivalents 0.076 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_ambient_temperature 123.15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 25019 _reflns_number_gt 19654 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2292 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 25019 _refine_ls_number_parameters 1048 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1245P)^2^+312.9670P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0090 _refine_diff_density_max 2.81 _refine_diff_density_min -2.01 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.286647(16) 0.583616(19) 0.567104(17) 0.05552(14) Uani 1 1 d . . . Ir2 Ir 0.167438(14) 0.410004(15) 0.488836(13) 0.04159(11) Uani 1 1 d . . . Cl1 Cl 0.26951(13) 0.59266(12) 0.49042(12) 0.0648(7) Uani 1 1 d . . . N1 N 0.2153(3) 0.6219(4) 0.5384(3) 0.0518(19) Uani 1 1 d U . . N2 N 0.1513(3) 0.4923(3) 0.4958(3) 0.0408(15) Uani 1 1 d U . . N3 N 0.0906(3) 0.5631(3) 0.4758(3) 0.0442(17) Uani 1 1 d U . . H3N H 0.0595 0.5719 0.4642 0.053 Uiso 1 1 calc R . . N4 N 0.1127(3) 0.6540(3) 0.4962(3) 0.0451(16) Uani 1 1 d U . . C1 C 0.1769(4) 0.5859(4) 0.5186(4) 0.0446(18) Uani 1 1 d U . . C2 C 0.1887(4) 0.5288(4) 0.5185(4) 0.0427(17) Uani 1 1 d U . . C3 C 0.1011(4) 0.5094(4) 0.4717(3) 0.0423(18) Uani 1 1 d U . . C4 C 0.1255(4) 0.6025(4) 0.4967(3) 0.0421(17) Uani 1 1 d U . . C5 C 0.1504(4) 0.6905(4) 0.5152(4) 0.053(2) Uani 1 1 d U . . C6 C 0.1384(5) 0.7476(5) 0.5127(5) 0.067(3) Uani 1 1 d U . . H6 H 0.1053 0.7580 0.5018 0.080 Uiso 1 1 calc R . . C7 C 0.1736(6) 0.7856(5) 0.5259(6) 0.081(3) Uani 1 1 d U . . H7 H 0.1651 0.8223 0.5240 0.098 Uiso 1 1 calc R . . C8 C 0.2248(6) 0.7701(6) 0.5431(6) 0.095(4) Uani 1 1 d U . . H8 H 0.2492 0.7968 0.5508 0.114 Uiso 1 1 calc R . . C9 C 0.2375(5) 0.7180(5) 0.5479(6) 0.083(3) Uani 1 1 d U . . H9 H 0.2712 0.7088 0.5609 0.099 Uiso 1 1 calc R . . C10 C 0.2007(4) 0.6751(5) 0.5339(5) 0.061(2) Uani 1 1 d U . . O1 O 0.2346(3) 0.5159(3) 0.5395(3) 0.0492(16) Uani 1 1 d U . . O2 O 0.0670(3) 0.4776(3) 0.4459(3) 0.0533(18) Uani 1 1 d U . . C11 C 0.3677(6) 0.5812(8) 0.6010(6) 0.092(2) Uani 1 1 d U . . C12 C 0.3512(5) 0.5375(7) 0.6176(6) 0.083(2) Uani 1 1 d U . . C13 C 0.3287(5) 0.5602(7) 0.6402(5) 0.0804(19) Uani 1 1 d U . . C14 C 0.3282(6) 0.6192(7) 0.6358(6) 0.088(2) Uani 1 1 d U . . C15 C 0.3544(6) 0.6277(8) 0.6114(6) 0.093(2) Uani 1 1 d U . . C16 C 0.3955(6) 0.5735(9) 0.5762(7) 0.102(3) Uani 1 1 d U . . H16A H 0.3925 0.6061 0.5592 0.122 Uiso 1 1 calc R . . H16B H 0.3811 0.5433 0.5550 0.122 Uiso 1 1 calc R . . H16C H 0.4306 0.5663 0.5989 0.122 Uiso 1 1 calc R . . C17 C 0.3570(6) 0.4758(7) 0.6145(6) 0.095(3) Uani 1 1 d U . . H17A H 0.3921 0.4660 0.6338 0.114 Uiso 1 1 calc R . . H17B H 0.3444 0.4659 0.5827 0.114 Uiso 1 1 calc R . . H17C H 0.3382 0.4567 0.6249 0.114 Uiso 1 1 calc R . . C18 C 0.3099(6) 0.5293(7) 0.6652(5) 0.081(3) Uani 1 1 d U . . H18A H 0.3019 0.5542 0.6821 0.097 Uiso 1 1 calc R . . H18B H 0.3355 0.5042 0.6866 0.097 Uiso 1 1 calc R . . H18C H 0.2800 0.5093 0.6431 0.097 Uiso 1 1 calc R . . C19 C 0.3087(6) 0.6556(7) 0.6576(6) 0.094(3) Uani 1 1 d U . . H19A H 0.2781 0.6729 0.6337 0.113 Uiso 1 1 calc R . . H19B H 0.3335 0.6830 0.6760 0.113 Uiso 1 1 calc R . . H19C H 0.3019 0.6343 0.6773 0.113 Uiso 1 1 calc R . . C20 C 0.3675(6) 0.6863(8) 0.6031(7) 0.106(3) Uani 1 1 d U . . H20A H 0.4036 0.6908 0.6207 0.127 Uiso 1 1 calc R . . H20B H 0.3528 0.7128 0.6131 0.127 Uiso 1 1 calc R . . H20C H 0.3543 0.6912 0.5705 0.127 Uiso 1 1 calc R . . Ir3 Ir 0.202550(15) 0.476685(17) 0.784724(13) 0.04712(12) Uani 1 1 d . . . Ir4 Ir 0.104320(15) 0.332463(15) 0.645968(13) 0.04209(11) Uani 1 1 d . . . Cl2 Cl 0.14463(12) 0.44433(14) 0.80434(10) 0.0639(7) Uani 1 1 d . . . N5 N 0.1389(3) 0.5246(3) 0.7374(3) 0.0464(19) Uani 1 1 d . . . N6 N 0.0899(3) 0.4162(3) 0.6530(3) 0.0385(17) Uani 1 1 d . . . N7 N 0.0315(3) 0.4899(4) 0.6233(3) 0.0470(19) Uani 1 1 d . . . H7N H 0.0039 0.5035 0.6005 0.056 Uiso 1 1 calc R . . N8 N 0.0458(3) 0.5709(3) 0.6647(3) 0.049(2) Uani 1 1 d . . . C21 C 0.1076(4) 0.4990(4) 0.6972(3) 0.041(2) Uani 1 1 d . . . C22 C 0.1206(4) 0.4439(4) 0.6906(3) 0.042(2) Uani 1 1 d . . . C23 C 0.0434(4) 0.4378(4) 0.6190(3) 0.043(2) Uani 1 1 d . . . C24 C 0.0610(4) 0.5222(4) 0.6618(4) 0.044(2) Uani 1 1 d . . . C25 C 0.0767(4) 0.5977(4) 0.7056(4) 0.055(3) Uani 1 1 d . . . C26 C 0.0612(5) 0.6491(5) 0.7122(5) 0.067(3) Uani 1 1 d . . . H26 H 0.0321 0.6653 0.6878 0.080 Uiso 1 1 calc R . . C27 C 0.0884(6) 0.6751(6) 0.7538(6) 0.085(5) Uani 1 1 d . . . H27 H 0.0782 0.7091 0.7580 0.102 Uiso 1 1 calc R A . C28 C 0.1333(5) 0.6494(6) 0.7916(6) 0.075(4) Uani 1 1 d . . . H28 H 0.1508 0.6665 0.8205 0.089 Uiso 1 1 calc R . . C29 C 0.1506(5) 0.6026(5) 0.7864(4) 0.060(3) Uani 1 1 d . . . H29 H 0.1806 0.5883 0.8112 0.072 Uiso 1 1 calc R A . C30 C 0.1238(5) 0.5738(5) 0.7433(4) 0.057(3) Uani 1 1 d . . . O3 O 0.1620(3) 0.4248(3) 0.7243(2) 0.0467(16) Uani 1 1 d . . . O4 O 0.0119(3) 0.4107(3) 0.5849(3) 0.0539(19) Uani 1 1 d . . . C31 C 0.2705(5) 0.4551(7) 0.8496(4) 0.072(2) Uani 1 1 d U . . C32 C 0.2739(5) 0.4365(6) 0.8121(5) 0.067(2) Uani 1 1 d U . . C33 C 0.2711(4) 0.4841(5) 0.7854(4) 0.058(2) Uani 1 1 d U . . C34 C 0.2654(4) 0.5313(5) 0.8064(4) 0.058(2) Uani 1 1 d U . . C35 C 0.2641(5) 0.5138(7) 0.8472(4) 0.070(2) Uani 1 1 d U . . C36 C 0.2721(6) 0.4212(8) 0.8875(5) 0.089(4) Uani 1 1 d U . . H36A H 0.2635 0.4438 0.9053 0.107 Uiso 1 1 calc R . . H36B H 0.3055 0.4066 0.9077 0.107 Uiso 1 1 calc R . . H36C H 0.2482 0.3917 0.8736 0.107 Uiso 1 1 calc R . . C37 C 0.2822(6) 0.3797(6) 0.8029(6) 0.081(3) Uani 1 1 d U . . H37A H 0.2662 0.3549 0.8129 0.097 Uiso 1 1 calc R . . H37B H 0.3179 0.3723 0.8198 0.097 Uiso 1 1 calc R . . H37C H 0.2680 0.3750 0.7701 0.097 Uiso 1 1 calc R . . C38 C 0.2769(5) 0.4844(6) 0.7454(5) 0.065(3) Uani 1 1 d U . . H38A H 0.3121 0.4813 0.7563 0.078 Uiso 1 1 calc R . . H38B H 0.2637 0.5179 0.7284 0.078 Uiso 1 1 calc R . . H38C H 0.2587 0.4541 0.7253 0.078 Uiso 1 1 calc R . . C39 C 0.2648(6) 0.5882(6) 0.7904(6) 0.076(3) Uani 1 1 d U . . H39A H 0.2400 0.5910 0.7576 0.091 Uiso 1 1 calc R . . H39B H 0.2976 0.5971 0.7964 0.091 Uiso 1 1 calc R . . H39C H 0.2564 0.6132 0.8070 0.091 Uiso 1 1 calc R . . C40 C 0.2675(5) 0.5499(8) 0.8827(5) 0.082(3) Uani 1 1 d U . . H40A H 0.2589 0.5864 0.8707 0.098 Uiso 1 1 calc R . . H40B H 0.3014 0.5493 0.9097 0.098 Uiso 1 1 calc R . . H40C H 0.2444 0.5377 0.8912 0.098 Uiso 1 1 calc R . . N9 N 0.1220(2) 0.3860(3) 0.52057(16) 0.035(3) Uiso 0.516(10) 1 d PG A 1 N10 N 0.23610(18) 0.3872(3) 0.63739(19) 0.020(2) Uiso 0.516(10) 1 d PG A 1 N11 N 0.1659(2) 0.3595(3) 0.64106(16) 0.039(3) Uiso 0.516(10) 1 d PG A 1 N12 N 0.08382(19) 0.3532(3) 0.5763(2) 0.040(3) Uiso 0.516(10) 1 d PG A 1 C41 C 0.15154(17) 0.3820(2) 0.56797(16) 0.033(3) Uiso 0.516(10) 1 d PG A 1 C42 C 0.20498(18) 0.3953(3) 0.59060(19) 0.038(4) Uiso 0.516(10) 1 d PG A 1 C43 C 0.2171(2) 0.3662(3) 0.66204(16) 0.055(5) Uiso 0.516(10) 1 d PG A 1 C44 C 0.13277(18) 0.3648(2) 0.59555(16) 0.033(3) Uiso 0.516(10) 1 d PG A 1 C45 C 0.05414(17) 0.3557(3) 0.5296(2) 0.046(6) Uiso 0.516(10) 1 d PG A 1 C46 C 0.00152(18) 0.3414(4) 0.5079(3) 0.038(4) Uiso 0.516(10) 1 d PG A 1 H46 H -0.0120 0.3348 0.5259 0.045 Uiso 0.516(10) 1 calc PR A 1 C47 C -0.02810(19) 0.3376(4) 0.4602(3) 0.040(4) Uiso 0.516(10) 1 d PG A 1 H47 H -0.0625 0.3304 0.4455 0.048 Uiso 0.516(10) 1 calc PR A 1 C48 C -0.0072(2) 0.3445(4) 0.4342(2) 0.068(7) Uiso 0.516(10) 1 d PG A 1 H48 H -0.0266 0.3357 0.4027 0.082 Uiso 0.516(10) 1 calc PR A 1 C49 C 0.0420(2) 0.3642(4) 0.45251(17) 0.066(7) Uiso 0.516(10) 1 d PG A 1 H49 H 0.0533 0.3736 0.4332 0.079 Uiso 0.516(10) 1 calc PR A 1 C50 C 0.07391(19) 0.3692(3) 0.50213(17) 0.036(7) Uiso 0.516(10) 1 d PG A 1 O5 O 0.2202(2) 0.4113(4) 0.5660(2) 0.048(3) Uiso 0.516(10) 1 d PG A 1 O6 O 0.2464(3) 0.3514(4) 0.70359(17) 0.065(4) Uiso 0.516(10) 1 d PG A 1 N9A N 0.1000(2) 0.3518(3) 0.57906(18) 0.023(3) Uiso 0.484(10) 1 d PG A 2 N10A N 0.2318(2) 0.3950(3) 0.64658(19) 0.073(7) Uiso 0.484(10) 1 d PG A 2 N11A N 0.1985(2) 0.4055(3) 0.5657(2) 0.055(5) Uiso 0.484(10) 1 d PG A 2 N12A N 0.1162(2) 0.3826(3) 0.50735(16) 0.039(4) Uiso 0.484(10) 1 d PG A 2 C41A C 0.14545(19) 0.3697(2) 0.58793(16) 0.024(3) Uiso 0.484(10) 1 d PG A 2 C42A C 0.1873(2) 0.3729(3) 0.63653(16) 0.037(4) Uiso 0.484(10) 1 d PG A 2 C43A C 0.24095(19) 0.3960(3) 0.6042(2) 0.042(4) Uiso 0.484(10) 1 d PG A 2 C44A C 0.15330(19) 0.3859(2) 0.55240(17) 0.029(3) Uiso 0.484(10) 1 d PG A 2 C45A C 0.0708(2) 0.3663(3) 0.49769(16) 0.045(9) Uiso 0.484(10) 1 d PG A 2 C46A C 0.0297(2) 0.3645(4) 0.44933(17) 0.032(4) Uiso 0.484(10) 1 d PG A 2 H46A H 0.0356 0.3703 0.4257 0.038 Uiso 0.484(10) 1 calc PR A 2 C47A C -0.0181(2) 0.3539(4) 0.4390(2) 0.033(4) Uiso 0.484(10) 1 d PG A 2 H47A H -0.0448 0.3505 0.4080 0.040 Uiso 0.484(10) 1 calc PR A 2 C48A C -0.02674(19) 0.3482(4) 0.4741(3) 0.049(5) Uiso 0.484(10) 1 d PG A 2 H48A H -0.0601 0.3474 0.4662 0.059 Uiso 0.484(10) 1 calc PR A 2 C49A C 0.0119(2) 0.3437(4) 0.5214(2) 0.041(4) Uiso 0.484(10) 1 d PG A 2 H49A H 0.0050 0.3344 0.5439 0.050 Uiso 0.484(10) 1 calc PR A 2 C50A C 0.06245(19) 0.3539(3) 0.53354(19) 0.031(5) Uiso 0.484(10) 1 d PG A 2 O5A O 0.1798(3) 0.3574(4) 0.66679(16) 0.045(3) Uiso 0.484(10) 1 d PG A 2 O6A O 0.2827(2) 0.4067(4) 0.6144(3) 0.050(4) Uiso 0.484(10) 1 d PG A 2 C51 C 0.1364(4) 0.3852(5) 0.4170(3) 0.058(3) Uani 1 1 d . . . C52 C 0.1734(5) 0.4282(5) 0.4297(4) 0.059(3) Uani 1 1 d . . . C53 C 0.2210(4) 0.4090(5) 0.4683(4) 0.052(3) Uani 1 1 d . . . C54 C 0.2135(4) 0.3541(5) 0.4787(4) 0.053(3) Uani 1 1 d . . . C55 C 0.1633(5) 0.3382(5) 0.4491(4) 0.061(3) Uani 1 1 d . . . C56 C 0.0844(5) 0.3844(7) 0.3770(4) 0.078(4) Uani 1 1 d . . . H56A H 0.0841 0.3781 0.3491 0.093 Uiso 1 1 calc R . . H56B H 0.0686 0.4189 0.3748 0.093 Uiso 1 1 calc R . . H56C H 0.0661 0.3557 0.3809 0.093 Uiso 1 1 calc R . . C57 C 0.1626(6) 0.4829(6) 0.4064(5) 0.073(4) Uani 1 1 d . . . H57A H 0.1276 0.4920 0.3932 0.088 Uiso 1 1 calc R . . H57B H 0.1695 0.4816 0.3822 0.088 Uiso 1 1 calc R . . H57C H 0.1836 0.5100 0.4290 0.088 Uiso 1 1 calc R . . C58 C 0.2711(5) 0.4382(6) 0.4906(5) 0.070(3) Uani 1 1 d . . . H58A H 0.2938 0.4237 0.5213 0.083 Uiso 1 1 calc R . . H58B H 0.2661 0.4765 0.4927 0.083 Uiso 1 1 calc R . . H58C H 0.2852 0.4329 0.4719 0.083 Uiso 1 1 calc R . . C59 C 0.2556(4) 0.3213(5) 0.5179(4) 0.059(3) Uani 1 1 d . . . H59A H 0.2759 0.3054 0.5076 0.071 Uiso 1 1 calc R . . H59B H 0.2415 0.2929 0.5269 0.071 Uiso 1 1 calc R . . H59C H 0.2762 0.3448 0.5441 0.071 Uiso 1 1 calc R . . C60 C 0.1402(6) 0.2865(5) 0.4466(6) 0.081(4) Uani 1 1 d . . . H60A H 0.1557 0.2713 0.4773 0.097 Uiso 1 1 calc R . . H60B H 0.1447 0.2619 0.4271 0.097 Uiso 1 1 calc R . . H60C H 0.1047 0.2917 0.4336 0.097 Uiso 1 1 calc R . . C61 C 0.0466(5) 0.2788(5) 0.6392(5) 0.059(3) Uani 1 1 d . . . C62 C 0.0843(5) 0.2478(4) 0.6358(5) 0.061(3) Uani 1 1 d . . . C63 C 0.1317(5) 0.2537(4) 0.6783(5) 0.062(3) Uani 1 1 d . . . C64 C 0.1245(5) 0.2887(4) 0.7087(4) 0.056(3) Uani 1 1 d . . . C65 C 0.0714(5) 0.3029(5) 0.6837(4) 0.058(3) Uani 1 1 d . . . C66 C -0.0092(5) 0.2802(6) 0.6043(5) 0.067(3) Uani 1 1 d . . . H66A H -0.0156 0.2778 0.5734 0.080 Uiso 1 1 calc R . . H66B H -0.0228 0.3138 0.6075 0.080 Uiso 1 1 calc R . . H66C H -0.0249 0.2499 0.6096 0.080 Uiso 1 1 calc R . . C67 C 0.0732(7) 0.2134(5) 0.5949(6) 0.082(4) Uani 1 1 d . . . H67A H 0.0416 0.2246 0.5679 0.098 Uiso 1 1 calc R . . H67B H 0.0712 0.1757 0.6015 0.098 Uiso 1 1 calc R . . H67C H 0.0998 0.2180 0.5892 0.098 Uiso 1 1 calc R . . C68 C 0.1795(7) 0.2263(7) 0.6918(7) 0.099(6) Uani 1 1 d . . . H68A H 0.1831 0.2253 0.6656 0.119 Uiso 1 1 calc R . . H68B H 0.1792 0.1896 0.7018 0.119 Uiso 1 1 calc R . . H68C H 0.2073 0.2460 0.7169 0.119 Uiso 1 1 calc R . . C69 C 0.1637(6) 0.3017(6) 0.7561(4) 0.077(4) Uani 1 1 d . . . H69A H 0.1579 0.3375 0.7637 0.092 Uiso 1 1 calc R . . H69B H 0.1960 0.3009 0.7592 0.092 Uiso 1 1 calc R . . H69C H 0.1634 0.2753 0.7768 0.092 Uiso 1 1 calc R . . C70 C 0.0475(6) 0.3378(5) 0.7015(5) 0.066(3) Uani 1 1 d . . . H70A H 0.0707 0.3661 0.7207 0.079 Uiso 1 1 calc R . . H70B H 0.0389 0.3162 0.7197 0.079 Uiso 1 1 calc R . . H70C H 0.0175 0.3540 0.6758 0.079 Uiso 1 1 calc R . . P1 P 0.15352(12) 0.55317(14) 0.61857(11) 0.0586(7) Uani 1 1 d . . . F1 F 0.2047(3) 0.5786(4) 0.6610(3) 0.094(3) Uani 1 1 d . . . F2 F 0.1251(4) 0.5829(4) 0.6407(4) 0.104(3) Uani 1 1 d . . . F3 F 0.1029(5) 0.5304(5) 0.5772(5) 0.148(5) Uani 1 1 d . . . F4 F 0.1843(4) 0.5262(4) 0.5988(3) 0.089(3) Uani 1 1 d . . . F5 F 0.1464(4) 0.6072(4) 0.5904(3) 0.094(3) Uani 1 1 d . . . F6 F 0.1618(4) 0.4999(4) 0.6477(3) 0.088(3) Uani 1 1 d . . . P2 P 0.2249(2) 0.2189(2) 0.59983(19) 0.1005(13) Uani 1 1 d U . . F7 F 0.2660(5) 0.2622(6) 0.6065(4) 0.135(3) Uani 1 1 d U . . F8 F 0.1955(5) 0.2183(6) 0.5468(4) 0.135(3) Uani 1 1 d U . . F9 F 0.1846(5) 0.1763(4) 0.5963(4) 0.108(2) Uani 1 1 d U . . F10 F 0.2559(5) 0.2097(5) 0.6531(4) 0.117(3) Uani 1 1 d U . . F11 F 0.1953(5) 0.2661(4) 0.6031(4) 0.131(3) Uani 1 1 d U . . F12 F 0.2577(6) 0.1739(6) 0.5963(5) 0.146(3) Uani 1 1 d U . . C71 C 0.4743(4) 0.9985(3) 0.2359(4) 0.085(8) Uiso 0.50 1 d PG B -3 H71 H 0.4397 0.9944 0.2256 0.102 Uiso 0.50 1 d PG B -3 Cl3 Cl 0.5033(8) 0.9334(2) 0.2481(6) 0.108(3) Uiso 0.50 1 d PG B -3 Cl4 Cl 0.4787(5) 1.0308(4) 0.1917(3) 0.113(3) Uiso 0.50 1 d PG B -3 Cl5 Cl 0.5052(5) 1.0391(4) 0.2870(3) 0.132(4) Uiso 0.50 1 d PG B -3 C72 C 0.1601(2) 0.29107(18) 0.16002(17) 0.166(13) Uani 1 1 d G . . H72 H 0.1497 0.3279 0.1469 0.199 Uiso 1 1 d G . . Cl6 Cl 0.1864(2) 0.2934(3) 0.22089(18) 0.152(3) Uani 1 1 d G . . Cl7 Cl 0.1069(2) 0.2472(3) 0.1334(2) 0.212(5) Uani 1 1 d G . . Cl8 Cl 0.2059(3) 0.2661(3) 0.1494(3) 0.187(4) Uani 1 1 d G . . C73 C 0.9090(2) 0.1610(2) 0.0057(2) 0.27(3) Uani 1 1 d G . . H73 H 0.8776 0.1785 -0.0187 0.326 Uiso 1 1 d G . . Cl9 Cl 0.9591(3) 0.2089(3) 0.0289(3) 0.164(3) Uani 1 1 d G . . Cl10 Cl 0.9013(3) 0.1376(3) 0.0507(3) 0.181(3) Uani 1 1 d G . . Cl11 Cl 0.9230(4) 0.1050(3) -0.0183(3) 0.192(4) Uani 1 1 d G . . C74 C 0.9452(3) 0.9063(3) -0.0211(3) 0.24(2) Uani 1 1 d G . . H74 H 0.9771 0.9194 -0.0165 0.284 Uiso 1 1 d G . . Cl12 Cl 0.9581(4) 0.8650(3) 0.0267(4) 0.210(5) Uani 1 1 d G . . Cl13 Cl 0.9080(5) 0.9630(3) -0.0253(3) 0.229(5) Uani 1 1 d G . . Cl14 Cl 0.9120(6) 0.8676(5) -0.0732(4) 0.349(11) Uani 1 1 d G . . C75 C 0.3825(3) 0.1521(3) 0.1490(2) 0.27(3) Uani 1 1 d G . . H75 H 0.3874 0.1206 0.1689 0.324 Uiso 1 1 d G . . Cl15 Cl 0.3209(2) 0.1788(5) 0.1251(4) 0.222(5) Uani 1 1 d G . . Cl16 Cl 0.4277(2) 0.2031(4) 0.18290(18) 0.180(4) Uani 1 1 d G . . Cl17 Cl 0.3900(5) 0.1314(6) 0.1034(4) 0.71(3) Uani 1 1 d G . . O7 O 0.9807(6) 0.2313(6) 0.1552(5) 0.067(5) Uiso 0.60(2) 1 d P C 4 O8 O 0.9634(6) 0.2000(6) 0.1765(5) 0.035(5) Uiso 0.40(2) 1 d P C 5 O9 O 0.0172(5) 0.8552(6) 0.1568(5) 0.049(3) Uiso 0.510(4) 1 d P D 6 O10 O 0.0369(6) 0.8491(7) 0.2134(5) 0.008(4) Uiso 0.239(15) 1 d P E 7 O11 O 0.0693(7) 0.8013(7) 0.2452(6) 0.017(5) Uiso 0.252(15) 1 d P F 8 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 0.0367(2) 0.0516(3) 0.0656(3) 0.01339(19) 0.01927(19) -0.00074(17) Ir2 0.0391(2) 0.0354(2) 0.0430(2) 0.00056(13) 0.01737(16) 0.00794(14) Cl1 0.0656(18) 0.0519(16) 0.0713(18) 0.0143(13) 0.0333(15) -0.0031(13) N1 0.037(3) 0.042(3) 0.062(4) 0.000(3) 0.017(3) -0.003(3) N2 0.044(3) 0.023(3) 0.051(4) 0.002(3) 0.023(3) 0.006(3) N3 0.039(3) 0.033(3) 0.048(4) -0.003(3) 0.015(3) 0.004(3) N4 0.045(4) 0.033(3) 0.053(4) -0.003(3) 0.024(3) 0.000(3) C1 0.038(3) 0.036(3) 0.054(4) 0.008(3) 0.021(3) -0.001(3) C2 0.041(3) 0.033(3) 0.050(4) 0.004(3) 0.022(3) 0.002(3) C3 0.040(3) 0.029(3) 0.048(4) -0.002(3) 0.018(3) 0.006(3) C4 0.040(3) 0.036(3) 0.049(4) 0.001(3) 0.023(3) -0.002(3) C5 0.050(4) 0.033(3) 0.065(5) 0.001(3) 0.025(4) -0.003(3) C6 0.062(5) 0.035(4) 0.086(6) 0.005(4) 0.029(5) 0.000(4) C7 0.068(5) 0.037(4) 0.107(7) 0.004(5) 0.026(5) -0.006(4) C8 0.063(5) 0.049(5) 0.125(7) 0.014(6) 0.020(6) -0.015(5) C9 0.051(5) 0.050(5) 0.109(7) 0.016(5) 0.019(5) -0.013(4) C10 0.047(4) 0.040(4) 0.074(5) 0.006(4) 0.019(4) -0.006(3) O1 0.036(3) 0.041(3) 0.062(4) 0.011(3) 0.021(3) 0.004(3) O2 0.042(3) 0.033(3) 0.060(4) -0.002(3) 0.011(3) 0.003(3) C11 0.058(4) 0.111(5) 0.086(4) 0.019(4) 0.025(3) 0.001(4) C12 0.055(4) 0.097(4) 0.078(4) 0.016(4) 0.022(3) 0.011(3) C13 0.054(4) 0.089(4) 0.076(4) 0.011(4) 0.022(3) 0.005(3) C14 0.060(4) 0.090(4) 0.083(4) 0.008(4) 0.019(3) -0.001(3) C15 0.058(4) 0.101(5) 0.089(4) 0.014(4) 0.020(3) -0.008(4) C16 0.065(5) 0.129(6) 0.093(6) 0.023(5) 0.031(4) 0.002(5) C17 0.069(5) 0.097(5) 0.080(6) 0.011(5) 0.015(5) 0.020(5) C18 0.059(5) 0.090(6) 0.075(5) 0.011(4) 0.024(4) 0.007(4) C19 0.071(5) 0.090(6) 0.084(6) 0.001(5) 0.017(4) 0.002(5) C20 0.065(5) 0.107(5) 0.100(6) 0.018(5) 0.014(5) -0.017(5) Ir3 0.0463(2) 0.0481(2) 0.0380(2) -0.00378(15) 0.01691(17) -0.00458(16) Ir4 0.0438(2) 0.03169(19) 0.0427(2) -0.00027(13) 0.01806(16) 0.00547(14) Cl2 0.0661(18) 0.0694(19) 0.0575(15) -0.0123(13) 0.0343(14) -0.0182(14) N5 0.036(4) 0.043(5) 0.052(5) -0.002(3) 0.018(4) 0.004(3) N6 0.044(4) 0.020(3) 0.044(4) -0.001(3) 0.019(3) 0.009(3) N7 0.039(4) 0.045(5) 0.048(4) -0.004(4) 0.017(4) 0.006(3) N8 0.049(5) 0.033(4) 0.059(5) -0.007(4) 0.024(4) 0.001(4) C21 0.042(5) 0.036(5) 0.038(4) 0.003(3) 0.017(4) -0.001(4) C22 0.049(5) 0.039(5) 0.038(4) 0.002(4) 0.022(4) 0.000(4) C23 0.036(5) 0.037(5) 0.043(5) -0.002(4) 0.014(4) 0.005(4) C24 0.040(5) 0.036(5) 0.050(5) 0.001(4) 0.021(4) 0.003(4) C25 0.045(6) 0.039(6) 0.075(7) -0.011(5) 0.028(5) -0.004(4) C26 0.059(7) 0.046(6) 0.084(9) -0.021(6) 0.032(7) -0.010(5) C27 0.063(8) 0.057(8) 0.115(12) -0.044(8) 0.035(8) -0.003(6) C28 0.071(8) 0.059(8) 0.097(10) -0.040(7) 0.048(8) -0.020(6) C29 0.051(6) 0.064(7) 0.054(6) -0.021(5) 0.022(5) -0.012(5) C30 0.065(7) 0.045(6) 0.053(6) -0.013(5) 0.026(5) -0.011(5) O3 0.046(4) 0.040(4) 0.045(4) -0.003(3) 0.018(3) 0.001(3) O4 0.042(4) 0.047(4) 0.054(4) -0.011(3) 0.014(3) 0.009(3) C31 0.055(5) 0.098(5) 0.050(4) 0.014(4) 0.020(4) -0.007(5) C32 0.055(5) 0.073(5) 0.064(5) 0.016(4) 0.026(4) 0.007(4) C33 0.049(4) 0.059(4) 0.057(4) 0.005(4) 0.023(4) 0.003(4) C34 0.044(4) 0.066(4) 0.061(4) -0.004(4) 0.026(4) -0.006(4) C35 0.052(5) 0.094(5) 0.050(4) -0.009(4) 0.019(4) -0.014(5) C36 0.066(7) 0.124(8) 0.057(6) 0.029(6) 0.020(5) -0.006(7) C37 0.066(6) 0.062(6) 0.096(7) 0.023(5) 0.032(6) 0.010(5) C38 0.064(6) 0.067(6) 0.065(6) 0.008(5) 0.036(5) 0.004(5) C39 0.060(6) 0.064(5) 0.089(7) -0.006(5) 0.031(6) -0.006(5) C40 0.059(6) 0.118(8) 0.054(5) -0.018(6) 0.021(5) -0.017(6) C51 0.056(6) 0.068(7) 0.034(5) -0.006(5) 0.013(4) 0.017(6) C52 0.066(7) 0.074(8) 0.039(5) 0.015(5) 0.030(5) 0.027(6) C53 0.041(5) 0.067(7) 0.048(5) 0.004(5) 0.023(5) 0.008(5) C54 0.056(6) 0.054(6) 0.050(5) 0.001(4) 0.030(5) 0.032(5) C55 0.058(7) 0.052(7) 0.067(7) -0.024(5) 0.031(6) 0.005(5) C56 0.047(6) 0.129(13) 0.039(5) -0.014(7) 0.012(5) 0.024(7) C57 0.076(9) 0.087(10) 0.068(8) 0.030(7) 0.046(7) 0.038(8) C58 0.059(7) 0.087(10) 0.063(7) 0.018(7) 0.033(6) 0.026(7) C59 