# 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 'Ernesto Carmona' _publ_contact_author_email GUZMAN@US.ES _publ_section_title ; Synthesis and Structural Characterization of a Binuclear Iridium Complex with Bridging, Bidentate N-Heterocyclic Carbene Coordination of 2,2':6',2''-Terpyridine ; loop_ _publ_author_name 'Ernesto Carmona' 'Eleuterio Alvarez' 'Margarita Paneque' 'Manuel L Poveda' 'Florencia Vattier' # Attachment 'Copia de Global for 2_M, 2_T and 3_New.cif' #=============================================================================80 # Data Global for compounds 2_M, 2_T and 3 #=============================================================================80 data_2_M _database_code_depnum_ccdc_archive 'CCDC 731545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H43 B Ir N9' _chemical_formula_sum 'C36 H43 B Ir N9' _chemical_formula_weight 804.80 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0676(3) _cell_length_b 22.2040(7) _cell_length_c 13.7392(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.8360(10) _cell_angle_gamma 90.00 _cell_volume 3484.25(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8693 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.08 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 3.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 0.559 _exptl_absorpt_process_details ; SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. ; _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-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 91260 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.52 _reflns_number_total 10431 _reflns_number_gt 8440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker (2006). APEX 2. Version 2.1.' _computing_cell_refinement 'Bruker (2006). APEX 2. Version 2.1.' _computing_data_reduction 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_solution 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2003)' _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. The asymmetric unit of the structure is formed by one mononuclear Ir(III) complex 2. In this monoclinic polymorph crystal form of 2 the polypyridine moiety occupies a region of the space opposite to that of the Tp^Me2^ ligand and features a trans-trans conformation of the pyridine rings. All the non-hydrogen atoms were refined with anisotropic displacement parameters. Some few reflections to low angle that present values very below their calculated values, possibly partially covered for "beam stopper" were eliminated at the end of the refinement (OMIT command). The hydrogen atoms bonded to the nitrogen atoms were located from the difference Fourier synthesis and refined isotropically with geometric restraints. The other hydrogen atoms were placed in calculated positions and refined with isotropic displacement parameters by using a riding model. ; _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^)+(0.0221P)^2^+2.9293P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10431 _refine_ls_number_parameters 435 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0533 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.172131(7) 0.176468(4) 0.574158(6) 0.02077(3) Uani 1 1 d . . . N1 N 0.23585(18) 0.17633(10) 0.74204(16) 0.0301(4) Uani 1 1 d . . . N2 N 0.16617(18) 0.20601(10) 0.78885(15) 0.0293(4) Uani 1 1 d . . . N3 N -0.00088(16) 0.16538(8) 0.58667(15) 0.0237(4) Uani 1 1 d . . . N4 N -0.03128(17) 0.20113(9) 0.65520(15) 0.0277(4) Uani 1 1 d . . . N5 N 0.14772(17) 0.27163(9) 0.58679(15) 0.0266(4) Uani 1 1 d . . . N6 N 0.10055(18) 0.29018(9) 0.66084(15) 0.0284(4) Uani 1 1 d . . . N7 N 0.15341(17) 0.14136(9) 0.36641(15) 0.0252(4) Uani 1 1 d D . . H7N H 0.2174(18) 0.1221(11) 0.4024(19) 0.030 Uiso 1 1 d D . . N8 N 0.12684(19) 0.08090(9) 0.11524(16) 0.0307(4) Uani 1 1 d . . . N9 N 0.1783(2) -0.00291(12) -0.08998(19) 0.0485(6) Uani 1 1 d . . . C1 C 0.3197(2) 0.14874(13) 0.8177(2) 0.0362(6) Uani 1 1 d . . . C2 C 0.3019(3) 0.16012(15) 0.9119(2) 0.0429(7) Uani 1 1 d . . . H2 H 0.3487 0.1459 0.9775 0.051 Uiso 1 1 calc R . . C3 C 0.2051(3) 0.19541(13) 0.8915(2) 0.0375(6) Uani 1 1 d . . . C4 C 0.4158(3) 0.11180(17) 0.8026(2) 0.0521(8) Uani 1 1 d . . . H4A H 0.3852 0.0722 0.7754 0.078 Uiso 1 1 calc R . . H4B H 0.4781 0.1068 0.8687 0.078 Uiso 1 1 calc R . . H4C H 0.4473 0.1321 0.7539 0.078 Uiso 1 1 calc R . . C5 C 0.1435(3) 0.21881(15) 0.9626(2) 0.0496(8) Uani 1 1 d . . . H5A H 0.1537 0.2626 0.9695 0.074 Uiso 1 1 calc R . . H5B H 0.1767 0.1999 1.0303 0.074 Uiso 1 1 calc R . . H5C H 0.0599 0.2093 0.9346 0.074 Uiso 1 1 calc R . . C6 C -0.09559(19) 0.13222(11) 0.53764(19) 0.0271(5) Uani 1 1 d . . . C7 C -0.1860(2) 0.14677(13) 0.5762(2) 0.0344(6) Uani 1 1 d . . . H7 H -0.2625 0.1300 0.5554 0.041 Uiso 1 1 calc R . . C8 C -0.1428(2) 0.19017(12) 0.6501(2) 0.0335(6) Uani 1 1 d . . . C9 C -0.0993(2) 0.08750(12) 0.4560(2) 0.0347(6) Uani 1 1 d . . . H9A H -0.0288 0.0916 0.4358 0.052 Uiso 1 1 calc R . . H9B H -0.1688 0.0947 0.3961 0.052 Uiso 1 1 calc R . . H9C H -0.1026 0.0467 0.4822 0.052 Uiso 1 1 calc R . . C10 C -0.2002(3) 0.22121(16) 0.7185(2) 0.0494(8) Uani 1 1 d . . . H10A H -0.1607 0.2095 0.7902 0.074 Uiso 1 1 calc R . . H10B H -0.2828 0.2094 0.6984 0.074 Uiso 1 1 calc R . . H10C H -0.1946 0.2649 0.7116 0.074 Uiso 1 1 calc R . . C11 C 0.1725(2) 0.32216(11) 0.5429(2) 0.0300(5) Uani 1 1 d . . . C12 C 0.1422(3) 0.37256(12) 0.5898(2) 0.0374(6) Uani 1 1 d . . . H12 H 0.1509 0.4136 0.5741 0.045 Uiso 1 1 calc R . . C13 C 0.0975(3) 0.35116(12) 0.6625(2) 0.0380(6) Uani 1 1 d . . . C14 C 0.2246(3) 0.32093(12) 0.4584(2) 0.0368(6) Uani 1 1 d . . . H14A H 0.3079 0.3108 0.4866 0.055 Uiso 1 1 calc R . . H14B H 0.2158 0.3606 0.4255 0.055 Uiso 1 1 calc R . . H14C H 0.1843 0.2906 0.4074 0.055 Uiso 1 1 calc R . . C15 C 0.0501(4) 0.38509(14) 0.7348(3) 0.0596(10) Uani 1 1 d . . . H15A H -0.0326 0.3747 0.7208 0.089 Uiso 1 1 calc R . . H15B H 0.0571 0.4285 0.7249 0.089 Uiso 1 1 calc R . . H15C H 0.0946 0.3743 0.8058 0.089 Uiso 1 1 calc R . . C16 C 0.3390(2) 0.18320(11) 0.5626(2) 0.0290(5) Uani 1 1 d . . . H16A H 0.3362 0.2083 0.5023 0.035 Uiso 1 1 calc R . . H16B H 0.3915 0.2033 0.6248 0.035 Uiso 1 1 calc R . . C17 C 0.3873(2) 0.12213(12) 0.5515(2) 0.0296(5) Uani 1 1 d . . . C18 C 0.3229(2) 0.07383(11) 0.55746(19) 0.0280(5) Uani 1 1 d . . . C19 C 0.20613(19) 0.08504(10) 0.57180(18) 0.0254(5) Uani 1 1 d . . . H19A H 0.2055 0.0666 0.6372 0.030 Uiso 1 1 calc R . . H19B H 0.1437 0.0657 0.5150 0.030 Uiso 1 1 calc R . . C20 C 0.5066(2) 0.12111(14) 0.5401(3) 0.0474(8) Uani 1 1 d . . . H20A H 0.5298 0.0793 0.5342 0.071 Uiso 1 1 calc R . . H20B H 0.5630 0.1399 0.6005 0.071 Uiso 1 1 calc R . . H20C H 0.5050 0.1435 0.4782 0.071 Uiso 1 1 calc R . . C21 C 0.3595(2) 0.00975(12) 0.5541(2) 0.0398(6) Uani 1 1 d . . . H21A H 0.4389 0.0085 0.5495 0.060 Uiso 1 1 calc R . . H21B H 0.3053 -0.0102 0.4939 0.060 Uiso 1 1 calc R . . H21C H 0.3585 -0.0110 0.6167 0.060 Uiso 1 1 calc R . . C22 C 0.1054(2) 0.17622(10) 0.42510(17) 0.0236(4) Uani 1 1 d . . . C23 C 0.0020(2) 0.20686(11) 0.36546(19) 0.0294(5) Uani 1 1 d . . . H23 H -0.0346 0.2342 0.3987 0.035 Uiso 1 1 calc R . . C24 C -0.0460(2) 0.19815(12) 0.2619(2) 0.0345(6) Uani 1 1 d . . . H24 H -0.1161 0.2186 0.2249 0.041 Uiso 1 1 calc R . . C25 C 0.0070(3) 0.15930(12) 0.2093(2) 0.0361(6) Uani 1 1 d . . . H25 H -0.0275 0.1528 0.1375 0.043 Uiso 1 1 calc R . . C26 C 0.1091(2) 0.13099(11) 0.26310(18) 0.0288(5) Uani 1 1 d . . . C27 C 0.1713(2) 0.08694(11) 0.21796(19) 0.0310(5) Uani 1 1 d . . . C28 C 0.2666(3) 0.05349(14) 0.2775(2) 0.0418(7) Uani 1 1 d . . . H28 H 0.2965 0.0589 0.3499 0.050 Uiso 1 1 calc R . . C29 C 0.3172(3) 0.01177(15) 0.2287(2) 0.0464(7) Uani 1 1 d . . . H29 H 0.3819 -0.0120 0.2674 0.056 Uiso 1 1 calc R . . C30 C 0.2720(3) 0.00553(13) 0.1234(2) 0.0410(6) Uani 1 1 d . . . H30 H 0.3056 -0.0223 0.0884 0.049 Uiso 1 1 calc R . . C31 C 0.1763(2) 0.04060(11) 0.06915(19) 0.0326(5) Uani 1 1 d . . . C32 C 0.1236(2) 0.03472(12) -0.04425(19) 0.0340(5) Uani 1 1 d . . . C33 C 0.0232(3) 0.06598(13) -0.0983(2) 0.0398(6) Uani 1 1 d . . . H33 H -0.0148 0.0914 -0.0634 0.048 Uiso 1 1 calc R . . C34 C -0.0206(3) 0.05941(14) -0.2043(2) 0.0496(8) Uani 1 1 d . . . H34 H -0.0882 0.0810 -0.2435 0.059 Uiso 1 1 calc R . . C35 C 0.0357(3) 0.02090(16) -0.2516(2) 0.0533(8) Uani 1 1 d . . . H35 H 0.0075 0.0152 -0.3240 0.064 Uiso 1 1 calc R . . C36 C 0.1329(3) -0.00884(17) -0.1920(2) 0.0575(9) Uani 1 1 d . . . H36 H 0.1708 -0.0355 -0.2252 0.069 Uiso 1 1 calc R . . B1 B 0.0615(3) 0.24373(13) 0.7259(2) 0.0307(6) Uani 1 1 d . . . H1 H 0.0271 0.2651 0.7735 0.037 Uiso 1 1 calc R . . 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 0.01880(4) 0.02137(4) 0.02300(4) -0.00267(4) 0.00795(3) -0.00174(3) N1 0.0285(10) 0.0337(11) 0.0268(10) -0.0015(9) 0.0073(8) -0.0015(9) N2 0.0337(11) 0.0306(11) 0.0236(10) -0.0051(8) 0.0095(8) -0.0053(9) N3 0.0206(9) 0.0260(10) 0.0270(10) -0.0034(8) 0.0112(8) -0.0012(7) N4 0.0288(10) 0.0302(10) 0.0275(10) -0.0046(8) 0.0140(8) 0.0002(8) N5 0.0300(10) 0.0253(10) 0.0264(10) -0.0047(8) 0.0118(8) -0.0034(8) N6 0.0358(11) 0.0257(10) 0.0260(10) -0.0065(8) 0.0130(9) -0.0015(8) N7 0.0263(10) 0.0261(10) 0.0241(10) -0.0015(8) 0.0093(8) 0.0031(8) N8 0.0389(11) 0.0272(10) 0.0287(11) -0.0040(8) 0.0147(9) -0.0001(9) N9 0.0593(16) 0.0525(16) 0.0368(13) -0.0113(12) 0.0196(12) 0.0094(13) C1 0.0328(13) 0.0395(15) 0.0302(13) 0.0010(11) 0.0019(11) -0.0027(11) C2 0.0483(17) 0.0479(17) 0.0262(14) 0.0016(12) 0.0034(12) -0.0066(13) C3 0.0488(16) 0.0361(14) 0.0268(13) -0.0032(11) 0.0112(12) -0.0110(12) C4 0.0405(16) 0.068(2) 0.0398(16) 0.0027(15) 0.0015(13) 0.0150(15) C5 0.071(2) 0.0519(19) 0.0297(14) -0.0045(13) 0.0220(15) -0.0050(16) C6 0.0201(10) 0.0294(12) 0.0310(12) -0.0006(10) 0.0072(9) -0.0013(9) C7 0.0208(11) 0.0443(15) 0.0396(14) -0.0026(12) 0.0119(10) -0.0023(10) C8 0.0285(12) 0.0425(15) 0.0345(13) 0.0021(11) 0.0170(11) 0.0038(10) C9 0.0285(12) 0.0324(13) 0.0419(15) -0.0114(11) 0.0098(11) -0.0087(10) C10 0.0410(16) 0.069(2) 0.0478(18) -0.0078(16) 0.0275(14) 0.0044(15) C11 0.0331(12) 0.0275(12) 0.0289(11) -0.0006(10) 0.0092(10) -0.0052(10) C12 0.0506(16) 0.0232(12) 0.0367(14) -0.0025(11) 0.0119(12) -0.0046(11) C13 0.0511(16) 0.0271(13) 0.0360(14) -0.0068(11) 0.0142(13) 0.0001(12) C14 0.0427(14) 0.0319(13) 0.0398(14) 0.0049(12) 0.0188(12) -0.0046(11) C15 0.101(3) 0.0338(16) 0.057(2) -0.0136(15) 0.043(2) 0.0040(17) C16 0.0219(10) 0.0290(13) 0.0383(13) -0.0053(10) 0.0127(10) -0.0043(9) C17 