# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_contact_letter ; This CIF contains details of the 6 crystal structures in the paper'Luminescent cyanometallates based on phenylpyridine...' by V. L. MacLeod et al, submitted to Dalton Trans. for publication. ; _publ_contact_author_name 'Prof. Mike Ward' loop_ _publ_author_name M.M.Ali V.MacLeod P.Jennison I.Sazanovich C.Hunter J.Weinstein M.Ward #======================================================== data_imw1406 _database_code_depnum_ccdc_archive 'CCDC 834573' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H47 Cl Ir N5 P2' _chemical_formula_weight 1133.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1090(10) _cell_length_b 14.5474(13) _cell_length_c 16.2425(13) _cell_angle_alpha 97.755(6) _cell_angle_beta 109.636(5) _cell_angle_gamma 97.349(6) _cell_volume 2623.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5567 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 22.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 2.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5756 _exptl_absorpt_correction_T_max 0.7204 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27643 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.67 _reflns_number_total 11745 _reflns_number_gt 9037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The argest residual electron density peaks is located very close to the Ir atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1236P)^2^+13.7935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11745 _refine_ls_number_parameters 634 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2222 _refine_ls_wR_factor_gt 0.2050 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.043 _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 0.02232(3) 0.38669(2) 0.26328(2) 0.04142(14) Uani 1 1 d . . . P1 P 0.67109(19) 0.90507(17) 0.31582(14) 0.0378(5) Uani 1 1 d . . . P2 P 0.6551(2) 0.83876(16) 0.13234(15) 0.0371(5) Uani 1 1 d . . . C1 C -0.1095(10) 0.3193(8) 0.0655(7) 0.056(3) Uani 1 1 d . . . H2 H -0.1047 0.2577 0.0779 0.067 Uiso 1 1 calc R . . C2 C -0.1683(11) 0.3302(10) -0.0214(7) 0.066(3) Uani 1 1 d . . . H3 H -0.2037 0.2761 -0.0675 0.079 Uiso 1 1 calc R . . C3 C -0.1753(11) 0.4193(10) -0.0407(7) 0.069(3) Uani 1 1 d . . . H4 H -0.2138 0.4277 -0.0999 0.083 Uiso 1 1 calc R . . C4 C -0.1254(9) 0.4949(9) 0.0279(7) 0.059(3) Uani 1 1 d . . . H5 H -0.1334 0.5565 0.0165 0.070 Uiso 1 1 calc R . . C5 C -0.0628(8) 0.4840(7) 0.1144(6) 0.045(2) Uani 1 1 d . . . C6 C -0.0046(7) 0.5601(6) 0.1908(6) 0.0395(19) Uani 1 1 d . . . C7 C -0.0006(9) 0.6554(8) 0.1863(8) 0.055(3) Uani 1 1 d . . . H8 H -0.0314 0.6741 0.1304 0.066 Uiso 1 1 calc R . . C8 C 0.0494(9) 0.7231(7) 0.2650(9) 0.060(3) Uani 1 1 d . . . H9 H 0.0501 0.7881 0.2629 0.072 Uiso 1 1 calc R . . C9 C 0.0971(9) 0.6961(7) 0.3447(8) 0.057(3) Uani 1 1 d . . . H10 H 0.1317 0.7424 0.3979 0.068 Uiso 1 1 calc R . . C10 C 0.0954(9) 0.6024(7) 0.3484(8) 0.052(2) Uani 1 1 d . . . H11 H 0.1326 0.5857 0.4045 0.062 Uiso 1 1 calc R . . C11 C 0.0416(8) 0.5303(6) 0.2737(6) 0.0407(19) Uani 1 1 d . . . C12 C 0.1913(8) 0.3940(6) 0.2635(7) 0.043(2) Uani 1 1 d . . . C13 C 0.2288(9) 0.3903(7) 0.1898(7) 0.052(2) Uani 1 1 d . . . H13 H 0.1724 0.3892 0.1324 0.063 Uiso 1 1 calc R . . C14 C 0.3488(11) 0.3882(9) 0.2003(9) 0.068(3) Uani 1 1 d . . . H14 H 0.3721 0.3853 0.1498 0.081 Uiso 1 1 calc R . . C15 C 0.4353(11) 0.3904(9) 0.2853(9) 0.072(3) Uani 1 1 d . . . H15 H 0.5161 0.3880 0.2928 0.086 Uiso 1 1 calc R . . C16 C 0.3974(10) 0.3962(9) 0.3566(8) 0.063(3) Uani 1 1 d . . . H16 H 0.4535 0.3981 0.4144 0.076 Uiso 1 1 calc R . . C17 C 0.2797(9) 0.3992(7) 0.3463(7) 0.052(2) Uani 1 1 d . . . C18 C 0.2374(9) 0.4056(7) 0.4219(6) 0.047(2) Uani 1 1 d . . . C19 C 0.3081(11) 0.4236(9) 0.5107(7) 0.065(3) Uani 1 1 d . . . H19 H 0.3921 0.4294 0.5275 0.079 Uiso 1 1 calc R . . C20 C 0.2589(12) 0.4333(9) 0.5754(8) 0.069(3) Uani 1 1 d . . . H20 H 0.3081 0.4482 0.6366 0.083 Uiso 1 1 calc R . . C21 C 0.1367(11) 0.4210(9) 0.5496(8) 0.064(3) Uani 1 1 d . . . H21 H 0.0996 0.4255 0.5927 0.077 Uiso 1 1 calc R . . C22 C 0.0688(10) 0.4019(7) 0.4591(6) 0.050(2) Uani 1 1 d . . . H22 H -0.0156 0.3928 0.4416 0.060 Uiso 1 1 calc R . . C23 C -0.0005(10) 0.2412(7) 0.2420(7) 0.054(3) Uani 1 1 d . . . C24 C -0.1450(9) 0.3804(6) 0.2747(6) 0.042(2) Uani 1 1 d . . . C25 C 0.6296(8) 0.7155(6) 0.1383(6) 0.0406(19) Uani 1 1 d . . . C26 C 0.7248(8) 0.6795(7) 0.1873(7) 0.048(2) Uani 1 1 d . . . H26 H 0.8005 0.7194 0.2174 0.057 Uiso 1 1 calc R . . C27 C 0.7097(10) 0.5835(8) 0.1928(8) 0.059(3) Uani 1 1 d . . . H27 H 0.7761 0.5582 0.2251 0.070 Uiso 1 1 calc R . . C28 C 0.5995(11) 0.5256(8) 0.1516(8) 0.060(3) Uani 1 1 d . . . H28 H 0.5899 0.4607 0.1557 0.072 Uiso 1 1 calc R . . C29 C 0.5036(11) 0.5624(8) 0.1047(9) 0.066(3) Uani 1 1 d . . . H29 H 0.4272 0.5229 0.0774 0.079 Uiso 1 1 calc R . . C30 C 0.5173(9) 0.6572(7) 0.0967(7) 0.053(2) Uani 1 1 d . . . H30 H 0.4510 0.6819 0.0633 0.064 Uiso 1 1 calc R . . C31 C 0.5232(8) 0.8588(7) 0.0491(6) 0.045(2) Uani 1 1 d . . . C32 C 0.4869(11) 0.8084(8) -0.0395(8) 0.066(3) Uani 1 1 d . . . H32 H 0.5349 0.7679 -0.0557 0.080 Uiso 1 1 calc R . . C33 C 0.3826(14) 0.8187(9) -0.1015(8) 0.084(5) Uani 1 1 d . . . H33 H 0.3567 0.7843 -0.1607 0.101 Uiso 1 1 calc R . . C34 C 0.3143(11) 0.8798(10) -0.0774(9) 0.072(4) Uani 1 1 d . . . H34 H 0.2415 0.8870 -0.1201 0.086 Uiso 1 1 calc R . . C35 C 0.3511(11) 0.9282(10) 0.0057(10) 0.073(4) Uani 1 1 d . . . H35 H 0.3037 0.9697 0.0212 0.088 Uiso 1 1 calc R . . C36 C 0.4569(9) 0.9196(8) 0.0704(7) 0.054(2) Uani 1 1 d . . . H36 H 0.4825 0.9561 0.1288 0.065 Uiso 1 1 calc R . . C37 C 0.7819(8) 0.8569(6) 0.0967(6) 0.0404(19) Uani 1 1 d . . . C38 C 0.7910(11) 0.7909(8) 0.0309(8) 0.061(3) Uani 1 1 d . . . H38 H 0.7330 0.7345 0.0054 0.074 Uiso 1 1 calc R . . C39 C 0.8881(12) 0.8088(9) 0.0023(9) 0.070(3) Uani 1 1 d . . . H39 H 0.8944 0.7652 -0.0443 0.084 Uiso 1 1 calc R . . C40 C 0.9722(12) 0.8877(9) 0.0408(10) 0.070(3) Uani 1 1 d . . . H40 H 1.0378 0.8982 0.0216 0.084 Uiso 1 1 calc R . . C41 C 0.9648(11) 0.9527(9) 0.1072(9) 0.067(3) Uani 1 1 d . . . H41 H 1.0250 1.0075 0.1342 0.081 Uiso 1 1 calc R . . C42 C 0.8666(9) 0.9372(7) 0.1348(7) 0.051(2) Uani 1 1 d . . . H42 H 0.8591 0.9824 0.1797 0.061 Uiso 1 1 calc R . . C43 C 0.6524(8) 1.0205(7) 0.3601(6) 0.044(2) Uani 1 1 d . . . C44 C 0.6687(10) 1.0949(8) 0.3212(8) 0.061(3) Uani 1 1 d . . . H44 H 0.6842 1.0863 0.2674 0.074 Uiso 1 1 calc R . . C45 C 0.6623(13) 1.1873(9) 0.3620(10) 0.077(4) Uani 1 1 d . . . H45 H 0.6773 1.2404 0.3365 0.092 Uiso 1 1 calc R . . C46 C 0.6353(13) 1.1987(10) 0.4354(9) 0.080(4) Uani 1 1 d . . . H46 H 0.6274 1.2594 0.4601 0.097 Uiso 1 1 calc R . . C47 C 0.6189(13) 1.1230(10) 0.4759(9) 0.077(4) Uani 1 1 d . . . H47 H 0.6012 1.1315 0.5288 0.093 Uiso 1 1 calc R . . C48 C 0.6285(11) 1.0351(8) 0.4383(7) 0.059(3) Uani 1 1 d . . . H48 H 0.6184 0.9832 0.4666 0.070 Uiso 1 1 calc R . . C49 C 0.5442(8) 0.8213(7) 0.3092(6) 0.043(2) Uani 1 1 d . . . C50 C 0.4329(8) 0.8466(8) 0.2809(7) 0.053(2) Uani 1 1 d . . . H50 H 0.4260 0.9092 0.2722 0.064 Uiso 1 1 calc R . . C51 C 0.3320(10) 0.7807(9) 0.2654(8) 0.063(3) Uani 1 1 d . . . H51 H 0.2557 0.7981 0.2452 0.076 Uiso 1 1 calc R . . C52 C 0.3405(10) 0.6911(9) 0.2785(8) 0.064(3) Uani 1 1 d . . . H52 H 0.2703 0.6466 0.2681 0.077 Uiso 1 1 calc R . . C53 C 0.4499(12) 0.6645(8) 0.3067(9) 0.068(3) Uani 1 1 d . . . H53 H 0.4552 0.6018 0.3158 0.082 Uiso 1 1 calc R . . C54 C 0.5551(10) 0.7304(8) 0.3223(7) 0.054(2) Uani 1 1 d . . . H54 H 0.6312 0.7126 0.3413 0.065 Uiso 1 1 calc R . . C55 C 0.8010(8) 0.8798(7) 0.3960(6) 0.047(2) Uani 1 1 d . . . C56 C 0.7995(11) 0.8525(9) 0.4732(7) 0.065(3) Uani 1 1 d . . . H56 H 0.7262 0.8415 0.4828 0.078 Uiso 1 1 calc R . . C57 C 0.9029(14) 0.8408(10) 0.5372(9) 0.085(4) Uani 1 1 d . . . H57 H 0.9000 0.8196 0.5894 0.102 Uiso 1 1 calc R . . C58 C 1.0097(14) 0.8599(11) 0.5254(11) 0.099(6) Uani 1 1 d . . . H58 H 1.0816 0.8541 0.5701 0.119 Uiso 1 1 calc R . . C59 C 1.0117(11) 0.8867(10) 0.4509(11) 0.080(4) Uani 1 1 d . . . H59 H 1.0860 0.8987 0.4428 0.096 Uiso 1 1 calc R . . C60 C 0.9090(9) 0.8979(8) 0.3840(8) 0.060(3) Uani 1 1 d . . . H60 H 0.9131 0.9175 0.3314 0.072 Uiso 1 1 calc R . . C1S C 0.276(2) 0.1351(12) 0.2707(11) 0.059(5) Uiso 0.50 1 d PD . . Cl1X Cl 0.3423(18) 0.1137(15) 0.1902(10) 0.068(5) Uiso 0.228(17) 1 d PDU A 1 Cl2X Cl 0.2915(19) 0.0611(15) 0.3404(12) 0.070(5) Uiso 0.228(17) 1 d PDU A 1 Cl1Y Cl 0.3029(18) 0.0792(14) 0.1783(9) 0.077(4) Uiso 0.272(17) 1 d PDU A 2 Cl2Y Cl 0.2554(16) 0.0290(12) 0.3219(10) 0.071(4) Uiso 0.272(17) 1 d PDU A 2 N1 N 0.6853(7) 0.9092(6) 0.2229(5) 0.0427(17) Uani 1 1 d . . . N2 N -0.0596(7) 0.3942(6) 0.1317(5) 0.0440(17) Uani 1 1 d . . . N3 N 0.1146(7) 0.3959(5) 0.3975(5) 0.0439(17) Uani 1 1 d . . . N4 N -0.0102(10) 0.1616(7) 0.2283(8) 0.084(4) Uani 1 1 d . . . N5 N -0.2381(8) 0.3792(7) 0.2787(7) 0.061(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0457(2) 0.0384(2) 0.0339(2) 0.00664(13) 0.00631(15) 0.00790(14) P1 0.0319(11) 0.0478(12) 0.0303(10) 0.0061(9) 0.0081(9) 0.0052(9) P2 0.0350(11) 0.0425(11) 0.0320(11) 0.0080(9) 0.0113(9) 0.0025(9) C1 0.056(6) 0.063(6) 0.038(5) 0.001(5) 0.008(5) 0.007(5) C2 0.062(7) 0.092(9) 0.029(5) 0.003(5) 0.007(5) -0.001(6) C3 0.065(7) 0.107(10) 0.033(5) 0.027(6) 0.009(5) 0.011(7) C4 0.051(6) 0.087(8) 0.048(6) 0.037(6) 0.019(5) 0.017(6) C5 0.029(4) 0.066(6) 0.045(5) 0.018(4) 0.018(4) 0.013(4) C6 0.031(4) 0.043(4) 0.054(5) 0.017(4) 0.024(4) 0.009(3) C7 0.041(5) 0.067(6) 0.075(7) 0.037(6) 0.031(5) 0.017(5) C8 0.040(5) 0.038(5) 0.110(10) 0.015(6) 0.037(6) 0.002(4) C9 0.048(6) 0.043(5) 0.078(8) 0.001(5) 0.028(6) 0.001(4) C10 0.050(6) 0.046(5) 0.058(6) 0.009(4) 0.019(5) 0.005(4) C11 0.037(4) 0.043(4) 0.044(5) 0.004(4) 0.019(4) 0.008(4) C12 0.038(5) 0.035(4) 0.056(6) 0.011(4) 0.014(4) 0.007(4) C13 0.054(6) 0.058(6) 0.045(5) 0.010(5) 0.017(5) 0.008(5) C14 0.066(7) 0.069(7) 0.065(7) 0.003(6) 0.029(6) -0.005(6) C15 0.057(7) 0.078(8) 0.084(9) 0.006(7) 0.034(7) 0.013(6) C16 0.047(6) 0.077(8) 0.057(7) 0.009(6) 0.008(5) 0.010(5) C17 0.048(5) 0.048(5) 0.048(6) 0.005(4) 0.004(4) 0.002(4) C18 0.051(5) 0.050(5) 0.037(5) 0.006(4) 0.013(4) 0.009(4) C19 0.062(7) 0.073(7) 0.044(6) 0.007(5) -0.002(5) 0.011(6) C20 0.080(8) 0.076(8) 0.038(6) 0.006(5) 0.008(6) 0.007(6) C21 0.069(8) 0.082(8) 0.045(6) 0.013(6) 0.023(6) 0.015(6) C22 0.054(6) 0.058(6) 0.038(5) 0.013(4) 0.014(4) 0.015(5) C23 0.062(6) 0.043(5) 0.039(5) 0.004(4) -0.006(4) 0.017(5) C24 0.053(6) 0.037(4) 0.038(5) 0.013(4) 0.016(4) 0.008(4) C25 0.038(5) 0.043(4) 0.041(5) 0.012(4) 0.015(4) 0.003(4) C26 0.037(5) 0.056(5) 0.055(6) 0.019(5) 0.020(4) 0.009(4) C27 0.056(6) 0.066(7) 0.070(7) 0.032(6) 0.031(6) 0.022(5) C28 0.073(7) 0.053(6) 0.069(7) 0.027(5) 0.040(6) 0.014(5) C29 0.052(6) 0.056(6) 0.078(8) 0.019(6) 0.012(6) -0.004(5) C30 0.044(5) 0.050(5) 0.054(6) 0.012(5) 0.005(5) -0.002(4) C31 0.042(5) 0.045(5) 0.040(5) 0.011(4) 0.004(4) 0.001(4) C32 0.076(8) 0.054(6) 0.052(6) 0.003(5) 0.005(6) 0.011(6) C33 0.105(11) 0.063(7) 0.044(6) 0.017(5) -0.020(7) -0.009(7) C34 0.049(6) 0.081(8) 0.067(8) 0.034(7) -0.003(6) -0.004(6) C35 0.053(7) 0.096(9) 0.081(9) 0.045(8) 0.023(6) 0.023(6) C36 0.048(5) 0.063(6) 0.048(6) 0.018(5) 0.013(5) 0.007(5) C37 0.041(5) 0.043(4) 0.044(5) 0.012(4) 0.021(4) 0.007(4) C38 0.073(7) 0.049(6) 0.064(7) 0.002(5) 0.032(6) 0.006(5) C39 0.085(9) 0.067(7) 0.080(8) 0.002(6) 0.060(7) 0.022(7) C40 0.075(8) 0.064(7) 0.093(10) 0.020(7) 0.058(8) 0.012(6) C41 0.066(7) 0.064(7) 0.074(8) 0.009(6) 0.037(6) -0.010(6) C42 0.047(5) 0.045(5) 0.065(7) 0.003(5) 0.030(5) 0.003(4) C43 0.035(4) 0.050(5) 0.044(5) 0.012(4) 0.009(4) 0.003(4) C44 0.063(7) 0.064(7) 0.059(7) 0.019(5) 0.019(6) 0.021(5) C45 0.089(9) 0.057(7) 0.087(10) 0.024(7) 0.030(8) 0.018(6) C46 0.093(10) 0.067(8) 0.072(9) -0.007(7) 0.020(7) 0.030(7) C47 0.090(10) 0.081(9) 0.063(8) -0.004(7) 0.039(7) 0.013(7) C48 0.073(7) 0.058(6) 0.048(6) 0.011(5) 0.027(5) 0.009(5) C49 0.037(5) 0.058(5) 0.035(4) 0.008(4) 0.016(4) 0.002(4) C50 0.037(5) 0.070(7) 0.056(6) 0.012(5) 0.021(5) 0.006(5) C51 0.046(6) 0.085(8) 0.061(7) 0.011(6) 0.026(5) 0.005(6) C52 0.052(6) 0.085(8) 0.055(6) 0.007(6) 0.032(5) -0.014(6) C53 0.079(8) 0.056(6) 0.071(8) 0.015(6) 0.036(7) -0.010(6) C54 0.055(6) 0.063(6) 0.051(6) 0.019(5) 0.022(5) 0.011(5) C55 0.043(5) 0.051(5) 0.038(5) 0.005(4) 0.001(4) 0.010(4) C56 0.058(7) 0.084(8) 0.043(6) 0.019(6) 0.003(5) 0.014(6) C57 0.096(11) 0.076(9) 0.057(8) 0.017(6) -0.012(7) 0.029(8) C58 0.076(10) 0.080(9) 0.088(11) -0.018(8) -0.033(8) 0.039(8) C59 0.050(7) 0.077(8) 0.087(10) -0.015(7) 0.000(7) 0.023(6) C60 0.037(5) 0.068(7) 0.060(6) -0.013(5) 0.006(5) 0.012(5) N1 0.040(4) 0.053(4) 0.034(4) 0.008(3) 0.015(3) 0.002(3) N2 0.038(4) 0.056(5) 0.036(4) 0.010(3) 0.008(3) 0.012(3) N3 0.048(4) 0.043(4) 0.039(4) 0.010(3) 0.012(3) 0.011(3) N4 0.078(7) 0.045(5) 0.087(8) -0.008(5) -0.016(6) 0.014(5) N5 0.053(5) 0.060(5) 0.074(7) 0.018(5) 0.025(5) 0.016(4) _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 C12 2.034(9) . ? Ir1 C11 2.050(9) . ? Ir1 N2 2.057(7) . ? Ir1 C23 2.064(10) . ? Ir1 N3 2.066(8) . ? Ir1 C24 2.088(10) . ? P1 N1 1.583(8) . ? P1 C55 1.791(9) . ? P1 C49 1.797(10) . ? P1 C43 1.808(10) . ? P2 N1 1.576(8) . ? P2 C31 1.800(9) . ? P2 C25 1.802(9) . ? P2 C37 1.817(9) . ? C1 N2 1.336(13) . ? C1 C2 1.391(15) . ? C1 H2 0.9500 . ? C2 C3 1.380(19) . ? C2 H3 0.9500 . ? C3 C4 1.365(17) . ? C3 H4 0.9500 . ? C4 C5 1.396(13) . ? C4 H5 0.9500 . ? C5 N2 1.376(12) . ? C5 C6 1.450(14) . ? C6 C7 1.394(13) . ? C6 C11 1.424(13) . ? C7 C8 1.400(17) . ? C7 H8 0.9500 . ? C8 C9 1.362(17) . ? C8 H9 0.9500 . ? C9 C10 1.370(14) . ? C9 H10 0.9500 . ? C10 C11 1.395(13) . ? C10 H11 0.9500 . ? C12 C17 1.394(14) . ? C12 C13 1.413(14) . ? C13 C14 1.410(16) . ? C13 H13 0.9500 . ? C14 C15 1.418(18) . ? C14 H14 0.9500 . ? C15 C16 1.379(17) . ? C15 H15 0.9500 . ? C16 C17 1.385(15) . ? C16 H16 0.9500 . ? C17 C18 1.477(15) . ? C18 C19 1.376(14) . ? C18 N3 1.387(13) . ? C19 C20 1.371(17) . ? C19 H19 0.9500 . ? C20 C21 1.375(17) . ? C20 H20 0.9500 . ? C21 C22 1.390(15) . ? C21 H21 0.9500 . ? C22 N3 1.296(13) . ? C22 H22 0.9500 . ? C23 N4 1.134(13) . ? C24 N5 1.147(13) . ? C25 C26 1.373(13) . ? C25 C30 1.399(13) . ? C26 C27 1.404(14) . ? C26 H26 0.9500 . ? C27 C28 1.377(16) . ? C27 H27 0.9500 . ? C28 C29 1.375(16) . ? C28 H28 0.9500 . ? C29 C30 1.397(15) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.354(14) . ? C31 C32 1.417(15) . ? C32 C33 1.366(17) . ? C32 H32 0.9500 . ? C33 C34 1.39(2) . ? C33 H33 0.9500 . ? C34 C35 1.332(19) . ? C34 H34 0.9500 . ? C35 C36 1.390(15) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.367(13) . ? C37 C38 1.381(14) . ? C38 C39 1.409(16) . ? C38 H38 0.9500 . ? C39 C40 1.350(18) . ? C39 H39 0.9500 . ? C40 C41 1.370(17) . ? C40 H40 0.9500 . ? C41 C42 1.408(15) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.351(15) . ? C43 C48 1.391(14) . ? C44 C45 1.439(17) . ? C44 H44 0.9500 . ? C45 C46 1.333(19) . ? C45 H45 0.9500 . ? C46 C47 1.38(2) . ? C46 H46 0.9500 . ? C47 C48 1.377(16) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.383(14) . ? C49 C50 1.386(13) . ? C50 C51 1.380(15) . ? C50 H50 0.9500 . ? C51 C52 1.361(18) . ? C51 H51 0.9500 . ? C52 C53 1.374(18) . ? C52 H52 0.9500 . ? C53 C54 1.418(16) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.371(15) . ? C55 C60 1.383(15) . ? C56 C57 1.380(16) . ? C56 H56 0.9500 . ? C57 C58 1.37(2) . ? C57 H57 0.9500 . ? C58 C59 1.33(2) . ? C58 H58 0.9500 . ? C59 C60 1.394(16) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C1S Cl2X 1.649(16) . ? C1S Cl1Y 1.756(16) . ? C1S Cl1X 1.762(16) . ? C1S Cl2Y 1.878(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ir1 C11 89.6(3) . . ? C12 Ir1 N2 97.4(4) . . ? C11 Ir1 N2 80.2(3) . . ? C12 Ir1 C23 89.8(4) . . ? C11 Ir1 C23 175.5(4) . . ? N2 Ir1 C23 95.4(3) . . ? C12 Ir1 N3 80.0(4) . . ? C11 Ir1 N3 93.3(3) . . ? N2 Ir1 N3 173.1(3) . . ? C23 Ir1 N3 91.0(3) . . ? C12 Ir1 C24 175.1(4) . . ? C11 Ir1 C24 90.5(3) . . ? N2 Ir1 C24 87.4(3) . . ? C23 Ir1 C24 90.4(4) . . ? N3 Ir1 C24 95.1(3) . . ? N1 P1 C55 112.5(5) . . ? N1 P1 C49 114.0(4) . . ? C55 P1 C49 108.1(5) . . ? N1 P1 C43 107.9(4) . . ? C55 P1 C43 106.6(4) . . ? C49 P1 C43 107.5(4) . . ? N1 P2 C31 110.5(4) . . ? N1 P2 C25 115.0(4) . . ? C31 P2 C25 106.8(4) . . ? N1 P2 C37 108.2(4) . . ? C31 P2 C37 110.4(4) . . ? C25 P2 C37 105.9(4) . . ? N2 C1 C2 121.1(11) . . ? N2 C1 H2 119.4 . . ? C2 C1 H2 119.4 . . ? C3 C2 C1 120.2(11) . . ? C3 C2 H3 119.9 . . ? C1 C2 H3 119.9 . . ? C4 C3 C2 118.0(10) . . ? C4 C3 H4 121.0 . . ? C2 C3 H4 121.0 . . ? C3 C4 C5 121.7(11) . . ? C3 C4 H5 119.2 . . ? C5 C4 H5 119.2 . . ? N2 C5 C4 118.7(10) . . ? N2 C5 C6 115.7(8) . . ? C4 C5 C6 125.5(10) . . ? C7 C6 C11 121.3(9) . . ? C7 C6 C5 123.7(9) . . ? C11 C6 C5 114.8(8) . . ? C6 C7 C8 119.2(10) . . ? C6 C7 H8 120.4 . . ? C8 C7 H8 120.4 . . ? C9 C8 C7 120.2(10) . . ? C9 C8 H9 119.9 . . ? C7 C8 H9 119.9 . . ? C8 C9 C10 120.3(11) . . ? C8 C9 H10 119.9 . . ? C10 C9 H10 119.9 . . ? C9 C10 C11 123.1(11) . . ? C9 C10 H11 118.5 . . ? C11 C10 H11 118.5 . . ? C10 C11 C6 115.8(9) . . ? C10 C11 Ir1 130.2(8) . . ? C6 C11 Ir1 114.0(6) . . ? C17 C12 C13 116.5(9) . . ? C17 C12 Ir1 115.6(8) . . ? C13 C12 Ir1 127.9(7) . . ? C14 C13 C12 120.9(10) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.9(11) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 117.3(11) . . ? C16 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C15 C16 C17 121.8(11) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C12 122.6(10) . . ? C16 C17 C18 122.6(9) . . ? C12 C17 C18 114.8(9) . . ? C19 C18 N3 119.5(10) . . ? C19 C18 C17 126.1(10) . . ? N3 C18 C17 114.4(8) . . ? C20 C19 C18 120.9(11) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 118.6(11) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C20 C21 C22 118.5(11) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? N3 C22 C21 123.4(10) . . ? N3 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N4 C23 Ir1 177.2(12) . . ? N5 C24 Ir1 177.4(8) . . ? C26 C25 C30 119.9(9) . . ? C26 C25 P2 117.7(7) . . ? C30 C25 P2 122.4(7) . . ? C25 C26 C27 119.7(9) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.6(10) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 119.6(10) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.7(10) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 119.4(10) . . ? C29 C30 H30 120.3 . . ? C25 C30 H30 120.3 . . ? C36 C31 C32 119.7(9) . . ? C36 C31 P2 120.9(8) . . ? C32 C31 P2 119.4(8) . . ? C33 C32 C31 119.5(12) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 119.7(12) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.0(11) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 121.9(13) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C31 C36 C35 119.2(11) . . ? C31 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C42 C37 C38 120.8(9) . . ? C42 C37 P2 119.2(7) . . ? C38 C37 P2 120.0(8) . . ? C37 C38 C39 118.6(11) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 120.3(10) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 121.3(11) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C40 C41 C42 119.1(11) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C37 C42 C41 119.8(10) . . ? C37 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C48 118.9(10) . . ? C44 C43 P1 120.8(8) . . ? C48 C43 P1 120.2(8) . . ? C43 C44 C45 119.4(12) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 120.3(12) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 120.6(12) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 119.1(12) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C47 C48 C43 121.6(11) . . ? C47 C48 H48 119.2 . . ? C43 C48 H48 119.2 . . ? C54 C49 C50 120.5(9) . . ? C54 C49 P1 120.9(7) . . ? C50 C49 P1 118.3(8) . . ? C51 C50 C49 119.9(11) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 120.7(11) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 120.4(11) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C52 C53 C54 120.2(11) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C49 C54 C53 118.3(10) . . ? C49 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C56 C55 C60 118.8(10) . . ? C56 C55 P1 122.1(8) . . ? C60 C55 P1 118.7(8) . . ? C55 C56 C57 121.0(13) . . ? C55 C56 H56 119.5 . . ? C57 C56 H56 119.5 . . ? C58 C57 C56 119.9(14) . . ? C58 C57 H57 120.1 . . ? C56 C57 H57 120.1 . . ? C59 C58 C57 119.3(12) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 122.6(14) . . ? C58 C59 H59 118.7 . . ? C60 C59 H59 118.7 . . ? C55 C60 C59 118.4(13) . . ? C55 C60 H60 120.8 . . ? C59 C60 H60 120.8 . . ? Cl2X C1S Cl1Y 106.5(11) . . ? Cl2X C1S Cl1X 115.3(12) . . ? Cl1Y C1S Cl1X 19.8(6) . . ? Cl2X C1S Cl2Y 16.9(7) . . ? Cl1Y C1S Cl2Y 98.3(11) . . ? Cl1X C1S Cl2Y 111.8(11) . . ? P2 N1 P1 137.0(5) . . ? C1 N2 C5 120.2(9) . . ? C1 N2 Ir1 124.6(7) . . ? C5 N2 Ir1 115.2(6) . . ? C22 N3 C18 119.1(8) . . ? C22 N3 Ir1 125.6(7) . . ? C18 N3 Ir1 115.0(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 N2 C1 C2 C3 0.4(18) . . . . ? C1 C2 C3 C4 -1.3(18) . . . . ? C2 C3 C4 C5 3.6(17) . . . . ? C3 C4 C5 N2 -5.0(15) . . . . ? C3 C4 C5 C6 178.5(10) . . . . ? N2 C5 C6 C7 -178.9(8) . . . . ? C4 C5 C6 C7 -2.4(14) . . . . ? N2 C5 C6 C11 -3.4(11) . . . . ? C4 C5 C6 C11 173.1(9) . . . . ? C11 C6 C7 C8 -0.3(13) . . . . ? C5 C6 C7 C8 174.9(8) . . . . ? C6 C7 C8 C9 2.2(14) . . . . ? C7 C8 C9 C10 -0.6(15) . . . . ? C8 C9 C10 C11 -2.9(16) . . . . ? C9 C10 C11 C6 4.6(14) . . . . ? C9 C10 C11 Ir1 -177.5(8) . . . . ? C7 C6 C11 C10 -2.9(12) . . . . ? C5 C6 C11 C10 -178.5(8) . . . . ? C7 C6 C11 Ir1 178.8(6) . . . . ? C5 C6 C11 Ir1 3.2(9) . . . . ? C12 Ir1 C11 C10 -82.1(9) . . . . ? N2 Ir1 C11 C10 -179.6(9) . . . . ? C23 Ir1 C11 C10 -165(5) . . . . ? N3 Ir1 C11 C10 -2.1(9) . . . . ? C24 Ir1 C11 C10 93.1(9) . . . . ? C12 Ir1 C11 C6 95.9(7) . . . . ? N2 Ir1 C11 C6 -1.7(6) . . . . ? C23 Ir1 C11 C6 13(5) . . . . ? N3 Ir1 C11 C6 175.9(6) . . . . ? C24 Ir1 C11 C6 -88.9(6) . . . . ? C11 Ir1 C12 C17 94.6(7) . . . . ? N2 Ir1 C12 C17 174.6(7) . . . . ? C23 Ir1 C12 C17 -89.9(7) . . . . ? N3 Ir1 C12 C17 1.2(7) . . . . ? C24 Ir1 C12 C17 4(4) . . . . ? C11 Ir1 C12 C13 -88.4(9) . . . . ? N2 Ir1 C12 C13 -8.3(9) . . . . ? C23 Ir1 C12 C13 87.1(9) . . . . ? N3 Ir1 C12 C13 178.2(9) . . . . ? C24 Ir1 C12 C13 -179(100) . . . . ? C17 C12 C13 C14 2.5(15) . . . . ? Ir1 C12 C13 C14 -174.5(8) . . . . ? C12 C13 C14 C15 -0.4(17) . . . . ? C13 C14 C15 C16 -1.0(19) . . . . ? C14 C15 C16 C17 0.3(19) . . . . ? C15 C16 C17 C12 1.9(18) . . . . ? C15 C16 C17 C18 -179.9(11) . . . . ? C13 C12 C17 C16 -3.3(15) . . . . ? Ir1 C12 C17 C16 174.1(9) . . . . ? C13 C12 C17 C18 178.4(9) . . . . ? Ir1 C12 C17 C18 -4.2(11) . . . . ? C16 C17 C18 C19 10.6(17) . . . . ? C12 C17 C18 C19 -171.1(10) . . . . ? C16 C17 C18 N3 -172.2(10) . . . . ? C12 C17 C18 N3 6.1(13) . . . . ? N3 C18 C19 C20 -0.9(17) . . . . ? C17 C18 C19 C20 176.2(11) . . . . ? C18 C19 C20 C21 2.5(19) . . . . ? C19 C20 C21 C22 -1.8(19) . . . . ? C20 C21 C22 N3 -0.7(18) . . . . ? C12 Ir1 C23 N4 -36(20) . . . . ? C11 Ir1 C23 N4 47(22) . . . . ? N2 Ir1 C23 N4 62(20) . . . . ? N3 Ir1 C23 N4 -116(20) . . . . ? C24 Ir1 C23 N4 149(20) . . . . ? C12 Ir1 C24 N5 138(19) . . . . ? C11 Ir1 C24 N5 47(20) . . . . ? N2 Ir1 C24 N5 -33(20) . . . . ? C23 Ir1 C24 N5 -128(20) . . . . ? N3 Ir1 C24 N5 141(20) . . . . ? N1 P2 C25 C26 -66.9(9) . . . . ? C31 P2 C25 C26 170.1(8) . . . . ? C37 P2 C25 C26 52.5(9) . . . . ? N1 P2 C25 C30 111.8(9) . . . . ? C31 P2 C25 C30 -11.2(10) . . . . ? C37 P2 C25 C30 -128.9(9) . . . . ? C30 C25 C26 C27 2.3(15) . . . . ? P2 C25 C26 C27 -179.0(8) . . . . ? C25 C26 C27 C28 -2.0(16) . . . . ? C26 C27 C28 C29 0.1(17) . . . . ? C27 C28 C29 C30 1.4(19) . . . . ? C28 C29 C30 C25 -1.1(19) . . . . ? C26 C25 C30 C29 -0.8(16) . . . . ? P2 C25 C30 C29 -179.4(9) . . . . ? N1 P2 C31 C36 -7.1(10) . . . . ? C25 P2 C31 C36 118.7(9) . . . . ? C37 P2 C31 C36 -126.7(9) . . . . ? N1 P2 C31 C32 174.3(8) . . . . ? C25 P2 C31 C32 -59.9(10) . . . . ? C37 P2 C31 C32 54.7(10) . . . . ? C36 C31 C32 C33 -3.0(18) . . . . ? P2 C31 C32 C33 175.6(10) . . . . ? C31 C32 C33 C34 1(2) . . . . ? C32 C33 C34 C35 0(2) . . . . ? C33 C34 C35 C36 0(2) . . . . ? C32 C31 C36 C35 3.2(16) . . . . ? P2 C31 C36 C35 -175.4(9) . . . . ? C34 C35 C36 C31 -1.7(18) . . . . ? N1 P2 C37 C42 -15.8(9) . . . . ? C31 P2 C37 C42 105.2(9) . . . . ? C25 P2 C37 C42 -139.6(8) . . . . ? N1 P2 C37 C38 165.2(9) . . . . ? C31 P2 C37 C38 -73.7(9) . . . . ? C25 P2 C37 C38 41.4(10) . . . . ? C42 C37 C38 C39 -1.4(17) . . . . ? P2 C37 C38 C39 177.6(9) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C39 C40 C41 C42 -1(2) . . . . ? C38 C37 C42 C41 -0.4(16) . . . . ? P2 C37 C42 C41 -179.4(9) . . . . ? C40 C41 C42 C37 1.5(18) . . . . ? N1 P1 C43 C44 -9.2(10) . . . . ? C55 P1 C43 C44 111.8(9) . . . . ? C49 P1 C43 C44 -132.5(9) . . . . ? N1 P1 C43 C48 174.9(8) . . . . ? C55 P1 C43 C48 -64.1(9) . . . . ? C49 P1 C43 C48 51.6(9) . . . . ? C48 C43 C44 C45 0.8(16) . . . . ? P1 C43 C44 C45 -175.2(9) . . . . ? C43 C44 C45 C46 -3(2) . . . . ? C44 C45 C46 C47 3(2) . . . . ? C45 C46 C47 C48 -1(2) . . . . ? C46 C47 C48 C43 -1(2) . . . . ? C44 C43 C48 C47 1.2(17) . . . . ? P1 C43 C48 C47 177.2(10) . . . . ? N1 P1 C49 C54 93.7(9) . . . . ? C55 P1 C49 C54 -32.1(9) . . . . ? C43 P1 C49 C54 -146.8(8) . . . . ? N1 P1 C49 C50 -79.2(8) . . . . ? C55 P1 C49 C50 155.0(8) . . . . ? C43 P1 C49 C50 40.3(9) . . . . ? C54 C49 C50 C51 -0.2(15) . . . . ? P1 C49 C50 C51 172.7(8) . . . . ? C49 C50 C51 C52 0.8(17) . . . . ? C50 C51 C52 C53 -0.7(18) . . . . ? C51 C52 C53 C54 0.0(18) . . . . ? C50 C49 C54 C53 -0.4(15) . . . . ? P1 C49 C54 C53 -173.2(8) . . . . ? C52 C53 C54 C49 0.5(17) . . . . ? N1 P1 C55 C56 -165.3(9) . . . . ? C49 P1 C55 C56 -38.6(10) . . . . ? C43 P1 C55 C56 76.7(10) . . . . ? N1 P1 C55 C60 21.6(9) . . . . ? C49 P1 C55 C60 148.3(8) . . . . ? C43 P1 C55 C60 -96.5(8) . . . . ? C60 C55 C56 C57 -1.6(18) . . . . ? P1 C55 C56 C57 -174.7(10) . . . . ? C55 C56 C57 C58 2(2) . . . . ? C56 C57 C58 C59 -2(2) . . . . ? C57 C58 C59 C60 1(2) . . . . ? C56 C55 C60 C59 0.6(16) . . . . ? P1 C55 C60 C59 173.9(9) . . . . ? C58 C59 C60 C55 -0.4(19) . . . . ? C31 P2 N1 P1 102.6(8) . . . . ? C25 P2 N1 P1 -18.4(9) . . . . ? C37 P2 N1 P1 -136.4(7) . . . . ? C55 P1 N1 P2 93.0(8) . . . . ? C49 P1 N1 P2 -30.5(9) . . . . ? C43 P1 N1 P2 -149.7(7) . . . . ? C2 C1 N2 C5 -1.8(15) . . . . ? C2 C1 N2 Ir1 176.9(8) . . . . ? C4 C5 N2 C1 4.0(13) . . . . ? C6 C5 N2 C1 -179.2(8) . . . . ? C4 C5 N2 Ir1 -174.8(7) . . . . ? C6 C5 N2 Ir1 2.0(10) . . . . ? C12 Ir1 N2 C1 92.8(8) . . . . ? C11 Ir1 N2 C1 -178.9(9) . . . . ? C23 Ir1 N2 C1 2.2(9) . . . . ? N3 Ir1 N2 C1 161(2) . . . . ? C24 Ir1 N2 C1 -88.0(8) . . . . ? C12 Ir1 N2 C5 -88.5(6) . . . . ? C11 Ir1 N2 C5 -0.2(6) . . . . ? C23 Ir1 N2 C5 -179.0(7) . . . . ? N3 Ir1 N2 C5 -21(3) . . . . ? C24 Ir1 N2 C5 90.8(6) . . . . ? C21 C22 N3 C18 2.3(15) . . . . ? C21 C22 N3 Ir1 -170.8(8) . . . . ? C19 C18 N3 C22 -1.5(14) . . . . ? C17 C18 N3 C22 -178.9(9) . . . . ? C19 C18 N3 Ir1 172.3(8) . . . . ? C17 C18 N3 Ir1 -5.1(10) . . . . ? C12 Ir1 N3 C22 175.6(9) . . . . ? C11 Ir1 N3 C22 86.6(8) . . . . ? N2 Ir1 N3 C22 107(2) . . . . ? C23 Ir1 N3 C22 -94.7(9) . . . . ? C24 Ir1 N3 C22 -4.2(9) . . . . ? C12 Ir1 N3 C18 2.3(6) . . . . ? C11 Ir1 N3 C18 -86.7(7) . . . . ? N2 Ir1 N3 C18 -67(3) . . . . ? C23 Ir1 N3 C18 91.9(7) . . . . ? C24 Ir1 N3 C18 -177.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 9.995 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.188 #===END data_ianp1 _database_code_depnum_ccdc_archive 'CCDC 834574' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H68 Cl6 Ir N5 P2' _chemical_formula_weight 1458.14 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' Ir Ir -1.4442 7.9887 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6650(7) _cell_length_b 17.0116(9) _cell_length_c 17.1118(9) _cell_angle_alpha 109.362(2) _cell_angle_beta 99.524(2) _cell_angle_gamma 101.425(2) _cell_volume 3301.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.59 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 2.359 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5189 _exptl_absorpt_correction_T_max 0.7813 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41904 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.56 _reflns_number_total 14404 _reflns_number_gt 10990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure solved using direct methods. Hydrogens added in calculated positions. ; _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^)+(0.0834P)^2^+21.3915P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14404 _refine_ls_number_parameters 772 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.02323(3) 0.253533(18) 1.004274(17) 0.01898(10) Uani 1 1 d . . . C1 C 0.1299(6) 0.1609(5) 1.1071(4) 0.0222(15) Uani 1 1 d . . . H1 H 0.1335 0.2098 1.1558 0.027 Uiso 1 1 calc R . . C2 C 0.1734(7) 0.0982(5) 1.1192(5) 0.0304(17) Uani 1 1 d . . . H2 H 0.2053 0.1024 1.1752 0.036 Uiso 1 1 calc R . . C3 C 0.1706(7) 0.0273(5) 1.0476(5) 0.0294(17) Uani 1 1 d . . . H3 H 0.2016 -0.0172 1.0544 0.035 Uiso 1 1 calc R . . C4 C 0.1234(7) 0.0223(5) 0.9683(5) 0.0270(16) Uani 1 1 d . . . H4 H 0.1222 -0.0257 0.9195 0.032 Uiso 1 1 calc R . . C5 C 0.0763(6) 0.0873(5) 0.9575(4) 0.0220(15) Uani 1 1 d . . . C6 C 0.0219(6) 0.0883(5) 0.8762(4) 0.0224(15) Uani 1 1 d . . . C7 C -0.0004(7) 0.0206(5) 0.7973(5) 0.0293(17) Uani 1 1 d . . . H7 H 0.0198 -0.0310 0.7944 0.035 Uiso 1 1 calc R . . C8 C -0.0515(7) 0.0281(5) 0.7234(5) 0.0287(17) Uani 1 1 d . . . H8 H -0.0651 -0.0184 0.6702 0.034 Uiso 1 1 calc R . . C9 C -0.0833(6) 0.1015(5) 0.7249(4) 0.0245(16) Uani 1 1 d . . . C10 C -0.1364(7) 0.1087(5) 0.6412(5) 0.0301(18) Uani 1 1 d . . . C11 C -0.2478(7) 0.0378(6) 0.5983(5) 0.0358(19) Uani 1 1 d . . . H11A H -0.2342 -0.0193 0.5859 0.054 Uiso 1 1 calc R . . H11B H -0.2827 0.0422 0.5449 0.054 Uiso 1 1 calc R . . H11C H -0.2973 0.0455 0.6370 0.054 Uiso 1 1 calc R . . C12 C -0.0581(8) 0.0930(7) 0.5801(5) 0.043(2) Uani 1 1 d . . . H12A H 0.0132 0.1375 0.6064 0.064 Uiso 1 1 calc R . . H12B H -0.0925 0.0960 0.5258 0.064 Uiso 1 1 calc R . . H12C H -0.0457 0.0358 0.5695 0.064 Uiso 1 1 calc R . . C13 C -0.1581(8) 0.1965(6) 0.6539(5) 0.039(2) Uani 1 1 d . . . H13A H -0.2140 0.2044 0.6870 0.058 Uiso 1 1 calc R . . H13B H -0.1855 0.1991 0.5980 0.058 Uiso 1 1 calc R . . H13C H -0.0889 0.2424 0.6848 0.058 Uiso 1 1 calc R . . C14 C -0.0637(6) 0.1683(5) 0.8051(4) 0.0212(14) Uani 1 1 d . . . H14 H -0.0864 0.2188 0.8072 0.025 Uiso 1 1 calc R . . C15 C -0.0123(6) 0.1639(5) 0.8819(5) 0.0236(15) Uani 1 1 d . . . C16 C -0.1277(7) 0.3495(5) 0.9432(5) 0.0279(17) Uani 1 1 d . . . H16 H -0.1824 0.3169 0.9606 0.033 Uiso 1 1 calc R . . C17 C -0.1593(7) 0.4022(5) 0.9018(5) 0.0295(17) Uani 1 1 d . . . H17 H -0.2342 0.4050 0.8904 0.035 Uiso 1 1 calc R . . C18 C -0.0787(7) 0.4504(5) 0.8778(5) 0.0297(17) Uani 1 1 d . . . H18 H -0.0975 0.4872 0.8495 0.036 Uiso 1 1 calc R . . C19 C 0.0288(7) 0.4447(5) 0.8952(5) 0.0241(15) Uani 1 1 d . . . H19 H 0.0842 0.4777 0.8786 0.029 Uiso 1 1 calc R . . C20 C 0.0577(6) 0.3909(5) 0.9369(4) 0.0219(15) Uani 1 1 d . . . C21 C 0.1663(6) 0.3766(4) 0.9556(4) 0.0193(14) Uani 1 1 d . . . C22 C 0.2618(6) 0.4235(5) 0.9429(4) 0.0231(15) Uani 1 1 d . . . H22 H 0.2577 0.4701 0.9246 0.028 Uiso 1 1 calc R . . C23 C 0.3614(6) 0.4032(5) 0.9565(4) 0.0244(16) Uani 1 1 d . . . H23 H 0.4250 0.4351 0.9467 0.029 Uiso 1 1 calc R . . C24 C 0.3697(6) 0.3349(5) 0.9850(4) 0.0203(14) Uani 1 1 d . . . C25 C 0.4792(7) 0.3098(5) 0.9971(5) 0.0257(16) Uani 1 1 d . . . C26 C 0.5425(7) 0.3243(6) 0.9313(5) 0.0343(19) Uani 1 1 d . . . H26A H 0.4921 0.2972 0.8739 0.051 Uiso 1 1 calc R . . H26B H 0.6051 0.2985 0.9329 0.051 Uiso 1 1 calc R . . H26C H 0.5707 0.3866 0.9452 0.051 Uiso 1 1 calc R . . C27 C 0.5527(7) 0.3663(6) 1.0871(5) 0.0344(19) Uani 1 1 d . . . H27A H 0.5664 0.4274 1.0948 0.052 Uiso 1 1 calc R . . H27B H 0.6238 0.3516 1.0942 0.052 Uiso 1 1 calc R . . H27C H 0.5150 0.3560 1.1298 0.052 Uiso 1 1 calc R . . C28 C 0.4590(8) 0.2146(6) 0.9850(7) 0.042(2) Uani 1 1 d . . . H28A H 0.4246 0.2044 1.0293 0.063 Uiso 1 1 calc R . . H28B H 0.5301 0.1997 0.9896 0.063 Uiso 1 1 calc R . . H28C H 0.4094 0.1785 0.9285 0.063 Uiso 1 1 calc R . . C29 C 0.2747(6) 0.2921(5) 1.0016(4) 0.0228(15) Uani 1 1 d . . . H29 H 0.2800 0.2480 1.0234 0.027 Uiso 1 1 calc R . . C30 C 0.1725(6) 0.3111(4) 0.9877(4) 0.0178(14) Uani 1 1 d . . . C31 C 0.0682(6) 0.3378(4) 1.1301(4) 0.0168(13) Uani 1 1 d . . . C32 C -0.1317(6) 0.2054(5) 1.0188(4) 0.0228(15) Uani 1 1 d . . . C33 C 0.9123(7) 0.7387(5) 0.6084(5) 0.0281(17) Uani 1 1 d . . . C34 C 0.9682(7) 0.8004(5) 0.5818(5) 0.0297(17) Uani 1 1 d . . . H34 H 0.9336 0.8081 0.5322 0.036 Uiso 1 1 calc R . . C35 C 1.0740(8) 0.8502(6) 0.6279(5) 0.039(2) Uani 1 1 d . . . H35 H 1.1119 0.8928 0.6102 0.046 Uiso 1 1 calc R . . C36 C 1.1262(8) 0.8390(6) 0.6999(5) 0.042(2) Uani 1 1 d . . . H36 H 1.1998 0.8729 0.7307 0.051 Uiso 1 1 calc R . . C37 C 1.0700(8) 0.7776(6) 0.7268(5) 0.041(2) Uani 1 1 d . . . H37 H 1.1049 0.7709 0.7769 0.049 Uiso 1 1 calc R . . C38 C 0.9645(7) 0.7267(5) 0.6815(5) 0.0333(19) Uani 1 1 d . . . H38 H 0.9271 0.6839 0.6992 0.040 Uiso 1 1 calc R . . C39 C 0.7583(7) 0.5635(5) 0.5172(5) 0.0273(17) Uani 1 1 d . . . C40 C 0.8481(8) 0.5295(6) 0.5222(6) 0.038(2) Uani 1 1 d . . . H40 H 0.9211 0.5670 0.5483 0.045 Uiso 1 1 calc R . . C41 C 0.8316(9) 0.4400(6) 0.4889(7) 0.048(2) Uani 1 1 d . . . H41 H 0.8937 0.4166 0.4921 0.058 Uiso 1 1 calc R . . C42 C 0.7262(9) 0.3856(6) 0.4514(6) 0.042(2) Uani 1 1 d . . . H42 H 0.7155 0.3247 0.4289 0.051 Uiso 1 1 calc R . . C43 C 0.6349(8) 0.4195(6) 0.4464(5) 0.038(2) Uani 1 1 d . . . H43 H 0.5620 0.3818 0.4203 0.046 Uiso 1 1 calc R . . C44 C 0.6504(7) 0.5075(5) 0.4793(5) 0.0308(18) Uani 1 1 d . . . H44 H 0.5881 0.5307 0.4765 0.037 Uiso 1 1 calc R . . C45 C 0.6884(7) 0.7003(5) 0.6292(4) 0.0261(16) Uani 1 1 d . . . C46 C 0.6892(8) 0.6579(6) 0.6868(5) 0.0352(19) Uani 1 1 d . . . H46 H 0.7294 0.6158 0.6831 0.042 Uiso 1 1 calc R . . C47 C 0.6312(8) 0.6777(6) 0.7488(5) 0.039(2) Uani 1 1 d . . . H47 H 0.6326 0.6501 0.7888 0.047 Uiso 1 1 calc R . . C48 C 0.5713(8) 0.7378(6) 0.7527(5) 0.042(2) Uani 1 1 d . . . H48 H 0.5312 0.7509 0.7955 0.051 Uiso 1 1 calc R . . C49 C 0.5684(8) 0.7793(6) 0.6952(5) 0.037(2) Uani 1 1 d . . . H49 H 0.5256 0.8197 0.6977 0.045 Uiso 1 1 calc R . . C50 C 0.6290(7) 0.7610(5) 0.6340(5) 0.0296(17) Uani 1 1 d . . . H50 H 0.6297 0.7903 0.5954 0.035 Uiso 1 1 calc R . . C51 C 0.5622(6) 0.6174(4) 0.3269(5) 0.0223(15) Uani 1 1 d . . . C52 C 0.5259(7) 0.5761(5) 0.2374(5) 0.0256(16) Uani 1 1 d . . . H52 H 0.5777 0.5780 0.2033 0.031 Uiso 1 1 calc R . . C53 C 0.4150(8) 0.5328(5) 0.1990(5) 0.0350(19) Uani 1 1 d . . . H53 H 0.3907 0.5046 0.1386 0.042 Uiso 1 1 calc R . . C54 C 0.3394(8) 0.5305(6) 0.2485(6) 0.037(2) Uani 1 1 d . . . H54 H 0.2636 0.4991 0.2223 0.044 Uiso 1 1 calc R . . C55 C 0.3748(7) 0.5747(6) 0.3376(6) 0.036(2) Uani 1 1 d . . . H55 H 0.3226 0.5748 0.3715 0.044 Uiso 1 1 calc R . . C56 C 0.4850(7) 0.6179(5) 0.3758(5) 0.0295(17) Uani 1 1 d . . . H56 H 0.5085 0.6483 0.4360 0.035 Uiso 1 1 calc R . . C57 C 0.7300(7) 0.8410(5) 0.3909(5) 0.0280(17) Uani 1 1 d . . . H57 H 0.7120 0.8503 0.4445 0.034 Uiso 1 1 calc R . . C58 C 0.7440(7) 0.9065(5) 0.3604(5) 0.0307(18) Uani 1 1 d . . . H58 H 0.7347 0.9609 0.3926 0.037 Uiso 1 1 calc R . . C59 C 0.7718(7) 0.8937(5) 0.2824(5) 0.0298(17) Uani 1 1 d . . . H59 H 0.7816 0.9397 0.2621 0.036 Uiso 1 1 calc R . . C60 C 0.7850(7) 0.8154(5) 0.2347(5) 0.0290(17) Uani 1 1 d . . . H60 H 0.8053 0.8072 0.1821 0.035 Uiso 1 1 calc R . . C61 C 0.7682(7) 0.7475(5) 0.2645(4) 0.0268(16) Uani 1 1 d . . . H61 H 0.7745 0.6923 0.2311 0.032 Uiso 1 1 calc R . . C62 C 0.7424(6) 0.7609(5) 0.3430(4) 0.0226(15) Uani 1 1 d . . . C63 C 0.7874(7) 0.5973(5) 0.3373(4) 0.0258(16) Uani 1 1 d . . . C64 C 0.9025(7) 0.6314(6) 0.3530(5) 0.0314(18) Uani 1 1 d . . . H64 H 0.9349 0.6921 0.3802 0.038 Uiso 1 1 calc R . . C65 C 0.9682(8) 0.5774(7) 0.3292(6) 0.041(2) Uani 1 1 d . . . H65 H 1.0460 0.6010 0.3396 0.049 Uiso 1 1 calc R . . C66 C 0.9225(8) 0.4889(6) 0.2901(5) 0.038(2) Uani 1 1 d . . . H66 H 0.9685 0.4517 0.2736 0.045 Uiso 1 1 calc R . . C67 C 0.8076(9) 0.4544(6) 0.2750(5) 0.040(2) Uani 1 1 d . . . H67 H 0.7755 0.3936 0.2483 0.048 Uiso 1 1 calc R . . C68 C 0.7411(7) 0.5091(5) 0.2991(5) 0.0308(18) Uani 1 1 d . . . H68 H 0.6633 0.4858 0.2893 0.037 Uiso 1 1 calc R . . N1 N 0.7276(5) 0.7099(4) 0.4780(4) 0.0256(14) Uani 1 1 d . . . N2 N 0.0805(5) 0.1571(4) 1.0273(4) 0.0201(12) Uani 1 1 d . . . N3 N -0.0245(5) 0.3429(4) 0.9593(3) 0.0217(13) Uani 1 1 d . . . N4 N -0.2200(6) 0.1810(5) 1.0256(5) 0.0372(17) Uani 1 1 d . . . N5 N 0.0973(6) 0.3849(4) 1.2006(4) 0.0252(13) Uani 1 1 d . . . P1 P 0.77063(17) 0.67848(13) 0.55248(12) 0.0247(4) Uani 1 1 d . . . P2 P 0.70708(16) 0.67180(12) 0.37714(11) 0.0213(4) Uani 1 1 d . . . C1S C 0.6498(9) 0.1131(6) 0.8240(6) 0.043(2) Uani 1 1 d . . . H1S1 H 0.7262 0.1446 0.8274 0.052 Uiso 1 1 calc R . . H1S2 H 0.6359 0.1352 0.8815 0.052 Uiso 1 1 calc R . . C2S C 0.4042(14) 0.9014(9) 0.8987(10) 0.084(4) Uani 1 1 d . . . H2S1 H 0.3685 0.8920 0.9434 0.100 Uiso 1 1 calc R . . H2S2 H 0.4853 0.9118 0.9198 0.100 Uiso 1 1 calc R . . C3S C 0.4651(8) 0.9237(6) 0.5732(6) 0.038(2) Uani 1 1 d . . . H3S1 H 0.4601 0.9802 0.5708 0.046 Uiso 1 1 calc R . . H3S2 H 0.5314 0.9344 0.6191 0.046 Uiso 1 1 calc R . . Cl1S Cl 0.6395(3) 0.0029(2) 0.79300(19) 0.0808(11) Uani 1 1 d . . . Cl2S Cl 0.5529(3) 0.1331(2) 0.75043(16) 0.0686(9) Uani 1 1 d . . . Cl3S Cl 0.3554(3) 0.8083(2) 0.8068(2) 0.0806(10) Uani 1 1 d . . . Cl4S Cl 0.3797(4) 0.9915(2) 0.8843(3) 0.1001(13) Uani 1 1 d . . . Cl5S Cl 0.4815(2) 0.85763(18) 0.47489(15) 0.0509(6) Uani 1 1 d . . . Cl6S Cl 0.3452(2) 0.87628(16) 0.59845(15) 0.0425(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02205(16) 