0.052(6) 0.053(6) 0.065(7) 0.000(5) 0.028(6) 0.018(5) C60 0.074(9) 0.046(7) 0.103(11) -0.015(7) 0.034(8) 0.012(6) C61 0.054(6) 0.041(6) 0.078(8) -0.016(5) 0.034(6) -0.019(5) C62 0.078(8) 0.029(5) 0.075(8) -0.006(5) 0.040(7) 0.001(5) C63 0.072(8) 0.029(5) 0.091(9) 0.017(5) 0.048(7) 0.016(5) C64 0.070(7) 0.035(5) 0.057(6) 0.014(4) 0.032(6) 0.008(5) C65 0.064(7) 0.050(6) 0.062(7) 0.008(5) 0.036(6) -0.003(5) C66 0.061(7) 0.065(8) 0.074(8) -0.002(6) 0.036(6) -0.011(6) C67 0.123(13) 0.038(6) 0.093(10) -0.020(6) 0.064(10) -0.012(7) C68 0.086(11) 0.074(10) 0.122(14) 0.049(10) 0.046(10) 0.034(9) C69 0.072(8) 0.087(10) 0.049(6) 0.025(6) 0.017(6) -0.012(7) C70 0.081(9) 0.063(8) 0.074(8) -0.006(6) 0.055(7) -0.008(6) P1 0.0508(16) 0.0648(19) 0.0532(16) 0.0055(13) 0.0235(13) 0.0030(14) F1 0.076(5) 0.086(6) 0.074(5) -0.014(4) 0.009(4) 0.003(4) F2 0.124(8) 0.099(7) 0.137(9) 0.020(6) 0.102(8) 0.016(6) F3 0.099(8) 0.117(9) 0.130(10) -0.015(7) -0.002(7) -0.025(7) F4 0.130(8) 0.071(5) 0.092(6) 0.006(4) 0.077(6) 0.011(5) F5 0.116(7) 0.099(7) 0.072(5) 0.028(5) 0.054(5) 0.034(6) F6 0.111(7) 0.074(5) 0.104(6) 0.023(5) 0.073(6) 0.006(5) P2 0.130(3) 0.093(3) 0.097(3) 0.015(2) 0.073(3) 0.012(2) F7 0.153(6) 0.136(6) 0.110(6) 0.024(5) 0.067(5) -0.021(5) F8 0.144(7) 0.161(8) 0.098(5) 0.007(5) 0.065(5) -0.012(6) F9 0.134(6) 0.080(5) 0.113(6) 0.007(5) 0.068(5) 0.004(4) F10 0.125(6) 0.120(6) 0.104(5) 0.039(4) 0.061(4) 0.024(5) F11 0.142(6) 0.073(5) 0.138(6) 0.007(5) 0.048(6) 0.033(5) F12 0.147(7) 0.148(7) 0.151(7) -0.013(6) 0.085(6) 0.027(6) C72 0.082(13) 0.084(14) 0.23(3) 0.064(17) 0.021(16) 0.024(11) Cl6 0.132(5) 0.177(7) 0.123(5) 0.003(4) 0.053(4) -0.036(5) Cl7 0.130(5) 0.101(4) 0.201(7) 0.032(5) -0.046(5) 0.001(4) Cl8 0.282(11) 0.119(5) 0.222(9) 0.074(5) 0.177(9) 0.078(6) C73 0.58(9) 0.12(2) 0.18(3) -0.06(2) 0.24(5) -0.17(4) Cl9 0.185(7) 0.152(6) 0.167(6) -0.012(5) 0.103(6) -0.036(5) Cl10 0.157(7) 0.159(7) 0.224(9) 0.026(6) 0.099(7) -0.030(5) Cl11 0.219(10) 0.141(6) 0.215(9) 0.004(6) 0.117(8) 0.042(6) C74 0.23(5) 0.21(4) 0.27(5) -0.01(4) 0.14(4) 0.09(3) Cl12 0.218(10) 0.138(7) 0.316(14) 0.075(8) 0.172(10) 0.057(6) Cl13 0.248(12) 0.157(8) 0.195(9) -0.001(7) 0.062(8) 0.050(8) Cl14 0.248(15) 0.34(2) 0.33(2) -0.160(17) 0.070(14) -0.034(15) C75 0.24(4) 0.30(5) 0.26(5) 0.22(4) 0.12(4) 0.12(4) Cl15 0.162(8) 0.230(11) 0.221(10) 0.079(9) 0.069(7) 0.011(7) Cl16 0.105(4) 0.332(13) 0.100(4) 0.058(6) 0.052(3) 0.046(6) Cl17 1.11(6) 0.96(5) 0.38(2) -0.53(3) 0.60(3) -0.92(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction 'CrystalStructure (Rigaku & RAC 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure (Rigaku & RAC 2007)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; 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 N1 2.119(9) . ? Ir1 C15 2.122(16) . ? Ir1 C12 2.140(14) . ? Ir1 C14 2.153(17) . ? Ir1 O1 2.155(7) . ? Ir1 C11 2.156(16) . ? Ir1 C13 2.173(15) . ? Ir1 Cl1 2.375(3) . ? Ir2 N2 2.121(7) . ? Ir2 N12A 2.128(5) . ? Ir2 C53 2.144(11) . ? Ir2 C54 2.151(9) . ? Ir2 C52 2.167(11) . ? Ir2 C51 2.173(10) . ? Ir2 C55 2.179(10) . ? Ir2 O5 2.224(7) . ? Ir2 N11A 2.248(6) . ? Ir2 N9 2.284(5) . ? Ir2 C44A 2.504(5) . ? N1 C1 1.345(13) . ? N1 C10 1.361(14) . ? N2 C2 1.341(13) . ? N2 C3 1.391(12) . ? N3 C4 1.339(12) . ? N3 C3 1.381(12) . ? N4 C4 1.322(13) . ? N4 C5 1.338(13) . ? C1 C4 1.423(14) . ? C1 C2 1.446(13) . ? C2 O1 1.256(12) . ? C3 O2 1.228(12) . ? C5 C10 1.399(16) . ? C5 C6 1.439(15) . ? C6 C7 1.325(18) . ? C7 C8 1.43(2) . ? C8 C9 1.32(2) . ? C9 C10 1.438(16) . ? C11 C15 1.33(3) . ? C11 C12 1.43(2) . ? C11 C16 1.52(3) . ? C12 C13 1.41(2) . ? C12 C17 1.53(2) . ? C13 C14 1.45(2) . ? C13 C18 1.48(2) . ? C14 C15 1.47(3) . ? C14 C19 1.49(3) . ? C15 C20 1.56(3) . ? Ir3 N5 2.119(8) . ? Ir3 C32 2.146(13) . ? Ir3 C31 2.150(13) . ? Ir3 C33 2.151(12) . ? Ir3 O3 2.154(7) . ? Ir3 C35 2.156(12) . ? Ir3 C34 2.157(12) . ? Ir3 Cl2 2.387(3) . ? Ir4 N11 2.135(6) . ? Ir4 C62 2.138(11) . ? Ir4 N6 2.140(7) . ? Ir4 C61 2.149(11) . ? Ir4 C63 2.155(10) . ? Ir4 C64 2.155(10) . ? Ir4 N12 2.157(6) . ? Ir4 C65 2.162(12) . ? Ir4 O5A 2.165(7) . ? Ir4 N9A 2.258(5) . ? Ir4 C44 2.456(5) . ? N5 C21 1.334(12) . ? N5 C30 1.349(14) . ? N6 C22 1.303(12) . ? N6 C23 1.388(12) . ? N7 C23 1.358(13) . ? N7 C24 1.375(13) . ? N8 C24 1.307(13) . ? N8 C25 1.361(14) . ? C21 C24 1.420(13) . ? C21 C22 1.460(14) . ? C22 O3 1.270(12) . ? C23 O4 1.235(12) . ? C25 C26 1.409(16) . ? C25 C30 1.458(17) . ? C26 C27 1.355(19) . ? C27 C28 1.44(2) . ? C28 C29 1.320(18) . ? C29 C30 1.425(15) . ? C31 C32 1.41(2) . ? C31 C35 1.45(2) . ? C31 C36 1.513(18) . ? C32 C33 1.452(18) . ? C32 C37 1.48(2) . ? C33 C34 1.420(18) . ? C33 C38 1.468(17) . ? C34 C35 1.473(18) . ? C34 C39 1.493(19) . ? C35 C40 1.46(2) . ? N9 C50 1.3498 . ? N9 C41 1.3631 . ? N10 C42 1.3608 . ? N10 C43 1.3657 . ? N11 C44 1.3261 . ? N11 C43 1.3732 . ? N12 C44 1.3365 . ? N12 C45 1.3411 . ? C41 C44 1.4161 . ? C41 C42 1.4568 . ? C42 O5 1.2323 . ? C43 O6 1.2542 . ? C45 C50 1.4136 . ? C45 C46 1.4435 . ? C46 C47 1.3705 . ? C47 C48 1.3688 . ? C48 C49 1.4022 . ? C49 C50 1.4303 . ? N9A C50A 1.3497 . ? N9A C41A 1.3626 . ? N10A C42A 1.3607 . ? N10A C43A 1.6173 . ? N11A C43A 1.2898 . ? N11A C44A 1.3259 . ? N12A C44A 1.3365 . ? N12A C45A 1.3415 . ? C41A C44A 1.4161 . ? C41A C42A 1.4568 . ? C42A O5A 1.2327 . ? C43A O6A 1.1902 . ? C45A C50A 1.4136 . ? C45A C46A 1.4435 . ? C46A C47A 1.3700 . ? C47A C48A 1.3694 . ? C48A C49A 1.4018 . ? C49A C50A 1.4303 . ? C51 C52 1.449(19) . ? C51 C56 1.458(15) . ? C51 C55 1.494(17) . ? C52 C53 1.435(15) . ? C52 C57 1.498(18) . ? C53 C54 1.441(17) . ? C53 C58 1.507(18) . ? C54 C55 1.392(17) . ? C54 C59 1.506(15) . ? C55 C60 1.438(19) . ? C61 C65 1.405(17) . ? C61 C62 1.462(17) . ? C61 C66 1.495(17) . ? C62 C63 1.415(19) . ? C62 C67 1.498(17) . ? C63 C64 1.452(17) . ? C63 C68 1.473(19) . ? C64 C69 1.440(17) . ? C64 C65 1.448(17) . ? C65 C70 1.468(18) . ? P1 F3 1.551(11) . ? P1 F6 1.573(9) . ? P1 F5 1.576(10) . ? P1 F4 1.590(9) . ? P1 F1 1.597(9) . ? P1 F2 1.619(10) . ? P2 F8 1.520(13) . ? P2 F11 1.523(12) . ? P2 F10 1.542(12) . ? P2 F12 1.558(14) . ? P2 F7 1.589(14) . ? P2 F9 1.594(13) . ? C71 Cl5 1.7699 . ? C71 Cl4 1.7701 . ? C71 Cl3 1.7702 . ? C72 Cl7 1.7699 . ? C72 Cl6 1.7699 . ? C72 Cl8 1.7704 . ? C73 Cl11 1.7699 . ? C73 Cl9 1.7700 . ? C73 Cl10 1.7700 . ? C74 Cl14 1.7700 . ? C74 Cl13 1.7701 . ? C74 Cl12 1.7702 . ? C75 Cl15 1.7699 . ? C75 Cl16 1.7700 . ? C75 Cl17 1.7700 . ? 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 N1 Ir1 C15 120.5(6) . . ? N1 Ir1 C12 155.7(5) . . ? C15 Ir1 C12 62.9(7) . . ? N1 Ir1 C14 101.1(5) . . ? C15 Ir1 C14 40.1(7) . . ? C12 Ir1 C14 65.4(7) . . ? N1 Ir1 O1 77.0(3) . . ? C15 Ir1 O1 159.2(5) . . ? C12 Ir1 O1 96.4(5) . . ? C14 Ir1 O1 131.1(5) . . ? N1 Ir1 C11 155.3(6) . . ? C15 Ir1 C11 36.1(7) . . ? C12 Ir1 C11 38.9(6) . . ? C14 Ir1 C11 65.2(7) . . ? O1 Ir1 C11 127.7(6) . . ? N1 Ir1 C13 118.9(5) . . ? C15 Ir1 C13 64.1(6) . . ? C12 Ir1 C13 38.2(6) . . ? C14 Ir1 C13 39.2(6) . . ? O1 Ir1 C13 98.4(5) . . ? C11 Ir1 C13 64.4(6) . . ? N1 Ir1 Cl1 84.0(3) . . ? C15 Ir1 Cl1 106.2(5) . . ? C12 Ir1 Cl1 119.1(5) . . ? C14 Ir1 Cl1 143.2(5) . . ? O1 Ir1 Cl1 85.7(2) . . ? C11 Ir1 Cl1 95.3(5) . . ? C13 Ir1 Cl1 157.1(4) . . ? N2 Ir2 N12A 90.0(3) . . ? N2 Ir2 C53 108.9(4) . . ? N12A Ir2 C53 161.0(4) . . ? N2 Ir2 C54 147.6(4) . . ? N12A Ir2 C54 122.0(4) . . ? C53 Ir2 C54 39.2(5) . . ? N2 Ir2 C52 93.2(4) . . ? N12A Ir2 C52 143.0(4) . . ? C53 Ir2 C52 38.9(4) . . ? C54 Ir2 C52 65.0(4) . . ? N2 Ir2 C51 113.7(4) . . ? N12A Ir2 C51 107.1(4) . . ? C53 Ir2 C51 65.4(5) . . ? C54 Ir2 C51 64.7(4) . . ? C52 Ir2 C51 39.0(5) . . ? N2 Ir2 C55 153.8(4) . . ? N12A Ir2 C55 97.4(4) . . ? C53 Ir2 C55 65.3(5) . . ? C54 Ir2 C55 37.5(5) . . ? C52 Ir2 C55 66.1(5) . . ? C51 Ir2 C55 40.1(5) . . ? N2 Ir2 O5 85.7(3) . . ? N12A Ir2 O5 81.68(19) . . ? C53 Ir2 O5 99.8(3) . . ? C54 Ir2 O5 93.6(4) . . ? C52 Ir2 O5 135.3(4) . . ? C51 Ir2 O5 158.1(4) . . ? C55 Ir2 O5 120.1(4) . . ? N2 Ir2 N11A 84.0(3) . . ? N12A Ir2 N11A 64.04(13) . . ? C53 Ir2 N11A 117.1(3) . . ? C54 Ir2 N11A 104.5(3) . . ? C52 Ir2 N11A 152.9(4) . . ? C51 Ir2 N11A 160.9(4) . . ? C55 Ir2 N11A 121.8(4) . . ? O5 Ir2 N11A 17.78(18) . . ? N2 Ir2 N9 86.7(3) . . ? N12A Ir2 N9 9.4(2) . . ? C53 Ir2 N9 162.4(4) . . ? C54 Ir2 N9 124.0(4) . . ? C52 Ir2 N9 151.9(4) . . ? C51 Ir2 N9 116.5(4) . . ? C55 Ir2 N9 104.1(4) . . ? O5 Ir2 N9 72.70(15) . . ? N11A Ir2 N9 54.97(19) . . ? N2 Ir2 C44A 87.8(3) . . ? N12A Ir2 C44A 32.26(7) . . ? C53 Ir2 C44A 144.8(3) . . ? C54 Ir2 C44A 116.0(3) . . ? C52 Ir2 C44A 175.2(4) . . ? C51 Ir2 C44A 136.5(4) . . ? C55 Ir2 C44A 111.6(4) . . ? O5 Ir2 C44A 49.42(17) . . ? N11A Ir2 C44A 31.83(7) . . ? N9 Ir2 C44A 23.42(18) . . ? C1 N1 C10 114.4(9) . . ? C1 N1 Ir1 112.4(7) . . ? C10 N1 Ir1 133.1(7) . . ? C2 N2 C3 120.1(8) . . ? C2 N2 Ir2 120.6(6) . . ? C3 N2 Ir2 118.9(6) . . ? C4 N3 C3 124.5(9) . . ? C4 N4 C5 116.4(9) . . ? N1 C1 C4 122.3(9) . . ? N1 C1 C2 118.1(9) . . ? C4 C1 C2 119.5(9) . . ? O1 C2 N2 122.7(9) . . ? O1 C2 C1 117.3(9) . . ? N2 C2 C1 120.0(9) . . ? O2 C3 N3 120.8(9) . . ? O2 C3 N2 120.3(8) . . ? N3 C3 N2 118.9(8) . . ? N4 C4 N3 121.6(9) . . ? N4 C4 C1 122.0(9) . . ? N3 C4 C1 116.5(9) . . ? N4 C5 C10 122.0(10) . . ? N4 C5 C6 118.9(10) . . ? C10 C5 C6 118.9(10) . . ? C7 C6 C5 121.1(13) . . ? C6 C7 C8 120.0(13) . . ? C9 C8 C7 120.1(13) . . ? C8 C9 C10 122.0(14) . . ? N1 C10 C5 122.5(10) . . ? N1 C10 C9 120.0(11) . . ? C5 C10 C9 117.5(11) . . ? C2 O1 Ir1 115.0(6) . . ? C15 C11 C12 