0.0198(10) 0.0321(13) 0.0381(13) -0.0044(11) 0.0109(10) -0.0003(9) C18 0.0236(11) 0.0280(12) 0.0327(13) -0.0023(10) 0.0095(10) 0.0008(9) C19 0.0210(10) 0.0258(11) 0.0302(12) -0.0009(9) 0.0095(9) -0.0016(8) C20 0.0282(13) 0.0419(16) 0.079(2) -0.0087(16) 0.0275(15) -0.0034(12) C21 0.0338(13) 0.0314(14) 0.0584(18) 0.0030(13) 0.0206(13) 0.0060(11) C22 0.0261(10) 0.0205(10) 0.0261(11) -0.0032(9) 0.0110(9) -0.0016(9) C23 0.0318(12) 0.0266(12) 0.0311(12) 0.0001(10) 0.0121(10) 0.0057(10) C24 0.0368(14) 0.0335(13) 0.0319(13) 0.0041(11) 0.0091(11) 0.0117(11) C25 0.0440(15) 0.0381(14) 0.0243(12) 0.0004(10) 0.0083(11) 0.0103(12) C26 0.0329(12) 0.0291(12) 0.0258(12) -0.0026(10) 0.0116(10) 0.0012(10) C27 0.0362(13) 0.0310(13) 0.0281(12) -0.0047(10) 0.0138(11) 0.0011(10) C28 0.0422(15) 0.0506(17) 0.0303(14) -0.0080(12) 0.0087(12) 0.0113(13) C29 0.0426(16) 0.0532(19) 0.0407(16) -0.0081(14) 0.0096(13) 0.0156(14) C30 0.0434(15) 0.0419(16) 0.0413(15) -0.0097(13) 0.0189(13) 0.0083(12) C31 0.0414(14) 0.0290(12) 0.0311(12) -0.0051(10) 0.0167(11) -0.0028(11) C32 0.0472(15) 0.0283(13) 0.0307(13) -0.0047(10) 0.0184(11) -0.0038(11) C33 0.0563(17) 0.0326(14) 0.0322(14) -0.0022(11) 0.0168(13) 0.0013(13) C34 0.069(2) 0.0409(17) 0.0347(15) 0.0058(13) 0.0104(15) 0.0018(15) C35 0.082(2) 0.054(2) 0.0264(14) -0.0043(13) 0.0211(16) -0.0040(18) C36 0.078(2) 0.065(2) 0.0343(16) -0.0120(15) 0.0248(17) 0.0096(19) B1 0.0368(15) 0.0316(14) 0.0278(14) -0.0062(11) 0.0160(12) -0.0021(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C22 1.944(2) . ? Ir1 C19 2.073(2) . ? Ir1 C16 2.076(2) . ? Ir1 N5 2.148(2) . ? Ir1 N3 2.1635(18) . ? Ir1 N1 2.183(2) . ? N1 C1 1.342(3) . ? N1 N2 1.380(3) . ? N2 C3 1.355(3) . ? N2 B1 1.529(4) . ? N3 C6 1.344(3) . ? N3 N4 1.369(3) . ? N4 C8 1.347(3) . ? N4 B1 1.546(4) . ? N5 C11 1.352(3) . ? N5 N6 1.379(3) . ? N6 C13 1.355(3) . ? N6 B1 1.535(4) . ? N7 C26 1.365(3) . ? N7 C22 1.373(3) . ? N7 H7N 0.882(17) . ? N8 C31 1.343(3) . ? N8 C27 1.345(3) . ? N9 C36 1.337(4) . ? N9 C32 1.340(3) . ? C1 C2 1.402(4) . ? C1 C4 1.488(4) . ? C2 C3 1.359(4) . ? C2 H2 0.9500 . ? C3 C5 1.499(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.396(3) . ? C6 C9 1.489(3) . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 C10 1.503(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.397(4) . ? C11 C14 1.489(4) . ? C12 C13 1.365(4) . ? C12 H12 0.9500 . ? C13 C15 1.499(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.503(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.342(3) . ? C17 C20 1.497(3) . ? C18 C21 1.495(3) . ? C18 C19 1.506(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.425(3) . ? C23 C24 1.366(4) . ? C23 H23 0.9500 . ? C24 C25 1.405(4) . ? C24 H24 0.9500 . ? C25 C26 1.368(4) . ? C25 H25 0.9500 . ? C26 C27 1.486(3) . ? C27 C28 1.391(4) . ? C28 C29 1.395(4) . ? C28 H28 0.9500 . ? C29 C30 1.378(4) . ? C29 H29 0.9500 . ? C30 C31 1.393(4) . ? C30 H30 0.9500 . ? C31 C32 1.486(3) . ? C32 C33 1.385(4) . ? C33 C34 1.387(4) . ? C33 H33 0.9500 . ? C34 C35 1.379(5) . ? C34 H34 0.9500 . ? C35 C36 1.364(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? B1 H1 1.0000 . ? 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 C22 Ir1 C19 89.86(9) . . ? C22 Ir1 C16 90.10(10) . . ? C19 Ir1 C16 82.39(9) . . ? C22 Ir1 N5 93.84(8) . . ? C19 Ir1 N5 175.79(8) . . ? C16 Ir1 N5 95.57(8) . . ? C22 Ir1 N3 90.07(8) . . ? C19 Ir1 N3 95.21(8) . . ? C16 Ir1 N3 177.59(8) . . ? N5 Ir1 N3 86.82(7) . . ? C22 Ir1 N1 176.38(8) . . ? C19 Ir1 N1 90.64(9) . . ? C16 Ir1 N1 93.52(9) . . ? N5 Ir1 N1 85.80(8) . . ? N3 Ir1 N1 86.31(8) . . ? C1 N1 N2 106.1(2) . . ? C1 N1 Ir1 137.68(18) . . ? N2 N1 Ir1 115.59(15) . . ? C3 N2 N1 110.1(2) . . ? C3 N2 B1 129.0(2) . . ? N1 N2 B1 120.95(19) . . ? C6 N3 N4 106.80(18) . . ? C6 N3 Ir1 135.16(16) . . ? N4 N3 Ir1 117.93(14) . . ? C8 N4 N3 110.2(2) . . ? C8 N4 B1 130.7(2) . . ? N3 N4 B1 119.09(18) . . ? C11 N5 N6 106.50(19) . . ? C11 N5 Ir1 136.43(17) . . ? N6 N5 Ir1 116.96(14) . . ? C13 N6 N5 109.3(2) . . ? C13 N6 B1 130.3(2) . . ? N5 N6 B1 120.40(19) . . ? C26 N7 C22 127.4(2) . . ? C26 N7 H7N 118.7(18) . . ? C22 N7 H7N 113.8(18) . . ? C31 N8 C27 118.3(2) . . ? C36 N9 C32 117.1(3) . . ? N1 C1 C2 109.3(3) . . ? N1 C1 C4 124.8(3) . . ? C2 C1 C4 125.9(3) . . ? C3 C2 C1 106.9(2) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? N2 C3 C2 107.5(2) . . ? N2 C3 C5 122.7(3) . . ? C2 C3 C5 129.8(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 109.0(2) . . ? N3 C6 C9 123.9(2) . . ? C7 C6 C9 127.1(2) . . ? C8 C7 C6 106.6(2) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N4 C8 C7 107.4(2) . . ? N4 C8 C10 122.6(3) . . ? C7 C8 C10 129.9(2) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 109.3(2) . . ? N5 C11 C14 122.8(2) . . ? C12 C11 C14 127.8(2) . . ? C13 C12 C11 106.4(2) . . ? C13 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? N6 C13 C12 108.4(2) . . ? N6 C13 C15 122.1(3) . . ? C12 C13 C15 129.5(3) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 Ir1 111.12(15) . . ? C17 C16 H16A 109.4 . . ? Ir1 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? Ir1 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C20 126.1(2) . . ? C18 C17 C16 117.6(2) . . ? C20 C17 C16 116.2(2) . . ? C17 C18 C21 125.2(2) . . ? C17 C18 C19 117.4(2) . . ? C21 C18 C19 117.4(2) . . ? C18 C19 Ir1 111.24(16) . . ? C18 C19 H19A 109.4 . . ? Ir1 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? Ir1 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 112.9(2) . . ? N7 C22 Ir1 120.69(17) . . ? C23 C22 Ir1 126.33(17) . . ? C24 C23 C22 122.0(2) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 120.8(2) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.0(2) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N7 C26 C25 117.8(2) . . ? N7 C26 C27 117.6(2) . . ? C25 C26 C27 124.5(2) . . ? N8 C27 C28 122.5(2) . . ? N8 C27 C26 114.8(2) . . ? C28 C27 C26 122.6(2) . . ? C27 C28 C29 118.6(3) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 119.0(3) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 119.0(2) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? N8 C31 C30 122.6(2) . . ? N8 C31 C32 116.6(2) . . ? C30 C31 C32 120.8(2) . . ? N9 C32 C33 122.6(2) . . ? N9 C32 C31 115.9(2) . . ? C33 C32 C31 121.5(2) . . ? C34 C33 C32 118.8(3) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 118.7(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C36 C35 C34 118.5(3) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? N9 C36 C35 124.3(3) . . ? N9 C36 H36 117.9 . . ? C35 C36 H36 117.9 . . ? N2 B1 N6 110.2(2) . . ? N2 B1 N4 108.6(2) . . ? N6 B1 N4 110.0(2) . . ? N2 B1 H1 109.4 . . ? N6 B1 H1 109.4 . . ? N4 B1 H1 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Ir1 N1 C1 35.7(3) . . . . ? C16 Ir1 N1 C1 -46.7(3) . . . . ? N5 Ir1 N1 C1 -142.0(3) . . . . ? N3 Ir1 N1 C1 130.9(3) . . . . ? C19 Ir1 N1 N2 -133.74(17) . . . . ? C16 Ir1 N1 N2 143.85(17) . . . . ? N5 Ir1 N1 N2 48.51(16) . . . . ? N3 Ir1 N1 N2 -38.56(16) . . . . ? C1 N1 N2 C3 -1.6(3) . . . . ? Ir1 N1 N2 C3 171.05(17) . . . . ? C1 N1 N2 B1 178.9(2) . . . . ? Ir1 N1 N2 B1 -8.4(3) . . . . ? C22 Ir1 N3 C6 41.7(2) . . . . ? C19 Ir1 N3 C6 -48.2(2) . . . . ? N5 Ir1 N3 C6 135.5(2) . . . . ? N1 Ir1 N3 C6 -138.5(2) . . . . ? C22 Ir1 N3 N4 -134.01(17) . . . . ? C19 Ir1 N3 N4 136.12(17) . . . . ? N5 Ir1 N3 N4 -40.17(16) . . . . ? N1 Ir1 N3 N4 45.82(17) . . . . ? C6 N3 N4 C8 0.7(3) . . . . ? Ir1 N3 N4 C8 177.48(16) . . . . ? C6 N3 N4 B1 178.4(2) . . . . ? Ir1 N3 N4 B1 -4.8(3) . . . . ? C22 Ir1 N5 C11 -50.3(2) . . . . ? C16 Ir1 N5 C11 40.2(3) . . . . ? N3 Ir1 N5 C11 -140.1(2) . . . . ? N1 Ir1 N5 C11 133.3(2) . . . . ? C22 Ir1 N5 N6 134.06(17) . . . . ? C16 Ir1 N5 N6 -135.46(17) . . . . ? N3 Ir1 N5 N6 44.20(16) . . . . ? N1 Ir1 N5 N6 -42.33(16) . . . . ? C11 N5 N6 C13 -0.4(3) . . . . ? Ir1 N5 N6 C13 176.47(17) . . . . ? C11 N5 N6 B1 179.7(2) . . . . ? Ir1 N5 N6 B1 -3.4(3) . . . . ? N2 N1 C1 C2 1.0(3) . . . . ? Ir1 N1 C1 C2 -169.1(2) . . . . ? N2 N1 C1 C4 -179.2(3) . . . . ? Ir1 N1 C1 C4 10.7(5) . . . . ? N1 C1 C2 C3 -0.1(3) . . . . ? C4 C1 C2 C3 -179.9(3) . . . . ? N1 N2 C3 C2 1.6(3) . . . . ? B1 N2 C3 C2 -179.0(3) . . . . ? N1 N2 C3 C5 -176.6(2) . . . . ? B1 N2 C3 C5 2.8(4) . . . . ? C1 C2 C3 N2 -0.9(3) . . . . ? C1 C2 C3 C5 177.1(3) . . . . ? N4 N3 C6 C7 -0.5(3) . . . . ? Ir1 N3 C6 C7 -176.55(18) . . . . ? N4 N3 C6 C9 179.6(2) . . . . ? Ir1 N3 C6 C9 3.6(4) . . . . ? N3 C6 C7 C8 0.2(3) . . . . ? C9 C6 C7 C8 -180.0(3) . . . . ? N3 N4 C8 C7 -0.5(3) . . . . ? B1 N4 C8 C7 -177.9(3) . . . . ? N3 N4 C8 C10 178.1(2) . . . . ? B1 N4 C8 C10 0.7(4) . . . . ? C6 C7 C8 N4 0.2(3) . . . . ? C6 C7 C8 C10 -178.3(3) . . . . ? N6 N5 C11 C12 0.6(3) . . . . ? Ir1 N5 C11 C12 -175.42(18) . . . . ? N6 N5 C11 C14 -179.7(2) . . . . ? Ir1 N5 C11 C14 4.3(4) . . . . ? N5 C11 C12 C13 -0.5(3) . . . . ? C14 C11 C12 C13 179.8(3) . . . . ? N5 N6 C13 C12 0.1(3) . . . . ? B1 N6 C13 C12 180.0(3) . . . . ? N5 N6 C13 C15 179.7(3) . . . . ? B1 N6 C13 C15 -0.5(5) . . . . ? C11 C12 C13 N6 0.2(3) . . . . ? C11 C12 C13 C15 -179.3(3) . . . . ? C22 Ir1 C16 C17 -85.85(19) . . . . ? C19 Ir1 C16 C17 4.00(18) . . . . ? N5 Ir1 C16 C17 -179.71(18) . . . . ? N1 Ir1 C16 C17 94.17(18) . . . . ? Ir1 C16 C17 C18 -4.3(3) . . . . ? Ir1 C16 C17 C20 178.7(2) . . . . ? C20 C17 C18 C21 0.3(5) . . . . ? C16 C17 C18 C21 -176.4(2) . . . . ? C20 C17 C18 C19 178.3(3) . . . . ? C16 C17 C18 C19 1.6(4) . . . . ? C17 C18 C19 Ir1 1.8(3) . . . . ? C21 C18 C19 Ir1 -179.93(19) . . . . ? C22 Ir1 C19 C18 86.89(17) . . . . ? C16 Ir1 C19 C18 -3.23(17) . . . . ? N3 Ir1 C19 C18 176.95(16) . . . . ? N1 Ir1 C19 C18 -96.70(17) . . . . ? C26 N7 C22 C23 -4.5(3) . . . . ? C26 N7 C22 Ir1 171.71(19) . . . . ? C19 Ir1 C22 N7 -37.44(19) . . . . ? C16 Ir1 C22 N7 44.95(19) . . . . ? N5 Ir1 C22 N7 140.54(18) . . . . ? N3 Ir1 C22 N7 -132.65(18) . . . . ? C19 Ir1 C22 C23 138.2(2) . . . . ? C16 Ir1 C22 C23 -139.4(2) . . . . ? N5 Ir1 C22 C23 -43.8(2) . . . . ? N3 Ir1 C22 C23 43.0(2) . . . . ? N7 C22 C23 C24 4.1(3) . . . . ? Ir1 C22 C23 C24 -171.9(2) . . . . ? C22 C23 C24 C25 -1.6(4) . . . . ? C23 C24 C25 C26 -1.2(4) . . . . ? C22 N7 C26 C25 2.0(4) . . . . ? C22 N7 C26 C27 -174.4(2) . . . . ? C24 C25 C26 N7 1.1(4) . . . . ? C24 C25 C26 C27 177.3(3) . . . . ? C31 N8 C27 C28 0.5(4) . . . . ? C31 N8 C27 C26 -178.1(2) . . . . ? N7 C26 C27 N8 -176.9(2) . . . . ? C25 C26 C27 N8 6.9(4) . . . . ? N7 C26 C27 C28 4.5(4) . . . . ? C25 C26 C27 C28 -171.7(3) . . . . ? N8 C27 C28 C29 -0.5(5) . . . . ? C26 C27 C28 C29 178.0(3) . . . . ? C27 C28 C29 C30 0.6(5) . . . . ? C28 C29 C30 C31 -0.7(5) . . . . ? C27 N8 C31 C30 -0.6(4) . . . . ? C27 N8 C31 C32 179.2(2) . . . . ? C29 C30 C31 N8 0.7(4) . . . . ? C29 C30 C31 C32 -179.1(3) . . . . ? C36 N9 C32 C33 1.0(5) . . . . ? C36 N9 C32 C31 -179.7(3) . . . . ? N8 C31 C32 N9 176.0(2) . . . . ? C30 C31 C32 N9 -4.2(4) . . . . ? N8 C31 C32 C33 -4.7(4) . . . . ? C30 C31 C32 C33 175.2(3) . . . . ? N9 C32 C33 C34 -1.8(4) . . . . ? C31 C32 C33 C34 178.9(3) . . . . ? C32 C33 C34 C35 1.5(5) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C32 N9 C36 C35 0.2(5) . . . . ? C34 C35 C36 N9 -0.4(6) . . . . ? C3 N2 B1 N6 126.8(3) . . . . ? N1 N2 B1 N6 -53.8(3) . . . . ? C3 N2 B1 N4 -112.7(3) . . . . ? N1 N2 B1 N4 66.7(3) . . . . ? C13 N6 B1 N2 -118.1(3) . . . . ? N5 N6 B1 N2 61.8(3) . . . . ? C13 N6 B1 N4 122.3(3) . . . . ? N5 N6 B1 N4 -57.9(3) . . . . ? C8 N4 B1 N2 119.2(3) . . . . ? N3 N4 B1 N2 -58.0(3) . . . . ? C8 N4 B1 N6 -120.2(3) . . . . ? N3 N4 B1 N6 62.