0.02327(15) 0.01505(13) 0.01062(10) 0.00665(10) 0.00601(10) C1 0.028(4) 0.027(4) 0.018(3) 0.017(3) 0.005(3) 0.008(3) C2 0.033(5) 0.036(4) 0.026(4) 0.016(3) 0.006(3) 0.010(4) C3 0.029(5) 0.026(4) 0.039(4) 0.018(3) 0.013(4) 0.007(3) C4 0.032(5) 0.025(4) 0.028(4) 0.012(3) 0.013(3) 0.008(3) C5 0.021(4) 0.027(4) 0.022(3) 0.013(3) 0.012(3) 0.004(3) C6 0.021(4) 0.025(4) 0.019(3) 0.009(3) 0.006(3) 0.000(3) C7 0.039(5) 0.026(4) 0.025(4) 0.010(3) 0.014(3) 0.007(3) C8 0.034(5) 0.035(4) 0.016(3) 0.007(3) 0.010(3) 0.008(3) C9 0.026(4) 0.028(4) 0.019(3) 0.008(3) 0.008(3) 0.006(3) C10 0.030(5) 0.044(5) 0.015(3) 0.012(3) 0.007(3) 0.005(4) C11 0.029(5) 0.045(5) 0.026(4) 0.009(4) 0.006(3) 0.003(4) C12 0.035(5) 0.075(7) 0.019(4) 0.021(4) 0.008(4) 0.010(5) C13 0.045(6) 0.044(5) 0.025(4) 0.017(4) 0.001(4) 0.010(4) C14 0.018(4) 0.029(4) 0.019(3) 0.011(3) 0.007(3) 0.006(3) C15 0.028(4) 0.021(3) 0.024(4) 0.013(3) 0.009(3) 0.001(3) C16 0.030(5) 0.035(4) 0.025(4) 0.014(3) 0.016(3) 0.012(3) C17 0.029(5) 0.032(4) 0.033(4) 0.016(3) 0.007(3) 0.012(3) C18 0.039(5) 0.031(4) 0.029(4) 0.019(3) 0.011(4) 0.016(4) C19 0.028(4) 0.027(4) 0.024(4) 0.016(3) 0.009(3) 0.010(3) C20 0.026(4) 0.025(4) 0.016(3) 0.009(3) 0.007(3) 0.009(3) C21 0.024(4) 0.021(3) 0.016(3) 0.010(3) 0.008(3) 0.003(3) C22 0.032(4) 0.025(4) 0.019(3) 0.012(3) 0.012(3) 0.013(3) C23 0.028(4) 0.023(4) 0.017(3) 0.006(3) 0.008(3) -0.004(3) C24 0.020(4) 0.027(4) 0.012(3) 0.005(3) 0.005(3) 0.008(3) C25 0.028(4) 0.032(4) 0.023(4) 0.012(3) 0.012(3) 0.011(3) C26 0.032(5) 0.047(5) 0.032(4) 0.020(4) 0.017(4) 0.014(4) C27 0.030(5) 0.043(5) 0.029(4) 0.012(4) 0.005(4) 0.013(4) C28 0.035(5) 0.037(5) 0.066(6) 0.026(4) 0.022(5) 0.018(4) C29 0.033(4) 0.027(4) 0.012(3) 0.012(3) 0.006(3) 0.006(3) C30 0.015(4) 0.024(3) 0.013(3) 0.005(3) 0.006(3) 0.004(3) C31 0.018(4) 0.024(3) 0.012(3) 0.011(3) 0.006(3) 0.005(3) C32 0.025(4) 0.033(4) 0.021(3) 0.017(3) 0.014(3) 0.010(3) C33 0.032(5) 0.033(4) 0.021(4) 0.013(3) 0.007(3) 0.006(3) C34 0.031(5) 0.035(4) 0.021(4) 0.013(3) 0.004(3) 0.003(3) C35 0.035(5) 0.049(5) 0.026(4) 0.015(4) 0.009(4) -0.005(4) C36 0.031(5) 0.057(6) 0.029(4) 0.015(4) 0.004(4) -0.005(4) C37 0.034(5) 0.063(6) 0.018(4) 0.019(4) -0.003(3) 0.001(4) C38 0.037(5) 0.039(5) 0.028(4) 0.023(4) 0.008(4) 0.002(4) C39 0.034(5) 0.032(4) 0.021(4) 0.018(3) 0.006(3) 0.006(3) C40 0.031(5) 0.043(5) 0.043(5) 0.021(4) 0.010(4) 0.010(4) C41 0.059(7) 0.046(6) 0.060(6) 0.032(5) 0.028(5) 0.028(5) C42 0.063(7) 0.030(4) 0.040(5) 0.016(4) 0.022(5) 0.013(4) C43 0.044(6) 0.040(5) 0.031(4) 0.019(4) 0.012(4) 0.000(4) C44 0.039(5) 0.031(4) 0.022(4) 0.016(3) 0.006(3) 0.002(4) C45 0.029(4) 0.033(4) 0.012(3) 0.010(3) 0.004(3) -0.002(3) C46 0.039(5) 0.037(5) 0.030(4) 0.018(4) 0.005(4) 0.004(4) C47 0.052(6) 0.043(5) 0.025(4) 0.020(4) 0.012(4) 0.003(4) C48 0.055(6) 0.043(5) 0.026(4) 0.013(4) 0.019(4) 0.000(4) C49 0.047(6) 0.038(5) 0.026(4) 0.013(3) 0.012(4) 0.005(4) C50 0.035(5) 0.034(4) 0.018(3) 0.010(3) 0.006(3) 0.003(3) C51 0.027(4) 0.021(3) 0.024(3) 0.015(3) 0.008(3) 0.004(3) C52 0.027(4) 0.026(4) 0.025(4) 0.012(3) 0.002(3) 0.008(3) C53 0.037(5) 0.034(4) 0.029(4) 0.011(3) 0.001(4) 0.007(4) C54 0.028(5) 0.039(5) 0.044(5) 0.025(4) -0.002(4) 0.004(4) C55 0.028(5) 0.052(5) 0.041(5) 0.028(4) 0.015(4) 0.011(4) C56 0.030(5) 0.037(4) 0.025(4) 0.016(3) 0.009(3) 0.006(3) C57 0.034(5) 0.031(4) 0.025(4) 0.013(3) 0.014(3) 0.013(3) C58 0.038(5) 0.031(4) 0.033(4) 0.017(3) 0.013(4) 0.017(4) C59 0.028(4) 0.033(4) 0.034(4) 0.023(3) 0.007(3) 0.005(3) C60 0.031(5) 0.039(4) 0.019(3) 0.015(3) 0.008(3) 0.005(3) C61 0.035(5) 0.027(4) 0.015(3) 0.005(3) 0.005(3) 0.007(3) C62 0.020(4) 0.030(4) 0.019(3) 0.011(3) 0.006(3) 0.005(3) C63 0.028(4) 0.036(4) 0.018(3) 0.013(3) 0.007(3) 0.014(3) C64 0.031(5) 0.042(5) 0.032(4) 0.023(4) 0.012(4) 0.014(4) C65 0.034(5) 0.061(6) 0.045(5) 0.033(5) 0.021(4) 0.023(5) C66 0.047(6) 0.057(6) 0.030(4) 0.026(4) 0.019(4) 0.033(5) C67 0.061(7) 0.040(5) 0.026(4) 0.016(4) 0.010(4) 0.025(5) C68 0.034(5) 0.037(4) 0.024(4) 0.013(3) 0.008(3) 0.012(4) N1 0.029(4) 0.029(3) 0.021(3) 0.013(3) 0.005(3) 0.009(3) N2 0.018(3) 0.022(3) 0.024(3) 0.013(2) 0.010(2) 0.003(2) N3 0.036(4) 0.024(3) 0.013(3) 0.010(2) 0.010(2) 0.015(3) N4 0.032(4) 0.040(4) 0.044(4) 0.022(3) 0.010(3) 0.008(3) N5 0.031(4) 0.027(3) 0.022(3) 0.015(3) 0.005(3) 0.008(3) P1 0.0274(11) 0.0296(10) 0.0184(9) 0.0140(8) 0.0045(8) 0.0033(8) P2 0.0244(10) 0.0260(9) 0.0157(8) 0.0103(7) 0.0064(7) 0.0064(8) C1S 0.049(6) 0.049(5) 0.030(4) 0.013(4) 0.007(4) 0.014(5) C2S 0.093(11) 0.095(10) 0.094(11) 0.060(9) 0.044(9) 0.034(9) C3S 0.033(5) 0.049(5) 0.034(4) 0.020(4) 0.009(4) 0.007(4) Cl1S 0.125(3) 0.0560(17) 0.0471(15) 0.0130(13) -0.0207(17) 0.0387(18) Cl2S 0.112(3) 0.0690(18) 0.0358(12) 0.0159(12) 0.0106(14) 0.0621(18) Cl3S 0.077(2) 0.086(2) 0.085(2) 0.0318(19) 0.0203(19) 0.0357(19) Cl4S 0.092(3) 0.064(2) 0.137(4) 0.041(2) 0.013(3) 0.0156(19) Cl5S 0.0491(15) 0.0734(17) 0.0362(12) 0.0184(11) 0.0174(11) 0.0279(13) Cl6S 0.0418(13) 0.0534(13) 0.0460(12) 0.0284(11) 0.0211(10) 0.0175(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N2 2.044(6) . ? Ir1 C15 2.052(7) . ? Ir1 C31 2.059(6) . ? Ir1 C30 2.059(7) . ? Ir1 C32 2.059(7) . ? Ir1 N3 2.062(6) . ? C1 C2 1.350(11) . ? C1 N2 1.380(9) . ? C1 H1 0.9500 . ? C2 C3 1.394(11) . ? C2 H2 0.9500 . ? C3 C4 1.357(11) . ? C3 H3 0.9500 . ? C4 C5 1.405(11) . ? C4 H4 0.9500 . ? C5 N2 1.361(9) . ? C5 C6 1.454(10) . ? C6 C7 1.394(10) . ? C6 C15 1.415(10) . ? C7 C8 1.380(11) . ? C7 H7 0.9500 . ? C8 C9 1.379(11) . ? C8 H8 0.9500 . ? C9 C14 1.407(10) . ? C9 C10 1.532(10) . ? C10 C13 1.523(12) . ? C10 C11 1.543(12) . ? C10 C12 1.553(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.400(10) . ? C14 H14 0.9500 . ? C16 N3 1.325(10) . ? C16 C17 1.391(11) . ? C16 H16 0.9500 . ? C17 C18 1.385(11) . ? C17 H17 0.9500 . ? C18 C19 1.375(11) . ? C18 H18 0.9500 . ? C19 C20 1.401(10) . ? C19 H19 0.9500 . ? C20 N3 1.378(9) . ? C20 C21 1.447(11) . ? C21 C22 1.402(10) . ? C21 C30 1.406(10) . ? C22 C23 1.376(11) . ? C22 H22 0.9500 . ? C23 C24 1.417(10) . ? C23 H23 0.9500 . ? C24 C29 1.400(10) . ? C24 C25 1.532(10) . ? C25 C28 1.526(12) . ? C25 C27 1.533(11) . ? C25 C26 1.543(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.397(11) . ? C29 H29 0.9500 . ? C31 N5 1.153(9) . ? C32 N4 1.152(10) . ? C33 C34 1.392(11) . ? C33 C38 1.412(11) . ? C33 P1 1.800(8) . ? C34 C35 1.375(12) . ? C34 H34 0.9500 . ? C35 C36 1.389(13) . ? C35 H35 0.9500 . ? C36 C37 1.393(13) . ? C36 H36 0.9500 . ? C37 C38 1.376(12) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.376(12) . ? C39 C44 1.406(12) . ? C39 P1 1.811(8) . ? C40 C41 1.395(13) . ? C40 H40 0.9500 . ? C41 C42 1.373(15) . ? C41 H41 0.9500 . ? C42 C43 1.394(14) . ? C42 H42 0.9500 . ? C43 C44 1.372(12) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.383(12) . ? C45 C46 1.401(11) . ? C45 P1 1.796(7) . ? C46 C47 1.378(12) . ? C46 H46 0.9500 . ? C47 C48 1.380(14) . ? C47 H47 0.9500 . ? C48 C49 1.389(12) . ? C48 H48 0.9500 . ? C49 C50 1.388(11) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.386(10) . ? C51 C52 1.406(10) . ? C51 P2 1.801(8) . ? C52 C53 1.383(12) . ? C52 H52 0.9500 . ? C53 C54 1.382(13) . ? C53 H53 0.9500 . ? C54 C55 1.403(12) . ? C54 H54 0.9500 . ? C55 C56 1.374(12) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.372(11) . ? C57 C62 1.393(10) . ? C57 H57 0.9500 . ? C58 C59 1.395(11) . ? C58 H58 0.9500 . ? C59 C60 1.372(11) . ? C59 H59 0.9500 . ? C60 C61 1.404(11) . ? C60 H60 0.9500 . ? C61 C62 1.391(9) . ? C61 H61 0.9500 . ? C62 P2 1.801(7) . ? C63 C68 1.376(11) . ? C63 C64 1.403(12) . ? C63 P2 1.809(8) . ? C64 C65 1.366(12) . ? C64 H64 0.9500 . ? C65 C66 1.381(14) . ? C65 H65 0.9500 . ? C66 C67 1.402(14) . ? C66 H66 0.9500 . ? C67 C68 1.385(12) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? N1 P2 1.585(6) . ? N1 P1 1.594(6) . ? C1S Cl1S 1.742(10) . ? C1S Cl2S 1.773(10) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S Cl4S 1.710(14) . ? C2S Cl3S 1.733(16) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S Cl5S 1.758(9) . ? C3S Cl6S 1.762(9) . ? C3S H3S1 0.9900 . ? C3S H3S2 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 N2 Ir1 C15 79.5(3) . . ? N2 Ir1 C31 95.8(3) . . ? C15 Ir1 C31 175.1(3) . . ? N2 Ir1 C30 93.3(3) . . ? C15 Ir1 C30 88.9(3) . . ? C31 Ir1 C30 89.8(3) . . ? N2 Ir1 C32 92.2(3) . . ? C15 Ir1 C32 92.2(3) . . ? C31 Ir1 C32 89.5(3) . . ? C30 Ir1 C32 174.5(3) . . ? N2 Ir1 N3 168.8(2) . . ? C15 Ir1 N3 91.1(3) . . ? C31 Ir1 N3 93.4(2) . . ? C30 Ir1 N3 80.3(3) . . ? C32 Ir1 N3 94.3(3) . . ? C2 C1 N2 123.1(7) . . ? C2 C1 H1 118.5 . . ? N2 C1 H1 118.5 . . ? C1 C2 C3 118.5(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.7(7) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N2 C5 C4 119.6(7) . . ? N2 C5 C6 114.7(6) . . ? C4 C5 C6 125.7(7) . . ? C7 C6 C15 120.4(7) . . ? C7 C6 C5 124.7(7) . . ? C15 C6 C5 114.9(6) . . ? C8 C7 C6 120.3(7) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 121.7(7) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C14 117.5(7) . . ? C8 C9 C10 120.2(6) . . ? C14 C9 C10 122.3(7) . . ? C13 C10 C9 113.3(6) . . ? C13 C10 C11 108.7(7) . . ? C9 C10 C11 108.9(6) . . ? C13 C10 C12 108.5(7) . . ? C9 C10 C12 109.0(7) . . ? C11 C10 C12 108.4(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C9 123.1(7) . . ? C15 C14 H14 118.5 . . ? C9 C14 H14 118.5 . . ? C14 C15 C6 116.9(6) . . ? C14 C15 Ir1 129.0(5) . . ? C6 C15 Ir1 114.1(5) . . ? N3 C16 C17 122.8(7) . . ? N3 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C18 C17 C16 118.2(8) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C19 C18 C17 119.4(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? N3 C20 C19 118.5(7) . . ? N3 C20 C21 115.3(6) . . ? C19 C20 C21 126.1(7) . . ? C22 C21 C30 120.3(7) . . ? C22 C21 C20 123.7(6) . . ? C30 C21 C20 116.1(6) . . ? C23 C22 C21 121.0(7) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C29 C24 C23 117.5(7) . . ? C29 C24 C25 122.0(7) . . ? C23 C24 C25 120.5(6) . . ? C28 C25 C24 111.4(7) . . ? C28 C25 C27 109.4(7) . . ? C24 C25 C27 109.4(6) . . ? C28 C25 C26 107.6(7) . . ? C24 C25 C26 110.5(6) . . ? C27 C25 C26 108.4(7) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C24 123.2(7) . . ? C30 C29 H29 118.4 . . ? C24 C29 H29 118.4 . . ? C29 C30 C21 117.5(6) . . ? C29 C30 Ir1 129.1(5) . . ? C21 C30 Ir1 113.4(5) . . ? N5 C31 Ir1 177.5(6) . . ? N4 C32 Ir1 177.0(7) . . ? C34 C33 C38 120.2(8) . . ? C34 C33 P1 119.6(6) . . ? C38 C33 P1 120.1(6) . . ? C35 C34 C33 119.5(8) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.8(8) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C37 119.6(8) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.6(8) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C33 119.2(7) . . ? C37 C38 H38 120.4 . . ? C33 C38 H38 120.4 . . ? C40 C39 C44 119.7(8) . . ? C40 C39 P1 123.6(7) . . ? C44 C39 P1 116.7(6) . . ? C39 C40 C41 119.9(9) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.2(9) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.1(9) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.9(9) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C39 120.1(8) . . ? C43 C44 H44 119.9 . . ? C39 C44 H44 119.9 . . ? C50 C45 C46 120.2(7) . . ? C50 C45 P1 120.6(6) . . ? C46 C45 P1 119.2(7) . . ? C47 C46 C45 119.6(8) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 119.8(8) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C49 121.2(8) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 119.0(9) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C45 C50 C49 120.1(7) . . ? C45 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C56 C51 C52 119.5(7) . . ? C56 C51 P2 120.4(6) . . ? C52 C51 P2 120.1(6) . . ? C53 C52 C51 120.0(7) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 120.1(8) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 119.8(8) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 120.2(8) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C51 120.3(7) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C58 C57 C62 119.6(7) . . ? C58 C57 H57 120.2 . . ? C62 C57 H57 120.2 . . ? C57 C58 C59 120.6(7) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C60 C59 C58 120.6(7) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C59 C60 C61 119.2(7) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 C60 120.0(7) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C57 120.1(7) . . ? C61 C62 P2 120.4(6) . . ? C57 C62 P2 119.1(5) . . ? C68 C63 C64 119.7(7) . . ? C68 C63 P2 122.4(6) . . ? C64 C63 P2 117.6(6) . . ? C65 C64 C63 120.1(8) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 120.6(9) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C67 119.5(8) . . ? C65 C66 H66 120.2 . . ? C67 C66 H66 120.2 . . ? C68 C67 C66 119.8(9) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C63 C68 C67 120.2(8) . . ? C63 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? P2 N1 P1 134.6(4) . . ? C5 N2 C1 118.4(6) . . ? C5 N2 Ir1 116.6(5) . . ? C1 N2 Ir1 124.8(5) . . ? C16 N3 C20 120.3(6) . . ? C16 N3 Ir1 124.7(5) . . ? C20 N3 Ir1 114.7(5) . . ? N1 P1 C45 109.0(4) . . ? N1 P1 C33 110.4(4) . . ? C45 P1 C33 106.9(3) . . ? N1 P1 C39 114.4(3) . . ? C45 P1 C39 105.9(4) . . ? C33 P1 C39 109.8(4) . . ? N1 P2 C51 110.5(3) . . ? N1 P2 C62 108.2(3) . . ? C51 P2 C62 107.0(3) . . ? N1 P2 C63 114.5(3) . . ? C51 P2 C63 108.1(4) . . ? C62 P2 C63 108.2(3) . . ? Cl1S C1S Cl2S 111.1(5) . . ? Cl1S C1S H1S1 109.4 . . ? Cl2S C1S H1S1 109.4 . . ? Cl1S C1S H1S2 109.4 . . ? Cl2S C1S H1S2 109.4 . . ? H1S1 C1S H1S2 108.0 . . ? Cl4S C2S Cl3S 113.7(9) . . ? Cl4S C2S H2S1 108.8 . . ? Cl3S C2S H2S1 108.8 . . ? Cl4S C2S H2S2 108.8 . . ? Cl3S C2S H2S2 108.8 . . ? H2S1 C2S H2S2 107.7 . . ? Cl5S C3S Cl6S 112.1(5) . . ? Cl5S C3S H3S1 109.2 . . ? Cl6S C3S H3S1 109.2 . . ? Cl5S C3S H3S2 109.2 . . ? Cl6S C3S H3S2 109.2 . . ? H3S1 C3S H3S2 107.9 . . ? 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 N2 C1 C2 C3 1.5(12) . . . . ? C1 C2 C3 C4 -0.9(12) . . . . ? C2 C3 C4 C5 -0.7(12) . . . . ? C3 C4 C5 N2 1.6(11) . . . . ? C3 C4 C5 C6 -178.8(7) . . . . ? N2 C5 C6 C7 -174.3(7) . . . . ? C4 C5 C6 C7 6.1(12) . . . . ? N2 C5 C6 C15 3.6(9) . . . . ? C4 C5 C6 C15 -176.0(7) . . . . ? C15 C6 C7 C8 2.9(11) . . . . ? C5 C6 C7 C8 -179.3(7) . . . . ? C6 C7 C8 C9 -0.8(12) . . . . ? C7 C8 C9 C14 -1.2(12) . . . . ? C7 C8 C9 C10 178.0(7) . . . . ? C8 C9 C10 C13 -175.5(7) . . . . ? C14 C9 C10 C13 3.6(11) . . . . ? C8 C9 C10 C11 63.4(9) . . . . ? C14 C9 C10 C11 -117.5(8) . . . . ? C8 C9 C10 C12 -54.6(10) . . . . ? C14 C9 C10 C12 124.5(8) . . . . ? C8 C9 C14 C15 1.1(11) . . . . ? C10 C9 C14 C15 -178.0(7) . . . . ? C9 C14 C15 C6 0.9(11) . . . . ? C9 C14 C15 Ir1 -179.8(6) . . . . ? C7 C6 C15 C14 -2.9(11) . . . . ? C5 C6 C15 C14 179.1(6) . . . . ? C7 C6 C15 Ir1 177.7(6) . . . . ? C5 C6 C15 Ir1 -0.3(8) . . . . ? N2 Ir1 C15 C14 178.8(7) . . . . ? C31 Ir1 C15 C14 -163(3) . . . . ? C30 Ir1 C15 C14 -87.6(7) . . . . ? C32 Ir1 C15 C14 87.0(7) . . . . ? N3 Ir1 C15 C14 -7.3(7) . . . . ? N2 Ir1 C15 C6 -1.9(5) . . . . ? C31 Ir1 C15 C6 17(4) . . . . ? C30 Ir1 C15 C6 91.7(6) . . . . ? C32 Ir1 C15 C6 -93.7(6) . . . . ? N3 Ir1 C15 C6 172.0(5) . . . . ? N3 C16 C17 C18 -0.9(12) . . . . ? C16 C17 C18 C19 0.1(12) . . . . ? C17 C18 C19 C20 -0.1(11) . . . . ? C18 C19 C20 N3 0.8(11) . . . . ? C18 C19 C20 C21 177.3(7) . . . . ? N3 C20 C21 C22 -175.5(6) . . . . ? C19 C20 C21 C22 8.0(11) . . . . ? N3 C20 C21 C30 4.8(9) . . . . ? C19 C20 C21 C30 -171.8(7) . . . . ? C30 C21 C22 C23 4.0(10) . . . . ? C20 C21 C22 C23 -175.7(6) . . . . ? C21 C22 C23 C24 -1.0(10) . . . . ? C22 C23 C24 C29 -2.4(10) . . . . ? C22 C23 C24 C25 177.8(6) . . . . ? C29 C24 C25 C28 27.9(9) . . . . ? C23 C24 C25 C28 -152.3(7) . . . . ? C29 C24 C25 C27 -93.2(8) . . . . ? C23 C24 C25 C27 86.6(8) . . . . ? C29 C24 C25 C26 147.4(7) . . . . ? C23 C24 C25 C26 -32.7(9) . . . . ? C23 C24 C29 C30 2.9(10) . . . . ? C25 C24 C29 C30 -177.2(6) . . . . ? C24 C29 C30 C21 0.0(10) . . . . ? C24 C29 C30 Ir1 177.8(5) . . . . ? C22 C21 C30 C29 -3.5(9) . . . . ? C20 C21 C30 C29 176.3(6) . . . . ? C22 C21 C30 Ir1 178.3(5) . . . . ? C20 C21 C30 Ir1 -1.9(7) . . . . ? N2 Ir1 C30 C29 -7.9(6) . . . . ? C15 Ir1 C30 C29 -87.3(6) . . . . ? C31 Ir1 C30 C29 87.9(6) . . . . ? C32 Ir1 C30 C29 171(3) . . . . ? N3 Ir1 C30 C29 -178.6(6) . . . . ? N2 Ir1 C30 C21 170.0(5) . . . . ? C15 Ir1 C30 C21 90.6(5) . . . . ? C31 Ir1 C30 C21 -94.2(5) . . . . ? C32 Ir1 C30 C21 -11(3) . . . . ? N3 Ir1 C30 C21 -0.7(5) . . . . ? N2 Ir1 C31 N5 56(14) . . . . ? C15 Ir1 C31 N5 38(15) . . . . ? C30 Ir1 C31 N5 -37(14) . . . . ? C32 Ir1 C31 N5 148(14) . . . . ? N3 Ir1 C31 N5 -117(13) . . . . ? N2 Ir1 C32 N4 -169(14) . . . . ? C15 Ir1 C32 N4 -90(14) . . . . ? C31 Ir1 C32 N4 95(14) . . . . ? C30 Ir1 C32 N4 12(15) . . . . ? N3 Ir1 C32 N4 2(14) . . . . ? C38 C33 C34 C35 -0.8(12) . . . . ? P1 C33 C34 C35 175.9(7) . . . . ? C33 C34 C35 C36 0.8(13) . . . . ? C34 C35 C36 C37 -1.1(15) . . . . ? C35 C36 C37 C38 1.6(15) . . . . ? C36 C37 C38 C33 -1.6(14) . . . . ? C34 C33 C38 C37 1.2(13) . . . . ? P1 C33 C38 C37 -175.5(7) . . . . ? C44 C39 C40 C41 0.7(12) . . . . ? P1 C39 C40 C41 -176.2(7) . . . . ? C39 C40 C41 C42 -0.3(14) . . . . ? C40 C41 C42 C43 0.0(14) . . . . ? C41 C42 C43 C44 -0.2(13) . . . . ? C42 C43 C44 C39 0.7(12) . . . . ? C40 C39 C44 C43 -0.9(11) . . . . ? P1 C39 C44 C43 176.2(6) . . . . ? C50 C45 C46 C47 -0.6(12) . . . . ? P1 C45 C46 C47 176.5(7) . . . . ? C45 C46 C47 C48 1.3(13) . . . . ? C46 C47 C48 C49 -0.3(14) . . . . ? C47 C48 C49 C50 -1.3(14) . . . . ? C46 C45 C50 C49 -1.0(12) . . . . ? P1 C45 C50 C49 -178.1(6) . . . . ? C48 C49 C50 C45 2.0(13) . . . . ? C56 C51 C52 C53 -3.3(11) . . . . ? P2 C51 C52 C53 178.7(6) . . . . ? C51 C52 C53 C54 0.5(12) . . . . ? C52 C53 C54 C55 2.1(13) . . . . ? C53 C54 C55 C56 -2.0(13) . . . . ? C54 C55 C56 C51 -0.8(13) . . . . ? C52 C51 C56 C55 3.4(12) . . . . ? P2 C51 C56 C55 -178.6(6) . . . . ? C62 C57 C58 C59 -0.8(13) . . . . ? C57 C58 C59 C60 0.4(13) . . . . ? C58 C59 C60 C61 1.2(12) . . . . ? C59 C60 C61 C62 -2.3(12) . . . . ? C60 C61 C62 C57 1.8(12) . . . . ? C60 C61 C62 P2 173.8(6) . . . . ? C58 C57 C62 C61 -0.3(12) . . . . ? C58 C57 C62 P2 -172.4(7) . . . . ? C68 C63 C64 C65 1.1(11) . . . . ? P2 C63 C64 C65 175.8(6) . . . . ? C63 C64 C65 C66 -0.5(12) . . . . ? C64 C65 C66 C67 -0.1(12) . . . . ? C65 C66 C67 C68 0.2(12) . . . . ? C64 C63 C68 C67 -1.1(11) . . . . ? P2 C63 C68 C67 -175.5(6) . . . . ? C66 C67 C68 C63 0.4(12) . . . . ? C4 C5 N2 C1 -0.9(10) . . . . ? C6 C5 N2 C1 179.4(6) . . . . ? C4 C5 N2 Ir1 174.3(5) . . . . ? C6 C5 N2 Ir1 -5.4(8) . . . . ? C2 C1 N2 C5 -0.6(11) . . . . ? C2 C1 N2 Ir1 -175.4(6) . . . . ? C15 Ir1 N2 C5 4.1(5) . . . . ? C31 Ir1 N2 C5 -174.4(5) . . . . ? C30 Ir1 N2 C5 -84.2(5) . . . . ? C32 Ir1 N2 C5 95.9(5) . . . . ? N3 Ir1 N2 C5 -29.4(15) . . . . ? C15 Ir1 N2 C1 178.9(6) . . . . ? C31 Ir1 N2 C1 0.5(6) . . . . ? C30 Ir1 N2 C1 90.6(6) . . . . ? C32 Ir1 N2 C1 -89.3(6) . . . . ? N3 Ir1 N2 C1 145.5(12) . . . . ? C17 C16 N3 C20 1.6(11) . . . . ? C17 C16 N3 Ir1 -170.7(6) . . . . ? C19 C20 N3 C16 -1.6(10) . . . . ? C21 C20 N3 C16 -178.4(6) . . . . ? C19 C20 N3 Ir1 171.5(5) . . . . ? C21 C20 N3 Ir1 -5.3(7) . . . . ? N2 Ir1 N3 C16 120.1(12) . . . . ? C15 Ir1 N3 C16 87.3(6) . . . . ? C31 Ir1 N3 C16 -94.7(6) . . . . ? C30 Ir1 N3 C16 176.1(6) . . . . ? C32 Ir1 N3 C16 -5.0(6) . . . . ? N2 Ir1 N3 C20 -52.6(15) . . . . ? C15 Ir1 N3 C20 -85.4(5) . . . . ? C31 Ir1 N3 C20 92.5(5) . . . . ? C30 Ir1 N3 C20 3.3(5) . . . . ? C32 Ir1 N3 C20 -177.7(5) . . . . ? P2 N1 P1 C45 -139.0(6) . . . . ? P2 N1 P1 C33 103.8(6) . . . . ? P2 N1 P1 C39 -20.7(8) . . . . ? C50 C45 P1 N1 -20.4(7) . . . . ? C46 C45 P1 N1 162.5(6) . . . . ? C50 C45 P1 C33 99.0(7) . . . . ? C46 C45 P1 C33 -78.1(7) . . . . ? C50 C45 P1 C39 -143.9(6) . . . . ? C46 C45 P1 C39 39.0(7) . . . . ? C34 C33 P1 N1 -2.0(8) . . . . ? C38 C33 P1 N1 174.7(6) . . . . ? C34 C33 P1 C45 -120.4(7) . . . . ? C38 C33 P1 C45 56.3(8) . . . . ? C34 C33 P1 C39 125.1(7) . . . . ? C38 C33 P1 C39 -58.2(7) . . . . ? C40 C39 P1 N1 116.0(7) . . . . ? C44 C39 P1 N1 -60.9(7) . . . . ? C40 C39 P1 C45 -123.9(7) . . . . ? C44 C39 P1 C45 59.1(6) . . . . ? C40 C39 P1 C33 -8.8(8) . . . . ? C44 C39 P1 C33 174.3(5) . . . . ? P1 N1 P2 C51 98.5(6) . . . . ? P1 N1 P2 C62 -144.6(6) . . . . ? P1 N1 P2 C63 -23.9(7) . . . . ? C56 C51 P2 N1 4.1(7) . . . . ? C52 C51 P2 N1 -177.9(6) . . . . ? C56 C51 P2 C62 -113.5(6) . . . . ? C52 C51 P2 C62 64.5(7) . . . . ? C56 C51 P2 C63 130.2(6) . . . . ? C52 C51 P2 C63 -51.8(7) . . . . ? C61 C62 P2 N1 158.5(6) . . . . ? C57 C62 P2 N1 -29.5(7) . . . . ? C61 C62 P2 C51 -82.4(7) . . . . ? C57 C62 P2 C51 89.7(7) . . . . ? C61 C62 P2 C63 33.9(7) . . . . ? C57 C62 P2 C63 -154.0(6) . . . . ? C68 C63 P2 N1 104.5(7) . . . . ? C64 C63 P2 N1 -70.0(7) . . . . ? C68 C63 P2 C51 -19.2(7) . . . . ? C64 C63 P2 C51 166.2(6) . . . . ? C68 C63 P2 C62 -134.8(6) . . . . ? C64 C63 P2 C62 50.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 3.414 _refine_diff_density_min -2.369 _refine_diff_density_rms 0.208 #===END data_imw1500p21c _database_code_depnum_ccdc_archive 'CCDC 834575' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H48 Ir2 K2 N8 O4' _chemical_formula_weight 1311.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' O O 0.0106 0.0060 '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 ' 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 15.3695(5) _cell_length_b 9.1499(3) _cell_length_c 18.3135(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.9190(10) _cell_angle_gamma 90.00 _cell_volume 2421.34(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9863 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.54 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.717 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4097 _exptl_absorpt_correction_T_max 0.7254 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43123 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5572 _reflns_number_gt 5000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by Patterson methods. Two coordinated methanol molecules exist in the system (O511 C512 and O611 C612). Both the alcohol and methyl protons of both of these residues were found from the data, improved in the case of the methyl protons and then fixed. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+1.9696P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5572 _refine_ls_number_parameters 307 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0430 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.050 _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 0.520535(6) 0.049513(10) 0.765617(5) 0.01556(4) Uani 1 1 d . . . K1 K 0.37279(4) 0.08747(7) 0.50883(3) 0.02673(12) Uani 1 1 d . . . N111 N 0.59494(13) 0.2402(2) 0.79148(11) 0.0183(4) Uani 1 1 d . . . C112 C 0.58570(16) 0.3199(3) 0.85144(14) 0.0195(5) Uani 1 1 d . . . C113 C 0.63703(19) 0.4486(3) 0.87440(16) 0.0269(6) Uani 1 1 d . . . H113 H 0.6301 0.5054 0.9155 0.032 Uiso 1 1 calc R . . C114 C 0.6973(2) 0.4939(3) 0.83828(17) 0.0312(6) Uani 1 1 d . . . H114 H 0.7317 0.5816 0.8540 0.037 Uiso 1 1 calc R . . C115 C 0.70726(19) 0.4097(3) 0.77849(17) 0.0307(6) Uani 1 1 d . . . H115 H 0.7496 0.4375 0.7534 0.037 Uiso 1 1 calc R . . C116 C 0.65461(17) 0.2855(3) 0.75650(15) 0.0253(6) Uani 1 1 d . . . H116 H 0.6604 0.2291 0.7149 0.030 Uiso 1 1 calc R . . C121 C 0.48491(16) 0.1201(3) 0.85784(13) 0.0185(5) Uani 1 1 d . . . C122 C 0.52298(16) 0.2569(3) 0.88728(13) 0.0189(5) Uani 1 1 d . . . C123 C 0.50299(18) 0.3232(3) 0.94894(15) 0.0251(6) Uani 1 1 d . . . H123 H 0.5283 0.4163 0.9675 0.030 Uiso 1 1 calc R . . C124 C 0.44647(18) 0.2531(3) 0.98262(15) 0.0271(6) Uani 1 1 d . . . H124 H 0.4332 0.2976 1.0245 0.033 Uiso 1 1 calc R . . C125 C 0.40929(17) 0.1180(3) 0.95507(14) 0.0247(6) Uani 1 1 d . . . H125 H 0.3709 0.0694 0.9785 0.030 Uiso 1 1 calc R . . C126 C 0.42752(17) 0.0530(3) 0.89363(15) 0.0217(5) Uani 1 1 d . . . H126 H 0.4006 -0.0392 0.8751 0.026 Uiso 1 1 calc R . . N211 N 0.43348(13) -0.1271(2) 0.74530(11) 0.0182(4) Uani 1 1 d . . . C212 C 0.34345(16) -0.1025(3) 0.70002(14) 0.0192(5) Uani 1 1 d . . . C213 C 0.27841(18) -0.2139(3) 0.68824(15) 0.0260(6) Uani 1 1 d . . . H213 H 0.2156 -0.1961 0.6577 0.031 Uiso 1 1 calc R . . C214 C 0.30455(19) -0.3494(3) 0.72056(15) 0.0278(6) Uani 1 1 d . . . H214 H 0.2602 -0.4255 0.7124 0.033 Uiso 1 1 calc R . . C215 C 0.39626(19) -0.3739(3) 0.76518(16) 0.0284(6) Uani 1 1 d . . . H215 H 0.4159 -0.4670 0.7877 0.034 Uiso 1 1 calc R . . C216 C 0.45817(18) -0.2609(3) 0.77614(14) 0.0240(5) Uani 1 1 d . . . H216 H 0.5210 -0.2778 0.8067 0.029 Uiso 1 1 calc R . . C221 C 0.40092(16) 0.1427(3) 0.69282(13) 0.0191(5) Uani 1 1 d . . . C222 C 0.32510(17) 0.0462(3) 0.66826(14) 0.0192(5) Uani 1 1 d . . . C223 C 0.23941(18) 0.0897(3) 0.61550(15) 0.0241(5) Uani 1 1 d . . . H223 H 0.1896 0.0220 0.5989 0.029 Uiso 1 1 calc R . . C224 C 0.22753(18) 0.2313(3) 0.58768(15) 0.0284(6) Uani 1 1 d . . . H224 H 0.1695 0.2617 0.5521 0.034 Uiso 1 1 calc R . . C225 C 0.30061(19) 0.3288(3) 0.61195(15) 0.0268(6) Uani 1 1 d . . . H225 H 0.2921 0.4263 0.5931 0.032 Uiso 1 1 calc R . . C226 C 0.38674(18) 0.2859(3) 0.66380(14) 0.0227(5) Uani 1 1 d . . . H226 H 0.4361 0.3544 0.6795 0.027 Uiso 1 1 calc R . . N312 N 0.43832(16) 0.0056(3) 0.39224(13) 0.0296(5) Uani 1 1 d . . . C311 C 0.55195(17) 0.0071(3) 0.66704(15) 0.0207(5) Uani 1 1 d . . . C411 C 0.63314(18) -0.0574(3) 0.84089(15) 0.0212(5) Uani 1 1 d . . . N412 N 0.69531(16) -0.1143(3) 0.88528(14) 0.0321(5) Uani 1 1 d . . . O511 O 0.29979(15) -0.1898(2) 0.50136(12) 0.0435(5) Uani 1 1 d . . . H511 H 0.2593 -0.2395 0.4591 0.052 Uiso 1 1 d R . . C512 C 0.3785(2) -0.2748(4) 0.5360(2) 0.0484(8) Uani 1 1 d U . . H51A H 0.4033 -0.2936 0.4954 0.073 Uiso 1 1 d R . . H51B H 0.3603 -0.3752 0.5354 0.073 Uiso 1 1 d R . . H51C H 0.4209 -0.2223 0.5788 0.073 Uiso 1 1 d R . . O611 O 0.32722(19) 0.3503(3) 0.43686(15) 0.0575(7) Uani 1 1 d . . . H611 H 0.2820 0.4246 0.4286 0.069 Uiso 1 1 d R . . C612 C 0.3817(3) 0.3899(5) 0.3929(3) 0.0737(12) Uani 1 1 d U . . H61A H 0.4037 0.4889 0.3970 0.110 Uiso 1 1 d R . . H61B H 0.4169 0.3068 0.3871 0.110 Uiso 1 1 d R . . H61C H 0.3454 0.3872 0.3386 0.110 Uiso 1 1 d 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 0.01418(5) 0.01783(6) 0.01363(5) -0.00253(3) 0.00340(4) 0.00025(3) K1 0.0298(3) 0.0294(3) 0.0220(3) -0.0020(2) 0.0102(2) 0.0025(2) N111 0.0157(10) 0.0200(11) 0.0172(10) -0.0018(8) 0.0032(8) -0.0008(8) C112 0.0156(11) 0.0219(13) 0.0174(11) -0.0006(10) 0.0010(9) 0.0012(9) C113 0.0282(14) 0.0253(14) 0.0257(14) -0.0067(11) 0.0074(11) -0.0029(11) C114 0.0292(15) 0.0278(14) 0.0342(16) -0.0046(13) 0.0076(12) -0.0102(12) C115 0.0262(14) 0.0363(16) 0.0309(15) -0.0015(13) 0.0112(12) -0.0103(12) C116 0.0222(13) 0.0314(15) 0.0225(13) -0.0021(11) 0.0080(10) -0.0028(11) C121 0.0161(11) 0.0217(13) 0.0148(11) -0.0009(10) 0.0016(9) 0.0040(10) C122 0.0159(11) 0.0232(13) 0.0155(11) -0.0019(10) 0.0024(9) 0.0029(10) C123 0.0243(13) 0.0249(14) 0.0244(13) -0.0075(11) 0.0062(10) 0.0039(11) C124 0.0260(13) 0.0379(16) 0.0184(12) -0.0060(11) 0.0088(10) 0.0070(12) C125 0.0218(13) 0.0327(15) 0.0212(13) 0.0039(11) 0.0093(10) 0.0042(11) C126 0.0182(12) 0.0246(14) 0.0204(13) 0.0003(10) 0.0042(10) 0.0013(10) N211 0.0190(10) 0.0203(11) 0.0155(10) -0.0032(8) 0.0061(8) 0.0002(8) C212 0.0186(12) 0.0250(13) 0.0151(11) -0.0046(10) 0.0071(9) -0.0009(10) C213 0.0218(13) 0.0306(15) 0.0234(13) -0.0049(11) 0.0049(10) -0.0071(11) C214 0.0323(15) 0.0270(14) 0.0255(13) -0.0056(11) 0.0114(11) -0.0106(12) C215 0.0361(15) 0.0222(14) 0.0274(14) -0.0008(11) 0.0113(12) -0.0019(11) C216 0.0248(13) 0.0238(13) 0.0215(12) -0.0011(11) 0.0057(10) 0.0022(11) C221 0.0194(11) 0.0222(12) 0.0147(11) -0.0042(10) 0.0048(9) 0.0023(10) C222 0.0170(12) 0.0245(13) 0.0157(11) -0.0045(10) 0.0052(9) 0.0026(10) C223 0.0186(12) 0.0312(14) 0.0200(12) -0.0047(11) 0.0034(10) 0.0004(11) C224 0.0226(13) 0.0359(16) 0.0225(13) -0.0020(12) 0.0020(10) 0.0087(12) C225 0.0315(14) 0.0206(14) 0.0256(13) 0.0004(11) 0.0061(11) 0.0078(11) C226 0.0235(13) 0.0220(13) 0.0194(12) -0.0046(10) 0.0035(10) 0.0002(10) N312 0.0260(12) 0.0413(14) 0.0221(12) -0.0075(11) 0.0088(10) 0.0002(11) C311 0.0165(12) 0.0215(12) 0.0215(13) -0.0053(10) 0.0030(10) -0.0003(10) C411 0.0205(13) 0.0235(13) 0.0190(12) -0.0029(10) 0.0060(10) -0.0030(10) N412 0.0267(12) 0.0337(14) 0.0310(13) 0.0061(11) 0.0034(10) 0.0031(11) O511 0.0462(13) 0.0355(12) 0.0379(12) -0.0049(10) 0.0002(10) -0.0070(10) C512 0.0476(11) 0.0458(12) 0.0484(11) -0.0033(9) 0.0120(8) -0.0013(9) O611 0.0757(18) 0.0468(15) 0.0541(15) 0.0172(12) 0.0276(14) 0.0219(13) C612 0.0738(15) 0.0729(15) 0.0755(15) 0.0041(9) 0.0270(10) 0.0021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C121 2.049(2) . ? Ir1 N211 2.049(2) . ? Ir1 N111 2.052(2) . ? Ir1 C221 2.053(2) . ? Ir1 C411 2.056(3) . ? Ir1 C311 2.058(3) . ? K1 O611 2.717(2) . ? K1 N312 2.757(2) . ? K1 O511 2.759(2) . ? K1 N312 2.975(2) 3_656 ? K1 C222 3.266(3) . ? K1 C223 3.278(3) . ? K1 C221 3.287(2) . ? K1 C226 3.314(3) . ? K1 C224 3.317(3) . ? K1 C311 3.329(3) . ? K1 C225 3.332(3) . ? K1 C114 3.441(3) 4_565 ? N111 C116 1.350(3) . ? N111 C112 1.365(3) . ? C112 C113 1.400(4) . ? C112 C122 1.457(3) . ? C113 C114 1.373(4) . ? C113 H113 0.9500 . ? C114 C115 1.389(4) . ? C114 K1 3.441(3) 4_666 ? C114 H114 0.9500 . ? C115 C116 1.373(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.407(4) . ? C121 C122 1.408(3) . ? C122 C123 1.405(3) . ? C123 C124 1.383(4) . ? C123 H123 0.9500 . ? C124 C125 1.383(4) . ? C124 H124 0.9500 . ? C125 C126 1.383(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? N211 C216 1.348(3) . ? N211 C212 1.368(3) . ? C212 C213 1.392(4) . ? C212 C222 1.468(4) . ? C213 C214 1.373(4) . ? C213 H213 0.9500 . ? C214 C215 1.386(4) . ? C214 H214 0.9500 . ? C215 C216 1.372(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.403(4) . ? C221 C222 1.409(3) . ? C222 C223 1.400(3) . ? C223 C224 1.382(4) . ? C223 H223 0.9500 . ? C224 C225 1.383(4) . ? C224 H224 0.9500 . ? C225 C226 1.397(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? N312 C311 1.151(3) 3_656 ? N312 K1 2.975(2) 3_656 ? C311 N312 1.151(3) 3_656 ? C411 N412 1.147(3) . ? O511 C512 1.396(4) . ? O511 H511 0.9297 . ? C512 H51A 0.9600 . ? C512 H51B 0.9601 . ? C512 H51C 0.9600 . ? O611 C612 1.394(5) . ? O611 H611 0.9463 . ? C612 H61A 0.9601 . ? C612 H61B 0.9601 . ? C612 H61C 0.9600 . ? 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 C121 Ir1 N211 93.27(9) . . ? C121 Ir1 N111 79.98(9) . . ? N211 Ir1 N111 172.17(8) . . ? C121 Ir1 C221 88.43(9) . . ? N211 Ir1 C221 79.91(9) . . ? N111 Ir1 C221 95.85(9) . . ? C121 Ir1 C411 89.87(10) . . ? N211 Ir1 C411 95.44(9) . . ? N111 Ir1 C411 88.53(9) . . ? C221 Ir1 C411 174.95(10) . . ? C121 Ir1 C311 172.15(10) . . ? N211 Ir1 C311 91.48(9) . . ? N111 Ir1 C311 94.82(9) . . ? C221 Ir1 C311 86.24(9) . . ? C411 Ir1 C311 95.91(10) . . ? O611 K1 N312 88.09(8) . . ? O611 K1 O511 139.18(8) . . ? N312 K1 O511 87.78(8) . . ? O611 K1 N312 125.84(8) . 3_656 ? N312 K1 N312 81.70(7) . 3_656 ? O511 K1 N312 93.61(7) . 3_656 ? O611 K1 C222 115.91(7) . . ? N312 K1 C222 156.00(7) . . ? O511 K1 C222 74.13(7) . . ? N312 K1 C222 83.81(6) 3_656 . ? O611 K1 C223 99.99(8) . . ? N312 K1 C223 158.56(7) . . ? O511 K1 C223 73.07(7) . . ? N312 K1 C223 108.50(7) 3_656 . ? C222 K1 C223 24.70(6) . . ? O611 K1 C221 106.46(7) . . ? N312 K1 C221 151.71(7) . . ? O511 K1 C221 95.83(7) . . ? N312 K1 C221 70.09(6) 3_656 . ? C222 K1 C221 24.82(6) . . ? C223 K1 C221 43.84(6) . . ? O611 K1 C226 82.02(7) . . ? N312 K1 C226 151.41(7) . . ? O511 K1 C226 116.94(7) . . ? N312 K1 C226 82.55(6) 3_656 . ? C222 K1 C226 42.82(6) . . ? C223 K1 C226 50.02(7) . . ? C221 K1 C226 24.54(6) . . ? O611 K1 C224 76.08(7) . . ? N312 K1 C224 157.35(7) . . ? O511 K1 C224 93.67(7) . . ? N312 K1 C224 120.69(6) 3_656 . ? C222 K1 C224 42.88(6) . . ? C223 K1 C224 24.19(7) . . ? C221 K1 C224 50.62(6) . . ? C226 K1 C224 42.81(6) . . ? O611 K1 C311 128.16(8) . . ? N312 K1 C311 101.65(7) . . ? O511 K1 C311 92.40(7) . . ? N312 K1 C311 20.04(6) 3_656 . ? C222 K1 C311 64.36(6) . . ? C223 K1 C311 88.99(6) . . ? C221 K1 C311 50.27(6) . . ? C226 K1 C311 65.34(6) . . ? C224 K1 C311 100.87(6) . . ? O611 K1 C225 66.91(7) . . ? N312 K1 C225 154.06(8) . . ? O511 K1 C225 115.42(7) . . ? N312 K1 C225 106.78(7) 3_656 . ? C222 K1 C225 49.48(6) . . ? C223 K1 C225 42.41(7) . . ? C221 K1 C225 43.10(6) . . ? C226 K1 C225 24.27(6) . . ? C224 K1 C225 24.02(7) . . ? C311 K1 C225 89.40(6) . . ? O611 K1 C114 76.02(8) . 4_565 ? N312 K1 C114 67.57(7) . 4_565 ? O511 K1 C114 64.93(7) . 4_565 ? N312 K1 C114 142.29(7) 3_656 4_565 ? C222 K1 C114 116.18(7) . 4_565 ? C223 K1 C114 94.95(7) . 4_565 ? C221 K1 C114 138.80(7) . 4_565 ? C226 K1 C114 134.25(7) . 4_565 ? C224 K1 C114 92.60(7) . 4_565 ? C311 K1 C114 154.45(7) . 4_565 ? C225 K1 C114 110.39(7) . 4_565 ? C116 N111 C112 119.4(2) . . ? C116 N111 Ir1 124.53(17) . . ? C112 N111 Ir1 115.93(16) . . ? N111 C112 C113 119.2(2) . . ? N111 C112 C122 114.7(2) . . ? C113 C112 C122 126.1(2) . . ? C114 C113 C112 120.9(3) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C113 C114 C115 119.1(3) . . ? C113 C114 K1 86.92(18) . 4_666 ? C115 C114 K1 109.44(19) . 4_666 ? C113 C114 H114 120.5 . . ? C115 C114 H114 120.5 . . ? K1 C114 H114 74.0 4_666 . ? C116 C115 C114 118.5(3) . . ? C116 C115 H115 120.7 . . ? C114 C115 H115 120.7 . . ? N111 C116 C115 122.8(3) . . ? N111 C116 H116 118.6 . . ? C115 C116 H116 118.6 . . ? C126 C121 C122 117.0(2) . . ? C126 C121 Ir1 129.23(18) . . ? C122 C121 Ir1 113.75(18) . . ? C123 C122 C121 121.0(2) . . ? C123 C122 C112 123.4(2) . . ? C121 C122 C112 115.6(2) . . ? C124 C123 C122 120.0(2) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 119.7(2) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C126 C125 C124 120.5(2) . . ? C126 C125 H125 119.7 . . ? C124 C125 H125 119.7 . . ? C125 C126 C121 121.6(2) . . ? C125 C126 H126 119.2 . . ? C121 C126 H126 119.2 . . ? C216 N211 C212 119.1(2) . . ? C216 N211 Ir1 124.55(17) . . ? C212 N211 Ir1 116.32(17) . . ? N211 C212 C213 119.9(2) . . ? N211 C212 C222 114.2(2) . . ? C213 C212 C222 125.9(2) . . ? C214 C213 C212 120.3(2) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C213 C214 C215 119.3(2) . . ? C213 C214 H214 120.3 . . ? C215 C214 H214 120.3 . . ? C216 C215 C214 118.7(3) . . ? C216 C215 H215 120.7 . . ? C214 C215 H215 120.7 . . ? N211 C216 C215 122.7(2) . . ? N211 C216 H216 118.6 . . ? C215 C216 H216 118.6 . . ? C226 C221 C222 117.4(2) . . ? C226 C221 Ir1 128.55(19) . . ? C222 C221 Ir1 114.03(18) . . ? C226 C221 K1 78.82(14) . . ? C222 C221 K1 76.74(14) . . ? Ir1 C221 K1 112.20(9) . . ? C223 C222 C221 121.6(2) . . ? C223 C222 C212 123.1(2) . . ? C221 C222 C212 115.4(2) . . ? C223 C222 K1 78.16(15) . . ? C221 C222 K1 78.43(14) . . ? C212 C222 K1 112.96(15) . . ? C224 C223 C222 119.8(2) . . ? C224 C223 K1 79.45(16) . . ? C222 C223 K1 77.14(15) . . ? C224 C223 H223 120.1 . . ? C222 C223 H223 120.1 . . ? K1 C223 H223 113.8 . . ? C223 C224 C225 119.7(2) . . ? C223 C224 K1 76.36(16) . . ? C225 C224 K1 78.60(16) . . ? C223 C224 H224 120.2 . . ? C225 C224 H224 120.2 . . ? K1 C224 H224 115.6 . . ? C224 C225 C226 121.0(2) . . ? C224 C225 K1 77.38(15) . . ? C226 C225 K1 77.17(15) . . ? C224 C225 H225 119.5 . . ? C226 C225 H225 119.5 . . ? K1 C225 H225 116.6 . . ? C225 C226 C221 120.6(2) . . ? C225 C226 K1 78.56(15) . . ? C221 C226 K1 76.64(14) . . ? C225 C226 H226 119.7 . . ? C221 C226 H226 119.7 . . ? K1 C226 H226 115.7 . . ? C311 N312 K1 163.1(2) 3_656 . ? C311 N312 K1 97.59(18) 3_656 3_656 ? K1 N312 K1 98.30(7) . 3_656 ? N312 C311 Ir1 172.2(2) 3_656 . ? N312 C311 K1 62.36(16) 3_656 . ? Ir1 C311 K1 110.49(9) . . ? N412 C411 Ir1 177.3(2) . . ? C512 O511 K1 102.39(18) . . ? C512 O511 H511 109.7 . . ? K1 O511 H511 129.5 . . ? O511 C512 H51A 105.0 . . ? O511 C512 H51B 108.9 . . ? H51A C512 H51B 90.5 . . ? O511 C512 H51C 109.6 . . ? H51A C512 H51C 112.6 . . ? H51B C512 H51C 127.1 . . ? C612 O611 K1 113.9(2) . . ? C612 O611 H611 105.9 . . ? K1 O611 H611 140.1 . . ? O611 C612 H61A 117.7 . . ? O611 C612 H61B 109.3 . . ? H61A C612 H61B 124.0 . . ? O611 C612 H61C 109.9 . . ? H61A C612 H61C 99.8 . . ? H61B C612 H61C 90.9 . . ? 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 C121 Ir1 N111 C116 175.0(2) . . . . ? N211 Ir1 N111 C116 -154.5(5) . . . . ? C221 Ir1 N111 C116 -97.7(2) . . . . ? C411 Ir1 N111 C116 84.8(2) . . . . ? C311 Ir1 N111 C116 -11.0(2) . . . . ? C121 Ir1 N111 C112 -1.18(16) . . . . ? N211 Ir1 N111 C112 29.4(6) . . . . ? C221 Ir1 N111 C112 86.18(17) . . . . ? C411 Ir1 N111 C112 -91.31(17) . . . . ? C311 Ir1 N111 C112 172.89(17) . . . . ? C116 N111 C112 C113 1.3(3) . . . . ? Ir1 N111 C112 C113 177.62(18) . . . . ? C116 N111 C112 C122 -177.0(2) . . . . ? Ir1 N111 C112 C122 -0.7(3) . . . . ? N111 C112 C113 C114 -1.1(4) . . . . ? C122 C112 C113 C114 177.0(3) . . . . ? C112 C113 C114 C115 -0.3(4) . . . . ? C112 C113 C114 K1 -110.9(2) . . . 