107.6(18) . . ? C15 C11 C16 127.8(18) . . ? C12 C11 C16 124.5(18) . . ? C15 C11 Ir1 70.6(10) . . ? C12 C11 Ir1 69.9(9) . . ? C16 C11 Ir1 125.1(12) . . ? C13 C12 C11 108.5(17) . . ? C13 C12 C17 122.7(16) . . ? C11 C12 C17 128.8(17) . . ? C13 C12 Ir1 72.2(9) . . ? C11 C12 Ir1 71.1(9) . . ? C17 C12 Ir1 124.1(11) . . ? C12 C13 C14 108.4(15) . . ? C12 C13 C18 125.8(16) . . ? C14 C13 C18 125.8(16) . . ? C12 C13 Ir1 69.6(9) . . ? C14 C13 Ir1 69.7(9) . . ? C18 C13 Ir1 127.5(10) . . ? C13 C14 C15 102.9(16) . . ? C13 C14 C19 121.8(16) . . ? C15 C14 C19 135.0(17) . . ? C13 C14 Ir1 71.2(9) . . ? C15 C14 Ir1 68.8(10) . . ? C19 C14 Ir1 127.8(11) . . ? C11 C15 C14 112.5(17) . . ? C11 C15 C20 126.1(19) . . ? C14 C15 C20 121.2(19) . . ? C11 C15 Ir1 73.3(11) . . ? C14 C15 Ir1 71.0(9) . . ? C20 C15 Ir1 127.0(11) . . ? N5 Ir3 C32 156.8(4) . . ? N5 Ir3 C31 157.4(5) . . ? C32 Ir3 C31 38.4(5) . . ? N5 Ir3 C33 119.3(4) . . ? C32 Ir3 C33 39.5(5) . . ? C31 Ir3 C33 65.0(5) . . ? N5 Ir3 O3 76.8(3) . . ? C32 Ir3 O3 94.9(4) . . ? C31 Ir3 O3 125.7(5) . . ? C33 Ir3 O3 97.6(4) . . ? N5 Ir3 C35 119.5(5) . . ? C32 Ir3 C35 66.0(6) . . ? C31 Ir3 C35 39.3(6) . . ? C33 Ir3 C35 66.0(5) . . ? O3 Ir3 C35 160.7(5) . . ? N5 Ir3 C34 103.3(4) . . ? C32 Ir3 C34 65.6(5) . . ? C31 Ir3 C34 65.4(5) . . ? C33 Ir3 C34 38.5(5) . . ? O3 Ir3 C34 130.7(4) . . ? C35 Ir3 C34 39.9(5) . . ? N5 Ir3 Cl2 81.3(3) . . ? C32 Ir3 Cl2 120.2(4) . . ? C31 Ir3 Cl2 96.6(4) . . ? C33 Ir3 Cl2 159.5(3) . . ? O3 Ir3 Cl2 85.7(2) . . ? C35 Ir3 Cl2 106.1(4) . . ? C34 Ir3 Cl2 143.6(3) . . ? N11 Ir4 C62 119.2(4) . . ? N11 Ir4 N6 88.1(3) . . ? C62 Ir4 N6 152.1(4) . . ? N11 Ir4 C61 158.3(4) . . ? C62 Ir4 C61 39.9(5) . . ? N6 Ir4 C61 112.3(4) . . ? N11 Ir4 C63 100.9(4) . . ? C62 Ir4 C63 38.5(5) . . ? N6 Ir4 C63 148.2(4) . . ? C61 Ir4 C63 65.7(5) . . ? N11 Ir4 C64 115.9(4) . . ? C62 Ir4 C64 65.3(5) . . ? N6 Ir4 C64 109.4(4) . . ? C61 Ir4 C64 65.3(5) . . ? C63 Ir4 C64 39.4(5) . . ? N11 Ir4 N12 65.51(13) . . ? C62 Ir4 N12 99.4(4) . . ? N6 Ir4 N12 86.7(3) . . ? C61 Ir4 N12 107.0(4) . . ? C63 Ir4 N12 124.9(4) . . ? C64 Ir4 N12 163.8(4) . . ? N11 Ir4 C65 153.4(4) . . ? C62 Ir4 C65 65.1(5) . . ? N6 Ir4 C65 93.2(4) . . ? C61 Ir4 C65 38.1(5) . . ? C63 Ir4 C65 65.5(5) . . ? C64 Ir4 C65 39.2(5) . . ? N12 Ir4 C65 141.1(4) . . ? N11 Ir4 O5A 19.81(18) . . ? C62 Ir4 O5A 120.1(5) . . ? N6 Ir4 O5A 87.4(3) . . ? C61 Ir4 O5A 156.9(4) . . ? C63 Ir4 O5A 91.2(4) . . ? C64 Ir4 O5A 97.6(4) . . ? N12 Ir4 O5A 85.24(18) . . ? C65 Ir4 O5A 133.7(4) . . ? N11 Ir4 N9A 54.49(19) . . ? C62 Ir4 N9A 100.8(4) . . ? N6 Ir4 N9A 90.6(3) . . ? C61 Ir4 N9A 115.6(4) . . ? C63 Ir4 N9A 119.5(4) . . ? C64 Ir4 N9A 158.3(4) . . ? N12 Ir4 N9A 11.8(2) . . ? C65 Ir4 N9A 151.9(4) . . ? O5A Ir4 N9A 74.30(16) . . ? N11 Ir4 C44 32.63(7) . . ? C62 Ir4 C44 112.7(4) . . ? N6 Ir4 C44 87.1(3) . . ? C61 Ir4 C44 136.6(4) . . ? C63 Ir4 C44 116.7(4) . . ? C64 Ir4 C44 146.0(4) . . ? N12 Ir4 C44 32.88(7) . . ? C65 Ir4 C44 173.9(4) . . ? O5A Ir4 C44 52.39(17) . . ? N9A Ir4 C44 22.08(18) . . ? C21 N5 C30 116.6(9) . . ? C21 N5 Ir3 113.0(6) . . ? C30 N5 Ir3 130.1(7) . . ? C22 N6 C23 120.6(8) . . ? C22 N6 Ir4 121.2(6) . . ? C23 N6 Ir4 117.6(6) . . ? C23 N7 C24 124.1(8) . . ? C24 N8 C25 115.4(9) . . ? N5 C21 C24 122.3(9) . . ? N5 C21 C22 118.6(8) . . ? C24 C21 C22 119.0(9) . . ? O3 C22 N6 123.3(9) . . ? O3 C22 C21 115.9(8) . . ? N6 C22 C21 120.7(9) . . ? O4 C23 N7 118.6(9) . . ? O4 C23 N6 121.8(8) . . ? N7 C23 N6 119.6(8) . . ? N8 C24 N7 120.8(9) . . ? N8 C24 C21 123.5(9) . . ? N7 C24 C21 115.7(9) . . ? N8 C25 C26 118.5(11) . . ? N8 C25 C30 122.0(10) . . ? C26 C25 C30 119.4(11) . . ? C27 C26 C25 120.6(13) . . ? C26 C27 C28 119.2(12) . . ? C29 C28 C27 122.3(12) . . ? C28 C29 C30 120.6(13) . . ? N5 C30 C29 122.4(11) . . ? N5 C30 C25 120.0(10) . . ? C29 C30 C25 117.6(11) . . ? C22 O3 Ir3 115.7(6) . . ? C32 C31 C35 110.0(12) . . ? C32 C31 C36 127.7(15) . . ? C35 C31 C36 122.2(14) . . ? C32 C31 Ir3 70.6(7) . . ? C35 C31 Ir3 70.6(7) . . ? C36 C31 Ir3 124.7(10) . . ? C31 C32 C33 107.5(13) . . ? C31 C32 C37 127.0(13) . . ? C33 C32 C37 125.4(13) . . ? C31 C32 Ir3 70.9(8) . . ? C33 C32 Ir3 70.4(7) . . ? C37 C32 Ir3 126.9(10) . . ? C34 C33 C32 108.4(11) . . ? C34 C33 C38 125.3(12) . . ? C32 C33 C38 126.1(12) . . ? C34 C33 Ir3 71.0(7) . . ? C32 C33 Ir3 70.1(7) . . ? C38 C33 Ir3 128.1(9) . . ? C33 C34 C35 108.4(12) . . ? C33 C34 C39 123.6(12) . . ? C35 C34 C39 127.8(13) . . ? C33 C34 Ir3 70.5(7) . . ? C35 C34 Ir3 70.0(7) . . ? C39 C34 Ir3 128.6(9) . . ? C31 C35 C40 127.5(14) . . ? C31 C35 C34 105.6(12) . . ? C40 C35 C34 125.5(14) . . ? C31 C35 Ir3 70.1(7) . . ? C40 C35 Ir3 134.4(10) . . ? C34 C35 Ir3 70.1(7) . . ? C50 N9 C41 113.8 . . ? C50 N9 Ir2 133.39(19) . . ? C41 N9 Ir2 112.29(18) . . ? C42 N10 C43 119.9 . . ? C44 N11 C43 123.8 . . ? C44 N11 Ir4 87.10(18) . . ? C43 N11 Ir4 148.54(19) . . ? C44 N12 C45 116.8 . . ? C44 N12 Ir4 85.93(18) . . ? C45 N12 Ir4 156.61(19) . . ? N9 C41 C44 123.1 . . ? N9 C41 C42 117.6 . . ? C44 C41 C42 119.3 . . ? O5 C42 N10 123.1 . . ? O5 C42 C41 118.1 . . ? N10 C42 C41 118.7 . . ? O6 C43 N10 120.3 . . ? O6 C43 N11 119.4 . . ? N10 C43 N11 120.2 . . ? N11 C44 N12 121.5 . . ? N11 C44 C41 117.3 . . ? N12 C44 C41 121.2 . . ? N11 C44 Ir4 60.27(17) . . ? N12 C44 Ir4 61.19(17) . . ? C41 C44 Ir4 177.1(2) . . ? N12 C45 C50 121.5 . . ? N12 C45 C46 117.8 . . ? C50 C45 C46 120.6 . . ? C47 C46 C45 118.7 . . ? C48 C47 C46 120.1 . . ? C47 C48 C49 123.6 . . ? C48 C49 C50 117.1 . . ? N9 C50 C45 123.0 . . ? N9 C50 C49 118.1 . . ? C45 C50 C49 118.9 . . ? C42 O5 Ir2 118.92(15) . . ? C50A N9A C41A 113.8 . . ? C50A N9A Ir4 134.87(19) . . ? C41A N9A Ir4 111.04(19) . . ? C42A N10A C43A 115.9 . . ? C43A N11A C44A 127.6 . . ? C43A N11A Ir2 138.8(2) . . ? C44A N11A Ir2 84.79(18) . . ? C44A N12A C45A 116.8 . . ? C44A N12A Ir2 89.53(19) . . ? C45A N12A Ir2 153.62(19) . . ? N9A C41A C44A 123.1 . . ? N9A C41A C42A 117.6 . . ? C44A C41A C42A 119.3 . . ? O5A C42A N10A 123.1 . . ? O5A C42A C41A 118.1 . . ? N10A C42A C41A 118.7 . . ? O6A C43A N11A 128.9 . . ? O6A C43A N10A 116.3 . . ? N11A C43A N10A 109.0 . . ? N11A C44A N12A 121.4 . . ? N11A C44A C41A 117.3 . . ? N12A C44A C41A 121.2 . . ? N11A C44A Ir2 63.39(18) . . ? N12A C44A Ir2 58.21(18) . . ? C41A C44A Ir2 177.3(3) . . ? N12A C45A C50A 121.5 . . ? N12A C45A C46A 117.8 . . ? C50A C45A C46A 120.6 . . ? C47A C46A C45A 118.7 . . ? C48A C47A C46A 120.1 . . ? C47A C48A C49A 123.6 . . ? C48A C49A C50A 117.1 . . ? N9A C50A C45A 123.0 . . ? N9A C50A C49A 118.1 . . ? C45A C50A C49A 118.9 . . ? C42A O5A Ir4 118.81(14) . . ? C52 C51 C56 127.1(12) . . ? C52 C51 C55 107.2(10) . . ? C56 C51 C55 125.3(13) . . ? C52 C51 Ir2 70.3(6) . . ? C56 C51 Ir2 130.5(9) . . ? C55 C51 Ir2 70.2(6) . . ? C53 C52 C51 107.9(10) . . ? C53 C52 C57 127.1(13) . . ? C51 C52 C57 125.0(11) . . ? C53 C52 Ir2 69.7(6) . . ? C51 C52 Ir2 70.7(6) . . ? C57 C52 Ir2 124.4(8) . . ? C52 C53 C54 107.5(10) . . ? C52 C53 C58 126.5(11) . . ? C54 C53 C58 125.6(10) . . ? C52 C53 Ir2 71.4(6) . . ? C54 C53 Ir2 70.6(6) . . ? C58 C53 Ir2 128.4(8) . . ? C55 C54 C53 110.8(10) . . ? C55 C54 C59 127.0(12) . . ? C53 C54 C59 122.2(11) . . ? C55 C54 Ir2 72.4(6) . . ? C53 C54 Ir2 70.1(6) . . ? C59 C54 Ir2 122.8(7) . . ? C54 C55 C60 128.9(12) . . ? C54 C55 C51 106.6(11) . . ? C60 C55 C51 124.5(12) . . ? C54 C55 Ir2 70.1(6) . . ? C60 C55 Ir2 127.2(10) . . ? C51 C55 Ir2 69.7(6) . . ? C65 C61 C62 107.5(11) . . ? C65 C61 C66 125.2(12) . . ? C62 C61 C66 127.0(11) . . ? C65 C61 Ir4 71.5(6) . . ? C62 C61 Ir4 69.7(6) . . ? C66 C61 Ir4 129.0(9) . . ? C63 C62 C61 108.5(10) . . ? C63 C62 C67 126.5(13) . . ? C61 C62 C67 124.9(13) . . ? C63 C62 Ir4 71.4(6) . . ? C61 C62 Ir4 70.5(6) . . ? C67 C62 Ir4 126.5(10) . . ? C62 C63 C64 107.8(10) . . ? C62 C63 C68 127.3(14) . . ? C64 C63 C68 124.8(14) . . ? C62 C63 Ir4 70.1(6) . . ? C64 C63 Ir4 70.3(6) . . ? C68 C63 Ir4 128.8(10) . . ? C69 C64 C65 128.5(12) . . ? C69 C64 C63 124.1(12) . . ? C65 C64 C63 107.2(11) . . ? C69 C64 Ir4 128.1(9) . . ? C65 C64 Ir4 70.6(6) . . ? C63 C64 Ir4 70.3(6) . . ? C61 C65 C64 109.0(11) . . ? C61 C65 C70 125.5(12) . . ? C64 C65 C70 125.5(12) . . ? C61 C65 Ir4 70.5(7) . . ? C64 C65 Ir4 70.2(6) . . ? C70 C65 Ir4 124.5(8) . . ? F3 P1 F6 90.9(7) . . ? F3 P1 F5 90.5(7) . . ? F6 P1 F5 178.6(7) . . ? F3 P1 F4 91.5(8) . . ? F6 P1 F4 89.6(5) . . ? F5 P1 F4 90.6(5) . . ? F3 P1 F1 178.1(7) . . ? F6 P1 F1 90.5(6) . . ? F5 P1 F1 88.1(6) . . ? F4 P1 F1 90.0(6) . . ? F3 P1 F2 91.9(8) . . ? F6 P1 F2 91.2(5) . . ? F5 P1 F2 88.5(5) . . ? F4 P1 F2 176.6(6) . . ? F1 P1 F2 86.7(6) . . ? F8 P2 F11 95.3(8) . . ? F8 P2 F10 170.8(9) . . ? F11 P2 F10 92.9(7) . . ? F8 P2 F12 84.4(8) . . ? F11 P2 F12 175.7(9) . . ? F10 P2 F12 87.8(8) . . ? F8 P2 F7 95.9(7) . . ? F11 P2 F7 88.0(8) . . ? F10 P2 F7 88.8(7) . . ? F12 P2 F7 87.8(9) . . ? F8 P2 F9 87.4(7) . . ? F11 P2 F9 90.6(7) . . ? F10 P2 F9 88.1(7) . . ? F12 P2 F9 93.6(8) . . ? F7 P2 F9 176.5(7) . . ? Cl5 C71 Cl4 109.4 . . ? Cl5 C71 Cl3 109.5 . . ? Cl4 C71 Cl3 109.5 . . ? Cl7 C72 Cl6 109.5 . . ? Cl7 C72 Cl8 109.4 . . ? Cl6 C72 Cl8 109.5 . . ? Cl11 C73 Cl9 109.5 . . ? Cl11 C73 Cl10 109.4 . . ? Cl9 C73 Cl10 109.5 . . ? Cl14 C74 Cl13 109.4 . . ? Cl14 C74 Cl12 109.5 . . ? Cl13 C74 Cl12 109.5 . . ? Cl15 C75 Cl16 109.5 . . ? Cl15 C75 Cl17 109.5 . . ? Cl16 C75 Cl17 109.4 . . ? #===END======================================================================== # Attachment '729384.cif' # VALIDATION REPLY FORM _verf_PLAT201_ALERT_2_A ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 16 RESPONSE: Disordered atoms heavily superimposed, see _publ_section_ exptl_refinement. ; _verf_PLAT242_ALERT_2_A ; PROBLEM: Check Low Ueq as Compared to Neighbors for C71 RESPONSE: No significant differences found, see _atom_site_U_iso_ or_equiv ; _verf_PLAT431_ALERT_2_A ; PROBLEM: Short Inter HL..A Contact Cl8 .. Cl21 .. 