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.193 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.087 ###END #========================================================================= # Data for compound 2_T (local labelling ea03808a) #========================================================================= data_2_T _database_code_depnum_ccdc_archive 'CCDC 731546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H43 B Ir N9), C4 H10 O' _chemical_formula_sum 'C76 H96 B2 Ir2 N18 O' _chemical_formula_weight 1683.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2938(15) _cell_length_b 11.8722(17) _cell_length_c 16.064(2) _cell_angle_alpha 100.103(4) _cell_angle_beta 102.473(3) _cell_angle_gamma 95.845(3) _cell_volume 1867.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9872 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.74 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 3.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5509 _exptl_absorpt_correction_T_max 0.7038 _exptl_absorpt_process_details ; SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 223(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-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 44999 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.77 _reflns_number_total 7919 _reflns_number_gt 6146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker (2006). APEX 2. Version 2.1.' _computing_cell_refinement 'Bruker (2006). APEX 2. Version 2.1.' _computing_data_reduction 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_solution 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2003)' _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. The asymmetric unit of the structure is formed by one mononuclear Ir(III) complex 2 and a half solvation diethyl ether molecule. In this triclinic polymorph crystal form of 2, on the contrary to the monoclinic crystal form, the polypyridine moiety occupies an adjacent region of the space to that of the Tp^Me2^ ligand and features a cis-trans conformation of the pyridine rings. The solvent diethyl ether molecule was observed close a crystallographic inversion centre. In this way, there are no atoms on the special position, but nevertheless the diethyl ether molecule is disordered around the inversion centre in a 1:1 ratio. Therefore in the refinement the disordered atoms have been flanked by PART -1 and PART 0 and the site occupation factors fixed to 0.5, taking into account the multiplicity of this special position. Several geometric restraints (DFIX commands) were needed to maintain a reasonable molecular geometry and other restraints (SIMU, DELU) have been used to make the ADP values of the disordered atoms more reasonable All the non-hydrogen atoms were refined with anisotropic displacement parameters. Some few reflections to low angle that present values very below their calculated values, possibly partially covered for "beam stopper" were eliminated at the end of the refinement (OMIT command). The hydrogen atoms bonded to the nitrogen atoms were located from the difference Fourier synthesis and refined isotropically with geometric restraints. The other hydrogen atoms were placed in calculated positions and refined with isotropic displacement parameters by using a riding model. ; _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^)+(0.0632P)^2^+9.5263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7919 _refine_ls_number_parameters 480 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _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 0.36654(3) 0.75562(2) 0.22552(2) 0.03258(11) Uani 1 1 d . . . N1 N 0.2147(6) 0.8392(5) 0.2809(4) 0.0375(14) Uani 1 1 d . . . N2 N 0.2352(6) 0.9592(5) 0.3001(4) 0.0380(15) Uani 1 1 d . . . N3 N 0.3637(6) 0.8871(5) 0.1482(4) 0.0356(14) Uani 1 1 d . . . N4 N 0.3617(6) 0.9999(5) 0.1880(4) 0.0345(14) Uani 1 1 d . . . N5 N 0.5161(6) 0.8821(6) 0.3234(4) 0.0408(15) Uani 1 1 d . . . N6 N 0.4862(7) 0.9932(5) 0.3419(4) 0.0398(15) Uani 1 1 d . . . N7 N 0.6112(7) 0.7654(5) 0.1677(4) 0.0366(14) Uani 1 1 d D . . H7N H 0.616(9) 0.842(2) 0.182(5) 0.044 Uiso 1 1 d D . . N8 N 0.7819(6) 0.9413(6) 0.1638(4) 0.0414(16) Uani 1 1 d . . . N9 N 0.9061(8) 1.2459(7) 0.1990(6) 0.061(2) Uani 1 1 d . . . C1 C 0.1007(8) 0.8069(7) 0.3038(6) 0.0395(18) Uani 1 1 d . . . C2 C 0.0494(8) 0.9044(7) 0.3367(6) 0.0432(19) Uani 1 1 d . . . H2 H -0.0297 0.9056 0.3569 0.052 Uiso 1 1 calc R . . C3 C 0.1357(8) 0.9979(7) 0.3340(5) 0.0362(17) Uani 1 1 d . . . C4 C 0.0396(9) 0.6838(7) 0.2935(7) 0.056(3) Uani 1 1 d . . . H4A H 0.0363 0.6419 0.2353 0.084 Uiso 1 1 calc R . . H4B H -0.0509 0.6814 0.3023 0.084 Uiso 1 1 calc R . . H4C H 0.0937 0.6483 0.3360 0.084 Uiso 1 1 calc R . . C5 C 0.1287(10) 1.1242(7) 0.3627(6) 0.051(2) Uani 1 1 d . . . H5A H 0.2086 1.1595 0.4077 0.077 Uiso 1 1 calc R . . H5B H 0.0496 1.1328 0.3855 0.077 Uiso 1 1 calc R . . H5C H 0.1236 1.1619 0.3134 0.077 Uiso 1 1 calc R . . C6 C 0.3614(7) 0.8879(7) 0.0645(5) 0.0359(16) Uani 1 1 d . . . C7 C 0.3563(8) 1.0011(7) 0.0507(5) 0.0393(18) Uani 1 1 d . . . H7 H 0.3532 1.0257 -0.0022 0.047 Uiso 1 1 calc R . . C8 C 0.3565(8) 1.0688(6) 0.1294(6) 0.0385(18) Uani 1 1 d . . . C9 C 0.3603(10) 0.7825(7) -0.0013(6) 0.049(2) Uani 1 1 d . . . H9A H 0.3958 0.7234 0.0280 0.074 Uiso 1 1 calc R . . H9B H 0.4156 0.8012 -0.0402 0.074 Uiso 1 1 calc R . . H9C H 0.2688 0.7541 -0.0345 0.074 Uiso 1 1 calc R . . C10 C 0.3442(10) 1.1955(7) 0.1480(7) 0.055(2) Uani 1 1 d . . . H10A H 0.2574 1.2051 0.1604 0.083 Uiso 1 1 calc R . . H10B H 0.3522 1.2281 0.0977 0.083 Uiso 1 1 calc R . . H10C H 0.4151 1.2351 0.1979 0.083 Uiso 1 1 calc R . . C11 C 0.6287(8) 0.8767(8) 0.3821(6) 0.048(2) Uani 1 1 d . . . C12 C 0.6705(10) 0.9841(9) 0.4379(6) 0.057(3) Uani 1 1 d . . . H12 H 0.7475 1.0046 0.4842 0.069 Uiso 1 1 calc R . . C13 C 0.5783(9) 1.0545(8) 0.4127(6) 0.049(2) Uani 1 1 d . . . C14 C 0.6921(10) 0.7702(9) 0.3848(7) 0.061(3) Uani 1 1 d . . . H14A H 0.6456 0.7204 0.4143 0.091 Uiso 1 1 calc R . . H14B H 0.7858 0.7907 0.4159 0.091 Uiso 1 1 calc R . . H14C H 0.6862 0.7298 0.3258 0.091 Uiso 1 1 calc R . . C15 C 0.5719(12) 1.1749(8) 0.4555(7) 0.070(3) Uani 1 1 d . . . H15A H 0.6256 1.2289 0.4332 0.105 Uiso 1 1 calc R . . H15B H 0.6066 1.1849 0.5179 0.105 Uiso 1 1 calc R . . H15C H 0.4793 1.1893 0.4435 0.105 Uiso 1 1 calc R . . C16 C 0.3597(9) 0.6279(7) 0.2984(6) 0.045(2) Uani 1 1 d . . . H16A H 0.4500 0.6075 0.3162 0.054 Uiso 1 1 calc R . . H16B H 0.3307 0.6579 0.3512 0.054 Uiso 1 1 calc R . . C17 C 0.2636(8) 0.5203(7) 0.2470(6) 0.042(2) Uani 1 1 d . . . C18 C 0.1977(8) 0.5222(6) 0.1666(6) 0.0421(19) Uani 1 1 d . . . C19 C 0.2203(8) 0.6343(7) 0.1343(5) 0.0413(18) Uani 1 1 d . . . H19A H 0.1357 0.6663 0.1228 0.050 Uiso 1 1 calc R . . H19B H 0.2487 0.6178 0.0795 0.050 Uiso 1 1 calc R . . C20 C 0.2496(11) 0.4217(8) 0.2945(7) 0.060(3) Uani 1 1 d . . . H20A H 0.1834 0.3590 0.2572 0.090 Uiso 1 1 calc R . . H20B H 0.2210 0.4486 0.3473 0.090 Uiso 1 1 calc R . . H20C H 0.3356 0.3943 0.3093 0.090 Uiso 1 1 calc R . . C21 C 0.1009(11) 0.4268(8) 0.1040(7) 0.062(3) Uani 1 1 d . . . H21A H 0.1318 0.4082 0.0509 0.093 Uiso 1 1 calc R . . H21B H 0.0129 0.4512 0.0905 0.093 Uiso 1 1 calc R . . H21C H 0.0949 0.3590 0.1297 0.093 Uiso 1 1 calc R . . C22 C 0.5069(7) 0.6906(6) 0.1774(5) 0.0362(17) Uani 1 1 d . . . C23 C 0.5171(8) 0.5724(7) 0.1465(6) 0.0421(19) Uani 1 1 d . . . H23 H 0.4502 0.5143 0.1497 0.050 Uiso 1 1 calc R . . C24 C 0.6215(10) 0.5420(8) 0.1126(6) 0.053(2) Uani 1 1 d . . . H24 H 0.6259 0.4631 0.0942 0.063 Uiso 1 1 calc R . . C25 C 0.7232(9) 0.6248(8) 0.1042(6) 0.051(2) Uani 1 1 d . . . H25 H 0.7947 0.6031 0.0801 0.061 Uiso 1 1 calc R . . C26 C 0.7133(8) 0.7365(7) 0.1322(5) 0.0401(18) Uani 1 1 d . . . C27 C 0.8123(8) 0.8368(8) 0.1296(6) 0.0437(19) Uani 1 1 d . . . C28 C 0.9260(8) 0.8279(9) 0.0949(6) 0.052(2) Uani 1 1 d . . . H28 H 0.9462 0.7552 0.0717 0.063 Uiso 1 1 calc R . . C29 C 1.0053(9) 0.9258(10) 0.0955(7) 0.060(3) Uani 1 1 d . . . H29 H 1.0816 0.9210 0.0725 0.072 Uiso 1 1 calc R . . C30 C 0.9768(9) 1.0326(10) 0.1291(6) 0.059(3) Uani 1 1 d . . . H30 H 1.0317 1.1006 0.1285 0.070 Uiso 1 1 calc R . . C31 C 0.8636(7) 1.0374(8) 0.1642(6) 0.0433(19) Uani 1 1 d . . . C32 C 0.8280(8) 1.1504(8) 0.2031(6) 0.046(2) Uani 1 1 d . . . C33 C 0.7188(10) 1.1561(9) 0.2395(7) 0.059(3) Uani 1 1 d . . . H33 H 0.6658 1.0879 0.2418 0.071 Uiso 1 1 calc R . . C34 C 0.6876(11) 1.2623(9) 0.2727(7) 0.065(3) Uani 1 1 d . . . H34 H 0.6135 1.2679 0.2978 0.079 Uiso 1 1 calc R . . C35 C 0.7690(13) 1.3614(10) 0.2679(8) 0.074(3) Uani 1 1 d . . . H35 H 0.7511 1.4356 0.2896 0.088 Uiso 1 1 calc R . . C36 C 0.8739(11) 1.3474(9) 0.2313(8) 0.070(3) Uani 1 1 d . . . H36 H 0.9284 1.4144 0.2284 0.084 Uiso 1 1 calc R . . B1 B 0.3605(9) 1.0273(7) 0.2850(6) 0.039(2) Uani 1 1 d . . . H1 H 0.3589 1.1111 0.3033 0.047 Uiso 1 1 calc R . . O1 O 0.163(4) 0.551(3) 0.512(2) 0.174(10) Uani 0.50 1 d PDU A -1 C37 C 0.023(5) 0.504(4) 0.504(11) 0.189(13) Uani 0.50 1 d PDU A -1 H37A H -0.0197 0.4555 0.4469 0.227 Uiso 0.50 1 calc PR A -1 H37B H 0.0116 0.4635 0.5506 0.227 Uiso 0.50 1 calc PR A -1 C38 C -0.018(8) 0.618(5) 0.516(4) 0.26(3) Uani 0.50 1 d PDU A -1 H38A H 0.0498 0.6737 0.5054 0.391 Uiso 0.50 1 calc PR A -1 H38B H -0.0286 0.6410 0.5745 0.391 Uiso 0.50 1 calc PR A -1 H38C H -0.1029 0.6163 0.4746 0.391 Uiso 0.50 1 calc PR A -1 C39 C 0.237(5) 0.456(4) 0.518(3) 0.181(14) Uani 0.50 1 d PDU A -1 H39A H 