4_666 ? C113 C114 C115 C116 1.5(4) . . . . ? K1 C114 C115 C116 99.0(3) 4_666 . . . ? C112 N111 C116 C115 -0.1(4) . . . . ? Ir1 N111 C116 C115 -176.1(2) . . . . ? C114 C115 C116 N111 -1.3(4) . . . . ? N211 Ir1 C121 C126 5.5(2) . . . . ? N111 Ir1 C121 C126 -178.5(2) . . . . ? C221 Ir1 C121 C126 85.3(2) . . . . ? C411 Ir1 C121 C126 -90.0(2) . . . . ? C311 Ir1 C121 C126 132.6(6) . . . . ? N211 Ir1 C121 C122 -173.17(17) . . . . ? N111 Ir1 C121 C122 2.85(16) . . . . ? C221 Ir1 C121 C122 -93.38(18) . . . . ? C411 Ir1 C121 C122 91.38(18) . . . . ? C311 Ir1 C121 C122 -46.1(7) . . . . ? C126 C121 C122 C123 -0.9(3) . . . . ? Ir1 C121 C122 C123 177.95(18) . . . . ? C126 C121 C122 C112 177.1(2) . . . . ? Ir1 C121 C122 C112 -4.1(3) . . . . ? N111 C112 C122 C123 -178.9(2) . . . . ? C113 C112 C122 C123 2.9(4) . . . . ? N111 C112 C122 C121 3.2(3) . . . . ? C113 C112 C122 C121 -175.0(2) . . . . ? C121 C122 C123 C124 1.2(4) . . . . ? C112 C122 C123 C124 -176.6(2) . . . . ? C122 C123 C124 C125 -0.4(4) . . . . ? C123 C124 C125 C126 -0.6(4) . . . . ? C124 C125 C126 C121 0.9(4) . . . . ? C122 C121 C126 C125 -0.1(3) . . . . ? Ir1 C121 C126 C125 -178.73(18) . . . . ? C121 Ir1 N211 C216 -91.7(2) . . . . ? N111 Ir1 N211 C216 -121.9(5) . . . . ? C221 Ir1 N211 C216 -179.6(2) . . . . ? C411 Ir1 N211 C216 -1.6(2) . . . . ? C311 Ir1 N211 C216 94.5(2) . . . . ? C121 Ir1 N211 C212 85.09(17) . . . . ? N111 Ir1 N211 C212 55.0(6) . . . . ? C221 Ir1 N211 C212 -2.74(17) . . . . ? C411 Ir1 N211 C212 175.27(17) . . . . ? C311 Ir1 N211 C212 -88.65(18) . . . . ? C216 N211 C212 C213 1.8(3) . . . . ? Ir1 N211 C212 C213 -175.20(18) . . . . ? C216 N211 C212 C222 -178.7(2) . . . . ? Ir1 N211 C212 C222 4.2(3) . . . . ? N211 C212 C213 C214 -1.3(4) . . . . ? C222 C212 C213 C214 179.3(2) . . . . ? C212 C213 C214 C215 0.2(4) . . . . ? C213 C214 C215 C216 0.5(4) . . . . ? C212 N211 C216 C215 -1.2(4) . . . . ? Ir1 N211 C216 C215 175.59(19) . . . . ? C214 C215 C216 N211 0.0(4) . . . . ? C121 Ir1 C221 C226 88.8(2) . . . . ? N211 Ir1 C221 C226 -177.6(2) . . . . ? N111 Ir1 C221 C226 9.1(2) . . . . ? C411 Ir1 C221 C226 159.2(10) . . . . ? C311 Ir1 C221 C226 -85.4(2) . . . . ? C121 Ir1 C221 C222 -92.99(18) . . . . ? N211 Ir1 C221 C222 0.60(17) . . . . ? N111 Ir1 C221 C222 -172.75(17) . . . . ? C411 Ir1 C221 C222 -22.6(11) . . . . ? C311 Ir1 C221 C222 92.78(19) . . . . ? C121 Ir1 C221 K1 -177.87(11) . . . . ? N211 Ir1 C221 K1 -84.27(9) . . . . ? N111 Ir1 C221 K1 102.37(9) . . . . ? C411 Ir1 C221 K1 -107.5(10) . . . . ? C311 Ir1 C221 K1 7.90(10) . . . . ? O611 K1 C221 C226 -5.38(17) . . . . ? N312 K1 C221 C226 113.02(19) . . . . ? O511 K1 C221 C226 -150.80(15) . . . . ? N312 K1 C221 C226 117.46(16) 3_656 . . . ? C222 K1 C221 C226 -121.9(2) . . . . ? C223 K1 C221 C226 -92.72(17) . . . . ? C224 K1 C221 C226 -60.83(15) . . . . ? C311 K1 C221 C226 120.93(17) . . . . ? C225 K1 C221 C226 -29.30(14) . . . . ? C114 K1 C221 C226 -92.80(17) 4_565 . . . ? O611 K1 C221 C222 116.52(15) . . . . ? N312 K1 C221 C222 -125.08(18) . . . . ? O511 K1 C221 C222 -28.90(15) . . . . ? N312 K1 C221 C222 -120.64(15) 3_656 . . . ? C223 K1 C221 C222 29.18(14) . . . . ? C226 K1 C221 C222 121.9(2) . . . . ? C224 K1 C221 C222 61.06(14) . . . . ? C311 K1 C221 C222 -117.17(16) . . . . ? C225 K1 C221 C222 92.60(16) . . . . ? C114 K1 C221 C222 29.10(19) 4_565 . . . ? O611 K1 C221 Ir1 -132.64(11) . . . . ? N312 K1 C221 Ir1 -14.2(2) . . . . ? O511 K1 C221 Ir1 81.94(11) . . . . ? N312 K1 C221 Ir1 -9.80(10) 3_656 . . . ? C222 K1 C221 Ir1 110.84(18) . . . . ? C223 K1 C221 Ir1 140.02(15) . . . . ? C226 K1 C221 Ir1 -127.3(2) . . . . ? C224 K1 C221 Ir1 171.90(15) . . . . ? C311 K1 C221 Ir1 -6.33(8) . . . . ? C225 K1 C221 Ir1 -156.57(16) . . . . ? C114 K1 C221 Ir1 139.94(10) 4_565 . . . ? C226 C221 C222 C223 1.5(4) . . . . ? Ir1 C221 C222 C223 -176.85(19) . . . . ? K1 C221 C222 C223 -68.2(2) . . . . ? C226 C221 C222 C212 179.8(2) . . . . ? Ir1 C221 C222 C212 1.4(3) . . . . ? K1 C221 C222 C212 110.09(19) . . . . ? C226 C221 C222 K1 69.7(2) . . . . ? Ir1 C221 C222 K1 -108.66(13) . . . . ? N211 C212 C222 C223 174.6(2) . . . . ? C213 C212 C222 C223 -6.0(4) . . . . ? N211 C212 C222 C221 -3.7(3) . . . . ? C213 C212 C222 C221 175.7(2) . . . . ? N211 C212 C222 K1 84.0(2) . . . . ? C213 C212 C222 K1 -96.6(3) . . . . ? O611 K1 C222 C223 53.53(18) . . . . ? N312 K1 C222 C223 -126.4(2) . . . . ? O511 K1 C222 C223 -83.91(16) . . . . ? N312 K1 C222 C223 -179.46(16) 3_656 . . . ? C221 K1 C222 C223 126.1(2) . . . . ? C226 K1 C222 C223 94.84(17) . . . . ? C224 K1 C222 C223 29.92(15) . . . . ? C311 K1 C222 C223 175.45(17) . . . . ? C225 K1 C222 C223 62.20(16) . . . . ? C114 K1 C222 C223 -33.00(17) 4_565 . . . ? O611 K1 C222 C221 -72.55(16) . . . . ? N312 K1 C222 C221 107.5(2) . . . . ? O511 K1 C222 C221 150.01(15) . . . . ? N312 K1 C222 C221 54.46(14) 3_656 . . . ? C223 K1 C222 C221 -126.1(2) . . . . ? C226 K1 C222 C221 -31.25(13) . . . . ? C224 K1 C222 C221 -96.16(16) . . . . ? C311 K1 C222 C221 49.37(14) . . . . ? C225 K1 C222 C221 -63.88(14) . . . . ? C114 K1 C222 C221 -159.08(14) 4_565 . . . ? O611 K1 C222 C212 174.62(16) . . . . ? N312 K1 C222 C212 -5.3(3) . . . . ? O511 K1 C222 C212 37.18(16) . . . . ? N312 K1 C222 C212 -58.36(17) 3_656 . . . ? C223 K1 C222 C212 121.1(2) . . . . ? C221 K1 C222 C212 -112.8(2) . . . . ? C226 K1 C222 C212 -144.1(2) . . . . ? C224 K1 C222 C212 151.0(2) . . . . ? C311 K1 C222 C212 -63.46(16) . . . . ? C225 K1 C222 C212 -176.7(2) . . . . ? C114 K1 C222 C212 88.09(17) 4_565 . . . ? C221 C222 C223 C224 -1.4(4) . . . . ? C212 C222 C223 C224 -179.5(2) . . . . ? K1 C222 C223 C224 -69.7(2) . . . . ? C221 C222 C223 K1 68.3(2) . . . . ? C212 C222 C223 K1 -109.8(2) . . . . ? O611 K1 C223 C224 -8.66(16) . . . . ? N312 K1 C223 C224 -119.5(2) . . . . ? O511 K1 C223 C224 -147.21(16) . . . . ? N312 K1 C223 C224 124.65(15) 3_656 . . . ? C222 K1 C223 C224 124.1(2) . . . . ? C221 K1 C223 C224 94.75(17) . . . . ? C226 K1 C223 C224 61.98(15) . . . . ? C311 K1 C223 C224 119.98(16) . . . . ? C225 K1 C223 C224 29.77(14) . . . . ? C114 K1 C223 C224 -85.30(16) 4_565 . . . ? O611 K1 C223 C222 -132.74(16) . . . . ? N312 K1 C223 C222 116.4(2) . . . . ? O511 K1 C223 C222 88.71(16) . . . . ? N312 K1 C223 C222 0.57(17) 3_656 . . . ? C221 K1 C223 C222 -29.33(14) . . . . ? C226 K1 C223 C222 -62.10(15) . . . . ? C224 K1 C223 C222 -124.1(2) . . . . ? C311 K1 C223 C222 -4.10(16) . . . . ? C225 K1 C223 C222 -94.31(17) . . . . ? C114 K1 C223 C222 150.62(16) 4_565 . . . ? C222 C223 C224 C225 0.3(4) . . . . ? K1 C223 C224 C225 -68.1(2) . . . . ? C222 C223 C224 K1 68.5(2) . . . . ? O611 K1 C224 C223 171.21(17) . . . . ? N312 K1 C224 C223 124.3(2) . . . . ? O511 K1 C224 C223 31.27(16) . . . . ? N312 K1 C224 C223 -65.12(17) 3_656 . . . ? C222 K1 C224 C223 -30.58(14) . . . . ? C221 K1 C224 C223 -63.26(15) . . . . ? C226 K1 C224 C223 -95.51(17) . . . . ? C311 K1 C224 C223 -61.88(16) . . . . ? C225 K1 C224 C223 -124.7(2) . . . . ? C114 K1 C224 C223 96.31(16) 4_565 . . . ? O611 K1 C224 C225 -64.13(16) . . . . ? N312 K1 C224 C225 -111.0(2) . . . . ? O511 K1 C224 C225 155.93(16) . . . . ? N312 K1 C224 C225 59.54(18) 3_656 . . . ? C222 K1 C224 C225 94.08(17) . . . . ? C223 K1 C224 C225 124.7(2) . . . . ? C221 K1 C224 C225 61.40(15) . . . . ? C226 K1 C224 C225 29.15(14) . . . . ? C311 K1 C224 C225 62.78(16) . . . . ? C114 K1 C224 C225 -139.03(16) 4_565 . . . ? C223 C224 C225 C226 0.5(4) . . . . ? K1 C224 C225 C226 -66.4(2) . . . . ? C223 C224 C225 K1 66.9(2) . . . . ? O611 K1 C225 C224 108.31(17) . . . . ? N312 K1 C225 C224 124.75(19) . . . . ? O511 K1 C225 C224 -26.78(17) . . . . ? N312 K1 C225 C224 -129.27(16) 3_656 . . . ? C222 K1 C225 C224 -63.22(16) . . . . ? C223 K1 C225 C224 -29.98(14) . . . . ? C221 K1 C225 C224 -96.70(18) . . . . ? C226 K1 C225 C224 -126.3(2) . . . . ? C311 K1 C225 C224 -119.15(16) . . . . ? C114 K1 C225 C224 44.33(17) 4_565 . . . ? O611 K1 C225 C226 -125.36(18) . . . . ? N312 K1 C225 C226 -108.9(2) . . . . ? O511 K1 C225 C226 99.56(16) . . . . ? N312 K1 C225 C226 -2.93(18) 3_656 . . . ? C222 K1 C225 C226 63.12(16) . . . . ? C223 K1 C225 C226 96.36(18) . . . . ? C221 K1 C225 C226 29.64(15) . . . . ? C224 K1 C225 C226 126.3(2) . . . . ? C311 K1 C225 C226 7.19(16) . . . . ? C114 K1 C225 C226 170.67(16) 4_565 . . . ? C224 C225 C226 C221 -0.3(4) . . . . ? K1 C225 C226 C221 -66.8(2) . . . . ? C224 C225 C226 K1 66.5(2) . . . . ? C222 C221 C226 C225 -0.7(4) . . . . ? Ir1 C221 C226 C225 177.43(19) . . . . ? K1 C221 C226 C225 67.9(2) . . . . ? C222 C221 C226 K1 -68.5(2) . . . . ? Ir1 C221 C226 K1 109.57(19) . . . . ? O611 K1 C226 C225 49.25(17) . . . . ? N312 K1 C226 C225 120.14(19) . . . . ? O511 K1 C226 C225 -92.56(17) . . . . ? N312 K1 C226 C225 177.17(17) 3_656 . . . ? C222 K1 C226 C225 -93.91(18) . . . . ? C223 K1 C226 C225 -61.00(16) . . . . ? C221 K1 C226 C225 -125.5(2) . . . . ? C224 K1 C226 C225 -28.85(15) . . . . ? C311 K1 C226 C225 -172.09(18) . . . . ? C114 K1 C226 C225 -12.3(2) 4_565 . . . ? O611 K1 C226 C221 174.79(16) . . . . ? N312 K1 C226 C221 -114.32(19) . . . . ? O511 K1 C226 C221 32.98(17) . . . . ? N312 K1 C226 C221 -57.29(15) 3_656 . . . ? C222 K1 C226 C221 31.63(14) . . . . ? C223 K1 C226 C221 64.54(15) . . . . ? C224 K1 C226 C221 96.69(17) . . . . ? C311 K1 C226 C221 -46.55(14) . . . . ? C225 K1 C226 C221 125.5(2) . . . . ? C114 K1 C226 C221 113.29(16) 4_565 . . . ? O611 K1 N312 C311 -33.6(8) . . . 3_656 ? O511 K1 N312 C311 105.8(8) . . . 3_656 ? N312 K1 N312 C311 -160.3(8) 3_656 . . 3_656 ? C222 K1 N312 C311 146.3(7) . . . 3_656 ? C223 K1 N312 C311 79.3(8) . . . 3_656 ? C221 K1 N312 C311 -156.0(7) . . . 3_656 ? C226 K1 N312 C311 -103.0(7) . . . 3_656 ? C224 K1 N312 C311 11.6(9) . . . 3_656 ? C311 K1 N312 C311 -162.2(7) . . . 3_656 ? C225 K1 N312 C311 -48.7(8) . . . 3_656 ? C114 K1 N312 C311 42.0(8) 4_565 . . 3_656 ? O611 K1 N312 K1 126.65(9) . . . 3_656 ? O511 K1 N312 K1 -93.97(8) . . . 3_656 ? N312 K1 N312 K1 0.0 3_656 . . 3_656 ? C222 K1 N312 K1 -53.43(19) . . . 3_656 ? C223 K1 N312 K1 -120.40(18) . . . 3_656 ? C221 K1 N312 K1 4.22(19) . . . 3_656 ? C226 K1 N312 K1 57.21(17) . . . 3_656 ? C224 K1 N312 K1 171.82(16) . . . 3_656 ? C311 K1 N312 K1 -1.98(9) . . . 3_656 ? C225 K1 N312 K1 111.54(15) . . . 3_656 ? C114 K1 N312 K1 -157.70(10) 4_565 . . 3_656 ? C121 Ir1 C311 N312 -33(2) . . . 3_656 ? N211 Ir1 C311 N312 94.3(18) . . . 3_656 ? N111 Ir1 C311 N312 -81.0(18) . . . 3_656 ? C221 Ir1 C311 N312 14.6(18) . . . 3_656 ? C411 Ir1 C311 N312 -170.0(18) . . . 3_656 ? C121 Ir1 C311 K1 -55.1(7) . . . . ? N211 Ir1 C311 K1 72.08(10) . . . . ? N111 Ir1 C311 K1 -103.28(9) . . . . ? C221 Ir1 C311 K1 -7.71(10) . . . . ? C411 Ir1 C311 K1 167.70(10) . . . . ? O611 K1 C311 N312 -91.1(2) . . . 3_656 ? N312 K1 C311 N312 5.7(2) . . . 3_656 ? O511 K1 C311 N312 94.0(2) . . . 3_656 ? C222 K1 C311 N312 165.1(2) . . . 3_656 ? C223 K1 C311 N312 167.0(2) . . . 3_656 ? C221 K1 C311 N312 -170.4(2) . . . 3_656 ? C226 K1 C311 N312 -147.4(2) . . . 3_656 ? C224 K1 C311 N312 -171.8(2) . . . 3_656 ? C225 K1 C311 N312 -150.6(2) . . . 3_656 ? C114 K1 C311 N312 67.6(3) 4_565 . . 3_656 ? O611 K1 C311 Ir1 85.61(13) . . . . ? N312 K1 C311 Ir1 -177.58(10) . . . . ? O511 K1 C311 Ir1 -89.35(11) . . . . ? N312 K1 C311 Ir1 176.7(3) 3_656 . . . ? C222 K1 C311 Ir1 -18.23(9) . . . . ? C223 K1 C311 Ir1 -16.33(11) . . . . ? C221 K1 C311 Ir1 6.24(8) . . . . ? C226 K1 C311 Ir1 29.32(9) . . . . ? C224 K1 C311 Ir1 4.85(12) . . . . ? C225 K1 C311 Ir1 26.07(11) . . . . ? C114 K1 C311 Ir1 -115.75(16) 4_565 . . . ? C121 Ir1 C411 N412 -10(5) . . . . ? N211 Ir1 C411 N412 -104(5) . . . . ? N111 Ir1 C411 N412 70(5) . . . . ? C221 Ir1 C411 N412 -81(5) . . . . ? C311 Ir1 C411 N412 164(5) . . . . ? O611 K1 O511 C512 157.84(19) . . . . ? N312 K1 O511 C512 73.34(19) . . . . ? N312 K1 O511 C512 -8.19(19) 3_656 . . . ? C222 K1 O511 C512 -90.71(19) . . . . ? C223 K1 O511 C512 -116.45(19) . . . . ? C221 K1 O511 C512 -78.53(19) . . . . ? C226 K1 O511 C512 -91.7(2) . . . . ? C224 K1 O511 C512 -129.29(19) . . . . ? C311 K1 O511 C512 -28.23(19) . . . . ? C225 K1 O511 C512 -118.70(19) . . . . ? C114 K1 O511 C512 139.5(2) 4_565 . . . ? N312 K1 O611 C612 -27.1(3) . . . . ? O511 K1 O611 C612 -111.5(3) . . . . ? N312 K1 O611 C612 51.2(3) 3_656 . . . ? C222 K1 O611 C612 152.9(3) . . . . ? C223 K1 O611 C612 172.9(3) . . . . ? C221 K1 O611 C612 128.2(3) . . . . ? C226 K1 O611 C612 126.0(3) . . . . ? C224 K1 O611 C612 169.2(3) . . . . ? C311 K1 O611 C612 76.2(3) . . . . ? C225 K1 O611 C612 145.8(3) . . . . ? C114 K1 O611 C612 -94.5(3) 4_565 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.080 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.094 #===END data_imw1429_0m _database_code_depnum_ccdc_archive 'CCDC 834576' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Ir N9 Nd O8' _chemical_formula_weight 980.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0888(4) _cell_length_b 12.1712(5) _cell_length_c 12.9413(5) _cell_angle_alpha 100.582(2) _cell_angle_beta 95.497(2) _cell_angle_gamma 90.196(2) _cell_volume 1708.62(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9756 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.52 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 5.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3938 _exptl_absorpt_correction_T_max 0.5852 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45791 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7855 _reflns_number_gt 7393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+2.2719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7855 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.554884(8) 0.779789(7) 0.742424(7) 0.01096(3) Uani 1 1 d . . . Nd1 Nd 0.251702(11) 1.094576(10) 0.580657(9) 0.01098(3) Uani 1 1 d . . . O1 O 0.14387(16) 1.04752(14) 0.73306(13) 0.0168(4) Uani 1 1 d . . . O2 O 0.05264(17) 0.88771(15) 0.73027(14) 0.0234(4) Uani 1 1 d . . . O3 O 0.13013(16) 0.92179(14) 0.58987(13) 0.0169(4) Uani 1 1 d . . . O4 O 0.13617(15) 1.00183(14) 0.40291(13) 0.0168(4) Uani 1 1 d . . . O5 O 0.20904(18) 0.86455(16) 0.29542(14) 0.0280(5) Uani 1 1 d . . . O6 O 0.31763(16) 0.94673(15) 0.43906(14) 0.0204(4) Uani 1 1 d . . . N1 N 0.67005(18) 0.87942(16) 0.85578(15) 0.0133(4) Uani 1 1 d . . . N2 N 0.43835(18) 0.66453(17) 0.64563(15) 0.0144(4) Uani 1 1 d . . . N3 N 0.39754(19) 0.98256(17) 0.68050(16) 0.0163(4) Uani 1 1 d . . . N4 N 0.10648(19) 0.95077(17) 0.68695(16) 0.0162(4) Uani 1 1 d . . . N5 N 0.2191(2) 0.93525(18) 0.37568(16) 0.0177(4) Uani 1 1 d . . . N6 N 0.72204(19) 0.78266(17) 0.55440(16) 0.0175(4) Uani 1 1 d . . . C1 C 0.7755(2) 0.9247(2) 0.8376(2) 0.0168(5) Uani 1 1 d . . . H2 H 0.7988 0.9113 0.7677 0.020 Uiso 1 1 calc R . . H3 H 0.9235 1.0147 0.9021 0.020 Uiso 1 1 d R . . C2 C 0.8504(2) 0.9897(2) 0.9165(2) 0.0206(6) Uani 1 1 d . . . C3 C 0.8169(2) 1.0089(2) 1.0190(2) 0.0225(6) Uani 1 1 d . . . H4 H 0.8668 1.0539 1.0747 0.027 Uiso 1 1 calc R . . C4 C 0.7099(2) 0.9615(2) 1.03864(19) 0.0184(5) Uani 1 1 d . . . H5 H 0.6868 0.9728 1.1085 0.022 Uiso 1 1 calc R . . C5 C 0.6360(2) 0.8972(2) 0.95641(19) 0.0152(5) Uani 1 1 d . . . C6 C 0.5216(2) 0.8419(2) 0.96721(19) 0.0147(5) Uani 1 1 d . . . C7 C 0.4726(2) 0.8496(2) 1.0641(2) 0.0196(5) Uani 1 1 d . . . H8 H 0.5126 0.8939 1.1261 0.024 Uiso 1 1 calc R . . C8 C 0.3657(3) 0.7926(2) 1.0694(2) 0.0225(6) Uani 1 1 d . . . H9 H 0.3322 0.7977 1.1349 0.027 Uiso 1 1 calc R . . C9 C 0.3075(3) 0.7275(2) 0.9780(2) 0.0229(6) Uani 1 1 d . . . H10 H 0.2353 0.6868 0.9817 0.027 Uiso 1 1 calc R . . C10 C 0.3551(2) 0.7220(2) 0.8812(2) 0.0188(5) Uani 1 1 d . . . H11 H 0.3136 0.6785 0.8195 0.023 Uiso 1 1 calc R . . C11 C 0.4626(2) 0.7791(2) 0.87276(19) 0.0143(5) Uani 1 1 d . . . C12 C 0.6331(2) 0.6341(2) 0.77074(19) 0.0147(5) Uani 1 1 d . . . C13 C 0.7372(2) 0.6200(2) 0.8372(2) 0.0205(5) Uani 1 1 d . . . H13 H 0.7788 0.6838 0.8788 0.025 Uiso 1 1 calc R . . C14 C 0.7803(3) 0.5144(2) 0.8431(2) 0.0250(6) Uani 1 1 d . . . H14 H 0.8514 0.5069 0.8882 0.030 Uiso 1 1 calc R . . C15 C 0.7210(3) 0.4194(2) 0.7842(2) 0.0261(6) Uani 1 1 d . . . H15 H 0.7522 0.3475 0.7880 0.031 Uiso 1 1 calc R . . C16 C 0.6162(3) 0.4298(2) 0.7197(2) 0.0231(6) Uani 1 1 d . . . H16 H 0.5743 0.3652 0.6800 0.028 Uiso 1 1 calc R . . C17 C 0.5724(2) 0.5365(2) 0.71360(19) 0.0169(5) Uani 1 1 d . . . C18 C 0.4633(2) 0.5545(2) 0.64526(19) 0.0164(5) Uani 1 1 d . . . C19 C 0.3873(2) 0.4709(2) 0.5834(2) 0.0235(6) Uani 1 1 d . . . H19 H 0.4041 0.3946 0.5842 0.028 Uiso 1 1 calc R . . C20 C 0.2886(2) 0.4981(2) 0.5214(2) 0.0258(6) Uani 1 1 d . . . H20 H 0.2375 0.4411 0.4789 0.031 Uiso 1 1 calc R . . C21 C 0.2644(2) 0.6102(2) 0.5216(2) 0.0235(6) Uani 1 1 d . . . H21 H 0.1967 0.6310 0.4791 0.028 Uiso 1 1 calc R . . C22 C 0.3409(2) 0.6906(2) 0.5848(2) 0.0186(5) Uani 1 1 d . . . H22 H 0.3240 0.7672 0.5855 0.022 Uiso 1 1 calc R . . C23 C 0.6624(2) 0.78136(19) 0.62319(19) 0.0137(5) Uani 1 1 d . . . C24 C 0.4590(2) 0.9136(2) 0.70607(18) 0.0133(5) Uani 1 1 d . . . C1S C 0.0163(3) 0.5088(2) 0.6478(2) 0.0264(6) Uani 1 1 d . . . C2S C 0.0099(3) 0.6276(2) 0.6914(3) 0.0364(8) Uani 1 1 d . . . H2S1 H 0.0403 0.6412 0.7664 0.055 Uiso 1 1 calc R . . H2S2 H -0.0744 0.6511 0.6839 0.055 Uiso 1 1 calc R . . H2S3 H 0.0595 0.6703 0.6533 0.055 Uiso 1 1 calc R . . C3S C 0.0241(3) 0.2704(3) 0.8766(3) 0.0549(10) Uani 1 1 d . . . H3S1 H 0.0925 0.2223 0.8892 0.082 Uiso 1 1 calc R . . H3S2 H -0.0173 0.2436 0.8061 0.082 Uiso 1 1 calc R . . H3S3 H -0.0328 0.2686 0.9298 0.082 Uiso 1 1 calc R . . C4S C 0.0684(3) 0.3850(3) 0.8839(3) 0.0393(8) Uani 1 1 d . . . C5S C 0.3958(3) 1.4068(2) 0.9005(2) 0.0254(6) Uani 1 1 d . . . C6S C 0.3417(2) 1.3242(2) 0.8104(2) 0.0192(5) Uani 1 1 d . . . N1S N 0.0217(2) 0.4159(2) 0.6126(2) 0.0329(6) Uani 1 1 d . . . N2S N 0.1037(3) 0.4748(3) 0.8911(2) 0.0465(8) Uani 1 1 d . . . N3S N 0.2992(2) 1.26009(18) 0.74025(17) 0.0221(5) Uani 1 1 d . . . O1S O 0.05463(15) 1.18404(14) 0.56539(13) 0.0166(4) Uani 1 1 d . . . O2S O 0.46781(16) 1.15766(15) 0.57661(15) 0.0223(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01205(5) 0.01095(5) 0.00990(5) 0.00185(3) 0.00124(3) 0.00074(3) Nd1 0.01066(7) 0.01111(6) 0.01083(6) 0.00128(5) 0.00065(5) 0.00101(5) O1 0.0198(9) 0.0152(9) 0.0144(8) 0.0006(7) 0.0008(7) -0.0015(7) O2 0.0278(11) 0.0230(10) 0.0219(9) 0.0103(8) 0.0039(8) -0.0065(8) O3 0.0187(9) 0.0178(9) 0.0131(8) 0.0000(7) 0.0018(7) -0.0010(7) O4 0.0159(9) 0.0179(9) 0.0159(8) 0.0015(7) 0.0012(7) 0.0028(7) O5 0.0368(12) 0.0255(10) 0.0175(9) -0.0080(8) 0.0041(8) 0.0002(9) O6 0.0172(9) 0.0232(10) 0.0188(9) -0.0011(7) 0.0011(7) 0.0049(8) N1 0.0136(10) 0.0137(10) 0.0127(10) 0.0035(8) 0.0000(8) 0.0030(8) N2 0.0143(11) 0.0158(10) 0.0130(10) 0.0015(8) 0.0029(8) -0.0011(8) N3 0.0166(11) 0.0160(10) 0.0160(10) 0.0033(8) -0.0003(8) -0.0002(9) N4 0.0156(11) 0.0189(11) 0.0145(10) 0.0049(8) -0.0001(8) 0.0013(9) N5 0.0199(12) 0.0180(11) 0.0149(10) 0.0017(8) 0.0032(9) -0.0013(9) N6 0.0200(11) 0.0168(11) 0.0155(10) 0.0017(8) 0.0035(9) -0.0013(9) C1 0.0167(13) 0.0172(12) 0.0168(12) 0.0041(10) 0.0004(10) 0.0012(10) C2 0.0149(13) 0.0214(13) 0.0243(14) 0.0032(11) -0.0017(11) -0.0009(11) C3 0.0198(14) 0.0246(14) 0.0198(13) -0.0005(11) -0.0059(11) 0.0011(11) C4 0.0211(14) 0.0202(13) 0.0118(11) -0.0002(10) -0.0026(10) 0.0059(11) C5 0.0176(13) 0.0150(12) 0.0138(11) 0.0048(9) 0.0008(10) 0.0059(10) C6 0.0164(13) 0.0126(11) 0.0165(12) 0.0053(9) 0.0028(10) 0.0041(10) C7 0.0269(15) 0.0184(13) 0.0144(12) 0.0035(10) 0.0046(11) 0.0065(11) C8 0.0297(16) 0.0214(13) 0.0199(13) 0.0074(11) 0.0128(11) 0.0065(11) C9 0.0223(14) 0.0202(13) 0.0290(15) 0.0071(11) 0.0119(12) 0.0016(11) C10 0.0195(14) 0.0181(12) 0.0189(12) 0.0025(10) 0.0043(10) 0.0019(10) C11 0.0151(12) 0.0137(11) 0.0148(11) 0.0039(9) 0.0028(10) 0.0045(9) C12 0.0160(13) 0.0161(12) 0.0143(11) 0.0053(9) 0.0085(10) 0.0038(10) C13 0.0227(14) 0.0222(13) 0.0174(12) 0.0050(10) 0.0036(11) 0.0047(11) C14 0.0247(15) 0.0293(15) 0.0245(14) 0.0124(12) 0.0056(12) 0.0118(12) C15 0.0310(16) 0.0196(14) 0.0326(15) 0.0127(12) 0.0130(13) 0.0103(12) C16 0.0294(16) 0.0148(12) 0.0272(14) 0.0048(11) 0.0118(12) 0.0026(11) C17 0.0187(13) 0.0170(12) 0.0173(12) 0.0055(10) 0.0095(10) 0.0012(10) C18 0.0189(13) 0.0161(12) 0.0156(12) 0.0021(10) 0.0101(10) 0.0005(10) C19 0.0258(15) 0.0158(13) 0.0284(14) -0.0011(11) 0.0098(12) -0.0037(11) C20 0.0210(15) 0.0245(14) 0.0280(15) -0.0055(12) 0.0035(12) -0.0082(11) C21 0.0172(14) 0.0276(14) 0.0231(14) -0.0014(11) 0.0001(11) -0.0021(11) C22 0.0174(13) 0.0177(12) 0.0197(12) 0.0013(10) 0.0010(10) -0.0007(10) C23 0.0152(12) 0.0107(11) 0.0141(11) 0.0015(9) -0.0027(10) -0.0002(9) C24 0.0138(12) 0.0143(12) 0.0109(11) 0.0005(9) 0.0009(9) -0.0019(10) C1S 0.0235(15) 0.0252(15) 0.0298(15) 0.0034(12) 0.0015(12) -0.0015(12) C2S 0.045(2) 0.0200(15) 0.0425(18) -0.0027(13) 0.0108(15) -0.0007(13) C3S 0.033(2) 0.053(2) 0.071(3) -0.010(2) 0.0091(18) 0.0014(17) C4S 0.0234(17) 0.055(2) 0.0324(17) -0.0078(16) -0.0028(13) 0.0109(16) C5S 0.0275(15) 0.0237(14) 0.0207(13) -0.0061(11) -0.0007(11) -0.0030(12) C6S 0.0179(13) 0.0183(13) 0.0222(13) 0.0035(11) 0.0060(11) 0.0022(10) N1S 0.0271(14) 0.0244(13) 0.0438(15) 0.0015(12) -0.0044(12) -0.0001(11) N2S 0.0343(17) 0.056(2) 0.0442(17) -0.0009(15) -0.0040(13) 0.0065(15) N3S 0.0247(12) 0.0189(11) 0.0218(11) -0.0002(9) 0.0052(10) 0.0001(9) O1S 0.0127(9) 0.0179(9) 0.0192(9) 0.0026(7) 0.0024(7) 0.0022(7) O2S 0.0138(9) 0.0232(10) 0.0308(10) 0.0074(8) 0.0022(8) -0.0003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C23 2.041(3) . ? Ir1 C24 2.050(2) . ? Ir1 C12 2.054(2) . ? Ir1 C11 2.056(2) . ? Ir1 N1 2.057(2) . ? Ir1 N2 2.059(2) . ? Nd1 O1S 2.4520(17) . ? Nd1 O6 2.4869(17) . ? Nd1 O3 2.5214(17) . ? Nd1 O2S 2.5221(18) . ? Nd1 N3 2.531(2) . ? Nd1 N6 2.535(2) 2_676 ? Nd1 O1 2.5514(17) . ? Nd1 O4 2.5843(17) . ? Nd1 N3S 2.619(2) . ? Nd1 N4 2.973(2) . ? Nd1 N5 2.975(2) . ? O1 N4 1.267(3) . ? O2 N4 1.216(3) . ? O3 N4 1.293(3) . ? O4 N5 1.260(3) . ? O5 N5 1.217(3) . ? O6 N5 1.293(3) . ? N1 C1 1.350(3) . ? N1 C5 1.370(3) . ? N2 C22 1.349(3) . ? N2 C18 1.368(3) . ? N3 C24 1.158(3) . ? N6 C23 1.161(3) . ? N6 Nd1 2.535(2) 2_676 ? C1 C2 1.377(3) . ? C1 H2 0.9500 . ? C2 C3 1.390(4) . ? C2 H3 0.9118 . ? C3 C4 1.383(4) . ? C3 H4 0.9500 . ? C4 C5 1.393(3) . ? C4 H5 0.9500 . ? C5 C6 1.465(3) . ? C6 C7 1.402(3) . ? C6 C11 1.416(3) . ? C7 C8 1.385(4) . ? C7 H8 0.9500 . ? C8 C9 1.396(4) . ? C8 H9 0.9500 . ? C9 C10 1.396(4) . ? C9 H10 0.9500 . ? C10 C11 1.401(4) . ? C10 H11 0.9500 . ? C12 C13 1.403(4) . ? C12 C17 1.409(3) . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 C17 1.401(4) . ? C16 H16 0.9500 . ? C17 C18 1.470(4) . ? C18 C19 1.397(4) . ? C19 C20 1.372(4) . ? C19 H19 0.9500 . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C1S N1S 1.144(4) . ? C1S C2S 1.456(4) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S C4S 1.461(5) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S N2S 1.144(5) . ? C5S C6S 1.470(4) . ? C6S N3S 1.145(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Ir1 C24 92.15(9) . . ? C23 Ir1 C12 89.68(9) . . ? C24 Ir1 C12 173.11(9) . . ? C23 Ir1 C11 174.14(9) . . ? C24 Ir1 C11 91.27(9) . . ? C12 Ir1 C11 87.47(9) . . ? C23 Ir1 N1 94.97(9) . . ? C24 Ir1 N1 92.76(8) . . ? C12 Ir1 N1 93.69(9) . . ? C11 Ir1 N1 80.12(9) . . ? C23 Ir1 N2 90.95(8) . . ? C24 Ir1 N2 93.42(9) . . ? C12 Ir1 N2 79.91(9) . . ? C11 Ir1 N2 93.59(9) . . ? N1 Ir1 N2 171.28(8) . . ? O1S Nd1 O6 122.53(6) . . ? O1S Nd1 O3 85.17(6) . . ? O6 Nd1 O3 74.61(6) . . ? O1S Nd1 O2S 134.32(6) . . ? O6 Nd1 O2S 79.49(6) . . ? O3 Nd1 O2S 140.42(6) . . ? O1S Nd1 N3 148.60(6) . . ? O6 Nd1 N3 76.75(6) . . ? O3 Nd1 N3 76.19(6) . . ? O2S Nd1 N3 69.03(6) . . ? O1S Nd1 N6 77.08(6) . 2_676 ? O6 Nd1 N6 82.49(6) . 2_676 ? O3 Nd1 N6 136.95(6) . 2_676 ? O2S Nd1 N6 66.13(6) . 2_676 ? N3 Nd1 N6 133.16(7) . 2_676 ? O1S Nd1 O1 75.42(6) . . ? O6 Nd1 O1 121.89(6) . . ? O3 Nd1 O1 50.60(5) . . ? O2S Nd1 O1 130.08(6) . . ? N3 Nd1 O1 73.21(6) . . ? N6 Nd1 O1 150.42(6) 2_676 . ? O1S Nd1 O4 72.22(5) . . ? O6 Nd1 O4 50.35(5) . . ? O3 Nd1 O4 65.85(5) . . ? O2S Nd1 O4 117.09(6) . . ? N3 Nd1 O4 120.28(6) . . ? N6 Nd1 O4 71.42(6) 2_676 . ? O1 Nd1 O4 109.67(5) . . ? O1S Nd1 N3S 83.28(6) . . ? O6 Nd1 N3S 151.41(7) . . ? O3 Nd1 N3S 123.79(6) . . ? O2S Nd1 N3S 72.93(7) . . ? N3 Nd1 N3S 86.38(7) . . ? N6 Nd1 N3S 92.94(7) 2_676 . ? O1 Nd1 N3S 73.26(6) . . ? O4 Nd1 N3S 153.19(6) . . ? O1S Nd1 N4 80.10(6) . . ? O6 Nd1 N4 98.30(6) . . ? O3 Nd1 N4 25.57(5) . . ? O2S Nd1 N4 140.56(6) . . ? N3 Nd1 N4 72.14(6) . . ? N6 Nd1 N4 153.18(6) 2_676 . ? O1 Nd1 N4 25.06(5) . . ? O4 Nd1 N4 88.36(6) . . ? N3S Nd1 N4 98.23(6) . . ? O1S Nd1 N5 97.18(6) . . ? O6 Nd1 N5 25.43(6) . . ? O3 Nd1 N5 67.11(5) . . ? O2S Nd1 N5 99.49(6) . . ? N3 Nd1 N5 98.46(6) . . ? N6 Nd1 N5 76.53(6) 2_676 . ? O1 Nd1 N5 117.54(6) . . ? O4 Nd1 N5 24.96(6) . . ? N3S Nd1 N5 169.01(6) . . ? N4 Nd1 N5 92.65(6) . . ? N4 O1 Nd1 96.42(13) . . ? N4 O3 Nd1 97.12(13) . . ? N5 O4 Nd1 95.13(13) . . ? N5 O6 Nd1 98.89(13) . . ? C1 N1 C5 119.3(2) . . ? C1 N1 Ir1 124.64(16) . . ? C5 N1 Ir1 116.04(16) . . ? C22 N2 C18 119.2(2) . . ? C22 N2 Ir1 124.60(17) . . ? C18 N2 Ir1 116.24(16) . . ? C24 N3 Nd1 164.78(18) . . ? O2 N4 O1 123.0(2) . . ? O2 N4 O3 121.3(2) . . ? O1 N4 O3 115.73(19) . . ? O2 N4 Nd1 176.21(17) . . ? O1 N4 Nd1 58.52(11) . . ? O3 N4 Nd1 57.31(11) . . ? O5 N5 O4 123.2(2) . . ? O5 N5 O6 121.3(2) . . ? O4 N5 O6 115.47(19) . . ? O5 N5 Nd1 175.57(17) . . ? O4 N5 Nd1 59.91(11) . . ? O6 N5 Nd1 55.68(11) . . ? C23 N6 Nd1 137.03(19) . 2_676 ? N1 C1 C2 122.5(2) . . ? N1 C1 H2 118.8 . . ? C2 C1 H2 118.8 . . ? C1 C2 C3 118.9(2) . . ? C1 C2 H3 119.9 . . ? C3 C2 H3 121.0 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H4 120.5 . . ? C2 C3 H4 120.5 . . ? C3 C4 C5 120.3(2) . . ? C3 C4 H5 119.8 . . ? C5 C4 H5 119.8 . . ? N1 C5 C4 120.0(2) . . ? N1 C5 C6 114.6(2) . . ? C4 C5 C6 125.5(2) . . ? C7 C6 C11 121.5(2) . . ? C7 C6 C5 122.8(2) . . ? C11 C6 C5 115.6(2) . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H8 120.0 . . ? C6 C7 H8 120.0 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H9 120.2 . . ? C9 C8 H9 120.2 . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H10 119.9 . . ? C8 C9 H10 119.9 . . ? C9 C10 C11 121.6(2) . . ? C9 C10 H11 119.2 . . ? C11 C10 H11 119.2 . . ? C10 C11 C6 116.9(2) . . ? C10 C11 Ir1 129.35(18) . . ? C6 C11 Ir1 113.64(17) . . ? C13 C12 C17 117.2(2) . . ? C13 C12 Ir1 128.85(19) . . ? C17 C12 Ir1 113.96(18) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C12 121.7(2) . . ? C16 C17 C18 122.7(2) . . ? C12 C17 C18 115.7(2) . . ? N2 C18 C19 119.9(2) . . ? N2 C18 C17 114.2(2) . . ? C19 C18 C17 125.9(2) . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.2(2) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 118.6(3) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? N2 C22 C21 122.6(2) . . ? N2 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N6 C23 Ir1 179.0(2) . . ? N3 C24 Ir1 174.1(2) . . ? N1S C1S C2S 179.2(3) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C4S C3S H3S1 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C4S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N2S C4S C3S 179.0(4) . . ? N3S C6S C5S 179.8(3) . . ? C6S N3S Nd1 166.9(2) . . ? 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 O1S Nd1 O1 N4 97.87(13) . . . . ? O6 Nd1 O1 N4 -21.65(15) . . . . ? O3 Nd1 O1 N4 2.08(12) . . . . ? O2S Nd1 O1 N4 -125.69(13) . . . . ? N3 Nd1 O1 N4 -83.63(13) . . . . ? N6 Nd1 O1 N4 120.03(15) 2_676 . . . ? O4 Nd1 O1 N4 33.21(14) . . . . ? N3S Nd1 O1 N4 -174.88(14) . . . . ? N5 Nd1 O1 N4 7.29(15) . . . . ? O1S Nd1 O3 N4 -77.12(13) . . . . ? O6 Nd1 O3 N4 157.22(14) . . . . ? O2S Nd1 O3 N4 106.27(14) . . . . ? N3 Nd1 O3 N4 77.42(13) . . . . ? N6 Nd1 O3 N4 -142.34(13) 2_676 . . . ? O1 Nd1 O3 N4 -2.04(12) . . . . ? O4 Nd1 O3 N4 -149.79(14) . . . . ? N3S Nd1 O3 N4 1.47(15) . . . . ? N5 Nd1 O3 N4 -177.02(14) . . . . ? O1S Nd1 O4 N5 179.99(14) . . . . ? O6 Nd1 O4 N5 2.33(12) . . . . ? O3 Nd1 O4 N5 -87.32(14) . . . . ? O2S Nd1 O4 N5 48.69(14) . . . . ? N3 Nd1 O4 N5 -31.72(15) . . . . ? N6 Nd1 O4 N5 98.04(14) 2_676 . . . ? O1 Nd1 O4 N5 -113.29(13) . . . . ? N3S Nd1 O4 N5 155.02(15) . . . . ? N4 Nd1 O4 N5 -99.87(13) . . . . ? O1S Nd1 O6 N5 -4.93(16) . . . . ? O3 Nd1 O6 N5 68.86(13) . . . . ? O2S Nd1 O6 N5 -141.35(14) . . . . ? N3 Nd1 O6 N5 147.93(14) . . . . ? N6 Nd1 O6 N5 -74.35(14) 2_676 . . . ? O1 Nd1 O6 N5 87.67(14) . . . . ? O4 Nd1 O6 N5 -2.29(12) . . . . ? N3S Nd1 O6 N5 -156.67(15) . . . . ? N4 Nd1 O6 N5 78.59(14) . . . . ? C23 Ir1 N1 C1 2.0(2) . . . . ? C24 Ir1 N1 C1 -90.4(2) . . . . ? C12 Ir1 N1 C1 92.0(2) . . . . ? C11 Ir1 N1 C1 178.8(2) . . . . ? N2 Ir1 N1 C1 134.5(5) . . . . ? C23 Ir1 N1 C5 -176.42(17) . . . . ? C24 Ir1 N1 C5 91.18(17) . . . . ? C12 Ir1 N1 C5 -86.42(17) . . . . ? C11 Ir1 N1 C5 0.36(17) . . . . ? N2 Ir1 N1 C5 -43.9(6) . . . . ? C23 Ir1 N2 C22 -90.5(2) . . . . ? C24 Ir1 N2 C22 1.7(2) . . . . ? C12 Ir1 N2 C22 180.0(2) . . . . ? C11 Ir1 N2 C22 93.2(2) . . . . ? N1 Ir1 N2 C22 136.7(5) . . . . ? C23 Ir1 N2 C18 90.00(18) . . . . ? C24 Ir1 N2 C18 -177.79(17) . . . . ? C12 Ir1 N2 C18 0.49(17) . . . . ? C11 Ir1 N2 C18 -86.29(18) . . . . ? N1 Ir1 N2 C18 -42.8(6) . . . . ? O1S Nd1 N3 C24 113.2(7) . . . . ? O6 Nd1 N3 C24 -19.2(7) . . . . ? O3 Nd1 N3 C24 57.9(7) . . . . ? O2S Nd1 N3 C24 -102.9(7) . . . . ? N6 Nd1 N3 C24 -85.3(7) 2_676 . . . ? O1 Nd1 N3 C24 110.4(7) . . . . ? O4 Nd1 N3 C24 7.1(8) . . . . ? N3S Nd1 N3 C24 -176.0(7) . . . . ? N4 Nd1 N3 C24 84.2(7) . . . . ? N5 Nd1 N3 C24 -5.9(7) . . . . ? Nd1 O1 N4 O2 175.9(2) . . . . ? Nd1 O1 N4 O3 -3.5(2) . . . . ? Nd1 O3 N4 O2 -175.84(19) . . . . ? Nd1 O3 N4 O1 3.5(2) . . . . ? O1S Nd1 N4 O2 169(2) . . . . ? O6 Nd1 N4 O2 47(2) . . . . ? O3 Nd1 N4 O2 69(2) . . . . ? O2S Nd1 N4 O2 -36(2) . . . . ? N3 Nd1 N4 O2 -26(2) . . . . ? N6 Nd1 N4 O2 137(2) 2_676 . . . ? O1 Nd1 N4 O2 -114(2) . . . . ? O4 Nd1 N4 O2 97(2) . . . . ? N3S Nd1 N4 O2 -109(2) . . . . ? N5 Nd1 N4 O2 72(2) . . . . ? O1S Nd1 N4 O1 -76.70(13) . . . . ? O6 Nd1 N4 O1 161.55(13) . . . . ? O3 Nd1 N4 O1 -176.3(2) . . . . ? O2S Nd1 N4 O1 78.03(16) . . . . ? N3 Nd1 N4 O1 88.43(13) . . . . ? N6 Nd1 N4 O1 -108.69(17) 2_676 . . . ? O4 Nd1 N4 O1 -148.94(13) . . . . ? N3S Nd1 N4 O1 4.96(14) . . . . ? N5 Nd1 N4 O1 -173.53(13) . . . . ? O1S Nd1 N4 O3 99.58(13) . . . . ? O6 Nd1 N4 O3 -22.17(13) . . . . ? O2S Nd1 N4 O3 -105.69(14) . . . . ? N3 Nd1 N4 O3 -95.29(13) . . . . ? N6 Nd1 N4 O3 67.60(19) 2_676 . . . ? O1 Nd1 N4 O3 176.3(2) . . . . ? O4 Nd1 N4 O3 27.34(13) . . . . ? N3S Nd1 N4 O3 -178.76(13) . . . . ? N5 Nd1 N4 O3 2.75(13) . . . . ? Nd1 O4 N5 O5 176.3(2) . . . . ? Nd1 O4 N5 O6 -3.8(2) . . . . ? Nd1 O6 N5 O5 -176.16(19) . . . . ? Nd1 O6 N5 O4 4.0(2) . . . . ? O1S Nd1 N5 O5 -136(2) . . . . ? O6 Nd1 N5 O5 48(2) . . . . ? O3 Nd1 N5 O5 -55(2) . . . . ? O2S Nd1 N5 O5 86(2) . . . . ? N3 Nd1 N5 O5 16(2) . . . . ? N6 Nd1 N5 O5 149(2) 2_676 . . . ? O1 Nd1 N5 O5 -59(2) . . . . ? O4 Nd1 N5 O5 -136(2) . . . . ? N3S Nd1 N5 O5 132(2) . . . . ? N4 Nd1 N5 O5 -56(2) . . . . ? O1S Nd1 N5 O4 -0.01(14) . . . . ? O6 Nd1 N5 O4 -175.8(2) . . . . ? O3 Nd1 N5 O4 81.63(13) . . . . ? O2S Nd1 N5 O4 -137.32(13) . . . . ? N3 Nd1 N5 O4 152.68(13) . . . . ? N6 Nd1 N5 O4 -74.83(14) 2_676 . . . ? O1 Nd1 N5 O4 77.26(14) . . . . ? N3S Nd1 N5 O4 -91.8(4) . . . . ? N4 Nd1 N5 O4 80.35(13) . . . . ? O1S Nd1 N5 O6 175.82(13) . . . . ? O3 Nd1 N5 O6 -102.55(14) . . . . ? O2S Nd1 N5 O6 38.50(14) . . . . ? N3 Nd1 N5 O6 -31.50(14) . . . . ? N6 Nd1 N5 O6 101.00(14) 2_676 . . . ? O1 Nd1 N5 O6 -106.92(14) . . . . ? O4 Nd1 N5 O6 175.8(2) . . . . ? N3S Nd1 N5 O6 84.0(4) . . . . ? N4 Nd1 N5 O6 -103.83(14) . . . . ? C5 N1 C1 C2 -0.7(4) . . . . ? Ir1 N1 C1 C2 -179.06(19) . . . . ? N1 C1 C2 C3 0.4(4) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C1 N1 C5 C4 0.0(3) . . . . ? Ir1 N1 C5 C4 178.52(18) . . . . ? C1 N1 C5 C6 -178.6(2) . . . . ? Ir1 N1 C5 C6 -0.1(3) . . . . ? C3 C4 C5 N1 0.9(4) . . . . ? C3 C4 C5 C6 179.3(2) . . . . ? N1 C5 C6 C7 179.5(2) . . . . ? C4 C5 C6 C7 1.0(4) . . . . ? N1 C5 C6 C11 -0.4(3) . . . . ? C4 C5 C6 C11 -178.9(2) . . . . ? C11 C6 C7 C8 1.8(4) . . . . ? C5 C6 C7 C8 -178.1(2) . . . . ? C6 C7 C8 C9 0.1(4) . . . . ? C7 C8 C9 C10 -1.5(4) . . . . ? C8 C9 C10 C11 1.2(4) . . . . ? C9 C10 C11 C6 0.6(4) . . . . ? C9 C10 C11 Ir1 177.19(19) . . . . ? C7 C6 C11 C10 -2.1(4) . . . . ? C5 C6 C11 C10 177.8(2) . . . . ? C7 C6 C11 Ir1 -179.20(19) . . . . ? C5 C6 C11 Ir1 0.7(3) . . . . ? C23 Ir1 C11 C10 -144.0(8) . . . . ? C24 Ir1 C11 C10 90.2(2) . . . . ? C12 Ir1 C11 C10 -83.1(2) . . . . ? N1 Ir1 C11 C10 -177.3(2) . . . . ? N2 Ir1 C11 C10 -3.4(2) . . . . ? C23 Ir1 C11 C6 32.7(10) . . . . ? C24 Ir1 C11 C6 -93.16(18) . . . . ? C12 Ir1 C11 C6 93.62(18) . . . . ? N1 Ir1 C11 C6 -0.58(17) . . . . ? N2 Ir1 C11 C6 173.34(18) . . . . ? C23 Ir1 C12 C13 88.5(2) . . . . ? C24 Ir1 C12 C13 -166.0(7) . . . . ? C11 Ir1 C12 C13 -86.3(2) . . . . ? N1 Ir1 C12 C13 -6.4(2) . . . . ? N2 Ir1 C12 C13 179.6(2) . . . . ? C23 Ir1 C12 C17 -90.74(18) . . . . ? C24 Ir1 C12 C17 14.7(8) . . . . ? C11 Ir1 C12 C17 94.38(18) . . . . ? N1 Ir1 C12 C17 174.30(18) . . . . ? N2 Ir1 C12 C17 0.28(17) . . . . ? C17 C12 C13 C14 2.2(4) . . . . ? Ir1 C12 C13 C14 -177.1(2) . . . . ? C12 C13 C14 C15 -0.6(4) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C15 C16 C17 C12 0.6(4) . . . . ? C15 C16 C17 C18 178.6(2) . . . . ? C13 C12 C17 C16 -2.2(4) . . . . ? Ir1 C12 C17 C16 177.17(19) . . . . ? C13 C12 C17 C18 179.7(2) . . . . ? Ir1 C12 C17 C18 -1.0(3) . . . . ? C22 N2 C18 C19 -0.8(3) . . . . ? Ir1 N2 C18 C19 178.72(18) . . . . ? C22 N2 C18 C17 179.4(2) . . . . ? Ir1 N2 C18 C17 -1.1(3) . . . . ? C16 C17 C18 N2 -176.7(2) . . . . ? C12 C17 C18 N2 1.4(3) . . . . ? C16 C17 C18 C19 3.4(4) . . . . ? C12 C17 C18 C19 -178.5(2) . . . . ? N2 C18 C19 C20 1.1(4) . . . . ? C17 C18 C19 C20 -179.1(2) . . . . ? C18 C19 C20 C21 -0.6(4) . . . . ? C19 C20 C21 C22 -0.2(4) . . . . ? C18 N2 C22 C21 0.0(4) . . . . ? Ir1 N2 C22 C21 -179.4(2) . . . . ? C20 C21 C22 N2 0.5(4) . . . . ? Nd1 N6 C23 Ir1 43(12) 2_676 . . . ? C24 Ir1 C23 N6 -38(12) . . . . ? C12 Ir1 C23 N6 136(12) . . . . ? C11 Ir1 C23 N6 -163(12) . . . . ? N1 Ir1 C23 N6 -131(12) . . . . ? N2 Ir1 C23 N6 56(12) . . . . ? Nd1 N3 C24 Ir1 -33(3) . . . . ? C23 Ir1 C24 N3 96(2) . . . . ? C12 Ir1 C24 N3 -10(3) . . . . ? C11 Ir1 C24 N3 -89(2) . . . . ? N1 Ir1 C24 N3 -169(2) . . . . ? N2 Ir1 C24 N3 5(2) . . . . ? C5S C6S N3S Nd1 177(100) . . . . ? O1S Nd1 N3S C6S -174.2(9) . . . . ? O6 Nd1 N3S C6S -17.9(10) . . . . ? O3 Nd1 N3S C6S 106.3(9) . . . . ? O2S Nd1 N3S C6S -33.6(9) . . . . ? N3 Nd1 N3S C6S 35.5(9) . . . . ? N6 Nd1 N3S C6S -97.5(9) 2_676 . . . ? O1 Nd1 N3S C6S 109.1(9) . . . . ? O4 Nd1 N3S C6S -150.3(9) . . . . ? N4 Nd1 N3S C6S 106.9(9) . . . . ? N5 Nd1 N3S C6S -81.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.910 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.094 #===END data_imw1543 _database_code_depnum_ccdc_archive 'CCDC 834577' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H58 Ir2 La2 N18 O16' _chemical_formula_weight 1949.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' O O 0.0106 0.0060 '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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1072(4) _cell_length_b 12.2186(4) _cell_length_c 12.9780(4) _cell_angle_alpha 100.351(2) _cell_angle_beta 95.361(2) _cell_angle_gamma 90.093(2) _cell_volume 1724.75(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9906 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.52 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 5.137 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4583 _exptl_absorpt_correction_T_max 0.6550 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31856 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.60 _reflns_number_total 7840 _reflns_number_gt 6844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. All hydrogen atoms were added in calculated positions apart from the water protons on O31 O41 which were found from the data and then fixed into position. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.4756P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7840 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.445025(10) 0.221437(9) 0.255947(8) 0.01177(4) Uani 1 1 d . . . La1 La 0.250748(15) 0.097407(13) 0.581062(12) 0.01208(4) Uani 1 1 d . . . N111 N 0.5617(2) 0.3350(2) 0.35234(19) 0.0148(5) Uani 1 1 d . . . C112 C 0.5363(3) 0.4441(2) 0.3534(2) 0.0163(6) Uani 1 1 d . . . C113 C 0.6119(3) 0.5267(3) 0.4164(3) 0.0234(7) Uani 1 1 d . . . H113 H 0.5941 0.6028 0.4170 0.028 Uiso 1 1 calc R . . C114 C 0.7110(3) 0.4993(3) 0.4773(3) 0.0260(8) Uani 1 1 d . . . H114 H 0.7620 0.5557 0.5197 0.031 Uiso 1 1 calc R . . C115 C 0.7356(3) 0.3871(3) 0.4756(3) 0.0238(7) Uani 1 1 d . . . H115 H 0.8031 0.3654 0.5175 0.029 Uiso 1 1 calc R . . C116 C 0.6603(3) 0.3086(3) 0.4122(2) 0.0195(7) Uani 1 1 d . . . H116 H 0.6779 0.2322 0.4102 0.023 Uiso 1 1 calc R . . C121 C 0.4281(3) 0.4640(2) 0.2866(2) 0.0171(6) Uani 1 1 d . . . C122 C 0.3679(3) 0.3676(2) 0.2281(2) 0.0148(6) Uani 1 1 d . . . C123 C 0.2644(3) 0.3825(3) 0.1622(2) 0.0204(7) Uani 1 1 d . . . H123 H 0.2231 0.3193 0.1207 0.025 Uiso 1 1 calc R . . C124 C 0.2209(3) 0.4878(3) 0.1564(3) 0.0253(7) Uani 1 1 d . . . H124 H 0.1505 0.4958 0.1110 0.030 Uiso 1 1 calc R . . C125 C 0.2799(3) 0.5816(3) 0.2165(3) 0.0265(8) Uani 1 1 d . . . H125 H 0.2488 0.6534 0.2132 0.032 Uiso 1 1 calc R . . C126 C 0.3835(3) 0.5707(3) 0.2812(3) 0.0225(7) Uani 1 1 d . . . H126 H 0.4243 0.6348 0.3217 0.027 Uiso 1 1 calc R . . N211 N 0.3305(2) 0.12286(19) 0.14334(19) 0.0137(5) Uani 1 1 d . . . C212 C 0.3649(3) 0.1049(2) 0.0430(2) 0.0157(6) Uani 1 1 d . . . C213 C 0.2912(3) 0.0402(2) -0.0385(2) 0.0190(7) Uani 1 1 d . . . H213 H 0.3146 0.0285 -0.1081 0.023 Uiso 1 1 calc R . . C214 C 0.1847(3) -0.0067(3) -0.0187(2) 0.0220(7) Uani 1 1 d . . . H214 H 0.1354 -0.0518 -0.0741 0.026 Uiso 1 1 calc R . . C215 C 0.1504(3) 0.0128(3) 0.0832(2) 0.0199(7) Uani 1 1 d . . . H215 H 0.0771 -0.0182 0.0986 0.024 Uiso 1 1 calc R . . C216 C 0.2248(3) 0.0779(2) 0.1615(2) 0.0167(6) Uani 1 1 d . . . H216 H 0.2010 0.0917 0.2310 0.020 Uiso 1 1 calc R . . C221 C 0.4795(3) 0.1589(2) 0.0325(2) 0.0147(6) Uani 1 1 d . . . C222 C 0.5380(3) 0.2217(2) 0.1258(2) 0.0152(6) Uani 1 1 d . . . C223 C 0.6458(3) 0.2776(3) 0.1178(3) 0.0201(7) Uani 1 1 d . . . H223 H 0.6871 0.3207 0.1791 0.024 Uiso 1 1 calc R . . C224 C 0.6936(3) 0.2712(3) 0.0210(3) 0.0223(7) Uani 1 1 d . . . H224 H 0.7661 0.3110 0.0170 0.027 Uiso 1 1 calc R . . C225 C 0.6356(3) 0.2068(3) -0.0698(3) 0.0243(7) Uani 1 1 d . . . H225 H 0.6691 0.2018 -0.1352 0.029 Uiso 1 1 calc R . . C226 C 0.5293(3) 0.1502(2) -0.0642(2) 0.0188(7) Uani 1 1 d . . . H226 H 0.4900 0.1056 -0.1257 0.023 Uiso 1 1 calc R . . N311 N 0.2762(2) 0.2228(2) 0.44318(19) 0.0176(5) Uani 1 1 d . . . C312 C 0.3364(3) 0.2219(2) 0.3745(2) 0.0150(6) Uani 1 1 d . . . N411 N 0.4013(2) -0.0167(2) 0.6822(2) 0.0182(6) Uani 1 1 d . . . C412 C 0.5386(3) 0.0867(2) 0.2919(2) 0.0149(6) Uani 1 1 d . . . O11 O 0.31535(19) -0.05449(18) 0.43604(17) 0.0214(5) Uani 1 1 d . . . O12 O 0.13427(19) 0.00222(17) 0.40119(16) 0.0187(5) Uani 1 1 d . . . O13 O 0.2058(2) -0.13552(19) 0.29424(17) 0.0290(6) Uani 1 1 d . . . N14 N 0.2165(2) -0.0650(2) 0.3740(2) 0.0188(6) Uani 1 1 d . . . O21 O 0.14015(19) 0.04548(17) 0.73471(16) 0.0182(5) Uani 1 1 d . . . O22 O 0.13047(19) -0.07995(17) 0.59248(16) 0.0183(5) Uani 1 1 d . . . O23 O 0.0519(2) -0.11488(19) 0.73195(18) 0.0254(5) Uani 1 1 d . . . N24 N 0.1052(2) -0.0513(2) 0.6889(2) 0.0174(5) Uani 1 1 d . . . N11S N 0.3023(3) 0.2641(2) 0.7453(2) 0.0239(6) Uani 1 1 d . . . C12S C 0.3454(3) 0.3273(3) 0.8148(3) 0.0208(7) Uani 1 1 d . . . C13S C 0.3999(3) 0.4084(3) 0.9034(3) 0.0234(7) Uani 1 1 d . . . H13A H 0.3619 0.4807 0.9029 0.035 Uiso 1 1 calc R . . H13B H 0.4867 0.4156 0.8974 0.035 Uiso 1 1 calc R . . H13C H 0.3876 0.3834 0.9694 0.035 Uiso 1 1 calc R . . N21S N 0.1041(3) 0.4755(3) 0.8916(3) 0.0430(9) Uani 1 1 d . . . C22S C 0.0699(3) 0.3865(4) 0.8845(3) 0.0394(10) Uani 1 1 d . . . C23S C 0.0255(4) 0.2720(4) 0.8768(4) 0.0570(13) Uani 1 1 d . . . H23A H 0.0938 0.2239 0.8894 0.085 Uiso 1 1 calc R . . H23B H -0.0152 0.2457 0.8064 0.085 Uiso 1 1 calc R . . H23C H -0.0317 0.2697 0.9295 0.085 Uiso 1 1 calc R . . N31S N 0.0181(3) 0.4182(2) 0.6127(2) 0.0332(7) Uani 1 1 d . . . C32S C 0.0133(3) 0.5104(3) 0.6487(3) 0.0266(8) Uani 1 1 d . . . C33S C 0.0074(4) 0.6282(3) 0.6937(3) 0.0361(9) Uani 1 1 d . . . H33A H 0.0453 0.6723 0.6490 0.054 Uiso 1 1 calc R . . H33B H 0.0503 0.6423 0.7644 0.054 Uiso 1 1 calc R . . H33C H -0.0773 0.6492 0.6979 0.054 Uiso 1 1 calc R . . O31 O 0.04836(19) 0.18770(17) 0.56399(16) 0.0179(5) Uani 1 1 d . . . H31B H -0.0131 0.1722 0.5048 0.021 Uiso 1 1 d R . . H31A H 0.0509 0.2689 0.5467 0.021 Uiso 1 1 d R . . O41 O 0.46984(19) 0.16034(18) 0.57337(17) 0.0217(5) Uani 1 1 d . . . H41A H 0.5339 0.1254 0.5928 0.026 Uiso 1 1 d R . . H41B H 0.4950 0.1822 0.5148 0.026 Uiso 1 1 d 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 0.01455(6) 0.00941(6) 0.01171(6) 0.00293(4) 0.00118(4) 0.00155(4) La1 0.01392(9) 0.00963(8) 0.01280(9) 0.00251(6) 0.00087(6) 0.00175(7) N111 0.0156(13) 0.0143(12) 0.0147(13) 0.0031(10) 0.0022(10) 0.0001(10) C112 0.0194(16) 0.0126(14) 0.0184(16) 0.0029(12) 0.0089(12) 0.0000(12) C113 0.0251(18) 0.0160(16) 0.0294(19) 0.0018(13) 0.0082(14) -0.0037(14) C114 0.0221(17) 0.0201(17) 0.032(2) -0.0050(14) 0.0039(15) -0.0072(14) C115 0.0197(17) 0.0241(17) 0.0251(18) -0.0011(14) 0.0004(14) 0.0003(14) C116 0.0210(16) 0.0178(16) 0.0189(16) 0.0014(12) 0.0014(13) 0.0025(13) C121 0.0238(16) 0.0128(14) 0.0170(16) 0.0057(12) 0.0079(13) 0.0029(12) C122 0.0202(15) 0.0164(15) 0.0103(14) 0.0058(11) 0.0072(12) 0.0045(12) C123 0.0262(17) 0.0196(16) 0.0167(16) 0.0064(13) 0.0025(13) 0.0064(13) C124 0.0311(19) 0.0252(18) 0.0236(18) 0.0125(14) 0.0066(14) 0.0104(15) C125 0.034(2) 0.0166(16) 0.034(2) 0.0135(14) 0.0141(16) 0.0105(15) C126 0.0294(18) 0.0123(15) 0.0276(18) 0.0046(13) 0.0103(14) 0.0011(13) N211 0.0156(13) 0.0108(12) 0.0150(13) 0.0036(9) 0.0008(10) 0.0037(10) C212 0.0200(16) 0.0120(14) 0.0165(15) 0.0068(11) 0.0010(12) 0.0077(12) C213 0.0265(17) 0.0166(15) 0.0132(15) 0.0020(12) -0.0008(13) 0.0050(13) C214 0.0244(17) 0.0200(16) 0.0190(17) 0.0005(13) -0.0057(13) 0.0021(14) C215 0.0178(16) 0.0194(16) 0.0221(17) 0.0035(13) -0.0004(13) -0.0001(13) C216 0.0169(15) 0.0169(15) 0.0173(16) 0.0056(12) 0.0015(12) 0.0029(12) C221 0.0180(15) 0.0101(14) 0.0179(16) 0.0072(11) 0.0034(12) 0.0046(12) C222 0.0192(15) 0.0095(14) 0.0181(16) 0.0045(11) 0.0048(12) 0.0059(12) C223 0.0226(17) 0.0166(15) 0.0222(17) 0.0055(13) 0.0036(13) 0.0032(13) C224 0.0238(17) 0.0176(16) 0.0283(18) 0.0067(13) 0.0117(14) 0.0025(13) C225 0.0327(19) 0.0194(17) 0.0236(18) 0.0065(13) 0.0123(15) 0.0074(14) C226 0.0275(17) 0.0128(15) 0.0167(16) 0.0038(12) 0.0027(13) 0.0053(13) N311 0.0241(14) 0.0132(13) 0.0158(14) 0.0034(10) 0.0013(11) -0.0010(11) C312 0.0190(15) 0.0079(13) 0.0178(16) 0.0040(11) -0.0021(12) 0.0015(12) N411 0.0198(14) 0.0144(13) 0.0199(14) 0.0034(10) -0.0005(11) 0.0021(11) C412 0.0172(15) 0.0132(14) 0.0129(15) -0.0017(11) 0.0021(12) -0.0021(12) O11 0.0194(12) 0.0239(12) 0.0197(12) 0.0012(9) 0.0007(9) 0.0069(10) O12 0.0202(12) 0.0161(11) 0.0194(12) 0.0018(9) 0.0028(9) 0.0048(9) O13 0.0401(15) 0.0233(13) 0.0197(13) -0.0078(10) 0.0054(10) -0.0014(11) N14 0.0248(15) 0.0160(13) 0.0162(14) 0.0040(10) 0.0025(11) -0.0003(11) O21 0.0251(12) 0.0119(10) 0.0169(11) 0.0004(8) 0.0023(9) -0.0008(9) O22 0.0229(12) 0.0169(11) 0.0147(11) 0.0015(8) 0.0032(9) -0.0010(9) O23 0.0314(13) 0.0229(12) 0.0245(13) 0.0108(10) 0.0040(10) -0.0073(10) N24 0.0180(13) 0.0177(13) 0.0173(14) 0.0061(10) -0.0004(10) 0.0018(11) N11S 0.0292(16) 0.0182(14) 0.0241(16) 0.0015(12) 0.0063(12) 0.0017(12) C12S 0.0237(17) 0.0162(16) 0.0232(18) 0.0040(13) 0.0056(14) 0.0021(13) C13S 0.0249(17) 0.0168(16) 0.0244(18) -0.0070(13) 0.0020(14) -0.0022(14) N21S 0.035(2) 0.050(2) 0.039(2) -0.0007(17) -0.0043(15) 0.0060(18) C22S 0.024(2) 0.059(3) 0.029(2) -0.0070(19) -0.0016(16) 0.012(2) C23S 0.036(2) 0.053(3) 0.075(4) -0.011(2) 0.012(2) 0.002(2) N31S 0.0301(17) 0.0235(16) 0.042(2) 0.0001(14) -0.0055(14) 0.0017(13) C32S 0.0234(18) 0.0238(19) 0.032(2) 0.0034(15) 0.0005(15) 0.0025(15) C33S 0.047(2) 0.0159(17) 0.044(2) -0.0003(15) 0.0107(19) 0.0012(17) O31 0.0182(11) 0.0160(11) 0.0198(12) 0.0050(9) -0.0003(9) 0.0026(9) O41 0.0157(11) 0.0220(12) 0.0300(13) 0.0105(10) 0.0035(9) 0.0017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C312 2.041(3) . ? Ir1 C412 2.049(3) . ? Ir1 N211 2.054(2) . ? Ir1 C122 2.057(3) . ? Ir1 N111 2.059(2) . ? Ir1 C222 2.060(3) . ? La1 O31 2.514(2) . ? La1 O11 2.550(2) . ? La1 O41 2.567(2) . ? La1 O22 2.578(2) . ? La1 N311 2.590(2) . ? La1 N411 2.592(3) . ? La1 O21 2.607(2) . ? La1 O12 2.633(2) . ? La1 N11S 2.689(3) . ? N111 C116 1.356(4) . ? N111 C112 1.362(4) . ? C112 C113 1.401(4) . ? C112 C121 1.461(4) . ? C113 C114 1.372(5) . ? C113 H113 0.9500 . ? C114 C115 1.396(5) . ? C114 H114 0.9500 . ? C115 C116 1.372(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.407(4) . ? C121 C122 1.412(4) . ? C122 C123 1.399(4) . ? C123 C124 1.387(4) . ? C123 H123 0.9500 . ? C124 C125 1.390(5) . ? C124 H124 0.9500 . ? C125 C126 1.381(5) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? N211 C216 1.353(4) . ? N211 C212 1.371(4) . ? C212 C213 1.397(4) . ? C212 C221 1.462(4) . ? C213 C214 1.379(4) . ? C213 H213 0.9500 . ? C214 C215 1.391(4) . ? C214 H214 0.9500 . ? C215 C216 1.378(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.405(4) . ? C221 C222 1.413(4) . ? C222 C223 1.399(4) . ? C223 C224 1.398(4) . ? C223 H223 0.9500 . ? C224 C225 1.395(5) . ? C224 H224 0.9500 . ? C225 C226 1.381(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? N311 C312 1.162(4) . ? N411 C412 1.164(4) 2_656 ? C412 N411 1.164(4) 2_656 ? O11 N14 1.291(3) . ? O12 N14 1.261(3) . ? O13 N14 1.219(3) . ? O21 N24 1.268(3) . ? O22 N24 1.294(3) . ? O23 N24 1.217(3) . ? N11S C12S 1.143(4) . ? C12S C13S 1.459(4) . ? C13S H13A 0.9800 . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? N21S C22S 1.136(5) . ? C22S C23S 1.466(6) . ? C23S H23A 0.9800 . ? C23S H23B 0.9800 . ? C23S H23C 0.9800 . ? N31S C32S 1.143(4) . ? C32S C33S 1.457(5) . ? C33S H33A 0.9800 . ? C33S H33B 0.9800 . ? C33S H33C 0.9800 . ? O31 H31B 0.9706 . ? O31 H31A 1.0567 . ? O41 H41A 0.8706 . ? O41 H41B 0.9162 . ? 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 C312 Ir1 C412 92.62(11) . . ? C312 Ir1 N211 95.07(10) . . ? C412 Ir1 N211 92.14(10) . . ? C312 Ir1 C122 88.89(11) . . ? C412 Ir1 C122 173.46(11) . . ? N211 Ir1 C122 94.07(11) . . ? C312 Ir1 N111 90.80(10) . . ? C412 Ir1 N111 93.75(11) . . ? N211 Ir1 N111 171.49(9) . . ? C122 Ir1 N111 79.86(11) . . ? C312 Ir1 C222 173.87(12) . . ? C412 Ir1 C222 91.33(11) . . ? N211 Ir1 C222 80.10(11) . . ? C122 Ir1 C222 87.71(11) . . ? N111 Ir1 C222 93.61(11) . . ? O31 La1 O11 121.32(7) . . ? O31 La1 O41 134.47(7) . . ? O11 La1 O41 79.66(7) . . ? O31 La1 O22 85.91(7) . . ? O11 La1 O22 73.61(7) . . ? O41 La1 O22 139.44(7) . . ? O31 La1 N311 76.66(7) . . ? O11 La1 N311 82.89(7) . . ? O41 La1 N311 65.84(8) . . ? O22 La1 N311 137.50(7) . . ? O31 La1 N411 149.27(7) . . ? O11 La1 N411 76.91(7) . . ? O41 La1 N411 69.03(7) . . ? O22 La1 N411 75.50(7) . . ? N311 La1 N411 133.03(8) . . ? O31 La1 O21 75.94(7) . . ? O11 La1 O21 120.35(7) . . ? O41 La1 O21 131.38(7) . . ? O22 La1 O21 49.50(6) . . ? N311 La1 O21 150.81(7) . . ? N411 La1 O21 73.37(7) . . ? O31 La1 O12 72.06(7) . . ? O11 La1 O12 49.29(7) . . ? O41 La1 O12 116.19(7) . . ? O22 La1 O12 66.15(6) . . ? N311 La1 O12 71.63(7) . . ? N411 La1 O12 119.81(7) . . ? O21 La1 O12 108.76(7) . . ? O31 La1 N11S 84.81(8) . . ? O11 La1 N11S 151.48(8) . . ? O41 La1 N11S 73.14(8) . . ? O22 La1 N11S 123.48(7) . . ? N311 La1 N11S 93.51(8) . . ? N411 La1 N11S 85.38(8) . . ? O21 La1 N11S 74.19(7) . . ? O12 La1 N11S 154.68(8) . . ? C116 N111 C112 119.1(3) . . ? C116 N111 Ir1 124.9(2) . . ? C112 N111 Ir1 116.0(2) . . ? N111 C112 C113 119.5(3) . . ? N111 C112 C121 115.0(3) . . ? C113 C112 C121 125.5(3) . . ? C114 C113 C112 121.1(3) . . ? C114 C113 H113 119.5 . . ? C112 C113 H113 119.5 . . ? C113 C114 C115 118.7(3) . . ? C113 C114 H114 120.6 . . ? C115 C114 H114 120.6 . . ? C116 C115 C114 118.6(3) . . ? C116 C115 H115 120.7 . . ? C114 C115 H115 120.7 . . ? N111 C116 C115 123.0(3) . . ? N111 C116 H116 118.5 . . ? C115 C116 H116 118.5 . . ? C126 C121 C122 121.1(3) . . ? C126 C121 C112 123.5(3) . . ? C122 C121 C112 115.4(3) . . ? C123 C122 C121 117.4(3) . . ? C123 C122 Ir1 128.8(2) . . ? C121 C122 Ir1 113.8(2) . . ? C124 C123 C122 121.4(3) . . ? C124 C123 H123 119.3 . . ? C122 C123 H123 119.3 . . ? C123 C124 C125 120.3(3) . . ? C123 C124 H124 119.9 . . ? C125 C124 H124 119.9 . . ? C126 C125 C124 120.2(3) . . ? C126 C125 H125 119.9 . . ? C124 C125 H125 119.9 . . ? C125 C126 C121 119.6(3) . . ? C125 C126 H126 120.2 . . ? C121 C126 H126 120.2 . . ? C216 N211 C212 119.2(2) . . ? C216 N211 Ir1 124.67(19) . . ? C212 N211 Ir1 116.09(19) . . ? N211 C212 C213 119.7(3) . . ? N211 C212 C221 114.4(3) . . ? C213 C212 C221 125.8(3) . . ? C214 C213 C212 120.5(3) . . ? C214 C213 H213 119.7 . . ? C212 C213 H213 119.7 . . ? C213 C214 C215 119.2(3) . . ? C213 C214 H214 120.4 . . ? C215 C214 H214 120.4 . . ? C216 C215 C214 118.7(3) . . ? C216 C215 H215 120.7 . . ? C214 C215 H215 120.7 . . ? N211 C216 C215 122.6(3) . . ? N211 C216 H216 118.7 . . ? C215 C216 H216 118.7 . . ? C226 C221 C222 121.4(3) . . ? C226 C221 C212 122.7(3) . . ? C222 C221 C212 116.0(3) . . ? C223 C222 C221 117.4(3) . . ? C223 C222 Ir1 129.2(2) . . ? C221 C222 Ir1 113.4(2) . . ? C224 C223 C222 121.2(3) . . ? C224 C223 H223 119.4 . . ? C222 C223 H223 119.4 . . ? C225 C224 C223 120.4(3) . . ? C225 C224 H224 119.8 . . ? C223 C224 H224 119.8 . . ? C226 C225 C224 119.7(3) . . ? C226 C225 H225 120.1 . . ? C224 C225 H225 120.1 . . ? C225 C226 C221 119.9(3) . . ? C225 C226 H226 120.0 . . ? C221 C226 H226 120.0 . . ? C312 N311 La1 135.4(2) . . ? N311 C312 Ir1 178.9(3) . . ? C412 N411 La1 164.5(2) 2_656 . ? N411 C412 Ir1 174.1(3) 2_656 . ? N14 O11 La1 98.92(16) . . ? N14 O12 La1 95.79(16) . . ? O13 N14 O12 123.3(3) . . ? O13 N14 O11 120.9(3) . . ? O12 N14 O11 115.8(2) . . ? N24 O21 La1 96.94(16) . . ? N24 O22 La1 97.59(15) . . ? O23 N24 O21 122.9(3) . . ? O23 N24 O22 121.3(3) . . ? O21 N24 O22 115.9(2) . . ? C12S N11S La1 167.3(3) . . ? N11S C12S C13S 179.7(4) . . ? C12S C13S H13A 109.5 . . ? C12S C13S H13B 109.5 . . ? H13A C13S H13B 109.5 . . ? C12S C13S H13C 109.5 . . ? H13A C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? N21S C22S C23S 179.2(5) . . ? C22S C23S H23A 109.5 . . ? C22S C23S H23B 109.5 . . ? H23A C23S H23B 109.5 . . ? C22S C23S H23C 109.5 . . ? H23A C23S H23C 109.5 . . ? H23B C23S H23C 109.5 . . ? N31S C32S C33S 179.4(4) . . ? C32S C33S H33A 109.5 . . ? C32S C33S H33B 109.5 . . ? H33A C33S H33B 109.5 . . ? C32S C33S H33C 109.5 . . ? H33A C33S H33C 109.5 . . ? H33B C33S H33C 109.5 . . ? La1 O31 H31B 126.9 . . ? La1 O31 H31A 115.0 . . ? H31B O31 H31A 85.3 . . ? La1 O41 H41A 125.1 . . ? La1 O41 H41B 122.0 . . ? H41A O41 H41B 99.7 . . ? 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 C312 Ir1 N111 C116 92.2(2) . . . . ? C412 Ir1 N111 C116 -0.5(3) . . . . ? N211 Ir1 N111 C116 -134.1(6) . . . . ? C122 Ir1 N111 C116 -179.1(3) . . . . ? C222 Ir1 N111 C116 -92.1(2) . . . . ? C312 Ir1 N111 C112 -88.6(2) . . . . ? C412 Ir1 N111 C112 178.8(2) . . . . ? N211 Ir1 N111 C112 45.1(7) . . . . ? C122 Ir1 N111 C112 0.2(2) . . . . ? C222 Ir1 N111 C112 87.2(2) . . . . ? C116 N111 C112 C113 -0.3(4) . . . . ? Ir1 N111 C112 C113 -179.6(2) . . . . ? C116 N111 C112 C121 -179.8(3) . . . . ? Ir1 N111 C112 C121 0.9(3) . . . . ? N111 C112 C113 C114 -0.1(5) . . . . ? C121 C112 C113 C114 179.3(3) . . . . ? C112 C113 C114 C115 -0.2(5) . . . . ? C113 C114 C115 C116 0.7(5) . . . . ? C112 N111 C116 C115 0.9(4) . . . . ? Ir1 N111 C116 C115 -179.9(2) . . . . ? C114 C115 C116 N111 -1.1(5) . . . . ? N111 C112 C121 C126 176.6(3) . . . . ? C113 C112 C121 C126 -2.8(5) . . . . ? N111 C112 C121 C122 -2.1(4) . . . . ? C113 C112 C121 C122 178.5(3) . . . . ? C126 C121 C122 C123 1.9(4) . . . . ? C112 C121 C122 C123 -179.4(3) . . . . ? C126 C121 C122 Ir1 -176.6(2) . . . . ? C112 C121 C122 Ir1 2.2(3) . . . . ? C312 Ir1 C122 C123 -88.5(3) . . . . ? C412 Ir1 C122 C123 168.1(8) . . . . ? N211 Ir1 C122 C123 6.5(3) . . . . ? N111 Ir1 C122 C123 -179.5(3) . . . . ? C222 Ir1 C122 C123 86.4(3) . . . . ? C312 Ir1 C122 C121 89.7(2) . . . . ? C412 Ir1 C122 C121 -13.7(10) . . . . ? N211 Ir1 C122 C121 -175.3(2) . . . . ? N111 Ir1 C122 C121 -1.3(2) . . . . ? C222 Ir1 C122 C121 -95.4(2) . . . . ? C121 C122 C123 C124 -1.4(4) . . . . ? Ir1 C122 C123 C124 176.8(2) . . . . ? C122 C123 C124 C125 -0.1(5) . . . . ? C123 C124 C125 C126 1.2(5) . . . . ? C124 C125 C126 C121 -0.7(5) . . . . ? C122 C121 C126 C125 -0.8(5) . . . . ? C112 C121 C126 C125 -179.5(3) . . . . ? C312 Ir1 N211 C216 -2.7(2) . . . . ? C412 Ir1 N211 C216 90.1(2) . . . . ? C122 Ir1 N211 C216 -92.0(2) . . . . ? N111 Ir1 N211 C216 -136.2(6) . . . . ? C222 Ir1 N211 C216 -178.9(3) . . . . ? C312 Ir1 N211 C212 175.8(2) . . . . ? C412 Ir1 N211 C212 -91.3(2) . . . . ? C122 Ir1 N211 C212 86.6(2) . . . . ? N111 Ir1 N211 C212 42.4(7) . . . . ? C222 Ir1 N211 C212 -0.4(2) . . . . ? C216 N211 C212 C213 -0.4(4) . . . . ? Ir1 N211 C212 C213 -179.0(2) . . . . ? C216 N211 C212 C221 179.1(3) . . . . ? Ir1 N211 C212 C221 0.5(3) . . . . ? N211 C212 C213 C214 -0.7(4) . . . . ? C221 C212 C213 C214 179.9(3) . . . . ? C212 C213 C214 C215 1.1(5) . . . . ? C213 C214 C215 C216 -0.5(5) . . . . ? C212 N211 C216 C215 1.0(4) . . . . ? Ir1 N211 C216 C215 179.5(2) . . . . ? C214 C215 C216 N211 -0.6(5) . . . . ? N211 C212 C221 C226 -179.8(3) . . . . ? C213 C212 C221 C226 -0.4(5) . . . . ? N211 C212 C221 C222 -0.3(4) . . . . ? C213 C212 C221 C222 179.2(3) . . . . ? C226 C221 C222 C223 1.8(4) . . . . ? C212 C221 C222 C223 -177.8(3) . . . . ? C226 C221 C222 Ir1 179.5(2) . . . . ? C212 C221 C222 Ir1 0.0(3) . . . . ? C312 Ir1 C222 C223 139.4(9) . . . . ? C412 Ir1 C222 C223 -90.4(3) . . . . ? N211 Ir1 C222 C223 177.6(3) . . . . ? C122 Ir1 C222 C223 83.1(3) . . . . ? N111 Ir1 C222 C223 3.4(3) . . . . ? C312 Ir1 C222 C221 -38.0(11) . . . . ? C412 Ir1 C222 C221 92.1(2) . . . . ? N211 Ir1 C222 C221 0.2(2) . . . . ? C122 Ir1 C222 C221 -94.3(2) . . . . ? N111 Ir1 C222 C221 -174.0(2) . . . . ? C221 C222 C223 C224 -0.1(4) . . . . ? Ir1 C222 C223 C224 -177.5(2) . . . . ? C222 C223 C224 C225 -1.2(5) . . . . ? C223 C224 C225 C226 0.9(5) . . . . ? C224 C225 C226 C221 0.7(5) . . . . ? C222 C221 C226 C225 -2.1(4) . . . . ? C212 C221 C226 C225 177.5(3) . . . . ? O31 La1 N311 C312 -154.2(3) . . . . ? O11 La1 N311 C312 -29.6(3) . . . . ? O41 La1 N311 C312 52.2(3) . . . . ? O22 La1 N311 C312 -85.8(3) . . . . ? N411 La1 N311 C312 35.0(4) . . . . ? O21 La1 N311 C312 -174.8(3) . . . . ? O12 La1 N311 C312 -79.0(3) . . . . ? N11S La1 N311 C312 122.0(3) . . . . ? La1 N311 C312 Ir1 -73(13) . . . . ? C412 Ir1 C312 N311 68(13) . . . . ? N211 Ir1 C312 N311 161(13) . . . . ? C122 Ir1 C312 N311 -105(13) . . . . ? N111 Ir1 C312 N311 -25(13) . . . . ? C222 Ir1 C312 N311 -161(12) . . . . ? O31 La1 N411 C412 106.9(9) . . . 2_656 ? O11 La1 N411 C412 -23.9(9) . . . 2_656 ? O41 La1 N411 C412 -107.7(9) . . . 2_656 ? O22 La1 N411 C412 52.3(9) . . . 2_656 ? N311 La1 N411 C412 -90.9(9) . . . 2_656 ? O21 La1 N411 C412 103.8(9) . . . 2_656 ? O12 La1 N411 C412 1.3(9) . . . 2_656 ? N11S La1 N411 C412 178.6(9) . . . 2_656 ? C312 Ir1 C412 N411 -92(3) . . . 2_656 ? N211 Ir1 C412 N411 173(3) . . . 2_656 ? C122 Ir1 C412 N411 11(3) . . . 2_656 ? N111 Ir1 C412 N411 -1(3) . . . 2_656 ? C222 Ir1 C412 N411 92(3) . . . 2_656 ? O31 La1 O11 N14 -4.59(19) . . . . ? O41 La1 O11 N14 -140.85(17) . . . . ? O22 La1 O11 N14 69.99(16) . . . . ? N311 La1 O11 N14 -74.22(17) . . . . ? N411 La1 O11 N14 148.48(17) . . . . ? O21 La1 O11 N14 86.94(17) . . . . ? O12 La1 O11 N14 -2.37(14) . . . . ? N11S La1 O11 N14 -158.46(17) . . . . ? O31 La1 O12 N14 -179.58(17) . . . . ? O11 La1 O12 N14 2.41(15) . . . . ? O41 La1 O12 N14 49.02(17) . . . . ? O22 La1 O12 N14 -86.07(16) . . . . ? N311 La1 O12 N14 98.93(17) . . . . ? N411 La1 O12 N14 -30.74(18) . . . . ? O21 La1 O12 N14 -111.90(16) . . . . ? N11S La1 O12 N14 155.50(18) . . . . ? La1 O12 N14 O13 176.5(2) . . . . ? La1 O12 N14 O11 -4.0(2) . . . . ? La1 O11 N14 O13 -176.3(2) . . . . ? La1 O11 N14 O12 4.2(3) . . . . ? O31 La1 O21 N24 98.61(17) . . . . ? O11 La1 O21 N24 -19.70(19) . . . . ? O41 La1 O21 N24 -123.51(16) . . . . ? O22 La1 O21 N24 1.88(15) . . . . ? N311 La1 O21 N24 119.22(19) . . . . ? N411 La1 O21 N24 -83.04(17) . . . . ? O12 La1 O21 N24 33.48(17) . . . . ? N11S La1 O21 N24 -172.88(18) . . . . ? O31 La1 O22 N24 -76.81(16) . . . . ? O11 La1 O22 N24 158.84(17) . . . . ? O41 La1 O22 N24 107.97(17) . . . . ? N311 La1 O22 N24 -141.95(16) . . . . ? N411 La1 O22 N24 78.50(16) . . . . ? O21 La1 O22 N24 -1.84(15) . . . . ? O12 La1 O22 N24 -148.99(18) . . . . ? N11S La1 O22 N24 4.21(19) . . . . ? La1 O21 N24 O23 176.3(2) . . . . ? La1 O21 N24 O22 -3.2(2) . . . . ? La1 O22 N24 O23 -176.2(2) . . . . ? La1 O22 N24 O21 3.2(3) . . . . ? O31 La1 N11S C12S -172.1(12) . . . . ? O11 La1 N11S C12S -14.3(12) . . . . ? O41 La1 N11S C12S -32.4(11) . . . . ? O22 La1 N11S C12S 106.3(11) . . . . ? N311 La1 N11S C12S -95.8(12) . . . . ? N411 La1 N11S C12S 37.1(12) . . . . ? O21 La1 N11S C12S 111.1(12) . . . . ? O12 La1 N11S C12S -148.3(11) . . . . ? La1 N11S C12S C13S 147(100) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.160 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.112 #===END data_imw1428_0m _database_code_depnum_ccdc_archive 'CCDC 834578' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Ir N9 O8 Pr' _chemical_formula_weight 976.73 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0880(5) _cell_length_b 12.1795(5) _cell_length_c 12.9537(6) _cell_angle_alpha 100.430(2) _cell_angle_beta 95.504(2) _cell_angle_gamma 90.287(2) _cell_volume 1712.06(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9238 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.58 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 5.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3996 _exptl_absorpt_correction_T_max 0.5906 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35933 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.60 _reflns_number_total 7809 _reflns_number_gt 7022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+2.2170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7809 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.554740(13) 0.779589(12) 0.743032(12) 0.01143(6) Uani 1 1 d . . . Pr1 Pr 0.251667(19) 1.095341(17) 0.580802(17) 0.01178(7) Uani 1 1 d . . . O1 O 0.1432(3) 1.0466(2) 0.7336(3) 0.0188(6) Uani 1 1 d . . . O2 O 0.0521(3) 0.8867(3) 0.7304(3) 0.0235(7) Uani 1 1 d . . . O3 O 0.1298(3) 0.9210(2) 0.5908(2) 0.0177(6) Uani 1 1 d . . . O4 O 0.1348(3) 1.0013(2) 0.4025(3) 0.0179(6) Uani 1 1 d . . . O5 O 0.2078(3) 0.8643(3) 0.2952(3) 0.0286(8) Uani 1 1 d . . . O6 O 0.3170(3) 0.9466(3) 0.4379(3) 0.0211(7) Uani 1 1 d . . . N1 N 0.6695(3) 0.8791(3) 0.8562(3) 0.0140(7) Uani 1 1 d . . . N2 N 0.4387(3) 0.6652(3) 0.6466(3) 0.0146(7) Uani 1 1 d . . . N3 N 0.3983(3) 0.9825(3) 0.6810(3) 0.0185(8) Uani 1 1 d . . . N4 N 0.1061(3) 0.9501(3) 0.6875(3) 0.0165(7) Uani 1 1 d . . . N5 N 0.2183(3) 0.9354(3) 0.3757(3) 0.0178(8) Uani 1 1 d . . . N6 N 0.7224(3) 0.7813(3) 0.5551(3) 0.0174(8) Uani 1 1 d . . . C1 C 0.7756(4) 0.9246(3) 0.8376(4) 0.0172(9) Uani 1 1 d . . . H2 H 0.7988 0.9114 0.7678 0.021 Uiso 1 1 calc R . . H3 H 0.9236 1.0146 0.9021 0.021 Uiso 1 1 d R . . C2 C 0.8504(4) 0.9892(4) 0.9164(4) 0.0211(10) Uani 1 1 d . . . C3 C 0.8170(4) 1.0089(4) 1.0188(4) 0.0225(10) Uani 1 1 d . . . H4 H 0.8670 1.0539 1.0744 0.027 Uiso 1 1 calc R . . C4 C 0.7093(4) 0.9615(4) 1.0382(4) 0.0206(9) Uani 1 1 d . . . H5 H 0.6857 0.9732 1.1079 0.025 Uiso 1 1 calc R . . C5 C 0.6358(4) 0.8971(3) 0.9565(4) 0.0162(9) Uani 1 1 d . . . C6 C 0.5207(4) 0.8419(3) 0.9676(3) 0.0150(8) Uani 1 1 d . . . C7 C 0.4712(4) 0.8498(4) 1.0640(4) 0.0204(9) Uani 1 1 d . . . H8 H 0.5108 0.8946 1.1257 0.024 Uiso 1 1 calc R . . C8 C 0.3650(4) 0.7925(4) 1.0696(4) 0.0223(10) Uani 1 1 d . . . H9 H 0.3317 0.7969 1.1351 0.027 Uiso 1 1 calc R . . C9 C 0.3071(4) 0.7279(4) 0.9782(4) 0.0224(10) Uani 1 1 d . . . H10 H 0.2345 0.6877 0.9818 0.027 Uiso 1 1 calc R . . C10 C 0.3543(4) 0.7219(4) 0.8819(4) 0.0181(9) Uani 1 1 d . . . H11 H 0.3128 0.6782 0.8205 0.022 Uiso 1 1 calc R . . C11 C 0.4621(4) 0.7791(3) 0.8735(3) 0.0142(8) Uani 1 1 d . . . C12 C 0.6328(4) 0.6342(3) 0.7713(3) 0.0149(8) Uani 1 1 d . . . C13 C 0.7364(4) 0.6202(4) 0.8380(4) 0.0205(9) Uani 1 1 d . . . H13 H 0.7772 0.6841 0.8802 0.025 Uiso 1 1 calc R . . C14 C 0.7811(5) 0.5137(4) 0.8438(4) 0.0273(11) Uani 1 1 d . . . H14 H 0.8522 0.5062 0.8888 0.033 Uiso 1 1 calc R . . C15 C 0.7219(5) 0.4199(4) 0.7844(4) 0.0260(11) Uani 1 1 d . . . H15 H 0.7532 0.3480 0.7880 0.031 Uiso 1 1 calc R . . C16 C 0.6167(4) 0.4299(4) 0.7192(4) 0.0230(10) Uani 1 1 d . . . H16 H 0.5755 0.3652 0.6789 0.028 Uiso 1 1 calc R . . C17 C 0.5721(4) 0.5368(3) 0.7137(4) 0.0178(9) Uani 1 1 d . . . C18 C 0.4636(4) 0.5548(4) 0.6456(4) 0.0175(9) Uani 1 1 d . . . C19 C 0.3874(4) 0.4719(4) 0.5841(4) 0.0230(10) Uani 1 1 d . . . H19 H 0.4039 0.3957 0.5854 0.028 Uiso 1 1 calc R . . C20 C 0.2887(4) 0.4986(4) 0.5215(4) 0.0263(11) Uani 1 1 d . . . H20 H 0.2380 0.4416 0.4785 0.032 Uiso 1 1 calc R . . C21 C 0.2646(4) 0.6105(4) 0.5222(4) 0.0231(10) Uani 1 1 d . . . H21 H 0.1969 0.6313 0.4798 0.028 Uiso 1 1 calc R . . C22 C 0.3403(4) 0.6910(4) 0.5854(4) 0.0198(9) Uani 1 1 d . . . H22 H 0.3229 0.7674 0.5861 0.024 Uiso 1 1 calc R . . C23 C 0.6628(4) 0.7806(3) 0.6245(4) 0.0154(8) Uani 1 1 d . . . C24 C 0.4590(4) 0.9136(3) 0.7065(3) 0.0144(8) Uani 1 1 d . . . C1S C 0.0152(4) 0.5091(4) 0.6474(4) 0.0261(11) Uani 1 1 d . . . C2S C 0.0090(6) 0.6266(4) 0.6926(5) 0.0357(13) Uani 1 1 d . . . H2S1 H 0.0442 0.6394 0.7662 0.054 Uiso 1 1 calc R . . H2S2 H -0.0758 0.6490 0.6895 0.054 Uiso 1 1 calc R . . H2S3 H 0.0544 0.6707 0.6525 0.054 Uiso 1 1 calc R . . C3S C 0.0252(6) 0.2704(6) 0.8759(7) 0.0554(19) Uani 1 1 d . . . H3S1 H 0.0929 0.2238 0.8942 0.083 Uiso 1 1 calc R . . H3S2 H -0.0099 0.2416 0.8036 0.083 Uiso 1 1 calc R . . H3S3 H -0.0368 0.2688 0.9247 0.083 Uiso 1 1 calc R . . C4S C 0.0691(5) 0.3852(6) 0.8835(5) 0.0366(14) Uani 1 1 d . . . C5S C 0.3978(5) 1.4074(4) 0.9022(4) 0.0258(10) Uani 1 1 d . . . C6S C 0.3427(4) 1.3254(4) 0.8115(4) 0.0215(10) Uani 1 1 d . . . N1S N 0.0206(4) 0.4167(4) 0.6126(4) 0.0321(10) Uani 1 1 d . . . N2S N 0.1038(5) 0.4750(5) 0.8914(4) 0.0433(13) Uani 1 1 d . . . N3S N 0.3004(4) 1.2610(3) 0.7416(3) 0.0231(8) Uani 1 1 d . . . O1S O 0.0533(3) 1.1851(2) 0.5650(3) 0.0175(6) Uani 1 1 d . . . O2S O 0.4688(3) 1.1587(3) 0.5757(3) 0.0230(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01322(9) 0.01215(9) 0.00950(10) 0.00397(6) 0.00023(6) 0.00066(6) Pr1 0.01257(12) 0.01253(11) 0.01060(13) 0.00366(9) -0.00006(9) 0.00105(8) O1 0.0223(16) 0.0170(15) 0.0166(17) 0.0035(12) -0.0003(13) -0.0026(12) O2 0.0303(18) 0.0225(16) 0.0196(18) 0.0087(13) 0.0029(14) -0.0059(13) O3 0.0203(15) 0.0207(15) 0.0126(16) 0.0035(12) 0.0037(12) -0.0027(12) O4 0.0175(15) 0.0193(15) 0.0173(17) 0.0045(12) 0.0007(13) 0.0012(12) O5 0.040(2) 0.0249(17) 0.0166(18) -0.0064(14) 0.0031(15) 0.0000(15) O6 0.0191(16) 0.0251(16) 0.0181(17) 0.0025(13) -0.0003(13) 0.0048(12) N1 0.0153(17) 0.0158(16) 0.0119(18) 0.0066(14) -0.0005(14) 0.0022(13) N2 0.0156(17) 0.0174(17) 0.0128(19) 0.0073(14) 0.0037(14) -0.0009(13) N3 0.0212(19) 0.0164(17) 0.018(2) 0.0046(15) -0.0025(16) 0.0013(14) N4 0.0151(18) 0.0206(18) 0.0141(19) 0.0064(15) -0.0025(14) 0.0018(14) N5 0.0214(19) 0.0191(18) 0.0134(19) 0.0043(15) 0.0022(15) -0.0005(14) N6 0.0181(18) 0.0185(17) 0.017(2) 0.0071(15) 0.0029(15) -0.0006(14) C1 0.018(2) 0.018(2) 0.017(2) 0.0070(17) 0.0023(17) 0.0025(16) C2 0.018(2) 0.023(2) 0.024(3) 0.0083(19) -0.0015(19) -0.0017(17) C3 0.025(2) 0.024(2) 0.017(2) 0.0026(18) -0.0034(19) 0.0017(18) C4 0.026(2) 0.023(2) 0.012(2) 0.0031(17) -0.0008(18) 0.0052(18) C5 0.022(2) 0.0141(19) 0.013(2) 0.0037(16) 0.0019(17) 0.0060(16) C6 0.019(2) 0.0150(19) 0.012(2) 0.0043(16) 0.0010(17) 0.0041(15) C7 0.030(2) 0.019(2) 0.012(2) 0.0043(17) 0.0012(19) 0.0073(18) C8 0.029(3) 0.022(2) 0.019(2) 0.0083(18) 0.010(2) 0.0031(18) C9 0.024(2) 0.020(2) 0.026(3) 0.0068(19) 0.013(2) 0.0019(17) C10 0.020(2) 0.017(2) 0.018(2) 0.0026(17) 0.0022(18) 0.0008(16) C11 0.018(2) 0.0128(18) 0.013(2) 0.0045(16) 0.0040(17) 0.0054(15) C12 0.017(2) 0.0185(19) 0.012(2) 0.0080(16) 0.0084(17) 0.0058(16) C13 0.023(2) 0.024(2) 0.016(2) 0.0081(18) 0.0020(18) 0.0059(18) C14 0.030(3) 0.030(3) 0.026(3) 0.015(2) 0.005(2) 0.013(2) C15 0.033(3) 0.021(2) 0.030(3) 0.014(2) 0.011(2) 0.0131(19) C16 0.027(2) 0.016(2) 0.029(3) 0.0076(19) 0.011(2) 0.0002(17) C17 0.021(2) 0.017(2) 0.018(2) 0.0078(17) 0.0075(18) 0.0017(16) C18 0.021(2) 0.018(2) 0.015(2) 0.0047(17) 0.0071(18) 0.0021(16) C19 0.027(2) 0.017(2) 0.024(3) 0.0005(18) 0.007(2) -0.0037(17) C20 0.024(2) 0.023(2) 0.027(3) -0.005(2) 0.001(2) -0.0070(18) C21 0.020(2) 0.026(2) 0.021(3) 0.0011(19) -0.0043(19) -0.0009(18) C22 0.018(2) 0.020(2) 0.019(2) -0.0001(17) -0.0014(18) 0.0008(16) C23 0.017(2) 0.0122(18) 0.017(2) 0.0050(16) -0.0020(17) 0.0006(15) C24 0.015(2) 0.0165(19) 0.011(2) 0.0021(16) 0.0016(16) -0.0037(15) C1S 0.024(2) 0.024(2) 0.029(3) 0.004(2) 0.000(2) 0.0000(18) C2S 0.047(3) 0.018(2) 0.041(3) 0.000(2) 0.011(3) -0.002(2) C3S 0.038(4) 0.050(4) 0.072(5) -0.008(3) 0.007(3) 0.000(3) C4S 0.019(3) 0.057(4) 0.028(3) -0.005(3) -0.001(2) 0.007(2) C5S 0.029(3) 0.025(2) 0.019(3) -0.0043(19) -0.005(2) -0.0021(19) C6S 0.021(2) 0.020(2) 0.025(3) 0.0061(19) 0.007(2) 0.0025(17) N1S 0.029(2) 0.026(2) 0.038(3) 0.0043(19) -0.007(2) 0.0027(17) N2S 0.036(3) 0.053(3) 0.037(3) 0.001(2) -0.004(2) 0.006(2) N3S 0.026(2) 0.0211(19) 0.022(2) 0.0015(17) 0.0039(17) -0.0003(15) O1S 0.0158(15) 0.0188(14) 0.0183(17) 0.0046(12) 0.0014(12) 0.0008(11) O2S 0.0142(15) 0.0271(17) 0.029(2) 0.0098(14) 0.0012(14) 0.0000(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 C23 2.037(5) . ? Ir1 N2 2.050(4) . ? Ir1 C12 2.051(4) . ? Ir1 C24 2.053(4) . ? Ir1 N1 2.054(4) . ? Ir1 C11 2.061(4) . ? Pr1 O1S 2.468(3) . ? Pr1 O6 2.508(3) . ? Pr1 O2S 2.535(3) . ? Pr1 O3 2.541(3) . ? Pr1 N3 2.545(4) . ? Pr1 N6 2.547(4) 2_676 ? Pr1 O1 2.567(3) . ? Pr1 O4 2.604(3) . ? Pr1 N3S 2.638(4) . ? Pr1 N5 2.987(4) . ? Pr1 N4 2.988(4) . ? O1 N4 1.266(5) . ? O2 N4 1.216(5) . ? O3 N4 1.290(5) . ? O4 N5 1.261(5) . ? O5 N5 1.224(5) . ? O6 N5 1.287(5) . ? N1 C1 1.357(6) . ? N1 C5 1.367(6) . ? N2 C22 1.359(6) . ? N2 C18 1.371(5) . ? N3 C24 1.153(6) . ? N6 C23 1.168(6) . ? N6 Pr1 2.547(4) 2_676 ? C1 C2 1.374(6) . ? C1 H2 0.9500 . ? C2 C3 1.391(7) . ? C2 H3 0.9137 . ? C3 C4 1.388(7) . ? C3 H4 0.9500 . ? C4 C5 1.388(6) . ? C4 H5 0.9500 . ? C5 C6 1.471(6) . ? C6 C7 1.400(6) . ? C6 C11 1.413(6) . ? C7 C8 1.380(7) . ? C7 H8 0.9500 . ? C8 C9 1.395(7) . ? C8 H9 0.9500 . ? C9 C10 1.388(6) . ? C9 H10 0.9500 . ? C10 C11 1.404(6) . ? C10 H11 0.9500 . ? C12 C13 1.399(6) . ? C12 C17 1.412(6) . ? C13 C14 1.403(6) . ? C13 H13 0.9500 . ? C14 C15 1.381(8) . ? C14 H14 0.9500 . ? C15 C16 1.392(7) . ? C15 H15 0.9500 . ? C16 C17 1.407(6) . ? C16 H16 0.9500 . ? C17 C18 1.464(6) . ? C18 C19 1.392(6) . ? C19 C20 1.375(7) . ? C19 H19 0.9500 . ? C20 C21 1.388(7) . ? C20 H20 0.9500 . ? C21 C22 1.380(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C1S N1S 1.138(6) . ? C1S C2S 1.449(7) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S C4S 1.462(10) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S N2S 1.141(8) . ? C5S C6S 1.477(7) . ? C6S N3S 1.145(6) . ? 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 C23 Ir1 N2 90.87(15) . . ? C23 Ir1 C12 89.25(16) . . ? N2 Ir1 C12 79.98(16) . . ? C23 Ir1 C24 92.48(16) . . ? N2 Ir1 C24 93.41(15) . . ? C12 Ir1 C24 173.20(16) . . ? C23 Ir1 N1 94.99(16) . . ? N2 Ir1 N1 171.40(13) . . ? C12 Ir1 N1 93.79(16) . . ? C24 Ir1 N1 92.62(15) . . ? C23 Ir1 C11 173.91(16) . . ? N2 Ir1 C11 93.78(16) . . ? C12 Ir1 C11 87.69(16) . . ? C24 Ir1 C11 91.17(16) . . ? N1 Ir1 C11 79.97(16) . . ? O1S Pr1 O6 122.15(10) . . ? O1S Pr1 O2S 134.27(10) . . ? O6 Pr1 O2S 79.52(11) . . ? O1S Pr1 O3 85.37(10) . . ? O6 Pr1 O3 74.49(10) . . ? O2S Pr1 O3 140.25(10) . . ? O1S Pr1 N3 148.71(12) . . ? O6 Pr1 N3 76.90(11) . . ? O2S Pr1 N3 69.22(11) . . ? O3 Pr1 N3 75.88(11) . . ? O1S Pr1 N6 76.91(11) . 2_676 ? O6 Pr1 N6 82.41(11) . 2_676 ? O2S Pr1 N6 66.06(11) . 2_676 ? O3 Pr1 N6 137.05(11) . 2_676 ? N3 Pr1 N6 133.28(12) . 2_676 ? O1S Pr1 O1 75.64(10) . . ? O6 Pr1 O1 121.57(10) . . ? O2S Pr1 O1 130.44(11) . . ? O3 Pr1 O1 50.24(10) . . ? N3 Pr1 O1 73.11(11) . . ? N6 Pr1 O1 150.58(11) 2_676 . ? O1S Pr1 O4 72.17(10) . . ? O6 Pr1 O4 50.04(10) . . ? O2S Pr1 O4 117.02(11) . . ? O3 Pr1 O4 65.75(10) . . ? N3 Pr1 O4 120.00(11) . . ? N6 Pr1 O4 71.61(11) 2_676 . ? O1 Pr1 O4 109.23(10) . . ? O1S Pr1 N3S 83.63(11) . . ? O6 Pr1 N3S 151.50(11) . . ? O2S Pr1 N3S 73.04(12) . . ? O3 Pr1 N3S 123.60(11) . . ? N3 Pr1 N3S 86.17(12) . . ? N6 Pr1 N3S 93.22(12) 2_676 . ? O1 Pr1 N3S 73.46(11) . . ? O4 Pr1 N3S 153.65(11) . . ? O1S Pr1 N5 97.04(10) . . ? O6 Pr1 N5 25.20(10) . . ? O2S Pr1 N5 99.39(11) . . ? O3 Pr1 N5 67.05(10) . . ? N3 Pr1 N5 98.34(11) . . ? N6 Pr1 N5 76.60(11) 2_676 . ? O1 Pr1 N5 117.10(10) . . ? O4 Pr1 N5 24.87(10) . . ? N3S Pr1 N5 169.30(12) . . ? O1S Pr1 N4 80.29(10) . . ? O6 Pr1 N4 98.08(11) . . ? O2S Pr1 N4 140.67(10) . . ? O3 Pr1 N4 25.37(10) . . ? N3 Pr1 N4 72.01(11) . . ? N6 Pr1 N4 153.12(11) 2_676 . ? O1 Pr1 N4 24.89(10) . . ? O4 Pr1 N4 88.03(10) . . ? N3S Pr1 N4 98.24(12) . . ? N5 Pr1 N4 92.38(10) . . ? N4 O1 Pr1 96.5(2) . . ? N4 O3 Pr1 97.1(2) . . ? N5 O4 Pr1 94.8(2) . . ? N5 O6 Pr1 98.7(2) . . ? C1 N1 C5 119.2(4) . . ? C1 N1 Ir1 124.4(3) . . ? C5 N1 Ir1 116.3(3) . . ? C22 N2 C18 118.6(4) . . ? C22 N2 Ir1 124.9(3) . . ? C18 N2 Ir1 116.5(3) . . ? C24 N3 Pr1 164.7(3) . . ? O2 N4 O1 123.0(4) . . ? O2 N4 O3 120.9(4) . . ? O1 N4 O3 116.1(4) . . ? O2 N4 Pr1 176.3(3) . . ? O1 N4 Pr1 58.6(2) . . ? O3 N4 Pr1 57.5(2) . . ? O5 N5 O4 122.8(4) . . ? O5 N5 O6 121.0(4) . . ? O4 N5 O6 116.3(4) . . ? O5 N5 Pr1 175.6(3) . . ? O4 N5 Pr1 60.3(2) . . ? O6 N5 Pr1 56.1(2) . . ? C23 N6 Pr1 136.7(3) . 2_676 ? N1 C1 C2 122.3(4) . . ? N1 C1 H2 118.9 . . ? C2 C1 H2 118.9 . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H3 120.0 . . ? C3 C2 H3 120.7 . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H4 120.7 . . ? C2 C3 H4 120.7 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H5 119.8 . . ? C3 C4 H5 119.8 . . ? N1 C5 C4 120.2(4) . . ? N1 C5 C6 114.5(4) . . ? C4 C5 C6 125.4(4) . . ? C7 C6 C11 121.5(4) . . ? C7 C6 C5 123.1(4) . . ? C11 C6 C5 115.5(4) . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H8 119.9 . . ? C6 C7 H8 119.9 . . ? C7 C8 C9 119.3(4) . . ? C7 C8 H9 120.3 . . ? C9 C8 H9 120.3 . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H10 119.6 . . ? C8 C9 H10 119.6 . . ? C9 C10 C11 121.3(4) . . ? C9 C10 H11 119.3 . . ? C11 C10 H11 119.3 . . ? C10 C11 C6 117.0(4) . . ? C10 C11 Ir1 129.2(3) . . ? C6 C11 Ir1 113.8(3) . . ? C13 C12 C17 117.4(4) . . ? C13 C12 Ir1 128.8(3) . . ? C17 C12 Ir1 113.8(3) . . ? C12 C13 C14 121.2(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.4(4) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C12 121.4(4) . . ? C16 C17 C18 122.7(4) . . ? C12 C17 C18 115.8(4) . . ? N2 C18 C19 120.0(4) . . ? N2 C18 C17 114.0(4) . . ? C19 C18 C17 126.0(4) . . ? C20 C19 C18 121.1(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 118.6(4) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N2 C22 C21 122.5(4) . . ? N2 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N6 C23 Ir1 178.5(4) . . ? N3 C24 Ir1 174.3(4) . . ? N1S C1S C2S 179.4(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C4S C3S H3S1 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C4S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N2S C4S C3S 178.7(7) . . ? N3S C6S C5S 179.4(5) . . ? C6S N3S Pr1 167.4(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 O1S Pr1 O1 N4 97.9(2) . . . . ? O6 Pr1 O1 N4 -21.2(3) . . . . ? O2S Pr1 O1 N4 -125.3(2) . . . . ? O3 Pr1 O1 N4 1.9(2) . . . . ? N3 Pr1 O1 N4 -83.5(2) . . . . ? N6 Pr1 O1 N4 119.5(3) 2_676 . . . ? O4 Pr1 O1 N4 33.0(2) . . . . ? N3S Pr1 O1 N4 -174.5(3) . . . . ? N5 Pr1 O1 N4 7.3(3) . . . . ? O1S Pr1 O3 N4 -77.0(2) . . . . ? O6 Pr1 O3 N4 157.8(2) . . . . ? O2S Pr1 O3 N4 106.7(2) . . . . ? N3 Pr1 O3 N4 77.7(2) . . . . ? N6 Pr1 O3 N4 -142.2(2) 2_676 . . . ? O1 Pr1 O3 N4 -1.9(2) . . . . ? O4 Pr1 O3 N4 -149.5(2) . . . . ? N3S Pr1 O3 N4 2.2(3) . . . . ? N5 Pr1 O3 N4 -176.7(2) . . . . ? O1S Pr1 O4 N5 179.6(3) . . . . ? O6 Pr1 O4 N5 2.3(2) . . . . ? O2S Pr1 O4 N5 48.4(3) . . . . ? O3 Pr1 O4 N5 -87.4(2) . . . . ? N3 Pr1 O4 N5 -32.1(3) . . . . ? N6 Pr1 O4 N5 97.9(2) 2_676 . . . ? O1 Pr1 O4 N5 -113.2(2) . . . . ? N3S Pr1 O4 N5 155.3(3) . . . . ? N4 Pr1 O4 N5 -100.0(2) . . . . ? O1S Pr1 O6 N5 -5.3(3) . . . . ? O2S Pr1 O6 N5 -141.5(3) . . . . ? O3 Pr1 O6 N5 68.9(2) . . . . ? N3 Pr1 O6 N5 147.6(3) . . . . ? N6 Pr1 O6 N5 -74.6(2) 2_676 . . . ? O1 Pr1 O6 N5 87.1(3) . . . . ? O4 Pr1 O6 N5 -2.3(2) . . . . ? N3S Pr1 O6 N5 -157.3(3) . . . . ? N4 Pr1 O6 N5 78.3(2) . . . . ? C23 Ir1 N1 C1 2.3(3) . . . . ? N2 Ir1 N1 C1 135.1(8) . . . . ? C12 Ir1 N1 C1 91.9(3) . . . . ? C24 Ir1 N1 C1 -90.4(3) . . . . ? C11 Ir1 N1 C1 178.9(3) . . . . ? C23 Ir1 N1 C5 -176.1(3) . . . . ? N2 Ir1 N1 C5 -43.3(10) . . . . ? C12 Ir1 N1 C5 -86.6(3) . . . . ? C24 Ir1 N1 C5 91.1(3) . . . . ? C11 Ir1 N1 C5 0.4(3) . . . . ? C23 Ir1 N2 C22 -91.1(4) . . . . ? C12 Ir1 N2 C22 179.8(4) . . . . ? C24 Ir1 N2 C22 1.4(4) . . . . ? N1 Ir1 N2 C22 135.8(8) . . . . ? C11 Ir1 N2 C22 92.8(4) . . . . ? C23 Ir1 N2 C18 89.3(3) . . . . ? C12 Ir1 N2 C18 0.2(3) . . . . ? C24 Ir1 N2 C18 -178.2(3) . . . . ? N1 Ir1 N2 C18 -43.8(10) . . . . ? C11 Ir1 N2 C18 -86.8(3) . . . . ? O1S Pr1 N3 C24 112.0(13) . . . . ? O6 Pr1 N3 C24 -20.0(13) . . . . ? O2S Pr1 N3 C24 -103.6(13) . . . . ? O3 Pr1 N3 C24 57.0(13) . . . . ? N6 Pr1 N3 C24 -86.1(13) 2_676 . . . ? O1 Pr1 N3 C24 109.2(13) . . . . ? O4 Pr1 N3 C24 6.4(14) . . . . ? N3S Pr1 N3 C24 -176.9(13) . . . . ? N5 Pr1 N3 C24 -6.7(13) . . . . ? N4 Pr1 N3 C24 83.1(13) . . . . ? Pr1 O1 N4 O2 176.1(3) . . . . ? Pr1 O1 N4 O3 -3.2(3) . . . . ? Pr1 O3 N4 O2 -176.1(3) . . . . ? Pr1 O3 N4 O1 3.3(4) . . . . ? O1S Pr1 N4 O2 166(5) . . . . ? O6 Pr1 N4 O2 45(5) . . . . ? O2S Pr1 N4 O2 -38(5) . . . . ? O3 Pr1 N4 O2 66(5) . . . . ? N3 Pr1 N4 O2 -29(5) . . . . ? N6 Pr1 N4 O2 134(5) 2_676 . . . ? O1 Pr1 N4 O2 -117(5) . . . . ? O4 Pr1 N4 O2 94(5) . . . . ? N3S Pr1 N4 O2 -112(5) . . . . ? N5 Pr1 N4 O2 69(5) . . . . ? O1S Pr1 N4 O1 -76.8(2) . . . . ? O6 Pr1 N4 O1 161.8(2) . . . . ? O2S Pr1 N4 O1 78.5(3) . . . . ? O3 Pr1 N4 O1 -176.5(4) . . . . ? N3 Pr1 N4 O1 88.5(2) . . . . ? N6 Pr1 N4 O1 -109.0(3) 2_676 . . . ? O4 Pr1 N4 O1 -149.0(2) . . . . ? N3S Pr1 N4 O1 5.3(2) . . . . ? N5 Pr1 N4 O1 -173.5(2) . . . . ? O1S Pr1 N4 O3 99.8(2) . . . . ? O6 Pr1 N4 O3 -21.6(2) . . . . ? O2S Pr1 N4 O3 -104.9(3) . . . . ? N3 Pr1 N4 O3 -94.9(2) . . . . ? N6 Pr1 N4 O3 67.5(3) 2_676 . . . ? O1 Pr1 N4 O3 176.5(4) . . . . ? O4 Pr1 N4 O3 27.5(2) . . . . ? N3S Pr1 N4 O3 -178.2(2) . . . . ? N5 Pr1 N4 O3 3.1(2) . . . . ? Pr1 O4 N5 O5 176.3(4) . . . . ? Pr1 O4 N5 O6 -3.8(4) . . . . ? Pr1 O6 N5 O5 -176.2(3) . . . . ? Pr1 O6 N5 O4 4.0(4) . . . . ? O1S Pr1 N5 O5 -136(4) . . . . ? O6 Pr1 N5 O5 49(4) . . . . ? O2S Pr1 N5 O5 87(4) . . . . ? O3 Pr1 N5 O5 -54(4) . . . . ? N3 Pr1 N5 O5 17(4) . . . . ? N6 Pr1 N5 O5 149(4) 2_676 . . . ? O1 Pr1 N5 O5 -58(4) . . . . ? O4 Pr1 N5 O5 -135(4) . . . . ? N3S Pr1 N5 O5 131(4) . . . . ? N4 Pr1 N5 O5 -55(4) . . . . ? O1S Pr1 N5 O4 -0.4(2) . . . . ? O6 Pr1 N5 O4 -175.9(4) . . . . ? O2S Pr1 N5 O4 -137.6(2) . . . . ? O3 Pr1 N5 O4 81.5(2) . . . . ? N3 Pr1 N5 O4 152.3(2) . . . . ? N6 Pr1 N5 O4 -75.1(2) 2_676 . . . ? O1 Pr1 N5 O4 77.0(2) . . . . ? N3S Pr1 N5 O4 -93.4(6) . . . . ? N4 Pr1 N5 O4 80.1(2) . . . . ? O1S Pr1 N5 O6 175.5(2) . . . . ? O2S Pr1 N5 O6 38.3(3) . . . . ? O3 Pr1 N5 O6 -102.6(3) . . . . ? N3 Pr1 N5 O6 -31.8(3) . . . . ? N6 Pr1 N5 O6 100.8(3) 2_676 . . . ? O1 Pr1 N5 O6 -107.1(2) . . . . ? O4 Pr1 N5 O6 175.9(4) . . . . ? N3S Pr1 N5 O6 82.5(7) . . . . ? N4 Pr1 N5 O6 -104.0(2) . . . . ? C5 N1 C1 C2 -0.5(6) . . . . ? Ir1 N1 C1 C2 -178.9(3) . . . . ? N1 C1 C2 C3 0.1(7) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C2 C3 C4 C5 -0.9(7) . . . . ? C1 N1 C5 C4 0.2(6) . . . . ? Ir1 N1 C5 C4 178.7(3) . . . . ? C1 N1 C5 C6 -178.8(4) . . . . ? Ir1 N1 C5 C6 -0.3(5) . . . . ? C3 C4 C5 N1 0.5(6) . . . . ? C3 C4 C5 C6 179.3(4) . . . . ? N1 C5 C6 C7 179.6(4) . . . . ? C4 C5 C6 C7 0.8(7) . . . . ? N1 C5 C6 C11 -0.2(5) . . . . ? C4 C5 C6 C11 -179.1(4) . . . . ? C11 C6 C7 C8 2.2(6) . . . . ? C5 C6 C7 C8 -177.6(4) . . . . ? C6 C7 C8 C9 -0.7(7) . . . . ? C7 C8 C9 C10 -0.7(7) . . . . ? C8 C9 C10 C11 0.8(7) . . . . ? C9 C10 C11 C6 0.6(6) . . . . ? C9 C10 C11 Ir1 177.3(3) . . . . ? C7 C6 C11 C10 -2.1(6) . . . . ? C5 C6 C11 C10 177.7(4) . . . . ? C7 C6 C11 Ir1 -179.3(3) . . . . ? C5 C6 C11 Ir1 0.5(5) . . . . ? C23 Ir1 C11 C10 -142.9(13) . . . . ? N2 Ir1 C11 C10 -3.2(4) . . . . ? C12 Ir1 C11 C10 -83.0(4) . . . . ? C24 Ir1 C11 C10 90.3(4) . . . . ? N1 Ir1 C11 C10 -177.3(4) . . . . ? C23 Ir1 C11 C6 33.9(15) . . . . ? N2 Ir1 C11 C6 173.6(3) . . . . ? C12 Ir1 C11 C6 93.8(3) . . . . ? C24 Ir1 C11 C6 -92.9(3) . . . . ? N1 Ir1 C11 C6 -0.5(3) . . . . ? C23 Ir1 C12 C13 88.8(4) . . . . ? N2 Ir1 C12 C13 179.9(4) . . . . ? C24 Ir1 C12 C13 -166.4(12) . . . . ? N1 Ir1 C12 C13 -6.1(4) . . . . ? C11 Ir1 C12 C13 -85.9(4) . . . . ? C23 Ir1 C12 C17 -90.5(3) . . . . ? N2 Ir1 C12 C17 0.5(3) . . . . ? C24 Ir1 C12 C17 14.2(15) . . . . ? N1 Ir1 C12 C17 174.5(3) . . . . ? C11 Ir1 C12 C17 94.7(3) . . . . ? C17 C12 C13 C14 2.7(7) . . . . ? Ir1 C12 C13 C14 -176.6(4) . . . . ? C12 C13 C14 C15 -1.0(7) . . . . ? C13 C14 C15 C16 -0.8(8) . . . . ? C14 C15 C16 C17 0.7(7) . . . . ? C15 C16 C17 C12 1.1(7) . . . . ? C15 C16 C17 C18 178.7(4) . . . . ? C13 C12 C17 C16 -2.8(6) . . . . ? Ir1 C12 C17 C16 176.6(3) . . . . ? C13 C12 C17 C18 179.5(4) . . . . ? Ir1 C12 C17 C18 -1.1(5) . . . . ? C22 N2 C18 C19 -1.2(6) . . . . ? Ir1 N2 C18 C19 178.5(3) . . . . ? C22 N2 C18 C17 179.5(4) . . . . ? Ir1 N2 C18 C17 -0.9(5) . . . . ? C16 C17 C18 N2 -176.4(4) . . . . ? C12 C17 C18 N2 1.3(6) . . . . ? C16 C17 C18 C19 4.3(7) . . . . ? C12 C17 C18 C19 -178.0(4) . . . . ? N2 C18 C19 C20 1.9(7) . . . . ? C17 C18 C19 C20 -178.9(5) . . . . ? C18 C19 C20 C21 -1.3(8) . . . . ? C19 C20 C21 C22 0.1(8) . . . . ? C18 N2 C22 C21 0.0(7) . . . . ? Ir1 N2 C22 C21 -179.6(4) . . . . ? C20 C21 C22 N2 0.6(8) . . . . ? Pr1 N6 C23 Ir1 54(14) 2_676 . . . ? N2 Ir1 C23 N6 45(13) . . . . ? C12 Ir1 C23 N6 125(13) . . . . ? C24 Ir1 C23 N6 -49(13) . . . . ? N1 Ir1 C23 N6 -141(13) . . . . ? C11 Ir1 C23 N6 -175(100) . . . . ? Pr1 N3 C24 Ir1 -31(5) . . . . ? C23 Ir1 C24 N3 95(4) . . . . ? N2 Ir1 C24 N3 4(4) . . . . ? C12 Ir1 C24 N3 -9(5) . . . . ? N1 Ir1 C24 N3 -170(4) . . . . ? C11 Ir1 C24 N3 -90(4) . . . . ? C5S C6S N3S Pr1 -46(61) . . . . ? O1S Pr1 N3S C6S -172.8(17) . . . . ? O6 Pr1 N3S C6S -16.3(18) . . . . ? O2S Pr1 N3S C6S -32.5(17) . . . . ? O3 Pr1 N3S C6S 107.1(17) . . . . ? N3 Pr1 N3S C6S 36.9(17) . . . . ? N6 Pr1 N3S C6S -96.3(17) 2_676 . . . ? O1 Pr1 N3S C6S 110.4(17) . . . . ? O4 Pr1 N3S C6S -149.6(16) . . . . ? N5 Pr1 N3S C6S -78.5(19) . . . . ? N4 Pr1 N3S C6S 108.