2.49 Ang. RESPONSE: Disordered atoms belonging to different groups in the same assembly, see _atom_site_disorder_assembly and _atom_site_ disorder_group ; _verf_PLAT601_ALERT_2_A ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . . 1372.00 A**3 RESPONSE: Other solvent molecules not located in the final d-Fourier map. ; #============================================================================== data_PROCESS _database_code_depnum_ccdc_archive 'CCDC 729384' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C73.5 H77.5 Cl14.5 Ir4 N12 O14 ' _chemical_formula_moiety 'C70 H74 Cl2 Ir4 N12 O6, 3.5(C H Cl3), 2(Cl O4) ' _chemical_formula_weight 2635.94 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' #------------------------------------------------------------------------------ _cell_length_a 27.1659(9) _cell_length_b 27.1659(9) _cell_length_c 60.5418(11) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 44679(2) _cell_formula_units_Z 16 _cell_measurement_reflns_used 68910 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 25.4 _cell_measurement_temperature 123.15 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20304.00 _exptl_absorpt_coefficient_mu 5.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.597 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type SATURN _diffrn_reflns_number 133871 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_max 25.35 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -72 _diffrn_reflns_limit_l_max 72 _diffrn_ambient_temperature 123.15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 20165 _reflns_number_gt 13925 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1078 _refine_ls_wR_factor_ref 0.3517 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 20165 _refine_ls_number_parameters 852 _refine_ls_goodness_of_fit_ref 1.346 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 5.21 _refine_diff_density_min -3.10 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.28941(3) 0.11097(3) 0.205746(11) 0.0798(3) Uani 1 1 d U . . Cl1 Cl 0.30814(19) 0.1388(2) 0.24219(7) 0.0934(14) Uani 1 1 d U . . Ir2 Ir 0.33161(3) 0.29792(3) 0.184775(12) 0.0779(3) Uani 1 1 d U . . O1 O 0.3108(4) 0.1830(4) 0.19591(19) 0.076(2) Uani 1 1 d U . . O2 O 0.4436(4) 0.2781(4) 0.18011(18) 0.073(2) Uani 1 1 d U . . N1 N 0.3665(5) 0.1041(5) 0.2021(2) 0.072(2) Uani 1 1 d U . . N2 N 0.3734(5) 0.2339(5) 0.1851(2) 0.067(2) Uani 1 1 d U A . N3 N 0.4559(5) 0.1979(5) 0.1845(2) 0.070(2) Uani 1 1 d U . . H3N H 0.4867 0.2010 0.1815 0.084 Uiso 1 1 calc R . . N4 N 0.4694(5) 0.1148(5) 0.1926(2) 0.074(3) Uani 1 1 d U . . C1 C 0.3887(6) 0.1473(6) 0.1943(3) 0.068(2) Uani 1 1 d U . . C2 C 0.3551(6) 0.1912(6) 0.1907(2) 0.067(2) Uani 1 1 d U . . C3 C 0.4263(6) 0.2397(6) 0.1832(3) 0.071(2) Uani 1 1 d U . . C4 C 0.4388(6) 0.1519(6) 0.1902(3) 0.070(2) Uani 1 1 d U . . C5 C 0.4494(4) 0.0728(3) 0.2016(2) 0.081(3) Uani 1 1 d GU . . C6 C 0.4813(4) 0.0341(4) 0.2063(2) 0.094(3) Uani 1 1 d GU . . H6 H 0.5147 0.0372 0.2032 0.113 Uiso 1 1 calc R . . C7 C 0.4633(5) -0.0092(4) 0.2154(2) 0.098(4) Uani 1 1 d GU . . H7 H 0.4846 -0.0350 0.2185 0.118 Uiso 1 1 calc R . . C8 C 0.4133(5) -0.0138(3) 0.2200(2) 0.100(4) Uani 1 1 d GU . . H8 H 0.4013 -0.0428 0.2261 0.120 Uiso 1 1 calc R . . C9 C 0.3814(4) 0.0248(4) 0.2154(2) 0.091(3) Uani 1 1 d GU . . H9 H 0.3480 0.0217 0.2184 0.109 Uiso 1 1 calc R . . C10 C 0.3995(4) 0.0681(4) 0.2062(2) 0.080(3) Uani 1 1 d GU . . C11 C 0.2174(5) 0.0817(5) 0.21536(19) 0.103(3) Uani 1 1 d GDU . . C12 C 0.2481(5) 0.0414(5) 0.2078(2) 0.100(3) Uani 1 1 d GDU . . C13 C 0.2624(5) 0.0515(5) 0.1852(2) 0.100(3) Uani 1 1 d GDU . . C14 C 0.2406(5) 0.0981(5) 0.17874(18) 0.097(3) Uani 1 1 d GDU . . C15 C 0.2127(5) 0.1168(5) 0.1974(2) 0.099(3) Uani 1 1 d GDU . . C16 C 0.1927(8) 0.0895(9) 0.2374(2) 0.106(4) Uani 1 1 d DU . . H16A H 0.2155 0.0821 0.2490 0.127 Uiso 1 1 calc R . . H16B H 0.1646 0.0682 0.2385 0.127 Uiso 1 1 calc R . . H16C H 0.1823 0.1232 0.2386 0.127 Uiso 1 1 calc R . . C17 C 0.2597(8) -0.0044(6) 0.2211(3) 0.107(4) Uani 1 1 d DU . . H17A H 0.2807 -0.0256 0.2126 0.129 Uiso 1 1 calc R . . H17B H 0.2297 -0.0214 0.2246 0.129 Uiso 1 1 calc R . . H17C H 0.2762 0.0048 0.2345 0.129 Uiso 1 1 calc R . . C18 C 0.2918(7) 0.0165(7) 0.1711(3) 0.111(4) Uani 1 1 d DU . . H18A H 0.3252 0.0155 0.1762 0.133 Uiso 1 1 calc R . . H18B H 0.2913 0.0275 0.1560 0.133 Uiso 1 1 calc R . . H18C H 0.2777 -0.0158 0.1720 0.133 Uiso 1 1 calc R . . C19 C 0.2448(8) 0.1236(8) 0.1567(2) 0.103(4) Uani 1 1 d DU . . H19A H 0.2272 0.1542 0.1571 0.123 Uiso 1 1 calc R . . H19B H 0.2311 0.1030 0.1454 0.123 Uiso 1 1 calc R . . H19C H 0.2789 0.1298 0.1535 0.123 Uiso 1 1 calc R . . C20 C 0.1803(7) 0.1617(6) 0.1987(4) 0.109(4) Uani 1 1 d DU . . H20A H 0.1982 0.1899 0.1934 0.131 Uiso 1 1 calc R . . H20B H 0.1705 0.1671 0.2137 0.131 Uiso 1 1 calc R . . H20C H 0.1516 0.1568 0.1897 0.131 Uiso 1 1 calc R . . Ir3 Ir 0.29764(2) 0.09699(3) 0.057383(11) 0.0754(3) Uani 1 1 d U . . Cl2 Cl 0.3149(3) 0.1137(3) 0.01951(8) 0.118(2) Uani 1 1 d U . . Ir4 Ir 0.33205(2) 0.29167(3) 0.070026(12) 0.0683(2) Uani 1 1 d U . . O3 O 0.3144(4) 0.1727(4) 0.06390(17) 0.068(2) Uani 1 1 d U . . O4 O 0.4439(4) 0.2760(4) 0.0759(2) 0.072(2) Uani 1 1 d U . . N5 N 0.3753(5) 0.0980(5) 0.06059(19) 0.065(2) Uani 1 1 d U . . N6 N 0.3767(4) 0.2277(5) 0.0720(2) 0.061(2) Uani 1 1 d U . . N7 N 0.4586(5) 0.1951(5) 0.0737(2) 0.065(2) Uani 1 1 d U . . H7N H 0.4891 0.1999 0.0769 0.078 Uiso 1 1 calc R . . N8 N 0.4778(5) 0.1121(5) 0.0673(2) 0.072(2) Uani 1 1 d U . . C21 C 0.3939(5) 0.1406(6) 0.0663(2) 0.060(2) Uani 1 1 d U . . C22 C 0.3596(5) 0.1818(6) 0.0678(2) 0.061(2) Uani 1 1 d U . . C23 C 0.4273(5) 0.2354(6) 0.0741(3) 0.064(2) Uani 1 1 d U . . C24 C 0.4439(5) 0.1473(6) 0.0686(2) 0.063(2) Uani 1 1 d U . . C25 C 0.4573(4) 0.0663(3) 0.0621(2) 0.082(3) Uani 1 1 d GU . . C26 C 0.4905(3) 0.0279(4) 0.0595(2) 0.093(3) Uani 1 1 d GU . . H26 H 0.5235 0.0323 0.0631 0.112 Uiso 1 1 calc R . . C27 C 0.4745(4) -0.0173(4) 0.0514(2) 0.098(4) Uani 1 1 d GU . . H27 H 0.4968 -0.0430 0.0496 0.117 Uiso 1 1 calc R . . C28 C 0.4253(5) -0.0240(3) 0.0459(2) 0.096(4) Uani 1 1 d GU . . H28 H 0.4146 -0.0542 0.0405 0.115 Uiso 1 1 calc R . . C29 C 0.3920(3) 0.0145(4) 0.0486(2) 0.087(3) Uani 1 1 d GU . . H29 H 0.3591 0.0100 0.0449 0.104 Uiso 1 1 calc R . . C30 C 0.4080(4) 0.0596(4) 0.0566(2) 0.078(3) Uani 1 1 d GU . . C31 C 0.2395(5) 0.0442(5) 0.0521(2) 0.094(3) Uani 1 1 d GDU . . C32 C 0.2698(5) 0.0240(5) 0.0689(2) 0.096(3) Uani 1 1 d GDU . . C33 C 0.2700(5) 0.0571(6) 0.0870(2) 0.096(3) Uani 1 1 d GDU . . C34 C 0.2398(5) 0.0979(5) 0.0814(2) 0.093(3) Uani 1 1 d GDU . . C35 C 0.2210(5) 0.0899(5) 0.0598(2) 0.095(3) Uani 1 1 d GDU . . C36 C 0.2271(7) 0.0240(8) 0.0295(3) 0.096(4) Uani 1 1 d DU . . H36A H 0.2146 0.0499 0.0204 0.116 Uiso 1 1 calc R . . H36B H 0.2027 -0.0014 0.0310 0.116 Uiso 1 1 calc R . . H36C H 0.2563 0.0104 0.0229 0.116 Uiso 1 1 calc R . . C37 C 0.2884(8) -0.0284(5) 0.0697(4) 0.107(4) Uani 1 1 d DU . . H37A H 0.2928 -0.0382 0.0848 0.128 Uiso 1 1 calc R . . H37B H 0.3193 -0.0305 0.0621 0.128 Uiso 1 1 calc R . . H37C H 0.2649 -0.0498 0.0628 0.128 Uiso 1 1 calc R . . C38 C 0.3011(7) 0.0473(9) 0.1072(3) 0.107(4) Uani 1 1 d DU . . H38A H 0.3348 0.0428 0.1028 0.129 Uiso 1 1 calc R . . H38B H 0.2895 0.0181 0.1144 0.129 Uiso 1 1 calc R . . H38C H 0.2988 0.0747 0.1171 0.129 Uiso 1 1 calc R . . C39 C 0.2357(9) 0.1341(8) 0.1002(3) 0.111(4) Uani 1 1 d DU . . H39A H 0.2384 0.1670 0.0946 0.133 Uiso 1 1 calc R . . H39B H 0.2616 0.1282 0.1106 0.133 Uiso 1 1 calc R . . H39C H 0.2044 0.1301 0.1074 0.133 Uiso 1 1 calc R . . C40 C 0.1881(7) 0.1256(7) 0.0477(4) 0.107(4) Uani 1 1 d DU . . H40A H 0.1888 0.1569 0.0550 0.129 Uiso 1 1 calc R . . H40B H 0.1550 0.1132 0.0475 0.129 Uiso 1 1 calc R . . H40C H 0.1996 0.1294 0.0328 0.129 Uiso 1 1 calc R . . N9 N 0.3546(4) 0.3059(5) 0.14951(14) 0.052(5) Uiso 0.435(14) 1 d PGU A 1 N10 N 0.2429(4) 0.2444(5) 0.1315(2) 0.074(7) Uiso 0.435(14) 1 d PGU A 1 N11 N 0.2880(4) 0.2734(5) 0.09921(17) 0.070(6) Uiso 0.435(14) 1 d PGU A 1 N12 N 0.3637(4) 0.3135(5) 0.10187(14) 0.056(5) Uiso 0.435(14) 1 d PGU A 1 C41 C 0.3221(3) 0.2867(4) 0.13466(15) 0.057(5) Uiso 0.435(14) 1 d PGU A 1 C42 C 0.2793(4) 0.2609(5) 0.14409(18) 0.079(6) Uiso 0.435(14) 1 d PGU A 1 C43 C 0.2447(4) 0.2551(5) 0.1070(2) 0.076(6) Uiso 0.435(14) 1 d PGU A 1 C44 C 0.3268(3) 0.2907(4) 0.11092(14) 0.053(5) Uiso 0.435(14) 1 d PGU A 1 C45 C 0.3983(4) 0.3346(4) 0.11634(16) 0.056(6) Uiso 0.435(14) 1 d PGU A 1 C46 C 0.4357(4) 0.3624(6) 0.1069(2) 0.052(6) Uiso 0.435(14) 1 d PGU A 1 H46 H 0.4394 0.3631 0.0916 0.062 Uiso 0.435(14) 1 calc PR A 1 C47 C 0.4676(4) 0.3891(6) 0.1202(3) 0.059(6) Uiso 0.435(14) 1 d PGU A 1 H47 H 0.4927 0.4077 0.1138 0.070 Uiso 0.435(14) 1 calc PR A 1 C48 C 0.4622(5) 0.3881(6) 0.1430(2) 0.058(6) Uiso 0.435(14) 1 d PGU A 1 H48 H 0.4835 0.4060 0.1519 0.070 Uiso 0.435(14) 1 calc PR A 1 C49 C 0.4247(4) 0.3603(5) 0.15250(19) 0.055(6) Uiso 0.435(14) 1 d PGU A 1 H49 H 0.4211 0.3596 0.1678 0.066 Uiso 0.435(14) 1 calc PR A 1 C50 C 0.3928(4) 0.3336(4) 0.13915(16) 0.056(6) Uiso 0.435(14) 1 d PGU A 1 O5 O 0.2784(5) 