0.2070 0.3954 0.4654 0.218 Uiso 0.50 1 calc PR A -1 H39B H 0.2262 0.4226 0.5684 0.218 Uiso 0.50 1 calc PR A -1 C40 C 0.378(5) 0.504(4) 0.529(4) 0.206(19) Uani 0.50 1 d PDU A -1 H40A H 0.3841 0.5530 0.4871 0.309 Uiso 0.50 1 calc PR A -1 H40B H 0.4307 0.4420 0.5199 0.309 Uiso 0.50 1 calc PR A -1 H40C H 0.4128 0.5502 0.5876 0.309 Uiso 0.50 1 calc PR A -1 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 0.02820(16) 0.02611(15) 0.04080(18) 0.00216(11) 0.01167(12) -0.00753(10) N1 0.028(3) 0.034(3) 0.049(4) 0.004(3) 0.011(3) 0.002(3) N2 0.037(3) 0.030(3) 0.044(4) 0.001(3) 0.014(3) -0.002(3) N3 0.029(3) 0.030(3) 0.049(4) 0.007(3) 0.014(3) -0.001(2) N4 0.032(3) 0.026(3) 0.044(4) 0.003(3) 0.014(3) -0.005(2) N5 0.032(3) 0.044(4) 0.041(4) 0.001(3) 0.010(3) -0.009(3) N6 0.039(4) 0.031(3) 0.042(4) -0.008(3) 0.016(3) -0.013(3) N7 0.035(3) 0.029(3) 0.045(4) 0.002(3) 0.015(3) -0.002(3) N8 0.028(3) 0.048(4) 0.046(4) 0.009(3) 0.009(3) -0.005(3) N9 0.043(4) 0.048(5) 0.087(6) 0.014(4) 0.016(4) -0.018(3) C1 0.030(4) 0.039(4) 0.050(5) 0.011(4) 0.013(3) -0.006(3) C2 0.032(4) 0.048(5) 0.049(5) 0.004(4) 0.017(4) -0.003(3) C3 0.035(4) 0.036(4) 0.038(4) 0.004(3) 0.012(3) 0.003(3) C4 0.042(5) 0.040(5) 0.093(8) 0.015(5) 0.036(5) -0.006(4) C5 0.056(5) 0.041(5) 0.058(6) 0.002(4) 0.024(5) 0.010(4) C6 0.030(4) 0.038(4) 0.038(4) 0.004(3) 0.011(3) -0.001(3) C7 0.035(4) 0.040(4) 0.045(5) 0.013(4) 0.012(3) -0.001(3) C8 0.031(4) 0.031(4) 0.056(5) 0.010(4) 0.017(4) -0.002(3) C9 0.060(6) 0.041(4) 0.042(5) 0.001(4) 0.015(4) -0.002(4) C10 0.063(6) 0.034(4) 0.075(7) 0.015(4) 0.028(5) 0.008(4) C11 0.036(4) 0.060(5) 0.041(5) 0.004(4) 0.006(4) -0.014(4) C12 0.048(5) 0.063(6) 0.046(5) 0.002(5) 0.004(4) -0.025(5) C13 0.045(5) 0.052(5) 0.044(5) -0.003(4) 0.018(4) -0.020(4) C14 0.042(5) 0.070(7) 0.060(6) 0.011(5) 0.000(4) -0.004(5) C15 0.083(8) 0.053(6) 0.057(6) -0.019(5) 0.022(6) -0.029(5) C16 0.046(5) 0.038(4) 0.052(5) 0.005(4) 0.018(4) -0.001(4) C17 0.043(4) 0.030(4) 0.062(6) 0.011(4) 0.028(4) 0.003(3) C18 0.039(4) 0.028(4) 0.058(5) 0.002(4) 0.019(4) -0.010(3) C19 0.037(4) 0.038(4) 0.041(4) -0.004(3) 0.008(3) -0.010(3) C20 0.072(7) 0.035(4) 0.076(7) 0.013(4) 0.028(6) -0.003(4) C21 0.073(7) 0.040(5) 0.065(6) -0.001(4) 0.024(5) -0.023(5) C22 0.030(4) 0.032(4) 0.040(4) 0.010(3) 0.000(3) -0.011(3) C23 0.042(4) 0.031(4) 0.051(5) 0.002(3) 0.017(4) -0.004(3) C24 0.067(6) 0.036(4) 0.057(6) 0.005(4) 0.018(5) 0.009(4) C25 0.041(5) 0.055(5) 0.064(6) 0.011(5) 0.028(4) 0.011(4) C26 0.034(4) 0.044(4) 0.041(5) 0.006(4) 0.011(3) 0.002(3) C27 0.026(4) 0.059(5) 0.045(5) 0.012(4) 0.009(3) -0.001(4) C28 0.033(4) 0.066(6) 0.060(6) 0.012(5) 0.018(4) 0.007(4) C29 0.031(4) 0.086(8) 0.063(6) 0.011(5) 0.020(4) -0.006(5) C30 0.034(5) 0.080(7) 0.059(6) 0.014(5) 0.014(4) -0.011(5) C31 0.023(4) 0.056(5) 0.048(5) 0.016(4) 0.005(3) -0.012(3) C32 0.035(4) 0.048(5) 0.054(5) 0.020(4) 0.005(4) -0.010(4) C33 0.052(6) 0.054(6) 0.068(6) 0.011(5) 0.021(5) -0.016(4) C34 0.060(6) 0.059(6) 0.076(7) 0.005(5) 0.028(5) -0.006(5) C35 0.082(8) 0.054(6) 0.085(8) 0.015(6) 0.023(7) 0.000(6) C36 0.062(7) 0.053(6) 0.090(8) 0.010(6) 0.021(6) -0.015(5) B1 0.038(5) 0.028(4) 0.050(5) 0.000(4) 0.017(4) -0.005(4) O1 0.23(2) 0.15(2) 0.144(18) 0.067(18) 0.03(2) 0.023(19) C37 0.24(3) 0.16(3) 0.17(3) 0.04(3) 0.05(4) 0.02(2) C38 0.32(4) 0.25(4) 0.24(5) 0.09(4) 0.04(4) 0.14(4) C39 0.24(3) 0.17(3) 0.13(2) 0.06(2) 0.02(3) 0.04(2) C40 0.23(3) 0.15(4) 0.20(4) 0.03(3) -0.02(4) 0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C22 1.945(8) . ? Ir1 C16 2.076(8) . ? Ir1 C19 2.087(7) . ? Ir1 N3 2.157(6) . ? Ir1 N5 2.179(6) . ? Ir1 N1 2.196(6) . ? N1 C1 1.343(9) . ? N1 N2 1.388(9) . ? N2 C3 1.344(10) . ? N2 B1 1.538(10) . ? N3 C6 1.342(10) . ? N3 N4 1.385(8) . ? N4 C8 1.348(10) . ? N4 B1 1.537(11) . ? N5 C11 1.343(11) . ? N5 N6 1.381(9) . ? N6 C13 1.352(11) . ? N6 B1 1.549(12) . ? N7 C26 1.345(10) . ? N7 C22 1.375(9) . ? N7 H7N 0.90(2) . ? N8 C31 1.345(10) . ? N8 C27 1.361(11) . ? N9 C36 1.329(14) . ? N9 C32 1.342(10) . ? C1 C2 1.389(12) . ? C1 C4 1.497(11) . ? C2 C3 1.362(11) . ? C2 H2 0.9400 . ? C3 C5 1.504(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.404(11) . ? C6 C9 1.487(11) . ? C7 C8 1.373(11) . ? C7 H7 0.9400 . ? C8 C10 1.506(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.391(13) . ? C11 C14 1.484(14) . ? C12 C13 1.370(14) . ? C12 H12 0.9400 . ? C13 C15 1.488(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.520(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.327(13) . ? C17 C20 1.517(11) . ? C18 C21 1.492(12) . ? C18 C19 1.526(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.427(11) . ? C23 C24 1.357(12) . ? C23 H23 0.9400 . ? C24 C25 1.407(13) . ? C24 H24 0.9400 . ? C25 C26 1.345(12) . ? C25 H25 0.9400 . ? C26 C27 1.499(11) . ? C27 C28 1.407(11) . ? C28 C29 1.348(13) . ? C28 H28 0.9400 . ? C29 C30 1.374(15) . ? C29 H29 0.9400 . ? C30 C31 1.402(12) . ? C30 H30 0.9400 . ? C31 C32 1.493(13) . ? C32 C33 1.377(13) . ? C33 C34 1.376(14) . ? C33 H33 0.9400 . ? C34 C35 1.397(14) . ? C34 H34 0.9400 . ? C35 C36 1.348(16) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? B1 H1 0.9900 . ? O1 C39 1.431(19) . ? O1 C37 1.45(2) . ? C37 C38 1.45(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.47(2) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? 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 C22 Ir1 C16 90.6(3) . . ? C22 Ir1 C19 90.3(3) . . ? C16 Ir1 C19 82.1(3) . . ? C22 Ir1 N3 91.2(3) . . ? C16 Ir1 N3 177.4(3) . . ? C19 Ir1 N3 96.0(3) . . ? C22 Ir1 N5 90.9(3) . . ? C16 Ir1 N5 97.0(3) . . ? C19 Ir1 N5 178.5(3) . . ? N3 Ir1 N5 84.8(3) . . ? C22 Ir1 N1 176.6(3) . . ? C16 Ir1 N1 91.8(3) . . ? C19 Ir1 N1 92.3(3) . . ? N3 Ir1 N1 86.4(2) . . ? N5 Ir1 N1 86.5(2) . . ? C1 N1 N2 105.9(6) . . ? C1 N1 Ir1 137.8(5) . . ? N2 N1 Ir1 116.3(4) . . ? C3 N2 N1 109.7(6) . . ? C3 N2 B1 129.7(6) . . ? N1 N2 B1 120.6(6) . . ? C6 N3 N4 106.6(6) . . ? C6 N3 Ir1 135.0(5) . . ? N4 N3 Ir1 118.3(5) . . ? C8 N4 N3 109.9(6) . . ? C8 N4 B1 130.8(6) . . ? N3 N4 B1 119.3(6) . . ? C11 N5 N6 107.1(7) . . ? C11 N5 Ir1 134.9(6) . . ? N6 N5 Ir1 117.2(5) . . ? C13 N6 N5 109.3(7) . . ? C13 N6 B1 131.0(7) . . ? N5 N6 B1 119.7(6) . . ? C26 N7 C22 126.6(7) . . ? C26 N7 H7N 111(6) . . ? C22 N7 H7N 123(6) . . ? C31 N8 C27 118.6(7) . . ? C36 N9 C32 117.4(9) . . ? N1 C1 C2 109.6(7) . . ? N1 C1 C4 124.1(7) . . ? C2 C1 C4 126.3(7) . . ? C3 C2 C1 106.8(7) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N2 C3 C2 108.0(7) . . ? N2 C3 C5 123.1(7) . . ? C2 C3 C5 128.9(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 109.1(7) . . ? N3 C6 C9 123.5(7) . . ? C7 C6 C9 127.3(7) . . ? C8 C7 C6 106.6(7) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N4 C8 C7 107.7(7) . . ? N4 C8 C10 124.8(8) . . ? C7 C8 C10 127.4(8) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 108.8(9) . . ? N5 C11 C14 123.4(8) . . ? C12 C11 C14 127.8(9) . . ? C13 C12 C11 107.2(8) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? N6 C13 C12 107.6(8) . . ? N6 C13 C15 124.2(10) . . ? C12 C13 C15 128.1(9) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 Ir1 111.5(6) . . ? C17 C16 H16A 109.3 . . ? Ir1 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? Ir1 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C20 126.2(8) . . ? C18 C17 C16 117.7(7) . . ? C20 C17 C16 116.0(8) . . ? C17 C18 C21 127.2(8) . . ? C17 C18 C19 117.2(7) . . ? C21 C18 C19 115.6(8) . . ? C18 C19 Ir1 111.2(6) . . ? C18 C19 H19A 109.4 . . ? Ir1 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? Ir1 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 112.6(7) . . ? N7 C22 Ir1 118.3(5) . . ? C23 C22 Ir1 129.0(5) . . ? C24 C23 C22 121.4(7) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 122.1(8) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 116.8(8) . . ? C26 C25 H25 121.6 . . ? C24 C25 H25 121.6 . . ? N7 C26 C25 120.5(7) . . ? N7 C26 C27 114.8(7) . . ? C25 C26 C27 124.6(7) . . ? N8 C27 C28 121.5(8) . . ? N8 C27 C26 113.5(7) . . ? C28 C27 C26 125.0(8) . . ? C29 C28 C27 118.6(9) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 121.2(8) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C31 118.3(9) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? N8 C31 C30 121.8(9) . . ? N8 C31 C32 117.1(7) . . ? C30 C31 C32 121.1(8) . . ? N9 C32 C33 121.8(9) . . ? N9 C32 C31 116.6(8) . . ? C33 C32 C31 121.7(8) . . ? C34 C33 C32 119.7(9) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 118.3(10) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 117.9(11) . . ? C36 C35 H35 121.0 . . ? C34 C35 H35 121.0 . . ? N9 C36 C35 124.9(10) . . ? N9 C36 H36 117.5 . . ? C35 C36 H36 117.5 . . ? N4 B1 N2 110.1(6) . . ? N4 B1 N6 111.1(6) . . ? N2 B1 N6 108.0(7) . . ? N4 B1 H1 109.2 . . ? N2 B1 H1 109.2 . . ? N6 B1 H1 109.2 . . ? C39 O1 C37 106(4) . . ? C38 C37 O1 93(4) . . ? C38 C37 H37A 113.1 . . ? O1 C37 H37A 113.1 . . ? C38 C37 H37B 113.1 . . ? O1 C37 H37B 113.1 . . ? H37A C37 H37B 110.