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.365 _refine_diff_density_min -1.500 _refine_diff_density_rms 0.195 #===END data_imw1493p-1 _database_code_depnum_ccdc_archive 'CCDC 834579' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H64 Cl Ir2 La N8 O10' _chemical_formula_weight 1543.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3521(3) _cell_length_b 17.6711(5) _cell_length_c 19.5092(6) _cell_angle_alpha 64.1940(10) _cell_angle_beta 88.939(2) _cell_angle_gamma 81.078(2) _cell_volume 2863.12(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.59 _exptl_crystal_description BLOCK _exptl_crystal_colour 'PALE YELLOW' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 5.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1376 _exptl_absorpt_correction_T_max 0.6104 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46621 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.62 _reflns_number_total 13188 _reflns_number_gt 11924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+5.7684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13188 _refine_ls_number_parameters 688 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.987510(12) 0.263718(7) 0.146108(7) 0.01636(4) Uani 1 1 d . . . Ir2 Ir 0.650877(12) 0.745302(7) 0.352930(6) 0.01557(4) Uani 1 1 d . . . La1 La 0.960208(18) 0.512798(11) 0.260402(10) 0.01694(4) Uani 1 1 d . . . C1 C 1.0717(3) 0.3488(2) 0.05184(18) 0.0213(6) Uani 1 1 d . . . C2 C 1.0005(3) 0.3358(2) 0.20294(18) 0.0203(6) Uani 1 1 d . . . C3 C 0.7053(4) 0.3856(2) 0.1159(2) 0.0266(7) Uani 1 1 d . . . H3 H 0.7531 0.4092 0.1427 0.032 Uiso 1 1 calc R . . C4 C 0.5617(4) 0.4178(2) 0.0915(2) 0.0323(8) Uani 1 1 d . . . H4 H 0.5108 0.4619 0.1023 0.039 Uiso 1 1 calc R . . C5 C 0.4933(4) 0.3844(3) 0.0508(2) 0.0345(9) Uani 1 1 d . . . H5 H 0.3942 0.4050 0.0339 0.041 Uiso 1 1 calc R . . C6 C 0.5694(4) 0.3220(2) 0.0355(2) 0.0296(8) Uani 1 1 d . . . H6 H 0.5239 0.3003 0.0063 0.035 Uiso 1 1 calc R . . C7 C 0.7149(4) 0.2892(2) 0.06247(19) 0.0226(7) Uani 1 1 d . A . C8 C 0.8069(4) 0.2206(2) 0.0517(2) 0.0251(7) Uani 1 1 d . A . C9 C 0.7599(4) 0.1813(3) 0.0096(2) 0.0340(8) Uani 1 1 d . . . H9 H 0.6639 0.1980 -0.0127 0.041 Uiso 1 1 calc R . . C10 C 0.8533(5) 0.1186(3) 0.0009(2) 0.0394(10) Uani 1 1 d . . . H10 H 0.8215 0.0909 -0.0268 0.047 Uiso 1 1 calc R . . C11 C 0.9950(5) 0.0953(3) 0.0326(2) 0.0342(8) Uani 1 1 d . . . H11 H 1.0602 0.0529 0.0253 0.041 Uiso 1 1 calc R . . C12 C 1.0408(4) 0.1341(2) 0.0750(2) 0.0257(7) Uani 1 1 d . . . H12 H 1.1371 0.1172 0.0969 0.031 Uiso 1 1 calc R . . C13 C 0.9485(3) 0.1972(2) 0.08609(18) 0.0202(6) Uani 1 1 d . . . C14 C 1.3100(3) 0.1993(2) 0.1610(2) 0.0236(7) Uani 1 1 d . . . H14 H 1.3139 0.2507 0.1165 0.028 Uiso 1 1 calc R . . C15 C 1.4359(4) 0.1412(2) 0.1906(2) 0.0300(8) Uani 1 1 d . . . H15 H 1.5249 0.1526 0.1670 0.036 Uiso 1 1 calc R . . C16 C 1.4305(4) 0.0666(2) 0.2549(2) 0.0322(8) Uani 1 1 d . . . H16 H 1.5155 0.0253 0.2758 0.039 Uiso 1 1 calc R . . C17 C 1.3000(4) 0.0524(2) 0.2888(2) 0.0295(8) Uani 1 1 d . . . H17 H 1.2950 0.0013 0.3333 0.035 Uiso 1 1 calc R . . C18 C 1.1756(4) 0.1131(2) 0.25772(19) 0.0225(7) Uani 1 1 d . A . C19 C 1.0300(4) 0.1055(2) 0.28703(19) 0.0236(7) Uani 1 1 d . A . C20 C 1.0010(4) 0.0374(2) 0.3549(2) 0.0328(8) Uani 1 1 d . . . H20 H 1.0775 -0.0062 0.3852 0.039 Uiso 1 1 calc R . . C21 C 0.8597(5) 0.0345(3) 0.3771(2) 0.0378(9) Uani 1 1 d . . . H21 H 0.8388 -0.0112 0.4228 0.045 Uiso 1 1 calc R . . C22 C 0.7489(4) 0.0980(3) 0.3326(2) 0.0346(9) Uani 1 1 d . . . H22 H 0.6521 0.0952 0.3479 0.042 Uiso 1 1 calc R . . C23 C 0.7771(4) 0.1654(2) 0.2664(2) 0.0285(7) Uani 1 1 d . . . H23 H 0.6993 0.2084 0.2369 0.034 Uiso 1 1 calc R . . C24 C 0.9186(3) 0.1715(2) 0.24169(18) 0.0208(6) Uani 1 1 d . . . C25 C 0.7268(3) 0.6773(2) 0.29442(18) 0.0190(6) Uani 1 1 d . . . C26 C 0.7790(3) 0.6586(2) 0.44607(19) 0.0206(6) Uani 1 1 d . . . C27 C 0.4540(4) 0.6139(2) 0.3861(2) 0.0301(8) Uani 1 1 d . . . H27 H 0.5135 0.5965 0.3539 0.036 Uiso 1 1 calc R . . C28 C 0.3430(5) 0.5697(3) 0.4207(3) 0.0393(10) Uani 1 1 d . . . H28 H 0.3264 0.5228 0.4120 0.047 Uiso 1 1 calc R . . C29 C 0.2570(4) 0.5941(3) 0.4675(3) 0.0403(10) Uani 1 1 d . . . H29 H 0.1817 0.5635 0.4927 0.048 Uiso 1 1 calc R . . C30 C 0.2814(4) 0.6642(3) 0.4778(2) 0.0325(8) Uani 1 1 d . . . H30 H 0.2213 0.6829 0.5091 0.039 Uiso 1 1 calc R . . C31 C 0.3945(3) 0.7071(2) 0.44194(18) 0.0223(6) Uani 1 1 d . A . C32 C 0.4333(3) 0.7805(2) 0.44956(18) 0.0218(6) Uani 1 1 d . A . C33 C 0.3542(4) 0.8197(2) 0.4899(2) 0.0299(8) Uani 1 1 d . . . H33 H 0.2699 0.7992 0.5142 0.036 Uiso 1 1 calc R . . C34 C 0.3988(4) 0.8886(2) 0.4946(2) 0.0321(8) Uani 1 1 d . . . H34 H 0.3445 0.9159 0.5216 0.039 Uiso 1 1 calc R . . C35 C 0.5228(4) 0.9175(2) 0.4599(2) 0.0321(8) Uani 1 1 d . . . H35 H 0.5539 0.9644 0.4635 0.038 Uiso 1 1 calc R . . C36 C 0.6021(4) 0.8783(2) 0.4196(2) 0.0242(7) Uani 1 1 d . . . H36 H 0.6874 0.8986 0.3967 0.029 Uiso 1 1 calc R . . C37 C 0.5593(3) 0.8099(2) 0.41220(17) 0.0181(6) Uani 1 1 d . . . C38 C 0.9373(4) 0.8092(2) 0.3403(2) 0.0269(7) Uani 1 1 d . . . H38 H 0.9652 0.7592 0.3864 0.032 Uiso 1 1 calc R . . C39 C 1.0350(4) 0.8647(3) 0.3087(2) 0.0328(8) Uani 1 1 d . . . H39 H 1.1291 0.8526 0.3323 0.039 Uiso 1 1 calc R . . C40 C 0.9940(4) 0.9377(3) 0.2426(2) 0.0366(9) Uani 1 1 d . . . H40 H 1.0594 0.9770 0.2204 0.044 Uiso 1 1 calc R . . C41 C 0.8577(4) 0.9536(2) 0.2088(2) 0.0319(8) Uani 1 1 d . . . H41 H 0.8284 1.0040 0.1633 0.038 Uiso 1 1 calc R . . C42 C 0.7623(4) 0.8950(2) 0.24201(19) 0.0233(7) Uani 1 1 d . A . C43 C 0.6153(4) 0.9031(2) 0.21150(19) 0.0239(7) Uani 1 1 d . A . C44 C 0.5553(4) 0.9701(2) 0.1426(2) 0.0335(8) Uani 1 1 d . . . H44 H 0.6102 1.0131 0.1130 0.040 Uiso 1 1 calc R . . C45 C 0.4156(5) 0.9736(3) 0.1176(2) 0.0403(10) Uani 1 1 d . . . H45 H 0.3746 1.0186 0.0707 0.048 Uiso 1 1 calc R . . C46 C 0.3366(4) 0.9113(3) 0.1614(2) 0.0382(9) Uani 1 1 d . . . H46 H 0.2403 0.9141 0.1447 0.046 Uiso 1 1 calc R . . C47 C 0.3962(4) 0.8441(3) 0.2297(2) 0.0302(8) Uani 1 1 d . . . H47 H 0.3399 0.8016 0.2587 0.036 Uiso 1 1 calc R . . C48 C 0.5375(3) 0.8381(2) 0.25649(18) 0.0212(6) Uani 1 1 d . . . C4S C 0.6440(7) 0.7952(3) 0.0828(3) 0.0607(15) Uani 1 1 d . . . H4S1 H 0.5664 0.8446 0.0617 0.091 Uiso 1 1 calc R . . H4S2 H 0.7217 0.8033 0.0471 0.091 Uiso 1 1 calc R . . H4S3 H 0.6825 0.7891 0.1316 0.091 Uiso 1 1 calc R . . C2X C 1.2117(7) 0.5017(4) 0.1138(4) 0.0334(15) Uiso 0.79 1 d PD A 1 H2X1 H 1.2711 0.4632 0.1603 0.050 Uiso 0.79 1 calc PR A 1 H2X2 H 1.2686 0.5434 0.0790 0.050 Uiso 0.79 1 calc PR A 1 H2X3 H 1.1808 0.4688 0.0889 0.050 Uiso 0.79 1 calc PR A 1 C2Y C 1.181(3) 0.5108(15) 0.0975(13) 0.037(6) Uiso 0.21 1 d PD B 2 H2Y1 H 1.2401 0.4542 0.1234 0.055 Uiso 0.21 1 calc PR B 2 H2Y2 H 1.2354 0.5486 0.0570 0.055 Uiso 0.21 1 calc PR B 2 H2Y3 H 1.0914 0.5063 0.0753 0.055 Uiso 0.21 1 calc PR B 2 C3X C 1.0513(15) 0.7371(3) 0.1683(7) 0.074(3) Uiso 0.50 1 d PDU C 1 H3X1 H 1.0723 0.7562 0.1145 0.111 Uiso 0.50 1 calc PR C 1 H3X2 H 1.1114 0.7612 0.1918 0.111 Uiso 0.50 1 calc PR C 1 H3X3 H 0.9487 0.7562 0.1723 0.111 Uiso 0.50 1 calc PR C 1 C3Y C 1.0839(9) 0.7201(4) 0.2282(5) 0.0372(17) Uiso 0.50 1 d PDU D 2 H3Y1 H 0.9828 0.7481 0.2145 0.056 Uiso 0.50 1 calc PR D 2 H3Y2 H 1.1465 0.7542 0.1902 0.056 Uiso 0.50 1 calc PR D 2 H3Y3 H 1.1120 0.7146 0.2785 0.056 Uiso 0.50 1 calc PR D 2 C8S C 0.3682(7) 0.2474(4) 0.3338(4) 0.0692(16) Uani 1 1 d . . . H6S1 H 0.4729 0.2413 0.3272 0.104 Uiso 1 1 calc R . . H6S2 H 0.3165 0.2826 0.2840 0.104 Uiso 1 1 calc R . . H6S3 H 0.3388 0.1911 0.3561 0.104 Uiso 1 1 calc R . . C10X C 0.6690(15) 0.3858(7) 0.3071(12) 0.038(6) Uiso 0.28 1 d PDU E 1 H10A H 0.7435 0.3467 0.2974 0.056 Uiso 0.28 1 calc PR E 1 H10B H 0.5771 0.3910 0.2809 0.056 Uiso 0.28 1 calc PR E 1 H10C H 0.6565 0.3636 0.3621 0.056 Uiso 0.28 1 calc PR E 1 C10Y C 0.6541(7) 0.3905(3) 0.3181(5) 0.033(2) Uiso 0.72 1 d PDU F 2 H10D H 0.6035 0.3953 0.2725 0.050 Uiso 0.72 1 calc PR F 2 H10E H 0.5867 0.3802 0.3591 0.050 Uiso 0.72 1 calc PR F 2 H10F H 0.7353 0.3430 0.3344 0.050 Uiso 0.72 1 calc PR F 2 N1 N 1.1209(3) 0.3955(2) -0.00159(18) 0.0333(7) Uani 1 1 d . . . N2 N 0.9937(3) 0.38004(19) 0.23292(17) 0.0270(6) Uani 1 1 d . . . N3 N 0.7801(3) 0.32199(18) 0.10310(16) 0.0221(6) Uani 1 1 d . . . N4 N 1.1821(3) 0.18558(17) 0.19303(16) 0.0196(5) Uani 1 1 d . . . N5 N 0.7731(3) 0.63696(18) 0.26327(16) 0.0221(6) Uani 1 1 d . . . N6 N 0.8550(3) 0.6094(2) 0.49729(17) 0.0297(7) Uani 1 1 d . . . N7 N 0.4804(3) 0.68124(18) 0.39688(15) 0.0202(5) Uani 1 1 d . . . N8 N 0.8032(3) 0.82371(17) 0.30781(16) 0.0201(5) Uani 1 1 d . . . Cl1 Cl 0.42309(10) 0.58747(7) 0.21475(7) 0.0419(2) Uani 1 1 d . . . O2X O 1.0872(4) 0.5451(2) 0.13281(19) 0.0283(7) Uiso 0.79 1 d PDU A 1 O2Y O 1.1461(15) 0.5451(8) 0.1517(7) 0.030(3) Uiso 0.21 1 d PDU B 2 O3X O 1.0826(6) 0.6462(3) 0.2069(3) 0.0218(12) Uiso 0.50 1 d PDU C 1 O3Y O 1.0993(7) 0.6374(4) 0.2303(4) 0.0354(16) Uiso 0.50 1 d PDU D 2 O4S O 0.5885(3) 0.72133(19) 0.09417(16) 0.0395(7) Uani 1 1 d . . . O5S O 1.2262(3) 0.45778(17) 0.30285(18) 0.0369(6) Uani 1 1 d . A . O6S O 0.9966(3) 0.53369(17) 0.38109(14) 0.0315(6) Uani 1 1 d . A . O7S O 0.9866(3) 0.37284(16) 0.38569(14) 0.0293(5) Uani 1 1 d . A . O8S O 0.3339(4) 0.2874(2) 0.3833(2) 0.0594(9) Uani 1 1 d . . . O9S O 0.7900(4) 0.5739(2) 0.14321(16) 0.0520(9) Uani 1 1 d . A . O10X O 0.7125(11) 0.4677(6) 0.2794(7) 0.025(2) Uiso 0.28 1 d PDU E 1 O10Y O 0.7079(4) 0.4679(2) 0.3011(3) 0.0270(10) Uiso 0.72 1 d PDU F 2 C11S C 0.9532(7) 0.8500(3) 0.5442(3) 0.0636(15) Uani 1 1 d D . . H11A H 0.8601 0.8664 0.5620 0.095 Uiso 1 1 calc R . . H11B H 0.9361 0.8327 0.5040 0.095 Uiso 1 1 calc R . . H11C H 1.0055 0.8986 0.5239 0.095 Uiso 1 1 calc R . . O11S O 1.0367(4) 0.7812(2) 0.60581(19) 0.0543(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01608(6) 0.01850(6) 0.01699(6) -0.01019(5) 0.00079(4) -0.00242(4) Ir2 0.01582(6) 0.01723(6) 0.01547(6) -0.00893(5) 0.00111(4) -0.00239(4) La1 0.01776(8) 0.01861(9) 0.01658(8) -0.00991(7) 0.00253(6) -0.00242(6) C1 0.0202(15) 0.0260(17) 0.0187(15) -0.0115(14) -0.0007(12) -0.0012(13) C2 0.0208(15) 0.0203(16) 0.0198(15) -0.0091(13) 0.0014(12) -0.0023(12) C3 0.0227(16) 0.0283(18) 0.0298(18) -0.0146(15) -0.0002(13) -0.0010(13) C4 0.0251(17) 0.031(2) 0.037(2) -0.0136(17) 0.0003(15) 0.0041(14) C5 0.0196(16) 0.037(2) 0.037(2) -0.0074(17) -0.0030(15) -0.0025(15) C6 0.0227(16) 0.034(2) 0.0300(18) -0.0107(16) -0.0040(14) -0.0070(14) C7 0.0227(15) 0.0235(16) 0.0202(15) -0.0070(13) 0.0002(12) -0.0078(13) C8 0.0246(16) 0.0260(17) 0.0256(17) -0.0112(14) -0.0018(13) -0.0063(13) C9 0.037(2) 0.035(2) 0.034(2) -0.0174(17) -0.0105(16) -0.0062(16) C10 0.055(3) 0.037(2) 0.037(2) -0.0258(19) -0.0086(19) -0.0086(19) C11 0.045(2) 0.032(2) 0.035(2) -0.0238(18) 0.0013(17) -0.0041(17) C12 0.0306(17) 0.0256(17) 0.0230(16) -0.0126(14) 0.0014(13) -0.0050(14) C13 0.0241(15) 0.0210(16) 0.0168(14) -0.0089(13) 0.0012(12) -0.0058(12) C14 0.0207(15) 0.0237(17) 0.0277(17) -0.0122(14) 0.0017(13) -0.0044(13) C15 0.0192(16) 0.034(2) 0.038(2) -0.0181(17) -0.0003(14) -0.0011(14) C16 0.0265(17) 0.0299(19) 0.038(2) -0.0161(17) -0.0080(15) 0.0053(14) C17 0.0347(19) 0.0206(17) 0.0282(18) -0.0077(15) -0.0053(15) 0.0017(14) C18 0.0253(16) 0.0217(16) 0.0245(16) -0.0137(14) -0.0006(13) -0.0035(13) C19 0.0308(17) 0.0236(17) 0.0195(16) -0.0114(14) 0.0053(13) -0.0080(14) C20 0.044(2) 0.0254(19) 0.0251(18) -0.0064(15) 0.0025(16) -0.0085(16) C21 0.049(2) 0.037(2) 0.030(2) -0.0123(18) 0.0135(17) -0.0217(19) C22 0.035(2) 0.048(2) 0.0276(19) -0.0185(18) 0.0097(15) -0.0182(17) C23 0.0267(17) 0.038(2) 0.0257(17) -0.0171(16) 0.0045(14) -0.0090(15) C24 0.0250(16) 0.0259(17) 0.0179(15) -0.0140(13) 0.0029(12) -0.0089(13) C25 0.0152(13) 0.0226(16) 0.0185(15) -0.0086(13) -0.0016(11) -0.0019(12) C26 0.0220(15) 0.0217(16) 0.0221(16) -0.0133(14) 0.0009(12) -0.0037(12) C27 0.0318(18) 0.035(2) 0.0345(19) -0.0224(17) 0.0093(15) -0.0148(15) C28 0.044(2) 0.045(2) 0.045(2) -0.029(2) 0.0115(18) -0.0271(19) C29 0.035(2) 0.054(3) 0.046(2) -0.029(2) 0.0166(18) -0.0276(19) C30 0.0293(18) 0.046(2) 0.0323(19) -0.0232(18) 0.0119(15) -0.0155(16) C31 0.0209(15) 0.0277(17) 0.0185(15) -0.0102(14) 0.0025(12) -0.0047(13) C32 0.0218(15) 0.0260(17) 0.0196(15) -0.0119(14) 0.0035(12) -0.0038(13) C33 0.0291(18) 0.037(2) 0.0271(18) -0.0177(16) 0.0091(14) -0.0045(15) C34 0.041(2) 0.032(2) 0.0292(19) -0.0207(17) 0.0068(16) 0.0020(16) C35 0.043(2) 0.0277(19) 0.0318(19) -0.0193(16) 0.0041(16) -0.0052(16) C36 0.0266(16) 0.0245(17) 0.0242(16) -0.0130(14) 0.0038(13) -0.0047(13) C37 0.0184(14) 0.0206(15) 0.0143(14) -0.0077(12) 0.0003(11) -0.0002(12) C38 0.0234(16) 0.0297(19) 0.0314(18) -0.0165(16) 0.0032(14) -0.0056(14) C39 0.0236(17) 0.038(2) 0.043(2) -0.0216(19) 0.0055(15) -0.0121(15) C40 0.036(2) 0.038(2) 0.045(2) -0.023(2) 0.0176(17) -0.0199(17) C41 0.041(2) 0.0261(19) 0.0298(19) -0.0115(16) 0.0096(16) -0.0117(16) C42 0.0288(17) 0.0197(16) 0.0244(16) -0.0125(14) 0.0077(13) -0.0043(13) C43 0.0273(16) 0.0210(16) 0.0220(16) -0.0092(14) 0.0029(13) -0.0001(13) C44 0.041(2) 0.0243(19) 0.0277(19) -0.0064(15) 0.0007(16) -0.0002(15) C45 0.046(2) 0.034(2) 0.0268(19) -0.0061(17) -0.0076(17) 0.0117(18) C46 0.0292(19) 0.049(3) 0.029(2) -0.0154(19) -0.0077(15) 0.0087(17) C47 0.0262(17) 0.038(2) 0.0231(17) -0.0118(16) -0.0035(14) -0.0014(15) C48 0.0222(15) 0.0226(16) 0.0200(15) -0.0122(13) 0.0013(12) 0.0018(12) C4S 0.095(4) 0.046(3) 0.038(3) -0.012(2) -0.011(3) -0.022(3) C8S 0.067(4) 0.057(3) 0.083(4) -0.035(3) -0.014(3) 0.007(3) N1 0.0329(16) 0.0366(18) 0.0268(16) -0.0103(14) 0.0052(13) -0.0072(14) N2 0.0310(15) 0.0259(15) 0.0267(15) -0.0144(13) 0.0018(12) -0.0036(12) N3 0.0170(12) 0.0232(14) 0.0255(14) -0.0106(12) -0.0004(11) -0.0015(10) N4 0.0184(12) 0.0188(13) 0.0228(13) -0.0107(11) -0.0014(10) -0.0015(10) N5 0.0213(13) 0.0252(15) 0.0221(14) -0.0134(12) 0.0008(11) -0.0009(11) N6 0.0309(16) 0.0312(17) 0.0250(15) -0.0115(13) -0.0042(12) -0.0015(13) N7 0.0205(13) 0.0231(14) 0.0194(13) -0.0105(11) 0.0015(10) -0.0068(11) N8 0.0198(13) 0.0210(14) 0.0225(13) -0.0121(11) 0.0034(10) -0.0042(10) Cl1 0.0237(4) 0.0440(6) 0.0532(6) -0.0148(5) 0.0014(4) -0.0121(4) O4S 0.0374(15) 0.0452(17) 0.0354(15) -0.0166(14) -0.0017(12) -0.0084(13) O5S 0.0197(12) 0.0290(14) 0.0587(19) -0.0160(14) 0.0055(12) -0.0045(10) O6S 0.0352(14) 0.0355(14) 0.0269(13) -0.0199(12) -0.0088(11) 0.0054(11) O7S 0.0341(13) 0.0326(14) 0.0238(12) -0.0127(11) 0.0019(10) -0.0121(11) O8S 0.069(2) 0.0401(19) 0.061(2) -0.0191(17) -0.0185(19) 0.0052(16) O9S 0.059(2) 0.065(2) 0.0258(14) -0.0261(15) -0.0106(14) 0.0271(16) C11S 0.083(4) 0.050(3) 0.051(3) -0.017(3) -0.014(3) -0.006(3) O11S 0.075(2) 0.0385(18) 0.0443(18) -0.0132(15) -0.0080(17) -0.0095(16) _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 C2 2.037(3) . ? Ir1 C1 2.042(3) . ? Ir1 C24 2.045(3) . ? Ir1 N3 2.053(3) . ? Ir1 C13 2.057(3) . ? Ir1 N4 2.059(3) . ? Ir2 C25 2.037(3) . ? Ir2 C26 2.043(3) . ? Ir2 C37 2.045(3) . ? Ir2 C48 2.049(3) . ? Ir2 N7 2.055(3) . ? Ir2 N8 2.056(3) . ? La1 O9S 2.526(3) . ? La1 O10X 2.535(10) . ? La1 O5S 2.538(3) . ? La1 O3X 2.571(5) . ? La1 O3Y 2.573(6) . ? La1 O6S 2.573(2) . ? La1 O7S 2.593(3) . ? La1 N2 2.598(3) . ? La1 O10Y 2.606(4) . ? La1 N5 2.606(3) . ? La1 O2X 2.607(3) . ? La1 O2Y 2.639(12) . ? C1 N1 1.153(5) . ? C2 N2 1.157(4) . ? C3 N3 1.345(4) . ? C3 C4 1.380(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.361(6) . ? C5 H5 0.9500 . ? C6 C7 1.407(5) . ? C6 H6 0.9500 . ? C7 N3 1.365(4) . ? C7 C8 1.465(5) . ? C8 C9 1.398(5) . ? C8 C13 1.412(4) . ? C9 C10 1.371(6) . ? C9 H9 0.9500 . ? C10 C11 1.396(6) . ? C10 H10 0.9500 . ? C11 C12 1.392(5) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C14 N4 1.346(4) . ? C14 C15 1.381(5) . ? C14 H14 0.9500 . ? C15 C16 1.376(6) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.393(5) . ? C17 H17 0.9500 . ? C18 N4 1.361(4) . ? C18 C19 1.470(5) . ? C19 C20 1.405(5) . ? C19 C24 1.409(5) . ? C20 C21 1.385(6) . ? C20 H20 0.9500 . ? C21 C22 1.381(6) . ? C21 H21 0.9500 . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 C24 1.404(5) . ? C23 H23 0.9500 . ? C25 N5 1.157(4) . ? C26 N6 1.157(4) . ? C27 N7 1.353(4) . ? C27 C28 1.382(5) . ? C27 H27 0.9500 . ? C28 C29 1.370(6) . ? C28 H28 0.9500 . ? C29 C30 1.390(6) . ? C29 H29 0.9500 . ? C30 C31 1.393(5) . ? C30 H30 0.9500 . ? C31 N7 1.355(4) . ? C31 C32 1.467(5) . ? C32 C33 1.393(5) . ? C32 C37 1.420(4) . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.393(5) . ? C35 H35 0.9500 . ? C36 C37 1.396(4) . ? C36 H36 0.9500 . ? C38 N8 1.352(4) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 H39 0.9500 . ? C40 C41 1.377(6) . ? C40 H40 0.9500 . ? C41 C42 1.404(5) . ? C41 H41 0.9500 . ? C42 N8 1.357(4) . ? C42 C43 1.470(5) . ? C43 C44 1.400(5) . ? C43 C48 1.406(5) . ? C44 C45 1.386(6) . ? C44 H44 0.9500 . ? C45 C46 1.377(6) . ? C45 H45 0.9500 . ? C46 C47 1.393(5) . ? C46 H46 0.9500 . ? C47 C48 1.402(5) . ? C47 H47 0.9500 . ? C4S O4S 1.406(6) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C2X O2X 1.426(6) . ? C2X H2X1 0.9800 . ? C2X H2X2 0.9800 . ? C2X H2X3 0.9800 . ? C2Y O2Y 1.441(16) . ? C2Y H2Y1 0.9800 . ? C2Y H2Y2 0.9800 . ? C2Y H2Y3 0.9800 . ? C3X O3X 1.4286(10) . ? C3X H3X1 0.9800 . ? C3X H3X2 0.9800 . ? C3X H3X3 0.9800 . ? C3Y O3Y 1.4281(10) . ? C3Y H3Y1 0.9800 . ? C3Y H3Y2 0.9800 . ? C3Y H3Y3 0.9800 . ? C8S O8S 1.431(7) . ? C8S H6S1 0.9800 . ? C8S H6S2 0.9800 . ? C8S H6S3 0.9800 . ? C10X O10X 1.4300(2) . ? C10X H10A 0.9800 . ? C10X H10B 0.9800 . ? C10X H10C 0.9800 . ? C10Y O10Y 1.4300(2) . ? C10Y H10D 0.9800 . ? C10Y H10E 0.9800 . ? C10Y H10F 0.9800 . ? C11S O11S 1.415(6) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ir1 C1 91.77(13) . . ? C2 Ir1 C24 90.09(12) . . ? C1 Ir1 C24 175.22(13) . . ? C2 Ir1 N3 93.13(12) . . ? C1 Ir1 N3 91.13(12) . . ? C24 Ir1 N3 93.17(12) . . ? C2 Ir1 C13 173.13(13) . . ? C1 Ir1 C13 89.43(13) . . ? C24 Ir1 C13 89.25(12) . . ? N3 Ir1 C13 80.08(12) . . ? C2 Ir1 N4 94.22(11) . . ? C1 Ir1 N4 95.65(12) . . ? C24 Ir1 N4 79.81(12) . . ? N3 Ir1 N4 169.83(11) . . ? C13 Ir1 N4 92.39(12) . . ? C25 Ir2 C26 89.52(12) . . ? C25 Ir2 C37 175.37(12) . . ? C26 Ir2 C37 91.78(12) . . ? C25 Ir2 C48 90.40(12) . . ? C26 Ir2 C48 174.92(13) . . ? C37 Ir2 C48 88.70(12) . . ? C25 Ir2 N7 95.75(12) . . ? C26 Ir2 N7 89.32(12) . . ? C37 Ir2 N7 79.83(12) . . ? C48 Ir2 N7 95.74(12) . . ? C25 Ir2 N8 90.42(12) . . ? C26 Ir2 N8 95.27(12) . . ? C37 Ir2 N8 93.88(12) . . ? C48 Ir2 N8 79.66(12) . . ? N7 Ir2 N8 172.34(11) . . ? O9S La1 O10X 63.7(3) . . ? O9S La1 O5S 141.51(10) . . ? O10X La1 O5S 142.5(2) . . ? O9S La1 O3X 91.17(16) . . ? O10X La1 O3X 141.7(3) . . ? O5S La1 O3X 75.00(14) . . ? O9S La1 O3Y 100.44(18) . . ? O10X La1 O3Y 145.0(3) . . ? O5S La1 O3Y 69.42(16) . . ? O3X La1 O3Y 9.71(17) . . ? O9S La1 O6S 138.99(9) . . ? O10X La1 O6S 101.0(3) . . ? O5S La1 O6S 74.19(9) . . ? O3X La1 O6S 78.80(15) . . ? O3Y La1 O6S 69.88(17) . . ? O9S La1 O7S 133.09(11) . . ? O10X La1 O7S 74.0(2) . . ? O5S La1 O7S 70.09(8) . . ? O3X La1 O7S 135.69(14) . . ? O3Y La1 O7S 126.26(17) . . ? O6S La1 O7S 66.19(8) . . ? O9S La1 N2 82.03(10) . . ? O10X La1 N2 76.1(3) . . ? O5S La1 N2 81.06(9) . . ? O3X La1 N2 131.40(14) . . ? O3Y La1 N2 135.16(16) . . ? O6S La1 N2 133.58(9) . . ? O7S La1 N2 68.65(9) . . ? O9S La1 O10Y 71.17(13) . . ? O10X La1 O10Y 9.3(3) . . ? O5S La1 O10Y 139.27(11) . . ? O3X La1 O10Y 140.47(15) . . ? O3Y La1 O10Y 141.41(16) . . ? O6S La1 O10Y 91.62(12) . . ? O7S La1 O10Y 69.26(11) . . ? N2 La1 O10Y 82.18(11) . . ? O9S La1 N5 71.32(9) . . ? O10X La1 N5 71.7(2) . . ? O5S La1 N5 133.89(9) . . ? O3X La1 N5 73.01(13) . . ? O3Y La1 N5 73.71(15) . . ? O6S La1 N5 67.71(8) . . ? O7S La1 N5 114.21(9) . . ? N2 La1 N5 144.81(9) . . ? O10Y La1 N5 67.90(11) . . ? O9S La1 O2X 65.21(11) . . ? O10X La1 O2X 121.1(3) . . ? O5S La1 O2X 76.53(10) . . ? O3X La1 O2X 63.91(15) . . ? O3Y La1 O2X 71.04(17) . . ? O6S La1 O2X 137.27(10) . . ? O7S La1 O2X 129.58(9) . . ? N2 La1 O2X 69.72(10) . . ? O10Y La1 O2X 130.37(13) . . ? N5 La1 O2X 116.19(10) . . ? O9S La1 O2Y 79.0(3) . . ? O10X La1 O2Y 135.4(4) . . ? O5S La1 O2Y 63.4(3) . . ? O3X La1 O2Y 56.2(3) . . ? O3Y La1 O2Y 61.6(3) . . ? O6S La1 O2Y 123.6(3) . . ? O7S La1 O2Y 124.3(3) . . ? N2 La1 O2Y 75.3(3) . . ? O10Y La1 O2Y 144.7(3) . . ? N5 La1 O2Y 119.7(3) . . ? O2X La1 O2Y 14.6(3) . . ? N1 C1 Ir1 178.6(3) . . ? N2 C2 Ir1 173.2(3) . . ? N3 C3 C4 122.4(3) . . ? N3 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 118.6(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? N3 C7 C6 119.3(3) . . ? N3 C7 C8 114.9(3) . . ? C6 C7 C8 125.8(3) . . ? C9 C8 C13 121.8(3) . . ? C9 C8 C7 122.8(3) . . ? C13 C8 C7 115.4(3) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.4(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 117.0(3) . . ? C12 C13 Ir1 129.3(2) . . ? C8 C13 Ir1 113.6(2) . . ? N4 C14 C15 122.2(3) . . ? N4 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 119.0(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? N4 C18 C17 119.9(3) . . ? N4 C18 C19 114.2(3) . . ? C17 C18 C19 125.8(3) . . ? C20 C19 C24 121.4(3) . . ? C20 C19 C18 123.3(3) . . ? C24 C19 C18 115.3(3) . . ? C21 C20 C19 119.3(4) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.8(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 121.3(4) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 117.2(3) . . ? C23 C24 Ir1 128.6(3) . . ? C19 C24 Ir1 114.2(2) . . ? N5 C25 Ir2 177.7(3) . . ? N6 C26 Ir2 177.8(3) . . ? N7 C27 C28 121.9(4) . . ? N7 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 119.0(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 119.7(4) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? N7 C31 C30 120.6(3) . . ? N7 C31 C32 114.5(3) . . ? C30 C31 C32 124.9(3) . . ? C33 C32 C37 121.5(3) . . ? C33 C32 C31 123.5(3) . . ? C37 C32 C31 115.0(3) . . ? C34 C33 C32 119.9(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 121.7(3) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C32 116.8(3) . . ? C36 C37 Ir2 129.1(2) . . ? C32 C37 Ir2 114.1(2) . . ? N8 C38 C39 122.2(3) . . ? N8 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C40 C39 C38 119.0(3) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 119.6(3) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C40 C41 C42 119.7(4) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? N8 C42 C41 120.2(3) . . ? N8 C42 C43 114.4(3) . . ? C41 C42 C43 125.5(3) . . ? C44 C43 C48 121.6(3) . . ? C44 C43 C42 123.2(3) . . ? C48 C43 C42 115.2(3) . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 119.5(4) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 120.9(4) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 116.9(3) . . ? C47 C48 Ir2 128.8(3) . . ? C43 C48 Ir2 114.3(2) . . ? O4S C4S H4S1 109.5 . . ? O4S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? O4S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O2Y C2Y H2Y1 109.5 . . ? O2Y C2Y H2Y2 109.5 . . ? H2Y1 C2Y H2Y2 109.5 . . ? O2Y C2Y H2Y3 109.5 . . ? H2Y1 C2Y H2Y3 109.5 . . ? H2Y2 C2Y H2Y3 109.5 . . ? O3Y C3Y H3Y1 109.5 . . ? O3Y C3Y H3Y2 109.5 . . ? H3Y1 C3Y H3Y2 109.5 . . ? O3Y C3Y H3Y3 109.5 . . ? H3Y1 C3Y H3Y3 109.5 . . ? H3Y2 C3Y H3Y3 109.5 . . ? O8S C8S H6S1 109.5 . . ? O8S C8S H6S2 109.5 . . ? H6S1 C8S H6S2 109.5 . . ? O8S C8S H6S3 109.5 . . ? H6S1 C8S H6S3 109.5 . . ? H6S2 C8S H6S3 109.5 . . ? O10Y C10Y H10D 109.5 . . ? O10Y C10Y H10E 109.5 . . ? H10D C10Y H10E 109.5 . . ? O10Y C10Y H10F 109.5 . . ? H10D C10Y H10F 109.5 . . ? H10E C10Y H10F 109.5 . . ? C2 N2 La1 163.5(3) . . ? C3 N3 C7 119.7(3) . . ? C3 N3 Ir1 124.4(2) . . ? C7 N3 Ir1 115.9(2) . . ? C14 N4 C18 119.5(3) . . ? C14 N4 Ir1 124.1(2) . . ? C18 N4 Ir1 116.2(2) . . ? C25 N5 La1 149.4(2) . . ? C27 N7 C31 119.2(3) . . ? C27 N7 Ir2 124.1(2) . . ? C31 N7 Ir2 116.6(2) . . ? C38 N8 C42 119.3(3) . . ? C38 N8 Ir2 124.2(2) . . ? C42 N8 Ir2 116.4(2) . . ? C2X O2X La1 132.4(3) . . ? C2Y O2Y La1 132.7(13) . . ? C3X O3X La1 142.2(6) . . ? C3Y O3Y La1 141.8(5) . . ? C10X O10X La1 131.9(8) . . ? C10Y O10Y La1 131.9(4) . . ? O11S C11S H11A 109.5 . . ? O11S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? O11S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 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 C2 Ir1 C1 N1 140(13) . . . . ? C24 Ir1 C1 N1 28(14) . . . . ? N3 Ir1 C1 N1 -127(13) . . . . ? C13 Ir1 C1 N1 -46(13) . . . . ? N4 Ir1 C1 N1 46(13) . . . . ? C1 Ir1 C2 N2 96(3) . . . . ? C24 Ir1 C2 N2 -88(3) . . . . ? N3 Ir1 C2 N2 5(3) . . . . ? C13 Ir1 C2 N2 -4(3) . . . . ? N4 Ir1 C2 N2 -168(3) . . . . ? N3 C3 C4 C5 -1.5(6) . . . . ? C3 C4 C5 C6 -0.7(6) . . . . ? C4 C5 C6 C7 2.0(6) . . . . ? C5 C6 C7 N3 -1.3(5) . . . . ? C5 C6 C7 C8 178.2(4) . . . . ? N3 C7 C8 C9 -178.0(3) . . . . ? C6 C7 C8 C9 2.5(6) . . . . ? N3 C7 C8 C13 1.2(4) . . . . ? C6 C7 C8 C13 -178.3(3) . . . . ? C13 C8 C9 C10 -0.3(6) . . . . ? C7 C8 C9 C10 178.8(4) . . . . ? C8 C9 C10 C11 -1.2(7) . . . . ? C9 C10 C11 C12 1.7(7) . . . . ? C10 C11 C12 C13 -0.8(6) . . . . ? C11 C12 C13 C8 -0.6(5) . . . . ? C11 C12 C13 Ir1 179.6(3) . . . . ? C9 C8 C13 C12 1.2(5) . . . . ? C7 C8 C13 C12 -178.0(3) . . . . ? C9 C8 C13 Ir1 -178.9(3) . . . . ? C7 C8 C13 Ir1 1.9(4) . . . . ? C2 Ir1 C13 C12 -174.3(9) . . . . ? C1 Ir1 C13 C12 85.6(3) . . . . ? C24 Ir1 C13 C12 -89.8(3) . . . . ? N3 Ir1 C13 C12 176.9(3) . . . . ? N4 Ir1 C13 C12 -10.0(3) . . . . ? C2 Ir1 C13 C8 5.9(12) . . . . ? C1 Ir1 C13 C8 -94.2(3) . . . . ? C24 Ir1 C13 C8 90.4(3) . . . . ? N3 Ir1 C13 C8 -2.9(2) . . . . ? N4 Ir1 C13 C8 170.2(2) . . . . ? N4 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 -1.0(6) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C16 C17 C18 N4 1.4(5) . . . . ? C16 C17 C18 C19 178.9(3) . . . . ? N4 C18 C19 C20 -177.2(3) . . . . ? C17 C18 C19 C20 5.1(5) . . . . ? N4 C18 C19 C24 3.6(4) . . . . ? C17 C18 C19 C24 -174.1(3) . . . . ? C24 C19 C20 C21 0.9(5) . . . . ? C18 C19 C20 C21 -178.3(3) . . . . ? C19 C20 C21 C22 0.1(6) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C22 C23 C24 C19 0.6(5) . . . . ? C22 C23 C24 Ir1 179.5(3) . . . . ? C20 C19 C24 C23 -1.2(5) . . . . ? C18 C19 C24 C23 178.1(3) . . . . ? C20 C19 C24 Ir1 179.7(3) . . . . ? C18 C19 C24 Ir1 -1.0(4) . . . . ? C2 Ir1 C24 C23 85.8(3) . . . . ? C1 Ir1 C24 C23 -161.4(13) . . . . ? N3 Ir1 C24 C23 -7.3(3) . . . . ? C13 Ir1 C24 C23 -87.4(3) . . . . ? N4 Ir1 C24 C23 -179.9(3) . . . . ? C2 Ir1 C24 C19 -95.3(2) . . . . ? C1 Ir1 C24 C19 17.6(15) . . . . ? N3 Ir1 C24 C19 171.6(2) . . . . ? C13 Ir1 C24 C19 91.6(2) . . . . ? N4 Ir1 C24 C19 -1.0(2) . . . . ? C26 Ir2 C25 N5 -6(7) . . . . ? C37 Ir2 C25 N5 -112(7) . . . . ? C48 Ir2 C25 N5 169(7) . . . . ? N7 Ir2 C25 N5 -95(7) . . . . ? N8 Ir2 C25 N5 90(7) . . . . ? C25 Ir2 C26 N6 40(8) . . . . ? C37 Ir2 C26 N6 -145(8) . . . . ? C48 Ir2 C26 N6 -49(8) . . . . ? N7 Ir2 C26 N6 136(8) . . . . ? N8 Ir2 C26 N6 -50(8) . . . . ? N7 C27 C28 C29 -0.3(7) . . . . ? C27 C28 C29 C30 1.5(7) . . . . ? C28 C29 C30 C31 -1.6(7) . . . . ? C29 C30 C31 N7 0.3(6) . . . . ? C29 C30 C31 C32 -178.6(4) . . . . ? N7 C31 C32 C33 176.5(3) . . . . ? C30 C31 C32 C33 -4.5(6) . . . . ? N7 C31 C32 C37 -3.4(4) . . . . ? C30 C31 C32 C37 175.6(3) . . . . ? C37 C32 C33 C34 -0.4(5) . . . . ? C31 C32 C33 C34 179.7(3) . . . . ? C32 C33 C34 C35 -0.8(6) . . . . ? C33 C34 C35 C36 0.6(6) . . . . ? C34 C35 C36 C37 0.7(6) . . . . ? C35 C36 C37 C32 -1.8(5) . . . . ? C35 C36 C37 Ir2 177.1(3) . . . . ? C33 C32 C37 C36 1.7(5) . . . . ? C31 C32 C37 C36 -178.4(3) . . . . ? C33 C32 C37 Ir2 -177.4(3) . . . . ? C31 C32 C37 Ir2 2.5(4) . . . . ? C25 Ir2 C37 C36 -162.4(14) . . . . ? C26 Ir2 C37 C36 91.3(3) . . . . ? C48 Ir2 C37 C36 -83.7(3) . . . . ? N7 Ir2 C37 C36 -179.8(3) . . . . ? N8 Ir2 C37 C36 -4.2(3) . . . . ? C25 Ir2 C37 C32 16.5(16) . . . . ? C26 Ir2 C37 C32 -89.8(2) . . . . ? C48 Ir2 C37 C32 95.2(2) . . . . ? N7 Ir2 C37 C32 -0.8(2) . . . . ? N8 Ir2 C37 C32 174.8(2) . . . . ? N8 C38 C39 C40 1.0(6) . . . . ? C38 C39 C40 C41 -0.8(6) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C40 C41 C42 N8 1.2(5) . . . . ? C40 C41 C42 C43 -178.9(3) . . . . ? N8 C42 C43 C44 -177.2(3) . . . . ? C41 C42 C43 C44 2.8(6) . . . . ? N8 C42 C43 C48 2.6(4) . . . . ? C41 C42 C43 C48 -177.4(3) . . . . ? C48 C43 C44 C45 0.4(6) . . . . ? C42 C43 C44 C45 -179.8(4) . . . . ? C43 C44 C45 C46 0.6(6) . . . . ? C44 C45 C46 C47 -1.1(7) . . . . ? C45 C46 C47 C48 0.6(6) . . . . ? C46 C47 C48 C43 0.4(5) . . . . ? C46 C47 C48 Ir2 -178.5(3) . . . . ? C44 C43 C48 C47 -0.9(5) . . . . ? C42 C43 C48 C47 179.3(3) . . . . ? C44 C43 C48 Ir2 178.2(3) . . . . ? C42 C43 C48 Ir2 -1.6(4) . . . . ? C25 Ir2 C48 C47 88.9(3) . . . . ? C26 Ir2 C48 C47 178(10) . . . . ? C37 Ir2 C48 C47 -86.5(3) . . . . ? N7 Ir2 C48 C47 -6.9(3) . . . . ? N8 Ir2 C48 C47 179.3(3) . . . . ? C25 Ir2 C48 C43 -90.0(3) . . . . ? C26 Ir2 C48 C43 -1.0(15) . . . . ? C37 Ir2 C48 C43 94.5(3) . . . . ? N7 Ir2 C48 C43 174.2(2) . . . . ? N8 Ir2 C48 C43 0.3(2) . . . . ? Ir1 C2 N2 La1 -60(3) . . . . ? O9S La1 N2 C2 28.3(9) . . . . ? O10X La1 N2 C2 93.0(10) . . . . ? O5S La1 N2 C2 -117.0(9) . . . . ? O3X La1 N2 C2 -56.2(10) . . . . ? O3Y La1 N2 C2 -68.5(10) . . . . ? O6S La1 N2 C2 -175.0(9) . . . . ? O7S La1 N2 C2 171.0(10) . . . . ? O10Y La1 N2 C2 100.2(9) . . . . ? N5 La1 N2 C2 68.8(10) . . . . ? O2X La1 N2 C2 -38.2(9) . . . . ? O2Y La1 N2 C2 -52.4(10) . . . . ? C4 C3 N3 C7 2.2(5) . . . . ? C4 C3 N3 Ir1 -174.1(3) . . . . ? C6 C7 N3 C3 -0.9(5) . . . . ? C8 C7 N3 C3 179.6(3) . . . . ? C6 C7 N3 Ir1 175.8(3) . . . . ? C8 C7 N3 Ir1 -3.7(4) . . . . ? C2 Ir1 N3 C3 1.2(3) . . . . ? C1 Ir1 N3 C3 -90.6(3) . . . . ? C24 Ir1 N3 C3 91.5(3) . . . . ? C13 Ir1 N3 C3 -179.9(3) . . . . ? N4 Ir1 N3 C3 137.4(6) . . . . ? C2 Ir1 N3 C7 -175.3(2) . . . . ? C1 Ir1 N3 C7 92.9(2) . . . . ? C24 Ir1 N3 C7 -85.0(2) . . . . ? C13 Ir1 N3 C7 3.7(2) . . . . ? N4 Ir1 N3 C7 -39.0(7) . . . . ? C15 C14 N4 C18 1.4(5) . . . . ? C15 C14 N4 Ir1 -173.8(3) . . . . ? C17 C18 N4 C14 -2.2(5) . . . . ? C19 C18 N4 C14 -180.0(3) . . . . ? C17 C18 N4 Ir1 173.4(2) . . . . ? C19 C18 N4 Ir1 -4.4(3) . . . . ? C2 Ir1 N4 C14 -92.3(3) . . . . ? C1 Ir1 N4 C14 -0.1(3) . . . . ? C24 Ir1 N4 C14 178.4(3) . . . . ? N3 Ir1 N4 C14 131.5(6) . . . . ? C13 Ir1 N4 C14 89.6(3) . . . . ? C2 Ir1 N4 C18 92.4(2) . . . . ? C1 Ir1 N4 C18 -175.4(2) . . . . ? C24 Ir1 N4 C18 3.1(2) . . . . ? N3 Ir1 N4 C18 -43.8(7) . . . . ? C13 Ir1 N4 C18 -85.8(2) . . . . ? Ir2 C25 N5 La1 -4(7) . . . . ? O9S La1 N5 C25 176.5(5) . . . . ? O10X La1 N5 C25 108.9(6) . . . . ? O5S La1 N5 C25 -38.3(5) . . . . ? O3X La1 N5 C25 -86.3(5) . . . . ? O3Y La1 N5 C25 -76.2(5) . . . . ? O6S La1 N5 C25 -1.7(5) . . . . ? O7S La1 N5 C25 46.8(5) . . . . ? N2 La1 N5 C25 133.6(5) . . . . ? O10Y La1 N5 C25 99.8(5) . . . . ? O2X La1 N5 C25 -134.8(5) . . . . ? O2Y La1 N5 C25 -118.7(6) . . . . ? C28 C27 N7 C31 -1.0(6) . . . . ? C28 C27 N7 Ir2 176.0(3) . . . . ? C30 C31 N7 C27 0.9(5) . . . . ? C32 C31 N7 C27 179.9(3) . . . . ? C30 C31 N7 Ir2 -176.3(3) . . . . ? C32 C31 N7 Ir2 2.7(4) . . . . ? C25 Ir2 N7 C27 3.2(3) . . . . ? C26 Ir2 N7 C27 -86.2(3) . . . . ? C37 Ir2 N7 C27 -178.2(3) . . . . ? C48 Ir2 N7 C27 94.2(3) . . . . ? N8 Ir2 N7 C27 146.8(7) . . . . ? C25 Ir2 N7 C31 -179.7(2) . . . . ? C26 Ir2 N7 C31 90.8(2) . . . . ? C37 Ir2 N7 C31 -1.1(2) . . . . ? C48 Ir2 N7 C31 -88.7(2) . . . . ? N8 Ir2 N7 C31 -36.1(9) . . . . ? C39 C38 N8 C42 -0.1(5) . . . . ? C39 C38 N8 Ir2 -178.6(3) . . . . ? C41 C42 N8 C38 -1.0(5) . . . . ? C43 C42 N8 C38 179.0(3) . . . . ? C41 C42 N8 Ir2 177.6(3) . . . . ? C43 C42 N8 Ir2 -2.3(4) . . . . ? C25 Ir2 N8 C38 -90.0(3) . . . . ? C26 Ir2 N8 C38 -0.4(3) . . . . ? C37 Ir2 N8 C38 91.7(3) . . . . ? C48 Ir2 N8 C38 179.7(3) . . . . ? N7 Ir2 N8 C38 126.2(7) . . . . ? C25 Ir2 N8 C42 91.5(2) . . . . ? C26 Ir2 N8 C42 -179.0(2) . . . . ? C37 Ir2 N8 C42 -86.8(2) . . . . ? C48 Ir2 N8 C42 1.1(2) . . . . ? N7 Ir2 N8 C42 -52.3(9) . . . . ? O9S La1 O2X C2X -142.5(5) . . . . ? O10X La1 O2X C2X -110.6(5) . . . . ? O5S La1 O2X C2X 33.2(4) . . . . ? O3X La1 O2X C2X 112.9(5) . . . . ? O3Y La1 O2X C2X 105.8(5) . . . . ? O6S La1 O2X C2X 81.0(5) . . . . ? O7S La1 O2X C2X -16.1(5) . . . . ? N2 La1 O2X C2X -52.1(4) . . . . ? O10Y La1 O2X C2X -111.8(4) . . . . ? N5 La1 O2X C2X 165.8(4) . . . . ? O2Y La1 O2X C2X 58.1(12) . . . . ? O9S La1 O2Y C2Y -65.3(18) . . . . ? O10X La1 O2Y C2Y -32.5(19) . . . . ? O5S La1 O2Y C2Y 106.5(18) . . . . ? O3X La1 O2Y C2Y -164.2(19) . . . . ? O3Y La1 O2Y C2Y -173.6(19) . . . . ? O6S La1 O2Y C2Y 152.2(17) . . . . ? O7S La1 O2Y C2Y 69.9(18) . . . . ? N2 La1 O2Y C2Y 19.3(17) . . . . ? O10Y La1 O2Y C2Y -33(2) . . . . ? N5 La1 O2Y C2Y -126.1(17) . . . . ? O2X La1 O2Y C2Y -46.3(17) . . . . ? O9S La1 O3X C3X 43.0(11) . . . . ? O10X La1 O3X C3X -3.4(13) . . . . ? O5S La1 O3X C3X -173.4(11) . . . . ? O3Y La1 O3X C3X -119.7(19) . . . . ? O6S La1 O3X C3X -96.9(11) . . . . ? O7S La1 O3X C3X -134.6(11) . . . . ? N2 La1 O3X C3X 123.4(11) . . . . ? O10Y La1 O3X C3X -18.2(12) . . . . ? N5 La1 O3X C3X -27.0(11) . . . . ? O2X La1 O3X C3X 104.5(11) . . . . ? O2Y La1 O3X C3X 118.9(12) . . . . ? O9S La1 O3Y C3Y 75.1(9) . . . . ? O10X La1 O3Y C3Y 16.7(12) . . . . ? O5S La1 O3Y C3Y -143.5(9) . . . . ? O3X La1 O3Y C3Y 92.7(16) . . . . ? O6S La1 O3Y C3Y -63.4(9) . . . . ? O7S La1 O3Y C3Y -100.1(9) . . . . ? N2 La1 O3Y C3Y 164.3(8) . . . . ? O10Y La1 O3Y C3Y 2.3(11) . . . . ? N5 La1 O3Y C3Y 8.3(8) . . . . ? O2X La1 O3Y C3Y 134.2(9) . . . . ? O2Y La1 O3Y C3Y 146.5(10) . . . . ? O9S La1 O10X C10X 120.9(16) . . . . ? O5S La1 O10X C10X -21.3(17) . . . . ? O3X La1 O10X C10X 174.7(14) . . . . ? O3Y La1 O10X C10X -170.0(14) . . . . ? O6S La1 O10X C10X -99.5(15) . . . . ? O7S La1 O10X C10X -38.4(15) . . . . ? N2 La1 O10X C10X 33.0(15) . . . . ? O10Y La1 O10X C10X -97(2) . . . . ? N5 La1 O10X C10X -161.4(16) . . . . ? O2X La1 O10X C10X 88.5(15) . . . . ? O2Y La1 O10X C10X 84.5(16) . . . . ? O9S La1 O10Y C10Y 99.8(5) . . . . ? O10X La1 O10Y C10Y 64.4(18) . . . . ? O5S La1 O10Y C10Y -50.8(6) . . . . ? O3X La1 O10Y C10Y 167.5(5) . . . . ? O3Y La1 O10Y C10Y -177.1(5) . . . . ? O6S La1 O10Y C10Y -118.2(5) . . . . ? O7S La1 O10Y C10Y -54.4(5) . . . . ? N2 La1 O10Y C10Y 15.6(5) . . . . ? N5 La1 O10Y C10Y 176.7(6) . . . . ? O2X La1 O10Y C10Y 70.5(6) . . . . ? O2Y La1 O10Y C10Y 66.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.263 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.123 #===END data_imw1496_0m _database_code_depnum_ccdc_archive 'CCDC 834580' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H67 Cl Gd Ir2 N8 O9.50' _chemical_formula_weight 1581.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2299(2) _cell_length_b 16.4704(4) _cell_length_c 20.0201(5) _cell_angle_alpha 86.093(2) _cell_angle_beta 88.2430(10) _cell_angle_gamma 76.4510(10) _cell_volume 2951.54(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9044 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.57 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 5.