0.2616(7) 0.16457(18) 0.098(8) Uiso 0.435(14) 1 d PGU A 1 O6 O 0.2122(4) 0.2430(6) 0.0954(3) 0.075(6) Uiso 0.435(14) 1 d PGU A 1 N9A N 0.3545(3) 0.3050(3) 0.10722(12) 0.054(4) Uiso 0.565(14) 1 d PGU A 2 N10A N 0.2433(3) 0.2415(3) 0.12470(16) 0.061(5) Uiso 0.565(14) 1 d PGU A 2 N11A N 0.2887(3) 0.2719(4) 0.15593(13) 0.079(5) Uiso 0.565(14) 1 d PGU A 2 N12A N 0.3623(3) 0.3165(4) 0.15361(12) 0.069(5) Uiso 0.565(14) 1 d PGU A 2 C41A C 0.3212(3) 0.2870(3) 0.12143(11) 0.052(4) Uiso 0.565(14) 1 d PGU A 2 C42A C 0.2791(3) 0.2596(3) 0.11123(13) 0.062(5) Uiso 0.565(14) 1 d PGU A 2 C43A C 0.2459(3) 0.2512(4) 0.14722(16) 0.078(5) Uiso 0.565(14) 1 d PGU A 2 C44A C 0.3235(3) 0.2922(3) 0.14279(11) 0.068(5) Uiso 0.565(14) 1 d PGU A 2 C45A C 0.3969(3) 0.3349(4) 0.13781(14) 0.076(6) Uiso 0.565(14) 1 d PGU A 2 C46A C 0.4359(4) 0.3609(5) 0.14699(18) 0.080(6) Uiso 0.565(14) 1 d PGU A 2 H46A H 0.4400 0.3617 0.1622 0.095 Uiso 0.565(14) 1 calc PR A 2 C47A C 0.4689(4) 0.3856(5) 0.1334(2) 0.079(6) Uiso 0.565(14) 1 d PGU A 2 H47A H 0.4950 0.4030 0.1395 0.095 Uiso 0.565(14) 1 calc PR A 2 C48A C 0.4628(4) 0.3843(5) 0.1106(2) 0.070(6) Uiso 0.565(14) 1 d PGU A 2 H48A H 0.4849 0.4009 0.1015 0.084 Uiso 0.565(14) 1 calc PR A 2 C49A C 0.4238(4) 0.3584(4) 0.10141(17) 0.063(5) Uiso 0.565(14) 1 d PGU A 2 H49A H 0.4197 0.3575 0.0862 0.076 Uiso 0.565(14) 1 calc PR A 2 C50A C 0.3908(3) 0.3336(3) 0.11502(14) 0.056(5) Uiso 0.565(14) 1 d PGU A 2 O5A O 0.2772(4) 0.2570(5) 0.09019(14) 0.076(5) Uiso 0.565(14) 1 d PGU A 2 O6A O 0.2120(4) 0.2385(5) 0.15889(19) 0.085(6) Uiso 0.565(14) 1 d PGU A 2 C51 C 0.2841(5) 0.3033(5) 0.2126(2) 0.104(3) Uani 1 1 d GDU . . C52 C 0.3352(6) 0.3061(5) 0.2198(2) 0.104(3) Uani 1 1 d GDU . . C53 C 0.3572(5) 0.3497(6) 0.2099(3) 0.109(3) Uani 1 1 d GDU . . C54 C 0.3197(6) 0.3739(5) 0.1965(3) 0.111(3) Uani 1 1 d GDU . . C55 C 0.2745(5) 0.3452(6) 0.1982(3) 0.108(3) Uani 1 1 d GDU . . C56 C 0.2481(8) 0.2649(7) 0.2205(4) 0.108(4) Uani 1 1 d DU . . H56A H 0.2302 0.2520 0.2081 0.130 Uiso 1 1 calc R . . H56B H 0.2255 0.2796 0.2307 0.130 Uiso 1 1 calc R . . H56C H 0.2657 0.2387 0.2276 0.130 Uiso 1 1 calc R . . C57 C 0.3623(8) 0.2744(7) 0.2362(3) 0.110(4) Uani 1 1 d DU . . H57A H 0.3946 0.2672 0.2307 0.132 Uiso 1 1 calc R . . H57B H 0.3445 0.2442 0.2384 0.132 Uiso 1 1 calc R . . H57C H 0.3650 0.2916 0.2500 0.132 Uiso 1 1 calc R . . C58 C 0.4092(6) 0.3674(9) 0.2138(4) 0.112(4) Uani 1 1 d DU . . H58A H 0.4269 0.3674 0.2001 0.134 Uiso 1 1 calc R . . H58B H 0.4252 0.3458 0.2241 0.134 Uiso 1 1 calc R . . H58C H 0.4084 0.4002 0.2197 0.134 Uiso 1 1 calc R . . C59 C 0.3258(10) 0.4165(6) 0.1807(3) 0.118(4) Uani 1 1 d DU . . H59A H 0.3041 0.4122 0.1683 0.141 Uiso 1 1 calc R . . H59B H 0.3592 0.4175 0.1755 0.141 Uiso 1 1 calc R . . H59C H 0.3181 0.4467 0.1881 0.141 Uiso 1 1 calc R . . C60 C 0.2263(6) 0.3542(9) 0.1864(3) 0.116(4) Uani 1 1 d DU . . H60A H 0.2249 0.3877 0.1815 0.139 Uiso 1 1 calc R . . H60B H 0.1995 0.3478 0.1963 0.139 Uiso 1 1 calc R . . H60C H 0.2240 0.3326 0.1738 0.139 Uiso 1 1 calc R . . C61 C 0.2892(4) 0.2930(5) 0.0403(2) 0.091(3) Uani 1 1 d GDU . . C62 C 0.2774(4) 0.3354(5) 0.0527(2) 0.096(3) Uani 1 1 d GDU . . C63 C 0.3207(5) 0.3639(5) 0.0549(2) 0.099(3) Uani 1 1 d GDU . . C64 C 0.3592(4) 0.3390(5) 0.0439(2) 0.097(3) Uani 1 1 d GDU . . C65 C 0.3398(5) 0.2952(5) 0.0348(2) 0.093(3) Uani 1 1 d GDU . . C66 C 0.2550(6) 0.2518(6) 0.0338(3) 0.094(4) Uani 1 1 d DU . . H66A H 0.2609 0.2238 0.0431 0.112 Uiso 1 1 calc R . . H66B H 0.2608 0.2429 0.0187 0.112 Uiso 1 1 calc R . . H66C H 0.2215 0.2624 0.0355 0.112 Uiso 1 1 calc R . . C67 C 0.2266(5) 0.3497(9) 0.0603(4) 0.105(4) Uani 1 1 d DU . . H67A H 0.2288 0.3658 0.0744 0.126 Uiso 1 1 calc R . . H67B H 0.2066 0.3207 0.0617 0.126 Uiso 1 1 calc R . . H67C H 0.2120 0.3717 0.0498 0.126 Uiso 1 1 calc R . . C68 C 0.3285(9) 0.4127(6) 0.0664(3) 0.111(4) Uani 1 1 d DU . . H68A H 0.3019 0.4186 0.0765 0.133 Uiso 1 1 calc R . . H68B H 0.3294 0.4386 0.0556 0.133 Uiso 1 1 calc R . . H68C H 0.3591 0.4120 0.0743 0.133 Uiso 1 1 calc R . . C69 C 0.4097(6) 0.3608(9) 0.0407(4) 0.108(4) Uani 1 1 d DU . . H69A H 0.4248 0.3663 0.0548 0.129 Uiso 1 1 calc R . . H69B H 0.4070 0.3915 0.0329 0.129 Uiso 1 1 calc R . . H69C H 0.4296 0.3384 0.0322 0.129 Uiso 1 1 calc R . . C70 C 0.3663(7) 0.2575(6) 0.0210(3) 0.095(4) Uani 1 1 d DU . . H70A H 0.4008 0.2583 0.0244 0.113 Uiso 1 1 calc R . . H70B H 0.3616 0.2648 0.0057 0.113 Uiso 1 1 calc R . . H70C H 0.3534 0.2254 0.0242 0.113 Uiso 1 1 calc R . . Cl3 Cl 0.38356(16) 0.16195(17) 0.12929(6) 0.0737(10) Uani 1 1 d U . . O7 O 0.3767(6) 0.1338(5) 0.1484(2) 0.101(3) Uani 1 1 d U . . O8 O 0.3353(5) 0.1764(5) 0.1213(2) 0.092(3) Uani 1 1 d U . . O9 O 0.4072(5) 0.2086(5) 0.1333(2) 0.099(3) Uani 1 1 d U . . O10 O 0.4072(6) 0.1315(5) 0.1139(2) 0.099(3) Uani 1 1 d U . . Cl4 Cl 0.2487(4) 0.4056(3) 0.12480(15) 0.151(3) Uani 1 1 d U . . O11 O 0.2331(9) 0.3589(8) 0.1226(4) 0.157(4) Uani 1 1 d U . . O12 O 0.3054(8) 0.4038(7) 0.1257(4) 0.155(4) Uani 1 1 d U . . O13 O 0.2337(8) 0.4321(8) 0.1080(4) 0.162(4) Uani 1 1 d U . . O14 O 0.2359(8) 0.4324(7) 0.1447(4) 0.160(4) Uani 1 1 d U . . C71 C 0.2798(4) 0.6932(3) 0.11164(17) 0.110(2) Uiso 0.50 1 d PG B 1 H71 H 0.2806 0.7289 0.1095 0.132 Uiso 0.50 1 calc PR B 1 Cl5 Cl 0.3025(5) 0.6786(6) 0.13826(16) 0.132(2) Uiso 0.50 1 d PG B 1 Cl6 Cl 0.2185(3) 0.6718(6) 0.1091(2) 0.132(2) Uiso 0.50 1 d PG B 1 Cl7 Cl 0.3170(4) 0.6645(6) 0.09139(18) 0.132(2) Uiso 0.50 1 d PG B 1 C71A C 0.2830(6) 0.6759(6) 0.1194(3) 0.176(5) Uiso 0.50 1 d PG B 2 H71A H 0.3163 0.6897 0.1187 0.212 Uiso 0.50 1 calc PR B 2 Cl5A Cl 0.2531(10) 0.6976(8) 0.1435(3) 0.212(6) Uiso 0.50 1 d PG B 2 Cl6A Cl 0.2492(10) 0.6941(8) 0.0958(3) 0.212(6) Uiso 0.50 1 d PG B 2 Cl7A Cl 0.2867(10) 0.6109(7) 0.1203(4) 0.212(6) Uiso 0.50 1 d PG B 2 C72 C 0.6010(6) 0.4895(6) -0.0096(3) 0.180(5) Uiso 0.50 1 d PG C 1 H72 H 0.6023 0.4638 0.0018 0.216 Uiso 0.50 1 calc PR C 1 Cl8 Cl 0.6452(7) 0.5355(9) -0.0035(4) 0.216(6) Uiso 0.50 1 d PG C 1 Cl9 Cl 0.6139(8) 0.4633(8) -0.0357(4) 0.216(6) Uiso 0.50 1 d PG C 1 Cl10 Cl 0.5415(6) 0.5161(9) -0.0100(4) 0.216(6) Uiso 0.50 1 d PG C 1 C73 C 0.3861(3) 0.4992(3) 0.12673(16) 0.106(2) Uiso 0.50 1 d PG B 3 H73 H 0.3723 0.4659 0.1254 0.127 Uiso 0.50 1 calc PR B 3 Cl11 Cl 0.4119(5) 0.5067(5) 0.15336(15) 0.127(2) Uiso 0.50 1 d PG B 3 Cl12 Cl 0.3388(4) 0.5431(5) 0.1227(2) 0.127(2) Uiso 0.50 1 d PG B 3 Cl13 Cl 0.4323(4) 0.5077(5) 0.10650(17) 0.127(2) Uiso 0.50 1 d PG B 3 C74 C 0.5616(7) 0.3553(8) 0.0044(4) 0.216(6) Uiso 0.50 1 d PG C 3 H74 H 0.5931 0.3605 0.0119 0.259 Uiso 0.50 1 calc PR C 3 Cl14 Cl 0.5295(12) 0.3065(9) 0.0173(5) 0.259(7) Uiso 0.50 1 d PG C 3 Cl15 Cl 0.5723(11) 0.3404(10) -0.0237(4) 0.259(7) Uiso 0.50 1 d PG C 3 Cl16 Cl 0.5260(12) 0.4098(8) 0.0059(5) 0.259(7) Uiso 0.50 1 d PG C 3 C76 C 0.7309(7) 0.6382(7) 0.0130(3) 0.190(5) Uiso 0.50 1 d PG C 2 H76 H 0.7365 0.6184 0.0263 0.228 Uiso 0.50 1 calc PR C 2 Cl20 Cl 0.6860(8) 0.6837(9) 0.0186(5) 0.228(6) Uiso 0.50 1 d PG C 2 Cl21 Cl 0.7099(8) 0.5995(8) -0.0086(4) 0.228(6) Uiso 0.50 1 d PG C 2 Cl22 Cl 0.7866(6) 0.6668(9) 0.0049(4) 0.228(6) Uiso 0.50 1 d PG C 2 C77 C 0.5877(4) 0.6823(5) 0.0643(2) 0.135(3) Uiso 0.50 1 d PG C 4 H77 H 0.5586 0.6925 0.0726 0.162 Uiso 0.50 1 calc PR C 4 Cl23 Cl 0.5703(6) 0.6664(6) 0.0370(2) 0.162(3) Uiso 0.50 1 d PG C 4 Cl24 Cl 0.6149(7) 0.6306(5) 0.0773(3) 0.162(3) Uiso 0.50 1 d PG C 4 Cl25 Cl 0.6307(6) 0.7312(5) 0.0635(3) 0.162(3) Uiso 0.50 1 d PG C 4 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 0.0859(5) 0.0974(5) 0.0563(4) -0.0106(3) 0.0150(3) -0.0393(4) Cl1 0.099(3) 0.121(4) 0.060(2) -0.022(2) 0.012(2) -0.028(3) Ir2 0.0845(5) 0.0776(4) 0.0716(5) -0.0208(3) 0.0233(3) -0.0127(3) O1 0.071(5) 0.085(5) 0.071(5) -0.009(4) 0.020(5) -0.016(4) O2 0.079(6) 0.077(5) 0.065(5) 0.000(5) 0.002(5) -0.027(5) N1 0.089(4) 0.071(5) 0.056(5) -0.011(4) 0.017(4) -0.026(4) N2 0.075(5) 0.072(4) 0.055(5) -0.010(4) 0.009(5) -0.020(3) N3 0.070(5) 0.073(5) 0.067(6) -0.006(5) 0.016(5) -0.020(4) N4 0.085(5) 0.071(5) 0.067(6) -0.002(5) 0.018(5) -0.012(4) C1 0.076(4) 0.073(4) 0.055(5) -0.008(5) 0.014(5) -0.023(4) C2 0.072(5) 0.075(4) 0.055(5) -0.015(5) 0.017(5) -0.022(4) C3 0.076(5) 0.073(5) 0.062(5) 0.001(5) 0.008(5) -0.022(4) C4 0.076(5) 0.073(5) 0.060(5) -0.005(5) 0.015(5) -0.018(4) C5 0.098(5) 0.070(5) 0.076(6) -0.008(5) 0.014(6) -0.016(5) C6 0.114(7) 0.074(6) 0.095(8) 0.001(6) 0.016(7) -0.011(5) C7 0.125(7) 0.074(6) 0.096(8) -0.001(6) 0.024(7) -0.016(6) C8 0.129(8) 0.072(6) 0.098(8) -0.005(6) 0.021(7) -0.019(6) C9 0.119(7) 0.067(6) 0.088(7) -0.007(6) 0.025(7) -0.027(5) C10 0.105(5) 0.068(5) 0.068(6) -0.007(5) 0.021(5) -0.024(4) C11 0.098(5) 0.139(7) 0.071(5) -0.012(5) 0.017(5) -0.057(5) C12 0.106(6) 0.122(6) 0.072(5) -0.012(5) 0.016(5) -0.065(5) C13 0.108(6) 0.125(6) 0.068(5) -0.023(4) 0.011(5) -0.053(5) C14 0.096(6) 0.133(7) 0.063(4) -0.020(5) 0.011(4) -0.051(5) C15 0.088(4) 0.139(7) 0.069(5) -0.018(5) 0.013(4) -0.049(5) C16 0.100(8) 0.150(10) 0.067(7) -0.009(7) 0.015(6) -0.044(8) C17 0.121(9) 0.121(7) 0.080(8) -0.010(6) 0.013(8) -0.069(7) C18 0.129(10) 0.129(9) 0.074(8) -0.030(7) 0.009(7) -0.044(8) C19 0.098(9) 0.140(10) 0.071(6) -0.014(7) 0.005(6) -0.043(8) C20 0.087(7) 0.150(10) 0.090(9) -0.018(8) 0.011(7) -0.038(6) Ir3 0.0681(4) 0.1047(5) 0.0533(4) -0.0182(3) 0.0007(3) -0.0274(3) Cl2 0.136(5) 0.170(6) 0.047(2) -0.002(3) -0.012(2) -0.028(4) Ir4 0.0544(3) 0.0785(4) 0.0720(4) 0.0162(3) 0.0007(3) 0.0028(3) O3 0.055(4) 0.094(5) 0.055(5) 0.010(4) -0.001(4) -0.012(4) O4 