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C40 106(4) . . ? O1 C39 H39A 110.6 . . ? C40 C39 H39A 110.6 . . ? O1 C39 H39B 110.6 . . ? C40 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Ir1 N1 C1 -39.0(9) . . . . ? C19 Ir1 N1 C1 43.1(9) . . . . ? N3 Ir1 N1 C1 139.0(9) . . . . ? N5 Ir1 N1 C1 -135.9(9) . . . . ? C16 Ir1 N1 N2 140.4(6) . . . . ? C19 Ir1 N1 N2 -137.4(6) . . . . ? N3 Ir1 N1 N2 -41.5(5) . . . . ? N5 Ir1 N1 N2 43.5(6) . . . . ? C1 N1 N2 C3 0.2(9) . . . . ? Ir1 N1 N2 C3 -179.4(5) . . . . ? C1 N1 N2 B1 178.0(7) . . . . ? Ir1 N1 N2 B1 -1.7(9) . . . . ? C22 Ir1 N3 C6 46.5(7) . . . . ? C19 Ir1 N3 C6 -44.0(7) . . . . ? N5 Ir1 N3 C6 137.3(7) . . . . ? N1 Ir1 N3 C6 -135.9(7) . . . . ? C22 Ir1 N3 N4 -134.7(5) . . . . ? C19 Ir1 N3 N4 134.9(5) . . . . ? N5 Ir1 N3 N4 -43.9(5) . . . . ? N1 Ir1 N3 N4 42.9(5) . . . . ? C6 N3 N4 C8 0.8(8) . . . . ? Ir1 N3 N4 C8 -178.4(5) . . . . ? C6 N3 N4 B1 178.7(6) . . . . ? Ir1 N3 N4 B1 -0.5(8) . . . . ? C22 Ir1 N5 C11 -51.9(8) . . . . ? C16 Ir1 N5 C11 38.9(8) . . . . ? N3 Ir1 N5 C11 -143.0(8) . . . . ? N1 Ir1 N5 C11 130.3(8) . . . . ? C22 Ir1 N5 N6 139.5(5) . . . . ? C16 Ir1 N5 N6 -129.7(5) . . . . ? N3 Ir1 N5 N6 48.4(5) . . . . ? N1 Ir1 N5 N6 -38.3(5) . . . . ? C11 N5 N6 C13 -1.3(8) . . . . ? Ir1 N5 N6 C13 170.3(5) . . . . ? C11 N5 N6 B1 -180.0(7) . . . . ? Ir1 N5 N6 B1 -8.4(8) . . . . ? N2 N1 C1 C2 0.1(9) . . . . ? Ir1 N1 C1 C2 179.6(6) . . . . ? N2 N1 C1 C4 179.3(9) . . . . ? Ir1 N1 C1 C4 -1.2(14) . . . . ? N1 C1 C2 C3 -0.4(10) . . . . ? C4 C1 C2 C3 -179.6(9) . . . . ? N1 N2 C3 C2 -0.5(9) . . . . ? B1 N2 C3 C2 -178.0(8) . . . . ? N1 N2 C3 C5 179.3(8) . . . . ? B1 N2 C3 C5 1.9(13) . . . . ? C1 C2 C3 N2 0.5(10) . . . . ? C1 C2 C3 C5 -179.3(9) . . . . ? N4 N3 C6 C7 -0.7(8) . . . . ? Ir1 N3 C6 C7 178.2(5) . . . . ? N4 N3 C6 C9 -179.0(7) . . . . ? Ir1 N3 C6 C9 0.0(12) . . . . ? N3 C6 C7 C8 0.5(9) . . . . ? C9 C6 C7 C8 178.6(8) . . . . ? N3 N4 C8 C7 -0.5(8) . . . . ? B1 N4 C8 C7 -178.1(7) . . . . ? N3 N4 C8 C10 175.9(7) . . . . ? B1 N4 C8 C10 -1.7(13) . . . . ? C6 C7 C8 N4 0.0(9) . . . . ? C6 C7 C8 C10 -176.3(8) . . . . ? N6 N5 C11 C12 0.0(9) . . . . ? Ir1 N5 C11 C12 -169.5(6) . . . . ? N6 N5 C11 C14 179.0(8) . . . . ? Ir1 N5 C11 C14 9.6(13) . . . . ? N5 C11 C12 C13 1.4(10) . . . . ? C14 C11 C12 C13 -177.6(9) . . . . ? N5 N6 C13 C12 2.2(9) . . . . ? B1 N6 C13 C12 -179.4(8) . . . . ? N5 N6 C13 C15 -175.0(8) . . . . ? B1 N6 C13 C15 3.4(13) . . . . ? C11 C12 C13 N6 -2.2(10) . . . . ? C11 C12 C13 C15 174.9(9) . . . . ? C22 Ir1 C16 C17 -87.4(6) . . . . ? C19 Ir1 C16 C17 2.8(6) . . . . ? N5 Ir1 C16 C17 -178.4(5) . . . . ? N1 Ir1 C16 C17 94.9(6) . . . . ? Ir1 C16 C17 C18 -1.1(9) . . . . ? Ir1 C16 C17 C20 -179.4(6) . . . . ? C20 C17 C18 C21 -3.0(15) . . . . ? C16 C17 C18 C21 178.9(8) . . . . ? C20 C17 C18 C19 175.8(8) . . . . ? C16 C17 C18 C19 -2.3(11) . . . . ? C17 C18 C19 Ir1 4.6(9) . . . . ? C21 C18 C19 Ir1 -176.5(6) . . . . ? C22 Ir1 C19 C18 86.7(6) . . . . ? C16 Ir1 C19 C18 -3.9(6) . . . . ? N3 Ir1 C19 C18 178.0(5) . . . . ? N1 Ir1 C19 C18 -95.4(6) . . . . ? C26 N7 C22 C23 1.2(12) . . . . ? C26 N7 C22 Ir1 -176.8(6) . . . . ? C16 Ir1 C22 N7 -139.6(6) . . . . ? C19 Ir1 C22 N7 138.3(6) . . . . ? N3 Ir1 C22 N7 42.3(6) . . . . ? N5 Ir1 C22 N7 -42.6(6) . . . . ? C16 Ir1 C22 C23 42.7(8) . . . . ? C19 Ir1 C22 C23 -39.4(8) . . . . ? N3 Ir1 C22 C23 -135.4(8) . . . . ? N5 Ir1 C22 C23 139.7(8) . . . . ? N7 C22 C23 C24 0.5(12) . . . . ? Ir1 C22 C23 C24 178.4(7) . . . . ? C22 C23 C24 C25 -1.5(15) . . . . ? C23 C24 C25 C26 0.6(15) . . . . ? C22 N7 C26 C25 -2.1(13) . . . . ? C22 N7 C26 C27 179.5(8) . . . . ? C24 C25 C26 N7 1.1(14) . . . . ? C24 C25 C26 C27 179.3(9) . . . . ? C31 N8 C27 C28 -0.3(12) . . . . ? C31 N8 C27 C26 -179.5(7) . . . . ? N7 C26 C27 N8 -0.1(11) . . . . ? C25 C26 C27 N8 -178.4(9) . . . . ? N7 C26 C27 C28 -179.3(8) . . . . ? C25 C26 C27 C28 2.4(14) . . . . ? N8 C27 C28 C29 -0.3(14) . . . . ? C26 C27 C28 C29 178.8(9) . . . . ? C27 C28 C29 C30 -0.1(15) . . . . ? C28 C29 C30 C31 1.0(16) . . . . ? C27 N8 C31 C30 1.2(13) . . . . ? C27 N8 C31 C32 -179.4(7) . . . . ? C29 C30 C31 N8 -1.6(14) . . . . ? C29 C30 C31 C32 179.1(9) . . . . ? C36 N9 C32 C33 -0.3(15) . . . . ? C36 N9 C32 C31 178.4(9) . . . . ? N8 C31 C32 N9 -176.6(8) . . . . ? C30 C31 C32 N9 2.8(13) . . . . ? N8 C31 C32 C33 2.1(13) . . . . ? C30 C31 C32 C33 -178.5(9) . . . . ? N9 C32 C33 C34 0.3(16) . . . . ? C31 C32 C33 C34 -178.4(9) . . . . ? C32 C33 C34 C35 0.0(17) . . . . ? C33 C34 C35 C36 -0.2(18) . . . . ? C32 N9 C36 C35 0.1(18) . . . . ? C34 C35 C36 N9 0(2) . . . . ? C8 N4 B1 N2 117.4(8) . . . . ? N3 N4 B1 N2 -60.0(9) . . . . ? C8 N4 B1 N6 -123.0(8) . . . . ? N3 N4 B1 N6 59.6(8) . . . . ? C3 N2 B1 N4 -121.5(8) . . . . ? N1 N2 B1 N4 61.2(10) . . . . ? C3 N2 B1 N6 117.0(9) . . . . ? N1 N2 B1 N6 -60.3(9) . . . . ? C13 N6 B1 N4 127.8(8) . . . . ? N5 N6 B1 N4 -54.0(8) . . . . ? C13 N6 B1 N2 -111.4(9) . . . . ? N5 N6 B1 N2 66.9(8) . . . . ? C39 O1 C37 C38 170(6) . . . . ? C37 O1 C39 C40 -178(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7N N8 0.90(2) 2.08(8) 2.608(9) 117(7) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.631 _refine_diff_density_min -2.369 _refine_diff_density_rms 0.172 ###END #========================================================================= # Data for compound 3 (local labelling ea17308a) #========================================================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 731547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H75 B2 Ir2 N15, C4 H8 O]' _chemical_formula_sum 'C61 H83 B2 Ir2 N15 O' _chemical_formula_weight 1448.44 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9949(9) _cell_length_b 17.1764(14) _cell_length_c 17.3819(14) _cell_angle_alpha 104.057(2) _cell_angle_beta 102.058(2) _cell_angle_gamma 93.350(2) _cell_volume 3093.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8439 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.12 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 4.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7661 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_process_details ; SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. ; _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-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40562 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.39 _reflns_number_total 12549 _reflns_number_gt 6786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker (2006). APEX 2. Version 2.1.' _computing_cell_refinement 'Bruker (2006). APEX 2. Version 2.1.' _computing_data_reduction 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_solution 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2003)' _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. The asymmetric unit of the structure is formed by one binuclear Ir(III) complex 3 and one salvation THF molecule. The solvent THF molecule was observed disordered in two positions. The occupancy factors for these two disordered moieties were first refined and the latest stages of refinement, due to the convergence, were both fixed to 0.5. All the non-hydrogen atoms were refined with anisotropic displacement parameters. Some few reflections to low angle that present values very below their calculated values, possibly partially covered for "beam stopper" were eliminated at the end of the refinement (OMIT command). The hydrogen atoms bonded to the nitrogen atoms were located from the difference Fourier synthesis and refined isotropically with restraints (N-H = 0.90 \%A). The other hydrogen atoms were placed in calculated positions and refined with isotropic displacement parameters by using a riding model. ; _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^)+(0.0392P)^2^+0.5076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12549 _refine_ls_number_parameters 797 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.32575(3) 0.11474(2) 0.21808(2) 0.02740(10) Uani 1 1 d U . . Ir2 Ir -0.08391(3) 0.39503(2) 0.69553(2) 0.03592(12) Uani 1 1 d U . . N1 N 0.3357(6) 0.0102(4) 0.1200(4) 0.0297(15) Uani 1 1 d U . . N2 N 0.3224(5) 0.0230(4) 0.0449(4) 0.0260(14) Uani 1 1 d U . . N3 N 0.1538(6) 0.1314(4) 0.1389(4) 0.0284(15) Uani 1 1 d U . . N4 N 0.1492(6) 0.1119(4) 0.0572(4) 0.0264(14) Uani 1 1 d U . . N5 N 0.4229(6) 0.1827(4) 0.1554(4) 0.0304(15) Uani 1 1 d U . . N6 N 0.3702(5) 0.1733(4) 0.0743(4) 0.0267(14) Uani 1 1 d U . . N7 N -0.2746(6) 0.4249(4) 0.6561(5) 0.0391(17) Uani 1 1 d U . . N8 N -0.3265(6) 0.4629(4) 0.7185(5) 0.0405(17) Uani 1 1 d U . . N9 N -0.0498(6) 0.5180(4) 0.7752(4) 0.0385(16) Uani 1 1 d U . . N10 N -0.1382(6) 0.5418(4) 0.8215(4) 0.0392(17) Uani 1 1 d U . . N11 N -0.1509(7) 0.3558(4) 0.7907(5) 0.0466(18) Uani 1 1 d U . . N12 N -0.2212(7) 0.4075(4) 0.8327(5) 0.0453(18) Uani 1 1 d U . . N13 N 0.3423(6) 0.2109(4) 0.3826(4) 0.0314(16) Uani 1 1 d DU . . H13N H 0.348(7) 0.164(3) 0.397(4) 0.038 Uiso 1 1 d D . . N14 N 0.3141(6) 0.2965(4) 0.5856(4) 0.0309(16) Uani 1 1 d U . . N15 N 0.1664(6) 0.3428(4) 0.6934(4) 0.0313(16) Uani 1 1 d DU . . H15N H 0.137(6) 0.335(4) 0.6400(15) 0.038 Uiso 1 1 d D . . C1 C 0.3680(7) -0.0650(5) 0.1131(5) 0.0322(18) Uani 1 1 d U . . C2 C 0.3738(7) -0.1000(5) 0.0320(5) 0.0313(19) Uani 1 1 d U . . H2 H 0.3941 -0.1527 0.0107 0.038 Uiso 1 1 calc R . . C3 C 0.3448(7) -0.0435(5) -0.0098(5) 0.0319(18) Uani 1 1 d U . . C4 C 0.3932(8) -0.1045(5) 0.1810(5) 0.044(2) Uani 1 1 d U . . H4A H 0.4727 -0.0795 0.2188 0.066 Uiso 1 1 calc R . . H4B H 0.3982 -0.1622 0.1591 0.066 Uiso 1 1 calc R . . H4C H 0.3254 -0.0980 0.2099 0.066 Uiso 1 1 calc R . . C5 C 0.3370(8) -0.0479(5) -0.0978(5) 0.040(2) Uani 1 1 d U . . H5A H 0.2516 -0.0411 -0.1239 0.060 Uiso 1 1 calc R . . H5B H 0.3585 -0.1005 -0.1250 0.060 Uiso 1 1 calc R . . H5C H 0.3957 -0.0048 -0.1021 0.060 Uiso 1 1 calc R . . C6 C 0.5151(7) 0.2450(5) 0.1781(5) 0.0322(18) Uani 1 1 d U . . C7 C 0.5186(7) 0.2738(5) 0.1104(5) 0.036(2) Uani 1 1 d U . . H7 H 0.5744 0.3175 0.1089 0.043 Uiso 1 1 calc R . . C8 C 0.4271(7) 0.2282(5) 0.0460(5) 0.0283(18) Uani 1 1 d U . . C9 C 0.5980(8) 0.2678(5) 0.2618(5) 0.043(2) Uani 1 1 d U . . H9A H 0.5469 0.2812 0.3021 0.065 Uiso 1 1 calc R . . H9B H 0.6575 0.3148 0.2675 0.065 Uiso 1 1 calc R . . H9C H 0.6440 0.2224 0.2707 0.065 Uiso 1 1 calc R . . C10 C 0.3914(8) 0.2357(5) -0.0384(5) 0.039(2) Uani 1 1 d U . . H10A H 0.3902 0.1831 -0.0766 0.059 Uiso 1 1 calc R . . H10B H 0.4523 0.2751 -0.0466 0.059 Uiso 1 1 calc R . . H10C H 0.3080 0.2538 -0.0481 0.059 Uiso 1 1 calc R . . C11 C 0.0363(7) 0.1451(5) 0.1462(5) 0.0301(19) Uani 1 1 d U . . C12 C -0.0410(8) 0.1347(5) 0.0718(5) 0.037(2) Uani 1 1 d U . . H12 H -0.1274 0.1418 0.0607 0.044 Uiso 1 1 calc R . . C13 C 0.0311(7) 0.1114(5) 0.0151(5) 0.0305(18) Uani 1 1 d U . . C14 C 0.0015(7) 0.1704(5) 0.2274(5) 0.045(2) Uani 1 1 d U . . H14A H 0.0617 0.1535 0.2685 0.067 Uiso 1 1 calc R . . H14B H -0.0827 0.1448 0.2229 0.067 Uiso 1 1 calc R . . H14C H 0.0027 0.2293 0.2434 0.067 Uiso 1 1 calc R . . C15 C -0.0066(7) 0.0861(5) -0.0770(5) 0.040(2) Uani 1 1 d U . . H15A H 0.0485 0.1174 -0.0990 0.061 Uiso 1 1 calc R . . H15B H -0.0934 0.0960 -0.0952 0.061 Uiso 1 1 calc R . . H15C H 0.0009 0.0284 -0.0965 0.061 Uiso 1 1 calc R . . C16 C 0.4833(7) 0.0900(5) 0.2931(5) 0.0346(19) Uani 1 1 d U . . H16A H 0.5351 0.0588 0.2592 0.041 Uiso 1 1 calc R . . H16B H 0.5340 0.1413 0.3260 0.041 Uiso 1 1 calc R . . C17 C 0.4482(8) 0.0428(5) 0.3485(5) 0.042(2) Uani 1 1 d U . . C18 C 0.3268(8) 0.0218(5) 0.3418(5) 0.039(2) Uani 1 1 d U . . C19 C 0.2351(7) 0.0471(5) 0.2767(5) 0.0335(18) Uani 1 1 d U . . H19A H 0.1751 0.0792 0.3021 0.040 Uiso 1 1 calc R . . H19B H 0.1871 -0.0016 0.2364 0.040 Uiso 1 1 calc R . . C20 C 0.5562(9) 0.0174(6) 0.4040(6) 0.063(3) Uani 1 1 d U . . H20A H 0.5240 -0.0062 0.4429 0.095 Uiso 1 1 calc R . . H20B H 0.6166 0.0648 0.4339 0.095 Uiso 1 1 calc R . . H20C H 0.5974 -0.0226 0.3711 0.095 Uiso 1 1 calc R . . C21 C 0.2721(9) -0.0273(6) 0.3904(6) 0.060(3) Uani 1 1 d