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2790 _exptl_absorpt_correction_T_max 0.6273 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45226 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13393 _reflns_number_gt 9816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+21.6070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13393 _refine_ls_number_parameters 704 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.03681(3) 0.287480(19) 0.370447(16) 0.02105(9) Uani 1 1 d . . . Ir2 Ir 0.36628(4) -0.299577(19) 0.132376(16) 0.02317(9) Uani 1 1 d . A . Gd1 Gd 0.35368(5) 0.00104(2) 0.24981(2) 0.02671(11) Uani 1 1 d . . . C1 C 0.3198(9) 0.3512(5) 0.3550(5) 0.0260(18) Uani 1 1 d . . . H25 H 0.3370 0.3297 0.4000 0.031 Uiso 1 1 calc R . . C2 C 0.4213(10) 0.3890(5) 0.3237(5) 0.032(2) Uani 1 1 d . . . H26 H 0.5088 0.3926 0.3459 0.038 Uiso 1 1 calc R . . C3 C 0.3945(10) 0.4225(5) 0.2582(5) 0.032(2) Uani 1 1 d . . . H27 H 0.4636 0.4495 0.2353 0.039 Uiso 1 1 calc R . . C4 C 0.2666(10) 0.4161(5) 0.2267(5) 0.034(2) Uani 1 1 d . . . H28 H 0.2464 0.4399 0.1824 0.040 Uiso 1 1 calc R . . C5 C 0.1670(9) 0.3744(5) 0.2605(4) 0.0253(18) Uani 1 1 d . . . C6 C 0.0293(9) 0.3613(5) 0.2336(4) 0.0279(19) Uani 1 1 d . . . C7 C -0.0125(10) 0.3856(6) 0.1670(5) 0.034(2) Uani 1 1 d . . . H31 H 0.0495 0.4099 0.1370 0.041 Uiso 1 1 calc R . . C8 C -0.1473(11) 0.3729(6) 0.1464(5) 0.036(2) Uani 1 1 d . . . H32 H -0.1782 0.3892 0.1017 0.043 Uiso 1 1 calc R . . C9 C -0.2376(10) 0.3371(6) 0.1896(5) 0.035(2) Uani 1 1 d . . . H33 H -0.3300 0.3294 0.1748 0.042 Uiso 1 1 calc R . . C10 C -0.1922(9) 0.3125(5) 0.2546(4) 0.0291(19) Uani 1 1 d . . . H34 H -0.2545 0.2871 0.2837 0.035 Uiso 1 1 calc R . . C11 C -0.0593(9) 0.3234(5) 0.2791(4) 0.0265(19) Uani 1 1 d . . . C12 C -0.0795(9) 0.3973(5) 0.4092(4) 0.0250(18) Uani 1 1 d . . . C13 C -0.0419(9) 0.4739(5) 0.4076(4) 0.0258(18) Uani 1 1 d . . . H37 H 0.0473 0.4804 0.3851 0.031 Uiso 1 1 calc R . . C14 C -0.1312(11) 0.5415(6) 0.4380(5) 0.037(2) Uani 1 1 d . . . H48 H -0.1037 0.5937 0.4362 0.044 Uiso 1 1 calc R . . C15 C -0.2604(11) 0.5322(6) 0.4707(5) 0.042(3) Uani 1 1 d . . . H47 H -0.3215 0.5784 0.4917 0.051 Uiso 1 1 calc R . . C16 C -0.3026(10) 0.4573(6) 0.4735(5) 0.038(2) Uani 1 1 d . . . H40 H -0.3926 0.4519 0.4958 0.045 Uiso 1 1 calc R . . C17 C -0.2109(9) 0.3890(5) 0.4431(4) 0.0278(19) Uani 1 1 d . . . C18 C -0.2450(10) 0.3067(5) 0.4439(4) 0.030(2) Uani 1 1 d . . . C19 C -0.3718(11) 0.2841(7) 0.4749(5) 0.042(2) Uani 1 1 d . . . H42 H -0.4404 0.3233 0.4999 0.051 Uiso 1 1 calc R . . C20 C -0.3952(12) 0.2065(7) 0.4688(6) 0.051(3) Uani 1 1 d . . . H43 H -0.4796 0.1909 0.4895 0.062 Uiso 1 1 calc R . . C21 C -0.2948(11) 0.1510(6) 0.4322(6) 0.045(3) Uani 1 1 d . . . H44 H -0.3111 0.0971 0.4262 0.053 Uiso 1 1 calc R . . C22 C -0.1723(10) 0.1731(6) 0.4047(5) 0.034(2) Uani 1 1 d . . . H45 H -0.1030 0.1334 0.3803 0.041 Uiso 1 1 calc R . . C23 C 0.1464(9) 0.2549(5) 0.4595(4) 0.0263(19) Uani 1 1 d . . . C24 C 0.1434(9) 0.1752(5) 0.3347(4) 0.0249(18) Uani 1 1 d . . . C25 C 0.3569(9) -0.1887(5) 0.1729(4) 0.0283(19) Uani 1 1 d . . . C26 C 0.4624(9) -0.2612(5) 0.0466(5) 0.0252(19) Uani 1 1 d . . . C27 C 0.2821(10) -0.3369(5) 0.2230(4) 0.0288(19) Uani 1 1 d . . . C28 C 0.1355(11) -0.3245(6) 0.2458(5) 0.037(2) Uani 1 1 d . . . H2 H 0.0575 -0.2997 0.2158 0.044 Uiso 1 1 calc R . . C29 C 0.1003(11) -0.3468(6) 0.3095(5) 0.038(2) Uani 1 1 d . . . H3 H -0.0015 -0.3387 0.3228 0.045 Uiso 1 1 calc R A . C30 C 0.2104(12) -0.3814(6) 0.3555(5) 0.039(2) Uani 1 1 d . . . H4 H 0.1840 -0.3949 0.4004 0.046 Uiso 1 1 calc R . . C31 C 0.3578(11) -0.3959(6) 0.3360(5) 0.035(2) Uani 1 1 d . . . H5 H 0.4337 -0.4202 0.3672 0.042 Uiso 1 1 calc R A . C32 C 0.3958(10) -0.3745(5) 0.2696(4) 0.028(2) Uani 1 1 d . . . C33 C 0.5489(10) -0.3878(5) 0.2447(4) 0.0269(19) Uani 1 1 d . . . C34 C 0.6769(10) -0.4326(5) 0.2777(4) 0.031(2) Uani 1 1 d . . . H8 H 0.6684 -0.4590 0.3208 0.037 Uiso 1 1 calc R . . C35 C 0.8139(11) -0.4389(6) 0.2483(5) 0.037(2) Uani 1 1 d . . . H9 H 0.9009 -0.4684 0.2713 0.044 Uiso 1 1 calc R A . C36 C 0.8258(10) -0.4024(6) 0.1852(5) 0.035(2) Uani 1 1 d . . . H10 H 0.9208 -0.4066 0.1642 0.042 Uiso 1 1 calc R . . C37 C 0.6981(9) -0.3594(5) 0.1527(5) 0.030(2) Uani 1 1 d . . . H11 H 0.7063 -0.3341 0.1092 0.036 Uiso 1 1 calc R A . C38 C 0.3569(9) -0.4094(5) 0.0932(4) 0.0251(18) Uani 1 1 d . . . C39 C 0.4611(10) -0.4875(5) 0.0959(4) 0.0281(19) Uani 1 1 d . . . H22 H 0.5524 -0.4925 0.1183 0.034 Uiso 1 1 calc R . . C40 C 0.4358(11) -0.5566(5) 0.0674(4) 0.032(2) Uani 1 1 d . . . H21 H 0.5098 -0.6076 0.0694 0.039 Uiso 1 1 calc R A . C41 C 0.3040(12) -0.5516(6) 0.0360(5) 0.040(2) Uani 1 1 d . . . H20 H 0.2864 -0.5996 0.0169 0.048 Uiso 1 1 calc R . . C42 C 0.1960(11) -0.4773(6) 0.0317(5) 0.035(2) Uani 1 1 d . . . H19 H 0.1053 -0.4740 0.0094 0.043 Uiso 1 1 calc R A . C43 C 0.2221(10) -0.4072(6) 0.0607(4) 0.030(2) Uani 1 1 d . . . C44 C 0.1175(10) -0.3253(6) 0.0565(4) 0.031(2) Uani 1 1 d . . . C45 C -0.0196(10) -0.3061(7) 0.0234(5) 0.040(2) Uani 1 1 d . . . H15 H -0.0515 -0.3486 0.0022 0.047 Uiso 1 1 calc R . . C46 C -0.1074(11) -0.2264(7) 0.0215(5) 0.047(3) Uani 1 1 d . . . H14 H -0.2004 -0.2134 -0.0006 0.056 Uiso 1 1 calc R A . C47 C -0.0580(11) -0.1649(7) 0.0525(5) 0.046(3) Uani 1 1 d . . . H13 H -0.1152 -0.1088 0.0510 0.055 Uiso 1 1 calc R . . C48 C 0.0738(10) -0.1871(6) 0.0849(5) 0.039(2) Uani 1 1 d . . . H12 H 0.1048 -0.1453 0.1075 0.047 Uiso 1 1 calc R A . N1 N 0.1948(7) 0.3428(4) 0.3247(4) 0.0229(15) Uani 1 1 d . . . N2 N -0.1453(7) 0.2487(4) 0.4106(3) 0.0256(15) Uani 1 1 d . . . N3 N 0.2087(9) 0.2335(5) 0.5088(4) 0.042(2) Uani 1 1 d . . . N4 N 0.2068(8) 0.1139(5) 0.3134(4) 0.0352(18) Uani 1 1 d . . . N5 N 0.3489(8) -0.1267(4) 0.1984(4) 0.0329(18) Uani 1 1 d . . . N6 N 0.5172(9) -0.2357(5) -0.0011(4) 0.043(2) Uani 1 1 d . . . N7 N 0.5630(8) -0.3527(4) 0.1812(3) 0.0245(15) Uani 1 1 d . A . N8 N 0.1627(8) -0.2640(5) 0.0870(4) 0.0311(17) Uani 1 1 d . A . Cl1 Cl 0.8537(4) 0.0095(3) 0.2841(2) 0.1005(15) Uani 1 1 d . . . C1X C 0.523(2) 0.1663(10) 0.2765(9) 0.046(4) Uiso 0.61 1 d PDU A 1 H1X1 H 0.4309 0.2101 0.2785 0.068 Uiso 0.61 1 calc PR A 1 H1X2 H 0.6041 0.1909 0.2581 0.068 Uiso 0.61 1 calc PR A 1 H1X3 H 0.5487 0.1412 0.3216 0.068 Uiso 0.61 1 calc PR A 1 O1X O 0.5034(13) 0.1066(7) 0.2366(6) 0.043(3) Uiso 0.61 1 d PDU A 1 C1Y C 0.489(3) 0.1960(14) 0.2317(15) 0.049(4) Uiso 0.39 1 d PDU A 2 H1Y1 H 0.4830 0.2073 0.2793 0.073 Uiso 0.39 1 calc PR A 2 H1Y2 H 0.4210 0.2413 0.2064 0.073 Uiso 0.39 1 calc PR A 2 H1Y3 H 0.5915 0.1924 0.2151 0.073 Uiso 0.39 1 calc PR A 2 O1Y O 0.451(2) 0.1219(11) 0.2238(10) 0.041(3) Uiso 0.39 1 d PDU A 2 O2S O 0.1134(8) 0.0485(4) 0.1950(4) 0.052(2) Uani 1 1 d . A . C2S C 0.0669(15) 0.1366(8) 0.1679(7) 0.072(4) Uani 1 1 d . . . H54A H 0.0260 0.1725 0.2043 0.108 Uiso 1 1 calc R A . H54B H -0.0094 0.1412 0.1340 0.108 Uiso 1 1 calc R . . H54C H 0.1534 0.1543 0.1476 0.108 Uiso 1 1 calc R . . O3S O 0.4818(8) -0.0264(5) 0.3515(4) 0.0504(19) Uani 1 1 d . A . C3S C 0.4336(19) -0.0021(12) 0.4177(9) 0.108(6) Uani 1 1 d . . . H3S1 H 0.4237 0.0582 0.4198 0.162 Uiso 1 1 calc R A . H3S2 H 0.5071 -0.0325 0.4503 0.162 Uiso 1 1 calc R . . H3S3 H 0.3370 -0.0155 0.4280 0.162 Uiso 1 1 calc R . . O4S O 0.1960(8) -0.0645(4) 0.3235(4) 0.0489(19) Uani 1 1 d . A . C4S C 0.206(2) -0.1508(8) 0.3446(9) 0.111(7) Uani 1 1 d . . . H52A H 0.2925 -0.1860 0.3230 0.166 Uiso 1 1 calc R A . H52B H 0.1151 -0.1668 0.3320 0.166 Uiso 1 1 calc R . . H52C H 0.2166 -0.1583 0.3933 0.166 Uiso 1 1 calc R . . O5S O 0.6145(7) -0.0698(4) 0.2348(4) 0.0496(19) Uani 1 1 d . A . C5S C 0.6940(14) -0.1200(9) 0.1840(7) 0.074(4) Uani 1 1 d . . . H57A H 0.6852 -0.1779 0.1927 0.111 Uiso 1 1 calc R A . H57B H 0.7993 -0.1181 0.1843 0.111 Uiso 1 1 calc R . . H57C H 0.6521 -0.0983 0.1402 0.111 Uiso 1 1 calc R . . O6S O 0.3978(9) 0.0336(4) 0.1326(4) 0.0495(19) Uani 1 1 d . A . C6S C 0.3455(15) 0.0034(8) 0.0731(6) 0.064(3) Uani 1 1 d . . . H55A H 0.4131 -0.0495 0.0623 0.096 Uiso 1 1 calc R A . H55B H 0.3432 0.0449 0.0355 0.096 Uiso 1 1 calc R . . H55C H 0.2450 -0.0054 0.0817 0.096 Uiso 1 1 calc R . . O7S O 0.6516(12) 0.8243(5) 0.3762(5) 0.083(3) Uani 1 1 d . . . C7S C 0.6359(19) 0.7578(8) 0.3426(8) 0.092(5) Uani 1 1 d . . . H7S1 H 0.7323 0.7307 0.3229 0.138 Uiso 1 1 calc R . . H7S2 H 0.5632 0.7772 0.3069 0.138 Uiso 1 1 calc R . . H7S3 H 0.6011 0.7176 0.3737 0.138 Uiso 1 1 calc R . . O8S O 0.6167(11) 0.0882(7) 0.0738(5) 0.088(3) Uani 1 1 d . . . C8S C 0.7485(17) 0.1053(11) 0.0984(8) 0.092(5) Uani 1 1 d . . . H8S1 H 0.7397 0.1659 0.0956 0.138 Uiso 1 1 calc R . . H8S2 H 0.8343 0.0783 0.0713 0.138 Uiso 1 1 calc R . . H8S3 H 0.7624 0.0835 0.1451 0.138 Uiso 1 1 calc R . . O9X O 1.055(2) 0.9843(13) 0.4407(11) 0.090(6) Uiso 0.50 1 d P B 1 O9Y O 0.878(2) 0.9393(12) 0.4530(10) 0.084(6) Uiso 0.50 1 d P C 2 O10S O 0.3601(18) 0.2439(10) 0.1328(8) 0.062(4) Uiso 0.50 1 d P . . 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 0.01810(16) 0.02079(16) 0.02326(18) -0.00241(12) 0.00024(12) -0.00226(12) Ir2 0.02500(18) 0.02278(17) 0.02357(18) -0.00354(13) -0.00579(13) -0.00799(13) Gd1 0.0290(2) 0.0205(2) 0.0305(2) -0.00620(17) -0.00004(18) -0.00430(16) C1 0.025(4) 0.017(4) 0.034(5) -0.002(3) -0.001(4) -0.002(3) C2 0.024(5) 0.023(4) 0.050(6) -0.007(4) 0.003(4) -0.006(3) C3 0.029(5) 0.031(5) 0.043(6) -0.012(4) 0.011(4) -0.017(4) C4 0.036(5) 0.028(5) 0.036(5) -0.005(4) 0.007(4) -0.004(4) C5 0.027(5) 0.023(4) 0.027(5) -0.002(3) 0.008(4) -0.007(3) C6 0.026(5) 0.027(4) 0.030(5) -0.001(4) 0.003(4) -0.005(4) C7 0.034(5) 0.036(5) 0.033(5) 0.002(4) 0.001(4) -0.009(4) C8 0.037(5) 0.043(6) 0.023(5) 0.003(4) -0.004(4) -0.002(4) C9 0.027(5) 0.044(5) 0.035(5) -0.004(4) -0.008(4) -0.010(4) C10 0.023(4) 0.033(5) 0.031(5) -0.004(4) -0.002(4) -0.005(4) C11 0.025(4) 0.022(4) 0.032(5) -0.012(4) 0.004(4) -0.003(3) C12 0.024(4) 0.025(4) 0.025(4) -0.006(3) 0.000(3) -0.001(3) C13 0.022(4) 0.030(5) 0.020(4) -0.001(3) -0.004(3) 0.002(3) C14 0.044(6) 0.030(5) 0.032(5) -0.003(4) -0.013(4) 0.004(4) C15 0.042(6) 0.038(6) 0.035(6) -0.008(4) -0.005(5) 0.017(5) C16 0.027(5) 0.045(6) 0.033(5) -0.008(4) -0.001(4) 0.010(4) C17 0.017(4) 0.037(5) 0.024(5) -0.001(4) 0.002(3) 0.003(3) C18 0.027(5) 0.034(5) 0.023(5) 0.001(4) -0.002(4) 0.002(4) C19 0.027(5) 0.054(7) 0.038(6) 0.007(5) 0.007(4) 0.002(4) C20 0.031(6) 0.055(7) 0.063(8) 0.017(6) 0.004(5) -0.005(5) C21 0.035(6) 0.041(6) 0.059(7) 0.013(5) 0.002(5) -0.014(5) C22 0.026(5) 0.033(5) 0.045(6) 0.001(4) 0.011(4) -0.012(4) C23 0.026(5) 0.017(4) 0.034(5) -0.004(4) 0.004(4) -0.001(3) C24 0.023(4) 0.017(4) 0.034(5) -0.001(3) 0.001(4) -0.005(3) C25 0.026(5) 0.033(5) 0.027(5) -0.001(4) -0.004(4) -0.010(4) C26 0.026(5) 0.017(4) 0.035(5) -0.004(4) -0.013(4) -0.006(3) C27 0.032(5) 0.028(5) 0.029(5) -0.002(4) -0.004(4) -0.013(4) C28 0.035(5) 0.044(6) 0.035(6) 0.000(4) -0.007(4) -0.017(4) C29 0.035(5) 0.057(6) 0.029(5) -0.006(4) 0.004(4) -0.027(5) C30 0.052(6) 0.041(6) 0.025(5) 0.001(4) 0.002(4) -0.017(5) C31 0.045(6) 0.032(5) 0.028(5) -0.001(4) -0.011(4) -0.008(4) C32 0.041(5) 0.015(4) 0.031(5) -0.001(3) -0.007(4) -0.010(4) C33 0.036(5) 0.022(4) 0.023(4) -0.001(3) -0.012(4) -0.007(4) C34 0.043(6) 0.025(4) 0.026(5) -0.004(4) -0.011(4) -0.007(4) C35 0.038(6) 0.032(5) 0.037(6) -0.007(4) -0.018(4) 0.002(4) C36 0.025(5) 0.041(5) 0.037(6) -0.011(4) -0.009(4) -0.004(4) C37 0.024(5) 0.034(5) 0.035(5) -0.002(4) -0.006(4) -0.008(4) C38 0.026(4) 0.031(5) 0.021(4) -0.003(3) -0.001(3) -0.013(4) C39 0.033(5) 0.029(5) 0.027(5) -0.002(4) -0.001(4) -0.015(4) C40 0.043(6) 0.027(5) 0.030(5) -0.005(4) 0.001(4) -0.012(4) C41 0.059(7) 0.042(6) 0.030(5) -0.015(4) 0.010(5) -0.032(5) C42 0.040(6) 0.046(6) 0.030(5) -0.005(4) 0.000(4) -0.029(5) C43 0.034(5) 0.042(5) 0.020(4) -0.004(4) 0.001(4) -0.024(4) C44 0.027(5) 0.045(5) 0.022(5) 0.004(4) -0.003(4) -0.010(4) C45 0.032(5) 0.066(7) 0.023(5) -0.005(5) -0.005(4) -0.016(5) C46 0.028(5) 0.066(7) 0.044(6) -0.011(5) -0.009(5) -0.002(5) C47 0.034(6) 0.056(7) 0.040(6) -0.007(5) 0.002(5) 0.007(5) C48 0.030(5) 0.042(6) 0.043(6) -0.004(4) -0.009(4) -0.003(4) N1 0.017(3) 0.018(3) 0.035(4) -0.006(3) 0.001(3) -0.006(3) N2 0.018(4) 0.029(4) 0.027(4) 0.001(3) 0.001(3) 0.000(3) N3 0.042(5) 0.043(5) 0.040(5) 0.006(4) -0.016(4) -0.006(4) N4 0.027(4) 0.040(5) 0.040(5) -0.008(4) 0.000(3) -0.006(3) N5 0.035(4) 0.023(4) 0.041(5) -0.007(3) -0.005(4) -0.006(3) N6 0.040(5) 0.049(5) 0.039(5) 0.007(4) -0.001(4) -0.013(4) N7 0.025(4) 0.024(4) 0.025(4) -0.002(3) -0.008(3) -0.008(3) N8 0.024(4) 0.037(4) 0.030(4) -0.002(3) -0.005(3) -0.004(3) Cl1 0.067(2) 0.128(3) 0.130(4) -0.059(3) 0.028(2) -0.060(2) O2S 0.049(5) 0.045(4) 0.052(5) -0.005(3) -0.017(4) 0.009(3) C2S 0.058(8) 0.075(9) 0.074(9) -0.015(7) -0.012(7) 0.010(7) O3S 0.048(5) 0.070(5) 0.029(4) -0.010(4) -0.008(3) -0.003(4) C3S 0.082(12) 0.135(16) 0.113(15) 0.029(12) -0.031(11) -0.043(11) O4S 0.052(5) 0.035(4) 0.061(5) -0.011(3) 0.012(4) -0.011(3) C4S 0.166(17) 0.037(7) 0.123(14) -0.004(8) 0.084(13) -0.022(9) O5S 0.034(4) 0.056(5) 0.059(5) -0.031(4) 0.008(3) -0.002(3) C5S 0.054(8) 0.081(10) 0.087(10) -0.045(8) 0.021(7) -0.006(7) O6S 0.063(5) 0.046(4) 0.039(4) -0.004(3) 0.006(4) -0.014(4) C6S 0.069(9) 0.079(9) 0.043(7) 0.009(6) -0.004(6) -0.021(7) O7S 0.128(8) 0.041(5) 0.077(7) 0.001(4) -0.059(6) -0.007(5) C7S 0.124(14) 0.044(8) 0.104(12) -0.013(8) -0.038(11) -0.002(8) O8S 0.083(7) 0.121(8) 0.073(7) 0.021(6) -0.015(5) -0.057(6) C8S 0.081(11) 0.130(14) 0.078(11) 0.002(10) -0.026(9) -0.048(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C24 2.045(8) . ? Ir1 C11 2.046(9) . ? Ir1 C23 2.054(9) . ? Ir1 N1 2.055(7) . ? Ir1 N2 2.056(7) . ? Ir1 C12 2.063(8) . ? Ir2 C25 2.030(9) . ? Ir2 C26 2.040(10) . ? Ir2 C38 2.041(8) . ? Ir2 N8 2.053(7) . ? Ir2 C27 2.064(9) . ? Ir2 N7 2.065(6) . ? Gd1 O3S 2.349(7) . ? Gd1 O1Y 2.389(18) . ? Gd1 O6S 2.414(7) . ? Gd1 N5 2.415(7) . ? Gd1 O4S 2.418(7) . ? Gd1 O5S 2.436(6) . ? Gd1 N4 2.440(7) . ? Gd1 O2S 2.440(7) . ? Gd1 O1X 2.458(12) . ? C1 C2 1.357(12) . ? C1 N1 1.358(10) . ? C1 H25 0.9500 . ? C2 C3 1.392(13) . ? C2 H26 0.9500 . ? C3 C4 1.384(13) . ? C3 H27 0.9500 . ? C4 C5 1.404(12) . ? C4 H28 0.9500 . ? C5 N1 1.364(11) . ? C5 C6 1.462(12) . ? C6 C7 1.405(12) . ? C6 C11 1.417(12) . ? C7 C8 1.388(13) . ? C7 H31 0.9500 . ? C8 C9 1.381(13) . ? C8 H32 0.9500 . ? C9 C10 1.384(12) . ? C9 H33 0.9500 . ? C10 C11 1.389(11) . ? C10 H34 0.9500 . ? C12 C13 1.383(12) . ? C12 C17 1.402(12) . ? C13 C14 1.385(11) . ? C13 H37 0.9500 . ? C14 C15 1.378(15) . ? C14 H48 0.9500 . ? C15 C16 1.374(14) . ? C15 H47 0.9500 . ? C16 C17 1.404(11) . ? C16 H40 0.9500 . ? C17 C18 1.461(13) . ? C18 N2 1.356(10) . ? C18 C19 1.422(13) . ? C19 C20 1.359(15) . ? C19 H42 0.9500 . ? C20 C21 1.372(15) . ? C20 H43 0.9500 . ? C21 C22 1.358(13) . ? C21 H44 0.9500 . ? C22 N2 1.340(11) . ? C22 H45 0.9500 . ? C23 N3 1.149(11) . ? C24 N4 1.144(10) . ? C25 N5 1.159(11) . ? C26 N6 1.166(12) . ? C27 C28 1.388(13) . ? C27 C32 1.425(12) . ? C28 C29 1.354(13) . ? C28 H2 0.9500 . ? C29 C30 1.386(13) . ? C29 H3 0.9500 . ? C30 C31 1.375(14) . ? C30 H4 0.9500 . ? C31 C32 1.407(13) . ? C31 H5 0.9500 . ? C32 C33 1.456(13) . ? C33 N7 1.377(11) . ? C33 C34 1.396(11) . ? C34 C35 1.363(13) . ? C34 H8 0.9500 . ? C35 C36 1.374(14) . ? C35 H9 0.9500 . ? C36 C37 1.381(12) . ? C36 H10 0.9500 . ? C37 N7 1.338(11) . ? C37 H11 0.9500 . ? C38 C39 1.413(12) . ? C38 C43 1.413(11) . ? C39 C40 1.377(11) . ? C39 H22 0.9500 . ? C40 C41 1.369(13) . ? C40 H21 0.9500 . ? C41 C42 1.384(14) . ? C41 H20 0.9500 . ? C42 C43 1.400(12) . ? C42 H19 0.9500 . ? C43 C44 1.462(13) . ? C44 N8 1.365(11) . ? C44 C45 1.405(12) . ? C45 C46 1.369(14) . ? C45 H15 0.9500 . ? C46 C47 1.392(15) . ? C46 H14 0.9500 . ? C47 C48 1.357(13) . ? C47 H13 0.9500 . ? C48 N8 1.337(11) . ? C48 H12 0.9500 . ? C1X O1X 1.356(14) . ? C1X H1X1 0.9800 . ? C1X H1X2 0.9800 . ? C1X H1X3 0.9800 . ? C1Y O1Y 1.368(17) . ? C1Y H1Y1 0.9800 . ? C1Y H1Y2 0.9800 . ? C1Y H1Y3 0.9800 . ? O2S C2S 1.483(14) . ? C2S H54A 0.9800 . ? C2S H54B 0.9800 . ? C2S H54C 0.9800 . ? O3S C3S 1.437(19) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? O4S C4S 1.437(14) . ? C4S H52A 0.9800 . ? C4S H52B 0.9800 . ? C4S H52C 0.9800 . ? O5S C5S 1.427(12) . ? C5S H57A 0.9800 . ? C5S H57B 0.9800 . ? C5S H57C 0.9800 . ? O6S C6S 1.459(13) . ? C6S H55A 0.9800 . ? C6S H55B 0.9800 . ? C6S H55C 0.9800 . ? O7S C7S 1.362(14) . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? O8S C8S 1.420(15) . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Ir1 C11 89.6(3) . . ? C24 Ir1 C23 90.2(3) . . ? C11 Ir1 C23 175.8(4) . . ? C24 Ir1 N1 90.1(3) . . ? C11 Ir1 N1 80.1(3) . . ? C23 Ir1 N1 95.7(3) . . ? C24 Ir1 N2 96.5(3) . . ? C11 Ir1 N2 93.7(3) . . ? C23 Ir1 N2 90.5(3) . . ? N1 Ir1 N2 170.9(3) . . ? C24 Ir1 C12 176.7(3) . . ? C11 Ir1 C12 91.0(3) . . ? C23 Ir1 C12 89.4(3) . . ? N1 Ir1 C12 93.2(3) . . ? N2 Ir1 C12 80.2(3) . . ? C25 Ir2 C26 91.4(3) . . ? C25 Ir2 C38 175.2(3) . . ? C26 Ir2 C38 91.4(3) . . ? C25 Ir2 N8 96.1(3) . . ? C26 Ir2 N8 89.0(3) . . ? C38 Ir2 N8 80.0(3) . . ? C25 Ir2 C27 86.4(3) . . ? C26 Ir2 C27 175.8(3) . . ? C38 Ir2 C27 91.0(3) . . ? N8 Ir2 C27 94.8(3) . . ? C25 Ir2 N7 90.7(3) . . ? C26 Ir2 N7 96.2(3) . . ? C38 Ir2 N7 92.9(3) . . ? N8 Ir2 N7 171.3(3) . . ? C27 Ir2 N7 80.2(3) . . ? O3S Gd1 O1Y 91.1(5) . . ? O3S Gd1 O6S 140.0(3) . . ? O1Y Gd1 O6S 63.8(5) . . ? O3S Gd1 N5 111.5(3) . . ? O1Y Gd1 N5 137.4(5) . . ? O6S Gd1 N5 76.6(3) . . ? O3S Gd1 O4S 75.8(3) . . ? O1Y Gd1 O4S 146.7(5) . . ? O6S Gd1 O4S 141.5(3) . . ? N5 Gd1 O4S 75.5(2) . . ? O3S Gd1 O5S 67.7(2) . . ? O1Y Gd1 O5S 81.8(5) . . ? O6S Gd1 O5S 77.7(3) . . ? N5 Gd1 O5S 74.9(2) . . ? O4S Gd1 O5S 119.2(3) . . ? O3S Gd1 N4 80.1(2) . . ? O1Y Gd1 N4 72.6(5) . . ? O6S Gd1 N4 117.0(3) . . ? N5 Gd1 N4 144.3(3) . . ? O4S Gd1 N4 75.0(2) . . ? O5S Gd1 N4 138.2(2) . . ? O3S Gd1 O2S 146.8(3) . . ? O1Y Gd1 O2S 99.0(5) . . ? O6S Gd1 O2S 71.5(3) . . ? N5 Gd1 O2S 81.8(2) . . ? O4S Gd1 O2S 78.6(3) . . ? O5S Gd1 O2S 144.9(2) . . ? N4 Gd1 O2S 73.0(2) . . ? O3S Gd1 O1X 80.3(3) . . ? O1Y Gd1 O1X 13.0(5) . . ? O6S Gd1 O1X 69.7(3) . . ? N5 Gd1 O1X 136.1(3) . . ? O4S Gd1 O1X 146.4(3) . . ? O5S Gd1 O1X 71.2(3) . . ? N4 Gd1 O1X 77.9(3) . . ? O2S Gd1 O1X 111.9(3) . . ? C2 C1 N1 122.9(8) . . ? C2 C1 H25 118.6 . . ? N1 C1 H25 118.6 . . ? C1 C2 C3 118.7(8) . . ? C1 C2 H26 120.7 . . ? C3 C2 H26 120.7 . . ? C4 C3 C2 119.6(9) . . ? C4 C3 H27 120.2 . . ? C2 C3 H27 120.2 . . ? C3 C4 C5 119.7(9) . . ? C3 C4 H28 120.2 . . ? C5 C4 H28 120.2 . . ? N1 C5 C4 119.6(8) . . ? N1 C5 C6 114.3(7) . . ? C4 C5 C6 126.1(8) . . ? C7 C6 C11 122.4(8) . . ? C7 C6 C5 121.9(8) . . ? C11 C6 C5 115.7(8) . . ? C8 C7 C6 117.9(9) . . ? C8 C7 H31 121.1 . . ? C6 C7 H31 121.1 . . ? C9 C8 C7 121.4(9) . . ? C9 C8 H32 119.3 . . ? C7 C8 H32 119.3 . . ? C8 C9 C10 119.4(8) . . ? C8 C9 H33 120.3 . . ? C10 C9 H33 120.3 . . ? C9 C10 C11 122.7(9) . . ? C9 C10 H34 118.7 . . ? C11 C10 H34 118.7 . . ? C10 C11 C6 116.2(8) . . ? C10 C11 Ir1 130.1(7) . . ? C6 C11 Ir1 113.6(6) . . ? C13 C12 C17 118.3(7) . . ? C13 C12 Ir1 128.8(6) . . ? C17 C12 Ir1 112.9(6) . . ? C12 C13 C14 121.5(9) . . ? C12 C13 H37 119.2 . . ? C14 C13 H37 119.2 . . ? C15 C14 C13 119.3(9) . . ? C15 C14 H48 120.3 . . ? C13 C14 H48 120.3 . . ? C16 C15 C14 121.3(9) . . ? C16 C15 H47 119.4 . . ? C14 C15 H47 119.4 . . ? C15 C16 C17 119.1(9) . . ? C15 C16 H40 120.5 . . ? C17 C16 H40 120.5 . . ? C12 C17 C16 120.5(9) . . ? C12 C17 C18 116.2(7) . . ? C16 C17 C18 123.3(8) . . ? N2 C18 C19 119.1(8) . . ? N2 C18 C17 115.0(8) . . ? C19 C18 C17 125.9(8) . . ? C20 C19 C18 120.2(9) . . ? C20 C19 H42 119.9 . . ? C18 C19 H42 119.9 . . ? C19 C20 C21 118.8(10) . . ? C19 C20 H43 120.6 . . ? C21 C20 H43 120.6 . . ? C22 C21 C20 120.0(10) . . ? C22 C21 H44 120.0 . . ? C20 C21 H44 120.0 . . ? N2 C22 C21 122.5(9) . . ? N2 C22 H45 118.8 . . ? C21 C22 H45 118.8 . . ? N3 C23 Ir1 177.4(7) . . ? N4 C24 Ir1 177.3(8) . . ? N5 C25 Ir2 177.1(8) . . ? N6 C26 Ir2 176.7(7) . . ? C28 C27 C32 117.2(8) . . ? C28 C27 Ir2 129.7(7) . . ? C32 C27 Ir2 112.8(6) . . ? C29 C28 C27 122.0(9) . . ? C29 C28 H2 119.0 . . ? C27 C28 H2 119.0 . . ? C28 C29 C30 121.0(9) . . ? C28 C29 H3 119.5 . . ? C30 C29 H3 119.5 . . ? C31 C30 C29 119.8(9) . . ? C31 C30 H4 120.1 . . ? C29 C30 H4 120.1 . . ? C30 C31 C32 119.7(9) . . ? C30 C31 H5 120.1 . . ? C32 C31 H5 120.1 . . ? C31 C32 C27 120.2(9) . . ? C31 C32 C33 123.3(8) . . ? C27 C32 C33 116.5(8) . . ? N7 C33 C34 118.9(8) . . ? N7 C33 C32 114.1(7) . . ? C34 C33 C32 127.0(8) . . ? C35 C34 C33 120.4(9) . . ? C35 C34 H8 119.8 . . ? C33 C34 H8 119.8 . . ? C34 C35 C36 119.8(8) . . ? C34 C35 H9 120.1 . . ? C36 C35 H9 120.1 . . ? C35 C36 C37 119.2(9) . . ? C35 C36 H10 120.4 . . ? C37 C36 H10 120.4 . . ? N7 C37 C36 121.6(9) . . ? N7 C37 H11 119.2 . . ? C36 C37 H11 119.2 . . ? C39 C38 C43 115.5(7) . . ? C39 C38 Ir2 130.1(6) . . ? C43 C38 Ir2 114.3(6) . . ? C40 C39 C38 122.7(8) . . ? C40 C39 H22 118.7 . . ? C38 C39 H22 118.7 . . ? C41 C40 C39 119.9(9) . . ? C41 C40 H21 120.0 . . ? C39 C40 H21 120.0 . . ? C40 C41 C42 120.7(8) . . ? C40 C41 H20 119.6 . . ? C42 C41 H20 119.6 . . ? C41 C42 C43 119.2(9) . . ? C41 C42 H19 120.4 . . ? C43 C42 H19 120.4 . . ? C42 C43 C38 121.9(9) . . ? C42 C43 C44 123.2(8) . . ? C38 C43 C44 114.8(7) . . ? N8 C44 C45 119.5(9) . . ? N8 C44 C43 115.0(7) . . ? C45 C44 C43 125.5(9) . . ? C46 C45 C44 120.5(9) . . ? C46 C45 H15 119.8 . . ? C44 C45 H15 119.8 . . ? C45 C46 C47 118.8(9) . . ? C45 C46 H14 120.6 . . ? C47 C46 H14 120.6 . . ? C48 C47 C46 118.4(10) . . ? C48 C47 H13 120.8 . . ? C46 C47 H13 120.8 . . ? N8 C48 C47 124.2(9) . . ? N8 C48 H12 117.9 . . ? C47 C48 H12 117.9 . . ? C1 N1 C5 119.5(7) . . ? C1 N1 Ir1 124.3(6) . . ? C5 N1 Ir1 116.2(5) . . ? C22 N2 C18 119.4(8) . . ? C22 N2 Ir1 125.1(6) . . ? C18 N2 Ir1 115.5(6) . . ? C24 N4 Gd1 168.8(8) . . ? C25 N5 Gd1 175.3(7) . . ? C37 N7 C33 120.1(7) . . ? C37 N7 Ir2 123.7(6) . . ? C33 N7 Ir2 116.0(6) . . ? C48 N8 C44 118.6(8) . . ? C48 N8 Ir2 125.6(6) . . ? C44 N8 Ir2 115.8(6) . . ? C1X O1X Gd1 132.6(11) . . ? O1Y C1Y H1Y1 109.5 . . ? O1Y C1Y H1Y2 109.5 . . ? H1Y1 C1Y H1Y2 109.5 . . ? O1Y C1Y H1Y3 109.5 . . ? H1Y1 C1Y H1Y3 109.5 . . ? H1Y2 C1Y H1Y3 109.5 . . ? C1Y O1Y Gd1 159.6(18) . . ? C2S O2S Gd1 119.1(7) . . ? O2S C2S H54A 109.5 . . ? O2S C2S H54B 109.5 . . ? H54A C2S H54B 109.5 . . ? O2S C2S H54C 109.5 . . ? H54A C2S H54C 109.5 . . ? H54B C2S H54C 109.5 . . ? C3S O3S Gd1 130.3(8) . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C4S O4S Gd1 131.4(7) . . ? O4S C4S H52A 109.5 . . ? O4S C4S H52B 109.5 . . ? H52A C4S H52B 109.5 . . ? O4S C4S H52C 109.5 . . ? H52A C4S H52C 109.5 . . ? H52B C4S H52C 109.5 . . ? C5S O5S Gd1 133.3(7) . . ? O5S C5S H57A 109.5 . . ? O5S C5S H57B 109.5 . . ? H57A C5S H57B 109.5 . . ? O5S C5S H57C 109.5 . . ? H57A C5S H57C 109.5 . . ? H57B C5S H57C 109.5 . . ? C6S O6S Gd1 130.3(7) . . ? O6S C6S H55A 109.5 . . ? O6S C6S H55B 109.5 . . ? H55A C6S H55B 109.5 . . ? O6S C6S H55C 109.5 . . ? H55A C6S H55C 109.5 . . ? H55B C6S H55C 109.5 . . ? O7S C7S H7S1 109.5 . . ? O7S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? O7S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? O8S C8S H8S1 109.5 . . ? O8S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? O8S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 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 N1 C1 C2 C3 1.6(12) . . . . ? C1 C2 C3 C4 -0.3(12) . . . . ? C2 C3 C4 C5 -1.5(12) . . . . ? C3 C4 C5 N1 2.1(12) . . . . ? C3 C4 C5 C6 -178.9(8) . . . . ? N1 C5 C6 C7 -176.4(7) . . . . ? C4 C5 C6 C7 4.5(13) . . . . ? N1 C5 C6 C11 4.2(10) . . . . ? C4 C5 C6 C11 -174.9(8) . . . . ? C11 C6 C7 C8 1.3(13) . . . . ? C5 C6 C7 C8 -178.2(8) . . . . ? C6 C7 C8 C9 -0.5(14) . . . . ? C7 C8 C9 C10 -0.6(14) . . . . ? C8 C9 C10 C11 1.0(14) . . . . ? C9 C10 C11 C6 -0.1(12) . . . . ? C9 C10 C11 Ir1 -176.5(7) . . . . ? C7 C6 C11 C10 -1.0(12) . . . . ? C5 C6 C11 C10 178.5(7) . . . . ? C7 C6 C11 Ir1 175.9(7) . . . . ? C5 C6 C11 Ir1 -4.6(9) . . . . ? C24 Ir1 C11 C10 89.1(8) . . . . ? C23 Ir1 C11 C10 177(4) . . . . ? N1 Ir1 C11 C10 179.2(8) . . . . ? N2 Ir1 C11 C10 -7.4(8) . . . . ? C12 Ir1 C11 C10 -87.7(8) . . . . ? C24 Ir1 C11 C6 -87.4(6) . . . . ? C23 Ir1 C11 C6 1(4) . . . . ? N1 Ir1 C11 C6 2.8(6) . . . . ? N2 Ir1 C11 C6 176.2(6) . . . . ? C12 Ir1 C11 C6 95.9(6) . . . . ? C24 Ir1 C12 C13 172(5) . . . . ? C11 Ir1 C12 C13 -86.5(8) . . . . ? C23 Ir1 C12 C13 89.3(8) . . . . ? N1 Ir1 C12 C13 -6.3(8) . . . . ? N2 Ir1 C12 C13 180.0(8) . . . . ? C24 Ir1 C12 C17 -5(6) . . . . ? C11 Ir1 C12 C17 95.9(6) . . . . ? C23 Ir1 C12 C17 -88.3(6) . . . . ? N1 Ir1 C12 C17 176.1(6) . . . . ? N2 Ir1 C12 C17 2.4(6) . . . . ? C17 C12 C13 C14 -0.6(12) . . . . ? Ir1 C12 C13 C14 -178.1(6) . . . . ? C12 C13 C14 C15 0.2(13) . . . . ? C13 C14 C15 C16 -0.3(14) . . . . ? C14 C15 C16 C17 0.8(14) . . . . ? C13 C12 C17 C16 1.1(12) . . . . ? Ir1 C12 C17 C16 179.0(6) . . . . ? C13 C12 C17 C18 -179.4(7) . . . . ? Ir1 C12 C17 C18 -1.5(9) . . . . ? C15 C16 C17 C12 -1.2(13) . . . . ? C15 C16 C17 C18 179.4(8) . . . . ? C12 C17 C18 N2 -0.9(11) . . . . ? C16 C17 C18 N2 178.5(8) . . . . ? C12 C17 C18 C19 -179.8(8) . . . . ? C16 C17 C18 C19 -0.3(14) . . . . ? N2 C18 C19 C20 -2.6(14) . . . . ? C17 C18 C19 C20 176.2(9) . . . . ? C18 C19 C20 C21 -0.2(15) . . . . ? C19 C20 C21 C22 2.1(16) . . . . ? C20 C21 C22 N2 -1.2(16) . . . . ? C24 Ir1 C23 N3 -20(18) . . . . ? C11 Ir1 C23 N3 -108(18) . . . . ? N1 Ir1 C23 N3 -110(18) . . . . ? N2 Ir1 C23 N3 76(18) . . . . ? C12 Ir1 C23 N3 157(18) . . . . ? C11 Ir1 C24 N4 75(17) . . . . ? C23 Ir1 C24 N4 -100(17) . . . . ? N1 Ir1 C24 N4 -5(17) . . . . ? N2 Ir1 C24 N4 169(17) . . . . ? C12 Ir1 C24 N4 177(100) . . . . ? C26 Ir2 C25 N5 -179(100) . . . . ? C38 Ir2 C25 N5 55(17) . . . . ? N8 Ir2 C25 N5 92(15) . . . . ? C27 Ir2 C25 N5 -3(15) . . . . ? N7 Ir2 C25 N5 -83(15) . . . . ? C25 Ir2 C26 N6 2(13) . . . . ? C38 Ir2 C26 N6 178(100) . . . . ? N8 Ir2 C26 N6 98(13) . . . . ? C27 Ir2 C26 N6 -57(15) . . . . ? N7 Ir2 C26 N6 -89(13) . . . . ? C25 Ir2 C27 C28 84.8(8) . . . . ? C26 Ir2 C27 C28 143(4) . . . . ? C38 Ir2 C27 C28 -91.1(8) . . . . ? N8 Ir2 C27 C28 -11.1(8) . . . . ? N7 Ir2 C27 C28 176.1(9) . . . . ? C25 Ir2 C27 C32 -89.3(6) . . . . ? C26 Ir2 C27 C32 -31(5) . . . . ? C38 Ir2 C27 C32 94.8(6) . . . . ? N8 Ir2 C27 C32 174.9(6) . . . . ? N7 Ir2 C27 C32 2.0(6) . . . . ? C32 C27 C28 C29 0.0(13) . . . . ? Ir2 C27 C28 C29 -173.8(7) . . . . ? C27 C28 C29 C30 1.7(15) . . . . ? C28 C29 C30 C31 -2.1(15) . . . . ? C29 C30 C31 C32 0.9(14) . . . . ? C30 C31 C32 C27 0.8(13) . . . . ? C30 C31 C32 C33 -179.9(8) . . . . ? C28 C27 C32 C31 -1.3(12) . . . . ? Ir2 C27 C32 C31 173.6(6) . . . . ? C28 C27 C32 C33 179.4(7) . . . . ? Ir2 C27 C32 C33 -5.7(9) . . . . ? C31 C32 C33 N7 -171.8(7) . . . . ? C27 C32 C33 N7 7.5(10) . . . . ? C31 C32 C33 C34 9.6(13) . . . . ? C27 C32 C33 C34 -171.1(8) . . . . ? N7 C33 C34 C35 2.4(12) . . . . ? C32 C33 C34 C35 -179.2(8) . . . . ? C33 C34 C35 C36 -1.4(13) . . . . ? C34 C35 C36 C37 0.3(13) . . . . ? C35 C36 C37 N7 -0.1(13) . . . . ? C25 Ir2 C38 C39 -144(4) . . . . ? C26 Ir2 C38 C39 90.7(8) . . . . ? N8 Ir2 C38 C39 179.4(9) . . . . ? C27 Ir2 C38 C39 -85.9(8) . . . . ? N7 Ir2 C38 C39 -5.6(8) . . . . ? C25 Ir2 C38 C43 33(4) . . . . ? C26 Ir2 C38 C43 -92.0(7) . . . . ? N8 Ir2 C38 C43 -3.3(6) . . . . ? C27 Ir2 C38 C43 91.4(7) . . . . ? N7 Ir2 C38 C43 171.6(6) . . . . ? C43 C38 C39 C40 1.6(13) . . . . ? Ir2 C38 C39 C40 178.9(7) . . . . ? C38 C39 C40 C41 -1.4(14) . . . . ? C39 C40 C41 C42 0.9(14) . . . . ? C40 C41 C42 C43 -0.8(14) . . . . ? C41 C42 C43 C38 1.2(14) . . . . ? C41 C42 C43 C44 177.5(9) . . . . ? C39 C38 C43 C42 -1.5(13) . . . . ? Ir2 C38 C43 C42 -179.2(7) . . . . ? C39 C38 C43 C44 -178.2(8) . . . . ? Ir2 C38 C43 C44 4.2(10) . . . . ? C42 C43 C44 N8 -179.2(8) . . . . ? C38 C43 C44 N8 -2.6(11) . . . . ? C42 C43 C44 C45 -0.4(14) . . . . ? C38 C43 C44 C45 176.2(9) . . . . ? N8 C44 C45 C46 0.1(14) . . . . ? C43 C44 C45 C46 -178.6(9) . . . . ? C44 C45 C46 C47 0.5(16) . . . . ? C45 C46 C47 C48 -1.7(16) . . . . ? C46 C47 C48 N8 2.5(17) . . . . ? C2 C1 N1 C5 -1.0(11) . . . . ? C2 C1 N1 Ir1 -179.2(6) . . . . ? C4 C5 N1 C1 -0.9(11) . . . . ? C6 C5 N1 C1 180.0(7) . . . . ? C4 C5 N1 Ir1 177.4(6) . . . . ? C6 C5 N1 Ir1 -1.7(9) . . . . ? C24 Ir1 N1 C1 -92.7(6) . . . . ? C11 Ir1 N1 C1 177.7(6) . . . . ? C23 Ir1 N1 C1 -2.5(6) . . . . ? N2 Ir1 N1 C1 130.6(16) . . . . ? C12 Ir1 N1 C1 87.2(6) . . . . ? C24 Ir1 N1 C5 89.0(6) . . . . ? C11 Ir1 N1 C5 -0.6(5) . . . . ? C23 Ir1 N1 C5 179.3(6) . . . . ? N2 Ir1 N1 C5 -47.7(19) . . . . ? C12 Ir1 N1 C5 -91.0(6) . . . . ? C21 C22 N2 C18 -1.6(14) . . . . ? C21 C22 N2 Ir1 -179.9(7) . . . . ? C19 C18 N2 C22 3.4(12) . . . . ? C17 C18 N2 C22 -175.5(8) . . . . ? C19 C18 N2 Ir1 -178.1(6) . . . . ? C17 C18 N2 Ir1 3.0(9) . . . . ? C24 Ir1 N2 C22 -5.0(8) . . . . ? C11 Ir1 N2 C22 85.0(7) . . . . ? C23 Ir1 N2 C22 -95.3(7) . . . . ? N1 Ir1 N2 C22 131.3(16) . . . . ? C12 Ir1 N2 C22 175.4(8) . . . . ? C24 Ir1 N2 C18 176.6(6) . . . . ? C11 Ir1 N2 C18 -93.4(6) . . . . ? C23 Ir1 N2 C18 86.3(6) . . . . ? N1 Ir1 N2 C18 -47.1(19) . . . . ? C12 Ir1 N2 C18 -3.0(6) . . . . ? Ir1 C24 N4 Gd1 -27(20) . . . . ? O3S Gd1 N4 C24 124(4) . . . . ? O1Y Gd1 N4 C24 29(4) . . . . ? O6S Gd1 N4 C24 -18(4) . . . . ? N5 Gd1 N4 C24 -123(4) . . . . ? O4S Gd1 N4 C24 -158(4) . . . . ? O5S Gd1 N4 C24 84(4) . . . . ? O2S Gd1 N4 C24 -76(4) . . . . ? O1X Gd1 N4 C24 42(4) . . . . ? Ir2 C25 N5 Gd1 125(14) . . . . ? O3S Gd1 N5 C25 -70(9) . . . . ? O1Y Gd1 N5 C25 47(9) . . . . ? O6S Gd1 N5 C25 69(9) . . . . ? O4S Gd1 N5 C25 -138(9) . . . . ? O5S Gd1 N5 C25 -12(9) . . . . ? N4 Gd1 N5 C25 -173(9) . . . . ? O2S Gd1 N5 C25 142(9) . . . . ? O1X Gd1 N5 C25 29(9) . . . . ? C36 C37 N7 C33 1.0(12) . . . . ? C36 C37 N7 Ir2 -173.8(6) . . . . ? C34 C33 N7 C37 -2.2(11) . . . . ? C32 C33 N7 C37 179.2(7) . . . . ? C34 C33 N7 Ir2 173.1(6) . . . . ? C32 C33 N7 Ir2 -5.6(9) . . . . ? C25 Ir2 N7 C37 -96.7(7) . . . . ? C26 Ir2 N7 C37 -5.2(7) . . . . ? C38 Ir2 N7 C37 86.5(7) . . . . ? N8 Ir2 N7 C37 121.6(18) . . . . ? C27 Ir2 N7 C37 177.1(7) . . . . ? C25 Ir2 N7 C33 88.2(6) . . . . ? C26 Ir2 N7 C33 179.7(6) . . . . ? C38 Ir2 N7 C33 -88.6(6) . . . . ? N8 Ir2 N7 C33 -53(2) . . . . ? C27 Ir2 N7 C33 2.0(6) . . . . ? C47 C48 N8 C44 -1.9(15) . . . . ? C47 C48 N8 Ir2 177.6(8) . . . . ? C45 C44 N8 C48 0.5(13) . . . . ? C43 C44 N8 C48 179.4(8) . . . . ? C45 C44 N8 Ir2 -179.1(7) . . . . ? C43 C44 N8 Ir2 -0.2(10) . . . . ? C25 Ir2 N8 C48 5.3(8) . . . . ? C26 Ir2 N8 C48 -86.0(8) . . . . ? C38 Ir2 N8 C48 -177.6(9) . . . . ? C27 Ir2 N8 C48 92.2(8) . . . . ? N7 Ir2 N8 C48 146.7(17) . . . . ? C25 Ir2 N8 C44 -175.2(7) . . . . ? C26 Ir2 N8 C44 93.5(7) . . . . ? C38 Ir2 N8 C44 1.9(6) . . . . ? C27 Ir2 N8 C44 -88.3(7) . . . . ? N7 Ir2 N8 C44 -34(2) . . . . ? O3S Gd1 O1X C1X -51.5(14) . . . . ? O1Y Gd1 O1X C1X 95(3) . . . . ? O6S Gd1 O1X C1X 155.3(15) . . . . ? N5 Gd1 O1X C1X -162.5(13) . . . . ? O4S Gd1 O1X C1X -6.5(17) . . . . ? O5S Gd1 O1X C1X -121.2(14) . . . . ? N4 Gd1 O1X C1X 30.3(14) . . . . ? O2S Gd1 O1X C1X 96.2(14) . . . . ? O3S Gd1 O1Y C1Y -49(5) . . . . ? O6S Gd1 O1Y C1Y 164(5) . . . . ? N5 Gd1 O1Y C1Y -173(5) . . . . ? O4S Gd1 O1Y C1Y 17(6) . . . . ? O5S Gd1 O1Y C1Y -116(5) . . . . ? N4 Gd1 O1Y C1Y 31(5) . . . . ? O2S Gd1 O1Y C1Y 100(5) . . . . ? O1X Gd1 O1Y C1Y -82(6) . . . . ? O3S Gd1 O2S C2S 97.9(9) . . . . ? O1Y Gd1 O2S C2S -8.2(9) . . . . ? O6S Gd1 O2S C2S -66.6(8) . . . . ? N5 Gd1 O2S C2S -145.1(8) . . . . ? O4S Gd1 O2S C2S 138.1(8) . . . . ? O5S Gd1 O2S C2S -96.7(8) . . . . ? N4 Gd1 O2S C2S 60.4(8) . . . . ? O1X Gd1 O2S C2S -8.5(9) . . . . ? O1Y Gd1 O3S C3S 93.6(12) . . . . ? O6S Gd1 O3S C3S 142.0(11) . . . . ? N5 Gd1 O3S C3S -123.4(11) . . . . ? O4S Gd1 O3S C3S -55.4(11) . . . . ? O5S Gd1 O3S C3S 174.3(12) . . . . ? N4 Gd1 O3S C3S 21.5(11) . . . . ? O2S Gd1 O3S C3S -14.7(14) . . . . ? O1X Gd1 O3S C3S 100.8(12) . . . . ? O3S Gd1 O4S C4S -78.9(13) . . . . ? O1Y Gd1 O4S C4S -148.6(14) . . . . ? O6S Gd1 O4S C4S 83.1(13) . . . . ? N5 Gd1 O4S C4S 38.2(13) . . . . ? O5S Gd1 O4S C4S -24.9(13) . . . . ? N4 Gd1 O4S C4S -162.2(13) . . . . ? O2S Gd1 O4S C4S 122.5(13) . . . . ? O1X Gd1 O4S C4S -124.9(13) . . . . ? O3S Gd1 O5S C5S 157.2(11) . . . . ? O1Y Gd1 O5S C5S -108.2(12) . . . . ? O6S Gd1 O5S C5S -43.4(11) . . . . ? N5 Gd1 O5S C5S 35.8(11) . . . . ? O4S Gd1 O5S C5S 99.3(11) . . . . ? N4 Gd1 O5S C5S -160.4(10) . . . . ? O2S Gd1 O5S C5S -14.3(13) . . . . ? O1X Gd1 O5S C5S -115.9(11) . . . . ? O3S Gd1 O6S C6S 138.9(9) . . . . ? O1Y Gd1 O6S C6S -164.7(11) . . . . ? N5 Gd1 O6S C6S 31.3(9) . . . . ? O4S Gd1 O6S C6S -13.3(11) . . . . ? O5S Gd1 O6S C6S 108.5(9) . . . . ? N4 Gd1 O6S C6S -113.3(9) . . . . ? O2S Gd1 O6S C6S -54.3(9) . . . . ? O1X Gd1 O6S C6S -177.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.051 _refine_diff_density_min -2.223 _refine_diff_density_rms 0.209 #===END data_imw1436p-1 _database_code_depnum_ccdc_archive 'CCDC 834581' #TrackingRef '- Ward_combinedCIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H109 Eu2 Ir2 N21 O19 P4' _chemical_formula_weight 3081.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' P P 0.1023 0.0942 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5286(10) _cell_length_b 16.3216(13) _cell_length_c 31.872(3) _cell_angle_alpha 86.410(4) _cell_angle_beta 86.247(4) _cell_angle_gamma 73.232(4) _cell_volume 6220.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9685 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.63 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 3.