0.053(5) 0.079(5) 0.083(6) -0.009(5) 0.007(5) -0.005(4) N5 0.070(4) 0.078(5) 0.048(5) -0.006(5) 0.010(4) -0.011(4) N6 0.049(4) 0.078(4) 0.055(5) 0.004(4) 0.001(4) -0.007(3) N7 0.054(5) 0.079(5) 0.063(5) -0.006(5) 0.003(5) -0.004(4) N8 0.067(5) 0.074(5) 0.073(6) 0.001(5) 0.010(5) -0.003(4) C21 0.054(4) 0.078(4) 0.046(5) -0.002(5) 0.010(4) -0.010(4) C22 0.052(4) 0.081(4) 0.051(5) 0.004(5) 0.004(4) -0.012(4) C23 0.051(4) 0.076(5) 0.066(5) -0.003(5) 0.001(5) -0.005(4) C24 0.056(4) 0.075(4) 0.059(5) 0.002(5) 0.004(5) -0.005(4) C25 0.079(5) 0.080(5) 0.088(6) -0.007(5) 0.011(5) -0.004(4) C26 0.091(6) 0.083(6) 0.105(8) -0.008(7) 0.019(7) 0.003(5) C27 0.096(7) 0.082(6) 0.115(8) -0.009(7) 0.029(7) 0.000(6) C28 0.098(7) 0.080(6) 0.111(8) -0.008(7) 0.030(7) -0.008(6) C29 0.090(6) 0.078(6) 0.092(7) -0.012(6) 0.023(6) -0.014(5) C30 0.079(5) 0.076(5) 0.078(6) -0.005(5) 0.020(5) -0.011(4) C31 0.076(5) 0.104(6) 0.101(6) -0.018(5) -0.011(5) -0.024(4) C32 0.079(6) 0.107(5) 0.101(6) 0.004(5) -0.001(5) -0.026(5) C33 0.084(6) 0.115(6) 0.089(5) 0.007(4) 0.009(5) -0.037(5) C34 0.081(5) 0.111(6) 0.086(5) -0.010(5) 0.017(4) -0.034(5) C35 0.072(4) 0.110(6) 0.103(6) -0.015(5) -0.001(5) -0.021(5) C36 0.076(8) 0.101(9) 0.112(8) -0.025(7) -0.017(7) -0.021(7) C37 0.092(9) 0.115(6) 0.114(10) 0.003(7) -0.006(8) -0.016(7) C38 0.105(9) 0.123(9) 0.094(7) 0.018(7) 0.003(7) -0.040(8) C39 0.105(9) 0.132(9) 0.094(8) -0.027(7) 0.030(7) -0.039(8) C40 0.089(7) 0.121(9) 0.112(9) -0.014(8) 0.003(7) -0.008(7) C51 0.113(6) 0.114(7) 0.085(6) -0.039(5) 0.041(5) -0.010(5) C52 0.121(7) 0.111(7) 0.081(4) -0.043(5) 0.027(5) -0.017(6) C53 0.123(7) 0.104(6) 0.100(6) -0.046(5) 0.023(6) -0.019(5) C54 0.125(7) 0.095(5) 0.112(7) -0.043(5) 0.028(6) -0.009(5) C55 0.112(6) 0.110(6) 0.102(7) -0.038(6) 0.041(6) 0.001(5) C56 0.116(9) 0.119(9) 0.089(9) -0.042(7) 0.046(7) -0.018(7) C57 0.134(10) 0.123(9) 0.073(6) -0.046(6) 0.017(7) -0.018(8) C58 0.124(8) 0.113(9) 0.098(9) -0.048(8) 0.024(7) -0.027(7) C59 0.133(10) 0.089(6) 0.131(10) -0.039(7) 0.028(9) -0.005(8) C60 0.114(7) 0.118(10) 0.116(10) -0.035(8) 0.040(7) 0.014(7) C61 0.072(5) 0.118(7) 0.082(5) 0.042(5) -0.006(4) 0.001(5) C62 0.082(5) 0.110(6) 0.097(7) 0.050(5) -0.001(5) 0.008(4) C63 0.090(6) 0.106(5) 0.101(7) 0.047(5) -0.007(6) 0.002(5) C64 0.083(5) 0.120(6) 0.087(6) 0.044(5) -0.004(5) -0.008(5) C65 0.076(5) 0.122(7) 0.079(4) 0.040(5) -0.002(5) -0.004(5) C66 0.076(7) 0.126(9) 0.079(8) 0.037(7) -0.012(6) 0.000(6) C67 0.080(6) 0.118(9) 0.116(10) 0.037(8) -0.009(7) 0.018(7) C68 0.113(9) 0.100(6) 0.119(10) 0.045(7) -0.008(8) 0.007(7) C69 0.091(7) 0.135(10) 0.097(9) 0.051(8) -0.004(7) -0.021(7) C70 0.080(8) 0.135(9) 0.069(7) 0.034(6) 0.008(6) -0.003(7) Cl3 0.079(2) 0.088(2) 0.0544(19) -0.0063(17) 0.0037(17) -0.0068(19) O7 0.124(7) 0.111(7) 0.067(5) 0.005(5) 0.006(5) -0.007(6) O8 0.080(5) 0.090(6) 0.106(7) 0.009(6) 0.002(5) -0.014(5) O9 0.095(6) 0.098(6) 0.102(7) -0.008(5) -0.012(6) -0.013(5) O10 0.121(7) 0.106(7) 0.071(6) -0.003(5) 0.024(6) 0.010(6) Cl4 0.178(6) 0.108(4) 0.168(6) -0.004(4) 0.027(5) 0.075(4) O11 0.180(9) 0.118(6) 0.174(10) -0.003(7) 0.016(9) 0.057(8) O12 0.173(8) 0.116(8) 0.176(10) 0.001(8) 0.023(8) 0.062(7) O13 0.184(10) 0.123(8) 0.178(9) 0.005(7) 0.019(8) 0.070(8) O14 0.190(10) 0.112(8) 0.179(8) -0.006(7) 0.028(8) 0.076(8) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'PATTY (Beurskens, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure (Rigaku & RAC 2007)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; 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 N1 2.113(15) . ? Ir1 O1 2.128(11) . ? Ir1 C14 2.134(13) . ? Ir1 C15 2.149(14) . ? Ir1 C13 2.167(13) . ? Ir1 C11 2.191(13) . ? Ir1 C12 2.203(13) . ? Ir1 Cl1 2.387(4) . ? Ir2 N2 2.078(14) . ? Ir2 N12A 2.123(8) . ? Ir2 C51 2.126(13) . ? Ir2 O5 2.134(14) . ? Ir2 C52 2.134(14) . ? Ir2 C55 2.172(14) . ? Ir2 C53 2.185(14) . ? Ir2 C54 2.208(14) . ? Ir2 N11A 2.215(9) . ? Ir2 N9 2.235(9) . ? Ir2 C44A 2.556(7) . ? O1 C2 1.262(18) . ? O2 C3 1.159(18) . ? N1 C10 1.349(18) . ? N1 C1 1.402(19) . ? N2 C2 1.31(2) . ? N2 C3 1.45(2) . ? N3 C4 1.38(2) . ? N3 C3 1.39(2) . ? N4 C4 1.32(2) . ? N4 C5 1.377(15) . ? C1 C4 1.39(2) . ? C1 C2 1.52(2) . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C11 C15 1.451 . ? C11 C12 1.451 . ? C11 C16 1.509(19) . ? C12 C13 1.451 . ? C12 C17 1.515(10) . ? C13 C14 1.451 . ? C13 C18 1.507(10) . ? C14 C15 1.451 . ? C14 C19 1.508(19) . ? C15 C20 1.508(10) . ? Ir3 C35 2.097(14) . ? Ir3 N5 2.119(13) . ? Ir3 C34 2.139(13) . ? Ir3 O3 2.144(12) . ? Ir3 C31 2.157(13) . ? Ir3 C33 2.224(13) . ? Ir3 C32 2.235(13) . ? Ir3 Cl2 2.384(5) . ? Ir4 N6 2.122(13) . ? Ir4 C65 2.143(13) . ? Ir4 O5A 2.145(10) . ? Ir4 C61 2.145(13) . ? Ir4 C64 2.169(13) . ? Ir4 C62 2.173(13) . ? Ir4 C63 2.187(13) . ? Ir4 N11 2.191(11) . ? Ir4 N12 2.193(9) . ? Ir4 N9A 2.361(7) . ? Ir4 C44 2.480(9) . ? O3 C22 1.274(17) . ? O4 C23 1.196(18) . ? N5 C21 1.309(19) . ? N5 C30 1.391(16) . ? N6 C22 1.36(2) . ? N6 C23 1.396(18) . ? N7 C23 1.39(2) . ? N7 C24 1.39(2) . ? N8 C24 1.33(2) . ? N8 C25 1.399(16) . ? C21 C24 1.38(2) . ? C21 C22 1.46(2) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.419 . ? C31 C35 1.419 . ? C31 C36 1.51(2) . ? C32 C33 1.419 . ? C32 C37 1.511(10) . ? C33 C34 1.419 . ? C33 C38 1.510(10) . ? C34 C35 1.419 . ? C34 C39 1.510(10) . ? C35 C40 1.509(10) . ? N9 C41 1.3638 . ? N9 C50 1.4267 . ? N10 C42 1.3288 . ? N10 C43 1.5115 . ? N11 C44 1.3568 . ? N11 C43 1.3624 . ? N12 C44 1.2977 . ? N12 C45 1.4071 . ? C41 C44 1.4469 . ? C41 C42 1.4721 . ? C42 O5 1.2401 . ? C43 O6 1.1756 . ? C45 C50 1.3897 . ? C45 C46 1.3901 . ? C46 C47 1.3896 . ? C47 C48 1.3904 . ? C48 C49 1.3899 . ? C49 C50 1.3904 . ? N9A C41A 1.3404 . ? N9A C50A 1.3412 . ? N10A C42A 1.3615 . ? N10A C43A 1.3904 . ? N11A C44A 1.3522 . ? N11A C43A 1.3956 . ? N12A C44A 1.4056 . ? N12A C45A 1.4311 . ? C41A C44A 1.3023 . ? C41A C42A 1.4979 . ? C42A O5A 1.2770 . ? C43A O6A 1.2107 . ? C45A C50A 1.3901 . ? C45A C46A 1.3903 . ? C46A C47A 1.3898 . ? C47A C48A 1.3904 . ? C48A C49A 1.3898 . ? C49A C50A 1.3901 . ? C51 C55 1.458 . ? C51 C52 1.458 . ? C51 C56 1.507(10) . ? C52 C53 1.458 . ? C52 C57 1.506(10) . ? C53 C54 1.458 . ? C53 C58 1.509(10) . ? C54 C55 1.458 . ? C54 C59 1.511(10) . ? C55 C60 1.511(10) . ? C61 C62 1.413 . ? C61 C65 1.413 . ? C61 C66 1.507(10) . ? C62 C63 1.413 . ? C62 C67 1.507(10) . ? C63 C64 1.413 . ? C63 C68 1.512(10) . ? C64 C65 1.413 . ? C64 C69 1.51(2) . ? C65 C70 1.506(10) . ? Cl3 O7 1.398(14) . ? Cl3 O10 1.403(14) . ? Cl3 O9 1.440(14) . ? Cl3 O8 1.451(15) . ? Cl4 O13 1.31(2) . ? Cl4 O11 1.34(2) . ? Cl4 O14 1.45(2) . ? Cl4 O12 1.54(2) . ? C71 Cl7 1.7697 . ? C71 Cl6 1.7698 . ? C71 Cl5 1.7704 . ? C71A Cl7A 1.7698 . ? C71A Cl5A 1.7699 . ? C71A Cl6A 1.7700 . ? C72 Cl8 1.7699 . ? C72 Cl9 1.7700 . ? C72 Cl10 1.7702 . ? C73 Cl11 1.7696 . ? C73 Cl12 1.7699 . ? C73 Cl13 1.7702 . ? C74 Cl14 1.7698 . ? C74 Cl16 1.7698 . ? C74 Cl15 1.7706 . ? C76 Cl22 1.7699 . ? C76 Cl20 1.7699 . ? C76 Cl21 1.7700 . ? C77 Cl25 1.7701 . ? C77 Cl24 1.7702 . ? C77 Cl23 1.7702 . ? 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 N1 Ir1 O1 77.4(5) . . ? N1 Ir1 C14 121.3(5) . . ? O1 Ir1 C14 96.1(5) . . ? N1 Ir1 C15 160.3(5) . . ? O1 Ir1 C15 97.5(5) . . ? C14 Ir1 C15 39.6(3) . . ? N1 Ir1 C13 102.0(5) . . ? O1 Ir1 C13 128.1(5) . . ? C14 Ir1 C13 39.4(3) . . ? C15 Ir1 C13 65.9(4) . . ? N1 Ir1 C11 151.7(5) . . ? O1 Ir1 C11 130.7(5) . . ? C14 Ir1 C11 65.7(4) . . ? C15 Ir1 C11 39.0(3) . . ? C13 Ir1 C11 65.2(4) . . ? N1 Ir1 C12 115.8(5) . . ? O1 Ir1 C12 160.9(5) . . ? C14 Ir1 C12 65.5(4) . . ? C15 Ir1 C12 65.3(4) . . ? C13 Ir1 C12 38.8(3) . . ? C11 Ir1 C12 38.6(3) . . ? N1 Ir1 Cl1 85.1(4) . . ? O1 Ir1 Cl1 84.8(3) . . ? C14 Ir1 Cl1 153.2(4) . . ? C15 Ir1 Cl1 113.6(4) . . ? C13 Ir1 Cl1 147.0(4) . . ? C11 Ir1 Cl1 93.4(3) . . ? C12 Ir1 Cl1 109.2(4) . . ? N2 Ir2 N12A 89.6(5) . . ? N2 Ir2 C51 112.5(6) . . ? N12A Ir2 C51 157.7(6) . . ? N2 Ir2 O5 89.3(6) . . ? N12A Ir2 O5 82.3(3) . . ? C51 Ir2 O5 94.3(5) . . ? N2 Ir2 C52 93.1(5) . . ? N12A Ir2 C52 147.2(5) . . ? C51 Ir2 C52 40.0(3) . . ? O5 Ir2 C52 130.4(5) . . ? N2 Ir2 C55 152.0(6) . . ? N12A Ir2 C55 118.1(5) . . ? C51 Ir2 C55 39.6(3) . . ? O5 Ir2 C55 90.2(6) . . ? C52 Ir2 C55 66.4(4) . . ? N2 Ir2 C53 111.1(6) . . ? N12A Ir2 C53 109.9(5) . . ? C51 Ir2 C53 66.3(5) . . ? O5 Ir2 C53 155.7(6) . . ? C52 Ir2 C53 39.4(3) . . ? C55 Ir2 C53 65.6(4) . . ? N2 Ir2 C54 149.4(6) . . ? N12A Ir2 C54 96.9(5) . . ? C51 Ir2 C54 65.9(4) . . ? O5 Ir2 C54 121.2(7) . . ? C52 Ir2 C54 65.8(4) . . ? C55 Ir2 C54 38.9(3) . . ? C53 Ir2 C54 38.8(3) . . ? N2 Ir2 N11A 91.5(5) . . ? N12A Ir2 N11A 65.3(2) . . ? C51 Ir2 N11A 109.1(5) . . ? O5 Ir2 N11A 17.2(3) . . ? C52 Ir2 N11A 147.2(5) . . ? C55 Ir2 N11A 96.2(5) . . ? C53 Ir2 N11A 157.1(5) . . ? C54 Ir2 N11A 118.4(5) . . ? N2 Ir2 N9 86.3(5) . . ? N12A Ir2 N9 11.1(4) . . ? C51 Ir2 N9 156.8(6) . . ? O5 Ir2 N9 71.7(3) . . ? C52 Ir2 N9 157.9(5) . . ? C55 Ir2 N9 120.0(5) . . ? C53 Ir2 N9 120.9(5) . . ? C54 Ir2 N9 105.0(5) . . ? N11A Ir2 N9 54.9(3) . . ? N2 Ir2 C44A 90.2(4) . . ? N12A Ir2 C44A 33.36(10) . . ? C51 Ir2 C44A 137.6(5) . . ? O5 Ir2 C44A 49.0(3) . . ? C52 Ir2 C44A 176.6(4) . . ? C55 Ir2 C44A 110.2(4) . . ? C53 Ir2 C44A 139.3(5) . . ? C54 Ir2 C44A 111.4(5) . . ? N11A Ir2 C44A 31.92(10) . . ? N9 Ir2 C44A 23.1(3) . . ? C2 O1 Ir1 119.4(11) . . ? C10 N1 C1 112.5(13) . . ? C10 N1 Ir1 134.7(9) . . ? C1 N1 Ir1 112.8(12) . . ? C2 N2 C3 119.7(15) . . ? C2 N2 Ir2 122.4(11) . . ? C3 N2 Ir2 