U . . H21A H 0.3382 -0.0534 0.4183 0.090 Uiso 1 1 calc R . . H21B H 0.2065 -0.0687 0.3537 0.090 Uiso 1 1 calc R . . H21C H 0.2361 0.0083 0.4308 0.090 Uiso 1 1 calc R . . C22 C -0.3534(8) 0.4208(6) 0.5856(6) 0.048(2) Uani 1 1 d U . . C23 C -0.4589(8) 0.4568(6) 0.6025(6) 0.055(3) Uani 1 1 d U . . H23 H -0.5302 0.4627 0.5636 0.066 Uiso 1 1 calc R . . C24 C -0.4404(8) 0.4819(5) 0.6854(7) 0.048(2) Uani 1 1 d U . . C25 C -0.3331(9) 0.3825(6) 0.5034(6) 0.062(3) Uani 1 1 d U . . H25A H -0.2944 0.4235 0.4826 0.093 Uiso 1 1 calc R . . H25B H -0.4137 0.3587 0.4662 0.093 Uiso 1 1 calc R . . H25C H -0.2779 0.3402 0.5073 0.093 Uiso 1 1 calc R . . C26 C -0.5247(8) 0.5240(6) 0.7358(7) 0.067(3) Uani 1 1 d U . . H26A H -0.5340 0.4959 0.7773 0.100 Uiso 1 1 calc R . . H26B H -0.6069 0.5236 0.7005 0.100 Uiso 1 1 calc R . . H26C H -0.4880 0.5799 0.7623 0.100 Uiso 1 1 calc R . . C27 C 0.0416(8) 0.5785(5) 0.7989(5) 0.038(2) Uani 1 1 d U . . C28 C 0.0157(8) 0.6399(5) 0.8586(5) 0.044(2) Uani 1 1 d U . . H28 H 0.0668 0.6896 0.8855 0.053 Uiso 1 1 calc R . . C29 C -0.0951(8) 0.6165(5) 0.8717(6) 0.042(2) Uani 1 1 d U . . C30 C 0.1545(8) 0.5761(5) 0.7628(6) 0.049(2) Uani 1 1 d U . . H30A H 0.2174 0.5487 0.7917 0.073 Uiso 1 1 calc R . . H30B H 0.1898 0.6314 0.7680 0.073 Uiso 1 1 calc R . . H30C H 0.1300 0.5466 0.7050 0.073 Uiso 1 1 calc R . . C31 C -0.1693(8) 0.6592(5) 0.9300(5) 0.052(3) Uani 1 1 d U . . H31A H -0.2590 0.6465 0.9045 0.078 Uiso 1 1 calc R . . H31B H -0.1460 0.7176 0.9433 0.078 Uiso 1 1 calc R . . H31C H -0.1511 0.6410 0.9800 0.078 Uiso 1 1 calc R . . C32 C -0.1305(11) 0.2958(6) 0.8274(6) 0.062(3) Uani 1 1 d U . . C33 C -0.1889(11) 0.3101(6) 0.8939(6) 0.069(3) Uani 1 1 d U . . H33 H -0.1904 0.2767 0.9300 0.083 Uiso 1 1 calc R . . C34 C -0.2418(10) 0.3791(6) 0.8973(6) 0.058(3) Uani 1 1 d U . . C35 C -0.0582(12) 0.2298(6) 0.7990(7) 0.089(4) Uani 1 1 d U . . H35A H -0.0073 0.2458 0.7642 0.134 Uiso 1 1 calc R . . H35B H -0.1157 0.1814 0.7679 0.134 Uiso 1 1 calc R . . H35C H -0.0035 0.2181 0.8461 0.134 Uiso 1 1 calc R . . C36 C -0.3118(10) 0.4218(6) 0.9569(6) 0.078(3) Uani 1 1 d U . . H36A H -0.3198 0.3898 0.9956 0.116 Uiso 1 1 calc R . . H36B H -0.3953 0.4285 0.9277 0.116 Uiso 1 1 calc R . . H36C H -0.2662 0.4749 0.9865 0.116 Uiso 1 1 calc R . . C37 C -0.0300(7) 0.4268(5) 0.5992(5) 0.0366(19) Uani 1 1 d U . . H37A H -0.0837 0.4664 0.5814 0.044 Uiso 1 1 calc R . . H37B H 0.0577 0.4526 0.6171 0.044 Uiso 1 1 calc R . . C38 C -0.0407(8) 0.3535(6) 0.5290(5) 0.044(2) Uani 1 1 d U . . C39 C -0.0796(9) 0.2812(6) 0.5361(6) 0.056(3) Uani 1 1 d U . . C40 C -0.1214(9) 0.2799(5) 0.6135(6) 0.049(2) Uani 1 1 d U . . H40A H -0.0769 0.2409 0.6392 0.059 Uiso 1 1 calc R . . H40B H -0.2123 0.2620 0.6001 0.059 Uiso 1 1 calc R . . C41 C -0.0104(9) 0.3674(7) 0.4515(6) 0.071(3) Uani 1 1 d U . . H41A H 0.0209 0.3192 0.4226 0.106 Uiso 1 1 calc R . . H41B H 0.0537 0.4139 0.4657 0.106 Uiso 1 1 calc R . . H41C H -0.0863 0.3780 0.4165 0.106 Uiso 1 1 calc R . . C42 C -0.1028(12) 0.2028(6) 0.4703(6) 0.090(4) Uani 1 1 d U . . H42A H -0.0482 0.2052 0.4328 0.135 Uiso 1 1 calc R . . H42B H -0.1905 0.1943 0.4402 0.135 Uiso 1 1 calc R . . H42C H -0.0847 0.1581 0.4952 0.135 Uiso 1 1 calc R . . C43 C 0.3163(6) 0.2115(5) 0.3016(5) 0.0265(16) Uani 1 1 d U . . C44 C 0.2775(7) 0.2862(5) 0.2879(5) 0.0348(19) Uani 1 1 d U . . H44 H 0.2608 0.2926 0.2341 0.042 Uiso 1 1 calc R . . C45 C 0.2641(7) 0.3475(5) 0.3497(5) 0.038(2) Uani 1 1 d U . . H45 H 0.2364 0.3957 0.3381 0.045 Uiso 1 1 calc R . . C46 C 0.2899(8) 0.3418(5) 0.4299(5) 0.041(2) Uani 1 1 d U . . H46 H 0.2784 0.3853 0.4724 0.049 Uiso 1 1 calc R . . C47 C 0.3308(7) 0.2746(5) 0.4465(5) 0.0342(19) Uani 1 1 d U . . C48 C 0.3742(7) 0.2628(5) 0.5294(5) 0.0331(19) Uani 1 1 d U . . C49 C 0.4804(8) 0.2222(5) 0.5473(5) 0.043(2) Uani 1 1 d U . . H49 H 0.5198 0.1968 0.5057 0.051 Uiso 1 1 calc R . . C50 C 0.5254(9) 0.2207(6) 0.6278(6) 0.056(3) Uani 1 1 d U . . H50 H 0.5989 0.1962 0.6428 0.067 Uiso 1 1 calc R . . C51 C 0.4629(8) 0.2547(6) 0.6848(6) 0.046(2) Uani 1 1 d U . . H51 H 0.4912 0.2530 0.7398 0.056 Uiso 1 1 calc R . . C52 C 0.3573(7) 0.2920(5) 0.6622(5) 0.0327(19) Uani 1 1 d U . . C53 C 0.2887(8) 0.3298(5) 0.7234(5) 0.0328(19) Uani 1 1 d U . . C54 C 0.3353(8) 0.3508(5) 0.8048(5) 0.042(2) Uani 1 1 d U . . H54 H 0.4179 0.3413 0.8272 0.050 Uiso 1 1 calc R . . C55 C 0.2584(9) 0.3871(6) 0.8562(5) 0.049(3) Uani 1 1 d U . . H55 H 0.2906 0.4031 0.9135 0.059 Uiso 1 1 calc R . . C56 C 0.1439(9) 0.3991(5) 0.8260(5) 0.045(2) Uani 1 1 d U . . H56 H 0.0959 0.4239 0.8627 0.054 Uiso 1 1 calc R . . C57 C 0.0868(8) 0.3767(5) 0.7403(5) 0.037(2) Uani 1 1 d U . . B1 B 0.2704(8) 0.1006(5) 0.0274(6) 0.0282(19) Uani 1 1 d U . . H1 H 0.2536 0.0962 -0.0324 0.034 Uiso 1 1 calc R . . B2 B -0.2547(10) 0.4844(6) 0.8082(7) 0.042(2) Uani 1 1 d U . . H2A H -0.3101 0.5115 0.8429 0.051 Uiso 1 1 calc R . . O1A O 0.191(3) 0.1424(18) 0.705(2) 0.140(8) Uani 0.50 1 d PDU A 1 C58A C 0.117(3) 0.112(2) 0.625(2) 0.130(9) Uani 0.50 1 d PDU A 1 H58A H 0.0428 0.1414 0.6165 0.156 Uiso 0.50 1 calc PR A 1 H58B H 0.1654 0.1149 0.5843 0.156 Uiso 0.50 1 calc PR A 1 C59A C 0.081(4) 0.032(2) 0.622(2) 0.121(10) Uani 0.50 1 d PDU A 1 H59A H 0.1317 -0.0055 0.5927 0.145 Uiso 0.50 1 calc PR A 1 H59B H -0.0089 0.0155 0.5947 0.145 Uiso 0.50 1 calc PR A 1 C60A C 0.103(3) 0.032(2) 0.706(2) 0.123(9) Uani 0.50 1 d PDU A 1 H60A H 0.1214 -0.0227 0.7109 0.148 Uiso 0.50 1 calc PR A 1 H60B H 0.0268 0.0437 0.7256 0.148 Uiso 0.50 1 calc PR A 1 C61A C 0.206(4) 0.090(2) 0.756(2) 0.116(9) Uani 0.50 1 d PDU A 1 H61A H 0.1918 0.1140 0.8109 0.139 Uiso 0.50 1 calc PR A 1 H61B H 0.2870 0.0673 0.7608 0.139 Uiso 0.50 1 calc PR A 1 O1B O 0.2613(18) 0.1265(15) 0.7062(16) 0.109(7) Uani 0.50 1 d PDU B 2 C58B C 0.183(2) 0.1135(17) 0.6274(17) 0.088(6) Uani 0.50 1 d PDU B 2 H58C H 0.1269 0.1567 0.6272 0.094 Uiso 0.50 1 calc PR B 2 H58D H 0.2344 0.1156 0.5875 0.094 Uiso 0.50 1 calc PR B 2 C59B C 0.110(3) 0.0376(19) 0.605(2) 0.085(7) Uani 0.50 1 d PDU B 2 H59C H 0.1351 0.0017 0.5584 0.102 Uiso 0.50 1 calc PR B 2 H59D H 0.0206 0.0443 0.5874 0.102 Uiso 0.50 1 calc PR B 2 C60B C 0.127(3) 0.0014(19) 0.6721(18) 0.093(7) Uani 0.50 1 d PDU B 2 H60C H 0.1708 -0.0476 0.6616 0.112 Uiso 0.50 1 calc PR B 2 H60D H 0.0468 -0.0121 0.6855 0.112 Uiso 0.50 1 calc PR B 2 C61B C 0.204(4) 0.066(2) 0.735(2) 0.115(9) Uani 0.50 1 d PDU B 2 H61C H 0.1526 0.0924 0.7719 0.138 Uiso 0.50 1 calc PR B 2 H61D H 0.2711 0.0434 0.7675 0.138 Uiso 0.50 1 calc PR B 2 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 0.02562(19) 0.0329(2) 0.0221(2) 0.00251(16) 0.00676(16) 0.00565(15) Ir2 0.0430(2) 0.0309(2) 0.0382(3) 0.00703(19) 0.0190(2) 0.01164(18) N1 0.029(4) 0.030(4) 0.030(4) 0.004(3) 0.011(3) 0.007(3) N2 0.022(3) 0.025(3) 0.026(3) -0.001(3) 0.001(3) 0.004(3) N3 0.028(3) 0.035(4) 0.022(3) 0.004(3) 0.009(3) 0.008(3) N4 0.029(3) 0.025(4) 0.024(3) 0.002(3) 0.006(3) 0.010(3) N5 0.032(4) 0.030(4) 0.025(4) -0.003(3) 0.008(3) 0.005(3) N6 0.023(3) 0.025(4) 0.032(4) 0.007(3) 0.005(3) 0.011(3) N7 0.034(4) 0.039(5) 0.043(4) -0.004(3) 0.021(3) 0.005(3) N8 0.031(4) 0.035(5) 0.054(4) -0.003(3) 0.022(3) 0.007(3) N9 0.040(4) 0.035(4) 0.043(4) 0.006(3) 0.019(3) 0.011(3) N10 0.041(4) 0.034(4) 0.045(5) 0.001(3) 0.024(3) 0.009(3) N11 0.070(5) 0.027(4) 0.049(5) 0.004(3) 0.031(4) 0.009(3) N12 0.051(5) 0.037(4) 0.049(5) -0.001(3) 0.027(4) 0.002(3) N13 0.029(4) 0.042(4) 0.025(4) 0.006(3) 0.011(3) 0.013(3) N14 0.030(4) 0.036(4) 0.021(3) -0.001(3) 0.004(3) 0.008(3) N15 0.038(4) 0.035(4) 0.021(4) 0.001(3) 0.010(3) 0.019(3) C1 0.024(4) 0.033(5) 0.039(5) 0.007(4) 0.007(4) -0.001(4) C2 0.020(4) 0.032(5) 0.041(5) 0.003(4) 0.009(4) 0.013(4) C3 0.018(4) 0.038(5) 0.033(4) -0.004(4) 0.006(4) 0.006(4) C4 0.045(5) 0.039(6) 0.054(6) 0.017(5) 0.015(5) 0.015(4) C5 0.037(5) 0.044(6) 0.035(5) -0.004(4) 0.014(4) 0.010(4) C6 0.036(5) 0.028(5) 0.033(4) 0.002(4) 0.013(4) 0.012(3) C7 0.034(5) 0.034(5) 0.038(5) 0.004(4) 0.013(4) 0.000(4) C8 0.030(4) 0.029(5) 0.030(4) 0.005(4) 0.016(3) 0.013(3) C9 0.041(5) 0.047(6) 0.036(5) 0.002(4) 0.010(4) 0.000(4) C10 0.045(5) 0.035(6) 0.039(5) 0.007(4) 0.014(4) 0.007(4) C11 0.025(4) 0.021(5) 0.047(5) 0.004(4) 0.016(4) 0.011(4) C12 0.030(4) 0.031(5) 0.051(5) 0.009(4) 0.014(4) 0.010(4) C13 0.033(4) 0.024(5) 0.033(4) 0.009(4) 0.002(3) 0.002(4) C14 0.021(5) 0.063(7) 0.052(5) 0.010(5) 0.016(4) 0.015(4) C15 0.034(5) 0.044(6) 0.038(4) 0.013(4) -0.004(4) 0.001(4) C16 0.037(4) 0.039(5) 0.023(5) 0.001(4) 0.006(4) 0.006(4) C17 0.039(4) 0.062(6) 0.031(5) 0.019(4) 0.006(4) 0.014(4) C18 0.047(5) 0.047(6) 0.025(5) 0.014(4) 0.006(4) 0.004(4) C19 0.038(4) 0.033(5) 0.027(5) 0.000(4) 0.009(4) 0.014(4) C20 0.058(6) 0.086(8) 0.057(7) 0.037(6) 0.012(5) 0.021(6) C21 0.063(7) 0.074(8) 0.055(7) 0.037(6) 0.017(6) 0.014(5) C22 0.039(5) 0.044(6) 0.052(5) -0.001(5) 0.011(4) 0.005(4) C23 0.030(5) 0.057(7) 0.065(6) -0.002(5) 0.004(4) -0.002(4) C24 0.033(5) 0.029(6) 0.075(6) -0.004(5) 0.018(4) 0.000(4) C25 0.045(6) 0.080(8) 0.046(5) -0.006(6) 0.001(5) 0.015(5) C26 0.044(6) 0.053(7) 0.107(9) 0.001(6) 0.047(6) 0.012(5) C27 0.034(5) 0.037(5) 0.047(6) 0.014(4) 0.011(4) 0.001(4) C28 0.052(5) 0.033(5) 0.046(6) 0.007(4) 0.013(4) -0.001(4) C29 0.051(5) 0.024(5) 0.052(6) -0.001(4) 0.023(5) 0.013(4) C30 0.047(5) 0.048(6) 0.052(7) 0.009(5) 0.014(5) 0.010(4) C31 0.057(6) 0.042(6) 0.048(6) -0.011(5) 0.015(5) 0.011(5) C32 0.108(9) 0.033(6) 0.057(7) 0.012(5) 0.044(6) 0.010(5) C33 0.113(9) 0.051(6) 0.049(7) 0.012(5) 0.036(6) -0.003(5) C34 0.077(7) 0.047(6) 0.050(6) 0.003(5) 0.034(5) -0.009(5) C35 0.162(13) 0.045(7) 0.091(10) 0.034(6) 0.065(9) 0.044(7) C36 0.093(9) 0.079(8) 0.063(8) 0.001(6) 0.048(7) -0.010(6) C37 0.031(4) 0.050(5) 0.030(4) 0.012(4) 0.007(4) 0.010(4) C38 0.044(5) 0.060(5) 0.030(5) 0.010(4) 0.009(4) 0.029(5) C39 0.063(7) 0.045(5) 0.051(6) -0.009(4) 0.017(5) 0.016(5) C40 0.055(6) 0.038(5) 0.057(5) 0.002(4) 0.026(5) 0.014(4) C41 0.068(7) 0.113(10) 0.034(6) 0.017(6) 0.017(5) 0.032(6) C42 0.139(12) 0.062(7) 0.047(7) -0.019(5) 0.013(8) 0.012(8) C43 0.012(4) 0.036(4) 0.023(4) -0.005(3) 0.002(3) -0.011(3) C44 0.031(5) 0.042(5) 0.029(5) 0.001(4) 0.012(4) 0.006(4) C45 0.037(5) 0.037(5) 0.032(5) 0.000(4) 0.003(4) 0.002(4) C46 0.044(5) 0.042(5) 0.031(5) -0.003(4) 0.012(4) 0.008(4) C47 0.025(5) 0.046(5) 0.024(4) -0.006(4) 0.009(4) 0.006(4) C48 0.030(4) 0.041(6) 0.026(4) 0.001(4) 0.010(4) 0.007(4) C49 0.035(5) 0.060(6) 0.034(5) 0.005(5) 0.017(4) 0.018(4) C50 0.049(6) 0.078(8) 0.041(6) 0.016(5) 0.008(5) 