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6240 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 105706 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.66 _reflns_number_total 28768 _reflns_number_gt 23579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28768 _refine_ls_number_parameters 1608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.970021(9) 0.450147(7) 0.224323(4) 0.01118(3) Uani 1 1 d . . . Ir2 Ir 0.570627(10) 0.035825(7) 0.262560(4) 0.01182(3) Uani 1 1 d . . . Eu1 Eu 0.793559(13) 0.242962(10) 0.321804(5) 0.01331(4) Uani 1 1 d . . . Eu2 Eu 0.757161(12) 0.234079(10) 0.158556(5) 0.01307(4) Uani 1 1 d . . . C1 C 1.1497(3) 0.3040(2) 0.18503(10) 0.0162(7) Uani 1 1 d . . . H1 H 1.0892 0.2881 0.1749 0.019 Uiso 1 1 calc R . . C2 C 1.2572(3) 0.2579(2) 0.17352(10) 0.0203(7) Uani 1 1 d . . . H2 H 1.2704 0.2107 0.1560 0.024 Uiso 1 1 calc R . . C3 C 1.3460(3) 0.2814(2) 0.18782(11) 0.0235(8) Uani 1 1 d . . . H3 H 1.4208 0.2512 0.1798 0.028 Uiso 1 1 calc R . . C4 C 1.3239(3) 0.3489(2) 0.21375(11) 0.0215(7) Uani 1 1 d . . . H4 H 1.3840 0.3655 0.2238 0.026 Uiso 1 1 calc R . . C5 C 1.2143(3) 0.3937(2) 0.22552(10) 0.0154(7) Uani 1 1 d . . . C6 C 1.1799(3) 0.4652(2) 0.25386(10) 0.0164(7) Uani 1 1 d . . . C7 C 1.2562(3) 0.4929(2) 0.27517(11) 0.0231(8) Uani 1 1 d . . . H7 H 1.3339 0.4646 0.2720 0.028 Uiso 1 1 calc R . . C8 C 1.2181(3) 0.5615(2) 0.30081(11) 0.0255(8) Uani 1 1 d . . . H8 H 1.2695 0.5812 0.3151 0.031 Uiso 1 1 calc R . . C9 C 1.1044(3) 0.6015(2) 0.30552(10) 0.0233(8) Uani 1 1 d . . . H9 H 1.0782 0.6491 0.3230 0.028 Uiso 1 1 calc R . . C10 C 1.0288(3) 0.5729(2) 0.28507(10) 0.0180(7) Uani 1 1 d . . . H10 H 0.9513 0.6006 0.2892 0.022 Uiso 1 1 calc R . . C11 C 1.0639(3) 0.5041(2) 0.25850(9) 0.0131(6) Uani 1 1 d . . . C12 C 0.9844(3) 0.5364(2) 0.17592(9) 0.0134(6) Uani 1 1 d . . . C13 C 1.0708(3) 0.5314(2) 0.14555(10) 0.0200(7) Uani 1 1 d . . . H13 H 1.1316 0.4807 0.1448 0.024 Uiso 1 1 calc R . . C14 C 1.0708(3) 0.5984(2) 0.11623(11) 0.0244(8) Uani 1 1 d . . . H14 H 1.1311 0.5928 0.0959 0.029 Uiso 1 1 calc R . . C15 C 0.9834(3) 0.6732(2) 0.11658(11) 0.0240(8) Uani 1 1 d . . . H15 H 0.9836 0.7189 0.0966 0.029 Uiso 1 1 calc R . . C16 C 0.8949(3) 0.6811(2) 0.14645(11) 0.0194(7) Uani 1 1 d . . . H16 H 0.8346 0.7321 0.1469 0.023 Uiso 1 1 calc R . . C17 C 0.8955(3) 0.6132(2) 0.17582(10) 0.0150(6) Uani 1 1 d . . . C18 C 0.8056(3) 0.6163(2) 0.20810(10) 0.0164(7) Uani 1 1 d . . . C19 C 0.7082(3) 0.6837(2) 0.21246(11) 0.0211(7) Uani 1 1 d . . . H19 H 0.6975 0.7333 0.1941 0.025 Uiso 1 1 calc R . . C20 C 0.6272(3) 0.6789(2) 0.24325(12) 0.0256(8) Uani 1 1 d . . . H20 H 0.5610 0.7250 0.2464 0.031 Uiso 1 1 calc R . . C21 C 0.6442(3) 0.6053(2) 0.26959(11) 0.0232(8) Uani 1 1 d . . . H21 H 0.5897 0.6003 0.2910 0.028 Uiso 1 1 calc R . . C22 C 0.7410(3) 0.5403(2) 0.26401(10) 0.0179(7) Uani 1 1 d . . . H22 H 0.7520 0.4899 0.2818 0.021 Uiso 1 1 calc R . . C23 C 0.9408(2) 0.3746(2) 0.27474(10) 0.0135(6) Uani 1 1 d . . . C24 C 0.8911(2) 0.3839(2) 0.19138(9) 0.0133(6) Uani 1 1 d . . . C25 C 0.7886(3) -0.0747(2) 0.22402(10) 0.0182(7) Uani 1 1 d . . . H25 H 0.7825 -0.0277 0.2043 0.022 Uiso 1 1 calc R . . C26 C 0.8808(3) -0.1447(2) 0.22078(11) 0.0241(8) Uani 1 1 d . . . H26 H 0.9370 -0.1466 0.1991 0.029 Uiso 1 1 calc R . . C27 C 0.8896(3) -0.2126(2) 0.25011(12) 0.0267(8) Uani 1 1 d . . . H27 H 0.9523 -0.2619 0.2487 0.032 Uiso 1 1 calc R . . C28 C 0.8074(3) -0.2082(2) 0.28119(11) 0.0226(7) Uani 1 1 d . . . H28 H 0.8134 -0.2543 0.3014 0.027 Uiso 1 1 calc R . . C29 C 0.7145(3) -0.1357(2) 0.28314(10) 0.0172(7) Uani 1 1 d . . . C30 C 0.6246(3) -0.1214(2) 0.31625(10) 0.0157(6) Uani 1 1 d . . . C31 C 0.6179(3) -0.1830(2) 0.34836(11) 0.0219(7) Uani 1 1 d . . . H31 H 0.6700 -0.2384 0.3483 0.026 Uiso 1 1 calc R . . C32 C 0.5353(3) -0.1626(2) 0.38004(11) 0.0264(8) Uani 1 1 d . . . H32 H 0.5305 -0.2036 0.4020 0.032 Uiso 1 1 calc R . . C33 C 0.4589(3) -0.0810(2) 0.37941(11) 0.0245(8) Uani 1 1 d . . . H33 H 0.4029 -0.0663 0.4014 0.029 Uiso 1 1 calc R . . C34 C 0.4640(3) -0.0212(2) 0.34701(10) 0.0196(7) Uani 1 1 d . . . H34 H 0.4103 0.0334 0.3469 0.023 Uiso 1 1 calc R . . C35 C 0.5467(3) -0.0399(2) 0.31443(10) 0.0157(7) Uani 1 1 d . . . C36 C 0.4591(2) -0.0085(2) 0.23300(9) 0.0130(6) Uani 1 1 d . . . C37 C 0.4758(3) -0.0848(2) 0.21239(10) 0.0176(7) Uani 1 1 d . . . H37 H 0.5485 -0.1238 0.2106 0.021 Uiso 1 1 calc R . . C38 C 0.3886(3) -0.1053(2) 0.19429(11) 0.0211(7) Uani 1 1 d . . . H38 H 0.4022 -0.1584 0.1812 0.025 Uiso 1 1 calc R . . C39 C 0.2826(3) -0.0485(2) 0.19534(11) 0.0218(7) Uani 1 1 d . . . H39 H 0.2240 -0.0614 0.1822 0.026 Uiso 1 1 calc R . . C40 C 0.2624(3) 0.0273(2) 0.21561(10) 0.0198(7) Uani 1 1 d . . . H40 H 0.1898 0.0667 0.2161 0.024 Uiso 1 1 calc R . . C41 C 0.3482(3) 0.0462(2) 0.23538(10) 0.0147(6) Uani 1 1 d . . . C42 C 0.3305(3) 0.1210(2) 0.26104(10) 0.0154(6) Uani 1 1 d . . . C43 C 0.2275(3) 0.1779(2) 0.27244(11) 0.0206(7) Uani 1 1 d . . . H43 H 0.1612 0.1715 0.2620 0.025 Uiso 1 1 calc R . . C44 C 0.2211(3) 0.2434(2) 0.29881(10) 0.0224(8) Uani 1 1 d . . . H44 H 0.1508 0.2813 0.3071 0.027 Uiso 1 1 calc R . . C45 C 0.3188(3) 0.2527(2) 0.31297(11) 0.0220(7) Uani 1 1 d . . . H45 H 0.3167 0.2979 0.3307 0.026 Uiso 1 1 calc R . . C46 C 0.4189(3) 0.1960(2) 0.30106(10) 0.0183(7) Uani 1 1 d . . . H46 H 0.4857 0.2030 0.3108 0.022 Uiso 1 1 calc R . . C47 C 0.6080(2) 0.1032(2) 0.21004(10) 0.0129(6) Uani 1 1 d . . . C48 C 0.6696(3) 0.0896(2) 0.29257(10) 0.0159(7) Uani 1 1 d . . . C49 C 0.3948(3) 0.1494(2) 0.46177(10) 0.0147(6) Uani 1 1 d . . . C50 C 0.4610(3) 0.1282(2) 0.49637(10) 0.0198(7) Uani 1 1 d . . . H51 H 0.4275 0.1352 0.5240 0.024 Uiso 1 1 calc R . . C51 C 0.5758(3) 0.0968(2) 0.49052(11) 0.0238(8) Uani 1 1 d . . . H52 H 0.6210 0.0827 0.5142 0.029 Uiso 1 1 calc R . . C52 C 0.6250(3) 0.0858(2) 0.45029(11) 0.0228(8) Uani 1 1 d . . . H53 H 0.7038 0.0640 0.4464 0.027 Uiso 1 1 calc R . . C53 C 0.5593(3) 0.1067(2) 0.41575(11) 0.0234(8) Uani 1 1 d . . . H54 H 0.5931 0.0996 0.3881 0.028 Uiso 1 1 calc R . . C54 C 0.4446(3) 0.1380(2) 0.42132(10) 0.0200(7) Uani 1 1 d . . . H55 H 0.3997 0.1518 0.3976 0.024 Uiso 1 1 calc R . . C55 C 0.1960(3) 0.2788(2) 0.43444(10) 0.0159(7) Uani 1 1 d . . . C56 C 0.2611(3) 0.3342(2) 0.42388(11) 0.0223(7) Uani 1 1 d . . . H57 H 0.3328 0.3228 0.4350 0.027 Uiso 1 1 calc R . . C57 C 0.2222(3) 0.4057(2) 0.39739(11) 0.0250(8) Uani 1 1 d . . . H58 H 0.2671 0.4430 0.3900 0.030 Uiso 1 1 calc R . . C58 C 0.1169(3) 0.4224(2) 0.38169(11) 0.0255(8) Uani 1 1 d . . . H59 H 0.0899 0.4711 0.3633 0.031 Uiso 1 1 calc R . . C59 C 0.0509(3) 0.3689(2) 0.39255(11) 0.0247(8) Uani 1 1 d . . . H60 H -0.0215 0.3815 0.3819 0.030 Uiso 1 1 calc R . . C60 C 0.0897(3) 0.2968(2) 0.41890(10) 0.0196(7) Uani 1 1 d . . . H61 H 0.0442 0.2599 0.4263 0.024 Uiso 1 1 calc R . . C61 C 0.1903(3) 0.1042(2) 0.45400(10) 0.0163(7) Uani 1 1 d . . . C62 C 0.1823(3) 0.0900(2) 0.41182(11) 0.0203(7) Uani 1 1 d . . . H63 H 0.2014 0.1274 0.3905 0.024 Uiso 1 1 calc R . . C63 C 0.1464(3) 0.0212(2) 0.40050(12) 0.0247(8) Uani 1 1 d . . . H64 H 0.1403 0.0123 0.3717 0.030 Uiso 1 1 calc R . . C64 C 0.1198(3) -0.0341(2) 0.43172(12) 0.0266(8) Uani 1 1 d . . . H65 H 0.0964 -0.0814 0.4242 0.032 Uiso 1 1 calc R . . C65 C 0.1273(3) -0.0206(2) 0.47365(12) 0.0273(8) Uani 1 1 d . . . H66 H 0.1093 -0.0588 0.4948 0.033 Uiso 1 1 calc R . . C66 C 0.1610(3) 0.0484(2) 0.48493(11) 0.0186(7) Uani 1 1 d . . . H67 H 0.1643 0.0580 0.5138 0.022 Uiso 1 1 calc R . . C67 C 0.0050(3) 0.3244(2) 0.52980(10) 0.0192(7) Uani 1 1 d . . . C68 C -0.0340(3) 0.4135(2) 0.53092(11) 0.0246(8) Uani 1 1 d . . . H69 H 0.0097 0.4448 0.5423 0.030 Uiso 1 1 calc R . . C69 C -0.1373(3) 0.4559(3) 0.51532(13) 0.0354(10) Uani 1 1 d . . . H70 H -0.1646 0.5165 0.5161 0.042 Uiso 1 1 calc R . . C70 C -0.2005(3) 0.4103(3) 0.49872(13) 0.0363(10) Uani 1 1 d . . . H71 H -0.2713 0.4396 0.4882 0.044 Uiso 1 1 calc R . . C71 C -0.1611(3) 0.3217(3) 0.49741(13) 0.0344(10) Uani 1 1 d . . . H72 H -0.2049 0.2906 0.4859 0.041 Uiso 1 1 calc R . . C72 C -0.0589(3) 0.2791(3) 0.51275(11) 0.0265(8) Uani 1 1 d . . . H73 H -0.0320 0.2185 0.5117 0.032 Uiso 1 1 calc R . . C73 C 0.1010(3) 0.1959(2) 0.59235(10) 0.0179(7) Uani 1 1 d . . . C74 C -0.0005(3) 0.2217(2) 0.61566(11) 0.0257(8) Uani 1 1 d . . . H75 H -0.0532 0.2748 0.6087 0.031 Uiso 1 1 calc R . . C75 C -0.0244(4) 0.1699(3) 0.64904(12) 0.0371(10) Uani 1 1 d . . . H76 H -0.0930 0.1877 0.6651 0.044 Uiso 1 1 calc R . . C76 C 0.0523(4) 0.0920(3) 0.65875(13) 0.0388(11) Uani 1 1 d . . . H77 H 0.0361 0.0567 0.6817 0.047 Uiso 1 1 calc R . . C77 C 0.1518(4) 0.0653(3) 0.63563(12) 0.0347(10) Uani 1 1 d . . . H78 H 0.2029 0.0111 0.6421 0.042 Uiso 1 1 calc R . . C78 C 0.1771(3) 0.1176(2) 0.60289(11) 0.0259(8) Uani 1 1 d . . . H79 H 0.2468 0.0999 0.5875 0.031 Uiso 1 1 calc R . . C79 C 0.1994(3) 0.3355(2) 0.57187(10) 0.0193(7) Uani 1 1 d . . . C80 C 0.1515(3) 0.3799(2) 0.60773(11) 0.0232(8) Uani 1 1 d . . . H81 H 0.0855 0.3712 0.6213 0.028 Uiso 1 1 calc R . . C81 C 0.2011(3) 0.4368(2) 0.62345(12) 0.0297(9) Uani 1 1 d . . . H82 H 0.1680 0.4676 0.6476 0.036 Uiso 1 1 calc R . . C82 C 0.2978(3) 0.4491(2) 0.60441(13) 0.0332(9) Uani 1 1 d . . . H83 H 0.3313 0.4877 0.6156 0.040 Uiso 1 1 calc R . . C83 C 0.3458(3) 0.4051(3) 0.56896(13) 0.0310(9) Uani 1 1 d . . . H84 H 0.4121 0.4139 0.5558 0.037 Uiso 1 1 calc R . . C84 C 0.2976(3) 0.3481(2) 0.55249(11) 0.0238(8) Uani 1 1 d . . . H85 H 0.3310 0.3178 0.5282 0.029 Uiso 1 1 calc R . . C85 C 0.5105(3) 0.1961(2) 0.96543(10) 0.0148(6) Uani 1 1 d . . . C86 C 0.5388(3) 0.1073(2) 0.97319(10) 0.0188(7) Uani 1 1 d . . . H87 H 0.4937 0.0752 0.9635 0.023 Uiso 1 1 calc R . . C87 C 0.6326(3) 0.0668(2) 0.99506(11) 0.0221(7) Uani 1 1 d . . . H88 H 0.6521 0.0065 1.0003 0.027 Uiso 1 1 calc R . . C88 C 0.6987(3) 0.1129(2) 1.00938(11) 0.0237(8) Uani 1 1 d . . . H89 H 0.7625 0.0844 1.0247 0.028 Uiso 1 1 calc R . . C89 C 0.6718(3) 0.2011(2) 1.00131(11) 0.0222(7) Uani 1 1 d . . . H90 H 0.7177 0.2328 1.0108 0.027 Uiso 1 1 calc R . . C90 C 0.5778(3) 0.2426(2) 0.97940(11) 0.0189(7) Uani 1 1 d . . . H91 H 0.5591 0.3028 0.9739 0.023 Uiso 1 1 calc R . . C91 C 0.4063(3) 0.3257(2) 0.90138(10) 0.0145(6) Uani 1 1 d . . . C92 C 0.5026(3) 0.3025(2) 0.87494(10) 0.0164(7) Uani 1 1 d . . . H93 H 0.5576 0.2494 0.8797 0.020 Uiso 1 1 calc R . . C93 C 0.5172(3) 0.3581(2) 0.84162(10) 0.0211(7) Uani 1 1 d . . . H94 H 0.5815 0.3420 0.8231 0.025 Uiso 1 1 calc R . . C94 C 0.4386(3) 0.4367(2) 0.83519(11) 0.0237(8) Uani 1 1 d . . . H95 H 0.4496 0.4746 0.8125 0.028 Uiso 1 1 calc R . . C95 C 0.3444(3) 0.4599(2) 0.86174(11) 0.0232(8) Uani 1 1 d . . . H96 H 0.2913 0.5141 0.8575 0.028 Uiso 1 1 calc R . . C96 C 0.3268(3) 0.4043(2) 0.89459(10) 0.0204(7) Uani 1 1 d . . . H97 H 0.2609 0.4199 0.9123 0.024 Uiso 1 1 calc R . . C97 C 0.3237(3) 0.17695(19) 0.92289(10) 0.0139(6) Uani 1 1 d . . . C98 C 0.3757(3) 0.1319(2) 0.88751(10) 0.0165(7) Uani 1 1 d . . . H99 H 0.4386 0.1449 0.8735 0.020 Uiso 1 1 calc R . . C99 C 0.3358(3) 0.0686(2) 0.87288(11) 0.0209(7) Uani 1 1 d . . . H100 H 0.3713 0.0381 0.8489 0.025 Uiso 1 1 calc R . . C100 C 0.2434(3) 0.0499(2) 0.89343(11) 0.0228(8) Uani 1 1 d . . . H101 H 0.2161 0.0064 0.8836 0.027 Uiso 1 1 calc R . . C101 C 0.1915(3) 0.0943(2) 0.92794(12) 0.0252(8) Uani 1 1 d . . . H102 H 0.1282 0.0815 0.9416 0.030 Uiso 1 1 calc R . . C102 C 0.2307(3) 0.1577(2) 0.94307(11) 0.0202(7) Uani 1 1 d . . . H103 H 0.1946 0.1879 0.9670 0.024 Uiso 1 1 calc R . . C103 C 0.1108(3) 0.3603(2) 1.03050(10) 0.0148(6) Uani 1 1 d . . . C104 C 0.0472(3) 0.3747(2) 0.99551(11) 0.0211(7) Uani 1 1 d . . . H105 H 0.0823 0.3653 0.9682 0.025 Uiso 1 1 calc R . . C105 C -0.0684(3) 0.4031(2) 1.00054(11) 0.0249(8) Uani 1 1 d . . . H106 H -0.1125 0.4134 0.9766 0.030 Uiso 1 1 calc R . . C106 C -0.1197(3) 0.4165(2) 1.04039(11) 0.0234(8) Uani 1 1 d . . . H107 H -0.1988 0.4350 1.0437 0.028 Uiso 1 1 calc R . . C107 C -0.0559(3) 0.4030(2) 1.07517(11) 0.0268(8) Uani 1 1 d . . . H108 H -0.0909 0.4126 1.1025 0.032 Uiso 1 1 calc R . . C108 C 0.0590(3) 0.3755(2) 1.07018(11) 0.0230(8) Uani 1 1 d . . . H109 H 0.1030 0.3670 1.0941 0.028 Uiso 1 1 calc R . . C109 C 0.3044(3) 0.2252(2) 1.05749(10) 0.0143(6) Uani 1 1 d . . . C110 C 0.2331(3) 0.1741(2) 1.06780(11) 0.0197(7) Uani 1 1 d . . . H111 H 0.1593 0.1907 1.0583 0.024 Uiso 1 1 calc R . . C111 C 0.2712(3) 0.0988(2) 1.09207(11) 0.0232(8) Uani 1 1 d . . . H112 H 0.2232 0.0638 1.0991 0.028 Uiso 1 1 calc R . . C112 C 0.3786(3) 0.0745(2) 1.10606(11) 0.0232(8) Uani 1 1 d . . . H113 H 0.4039 0.0231 1.1228 0.028 Uiso 1 1 calc R . . C113 C 0.4497(3) 0.1251(2) 1.09561(10) 0.0206(7) Uani 1 1 d . . . H114 H 0.5235 0.1080 1.1052 0.025 Uiso 1 1 calc R . . C114 C 0.4132(3) 0.2004(2) 1.07131(10) 0.0171(7) Uani 1 1 d . . . H115 H 0.4617 0.2349 1.0641 0.021 Uiso 1 1 calc R . . C115 C 0.3162(2) 0.40096(19) 1.04487(10) 0.0137(6) Uani 1 1 d . . . C116 C 0.3245(3) 0.4059(2) 1.08787(10) 0.0176(7) Uani 1 1 d . . . H117 H 0.3057 0.3647 1.1071 0.021 Uiso 1 1 calc R . . C117 C 0.3604(3) 0.4714(2) 1.10273(11) 0.0212(7) Uani 1 1 d . . . H118 H 0.3669 0.4746 1.1321 0.025 Uiso 1 1 calc R . . C118 C 0.3868(3) 0.5322(2) 1.07451(11) 0.0227(7) Uani 1 1 d . . . H119 H 0.4096 0.5777 1.0847 0.027 Uiso 1 1 calc R . . C119 C 0.3800(3) 0.5265(2) 1.03197(11) 0.0201(7) Uani 1 1 d . . . H120 H 0.3987 0.5678 1.0128 0.024 Uiso 1 1 calc R . . C120 C 0.3458(2) 0.4606(2) 1.01690(10) 0.0164(7) Uani 1 1 d . . . H121 H 0.3426 0.4562 0.9875 0.020 Uiso 1 1 calc R . . N1 N 1.1273(2) 0.37131(17) 0.21039(8) 0.0147(5) Uani 1 1 d . . . N2 N 0.8224(2) 0.54489(16) 0.23406(8) 0.0137(5) Uani 1 1 d . . . N3 N 0.7059(2) -0.06983(16) 0.25417(8) 0.0143(5) Uani 1 1 d . . . N4 N 0.4260(2) 0.13025(17) 0.27593(8) 0.0142(5) Uani 1 1 d . . . N5 N 0.9147(2) 0.33304(18) 0.30161(9) 0.0194(6) Uani 1 1 d . . . N6 N 0.8505(2) 0.33864(18) 0.17595(9) 0.0180(6) Uani 1 1 d . . . N7 N 0.6394(2) 0.14083(18) 0.18256(9) 0.0185(6) Uani 1 1 d . . . N8 N 0.7252(2) 0.12420(18) 0.30726(9) 0.0219(6) Uani 1 1 d . . . N9 N 0.9897(2) 0.10735(19) 0.29383(10) 0.0240(7) Uani 1 1 d . . . N10 N 0.8454(2) 0.19147(19) 0.40762(9) 0.0212(6) Uani 1 1 d . . . N11 N 0.5877(3) 0.3716(2) 0.34459(10) 0.0275(7) Uani 1 1 d . . . N12 N 0.6376(2) 0.3348(2) 0.23417(10) 0.0259(7) Uani 1 1 d . . . N13 N 0.9065(2) 0.15634(18) 0.08827(9) 0.0221(6) Uani 1 1 d . . . N14 N 0.6310(2) 0.32677(18) 0.08970(8) 0.0176(6) Uani 1 1 d . . . P1 P 0.24560(7) 0.18695(5) 0.46969(3) 0.01377(16) Uani 1 1 d . . . P2 P 0.13601(7) 0.26278(5) 0.55010(3) 0.01505(17) Uani 1 1 d . . . P3 P 0.37916(6) 0.25511(5) 0.94387(2) 0.01253(16) Uani 1 1 d . . . P4 P 0.26035(6) 0.32182(5) 1.02465(3) 0.01263(16) Uani 1 1 d . . . O1 O 0.9299(2) 0.16150(16) 0.26753(8) 0.0256(6) Uani 1 1 d . . . O2 O 1.0601(2) 0.04355(17) 0.28159(9) 0.0369(7) Uani 1 1 d . . . O3 O 0.9705(2) 0.12472(18) 0.33158(8) 0.0345(7) Uani 1 1 d . . . O4 O 0.8654(2) 0.25839(16) 0.38993(8) 0.0281(6) Uani 1 1 d . . . O5 O 0.8826(2) 0.16068(17) 0.44133(8) 0.0313(6) Uani 1 1 d . . . O6 O 0.7831(2) 0.16024(17) 0.38796(8) 0.0284(6) Uani 1 1 d . . . O7 O 0.6822(2) 0.38757(16) 0.34004(9) 0.0307(6) Uani 1 1 d . . . O8 O 0.5012(2) 0.42644(19) 0.35185(10) 0.0418(7) Uani 1 1 d . . . O9 O 0.5922(2) 0.29312(17) 0.34059(9) 0.0340(6) Uani 1 1 d . . . O10 O 0.7225(2) 0.27310(16) 0.24460(7) 0.0233(5) Uani 1 1 d . . . O11 O 0.5849(3) 0.3880(2) 0.25857(9) 0.0614(10) Uani 1 1 d . . . O12 O 0.60954(19) 0.33903(15) 0.19682(8) 0.0232(5) Uani 1 1 d . . . O13 O 0.81188(19) 0.14170(15) 0.09840(7) 0.0221(5) Uani 1 1 d . . . O14 O 0.9633(2) 0.12450(18) 0.05759(8) 0.0360(7) Uani 1 1 d . . . O15 O 0.93574(19) 0.20407(15) 0.11201(8) 0.0248(5) Uani 1 1 d . . . O16 O 0.59457(18) 0.27484(15) 0.11370(7) 0.0207(5) Uani 1 1 d . . . O17 O 0.58569(19) 0.36050(16) 0.05798(7) 0.0260(6) Uani 1 1 d . . . O18 O 0.72048(18) 0.34050(15) 0.10070(7) 0.0216(5) Uani 1 1 d . . . N15 N 0.2195(2) 0.20385(18) 0.51799(8) 0.0181(6) Uani 1 1 d . . . N16 N 0.2925(2) 0.31094(17) 0.97606(8) 0.0159(6) Uani 1 1 d . . . C1S C 0.2966(4) 0.8704(3) 0.30347(14) 0.0376(10) Uani 1 1 d . . . H1S1 H 0.3573 0.8956 0.2950 0.056 Uiso 1 1 calc R . . H1S2 H 0.2875 0.8672 0.3343 0.056 Uiso 1 1 calc R . . H1S3 H 0.2271 0.9062 0.2918 0.056 Uiso 1 1 calc R . . C2S C 0.3227(3) 0.7856(3) 0.28784(15) 0.0407(11) Uani 1 1 d . . . C3S C 0.3442(5) 0.6349(4) 0.39498(18) 0.0737(17) Uani 1 1 d . . . H3S1 H 0.4182 0.6024 0.3840 0.111 Uiso 1 1 calc R . . H3S2 H 0.2996 0.6650 0.3716 0.111 Uiso 1 1 calc R . . H3S3 H 0.3069 0.5956 0.4098 0.111 Uiso 1 1 calc R . . C4S C 0.3557(5) 0.6963(4) 0.42360(17) 0.0554(13) Uani 1 1 d . . . C5S C 0.8848(4) 0.0811(3) 0.92596(13) 0.0407(10) Uani 1 1 d . . . H5S1 H 0.8042 0.0923 0.9236 0.061 Uiso 1 1 calc R . . H5S2 H 0.9015 0.1348 0.9307 0.061 Uiso 1 1 calc R . . H5S3 H 0.9097 0.0401 0.9496 0.061 Uiso 1 1 calc R . . C6S C 0.9429(3) 0.0457(2) 0.88719(12) 0.0268(8) Uani 1 1 d . . . C7S C 0.1757(4) 0.6714(4) 0.19948(15) 0.0533(14) Uani 1 1 d . . . H7S1 H 0.2334 0.6167 0.1961 0.080 Uiso 1 1 calc R . . H7S2 H 0.1023 0.6636 0.1957 0.080 Uiso 1 1 calc R . . H7S3 H 0.1775 0.6914 0.2277 0.080 Uiso 1 1 calc R . . C8S C 0.1963(3) 0.7334(3) 0.16859(13) 0.0311(9) Uani 1 1 d . . . C9S C 0.5851(3) 0.3164(3) 0.44581(14) 0.0410(10) Uani 1 1 d . . . H9S1 H 0.5540 0.2861 0.4264 0.061 Uiso 1 1 calc R . . H9S2 H 0.6012 0.2821 0.4722 0.061 Uiso 1 1 calc R . . H9S3 H 0.6542 0.3258 0.4330 0.061 Uiso 1 1 calc R . . C10S C 0.5055(4) 0.3980(3) 0.45433(15) 0.0435(11) Uani 1 1 d . . . N1S N 0.2159(3) 0.7808(3) 0.14401(13) 0.0499(10) Uani 1 1 d . . . N2S N 0.3428(4) 0.7190(3) 0.27473(18) 0.0732(15) Uani 1 1 d . . . N3S N 0.3674(5) 0.7431(4) 0.44720(16) 0.0826(17) Uani 1 1 d . . . N4S N 0.9877(3) 0.0162(2) 0.85731(11) 0.0333(8) Uani 1 1 d . . . N5S N 0.4425(4) 0.4624(3) 0.46046(17) 0.0767(15) Uani 1 1 d . . . O1S O 0.88985(19) 0.11819(15) 0.19252(7) 0.0236(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01182(6) 0.01122(6) 0.01049(6) -0.00013(4) -0.00152(4) -0.00311(5) Ir2 0.01380(6) 0.01051(6) 0.01124(6) 0.00053(4) -0.00252(4) -0.00341(5) Eu1 0.01443(8) 0.01461(8) 0.01202(8) -0.00056(6) -0.00201(6) -0.00567(6) Eu2 0.01408(8) 0.01355(8) 0.01237(8) 0.00007(6) -0.00266(6) -0.00488(6) C1 0.0212(16) 0.0150(16) 0.0117(16) 0.0026(12) -0.0019(13) -0.0043(13) C2 0.0256(18) 0.0159(17) 0.0153(17) 0.0008(13) 0.0004(14) -0.0003(14) C3 0.0186(17) 0.027(2) 0.0169(18) 0.0062(14) 0.0035(14) 0.0030(15) C4 0.0140(16) 0.0272(19) 0.0205(18) 0.0064(14) -0.0012(13) -0.0030(14) C5 0.0162(15) 0.0194(17) 0.0104(15) 0.0048(12) 0.0001(12) -0.0063(13) C6 0.0208(16) 0.0170(16) 0.0132(16) 0.0041(12) -0.0034(13) -0.0089(14) C7 0.0220(17) 0.029(2) 0.0226(19) 0.0018(15) -0.0072(14) -0.0132(16) C8 0.035(2) 0.028(2) 0.0218(19) 0.0000(15) -0.0093(16) -0.0212(17) C9 0.042(2) 0.0187(18) 0.0131(17) -0.0011(13) -0.0035(15) -0.0137(16) C10 0.0229(17) 0.0171(16) 0.0153(17) 0.0022(13) -0.0023(13) -0.0078(14) C11 0.0174(15) 0.0128(15) 0.0096(15) 0.0039(12) -0.0018(12) -0.0059(13) C12 0.0165(15) 0.0137(15) 0.0103(15) -0.0003(12) -0.0023(12) -0.0046(13) C13 0.0211(17) 0.0193(17) 0.0161(17) 0.0002(13) 0.0000(13) -0.0005(14) C14 0.0248(18) 0.030(2) 0.0160(18) 0.0025(14) 0.0039(14) -0.0059(16) C15 0.0278(19) 0.0245(19) 0.0200(18) 0.0124(14) -0.0037(15) -0.0102(16) C16 0.0208(17) 0.0160(17) 0.0204(18) 0.0022(13) -0.0080(14) -0.0027(14) C17 0.0170(15) 0.0159(16) 0.0130(16) -0.0010(12) -0.0044(12) -0.0052(13) C18 0.0147(15) 0.0169(16) 0.0189(17) -0.0021(13) -0.0032(13) -0.0057(13) C19 0.0197(17) 0.0167(17) 0.0239(19) 0.0013(14) -0.0030(14) -0.0006(14) C20 0.0151(16) 0.0247(19) 0.033(2) -0.0038(16) 0.0007(15) 0.0008(15) C21 0.0189(17) 0.027(2) 0.0221(19) -0.0034(15) 0.0038(14) -0.0049(15) C22 0.0170(16) 0.0211(17) 0.0151(17) -0.0024(13) 0.0014(13) -0.0051(14) C23 0.0108(14) 0.0164(16) 0.0146(16) -0.0057(13) -0.0027(12) -0.0041(13) C24 0.0147(15) 0.0159(16) 0.0080(15) 0.0011(12) 0.0006(12) -0.0028(13) C25 0.0202(16) 0.0184(17) 0.0152(17) -0.0011(13) -0.0006(13) -0.0042(14) C26 0.0237(18) 0.0241(19) 0.0225(19) -0.0040(15) 0.0007(14) -0.0033(15) C27 0.0259(19) 0.0174(18) 0.030(2) -0.0019(15) -0.0014(16) 0.0046(15) C28 0.0280(18) 0.0158(17) 0.0218(19) 0.0044(14) -0.0059(15) -0.0028(15) C29 0.0232(17) 0.0145(16) 0.0154(17) -0.0012(12) -0.0060(13) -0.0064(14) C30 0.0185(16) 0.0154(16) 0.0137(16) -0.0006(12) -0.0030(13) -0.0055(13) C31 0.0233(18) 0.0193(18) 0.0222(19) 0.0048(14) -0.0067(14) -0.0047(15) C32 0.032(2) 0.027(2) 0.0206(19) 0.0094(15) -0.0019(15) -0.0116(17) C33 0.0278(19) 0.031(2) 0.0141(17) 0.0028(14) 0.0027(14) -0.0098(16) C34 0.0233(17) 0.0176(17) 0.0167(17) -0.0007(13) -0.0014(14) -0.0040(14) C35 0.0202(16) 0.0161(16) 0.0128(16) 0.0006(12) -0.0054(13) -0.0075(13) C36 0.0152(15) 0.0147(16) 0.0111(15) 0.0021(12) -0.0015(12) -0.0076(13) C37 0.0187(16) 0.0178(17) 0.0154(17) 0.0005(13) 0.0025(13) -0.0047(14) C38 0.0256(18) 0.0226(18) 0.0180(18) -0.0045(14) 0.0020(14) -0.0117(15) C39 0.0218(17) 0.032(2) 0.0174(18) -0.0026(14) -0.0023(14) -0.0158(16) C40 0.0150(16) 0.0293(19) 0.0155(17) 0.0007(14) -0.0008(13) -0.0071(14) C41 0.0174(15) 0.0165(16) 0.0102(15) 0.0034(12) -0.0001(12) -0.0059(13) C42 0.0194(16) 0.0167(16) 0.0101(15) 0.0031(12) -0.0003(12) -0.0059(13) C43 0.0177(16) 0.0214(18) 0.0208(18) 0.0048(14) -0.0004(13) -0.0042(14) C44 0.0242(18) 0.0205(18) 0.0153(17) 0.0009(13) 0.0047(14) 0.0035(15) C45 0.0317(19) 0.0144(17) 0.0155(17) -0.0007(13) -0.0021(14) 0.0005(15) C46 0.0231(17) 0.0130(16) 0.0177(17) 0.0000(13) -0.0071(14) -0.0020(14) C47 0.0104(14) 0.0134(15) 0.0139(16) -0.0010(12) -0.0033(12) -0.0011(12) C48 0.0196(16) 0.0127(16) 0.0142(16) 0.0032(12) -0.0046(13) -0.0029(13) C49 0.0158(15) 0.0132(16) 0.0145(16) -0.0029(12) 0.0008(12) -0.0029(13) C50 0.0214(17) 0.0228(18) 0.0129(16) -0.0011(13) -0.0013(13) -0.0027(14) C51 0.0195(17) 0.029(2) 0.0207(19) 0.0016(15) -0.0048(14) -0.0033(15) C52 0.0151(16) 0.0218(18) 0.028(2) 0.0023(15) 0.0011(14) -0.0015(14) C53 0.0214(17) 0.030(2) 0.0174(18) -0.0006(14) 0.0042(14) -0.0058(15) C54 0.0209(17) 0.0248(18) 0.0140(17) -0.0015(13) -0.0018(13) -0.0058(15) C55 0.0192(16) 0.0140(16) 0.0128(16) -0.0013(12) 0.0002(12) -0.0019(13) C56 0.0234(18) 0.0229(19) 0.0204(18) -0.0039(14) 0.0004(14) -0.0060(15) C57 0.033(2) 0.0159(17) 0.026(2) 0.0007(14) 0.0025(16) -0.0083(16) C58 0.035(2) 0.0179(18) 0.0200(19) 0.0032(14) -0.0024(15) -0.0027(16) C59 0.0275(19) 0.0225(19) 0.0215(19) 0.0016(14) -0.0089(15) -0.0020(15) C60 0.0197(16) 0.0206(18) 0.0186(17) -0.0008(13) -0.0032(13) -0.0054(14) C61 0.0138(15) 0.0170(16) 0.0167(17) -0.0020(13) -0.0017(12) -0.0019(13) C62 0.0226(17) 0.0222(18) 0.0154(17) 0.0005(13) -0.0030(13) -0.0052(15) C63 0.0229(18) 0.0233(19) 0.026(2) -0.0063(15) -0.0064(15) -0.0019(15) C64 0.0258(19) 0.0190(18) 0.037(2) -0.0050(15) -0.0094(16) -0.0071(15) C65 0.0240(18) 0.0225(19) 0.035(2) 0.0059(16) -0.0033(16) -0.0077(16) C66 0.0184(16) 0.0194(17) 0.0159(17) 0.0020(13) -0.0038(13) -0.0019(14) C67 0.0162(16) 0.0257(18) 0.0110(16) -0.0018(13) 0.0008(12) 0.0012(14) C68 0.0252(18) 0.0228(19) 0.0221(19) -0.0015(14) -0.0045(15) 0.0000(15) C69 0.030(2) 0.029(2) 0.036(2) -0.0028(17) -0.0071(18) 0.0103(17) C70 0.0217(19) 0.049(3) 0.029(2) -0.0061(19) -0.0062(16) 0.0066(18) C71 0.0218(19) 0.047(3) 0.033(2) -0.0157(19) -0.0049(16) -0.0025(18) C72 0.0212(18) 0.031(2) 0.024(2) -0.0065(15) -0.0002(15) -0.0016(16) C73 0.0247(17) 0.0201(17) 0.0120(16) -0.0027(13) -0.0002(13) -0.0112(14) C74 0.032(2) 0.0251(19) 0.0220(19) -0.0073(15) 0.0091(15) -0.0119(17) C75 0.053(3) 0.042(3) 0.025(2) -0.0066(18) 0.0133(19) -0.030(2) C76 0.070(3) 0.037(2) 0.021(2) -0.0002(17) 0.004(2) -0.035(2) C77 0.060(3) 0.022(2) 0.024(2) 0.0047(16) -0.0101(19) -0.014(2) C78 0.035(2) 0.0212(19) 0.0199(19) -0.0006(14) -0.0076(15) -0.0049(16) C79 0.0256(18) 0.0146(16) 0.0161(17) 0.0024(13) -0.0063(14) -0.0028(14) C80 0.0275(19) 0.0194(18) 0.0205(18) 0.0006(14) -0.0057(15) -0.0026(15) C81 0.046(2) 0.0193(19) 0.022(2) -0.0064(15) -0.0108(17) -0.0035(17) C82 0.040(2) 0.022(2) 0.041(2) -0.0023(17) -0.0169(19) -0.0107(18) C83 0.0247(19) 0.033(2) 0.038(2) -0.0013(17) -0.0068(17) -0.0108(17) C84 0.0217(17) 0.0258(19) 0.0234(19) -0.0039(15) -0.0036(14) -0.0050(15) C85 0.0147(15) 0.0188(17) 0.0099(15) -0.0018(12) -0.0001(12) -0.0028(13) C86 0.0201(16) 0.0169(17) 0.0194(17) 0.0009(13) -0.0023(13) -0.0054(14) C87 0.0233(17) 0.0169(17) 0.0225(19) 0.0023(14) -0.0022(14) -0.0003(14) C88 0.0196(17) 0.031(2) 0.0160(17) 0.0004(14) -0.0034(14) 0.0000(15) C89 0.0161(16) 0.029(2) 0.0211(19) -0.0102(15) -0.0024(14) -0.0045(15) C90 0.0201(16) 0.0150(16) 0.0215(18) -0.0022(13) -0.0012(14) -0.0045(14) C91 0.0195(16) 0.0132(15) 0.0119(16) -0.0019(12) -0.0025(12) -0.0054(13) C92 0.0194(16) 0.0145(16) 0.0157(16) -0.0015(12) -0.0015(13) -0.0051(13) C93 0.0243(18) 0.0278(19) 0.0134(17) 0.0013(14) -0.0015(13) -0.0113(15) C94 0.033(2) 0.0231(19) 0.0185(18) 0.0068(14) -0.0060(15) -0.0137(16) C95 0.0310(19) 0.0157(17) 0.0209(18) 0.0017(14) -0.0066(15) -0.0032(15) C96 0.0232(17) 0.0211(18) 0.0160(17) -0.0043(13) -0.0028(14) -0.0040(15) C97 0.0155(15) 0.0104(15) 0.0151(16) -0.0001(12) -0.0027(12) -0.0022(12) C98 0.0176(16) 0.0165(16) 0.0161(17) -0.0014(13) -0.0037(13) -0.0050(13) C99 0.0229(17) 0.0149(17) 0.0230(18) -0.0018(13) -0.0080(14) -0.0007(14) C100 0.0259(18) 0.0207(18) 0.026(2) 0.0006(14) -0.0102(15) -0.0112(15) C101 0.0230(18) 0.027(2) 0.030(2) 0.0046(15) -0.0049(15) -0.0130(16) C102 0.0214(17) 0.0214(18) 0.0180(17) 0.0011(13) -0.0036(14) -0.0064(14) C103 0.0161(15) 0.0126(15) 0.0161(16) 0.0014(12) -0.0003(12) -0.0053(13) C104 0.0177(16) 0.0253(19) 0.0174(17) -0.0024(14) 0.0009(13) -0.0018(14) C105 0.0182(17) 0.034(2) 0.0204(19) -0.0010(15) -0.0069(14) -0.0037(16) C106 0.0130(15) 0.029(2) 0.0257(19) 0.0063(15) -0.0003(14) -0.0031(15) C107 0.0193(17) 0.039(2) 0.0162(18) 0.0058(15) 0.0043(14) -0.0017(16) C108 0.0196(17) 0.033(2) 0.0156(17) 0.0033(14) -0.0041(14) -0.0061(15) C109 0.0178(15) 0.0138(16) 0.0111(15) -0.0037(12) -0.0010(12) -0.0033(13) C110 0.0184(16) 0.0216(18) 0.0211(18) -0.0018(14) -0.0047(13) -0.0080(14) C111 0.0279(19) 0.0170(17) 0.027(2) 0.0000(14) -0.0020(15) -0.0095(15) C112 0.0298(19) 0.0145(17) 0.0211(18) 0.0005(13) 0.0011(15) -0.0005(15) C113 0.0170(16) 0.0213(18) 0.0182(17) 0.0019(14) 0.0009(13) 0.0018(14) C114 0.0150(15) 0.0215(17) 0.0148(16) -0.0009(13) 0.0015(12) -0.0059(14) C115 0.0122(14) 0.0127(15) 0.0154(16) -0.0005(12) -0.0006(12) -0.0022(12) C116 0.0222(17) 0.0164(17) 0.0141(16) -0.0015(13) 0.0022(13) -0.0060(14) C117 0.0243(18) 0.0246(19) 0.0168(17) -0.0052(14) 0.0011(14) -0.0096(15) C118 0.0236(18) 0.0219(18) 0.026(2) -0.0071(14) 0.0004(15) -0.0118(15) C119 0.0209(17) 0.0180(17) 0.0229(18) 0.0046(14) -0.0020(14) -0.0091(14) C120 0.0137(15) 0.0181(17) 0.0154(16) 0.0019(13) -0.0006(12) -0.0021(13) N1 0.0161(13) 0.0143(13) 0.0119(13) -0.0001(10) -0.0019(10) -0.0012(11) N2 0.0154(13) 0.0140(13) 0.0125(13) -0.0026(10) -0.0020(10) -0.0049(11) N3 0.0173(13) 0.0122(13) 0.0141(14) -0.0011(10) -0.0044(11) -0.0044(11) N4 0.0208(14) 0.0146(13) 0.0072(13) 0.0015(10) -0.0019(10) -0.0052(11) N5 0.0198(14) 0.0192(15) 0.0196(15) 0.0021(12) -0.0012(12) -0.0070(12) N6 0.0187(14) 0.0204(15) 0.0149(14) 0.0004(11) -0.0033(11) -0.0053(12) N7 0.0183(14) 0.0201(15) 0.0172(15) 0.0002(11) -0.0022(11) -0.0054(12) N8 0.0261(15) 0.0214(15) 0.0207(16) 0.0040(12) -0.0084(12) -0.0104(13) N9 0.0223(15) 0.0203(16) 0.0275(17) 0.0023(13) 0.0051(13) -0.0052(13) N10 0.0228(15) 0.0278(17) 0.0128(14) -0.0031(12) 0.0005(11) -0.0067(13) N11 0.0259(16) 0.0280(18) 0.0250(17) -0.0045(13) 0.0033(13) -0.0024(14) N12 0.0263(16) 0.0273(17) 0.0214(17) -0.0041(13) 0.0020(13) -0.0036(14) N13 0.0264(16) 0.0180(15) 0.0179(15) 0.0019(12) 0.0018(12) -0.0016(13) N14 0.0158(13) 0.0201(15) 0.0147(14) -0.0039(11) -0.0011(11) -0.0007(12) P1 0.0145(4) 0.0150(4) 0.0107(4) -0.0010(3) -0.0014(3) -0.0021(3) P2 0.0166(4) 0.0152(4) 0.0117(4) -0.0018(3) -0.0009(3) -0.0017(3) P3 0.0130(4) 0.0127(4) 0.0112(4) -0.0012(3) -0.0007(3) -0.0025(3) P4 0.0125(4) 0.0128(4) 0.0120(4) -0.0008(3) -0.0008(3) -0.0026(3) O1 0.0252(13) 0.0279(14) 0.0201(13) -0.0022(10) -0.0030(10) -0.0015(11) O2 0.0307(15) 0.0233(15) 0.0460(18) 0.0038(12) 0.0171(13) 0.0038(12) O3 0.0306(14) 0.0436(17) 0.0159(13) 0.0056(12) -0.0016(11) 0.0093(13) O4 0.0444(16) 0.0264(14) 0.0200(13) 0.0043(10) -0.0132(12) -0.0193(12) O5 0.0408(15) 0.0377(16) 0.0146(13) 0.0063(11) -0.0099(11) -0.0095(13) O6 0.0337(14) 0.0415(16) 0.0188(13) 0.0050(11) -0.0055(11) -0.0251(13) O7 0.0247(13) 0.0263(14) 0.0432(17) -0.0100(12) -0.0026(12) -0.0088(12) O8 0.0309(15) 0.0371(17) 0.0482(19) -0.0082(14) 0.0047(13) 0.0046(14) O9 0.0245(14) 0.0252(15) 0.0515(19) -0.0021(12) 0.0061(12) -0.0076(12) O10 0.0270(13) 0.0274(14) 0.0179(12) 0.0070(10) -0.0075(10) -0.0116(11) O11 0.081(3) 0.056(2) 0.0245(17) -0.0171(15) -0.0029(16) 0.0203(19) O12 0.0202(12) 0.0254(13) 0.0219(13) -0.0033(10) -0.0038(10) -0.0019(10) O13 0.0243(13) 0.0230(13) 0.0209(13) -0.0064(10) -0.0004(10) -0.0089(11) O14 0.0376(16) 0.0391(17) 0.0236(15) -0.0046(12) 0.0121(12) -0.0009(13) O15 0.0210(12) 0.0231(13) 0.0303(14) -0.0033(11) 0.0011(10) -0.0065(11) O16 0.0192(12) 0.0256(13) 0.0195(13) 0.0057(10) -0.0029(10) -0.0106(10) O17 0.0237(13) 0.0334(15) 0.0147(12) 0.0073(10) -0.0067(10) 0.0011(11) O18 0.0198(12) 0.0247(13) 0.0229(13) 0.0060(10) -0.0064(10) -0.0107(10) N15 0.0183(14) 0.0210(15) 0.0123(14) -0.0029(11) 0.0002(11) -0.0013(12) N16 0.0143(13) 0.0182(14) 0.0124(14) -0.0027(11) 0.0005(10) 0.0000(11) C1S 0.044(2) 0.037(2) 0.037(2) -0.0027(18) 0.0046(19) -0.021(2) C2S 0.030(2) 0.036(3) 0.061(3) 0.004(2) 0.006(2) -0.020(2) C3S 0.082(4) 0.090(5) 0.055(4) -0.022(3) -0.015(3) -0.026(4) C4S 0.064(3) 0.068(4) 0.044(3) -0.005(3) 0.006(3) -0.036(3) C5S 0.041(2) 0.044(3) 0.028(2) -0.0053(19) 0.0031(18) 0.001(2) C6S 0.0244(19) 0.0232(19) 0.029(2) -0.0017(16) -0.0036(16) -0.0011(16) C7S 0.051(3) 0.082(4) 0.038(3) 0.020(3) -0.011(2) -0.039(3) C8S 0.0242(19) 0.031(2) 0.037(2) 0.0006(18) -0.0034(17) -0.0051(17) C9S 0.036(2) 0.043(3) 0.045(3) -0.003(2) -0.008(2) -0.010(2) C10S 0.035(2) 0.055(3) 0.044(3) -0.015(2) 0.007(2) -0.017(2) N1S 0.045(2) 0.040(2) 0.063(3) 0.017(2) -0.012(2) -0.0108(19) N2S 0.064(3) 0.044(3) 0.117(4) -0.017(3) 0.031(3) -0.029(2) N3S 0.109(4) 0.102(4) 0.062(3) -0.024(3) 0.028(3) -0.072(4) N4S 0.0307(18) 0.0327(19) 0.0299(19) -0.0039(15) -0.0033(15) 0.0021(15) N5S 0.064(3) 0.070(3) 0.083(4) -0.034(3) 0.012(3) 0.003(3) O1S 0.0232(12) 0.0224(13) 0.0208(13) -0.0005(10) -0.0053(10) 0.0012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C24 2.036(3) . ? Ir1 C23 2.042(3) . ? Ir1 N1 2.056(3) . ? Ir1 C11 2.057(3) . ? Ir1 C12 2.057(3) . ? Ir1 N2 2.060(3) . ? Ir2 C48 2.028(3) . ? Ir2 C47 2.048(3) . ? Ir2 C36 2.050(3) . ? Ir2 N4 2.052(3) . ? Ir2 N3 2.057(3) . ? Ir2 C35 2.060(3) . ? Eu1 N8 2.414(3) . ? Eu1 N5 2.433(3) . ? Eu1 O6 2.449(2) . ? Eu1 O7 2.453(3) . ? Eu1 O4 2.458(2) . ? Eu1 O9 2.463(3) . ? Eu1 O1 2.504(2) . ? Eu1 O3 2.506(2) . ? Eu1 O10 2.640(2) . ? Eu1 N10 2.870(3) . ? Eu1 N11 2.900(3) . ? Eu1 N9 2.925(3) . ? Eu2 O1S 2.383(2) . ? Eu2 O18 2.424(2) . ? Eu2 N6 2.437(3) . ? Eu2 O12 2.445(2) . ? Eu2 O13 2.452(2) . ? Eu2 N7 2.466(3) . ? Eu2 O16 2.473(2) . ? Eu2 O15 2.544(2) . ? Eu2 O10 2.832(2) . ? Eu2 N14 2.875(3) . ? Eu2 N13 2.927(3) . ? Eu2 N12 3.059(3) . ? C1 N1 1.357(4) . ? C1 C2 1.379(5) . ? C1 H1 0.9500 . ? C2 C3 1.388(5) . ? C2 H2 0.9500 . ? C3 C4 1.372(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? C5 N1 1.370(4) . ? C5 C6 1.468(5) . ? C6 C7 1.398(4) . ? C6 C11 1.410(4) . ? C7 C8 1.380(5) . ? C7 H7 0.9500 . ? C8 C9 1.388(5) . ? C8 H8 0.9500 . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C10 C11 1.399(5) . ? C10 H10 0.9500 . ? C12 C13 1.392(4) . ? C12 C17 1.416(4) . ? C13 C14 1.394(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 C16 1.395(5) . ? C15 H15 0.9500 . ? C16 C17 1.403(4) . ? C16 H16 0.9500 . ? C17 C18 1.467(4) . ? C18 N2 1.359(4) . ? C18 C19 1.393(4) . ? C19 C20 1.381(5) . ? C19 H19 0.9500 . ? C20 C21 1.394(5) . ? C20 H20 0.9500 . ? C21 C22 1.372(5) . ? C21 H21 0.9500 . ? C22 N2 1.365(4) . ? C22 H22 0.9500 . ? C23 N5 1.148(4) . ? C24 N6 1.158(4) . ? C25 N3 1.354(4) . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C26 C27 1.389(5) . ? C26 H26 0.9500 . ? C27 C28 1.371(5) . ? C27 H27 0.9500 . ? C28 C29 1.401(5) . ? C28 H28 0.9500 . ? C29 N3 1.358(4) . ? C29 C30 1.470(5) . ? C30 C35 1.405(4) . ? C30 C31 1.405(4) . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 C33 1.397(5) . ? C32 H32 0.9500 . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.401(5) . ? C34 H34 0.9500 . ? C36 C37 1.400(5) . ? C36 C41 1.419(4) . ? C37 C38 1.399(4) . ? C37 H37 0.9500 . ? C38 C39 1.382(5) . ? C38 H38 0.9500 . ? C39 C40 1.381(5) . ? C39 H39 0.9500 . ? C40 C41 1.397(4) . ? C40 H40 0.9500 . ? C41 C42 1.468(5) . ? C42 N4 1.366(4) . ? C42 C43 1.396(5) . ? C43 C44 1.382(5) . ? C43 H43 0.9500 . ? C44 C45 1.384(5) . ? C44 H44 0.9500 . ? C45 C46 1.373(5) . ? C45 H45 0.9500 . ? C46 N4 1.358(4) . ? C46 H46 0.9500 . ? C47 N7 1.151(4) . ? C48 N8 1.152(4) . ? C49 C50 1.389(4) . ? C49 C54 1.394(5) . ? C49 P1 1.797(3) . ? C50 C51 1.385(5) . ? C50 H51 0.9500 . ? C51 C52 1.385(5) . ? C51 H52 0.9500 . ? C52 C53 1.384(5) . ? C52 H53 0.9500 . ? C53 C54 1.383(5) . ? C53 H54 0.9500 . ? C54 H55 0.9500 . ? C55 C56 1.396(5) . ? C55 C60 1.396(4) . ? C55 P1 1.799(3) . ? C56 C57 1.384(5) . ? C56 H57 0.9500 . ? C57 C58 1.389(5) . ? C57 H58 0.9500 . ? C58 C59 1.381(5) . ? C58 H59 0.9500 . ? C59 C60 1.388(5) . ? C59 H60 0.9500 . ? C60 H61 0.9500 . ? C61 C62 1.394(5) . ? C61 C66 1.403(4) . ? C61 P1 1.795(3) . ? C62 C63 1.398(5) . ? C62 H63 0.9500 . ? C63 C64 1.391(5) . ? C63 H64 0.9500 . ? C64 C65 1.381(5) . ? C64 H65 0.9500 . ? C65 C66 1.387(5) . ? C65 H66 0.9500 . ? C66 H67 0.9500 . ? C67 C72 1.391(5) . ? C67 C68 1.396(5) . ? C67 P2 1.797(3) . ? C68 C69 1.388(5) . ? C68 H69 0.9500 . ? C69 C70 1.381(6) . ? C69 H70 0.9500 . ? C70 C71 1.388(6) . ? C70 H71 0.9500 . ? C71 C72 1.374(5) . ? C71 H72 0.9500 . ? C72 H73 0.9500 . ? C73 C78 1.393(5) . ? C73 C74 1.398(5) . ? C73 P2 1.792(3) . ? C74 C75 1.389(5) . ? C74 H75 0.9500 . ? C75 C76 1.385(6) . ? C75 H76 0.9500 . ? C76 C77 1.376(6) . ? C76 H77 0.9500 . ? C77 C78 1.385(5) . ? C77 H78 0.9500 . ? C78 H79 0.9500 . ? C79 C80 1.398(5) . ? C79 C84 1.403(5) . ? C79 P2 1.799(3) . ? C80 C81 1.389(5) . ? C80 H81 0.9500 . ? C81 C82 1.380(6) . ? C81 H82 0.9500 . ? C82 C83 1.385(6) . ? C82 H83 0.9500 . ? C83 C84 1.391(5) . ? C83 H84 0.9500 . ? C84 H85 0.9500 . ? C85 C90 1.394(4) . ? C85 C86 1.399(4) . ? C85 P3 1.805(3) . ? C86 C87 1.381(4) . ? C86 H87 0.9500 . ? C87 C88 1.383(5) . ? C87 H88 0.9500 . ? C88 C89 1.391(5) . ? C88 H89 0.9500 . ? C89 C90 1.386(4) . ? C89 H90 0.9500 . ? C90 H91 0.9500 . ? C91 C96 1.393(4) . ? C91 C92 1.398(4) . ? C91 P3 1.803(3) . ? C92 C93 1.390(4) . ? C92 H93 0.9500 . ? C93 C94 1.388(5) . ? C93 H94 0.9500 . ? C94 C95 1.379(5) . ? C94 H95 0.9500 . ? C95 C96 1.390(5) . ? C95 H96 0.9500 . ? C96 H97 0.9500 . ? C97 C102 1.398(4) . ? C97 C98 1.403(4) . ? C97 P3 1.799(3) . ? C98 C99 1.388(4) . ? C98 H99 0.9500 . ? C99 C100 1.394(5) . ? C99 H100 0.9500 . ? C100 C101 1.375(5) . ? C100 H101 0.9500 . ? C101 C102 1.390(5) . ? C101 H102 0.9500 . ? C102 H103 0.9500 . ? C103 C104 1.382(4) . ? C103 C108 1.386(5) . ? C103 P4 1.797(3) . ? C104 C105 1.389(5) . ? C104 H105 0.9500 . ? C105 C106 1.386(5) . ? C105 H106 0.9500 . ? C106 C107 1.378(5) . ? C106 H107 0.9500 . ? C107 C108 1.380(5) . ? C107 H108 0.9500 . ? C108 H109 0.9500 . ? C109 C114 1.397(4) . ? C109 C110 1.400(4) . ? C109 P4 1.804(3) . ? C110 C111 1.388(5) . ? C110 H111 0.9500 . ? C111 C112 1.384(5) . ? C111 H112 0.9500 . ? C112 C113 1.392(5) . ? C112 H113 0.9500 . ? C113 C114 1.387(4) . ? C113 H114 0.9500 . ? C114 H115 0.9500 . ? C115 C116 1.391(4) . ? C115 C120 1.391(4) . ? C115 P4 1.805(3) . ? C116 C117 1.392(5) . ? C116 H117 0.9500 . ? C117 C118 1.394(5) . ? C117 H118 0.9500 . ? C118 C119 1.375(5) . ? C118 H119 0.9500 . ? C119 C120 1.390(5) . ? C119 H120 0.9500 . ? C120 H121 0.9500 . ? N9 O2 1.220(4) . ? N9 O3 1.246(4) . ? N9 O1 1.285(4) . ? N10 O5 1.219(3) . ? N10 O6 1.263(3) . ? N10 O4 1.279(4) . ? N11 O8 1.210(4) . ? N11 O9 1.279(4) . ? N11 O7 1.282(4) . ? N12 O11 1.217(4) . ? N12 O12 1.255(4) . ? N12 O10 1.281(4) . ? N13 O14 1.221(4) . ? N13 O15 1.260(4) . ? N13 O13 1.292(4) . ? N14 O17 1.213(3) . ? N14 O16 1.268(3) . ? N14 O18 1.280(3) . ? P1 N15 1.577(3) . ? P2 N15 1.572(3) . ? P3 N16 1.569(3) . ? P4 N16 1.582(3) . ? C1S C2S 1.441(6) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S N2S 1.141(6) . ? C3S C4S 1.439(8) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S N3S 1.150(7) . ? C5S C6S 1.456(6) . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C6S N4S 1.134(5) . ? C7S C8S 1.433(6) . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C8S N1S 1.132(5) . ? C9S C10S 1.444(6) . ? C9S H9S1 0.9800 . ? C9S H9S2 0.9800 . ? C9S H9S3 0.9800 . ? C10S N5S 1.136(6) . ? 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 C24 Ir1 C23 84.92(12) . . ? C24 Ir1 N1 94.52(11) . . ? C23 Ir1 N1 93.97(11) . . ? C24 Ir1 C11 173.43(12) . . ? C23 Ir1 C11 92.39(11) . . ? N1 Ir1 C11 79.67(11) . . ? C24 Ir1 C12 96.03(12) . . ? C23 Ir1 C12 173.73(12) . . ? N1 Ir1 C12 92.13(11) . . ? C11 Ir1 C12 87.29(12) . . ? C24 Ir1 N2 90.67(11) . . ? C23 Ir1 N2 94.17(11) . . ? N1 Ir1 N2 170.70(10) . . ? C11 Ir1 N2 95.51(11) . . ? C12 Ir1 N2 79.63(11) . . ? C48 Ir2 C47 85.52(12) . . ? C48 Ir2 C36 174.80(13) . . ? C47 Ir2 C36 93.80(12) . . ? C48 Ir2 N4 94.92(12) . . ? C47 Ir2 N4 92.09(11) . . ? C36 Ir2 N4 79.95(11) . . ? C48 Ir2 N3 88.48(11) . . ? C47 Ir2 N3 95.22(11) . . ? C36 Ir2 N3 96.72(11) . . ? N4 Ir2 N3 172.16(10) . . ? C48 Ir2 C35 93.58(12) . . ? C47 Ir2 C35 174.87(12) . . ? C36 Ir2 C35 87.54(12) . . ? N4 Ir2 C35 93.02(11) . . ? N3 Ir2 C35 79.70(12) . . ? N8 Eu1 N5 149.05(10) . . ? N8 Eu1 O6 71.98(9) . . ? N5 Eu1 O6 128.70(8) . . ? N8 Eu1 O7 127.23(9) . . ? N5 Eu1 O7 75.49(9) . . ? O6 Eu1 O7 102.10(9) . . ? N8 Eu1 O4 123.21(9) . . ? N5 Eu1 O4 78.44(9) . . ? O6 Eu1 O4 51.89(8) . . ? O7 Eu1 O4 77.76(9) . . ? N8 Eu1 O9 75.88(9) . . ? N5 Eu1 O9 126.14(9) . . ? O6 Eu1 O9 79.06(9) . . ? O7 Eu1 O9 52.01(8) . . ? O4 Eu1 O9 98.91(9) . . ? N8 Eu1 O1 74.81(9) . . ? N5 Eu1 O1 75.32(9) . . ? O6 Eu1 O1 113.76(9) . . ? O7 Eu1 O1 143.04(9) . . ? O4 Eu1 O1 117.49(8) . . ? O9 Eu1 O1 141.84(9) . . ? N8 Eu1 O3 81.73(10) . . ? N5 Eu1 O3 85.63(9) . . ? O6 Eu1 O3 68.96(9) . . ? O7 Eu1 O3 146.84(9) . . ? O4 Eu1 O3 71.83(9) . . ? O9 Eu1 O3 145.36(9) . . ? O1 Eu1 O3 50.64(8) . . ? N8 Eu1 O10 73.83(8) . . ? N5 Eu1 O10 86.97(8) . . ? O6 Eu1 O10 144.08(7) . . ? O7 Eu1 O10 89.88(8) . . ? O4 Eu1 O10 162.80(8) . . ? O9 Eu1 O10 82.29(9) . . ? O1 Eu1 O10 66.45(8) . . ? O3 Eu1 O10 116.45(8) . . ? N8 Eu1 N10 96.89(9) . . ? N5 Eu1 N10 103.01(9) . . ? O6 Eu1 N10 25.96(8) . . ? O7 Eu1 N10 93.02(9) . . ? O4 Eu1 N10 26.35(8) . . ? O9 Eu1 N10 91.96(9) . . ? O1 Eu1 N10 115.30(8) . . ? O3 Eu1 N10 64.67(8) . . ? O10 Eu1 N10 170.01(8) . . ? N8 Eu1 N11 101.41(10) . . ? N5 Eu1 N11 100.69(9) . . ? O6 Eu1 N11 91.49(9) . . ? O7 Eu1 N11 26.05(8) . . ? O4 Eu1 N11 89.08(9) . . ? O9 Eu1 N11 26.00(8) . . ? O1 Eu1 N11 150.91(8) . . ? O3 Eu1 N11 158.41(8) . . ? O10 Eu1 N11 84.68(8) . . ? N10 Eu1 N11 93.75(8) . . ? N8 Eu1 N9 74.22(9) . . ? N5 Eu1 N9 82.43(9) . . ? O6 Eu1 N9 89.66(9) . . ? O7 Eu1 N9 157.77(8) . . ? O4 Eu1 N9 95.55(9) . . ? O9 Eu1 N9 150.02(9) . . ? O1 Eu1 N9 25.93(8) . . ? O3 Eu1 N9 25.02(8) . . ? O10 Eu1 N9 91.46(8) . . ? N10 Eu1 N9 89.47(8) . . ? N11 Eu1 N9 174.88(9) . . ? O1S Eu2 O18 147.25(8) . . ? O1S Eu2 N6 93.07(8) . . ? O18 Eu2 N6 75.60(8) . . ? O1S Eu2 O12 123.20(8) . . ? O18 Eu2 O12 84.73(8) . . ? N6 Eu2 O12 77.20(9) . . ? O1S Eu2 O13 82.29(8) . . ? O18 Eu2 O13 79.48(8) . . ? N6 Eu2 O13 124.49(9) . . ? O12 Eu2 O13 147.89(8) . . ? O1S Eu2 N7 79.08(8) . . ? O18 Eu2 N7 125.83(8) . . ? N6 Eu2 N7 148.12(9) . . ? O12 Eu2 N7 81.48(9) . . ? O13 Eu2 N7 85.38(9) . . ? O1S Eu2 O16 145.34(8) . . ? O18 Eu2 O16 52.19(7) . . ? N6 Eu2 O16 121.28(8) . . ? O12 Eu2 O16 73.58(8) . . ? O13 Eu2 O16 74.64(8) . . ? N7 Eu2 O16 73.67(8) . . ? O1S Eu2 O15 73.48(8) . . ? O18 Eu2 O15 73.88(8) . . ? N6 Eu2 O15 74.23(9) . . ? O12 Eu2 O15 147.69(8) . . ? O13 Eu2 O15 51.32(8) . . ? N7 Eu2 O15 130.72(9) . . ? O16 Eu2 O15 109.26(8) . . ? O1S Eu2 O10 76.55(8) . . ? O18 Eu2 O10 124.20(8) . . ? N6 Eu2 O10 67.79(8) . . ? O12 Eu2 O10 47.70(7) . . ? O13 Eu2 O10 156.32(7) . . ? N7 Eu2 O10 80.33(8) . . ? O16 Eu2 O10 118.46(7) . . ? O15 Eu2 O10 129.48(7) . . ? O1S Eu2 N14 156.16(8) . . ? O18 Eu2 N14 26.22(7) . . ? N6 Eu2 N14 99.52(8) . . ? O12 Eu2 N14 79.59(8) . . ? O13 Eu2 N14 73.89(8) . . ? N7 Eu2 N14 99.61(8) . . ? O16 Eu2 N14 26.07(7) . . ? O15 Eu2 N14 90.50(8) . . ? O10 Eu2 N14 126.99(7) . . ? O1S Eu2 N13 77.38(8) . . ? O18 Eu2 N13 74.32(8) . . ? N6 Eu2 N13 98.98(9) . . ? O12 Eu2 N13 158.97(8) . . ? O13 Eu2 N13 25.93(8) . . ? N7 Eu2 N13 109.11(9) . . ? O16 Eu2 N13 91.61(8) . . ? O15 Eu2 N13 25.42(8) . . ? O10 Eu2 N13 149.89(7) . . ? N14 Eu2 N13 80.70(8) . . ? O1S Eu2 N12 101.10(8) . . ? O18 Eu2 N12 103.16(8) . . ? N6 Eu2 N12 69.18(9) . . ? O12 Eu2 N12 23.10(7) . . ? O13 Eu2 N12 165.99(8) . . ? N7 Eu2 N12 81.97(9) . . ? O16 Eu2 N12 95.92(8) . . ? O15 Eu2 N12 142.69(8) . . ? O10 Eu2 N12 24.74(7) . . ? N14 Eu2 N12 102.27(8) . . ? N13 Eu2 N12 168.06(8) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 119.8(3) . . ? N1 C5 C6 114.0(3) . . ? C4 C5 C6 126.1(3) . . ? C7 C6 C11 121.9(3) . . ? C7 C6 C5 122.6(3) . . ? C11 C6 C5 115.5(3) . . ? C8 C7 C6 119.6(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 119.7(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.5(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 116.7(3) . . ? C10 C11 Ir1 129.2(2) . . ? C6 C11 Ir1 114.1(2) . . ? C13 C12 C17 116.9(3) . . ? C13 C12 Ir1 129.2(2) . . ? C17 C12 Ir1 113.7(2) . . ? C12 C13 C14 122.0(3) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C12 121.4(3) . . ? C16 C17 C18 123.0(3) . . ? C12 C17 C18 115.6(3) . . ? N2 C18 C19 120.6(3) . . ? N2 C18 C17 114.2(3) . . ? C19 C18 C17 125.1(3) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 118.8(3) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 118.7(3) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N2 C22 C21 122.9(3) . . ? N2 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? N5 C23 Ir1 173.5(3) . . ? N6 C24 Ir1 172.3(3) . . ? N3 C25 C26 122.8(3) . . ? N3 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C27 118.2(3) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? N3 C29 C28 119.9(3) . . ? N3 C29 C30 114.9(3) . . ? C28 C29 C30 125.1(3) . . ? C35 C30 C31 121.8(3) . . ? C35 C30 C29 115.0(3) . . ? C31 C30 C29 123.1(3) . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.4(3) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 121.3(3) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C30 117.1(3) . . ? C34 C35 Ir2 128.9(2) . . ? C30 C35 Ir2 114.0(2) . . ? C37 C36 C41 116.3(3) . . ? C37 C36 Ir2 129.8(2) . . ? C41 C36 Ir2 113.9(2) . . ? C38 C37 C36 122.0(3) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 119.8(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 120.3(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C36 121.4(3) . . ? C40 C41 C42 123.3(3) . . ? C36 C41 C42 115.3(3) . . ? N4 C42 C43 119.8(3) . . ? N4 C42 C41 114.1(3) . . ? C43 C42 C41 126.0(3) . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 118.8(3) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C46 C45 C44 119.2(3) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? N4 C46 C45 122.5(3) . . ? N4 C46 H46 118.7 . . ? C45 C46 H46 118.7 . . ? N7 C47 Ir2 172.6(3) . . ? N8 C48 Ir2 175.2(3) . . ? C50 C49 C54 119.6(3) . . ? C50 C49 P1 119.6(2) . . ? C54 C49 P1 120.7(2) . . ? C51 C50 C49 119.9(3) . . ? C51 C50 H51 120.0 . . ? C49 C50 H51 120.0 . . ? C50 C51 C52 120.3(3) . . ? C50 C51 H52 119.9 . . ? C52 C51 H52 119.9 . . ? C53 C52 C51 119.9(3) . . ? C53 C52 H53 120.0 . . ? C51 C52 H53 120.0 . . ? C54 C53 C52 120.2(3) . . ? C54 C53 H54 119.9 . . ? C52 C53 H54 119.9 . . ? C53 C54 C49 120.1(3) . . ? C53 C54 H55 120.0 . . ? C49 C54 H55 120.0 . . ? C56 C55 C60 119.6(3) . . ? C56 C55 P1 120.6(2) . . ? C60 C55 P1 119.7(2) . . ? C57 C56 C55 120.6(3) . . ? C57 C56 H57 119.7 . . ? C55 C56 H57 119.7 . . ? C56 C57 C58 119.2(3) . . ? C56 C57 H58 120.4 . . ? C58 C57 H58 120.4 . . ? C59 C58 C57 120.7(3) . . ? C59 C58 H59 119.7 . . ? C57 C58 H59 119.7 . . ? C58 C59 C60 120.4(3) . . ? C58 C59 H60 119.8 . . ? C60 C59 H60 119.8 . . ? C59 C60 C55 119.4(3) . . ? C59 C60 H61 120.3 . . ? C55 C60 H61 120.3 . . ? C62 C61 C66 118.6(3) . . ? C62 C61 P1 122.0(3) . . ? C66 C61 P1 119.2(2) . . ? C61 C62 C63 120.7(3) . . ? C61 C62 H63 119.6 . . ? C63 C62 H63 119.6 . . ? C64 C63 C62 119.5(3) . . ? C64 C63 H64 120.2 . . ? C62 C63 H64 120.2 . . ? C65 C64 C63 120.3(3) . . ? C65 C64 H65 119.8 . . ? C63 C64 H65 119.8 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H66 119.9 . . ? C66 C65 H66 119.9 . . ? C65 C66 C61 120.6(3) . . ? C65 C66 H67 119.7 . . ? C61 C66 H67 119.7 . . ? C72 C67 C68 120.0(3) . . ? C72 C67 P2 116.8(3) . . ? C68 C67 P2 123.2(3) . . ? C69 C68 C67 119.4(4) . . ? C69 C68 H69 120.3 . . ? C67 C68 H69 120.3 . . ? C70 C69 C68 120.1(4) . . ? C70 C69 H70 119.9 . . ? C68 C69 H70 119.9 . . ? C69 C70 C71 120.3(3) . . ? C69 C70 H71 119.9 . . ? C71 C70 H71 119.9 . . ? C72 C71 C70 120.0(4) . . ? C72 C71 H72 120.0 . . ? C70 C71 H72 120.0 . . ? C71 C72 C67 120.1(4) . . ? C71 C72 H73 119.9 . . ? C67 C72 H73 119.9 . . ? C78 C73 C74 119.2(3) . . ? C78 C73 P2 119.7(3) . . ? C74 C73 P2 121.2(3) . . ? C75 C74 C73 120.1(4) . . ? C75 C74 H75 119.9 . . ? C73 C74 H75 119.9 . . ? C76 C75 C74 119.6(4) . . ? C76 C75 H76 120.2 . . ? C74 C75 H76 120.2 . . ? C77 C76 C75 120.8(4) . . ? C77 C76 H77 119.6 . . ? C75 C76 H77 119.6 . . ? C76 C77 C78 119.8(4) . . ? C76 C77 H78 120.1 . . ? C78 C77 H78 120.1 . . ? C77 C78 C73 120.5(4) . . ? C77 C78 H79 119.8 . . ? C73 C78 H79 119.8 . . ? C80 C79 C84 119.6(3) . . ? C80 C79 P2 120.8(3) . . ? C84 C79 P2 119.6(3) . . ? C81 C80 C79 119.6(3) . . ? C81 C80 H81 120.2 . . ? C79 C80 H81 120.2 . . ? C82 C81 C80 120.8(4) . . ? C82 C81 H82 119.6 . . ? C80 C81 H82 119.6 . . ? C81 C82 C83 119.9(4) . . ? C81 C82 H83 120.0 . . ? C83 C82 H83 120.0 . . ? C82 C83 C84 120.4(4) . . ? C82 C83 H84 119.8 . . ? C84 C83 H84 119.8 . . ? C83 C84 C79 119.7(3) . . ? C83 C84 H85 120.2 . . ? C79 C84 H85 120.2 . . ? C90 C85 C86 119.8(3) . . ? C90 C85 P3 118.0(2) . . ? C86 C85 P3 121.7(2) . . ? C87 C86 C85 119.4(3) . . ? C87 C86 H87 120.3 . . ? C85 C86 H87 120.3 . . ? C86 C87 C88 120.8(3) . . ? C86 C87 H88 119.6 . . ? C88 C87 H88 119.6 . . ? C87 C88 C89 120.0(3) . . ? C87 C88 H89 120.0 . . ? C89 C88 H89 120.0 . . ? C90 C89 C88 119.8(3) . . ? C90 C89 H90 120.1 . . ? C88 C89 H90 120.1 . . ? C89 C90 C85 120.1(3) . . ? C89 C90 H91 119.9 . . ? C85 C90 H91 119.9 . . ? C96 C91 C92 120.0(3) . . ? C96 C91 P3 118.2(2) . . ? C92 C91 P3 121.7(2) . . ? C93 C92 C91 119.3(3) . . ? C93 C92 H93 120.3 . . ? C91 C92 H93 120.3 . . ? C94 C93 C92 120.6(3) . . ? C94 C93 H94 119.7 . . ? C92 C93 H94 119.7 . . ? C95 C94 C93 119.9(3) . . ? C95 C94 H95 120.1 . . ? C93 C94 H95 120.1 . . ? C94 C95 C96 120.5(3) . . ? C94 C95 H96 119.8 . . ? C96 C95 H96 119.8 . . ? C95 C96 C91 119.7(3) . . ? C95 C96 H97 120.2 . . ? C91 C96 H97 120.2 . . ? C102 C97 C98 119.3(3) . . ? C102 C97 P3 119.9(3) . . ? C98 C97 P3 120.7(2) . . ? C99 C98 C97 120.3(3) . . ? C99 C98 H99 119.9 . . ? C97 C98 H99 119.9 . . ? C98 C99 C100 119.7(3) . . ? C98 C99 H100 120.1 . . ? C100 C99 H100 120.1 . . ? C101 C100 C99 120.2(3) . . ? C101 C100 H101 119.9 . . ? C99 C100 H101 119.9 . . ? C100 C101 C102 120.7(3) . . ? C100 C101 H102 119.6 . . ? C102 C101 H102 119.6 . . ? C101 C102 C97 119.7(3) . . ? C101 C102 H103 120.1 . . ? C97 C102 H103 120.1 . . ? C104 C103 C108 119.9(3) . . ? C104 C103 P4 120.1(3) . . ? C108 C103 P4 120.0(2) . . ? C103 C104 C105 119.6(3) . . ? C103 C104 H105 120.2 . . ? C105 C104 H105 120.2 . . ? C106 C105 C104 120.3(3) . . ? C106 C105 H106 119.9 . . ? C104 C105 H106 119.9 . . ? C107 C106 C105 120.0(3) . . ? C107 C106 H107 120.0 . . ? C105 C106 H107 120.0 . . ? C106 C107 C108 119.8(3) . . ? C106 C107 H108 120.1 . . ? C108 C107 H108 120.1 . . ? C107 C108 C103 120.5(3) . . ? C107 C108 H109 119.8 . . ? C103 C108 H109 119.8 . . ? C114 C109 C110 120.3(3) . . ? C114 C109 P4 118.6(2) . . ? C110 C109 P4 121.1(2) . . ? C111 C110 C109 119.4(3) . . ? C111 C110 H111 120.3 . . ? C109 C110 H111 120.3 . . ? C112 C111 C110 120.4(3) . . ? C112 C111 H112 119.8 . . ? C110 C111 H112 119.8 . . ? C111 C112 C113 120.2(3) . . ? C111 C112 H113 119.9 . . ? C113 C112 H113 119.9 . . ? C114 C113 C112 120.2(3) . . ? C114 C113 H114 119.9 . . ? C112 C113 H114 119.9 . . ? C113 C114 C109 119.5(3) . . ? C113 C114 H115 120.2 . . ? C109 C114 H115 120.2 . . ? C116 C115 C120 119.8(3) . . ? C116 C115 P4 121.1(2) . . ? C120 C115 P4 119.0(2) . . ? C115 C116 C117 119.8(3) . . ? C115 C116 H117 120.1 . . ? C117 C116 H117 120.1 . . ? C116 C117 C118 119.9(3) . . ? C116 C117 H118 120.0 . . ? C118 C117 H118 120.0 . . ? C119 C118 C117 120.1(3) . . ? C119 C118 H119 119.9 . . ? C117 C118 H119 119.9 . . ? C118 C119 C120 120.2(3) . . ? C118 C119 H120 119.9 . . ? C120 C119 H120 119.9 . . ? C119 C120 C115 120.1(3) . . ? C119 C120 H121 119.9 . . ? C115 C120 H121 119.9 . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Ir1 124.5(2) . . ? C5 N1 Ir1 116.3(2) . . ? C18 N2 C22 118.5(3) . . ? C18 N2 Ir1 116.7(2) . . ? C22 N2 Ir1 124.8(2) . . ? C25 N3 C29 119.3(3) . . ? C25 N3 Ir2 124.4(2) . . ? C29 N3 Ir2 116.1(2) . . ? C46 N4 C42 119.1(3) . . ? C46 N4 Ir2 124.2(2) . . ? C42 N4 Ir2 116.6(2) . . ? C23 N5 Eu1 144.5(2) . . ? C24 N6 Eu2 168.0(2) . . ? C47 N7 Eu2 147.8(2) . . ? C48 N8 Eu1 156.9(2) . . ? O2 N9 O3 123.7(3) . . ? O2 N9 O1 120.7(3) . . ? O3 N9 O1 115.7(3) . . ? O2 N9 Eu1 170.0(2) . . ? O3 N9 Eu1 58.32(16) . . ? O1 N9 Eu1 58.41(16) . . ? O5 N10 O6 122.4(3) . . ? O5 N10 O4 122.4(3) . . ? O6 N10 O4 115.2(3) . . ? O5 N10 Eu1 169.7(2) . . ? O6 N10 Eu1 58.04(15) . . ? O4 N10 Eu1 58.54(15) . . ? O8 N11 O9 122.8(3) . . ? O8 N11 O7 122.6(3) . . ? O9 N11 O7 114.6(3) . . ? O8 N11 Eu1 176.5(3) . . ? O9 N11 Eu1 57.57(16) . . ? O7 N11 Eu1 57.16(17) . . ? O11 N12 O12 120.0(3) . . ? O11 N12 O10 123.1(3) . . ? O12 N12 O10 117.0(3) . . ? O11 N12 Eu2 167.4(3) . . ? O12 N12 Eu2 49.84(15) . . ? O10 N12 Eu2 67.66(17) . . ? O14 N13 O15 123.1(3) . . ? O14 N13 O13 120.9(3) . . ? O15 N13 O13 116.0(3) . . ? O14 N13 Eu2 176.2(2) . . ? O15 N13 Eu2 60.05(16) . . ? O13 N13 Eu2 56.07(15) . . ? O17 N14 O16 122.8(3) . . ? O17 N14 O18 121.7(3) . . ? O16 N14 O18 115.5(2) . . ? O17 N14 Eu2 173.4(2) . . ? O16 N14 Eu2 59.00(14) . . ? O18 N14 Eu2 56.85(14) . . ? N15 P1 C61 111.58(15) . . ? N15 P1 C49 107.06(14) . . ? C61 P1 C49 107.23(15) . . ? N15 P1 C55 115.41(15) . . ? C61 P1 C55 107.47(15) . . ? C49 P1 C55 107.76(15) . . ? N15 P2 C73 108.29(15) . . ? N15 P2 C67 115.66(15) . . ? C73 P2 C67 105.45(16) . . ? N15 P2 C79 110.84(16) . . ? C73 P2 C79 108.19(15) . . ? C67 P2 C79 108.06(16) . . ? N16 P3 C97 110.67(15) . . ? N16 P3 C91 107.78(15) . . ? C97 P3 C91 108.90(14) . . ? N16 P3 C85 114.74(14) . . ? C97 P3 C85 106.19(14) . . ? C91 P3 C85 108.42(15) . . ? N16 P4 C103 107.50(14) . . ? N16 P4 C109 115.25(15) . . ? C103 P4 C109 107.50(14) . . ? N16 P4 C115 110.87(15) . . ? C103 P4 C115 107.61(15) . . ? C109 P4 C115 107.81(14) . . ? N9 O1 Eu1 95.66(19) . . ? N9 O3 Eu1 96.66(18) . . ? N10 O4 Eu1 95.11(17) . . ? N10 O6 Eu1 96.00(18) . . ? N11 O7 Eu1 96.8(2) . . ? N11 O9 Eu1 96.43(19) . . ? N12 O10 Eu1 123.7(2) . . ? N12 O10 Eu2 87.60(18) . . ? Eu1 O10 Eu2 148.51(10) . . ? N12 O12 Eu2 107.06(19) . . ? N13 O13 Eu2 98.00(18) . . ? N13 O15 Eu2 94.53(18) . . ? N14 O16 Eu2 94.93(16) . . ? N14 O18 Eu2 96.92(17) . . ? P2 N15 P1 143.47(18) . . ? P3 N16 P4 143.25(18) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N2S C2S C1S 178.7(6) . . ? C4S C3S H3S1 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C4S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N3S C4S C3S 177.6(7) . . ? C6S C5S H5S1 109.5 . . ? C6S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? C6S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? N4S C6S C5S 178.3(4) . . ? C8S C7S H7S1 109.5 . . ? C8S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C8S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? N1S C8S C7S 177.8(5) . . ? C10S C9S H9S1 109.5 . . ? C10S C9S H9S2 109.5 . . ? H9S1 C9S H9S2 109.5 . . ? C10S C9S H9S3 109.5 . . ? H9S1 C9S H9S3 109.5 . . ? H9S2 C9S H9S3 109.5 . . ? N5S C10S C9S 179.1(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 N1 C1 C2 C3 -0.8(5) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 N1 -1.4(5) . . . . ? C3 C4 C5 C6 178.2(3) . . . . ? N1 C5 C6 C7 174.7(3) . . . . ? C4 C5 C6 C7 -4.9(5) . . . . ? N1 C5 C6 C11 -4.9(4) . . . . ? C4 C5 C6 C11 175.5(3) . . . . ? C11 C6 C7 C8 -1.5(5) . . . . ? C5 C6 C7 C8 178.9(3) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C7 C8 C9 C10 0.6(5) . . . . ? C8 C9 C10 C11 -1.2(5) . . . . ? C9 C10 C11 C6 0.4(4) . . . . ? C9 C10 C11 Ir1 -179.4(2) . . . . ? C7 C6 C11 C10 0.9(4) . . . . ? C5 C6 C11 C10 -179.5(3) . . . . ? C7 C6 C11 Ir1 -179.2(2) . . . . ? C5 C6 C11 Ir1 0.4(3) . . . . ? C24 Ir1 C11 C10 -149.6(9) . . . . ? C23 Ir1 C11 C10 -84.0(3) . . . . ? N1 Ir1 C11 C10 -177.6(3) . . . . ? C12 Ir1 C11 C10 89.8(3) . . . . ? N2 Ir1 C11 C10 10.5(3) . . . . ? C24 Ir1 C11 C6 30.5(11) . . . . ? C23 Ir1 C11 C6 96.2(2) . . . . ? N1 Ir1 C11 C6 2.6(2) . . . . ? C12 Ir1 C11 C6 -90.1(2) . . . . ? N2 Ir1 C11 C6 -169.4(2) . . . . ? C24 Ir1 C12 C13 -90.8(3) . . . . ? C23 Ir1 C12 C13 170.7(9) . . . . ? N1 Ir1 C12 C13 3.9(3) . . . . ? C11 Ir1 C12 C13 83.5(3) . . . . ? N2 Ir1 C12 C13 179.6(3) . . . . ? C24 Ir1 C12 C17 93.2(2) . . . . ? C23 Ir1 C12 C17 -5.3(12) . . . . ? N1 Ir1 C12 C17 -172.1(2) . . . . ? C11 Ir1 C12 C17 -92.5(2) . . . . ? N2 Ir1 C12 C17 3.6(2) . . . . ? C17 C12 C13 C14 0.1(5) . . . . ? Ir1 C12 C13 C14 -175.8(3) . . . . ? C12 C13 C14 C15 0.1(5) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C15 C16 C17 C12 0.1(5) . . . . ? C15 C16 C17 C18 -179.8(3) . . . . ? C13 C12 C17 C16 -0.2(4) . . . . ? Ir1 C12 C17 C16 176.4(2) . . . . ? C13 C12 C17 C18 179.7(3) . . . . ? Ir1 C12 C17 C18 -3.7(3) . . . . ? C16 C17 C18 N2 -178.8(3) . . . . ? C12 C17 C18 N2 1.3(4) . . . . ? C16 C17 C18 C19 2.9(5) . . . . ? C12 C17 C18 C19 -176.9(3) . . . . ? N2 C18 C19 C20 -0.1(5) . . . . ? C17 C18 C19 C20 178.0(3) . . . . ? C18 C19 C20 C21 -0.5(5) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 N2 0.8(5) . . . . ? C24 Ir1 C23 N5 -40(3) . . . . ? N1 Ir1 C23 N5 -134(3) . . . . ? C11 Ir1 C23 N5 146(3) . . . . ? C12 Ir1 C23 N5 60(3) . . . . ? N2 Ir1 C23 N5 51(3) . . . . ? C23 Ir1 C24 N6 -28(2) . . . . ? N1 Ir1 C24 N6 66(2) . . . . ? C11 Ir1 C24 N6 38(3) . . . . ? C12 Ir1 C24 N6 158(2) . . . . ? N2 Ir1 C24 N6 -122(2) . . . . ? N3 C25 C26 C27 -0.8(5) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C26 C27 C28 C29 0.5(5) . . . . ? C27 C28 C29 N3 0.0(5) . . . . ? C27 C28 C29 C30 -176.2(3) . . . . ? N3 C29 C30 C35 -3.5(4) . . . . ? C28 C29 C30 C35 172.9(3) . . . . ? N3 C29 C30 C31 178.5(3) . . . . ? C28 C29 C30 C31 -5.1(5) . . . . ? C35 C30 C31 C32 -2.4(5) . . . . ? C29 C30 C31 C32 175.5(3) . . . . ? C30 C31 C32 C33 0.6(5) . . . . ? C31 C32 C33 C34 1.2(5) . . . . ? C32 C33 C34 C35 -1.3(5) . . . . ? C33 C34 C35 C30 -0.4(5) . . . . ? C33 C34 C35 Ir2 178.7(3) . . . . ? C31 C30 C35 C34 2.3(5) . . . . ? C29 C30 C35 C34 -175.7(3) . . . . ? C31 C30 C35 Ir2 -177.0(2) . . . . ? C29 C30 C35 Ir2 5.0(3) . . . . ? C48 Ir2 C35 C34 89.3(3) . . . . ? C47 Ir2 C35 C34 169.1(12) . . . . ? C36 Ir2 C35 C34 -85.6(3) . . . . ? N4 Ir2 C35 C34 -5.8(3) . . . . ? N3 Ir2 C35 C34 177.1(3) . . . . ? C48 Ir2 C35 C30 -91.6(2) . . . . ? C47 Ir2 C35 C30 -11.8(15) . . . . ? C36 Ir2 C35 C30 93.5(2) . . . . ? N4 Ir2 C35 C30 173.3(2) . . . . ? N3 Ir2 C35 C30 -3.8(2) . . . . ? C48 Ir2 C36 C37 175.3(12) . . . . ? C47 Ir2 C36 C37 92.9(3) . . . . ? N4 Ir2 C36 C37 -175.7(3) . . . . ? N3 Ir2 C36 C37 -2.8(3) . . . . ? C35 Ir2 C36 C37 -82.2(3) . . . . ? C48 Ir2 C36 C41 -7.0(14) . . . . ? C47 Ir2 C36 C41 -89.4(2) . . . . ? N4 Ir2 C36 C41 2.1(2) . . . . ? N3 Ir2 C36 C41 174.9(2) . . . . ? C35 Ir2 C36 C41 95.6(2) . . . . ? C41 C36 C37 C38 1.4(5) . . . . ? Ir2 C36 C37 C38 179.1(2) . . . . ? C36 C37 C38 C39 1.9(5) . . . . ? C37 C38 C39 C40 -2.3(5) . . . . ? C38 C39 C40 C41 -0.6(5) . . . . ? C39 C40 C41 C36 4.0(5) . . . . ? C39 C40 C41 C42 -173.7(3) . . . . ? C37 C36 C41 C40 -4.3(4) . . . . ? Ir2 C36 C41 C40 177.6(2) . . . . ? C37 C36 C41 C42 173.6(3) . . . . ? Ir2 C36 C41 C42 -4.5(3) . . . . ? C40 C41 C42 N4 -177.0(3) . . . . ? C36 C41 C42 N4 5.1(4) . . . . ? C40 C41 C42 C43 6.3(5) . . . . ? C36 C41 C42 C43 -171.5(3) . . . . ? N4 C42 C43 C44 -0.2(5) . . . . ? C41 C42 C43 C44 176.3(3) . . . . ? C42 C43 C44 C45 1.4(5) . . . . ? C43 C44 C45 C46 -1.1(5) . . . . ? C44 C45 C46 N4 -0.3(5) . . . . ? C48 Ir2 C47 N7 26(2) . . . . ? C36 Ir2 C47 N7 -159(2) . . . . ? N4 Ir2 C47 N7 120(2) . . . . ? N3 Ir2 C47 N7 -62(2) . . . . ? C35 Ir2 C47 N7 -54(3) . . . . ? C47 Ir2 C48 N8 16(4) . . . . ? C36 Ir2 C48 N8 -67(4) . . . . ? N4 Ir2 C48 N8 -76(4) . . . . ? N3 Ir2 C48 N8 111(4) . . . . ? C35 Ir2 C48 N8 -170(4) . . . . ? C54 C49 C50 C51 0.7(5) . . . . ? P1 C49 C50 C51 178.1(3) . . . . ? C49 C50 C51 C52 -0.5(5) . . . . ? C50 C51 C52 C53 0.4(5) . . . . ? C51 C52 C53 C54 -0.4(5) . . . . ? C52 C53 C54 C49 0.6(5) . . . . ? C50 C49 C54 C53 -0.7(5) . . . . ? P1 C49 C54 C53 -178.2(3) . . . . ? C60 C55 C56 C57 -1.5(5) . . . . ? P1 C55 C56 C57 -178.8(3) . . . . ? C55 C56 C57 C58 0.7(5) . . . . ? C56 C57 C58 C59 0.6(6) . . . . ? C57 C58 C59 C60 -1.0(6) . . . . ? C58 C59 C60 C55 0.1(5) . . . . ? C56 C55 C60 C59 1.1(5) . . . . ? P1 C55 C60 C59 178.4(3) . . . . ? C66 C61 C62 C63 -0.4(5) . . . . ? P1 C61 C62 C63 175.3(3) . . . . ? C61 C62 C63 C64 -0.8(5) . . . . ? C62 C63 C64 C65 0.8(5) . . . . ? C63 C64 C65 C66 0.3(5) . . . . ? C64 C65 C66 C61 -1.4(5) . . . . ? C62 C61 C66 C65 1.5(5) . . . . ? P1 C61 C66 C65 -174.3(3) . . . . ? C72 C67 C68 C69 0.6(5) . . . . ? P2 C67 C68 C69 -178.7(3) . . . . ? C67 C68 C69 C70 -0.2(6) . . . . ? C68 C69 C70 C71 -0.2(6) . . . . ? C69 C70 C71 C72 0.2(6) . . . . ? C70 C71 C72 C67 0.3(6) . . . . ? C68 C67 C72 C71 -0.7(5) . . . . ? P2 C67 C72 C71 178.7(3) . . . . ? C78 C73 C74 C75 0.4(5) . . . . ? P2 C73 C74 C75 -178.1(3) . . . . ? C73 C74 C75 C76 -0.8(6) . . . . ? C74 C75 C76 C77 -0.3(6) . . . . ? C75 C76 C77 C78 1.7(6) . . . . ? C76 C77 C78 C73 -2.0(6) . . . . ? C74 C73 C78 C77 1.0(5) . . . . ? P2 C73 C78 C77 179.6(3) . . . . ? C84 C79 C80 C81 0.8(5) . . . . ? P2 C79 C80 C81 -178.9(3) . . . . ? C79 C80 C81 C82 -0.9(5) . . . . ? C80 C81 C82 C83 0.7(6) . . . . ? C81 C82 C83 C84 -0.4(6) . . . . ? C82 C83 C84 C79 0.3(5) . . . . ? C80 C79 C84 C83 -0.5(5) . . . . ? P2 C79 C84 C83 179.1(3) . . . . ? C90 C85 C86 C87 0.7(5) . . . . ? P3 C85 C86 C87 -171.0(3) . . . . ? C85 C86 C87 C88 0.1(5) . . . . ? C86 C87 C88 C89 -0.9(5) . . . . ? C87 C88 C89 C90 0.9(5) . . . . ? C88 C89 C90 C85 -0.1(5) . . . . ? C86 C85 C90 C89 -0.7(5) . . . . ? P3 C85 C90 C89 171.3(3) . . . . ? C96 C91 C92 C93 -1.0(5) . . . . ? P3 C91 C92 C93 177.4(2) . . . . ? C91 C92 C93 C94 1.7(5) . . . . ? C92 C93 C94 C95 -0.8(5) . . . . ? C93 C94 C95 C96 -1.0(5) . . . . ? C94 C95 C96 C91 1.7(5) . . . . ? C92 C91 C96 C95 -0.7(5) . . . . ? P3 C91 C96 C95 -179.2(3) . . . . ? C102 C97 C98 C99 -0.4(5) . . . . ? P3 C97 C98 C99 176.6(2) . . . . ? C97 C98 C99 C100 0.1(5) . . . . ? C98 C99 C100 C101 0.3(5) . . . . ? C99 C100 C101 C102 -0.5(5) . . . . ? C100 C101 C102 C97 0.3(5) . . . . ? C98 C97 C102 C101 0.2(5) . . . . ? P3 C97 C102 C101 -176.8(2) . . . . ? C108 C103 C104 C105 -1.1(5) . . . . ? P4 C103 C104 C105 179.0(3) . . . . ? C103 C104 C105 C106 -0.3(5) . . . . ? C104 C105 C106 C107 1.1(6) . . . . ? C105 C106 C107 C108 -0.5(6) . . . . ? C106 C107 C108 C103 -0.9(6) . . . . ? C104 C103 C108 C107 1.7(5) . . . . ? P4 C103 C108 C107 -178.4(3) . . . . ? C114 C109 C110 C111 0.4(5) . . . . ? P4 C109 C110 C111 178.0(3) . . . . ? C109 C110 C111 C112 0.1(5) . . . . ? C110 C111 C112 C113 -0.5(5) . . . . ? C111 C112 C113 C114 0.3(5) . . . . ? C112 C113 C114 C109 0.2(5) . . . . ? C110 C109 C114 C113 -0.5(5) . . . . ? P4 C109 C114 C113 -178.2(3) . . . . ? C120 C115 C116 C117 1.2(5) . . . . ? P4 C115 C116 C117 -175.4(3) . . . . ? C115 C116 C117 C118 0.6(5) . . . . ? C116 C117 C118 C119 -1.5(5) . . . . ? C117 C118 C119 C120 0.6(5) . . . . ? C118 C119 C120 C115 1.3(5) . . . . ? C116 C115 C120 C119 -2.1(5) . . . . ? P4 C115 C120 C119 174.5(2) . . . . ? C2 C1 N1 C5 -0.8(4) . . . . ? C2 C1 N1 Ir1 173.9(2) . . . . ? C4 C5 N1 C1 1.9(4) . . . . ? C6 C5 N1 C1 -177.8(3) . . . . ? C4 C5 N1 Ir1 -173.2(2) . . . . ? C6 C5 N1 Ir1 7.2(3) . . . . ? C24 Ir1 N1 C1 2.8(3) . . . . ? C23 Ir1 N1 C1 88.0(3) . . . . ? C11 Ir1 N1 C1 179.8(3) . . . . ? C12 Ir1 N1 C1 -93.4(3) . . . . ? N2 Ir1 N1 C1 -120.9(6) . . . . ? C24 Ir1 N1 C5 177.6(2) . . . . ? C23 Ir1 N1 C5 -97.2(2) . . . . ? C11 Ir1 N1 C5 -5.5(2) . . . . ? C12 Ir1 N1 C5 81.4(2) . . . . ? N2 Ir1 N1 C5 53.9(7) . . . . ? C19 C18 N2 C22 1.0(4) . . . . ? C17 C18 N2 C22 -177.3(3) . . . . ? C19 C18 N2 Ir1 -179.8(2) . . . . ? C17 C18 N2 Ir1 1.9(3) . . . . ? C21 C22 N2 C18 -1.4(5) . . . . ? C21 C22 N2 Ir1 179.5(2) . . . . ? C24 Ir1 N2 C18 -99.0(2) . . . . ? C23 Ir1 N2 C18 176.0(2) . . . . ? N1 Ir1 N2 C18 25.0(7) . . . . ? C11 Ir1 N2 C18 83.2(2) . . . . ? C12 Ir1 N2 C18 -3.0(2) . . . . ? C24 Ir1 N2 C22 80.1(3) . . . . ? C23 Ir1 N2 C22 -4.9(3) . . . . ? N1 Ir1 N2 C22 -155.9(5) . . . . ? C11 Ir1 N2 C22 -97.7(3) . . . . ? C12 Ir1 N2 C22 176.1(3) . . . . ? C26 C25 N3 C29 1.3(5) . . . . ? C26 C25 N3 Ir2 176.4(2) . . . . ? C28 C29 N3 C25 -0.9(4) . . . . ? C30 C29 N3 C25 175.7(3) . . . . ? C28 C29 N3 Ir2 -176.4(2) . . . . ? C30 C29 N3 Ir2 0.2(3) . . . . ? C48 Ir2 N3 C25 -79.4(3) . . . . ? C47 Ir2 N3 C25 6.0(3) . . . . ? C36 Ir2 N3 C25 100.4(3) . . . . ? N4 Ir2 N3 C25 164.7(6) . . . . ? C35 Ir2 N3 C25 -173.3(3) . . . . ? C48 Ir2 N3 C29 95.8(2) . . . . ? C47 Ir2 N3 C29 -178.8(2) . . . . ? C36 Ir2 N3 C29 -84.3(2) . . . . ? N4 Ir2 N3 C29 -20.0(8) . . . . ? C35 Ir2 N3 C29 1.9(2) . . . . ? C45 C46 N4 C42 1.6(5) . . . . ? C45 C46 N4 Ir2 -172.8(2) . . . . ? C43 C42 N4 C46 -1.3(4) . . . . ? C41 C42 N4 C46 -178.1(3) . . . . ? C43 C42 N4 Ir2 173.5(2) . . . . ? C41 C42 N4 Ir2 -3.3(3) . . . . ? C48 Ir2 N4 C46 -5.6(3) . . . . ? C47 Ir2 N4 C46 -91.3(3) . . . . ? C36 Ir2 N4 C46 175.2(3) . . . . ? N3 Ir2 N4 C46 109.9(7) . . . . ? C35 Ir2 N4 C46 88.3(3) . . . . ? C48 Ir2 N4 C42 179.9(2) . . . . ? C47 Ir2 N4 C42 94.2(2) . . . . ? C36 Ir2 N4 C42 0.8(2) . . . . ? N3 Ir2 N4 C42 -64.6(8) . . . . ? C35 Ir2 N4 C42 -86.2(2) . . . . ? Ir1 C23 N5 Eu1 24(3) . . . . ? N8 Eu1 N5 C23 52.0(5) . . . . ? O6 Eu1 N5 C23 176.4(4) . . . . ? O7 Eu1 N5 C23 -89.6(4) . . . . ? O4 Eu1 N5 C23 -169.8(5) . . . . ? O9 Eu1 N5 C23 -77.1(5) . . . . ? O1 Eu1 N5 C23 67.5(4) . . . . ? O3 Eu1 N5 C23 117.9(4) . . . . ? O10 Eu1 N5 C23 1.1(4) . . . . ? N10 Eu1 N5 C23 -179.4(4) . . . . ? N11 Eu1 N5 C23 -82.9(4) . . . . ? N9 Eu1 N5 C23 92.9(4) . . . . ? Ir1 C24 N6 Eu2 38(3) . . . . ? O1S Eu2 N6 C24 -60.0(12) . . . . ? O18 Eu2 N6 C24 151.1(12) . . . . ? O12 Eu2 N6 C24 63.3(12) . . . . ? O13 Eu2 N6 C24 -142.8(12) . . . . ? N7 Eu2 N6 C24 14.1(13) . . . . ? O16 Eu2 N6 C24 124.8(12) . . . . ? O15 Eu2 N6 C24 -131.9(12) . . . . ? O10 Eu2 N6 C24 14.1(12) . . . . ? N14 Eu2 N6 C24 140.3(12) . . . . ? N13 Eu2 N6 C24 -137.7(12) . . . . ? N12 Eu2 N6 C24 40.7(12) . . . . ? Ir2 C47 N7 Eu2 -24(3) . . . . ? O1S Eu2 N7 C47 53.3(5) . . . . ? O18 Eu2 N7 C47 -150.1(4) . . . . ? N6 Eu2 N7 C47 -24.7(6) . . . . ? O12 Eu2 N7 C47 -73.0(5) . . . . ? O13 Eu2 N7 C47 136.4(5) . . . . ? O16 Eu2 N7 C47 -148.3(5) . . . . ? O15 Eu2 N7 C47 110.1(5) . . . . ? O10 Eu2 N7 C47 -24.7(5) . . . . ? N14 Eu2 N7 C47 -150.8(5) . . . . ? N13 Eu2 N7 C47 125.7(5) . . . . ? N12 Eu2 N7 C47 -49.7(5) . . . . ? Ir2 C48 N8 Eu1 31(4) . . . . ? N5 Eu1 N8 C48 -85.5(7) . . . . ? O6 Eu1 N8 C48 137.1(7) . . . . ? O7 Eu1 N8 C48 45.4(7) . . . . ? O4 Eu1 N8 C48 145.7(7) . . . . ? O9 Eu1 N8 C48 54.2(7) . . . . ? O1 Eu1 N8 C48 -101.1(7) . . . . ? O3 Eu1 N8 C48 -152.4(7) . . . . ? O10 Eu1 N8 C48 -31.7(7) . . . . ? N10 Eu1 N8 C48 144.5(7) . . . . ? N11 Eu1 N8 C48 49.2(7) . . . . ? N9 Eu1 N8 C48 -128.0(7) . . . . ? N8 Eu1 N9 O2 -0.1(14) . . . . ? N5 Eu1 N9 O2 -159.6(14) . . . . ? O6 Eu1 N9 O2 71.3(14) . . . . ? O7 Eu1 N9 O2 -166.1(13) . . . . ? O4 Eu1 N9 O2 122.9(14) . . . . ? O9 Eu1 N9 O2 4.2(15) . . . . ? O1 Eu1 N9 O2 -87.7(14) . . . . ? O3 Eu1 N9 O2 104.5(14) . . . . ? O10 Eu1 N9 O2 -72.8(14) . . . . ? N10 Eu1 N9 O2 97.2(14) . . . . ? N11 Eu1 N9 O2 -32(2) . . . . ? N8 Eu1 N9 O3 -104.6(2) . . . . ? N5 Eu1 N9 O3 95.9(2) . . . . ? O6 Eu1 N9 O3 -33.2(2) . . . . ? O7 Eu1 N9 O3 89.4(3) . . . . ? O4 Eu1 N9 O3 18.4(2) . . . . ? O9 Eu1 N9 O3 -100.3(3) . . . . ? O1 Eu1 N9 O3 167.8(3) . . . . ? O10 Eu1 N9 O3 -177.3(2) . . . . ? N10 Eu1 N9 O3 -7.3(2) . . . . ? N11 Eu1 N9 O3 -136.3(9) . . . . ? N8 Eu1 N9 O1 87.63(19) . . . . ? N5 Eu1 N9 O1 -71.86(19) . . . . ? O6 Eu1 N9 O1 158.98(19) . . . . ? O7 Eu1 N9 O1 -78.4(3) . . . . ? O4 Eu1 N9 O1 -149.39(18) . . . . ? O9 Eu1 N9 O1 91.9(2) . . . . ? O3 Eu1 N9 O1 -167.8(3) . . . . ? O10 Eu1 N9 O1 14.89(19) . . . . ? N10 Eu1 N9 O1 -175.06(19) . . . . ? N11 Eu1 N9 O1 55.9(10) . . . . ? N8 Eu1 N10 O5 79.1(13) . . . . ? N5 Eu1 N10 O5 -77.0(13) . . . . ? O6 Eu1 N10 O5 95.4(14) . . . . ? O7 Eu1 N10 O5 -152.8(13) . . . . ? O4 Eu1 N10 O5 -98.6(13) . . . . ? O9 Eu1 N10 O5 155.2(13) . . . . ? O1 Eu1 N10 O5 2.7(13) . . . . ? O3 Eu1 N10 O5 1.7(13) . . . . ? O10 Eu1 N10 O5 100.6(13) . . . . ? N11 Eu1 N10 O5 -179(100) . . . . ? N9 Eu1 N10 O5 5.1(13) . . . . ? N8 Eu1 N10 O6 -16.3(2) . . . . ? N5 Eu1 N10 O6 -172.41(19) . . . . ? O7 Eu1 N10 O6 111.8(2) . . . . ? O4 Eu1 N10 O6 166.0(3) . . . . ? O9 Eu1 N10 O6 59.7(2) . . . . ? O1 Eu1 N10 O6 -92.7(2) . . . . ? O3 Eu1 N10 O6 -93.7(2) . . . . ? O10 Eu1 N10 O6 5.1(6) . . . . ? N11 Eu1 N10 O6 85.7(2) . . . . ? N9 Eu1 N10 O6 -90.3(2) . . . . ? N8 Eu1 N10 O4 177.71(19) . . . . ? N5 Eu1 N10 O4 21.6(2) . . . . ? O6 Eu1 N10 O4 -166.0(3) . . . . ? O7 Eu1 N10 O4 -54.22(19) . . . . ? O9 Eu1 N10 O4 -106.28(19) . . . . ? O1 Eu1 N10 O4 101.3(2) . . . . ? O3 Eu1 N10 O4 100.3(2) . . . . ? O10 Eu1 N10 O4 -160.9(4) . . . . ? N11 Eu1 N10 O4 -80.3(2) . . . . ? N9 Eu1 N10 O4 103.68(19) . . . . ? N8 Eu1 N11 O8 -86(4) . . . . ? N5 Eu1 N11 O8 72(4) . . . . ? O6 Eu1 N11 O8 -158(4) . . . . ? O7 Eu1 N11 O8 87(4) . . . . ? O4 Eu1 N11 O8 150(4) . . . . ? O9 Eu1 N11 O8 -97(4) . . . . ? O1 Eu1 N11 O8 -7(4) . . . . ? O3 Eu1 N11 O8 177(100) . . . . ? O10 Eu1 N11 O8 -14(4) . . . . ? N10 Eu1 N11 O8 176(4) . . . . ? N9 Eu1 N11 O8 -55(5) . . . . ? N8 Eu1 N11 O9 11.0(2) . . . . ? N5 Eu1 N11 O9 169.2(2) . . . . ? O6 Eu1 N11 O9 -60.9(2) . . . . ? O7 Eu1 N11 O9 -176.0(3) . . . . ? O4 Eu1 N11 O9 -112.7(2) . . . . ? O1 Eu1 N11 O9 90.3(3) . . . . ? O3 Eu1 N11 O9 -85.4(3) . . . . ? O10 Eu1 N11 O9 83.3(2) . . . . ? N10 Eu1 N11 O9 -86.8(2) . . . . ? N9 Eu1 N11 O9 42.1(10) . . . . ? N8 Eu1 N11 O7 -173.0(2) . . . . ? N5 Eu1 N11 O7 -14.8(2) . . . . ? O6 Eu1 N11 O7 115.1(2) . . . . ? O4 Eu1 N11 O7 63.3(2) . . . . ? O9 Eu1 N11 O7 176.0(3) . . . . ? O1 Eu1 N11 O7 -93.8(3) . . . . ? O3 Eu1 N11 O7 90.6(3) . . . . ? O10 Eu1 N11 O7 -100.7(2) . . . . ? N10 Eu1 N11 O7 89.2(2) . . . . ? N9 Eu1 N11 O7 -141.9(9) . . . . ? O1S Eu2 N12 O11 156.9(13) . . . . ? O18 Eu2 N12 O11 -1.0(13) . . . . ? N6 Eu2 N12 O11 67.8(13) . . . . ? O12 Eu2 N12 O11 -38.9(12) . . . . ? O13 Eu2 N12 O11 -100.3(13) . . . . ? N7 Eu2 N12 O11 -126.0(13) . . . . ? O16 Eu2 N12 O11 -53.5(13) . . . . ? O15 Eu2 N12 O11 79.6(13) . . . . ? O10 Eu2 N12 O11 149.7(14) . . . . ? N14 Eu2 N12 O11 -27.9(13) . . . . ? N13 Eu2 N12 O11 75.4(14) . . . . ? O1S Eu2 N12 O12 -164.2(2) . . . . ? O18 Eu2 N12 O12 37.9(2) . . . . ? N6 Eu2 N12 O12 106.7(2) . . . . ? O13 Eu2 N12 O12 -61.4(4) . . . . ? N7 Eu2 N12 O12 -87.1(2) . . . . ? O16 Eu2 N12 O12 -14.6(2) . . . . ? O15 Eu2 N12 O12 118.5(2) . . . . ? O10 Eu2 N12 O12 -171.4(3) . . . . ? N14 Eu2 N12 O12 11.1(2) . . . . ? N13 Eu2 N12 O12 114.3(4) . . . . ? O1S Eu2 N12 O10 7.18(18) . . . . ? O18 Eu2 N12 O10 -150.65(17) . . . . ? N6 Eu2 N12 O10 -81.89(18) . . . . ? O12 Eu2 N12 O10 171.4(3) . . . . ? O13 Eu2 N12 O10 110.0(3) . . . . ? N7 Eu2 N12 O10 84.31(18) . . . . ? O16 Eu2 N12 O10 156.84(17) . . . . ? O15 Eu2 N12 O10 -70.1(2) . . . . ? N14 Eu2 N12 O10 -177.53(17) . . . . ? N13 Eu2 N12 O10 -74.3(4) . . . . ? O1S Eu2 N13 O14 137(3) . . . . ? O18 Eu2 N13 O14 -59(3) . . . . ? N6 Eu2 N13 O14 -131(3) . . . . ? O12 Eu2 N13 O14 -54(4) . . . . ? O13 Eu2 N13 O14 39(3) . . . . ? N7 Eu2 N13 O14 64(3) . . . . ? O16 Eu2 N13 O14 -9(3) . . . . ? O15 Eu2 N13 O14 -145(4) . . . . ? O10 Eu2 N13 O14 168(3) . . . . ? N14 Eu2 N13 O14 -33(3) . . . . ? N12 Eu2 N13 O14 -139(3) . . . . ? O1S Eu2 N13 O15 -78.01(18) . . . . ? O18 Eu2 N13 O15 85.33(18) . . . . ? N6 Eu2 N13 O15 13.14(18) . . . . ? O12 Eu2 N13 O15 90.8(3) . . . . ? O13 Eu2 N13 O15 -176.4(3) . . . . ? N7 Eu2 N13 O15 -151.57(17) . . . . ? O16 Eu2 N13 O15 135.17(18) . . . . ? O10 Eu2 N13 O15 -47.5(2) . . . . ? N14 Eu2 N13 O15 111.41(18) . . . . ? N12 Eu2 N13 O15 5.9(5) . . . . ? O1S Eu2 N13 O13 98.41(18) . . . . ? O18 Eu2 N13 O13 -98.25(17) . . . . ? N6 Eu2 N13 O13 -170.43(17) . . . . ? O12 Eu2 N13 O13 -92.8(3) . . . . ? N7 Eu2 N13 O13 24.86(19) . . . . ? O16 Eu2 N13 O13 -48.41(17) . . . . ? O15 Eu2 N13 O13 176.4(3) . . . . ? O10 Eu2 N13 O13 128.93(18) . . . . ? N14 Eu2 N13 O13 -72.17(17) . . . . ? N12 Eu2 N13 O13 -177.6(3) . . . . ? O1S Eu2 N14 O17 -17(2) . . . . ? O18 Eu2 N14 O17 79(2) . . . . ? N6 Eu2 N14 O17 104(2) . . . . ? O12 Eu2 N14 O17 179(100) . . . . ? O13 Eu2 N14 O17 -20(2) . . . . ? N7 Eu2 N14 O17 -102(2) . . . . ? O16 Eu2 N14 O17 -108(2) . . . . ? O15 Eu2 N14 O17 29(2) . . . . ? O10 Eu2 N14 O17 172.9(19) . . . . ? N13 Eu2 N14 O17 6(2) . . . . ? N12 Eu2 N14 O17 174(2) . . . . ? O1S Eu2 N14 O16 90.3(3) . . . . ? O18 Eu2 N14 O16 -173.1(3) . . . . ? N6 Eu2 N14 O16 -148.80(18) . . . . ? O12 Eu2 N14 O16 -73.82(18) . . . . ? O13 Eu2 N14 O16 87.89(18) . . . . ? N7 Eu2 N14 O16 5.58(19) . . . . ? O15 Eu2 N14 O16 137.12(18) . . . . ? O10 Eu2 N14 O16 -79.50(19) . . . . ? N13 Eu2 N14 O16 113.56(19) . . . . ? N12 Eu2 N14 O16 -78.21(19) . . . . ? O1S Eu2 N14 O18 -96.6(3) . . . . ? N6 Eu2 N14 O18 24.33(19) . . . . ? O12 Eu2 N14 O18 99.31(19) . . . . ? O13 Eu2 N14 O18 -98.99(19) . . . . ? N7 Eu2 N14 O18 178.71(18) . . . . ? O16 Eu2 N14 O18 173.1(3) . . . . ? O15 Eu2 N14 O18 -49.75(18) . . . . ? O10 Eu2 N14 O18 93.63(19) . . . . ? N13 Eu2 N14 O18 -73.31(18) . . . . ? N12 Eu2 N14 O18 94.92(19) . . . . ? C62 C61 P1 N15 166.5(3) . . . . ? C66 C61 P1 N15 -17.8(3) . . . . ? C62 C61 P1 C49 -76.5(3) . . . . ? C66 C61 P1 C49 99.1(3) . . . . ? C62 C61 P1 C55 39.1(3) . . . . ? C66 C61 P1 C55 -145.2(3) . . . . ? C50 C49 P1 N15 9.9(3) . . . . ? C54 C49 P1 N15 -172.7(3) . . . . ? C50 C49 P1 C61 -110.0(3) . . . . ? C54 C49 P1 C61 67.5(3) . . . . ? C50 C49 P1 C55 134.6(3) . . . . ? C54 C49 P1 C55 -48.0(3) . . . . ? C56 C55 P1 N15 86.8(3) . . . . ? C60 C55 P1 N15 -90.5(3) . . . . ? C56 C55 P1 C61 -148.0(3) . . . . ? C60 C55 P1 C61 34.7(3) . . . . ? C56 C55 P1 C49 -32.8(3) . . . . ? C60 C55 P1 C49 150.0(3) . . . . ? C78 C73 P2 N15 28.1(3) . . . . ? C74 C73 P2 N15 -153.4(3) . . . . ? C78 C73 P2 C67 152.5(3) . . . . ? C74 C73 P2 C67 -29.0(3) . . . . ? C78 C73 P2 C79 -92.1(3) . . . . ? C74 C73 P2 C79 86.4(3) . . . . ? C72 C67 P2 N15 57.2(3) . . . . ? C68 C67 P2 N15 -123.5(3) . . . . ? C72 C67 P2 C73 -62.4(3) . . . . ? C68 C67 P2 C73 116.9(3) . . . . ? C72 C67 P2 C79 -177.9(3) . . . . ? C68 C67 P2 C79 1.4(3) . . . . ? C80 C79 P2 N15 -165.2(3) . . . . ? C84 C79 P2 N15 15.1(3) . . . . ? C80 C79 P2 C73 -46.6(3) . . . . ? C84 C79 P2 C73 133.7(3) . . . . ? C80 C79 P2 C67 67.1(3) . . . . ? C84 C79 P2 C67 -112.6(3) . . . . ? C102 C97 P3 N16 -16.2(3) . . . . ? C98 C97 P3 N16 166.8(2) . . . . ? C102 C97 P3 C91 -134.5(3) . . . . ? C98 C97 P3 C91 48.5(3) . . . . ? C102 C97 P3 C85 108.9(3) . . . . ? C98 C97 P3 C85 -68.1(3) . . . . ? C96 C91 P3 N16 -22.1(3) . . . . ? C92 C91 P3 N16 159.4(3) . . . . ? C96 C91 P3 C97 98.0(3) . . . . ? C92 C91 P3 C97 -80.4(3) . . . . ? C96 C91 P3 C85 -146.9(2) . . . . ? C92 C91 P3 C85 34.7(3) . . . . ? C90 C85 P3 N16 -64.9(3) . . . . ? C86 C85 P3 N16 106.9(3) . . . . ? C90 C85 P3 C97 172.6(3) . . . . ? C86 C85 P3 C97 -15.6(3) . . . . ? C90 C85 P3 C91 55.7(3) . . . . ? C86 C85 P3 C91 -132.5(3) . . . . ? C104 C103 P4 N16 -0.1(3) . . . . ? C108 C103 P4 N16 179.9(3) . . . . ? C104 C103 P4 C109 -124.8(3) . . . . ? C108 C103 P4 C109 55.3(3) . . . . ? C104 C103 P4 C115 119.3(3) . . . . ? C108 C103 P4 C115 -60.6(3) . . . . ? C114 C109 P4 N16 84.1(3) . . . . ? C110 C109 P4 N16 -93.6(3) . . . . ? C114 C109 P4 C103 -156.1(3) . . . . ? C110 C109 P4 C103 26.2(3) . . . . ? C114 C109 P4 C115 -40.4(3) . . . . ? C110 C109 P4 C115 142.0(3) . . . . ? C116 C115 P4 N16 -163.0(2) . . . . ? C120 C115 P4 N16 20.3(3) . . . . ? C116 C115 P4 C103 79.7(3) . . . . ? C120 C115 P4 C103 -97.0(3) . . . . ? C116 C115 P4 C109 -36.0(3) . . . . ? C120 C115 P4 C109 147.4(2) . . . . ? O2 N9 O1 Eu1 168.3(3) . . . . ? O3 N9 O1 Eu1 -11.5(3) . . . . ? N8 Eu1 O1 N9 -85.06(19) . . . . ? N5 Eu1 O1 N9 103.14(19) . . . . ? O6 Eu1 O1 N9 -23.1(2) . . . . ? O7 Eu1 O1 N9 141.95(18) . . . . ? O4 Eu1 O1 N9 34.8(2) . . . . ? O9 Eu1 O1 N9 -126.06(19) . . . . ? O3 Eu1 O1 N9 6.65(18) . . . . ? O10 Eu1 O1 N9 -163.7(2) . . . . ? N10 Eu1 O1 N9 5.5(2) . . . . ? N11 Eu1 O1 N9 -171.26(19) . . . . ? O2 N9 O3 Eu1 -168.3(3) . . . . ? O1 N9 O3 Eu1 11.5(3) . . . . ? N8 Eu1 O3 N9 70.2(2) . . . . ? N5 Eu1 O3 N9 -81.4(2) . . . . ? O6 Eu1 O3 N9 144.0(2) . . . . ? O7 Eu1 O3 N9 -136.2(2) . . . . ? O4 Eu1 O3 N9 -160.7(2) . . . . ? O9 Eu1 O3 N9 120.1(2) . . . . ? O1 Eu1 O3 N9 -6.88(18) . . . . ? O10 Eu1 O3 N9 3.0(2) . . . . ? N10 Eu1 O3 N9 171.9(2) . . . . ? N11 Eu1 O3 N9 170.4(2) . . . . ? O5 N10 O4 Eu1 167.9(3) . . . . ? O6 N10 O4 Eu1 -13.1(3) . . . . ? N8 Eu1 O4 N10 -2.7(2) . . . . ? N5 Eu1 O4 N10 -158.6(2) . . . . ? O6 Eu1 O4 N10 7.73(17) . . . . ? O7 Eu1 O4 N10 124.0(2) . . . . ? O9 Eu1 O4 N10 76.19(19) . . . . ? O1 Eu1 O4 N10 -92.0(2) . . . . ? O3 Eu1 O4 N10 -69.40(19) . . . . ? O10 Eu1 O4 N10 168.9(2) . . . . ? N11 Eu1 O4 N10 100.35(19) . . . . ? N9 Eu1 O4 N10 -77.47(19) . . . . ? O5 N10 O6 Eu1 -167.8(3) . . . . ? O4 N10 O6 Eu1 13.2(3) . . . . ? N8 Eu1 O6 N10 163.0(2) . . . . ? N5 Eu1 O6 N10 9.5(2) . . . . ? O7 Eu1 O6 N10 -71.5(2) . . . . ? O4 Eu1 O6 N10 -7.84(17) . . . . ? O9 Eu1 O6 N10 -118.5(2) . . . . ? O1 Eu1 O6 N10 99.36(19) . . . . ? O3 Eu1 O6 N10 75.10(19) . . . . ? O10 Eu1 O6 N10 -178.48(17) . . . . ? N11 Eu1 O6 N10 -95.50(19) . . . . ? N9 Eu1 O6 N10 89.49(19) . . . . ? O8 N11 O7 Eu1 -175.9(3) . . . . ? O9 N11 O7 Eu1 3.7(3) . . . . ? N8 Eu1 O7 N11 8.6(2) . . . . ? N5 Eu1 O7 N11 165.0(2) . . . . ? O6 Eu1 O7 N11 -67.8(2) . . . . ? O4 Eu1 O7 N11 -114.0(2) . . . . ? O9 Eu1 O7 N11 -2.23(18) . . . . ? O1 Eu1 O7 N11 126.2(2) . . . . ? O3 Eu1 O7 N11 -137.7(2) . . . . ? O10 Eu1 O7 N11 78.1(2) . . . . ? N10 Eu1 O7 N11 -92.4(2) . . . . ? N9 Eu1 O7 N11 171.6(2) . . . . ? O8 N11 O9 Eu1 175.9(3) . . . . ? O7 N11 O9 Eu1 -3.7(3) . . . . ? N8 Eu1 O9 N11 -168.9(2) . . . . ? N5 Eu1 O9 N11 -13.2(2) . . . . ? O6 Eu1 O9 N11 117.2(2) . . . . ? O7 Eu1 O9 N11 2.24(18) . . . . ? O4 Eu1 O9 N11 69.0(2) . . . . ? O1 Eu1 O9 N11 -128.1(2) . . . . ? O3 Eu1 O9 N11 139.8(2) . . . . ? O10 Eu1 O9 N11 -93.7(2) . . . . ? N10 Eu1 O9 N11 94.5(2) . . . . ? N9 Eu1 O9 N11 -173.12(19) . . . . ? O11 N12 O10 Eu1 3.8(5) . . . . ? O12 N12 O10 Eu1 -176.4(2) . . . . ? Eu2 N12 O10 Eu1 176.21(19) . . . . ? O11 N12 O10 Eu2 -172.4(4) . . . . ? O12 N12 O10 Eu2 7.4(3) . . . . ? N8 Eu1 O10 N12 112.8(2) . . . . ? N5 Eu1 O10 N12 -91.8(2) . . . . ? O6 Eu1 O10 N12 94.4(3) . . . . ? O7 Eu1 O10 N12 -16.3(2) . . . . ? O4 Eu1 O10 N12 -60.0(4) . . . . ? O9 Eu1 O10 N12 35.3(2) . . . . ? O1 Eu1 O10 N12 -167.1(2) . . . . ? O3 Eu1 O10 N12 -175.4(2) . . . . ? N10 Eu1 O10 N12 90.6(5) . . . . ? N11 Eu1 O10 N12 9.2(2) . . . . ? N9 Eu1 O10 N12 -174.1(2) . . . . ? N8 Eu1 O10 Eu2 -74.50(18) . . . . ? N5 Eu1 O10 Eu2 80.94(18) . . . . ? O6 Eu1 O10 Eu2 -92.8(2) . . . . ? O7 Eu1 O10 Eu2 156.41(18) . . . . ? O4 Eu1 O10 Eu2 112.8(3) . . . . ? O9 Eu1 O10 Eu2 -151.97(18) . . . . ? O1 Eu1 O10 Eu2 5.64(16) . . . . ? O3 Eu1 O10 Eu2 -2.7(2) . . . . ? N10 Eu1 O10 Eu2 -96.7(5) . . . . ? N11 Eu1 O10 Eu2 -178.03(19) . . . . ? N9 Eu1 O10 Eu2 -1.40(18) . . . . ? O1S Eu2 O10 N12 -172.76(19) . . . . ? O18 Eu2 O10 N12 35.2(2) . . . . ? N6 Eu2 O10 N12 88.20(18) . . . . ? O12 Eu2 O10 N12 -4.55(17) . . . . ? O13 Eu2 O10 N12 -145.5(2) . . . . ? N7 Eu2 O10 N12 -91.79(18) . . . . ? O16 Eu2 O10 N12 -26.42(19) . . . . ? O15 Eu2 O10 N12 132.41(17) . . . . ? N14 Eu2 O10 N12 3.0(2) . . . . ? N13 Eu2 O10 N12 156.61(18) . . . . ? O1S Eu2 O10 Eu1 13.28(17) . . . . ? O18 Eu2 O10 Eu1 -138.72(16) . . . . ? N6 Eu2 O10 Eu1 -85.76(18) . . . . ? O12 Eu2 O10 Eu1 -178.5(2) . . . . ? O13 Eu2 O10 Eu1 40.5(3) . . . . ? N7 Eu2 O10 Eu1 94.25(18) . . . . ? O16 Eu2 O10 Eu1 159.62(16) . . . . ? O15 Eu2 O10 Eu1 -41.6(2) . . . . ? N14 Eu2 O10 Eu1 -170.94(15) . . . . ? N13 Eu2 O10 Eu1 -17.3(3) . . . . ? N12 Eu2 O10 Eu1 -174.0(3) . . . . ? O11 N12 O12 Eu2 170.9(3) . . . . ? O10 N12 O12 Eu2 -8.9(3) . . . . ? O1S Eu2 O12 N12 18.6(2) . . . . ? O18 Eu2 O12 N12 -143.0(2) . . . . ? N6 Eu2 O12 N12 -66.6(2) . . . . ? O13 Eu2 O12 N12 156.43(19) . . . . ? N7 Eu2 O12 N12 89.5(2) . . . . ? O16 Eu2 O12 N12 164.9(2) . . . . ? O15 Eu2 O12 N12 -94.9(2) . . . . ? O10 Eu2 O12 N12 4.85(18) . . . . ? N14 Eu2 O12 N12 -169.0(2) . . . . ? N13 Eu2 O12 N12 -148.3(2) . . . . ? O14 N13 O13 Eu2 -177.2(3) . . . . ? O15 N13 O13 Eu2 3.5(3) . . . . ? O1S Eu2 O13 N13 -76.94(17) . . . . ? O18 Eu2 O13 N13 75.73(17) . . . . ? N6 Eu2 O13 N13 11.5(2) . . . . ? O12 Eu2 O13 N13 137.59(18) . . . . ? N7 Eu2 O13 N13 -156.52(18) . . . . ? O16 Eu2 O13 N13 129.17(18) . . . . ? O15 Eu2 O13 N13 -1.97(15) . . . . ? O10 Eu2 O13 N13 -103.7(2) . . . . ? N14 Eu2 O13 N13 102.08(18) . . . . ? N12 Eu2 O13 N13 178.0(3) . . . . ? O14 N13 O15 Eu2 177.3(3) . . . . ? O13 N13 O15 Eu2 -3.3(3) . . . . ? O1S Eu2 O15 N13 95.34(18) . . . . ? O18 Eu2 O15 N13 -87.31(18) . . . . ? N6 Eu2 O15 N13 -166.50(19) . . . . ? O12 Eu2 O15 N13 -137.83(18) . . . . ? O13 Eu2 O15 N13 2.00(16) . . . . ? N7 Eu2 O15 N13 36.4(2) . . . . ? O16 Eu2 O15 N13 -48.29(19) . . . . ? O10 Eu2 O15 N13 151.37(16) . . . . ? N14 Eu2 O15 N13 -66.75(18) . . . . ? N12 Eu2 O15 N13 -177.98(16) . . . . ? O17 N14 O16 Eu2 172.5(3) . . . . ? O18 N14 O16 Eu2 -6.4(3) . . . . ? O1S Eu2 O16 N14 -134.72(18) . . . . ? O18 Eu2 O16 N14 3.84(16) . . . . ? N6 Eu2 O16 N14 36.7(2) . . . . ? O12 Eu2 O16 N14 100.01(19) . . . . ? O13 Eu2 O16 N14 -84.64(18) . . . . ? N7 Eu2 O16 N14 -174.3(2) . . . . ? O15 Eu2 O16 N14 -46.12(19) . . . . ? O10 Eu2 O16 N14 116.70(17) . . . . ? N13 Eu2 O16 N14 -64.82(18) . . . . ? N12 Eu2 O16 N14 105.91(18) . . . . ? O17 N14 O18 Eu2 -172.3(3) . . . . ? O16 N14 O18 Eu2 6.5(3) . . . . ? O1S Eu2 O18 N14 132.09(18) . . . . ? N6 Eu2 O18 N14 -155.2(2) . . . . ? O12 Eu2 O18 N14 -77.08(18) . . . . ? O13 Eu2 O18 N14 74.84(18) . . . . ? N7 Eu2 O18 N14 -1.6(2) . . . . ? O16 Eu2 O18 N14 -3.82(16) . . . . ? O15 Eu2 O18 N14 127.39(19) . . . . ? O10 Eu2 O18 N14 -105.46(18) . . . . ? N13 Eu2 O18 N14 100.95(19) . . . . ? N12 Eu2 O18 N14 -91.11(18) . . . . ? C73 P2 N15 P1 134.3(3) . . . . ? C67 P2 N15 P1 16.2(4) . . . . ? C79 P2 N15 P1 -107.2(3) . . . . ? C61 P1 N15 P2 -96.1(3) . . . . ? C49 P1 N15 P2 146.9(3) . . . . ? C55 P1 N15 P2 27.0(4) . . . . ? C97 P3 N16 P4 98.9(3) . . . . ? C91 P3 N16 P4 -142.1(3) . . . . ? C85 P3 N16 P4 -21.2(4) . . . . ? C103 P4 N16 P3 -146.4(3) . . . . ? C109 P4 N16 P3 -26.6(4) . . . . ? C115 P4 N16 P3 96.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.105 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.136 #===END