116.7(10) . . ? C4 N3 C3 124.0(14) . . ? C4 N4 C5 115.4(13) . . ? C4 C1 N1 123.8(16) . . ? C4 C1 C2 119.6(14) . . ? N1 C1 C2 116.6(14) . . ? O1 C2 N2 125.7(17) . . ? O1 C2 C1 113.6(14) . . ? N2 C2 C1 120.3(14) . . ? O2 C3 N3 120.6(16) . . ? O2 C3 N2 120.7(17) . . ? N3 C3 N2 118.6(13) . . ? N4 C4 N3 120.6(15) . . ? N4 C4 C1 122.1(15) . . ? N3 C4 C1 117.2(16) . . ? N4 C5 C6 117.3(10) . . ? N4 C5 C10 122.7(10) . . ? C6 C5 C10 120.0 . . ? C5 C6 C7 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? N1 C10 C9 116.9(9) . . ? N1 C10 C5 123.1(9) . . ? C9 C10 C5 120.0 . . ? C15 C11 C12 108.0 . . ? C15 C11 C16 122.2(14) . . ? C12 C11 C16 129.8(14) . . ? C15 C11 Ir1 68.9(5) . . ? C12 C11 Ir1 71.1(5) . . ? C16 C11 Ir1 125.5(11) . . ? C13 C12 C11 108.0 . . ? C13 C12 C17 127.0(13) . . ? C11 C12 C17 124.9(13) . . ? C13 C12 Ir1 69.3(5) . . ? C11 C12 Ir1 70.3(5) . . ? C17 C12 Ir1 128.9(11) . . ? C12 C13 C14 108.0 . . ? C12 C13 C18 123.9(13) . . ? C14 C13 C18 127.9(13) . . ? C12 C13 Ir1 71.9(5) . . ? C14 C13 Ir1 69.0(5) . . ? C18 C13 Ir1 128.1(11) . . ? C15 C14 C13 108.0 . . ? C15 C14 C19 124.7(14) . . ? C13 C14 C19 127.3(14) . . ? C15 C14 Ir1 70.8(5) . . ? C13 C14 Ir1 71.5(5) . . ? C19 C14 Ir1 123.8(11) . . ? C11 C15 C14 108.0 . . ? C11 C15 C20 123.0(13) . . ? C14 C15 C20 128.8(13) . . ? C11 C15 Ir1 72.1(5) . . ? C14 C15 Ir1 69.6(5) . . ? C20 C15 Ir1 127.9(11) . . ? C35 Ir3 N5 169.7(5) . . ? C35 Ir3 C34 39.1(3) . . ? N5 Ir3 C34 132.0(5) . . ? C35 Ir3 O3 106.7(5) . . ? N5 Ir3 O3 76.0(5) . . ? C34 Ir3 O3 91.2(4) . . ? C35 Ir3 C31 38.9(3) . . ? N5 Ir3 C31 138.7(5) . . ? C34 Ir3 C31 64.6(4) . . ? O3 Ir3 C31 145.2(5) . . ? C35 Ir3 C33 64.1(4) . . ? N5 Ir3 C33 105.6(5) . . ? C34 Ir3 C33 37.9(3) . . ? O3 Ir3 C33 113.0(5) . . ? C31 Ir3 C33 63.2(4) . . ? C35 Ir3 C32 63.9(4) . . ? N5 Ir3 C32 108.7(5) . . ? C34 Ir3 C32 63.3(4) . . ? O3 Ir3 C32 150.1(5) . . ? C31 Ir3 C32 37.6(3) . . ? C33 Ir3 C32 37.1(3) . . ? C35 Ir3 Cl2 106.3(4) . . ? N5 Ir3 Cl2 83.7(4) . . ? C34 Ir3 Cl2 142.7(4) . . ? O3 Ir3 Cl2 87.3(3) . . ? C31 Ir3 Cl2 97.3(4) . . ? C33 Ir3 Cl2 159.1(4) . . ? C32 Ir3 Cl2 122.4(4) . . ? N6 Ir4 C65 92.0(5) . . ? N6 Ir4 O5A 90.4(5) . . ? C65 Ir4 O5A 130.8(4) . . ? N6 Ir4 C61 111.7(5) . . ? C65 Ir4 C61 38.5(3) . . ? O5A Ir4 C61 96.2(4) . . ? N6 Ir4 C64 109.4(5) . . ? C65 Ir4 C64 38.3(3) . . ? O5A Ir4 C64 155.8(5) . . ? C61 Ir4 C64 64.0(4) . . ? N6 Ir4 C62 149.9(5) . . ? C65 Ir4 C62 64.0(4) . . ? O5A Ir4 C62 92.3(5) . . ? C61 Ir4 C62 38.2(3) . . ? C64 Ir4 C62 63.6(4) . . ? N6 Ir4 C63 147.0(5) . . ? C65 Ir4 C63 63.7(4) . . ? O5A Ir4 C63 122.3(5) . . ? C61 Ir4 C63 63.7(4) . . ? C64 Ir4 C63 37.9(3) . . ? C62 Ir4 C63 37.8(3) . . ? N6 Ir4 N11 94.8(5) . . ? C65 Ir4 N11 149.9(4) . . ? O5A Ir4 N11 20.2(3) . . ? C61 Ir4 N11 112.6(4) . . ? C64 Ir4 N11 155.3(5) . . ? C62 Ir4 N11 98.1(5) . . ? C63 Ir4 N11 117.6(5) . . ? N6 Ir4 N12 87.0(5) . . ? C65 Ir4 N12 145.5(4) . . ? O5A Ir4 N12 83.7(3) . . ? C61 Ir4 N12 161.2(5) . . ? C64 Ir4 N12 110.3(4) . . ? C62 Ir4 N12 123.0(5) . . ? C63 Ir4 N12 100.4(5) . . ? N11 Ir4 N12 64.3(2) . . ? N6 Ir4 N9A 85.7(4) . . ? C65 Ir4 N9A 156.3(4) . . ? O5A Ir4 N9A 72.8(2) . . ? C61 Ir4 N9A 159.9(4) . . ? C64 Ir4 N9A 121.1(4) . . ? C62 Ir4 N9A 123.7(4) . . ? C63 Ir4 N9A 107.4(4) . . ? N11 Ir4 N9A 53.6(3) . . ? N12 Ir4 N9A 11.0(3) . . ? N6 Ir4 C44 88.2(4) . . ? C65 Ir4 C44 176.9(4) . . ? O5A Ir4 C44 52.2(3) . . ? C61 Ir4 C44 143.9(4) . . ? C64 Ir4 C44 138.9(4) . . ? C62 Ir4 C44 116.7(4) . . ? C63 Ir4 C44 114.7(4) . . ? N11 Ir4 C44 33.04(13) . . ? N12 Ir4 C44 31.49(12) . . ? N9A Ir4 C44 20.6(3) . . ? C22 O3 Ir3 115.1(10) . . ? C21 N5 C30 117.5(12) . . ? C21 N5 Ir3 114.8(11) . . ? C30 N5 Ir3 127.7(9) . . ? C22 N6 C23 119.5(13) . . ? C22 N6 Ir4 123.1(10) . . ? C23 N6 Ir4 116.5(10) . . ? C23 N7 C24 124.4(13) . . ? C24 N8 C25 112.1(13) . . ? N5 C21 C24 121.6(15) . . ? N5 C21 C22 116.7(13) . . ? C24 C21 C22 121.4(14) . . ? O3 C22 N6 122.9(15) . . ? O3 C22 C21 117.1(14) . . ? N6 C22 C21 119.9(13) . . ? O4 C23 N7 120.0(13) . . ? O4 C23 N6 121.1(15) . . ? N7 C23 N6 118.9(14) . . ? N8 C24 C21 125.5(15) . . ? N8 C24 N7 119.1(13) . . ? C21 C24 N7 115.4(14) . . ? C26 C25 C30 120.0 . . ? C26 C25 N8 115.7(9) . . ? C30 C25 N8 123.6(9) . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 N5 121.5(9) . . ? C25 C30 N5 118.4(9) . . ? C32 C31 C35 108.0 . . ? C32 C31 C36 129.5(13) . . ? C35 C31 C36 122.5(13) . . ? C32 C31 Ir3 74.1(5) . . ? C35 C31 Ir3 68.2(5) . . ? C36 C31 Ir3 122.6(11) . . ? C33 C32 C31 108.0 . . ? C33 C32 C37 124.8(14) . . ? C31 C32 C37 125.7(14) . . ? C33 C32 Ir3 71.0(5) . . ? C31 C32 Ir3 68.2(5) . . ? C37 C32 Ir3 137.2(12) . . ? C32 C33 C34 108.0 . . ? C32 C33 C38 120.9(15) . . ? C34 C33 C38 131.0(15) . . ? C32 C33 Ir3 71.9(5) . . ? C34 C33 Ir3 67.8(5) . . ? C38 C33 Ir3 123.3(11) . . ? C33 C34 C35 108.0 . . ? C33 C34 C39 111.8(15) . . ? C35 C34 C39 140.1(15) . . ? C33 C34 Ir3 74.3(5) . . ? C35 C34 Ir3 68.8(5) . . ? C39 C34 Ir3 125.1(11) . . ? C31 C35 C34 108.0 . . ? C31 C35 C40 127.7(14) . . ? C34 C35 C40 124.2(14) . . ? C31 C35 Ir3 72.8(5) . . ? C34 C35 Ir3 72.1(5) . . ? C40 C35 Ir3 119.6(12) . . ? C41 N9 C50 112.5 . . ? C41 N9 Ir2 114.3(4) . . ? C50 N9 Ir2 132.4(4) . . ? C42 N10 C43 118.2 . . ? C44 N11 C43 128.1 . . ? C44 N11 Ir4 85.2(3) . . ? C43 N11 Ir4 146.6(3) . . ? C44 N12 C45 116.5 . . ? C44 N12 Ir4 86.6(3) . . ? C45 N12 Ir4 156.8(3) . . ? N9 C41 C44 124.7 . . ? N9 C41 C42 115.9 . . ? C44 C41 C42 119.4 . . ? O5 C42 N10 124.3 . . ? O5 C42 C41 113.4 . . ? N10 C42 C41 121.9 . . ? O6 C43 N11 122.6 . . ? O6 C43 N10 120.8 . . ? N11 C43 N10 116.1 . . ? N12 C44 N11 123.0 . . ? N12 C44 C41 121.6 . . ? N11 C44 C41 115.1 . . ? N12 C44 Ir4 62.0(3) . . ? N11 C44 Ir4 61.7(3) . . ? C41 C44 Ir4 175.8(4) . . ? C50 C45 C46 120.0 . . ? C50 C45 N12 122.6 . . ? C46 C45 N12 117.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C50 120.0 . . ? C45 C50 C49 120.0 . . ? C45 C50 N9 121.7 . . ? C49 C50 N9 118.3 . . ? C42 O5 Ir2 124.5(3) . . ? C41A N9A C50A 118.8 . . ? C41A N9A Ir4 112.4(3) . . ? C50A N9A Ir4 127.9(3) . . ? C42A N10A C43A 118.8 . . ? C44A N11A C43A 121.6 . . ? C44A N11A Ir2 88.1(3) . . ? C43A N11A Ir2 149.8(3) . . ? C44A N12A C45A 110.1 . . ? C44A N12A Ir2 90.5(3) . . ? C45A N12A Ir2 159.2(3) . . ? C44A C41A N9A 124.4 . . ? C44A C41A C42A 120.0 . . ? N9A C41A C42A 115.6 . . ? O5A C42A N10A 123.2 . . ? O5A C42A C41A 118.0 . . ? N10A C42A C41A 118.6 . . ? O6A C43A N10A 118.7 . . ? O6A C43A N11A 121.9 . . ? N10A C43A N11A 119.3 . . ? C41A C44A N11A 120.4 . . ? C41A C44A N12A 123.3 . . ? N11A C44A N12A 116.2 . . ? C41A C44A Ir2 176.4(5) . . ? N11A C44A Ir2 60.0(3) . . ? N12A C44A Ir2 56.2(3) . . ? C50A C45A C46A 120.0 . . ? C50A C45A N12A 125.2 . . ? C46A C45A N12A 114.3 . . ? C47A C46A C45A 120.0 . . ? C46A C47A C48A 120.0 . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? N9A C50A C49A 123.0 . . ? N9A C50A C45A 116.8 . . ? C49A C50A C45A 120.0 . . ? C42A O5A Ir4 121.0(2) . . ? C55 C51 C52 108.0 . . ? C55 C51 C56 127.9(16) . . ? C52 C51 C56 123.9(16) . . ? C55 C51 Ir2 71.9(5) . . ? C52 C51 Ir2 70.3(5) . . ? C56 C51 Ir2 126.7(10) . . ? C53 C52 C51 108.0 . . ? C53 C52 C57 122.4(15) . . ? C51 C52 C57 129.4(15) . . ? C53 C52 Ir2 72.2(5) . . ? C51 C52 Ir2 69.7(5) . . ? C57 C52 Ir2 128.2(11) . . ? C52 C53 C54 108.0 . . ? C52 C53 C58 125.3(16) . . ? C54 C53 C58 126.7(16) . . ? C52 C53 Ir2 68.4(5) . . ? C54 C53 Ir2 71.5(5) . . ? C58 C53 Ir2 127.7(11) . . ? C55 C54 C53 108.0 . . ? C55 C54 C59 123.0(16) . . ? C53 C54 C59 128.4(16) . . ? C55 C54 Ir2 69.2(5) . . ? C53 C54 Ir2 69.8(5) . . ? C59 C54 Ir2 119.6(11) . . ? C54 C55 C51 108.0 . . ? C54 C55 C60 127.7(16) . . ? C51 C55 C60 124.2(16) . . ? C54 C55 Ir2 71.9(5) . . ? C51 C55 Ir2 68.5(5) . . ? C60 C55 Ir2 122.5(11) . . ? C62 C61 C65 108.0 . . ? C62 C61 C66 127.2(13) . . ? C65 C61 C66 124.8(13) . . ? C62 C61 Ir4 71.9(5) . . ? C65 C61 Ir4 70.7(5) . . ? C66 C61 Ir4 122.7(10) . . ? C63 C62 C61 108.0 . . ? C63 C62 C67 126.2(14) . . ? C61 C62 C67 125.6(15) . . ? C63 C62 Ir4 71.6(5) . . ? C61 C62 Ir4 69.9(5) . . ? C67 C62 Ir4 128.1(11) . . ? C62 C63 C64 108.0 . . ? C62 C63 C68 129.9(14) . . ? C64 C63 C68 122.1(14) . . ? C62 C63 Ir4 70.5(5) . . ? C64 C63 Ir4 70.4(5) . . ? C68 C63 Ir4 125.1(11) . . ? C65 C64 C63 108.0 . . ? C65 C64 C69 128.3(15) . . ? C63 C64 C69 123.3(15) . . ? C65 C64 Ir4 69.9(5) . . ? C63 C64 Ir4 71.8(5) . . ? C69 C64 Ir4 129.6(11) . . ? C61 C65 C64 108.0 . . ? C61 C65 C70 124.4(13) . . ? C64 C65 C70 127.6(13) . . ? C61 C65 Ir4 70.9(5) . . ? C64 C65 Ir4 71.9(5) . . ? C70 C65 Ir4 124.6(10) . . ? O7 Cl3 O10 106.7(9) . . ? O7 Cl3 O9 113.7(9) . . ? O10 Cl3 O9 115.2(9) . . ? O7 Cl3 O8 107.6(9) . . ? O10 Cl3 O8 110.7(9) . . ? O9 Cl3 O8 102.8(8) . . ? O13 Cl4 O11 110.1(17) . . ? O13 Cl4 O14 107.1(13) . . ? O11 Cl4 O14 118.8(15) . . ? O13 Cl4 O12 110.9(15) . . ? O11 Cl4 O12 106.8(13) . . ? O14 Cl4 O12 103.0(14) . . ? Cl7 C71 Cl6 109.5 . . ? Cl7 C71 Cl5 109.5 . . ? Cl6 C71 Cl5 109.5 . . ? Cl7A C71A Cl5A 109.5 . . ? Cl7A C71A Cl6A 109.4 . . ? Cl5A C71A Cl6A 109.5 . . ? Cl8 C72 Cl9 109.5 . . ? Cl8 C72 Cl10 109.5 . . ? Cl9 C72 Cl10 109.4 . . ? Cl11 C73 Cl12 109.5 . . ? Cl11 C73 Cl13 109.5 . . ? Cl12 C73 Cl13 109.4 . . ? Cl14 C74 Cl16 109.5 . . ? Cl14 C74 Cl15 109.5 . . ? Cl16 C74 Cl15 109.4 . . ? Cl22 C76 Cl20 109.5 . . ? Cl22 C76 Cl21 109.4 . . ? Cl20 C76 Cl21 109.5 . . ? Cl25 C77 Cl24 109.4 . . ? Cl25 C77 Cl23 109.5 . . ? Cl24 C77 Cl23 109.5 . . ? #===END========================================================================