0.028(5) C51 0.043(5) 0.064(7) 0.039(5) 0.017(5) 0.015(4) 0.030(4) C52 0.033(5) 0.041(5) 0.027(4) 0.010(4) 0.010(4) 0.011(4) C53 0.040(5) 0.034(5) 0.025(4) 0.006(4) 0.008(4) 0.017(4) C54 0.053(5) 0.048(6) 0.025(4) 0.010(4) 0.007(4) 0.026(4) C55 0.079(6) 0.055(6) 0.009(4) 0.003(4) 0.002(4) 0.029(5) C56 0.064(6) 0.049(6) 0.025(5) 0.005(4) 0.017(4) 0.028(5) C57 0.057(4) 0.038(5) 0.021(4) 0.010(4) 0.015(3) 0.020(4) B1 0.033(4) 0.033(5) 0.019(5) 0.003(4) 0.010(4) 0.006(3) B2 0.049(5) 0.027(5) 0.050(5) -0.009(4) 0.033(4) 0.007(4) O1A 0.141(17) 0.113(14) 0.159(14) 0.029(11) 0.032(15) -0.004(13) C58A 0.13(2) 0.124(16) 0.147(14) 0.054(13) 0.032(16) 0.025(19) C59A 0.095(19) 0.139(15) 0.130(16) 0.035(15) 0.037(16) -0.017(15) C60A 0.103(17) 0.145(18) 0.133(18) 0.040(15) 0.059(15) -0.019(14) C61A 0.109(15) 0.125(19) 0.114(15) 0.016(13) 0.044(14) 0.012(15) O1B 0.085(14) 0.100(13) 0.140(13) 0.047(11) 0.004(11) 0.007(10) C58B 0.067(15) 0.112(12) 0.121(13) 0.052(11) 0.045(12) 0.020(11) C59B 0.059(15) 0.102(14) 0.114(13) 0.050(11) 0.041(11) 0.007(11) C60B 0.076(15) 0.106(15) 0.130(19) 0.063(12) 0.056(14) 0.018(11) C61B 0.124(16) 0.130(17) 0.110(14) 0.052(13) 0.042(14) 0.024(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C43 1.947(8) . ? Ir1 C19 2.060(8) . ? Ir1 C16 2.072(7) . ? Ir1 N5 2.156(6) . ? Ir1 N3 2.172(6) . ? Ir1 N1 2.181(7) . ? Ir2 C57 1.951(9) . ? Ir2 C37 2.067(8) . ? Ir2 C40 2.098(9) . ? Ir2 N11 2.174(7) . ? Ir2 N9 2.188(7) . ? Ir2 N7 2.197(7) . ? N1 C1 1.345(10) . ? N1 N2 1.356(8) . ? N2 C3 1.369(9) . ? N2 B1 1.551(11) . ? N3 C11 1.353(9) . ? N3 N4 1.366(8) . ? N4 C13 1.349(9) . ? N4 B1 1.535(10) . ? N5 C6 1.353(9) . ? N5 N6 1.373(8) . ? N6 C8 1.346(9) . ? N6 B1 1.549(10) . ? N7 C22 1.329(11) . ? N7 N8 1.373(9) . ? N8 C24 1.357(11) . ? N8 B2 1.538(12) . ? N9 C27 1.326(10) . ? N9 N10 1.405(9) . ? N10 C29 1.357(10) . ? N10 B2 1.512(11) . ? N11 C32 1.344(11) . ? N11 N12 1.385(9) . ? N12 C34 1.382(11) . ? N12 B2 1.524(12) . ? N13 C43 1.379(9) . ? N13 C47 1.391(10) . ? N13 H13N 0.90(6) . ? N14 C48 1.328(9) . ? N14 C52 1.340(9) . ? N15 C57 1.377(10) . ? N15 C53 1.388(10) . ? N15 H15N 0.889(19) . ? C1 C2 1.407(11) . ? C1 C4 1.485(11) . ? C2 C3 1.361(11) . ? C2 H2 0.9500 . ? C3 C5 1.497(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.390(11) . ? C6 C9 1.492(11) . ? C7 C8 1.375(11) . ? C7 H7 0.9500 . ? C8 C10 1.477(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.355(11) . ? C11 C14 1.508(11) . ? C12 C13 1.390(11) . ? C12 H12 0.9500 . ? C13 C15 1.512(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.495(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.335(11) . ? C17 C20 1.522(11) . ? C18 C21 1.512(11) . ? C18 C19 1.517(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.398(12) . ? C22 C25 1.489(13) . ? C23 C24 1.368(13) . ? C23 H23 0.9500 . ? C24 C26 1.502(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.377(12) . ? C27 C30 1.502(11) . ? C28 C29 1.341(11) . ? C28 H28 0.9500 . ? C29 C31 1.512(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.414(13) . ? C32 C35 1.469(13) . ? C33 C34 1.344(14) . ? C33 H33 0.9500 . ? C34 C36 1.495(13) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.505(12) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.332(12) . ? C38 C41 1.522(12) . ? C39 C42 1.509(13) . ? C39 C40 1.514(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.433(11) . ? C44 C45 1.348(11) . ? C44 H44 0.9500 . ? C45 C46 1.392(11) . ? C45 H45 0.9500 . ? C46 C47 1.336(11) . ? C46 H46 0.9500 . ? C47 C48 1.487(11) . ? C48 C49 1.412(11) . ? C49 C50 1.391(11) . ? C49 H49 0.9500 . ? C50 C51 1.358(12) . ? C50 H50 0.9500 . ? C51 C52 1.390(11) . ? C51 H51 0.9500 . ? C52 C53 1.476(11) . ? C53 C54 1.351(11) . ? C54 C55 1.416(12) . ? C54 H54 0.9500 . ? C55 C56 1.307(12) . ? C55 H55 0.9500 . ? C56 C57 1.436(11) . ? C56 H56 0.9500 . ? B1 H1 1.0000 . ? B2 H2A 1.0000 . ? O1A C61A 1.404(18) . ? O1A C58A 1.416(18) . ? C58A C59A 1.391(18) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C59A C60A 1.424(18) . ? C59A H59A 0.9900 . ? C59A H59B 0.9900 . ? C60A C61A 1.430(18) . ? C60A H60A 0.9900 . ? C60A H60B 0.9900 . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? O1B C58B 1.417(17) . ? O1B C61B 1.420(18) . ? C58B C59B 1.411(17) . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? C59B C60B 1.436(18) . ? C59B H59C 0.9900 . ? C59B H59D 0.9900 . ? C60B C61B 1.439(18) . ? C60B H60C 0.9900 . ? C60B H60D 0.9900 . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? 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 C43 Ir1 C19 89.1(3) . . ? C43 Ir1 C16 90.5(3) . . ? C19 Ir1 C16 82.4(3) . . ? C43 Ir1 N5 92.3(3) . . ? C19 Ir1 N5 178.5(3) . . ? C16 Ir1 N5 96.9(3) . . ? C43 Ir1 N3 91.9(3) . . ? C19 Ir1 N3 93.9(3) . . ? C16 Ir1 N3 175.6(3) . . ? N5 Ir1 N3 86.7(2) . . ? C43 Ir1 N1 177.0(3) . . ? C19 Ir1 N1 93.5(3) . . ? C16 Ir1 N1 91.4(3) . . ? N5 Ir1 N1 85.2(2) . . ? N3 Ir1 N1 86.3(2) . . ? C57 Ir2 C37 91.2(3) . . ? C57 Ir2 C40 92.3(4) . . ? C37 Ir2 C40 82.6(3) . . ? C57 Ir2 N11 91.3(3) . . ? C37 Ir2 N11 176.0(3) . . ? C40 Ir2 N11 94.3(3) . . ? C57 Ir2 N9 90.0(3) . . ? C37 Ir2 N9 95.0(3) . . ? C40 Ir2 N9 176.7(3) . . ? N11 Ir2 N9 88.1(3) . . ? C57 Ir2 N7 174.4(3) . . ? C37 Ir2 N7 91.5(3) . . ? C40 Ir2 N7 93.0(3) . . ? N11 Ir2 N7 86.3(3) . . ? N9 Ir2 N7 84.8(3) . . ? C1 N1 N2 106.1(7) . . ? C1 N1 Ir1 137.2(6) . . ? N2 N1 Ir1 116.0(5) . . ? N1 N2 C3 111.0(6) . . ? N1 N2 B1 120.4(6) . . ? C3 N2 B1 128.0(7) . . ? C11 N3 N4 105.9(6) . . ? C11 N3 Ir1 136.5(6) . . ? N4 N3 Ir1 116.6(4) . . ? C13 N4 N3 109.9(6) . . ? C13 N4 B1 130.1(7) . . ? N3 N4 B1 119.7(6) . . ? C6 N5 N6 107.0(6) . . ? C6 N5 Ir1 135.5(5) . . ? N6 N5 Ir1 116.4(4) . . ? C8 N6 N5 110.4(6) . . ? C8 N6 B1 129.4(7) . . ? N5 N6 B1 119.7(6) . . ? C22 N7 N8 108.8(7) . . ? C22 N7 Ir2 136.5(6) . . ? N8 N7 Ir2 114.6(5) . . ? C24 N8 N7 108.3(8) . . ? C24 N8 B2 129.3(8) . . ? N7 N8 B2 122.2(7) . . ? C27 N9 N10 106.0(7) . . ? C27 N9 Ir2 136.7(6) . . ? N10 N9 Ir2 117.0(5) . . ? C29 N10 N9 107.9(7) . . ? C29 N10 B2 133.6(8) . . ? N9 N10 B2 118.5(7) . . ? C32 N11 N12 107.8(8) . . ? C32 N11 Ir2 135.6(7) . . ? N12 N11 Ir2 116.2(5) . . ? C34 N12 N11 108.6(8) . . ? C34 N12 B2 130.7(8) . . ? N11 N12 B2 120.5(7) . . ? C43 N13 C47 124.9(7) . . ? C43 N13 H13N 121(5) . . ? C47 N13 H13N 112(5) . . ? C48 N14 C52 118.3(7) . . ? C57 N15 C53 125.2(7) . . ? C57 N15 H15N 115(5) . . ? C53 N15 H15N 120(5) . . ? N1 C1 C2 109.5(7) . . ? N1 C1 C4 124.8(8) . . ? C2 C1 C4 125.8(8) . . ? C3 C2 C1 106.7(8) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 N2 106.7(7) . . ? C2 C3 C5 129.8(8) . . ? N2 C3 C5 123.5(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 C7 107.9(7) . . ? N5 C6 C9 121.0(7) . . ? C7 C6 C9 131.0(7) . . ? C8 C7 C6 108.1(7) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? N6 C8 C7 106.5(7) . . ? N6 C8 C10 124.3(7) . . ? C7 C8 C10 129.2(7) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.6(8) . . ? N3 C11 C14 123.0(7) . . ? C12 C11 C14 126.4(7) . . ? C11 C12 C13 106.4(7) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? N4 C13 C12 107.1(7) . . ? N4 C13 C15 122.7(7) . . ? C12 C13 C15 130.1(7) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 Ir1 111.1(5) . . ? C17 C16 H16A 109.4 . . ? Ir1 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? Ir1 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 118.3(7) . . ? C18 C17 C20 125.5(8) . . ? C16 C17 C20 116.1(7) . . ? C17 C18 C21 126.5(8) . . ? C17 C18 C19 116.6(7) . . ? C21 C18 C19 116.9(7) . . ? C18 C19 Ir1 111.5(5) . . ? C18 C19 H19A 109.3 . . ? Ir1 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? Ir1 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 107.9(9) . . ? N7 C22 C25 125.6(9) . . ? C23 C22 C25 126.5(9) . . ? C24 C23 C22 107.2(9) . . ? C24 C23 H23 126.4 . . ? C22 C23 H23 126.4 . . ? N8 C24 C23 107.8(9) . . ? N8 C24 C26 123.1(9) . . ? C23 C24 C26 129.1(9) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N9 C27 C28 110.2(8) . . ? N9 C27 C30 122.2(8) . . ? C28 C27 C30 127.6(8) . . ? C29 C28 C27 107.3(8) . . ? C29 C28 H28 126.4 . . ? C27 C28 H28 126.4 . . ? C28 C29 N10 108.6(8) . . ? C28 C29 C31 130.5(8) . . ? N10 C29 C31 120.9(8) . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N11 C32 C33 107.8(9) . . ? N11 C32 C35 122.7(9) . . ? C33 C32 C35 129.5(10) . . ? C34 C33 C32 108.3(10) . . ? C34 C33 H33 125.8 . . ? C32 C33 H33 125.8 . . ? C33 C34 N12 107.5(9) . . ? C33 C34 C36 129.6(10) . . ? N12 C34 C36 122.9(10) . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 Ir2 110.6(6) . . ? C38 C37 H37A 109.5 . . ? Ir2 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? Ir2 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C37 119.5(8) . . ? C39 C38 C41 123.5(9) . . ? C37 C38 C41 117.0(8) . . ? C38 C39 C42 126.2(10) . . ? C38 C39 C40 116.4(8) . . ? C42 C39 C40 116.8(9) . . ? C39 C40 Ir2 110.6(6) . . ? C39 C40 H40A 109.5 . . ? Ir2 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? Ir2 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N13 C43 C44 113.6(7) . . ? N13 C43 Ir1 120.1(6) . . ? C44 C43 Ir1 126.2(6) . . ? C45 C44 C43 121.6(8) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 121.5(9) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C47 C46 C45 119.4(9) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 N13 118.9(8) . . ? C46 C47 C48 125.6(8) . . ? N13 C47 C48 115.3(8) . . ? N14 C48 C49 122.6(7) . . ? N14 C48 C47 117.1(7) . . ? C49 C48 C47 120.2(8) . . ? C50 C49 C48 117.9(8) . . ? C50 C49 H49 121.1 . . ? C48 C49 H49 121.1 . . ? C51 C50 C49 119.1(9) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C50 C51 C52 119.7(9) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? N14 C52 C51 122.4(8) . . ? N14 C52 C53 117.1(7) . . ? C51 C52 C53 120.5(8) . . ? C54 C53 N15 118.8(8) . . ? C54 C53 C52 124.9(8) . . ? N15 C53 C52 116.3(7) . . ? C53 C54 C55 118.6(8) . . ? C53 C54 H54 120.7 . . ? C55 C54 H54 120.7 . . ? C56 C55 C54 121.2(8) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C55 C56 C57 123.5(9) . . ? C55 C56 H56 118.2 . . ? C57 C56 H56 118.2 . . ? N15 C57 C56 112.8(7) . . ? N15 C57 Ir2 123.8(6) . . ? C56 C57 Ir2 123.4(6) . . ? N4 B1 N6 109.6(6) . . ? N4 B1 N2 109.5(6) . . ? N6 B1 N2 107.9(6) . . ? N4 B1 H1 109.9 . . ? N6 B1 H1 109.9 . . ? N2 B1 H1 109.9 . . ? N10 B2 N12 110.7(8) . . ? N10 B2 N8 110.5(8) . . ? N12 B2 N8 109.7(7) . . ? N10 B2 H2A 108.6 . . ? N12 B2 H2A 108.6 . . ? N8 B2 H2A 108.6 . . ? C61A O1A C58A 117(3) . . ? C59A C58A O1A 104(3) . . ? C59A C58A H58A 111.0 . . ? O1A C58A H58A 111.0 . . ? C59A C58A H58B 111.0 . . ? O1A C58A H58B 111.0 . . ? H58A C58A H58B 109.0 . . ? C58A C59A C60A 103(3) . . ? C58A C59A H59A 111.2 . . ? C60A C59A H59A 111.2 . . ? C58A C59A H59B 111.2 . . ? C60A C59A H59B 111.2 . . ? H59A C59A H59B 109.2 . . ? C59A C60A C61A 113(3) . . ? C59A C60A H60A 108.9 . . ? C61A C60A H60A 108.9 . . ? C59A C60A H60B 108.9 . . ? C61A C60A H60B 108.9 . . ? H60A C60A H60B 107.7 . . ? O1A C61A C60A 94(3) . . ? O1A C61A H61A 112.8 . . ? C60A C61A H61A 112.8 . . ? O1A C61A H61B 114.0 . . ? C60A C61A H61B 112.8 . . ? H61A C61A H61B 110.3 . . ? C58B O1B C61B 101(2) . . ? C59B C58B O1B 110(2) . . ? C59B C58B H58C 109.6 . . ? O1B C58B H58C 109.6 . . ? C59B C58B H58D 109.6 . . ? O1B C58B H58D 109.6 . . ? H58C C58B H58D 108.2 . . ? C58B C59B C60B 110(3) . . ? C58B C59B H59C 109.6 . . ? C60B C59B H59C 109.6 . . ? C58B C59B H59D 109.6 . . ? C60B C59B H59D 109.6 . . ? H59C C59B H59D 108.1 . . ? C59B C60B C61B 100(3) . . ? C59B C60B H60C 111.8 . . ? C61B C60B H60C 111.8 . . ? C59B C60B H60D 111.8 . . ? C61B C60B H60D 111.8 . . ? H60C C60B H60D 109.5 . . ? O1B C61B C60B 115(3) . . ? O1B C61B H61C 108.6 . . ? C60B C61B H61C 108.6 . . ? O1B C61B H61D 108.6 . . ? C60B C61B H61D 108.6 . . ? H61C C61B H61D 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Ir1 N1 C1 -47.0(8) . . . . ? C16 Ir1 N1 C1 35.5(8) . . . . ? N5 Ir1 N1 C1 132.3(8) . . . . ? N3 Ir1 N1 C1 -140.7(7) . . . . ? C19 Ir1 N1 N2 144.0(5) . . . . ? C16 Ir1 N1 N2 -133.5(5) . . . . ? N5 Ir1 N1 N2 -36.7(5) . . . . ? N3 Ir1 N1 N2 50.3(5) . . . . ? C1 N1 N2 C3 0.6(8) . . . . ? Ir1 N1 N2 C3 172.9(4) . . . . ? C1 N1 N2 B1 173.0(6) . . . . ? Ir1 N1 N2 B1 -14.8(8) . . . . ? C43 Ir1 N3 C11 -50.2(8) . . . . ? C19 Ir1 N3 C11 39.0(8) . . . . ? N5 Ir1 N3 C11 -142.4(8) . . . . ? N1 Ir1 N3 C11 132.3(8) . . . . ? C43 Ir1 N3 N4 142.8(5) . . . . ? C19 Ir1 N3 N4 -128.0(5) . . . . ? N5 Ir1 N3 N4 50.6(5) . . . . ? N1 Ir1 N3 N4 -34.7(5) . . . . ? C11 N3 N4 C13 -1.6(8) . . . . ? Ir1 N3 N4 C13 169.1(5) . . . . ? C11 N3 N4 B1 174.0(6) . . . . ? Ir1 N3 N4 B1 -15.3(8) . . . . ? C43 Ir1 N5 C6 40.9(8) . . . . ? C16 Ir1 N5 C6 -49.9(8) . . . . ? N3 Ir1 N5 C6 132.7(8) . . . . ? N1 Ir1 N5 C6 -140.7(8) . . . . ? C43 Ir1 N5 N6 -125.2(5) . . . . ? C16 Ir1 N5 N6 143.9(5) . . . . ? N3 Ir1 N5 N6 -33.4(5) . . . . ? N1 Ir1 N5 N6 53.2(5) . . . . ? C6 N5 N6 C8 -0.1(8) . . . . ? Ir1 N5 N6 C8 169.8(5) . . . . ? C6 N5 N6 B1 173.5(7) . . . . ? Ir1 N5 N6 B1 -16.6(8) . . . . ? C37 Ir2 N7 C22 34.2(9) . . . . ? C40 Ir2 N7 C22 -48.4(9) . . . . ? N11 Ir2 N7 C22 -142.5(9) . . . . ? N9 Ir2 N7 C22 129.1(9) . . . . ? C37 Ir2 N7 N8 -140.3(6) . . . . ? C40 Ir2 N7 N8 137.1(6) . . . . ? N11 Ir2 N7 N8 43.0(5) . . . . ? N9 Ir2 N7 N8 -45.4(5) . . . . ? C22 N7 N8 C24 0.5(9) . . . . ? Ir2 N7 N8 C24 176.5(5) . . . . ? C22 N7 N8 B2 -174.5(7) . . . . ? Ir2 N7 N8 B2 1.5(9) . . . . ? C57 Ir2 N9 C27 43.1(9) . . . . ? C37 Ir2 N9 C27 -48.1(9) . . . . ? N11 Ir2 N9 C27 134.4(9) . . . . ? N7 Ir2 N9 C27 -139.1(9) . . . . ? C57 Ir2 N9 N10 -129.8(6) . . . . ? C37 Ir2 N9 N10 139.1(6) . . . . ? N11 Ir2 N9 N10 -38.4(6) . . . . ? N7 Ir2 N9 N10 48.1(6) . . . . ? C27 N9 N10 C29 -0.1(9) . . . . ? Ir2 N9 N10 C29 174.7(6) . . . . ? C27 N9 N10 B2 -179.8(8) . . . . ? Ir2 N9 N10 B2 -5.0(10) . . . . ? C57 Ir2 N11 C32 -42.2(10) . . . . ? C40 Ir2 N11 C32 50.2(10) . . . . ? N9 Ir2 N11 C32 -132.2(10) . . . . ? N7 Ir2 N11 C32 142.9(10) . . . . ? C57 Ir2 N11 N12 128.8(6) . . . . ? C40 Ir2 N11 N12 -138.8(6) . . . . ? N9 Ir2 N11 N12 38.8(6) . . . . ? N7 Ir2 N11 N12 -46.1(6) . . . . ? C32 N11 N12 C34 1.2(10) . . . . ? Ir2 N11 N12 C34 -172.1(6) . . . . ? C32 N11 N12 B2 177.0(8) . . . . ? Ir2 N11 N12 B2 3.7(9) . . . . ? N2 N1 C1 C2 -0.6(8) . . . . ? Ir1 N1 C1 C2 -170.3(5) . . . . ? N2 N1 C1 C4 179.5(7) . . . . ? Ir1 N1 C1 C4 9.8(12) . . . . ? N1 C1 C2 C3 0.4(9) . . . . ? C4 C1 C2 C3 -179.8(7) . . . . ? C1 C2 C3 N2 0.0(8) . . . . ? C1 C2 C3 C5 179.8(8) . . . . ? N1 N2 C3 C2 -0.4(8) . . . . ? B1 N2 C3 C2 -172.0(7) . . . . ? N1 N2 C3 C5 179.8(7) . . . . ? B1 N2 C3 C5 8.2(11) . . . . ? N6 N5 C6 C7 0.1(9) . . . . ? Ir1 N5 C6 C7 -167.0(6) . . . . ? N6 N5 C6 C9 -175.7(7) . . . . ? Ir1 N5 C6 C9 17.3(12) . . . . ? N5 C6 C7 C8 0.0(10) . . . . ? C9 C6 C7 C8 175.2(8) . . . . ? N5 N6 C8 C7 0.1(8) . . . . ? B1 N6 C8 C7 -172.7(7) . . . . ? N5 N6 C8 C10 -178.7(7) . . . . ? B1 N6 C8 C10 8.5(12) . . . . ? C6 C7 C8 N6 0.0(9) . . . . ? C6 C7 C8 C10 178.7(8) . . . . ? N4 N3 C11 C12 0.0(8) . . . . ? Ir1 N3 C11 C12 -167.9(6) . . . . ? N4 N3 C11 C14 -178.6(7) . . . . ? Ir1 N3 C11 C14 13.5(12) . . . . ? N3 C11 C12 C13 1.5(9) . . . . ? C14 C11 C12 C13 -180.0(8) . . . . ? N3 N4 C13 C12 2.5(8) . . . . ? B1 N4 C13 C12 -172.5(7) . . . . ? N3 N4 C13 C15 -175.5(6) . . . . ? B1 N4 C13 C15 9.6(12) . . . . ? C11 C12 C13 N4 -2.4(9) . . . . ? C11 C12 C13 C15 175.3(7) . . . . ? C43 Ir1 C16 C17 86.4(6) . . . . ? C19 Ir1 C16 C17 -2.6(6) . . . . ? N5 Ir1 C16 C17 178.8(6) . . . . ? N1 Ir1 C16 C17 -95.9(6) . . . . ? Ir1 C16 C17 C18 1.7(11) . . . . ? Ir1 C16 C17 C20 177.2(7) . . . . ? C16 C17 C18 C21 178.5(9) . . . . ? C20 C17 C18 C21 3.4(16) . . . . ? C16 C17 C18 C19 0.9(13) . . . . ? C20 C17 C18 C19 -174.2(9) . . . . ? C17 C18 C19 Ir1 -3.0(10) . . . . ? C21 C18 C19 Ir1 179.1(6) . . . . ? C43 Ir1 C19 C18 -87.7(6) . . . . ? C16 Ir1 C19 C18 3.0(6) . . . . ? N3 Ir1 C19 C18 -179.5(6) . . . . ? N1 Ir1 C19 C18 93.9(6) . . . . ? N8 N7 C22 C23 -0.1(10) . . . . ? Ir2 N7 C22 C23 -174.7(6) . . . . ? N8 N7 C22 C25 -178.7(9) . . . . ? Ir2 N7 C22 C25 6.7(15) . . . . ? N7 C22 C23 C24 -0.4(11) . . . . ? C25 C22 C23 C24 178.2(9) . . . . ? N7 N8 C24 C23 -0.8(10) . . . . ? B2 N8 C24 C23 173.7(8) . . . . ? N7 N8 C24 C26 179.8(8) . . . . ? B2 N8 C24 C26 -5.6(14) . . . . ? C22 C23 C24 N8 0.8(11) . . . . ? C22 C23 C24 C26 -179.9(9) . . . . ? N10 N9 C27 C28 0.3(10) . . . . ? Ir2 N9 C27 C28 -173.1(6) . . . . ? N10 N9 C27 C30 -179.7(7) . . . . ? Ir2 N9 C27 C30 7.0(14) . . . . ? N9 C27 C28 C29 -0.3(11) . . . . ? C30 C27 C28 C29 179.7(9) . . . . ? C27 C28 C29 N10 0.2(11) . . . . ? C27 C28 C29 C31 179.9(9) . . . . ? N9 N10 C29 C28 0.0(10) . . . . ? B2 N10 C29 C28 179.6(10) . . . . ? N9 N10 C29 C31 -179.8(8) . . . . ? B2 N10 C29 C31 -0.1(16) . . . . ? N12 N11 C32 C33 -0.2(11) . . . . ? Ir2 N11 C32 C33 171.3(7) . . . . ? N12 N11 C32 C35 -179.8(10) . . . . ? Ir2 N11 C32 C35 -8.3(16) . . . . ? N11 C32 C33 C34 -1.0(13) . . . . ? C35 C32 C33 C34 178.6(11) . . . . ? C32 C33 C34 N12 1.7(12) . . . . ? C32 C33 C34 C36 -178.4(10) . . . . ? N11 N12 C34 C33 -1.8(11) . . . . ? B2 N12 C34 C33 -177.1(9) . . . . ? N11 N12 C34 C36 178.3(9) . . . . ? B2 N12 C34 C36 3.0(16) . . . . ? C57 Ir2 C37 C38 89.5(6) . . . . ? C40 Ir2 C37 C38 -2.6(6) . . . . ? N9 Ir2 C37 C38 179.7(6) . . . . ? N7 Ir2 C37 C38 -95.4(6) . . . . ? Ir2 C37 C38 C39 -0.7(10) . . . . ? Ir2 C37 C38 C41 177.1(6) . . . . ? C37 C38 C39 C42 176.2(10) . . . . ? C41 C38 C39 C42 -1.4(16) . . . . ? C37 C38 C39 C40 5.2(13) . . . . ? C41 C38 C39 C40 -172.4(8) . . . . ? C38 C39 C40 Ir2 -7.0(11) . . . . ? C42 C39 C40 Ir2 -178.9(8) . . . . ? C57 Ir2 C40 C39 -85.8(7) . . . . ? C37 Ir2 C40 C39 5.0(7) . . . . ? N11 Ir2 C40 C39 -177.3(7) . . . . ? N7 Ir2 C40 C39 96.1(7) . . . . ? C47 N13 C43 C44 1.2(10) . . . . ? C47 N13 C43 Ir1 -175.7(6) . . . . ? C19 Ir1 C43 N13 43.2(6) . . . . ? C16 Ir1 C43 N13 -39.1(6) . . . . ? N5 Ir1 C43 N13 -136.0(6) . . . . ? N3 Ir1 C43 N13 137.2(6) . . . . ? C19 Ir1 C43 C44 -133.3(6) . . . . ? C16 Ir1 C43 C44 144.3(6) . . . . ? N5 Ir1 C43 C44 47.4(6) . . . . ? N3 Ir1 C43 C44 -39.4(6) . . . . ? N13 C43 C44 C45 -2.4(10) . . . . ? Ir1 C43 C44 C45 174.3(6) . . . . ? C43 C44 C45 C46 1.4(12) . . . . ? C44 C45 C46 C47 1.1(13) . . . . ? C45 C46 C47 N13 -2.3(12) . . . . ? C45 C46 C47 C48 173.5(8) . . . . ? C43 N13 C47 C46 1.1(12) . . . . ? C43 N13 C47 C48 -175.1(7) . . . . ? C52 N14 C48 C49 0.6(12) . . . . ? C52 N14 C48 C47 -175.0(7) . . . . ? C46 C47 C48 N14 36.7(12) . . . . ? N13 C47 C48 N14 -147.4(7) . . . . ? C46 C47 C48 C49 -139.0(9) . . . . ? N13 C47 C48 C49 37.0(11) . . . . ? N14 C48 C49 C50 -2.5(13) . . . . ? C47 C48 C49 C50 172.9(8) . . . . ? C48 C49 C50 C51 2.9(14) . . . . ? C49 C50 C51 C52 -1.6(15) . . . . ? C48 N14 C52 C51 0.9(12) . . . . ? C48 N14 C52 C53 -179.9(7) . . . . ? C50 C51 C52 N14 -0.4(14) . . . . ? C50 C51 C52 C53 -179.6(9) . . . . ? C57 N15 C53 C54 0.7(12) . . . . ? C57 N15 C53 C52 179.5(8) . . . . ? N14 C52 C53 C54 -161.0(8) . . . . ? C51 C52 C53 C54 18.2(14) . . . . ? N14 C52 C53 N15 20.2(11) . . . . ? C51 C52 C53 N15 -160.6(8) . . . . ? N15 C53 C54 C55 -1.6(13) . . . . ? C52 C53 C54 C55 179.6(8) . . . . ? C53 C54 C55 C56 1.2(14) . . . . ? C54 C55 C56 C57 0.3(15) . . . . ? C53 N15 C57 C56 0.8(12) . . . . ? C53 N15 C57 Ir2 179.3(6) . . . . ? C55 C56 C57 N15 -1.2(13) . . . . ? C55 C56 C57 Ir2 -179.8(8) . . . . ? C37 Ir2 C57 N15 -37.7(7) . . . . ? C40 Ir2 C57 N15 44.9(8) . . . . ? N11 Ir2 C57 N15 139.2(7) . . . . ? N9 Ir2 C57 N15 -132.7(7) . . . . ? C37 Ir2 C57 C56 140.7(7) . . . . ? C40 Ir2 C57 C56 -136.7(7) . . . . ? N11 Ir2 C57 C56 -42.4(7) . . . . ? N9 Ir2 C57 C56 45.7(7) . . . . ? C13 N4 B1 N6 125.4(8) . . . . ? N3 N4 B1 N6 -49.2(9) . . . . ? C13 N4 B1 N2 -116.4(8) . . . . ? N3 N4 B1 N2 69.0(8) . . . . ? C8 N6 B1 N4 -117.8(8) . . . . ? N5 N6 B1 N4 70.0(8) . . . . ? C8 N6 B1 N2 122.9(8) . . . . ? N5 N6 B1 N2 -49.3(9) . . . . ? N1 N2 B1 N4 -49.9(9) . . . . ? C3 N2 B1 N4 121.0(8) . . . . ? N1 N2 B1 N6 69.4(8) . . . . ? C3 N2 B1 N6 -119.7(8) . . . . ? C29 N10 B2 N12 -115.3(11) . . . . ? N9 N10 B2 N12 64.4(10) . . . . ? C29 N10 B2 N8 123.0(10) . . . . ? N9 N10 B2 N8 -57.4(10) . . . . ? C34 N12 B2 N10 110.2(10) . . . . ? N11 N12 B2 N10 -64.5(10) . . . . ? C34 N12 B2 N8 -127.6(9) . . . . ? N11 N12 B2 N8 57.6(10) . . . . ? C24 N8 B2 N10 -112.9(10) . . . . ? N7 N8 B2 N10 60.9(10) . . . . ? C24 N8 B2 N12 124.8(9) . . . . ? N7 N8 B2 N12 -61.4(10) . . . . ? C61A O1A C58A C59A -1(5) . . . . ? O1A C58A C59A C60A 18(4) . . . . ? C58A C59A C60A C61A -31(5) . . . . ? C58A O1A C61A C60A -15(5) . . . . ? C59A C60A C61A O1A 28(5) . . . . ? C61B O1B C58B C59B -16(3) . . . . ? O1B C58B C59B C60B 7(4) . . . . ? C58B C59B C60B C61B 5(4) . . . . ? C58B O1B C61B C60B 21(4) . . . . ? C59B C60B C61B O1B -17(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N15 H15N N14 0.889(19) 2.39(7) 2.735(9) 103(5) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.437 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.156 ###END