# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_exp_845 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H44 Ir2 N8 Nd O10' _chemical_formula_weight 1661.8 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 8.97022(17) _cell_length_b 15.2256(4) _cell_length_c 23.7904(7) _cell_angle_alpha 74.036(2) _cell_angle_beta 88.6555(19) _cell_angle_gamma 82.0711(19) _cell_volume 3093.68(13) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 12261 _cell_measurement_theta_min 3.85 _cell_measurement_theta_max 73.079 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1634 _exptl_absorpt_coefficient_mu 15.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.12443 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22888 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 73.29 _reflns_number_total 11860 _reflns_number_gt 10567 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0716P)^2^+6.1619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11860 _refine_ls_number_parameters 797 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.005 _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 -0.33066(3) 0.999938(15) -0.200724(10) 0.02067(8) Uani 1 1 d . . . Ir2 Ir 0.78994(3) 0.458550(17) 0.326893(10) 0.02319(8) Uani 1 1 d . . . Nd1 Nd 0.19937(4) 0.54898(2) 0.003311(14) 0.02407(9) Uani 1 1 d . . . O2 O -0.3593(5) 0.5785(3) 0.01341(19) 0.0295(9) Uani 1 1 d . . . N6 N 0.8564(5) 0.5275(4) 0.2414(2) 0.0236(10) Uani 1 1 d . . . O3 O 0.2542(5) 0.6350(3) -0.0926(2) 0.0340(10) Uani 1 1 d . . . O5 O 0.2924(6) 0.4762(4) 0.0994(2) 0.0412(12) Uani 1 1 d . . . O8 O 1.0568(6) 0.6664(3) 0.0393(2) 0.0389(11) Uani 1 1 d . . . O1 O -0.6008(5) 0.6365(3) 0.0155(2) 0.0329(10) Uani 1 1 d . . . N2 N -0.3857(5) 0.8914(3) -0.1285(2) 0.0232(10) Uani 1 1 d . . . N5 N 0.5980(6) 0.4652(4) 0.2728(2) 0.0263(10) Uani 1 1 d . . . N3 N -0.3653(6) 0.9321(4) -0.2617(2) 0.0263(10) Uani 1 1 d . . . O6 O 0.1641(6) 0.3942(4) 0.1716(2) 0.0424(12) Uani 1 1 d . . . N1 N -0.1180(5) 0.9142(3) -0.1770(2) 0.0225(9) Uani 1 1 d . . . N7 N 0.8597(6) 0.3282(4) 0.3204(2) 0.0293(11) Uani 1 1 d . . . O4 O 0.3788(5) 0.7152(4) -0.1679(2) 0.0410(12) Uani 1 1 d . . . C59 C 0.7091(7) 0.3861(5) 0.4013(2) 0.0262(12) Uani 1 1 d . . . N4 N -0.3124(6) 1.0846(4) -0.1488(2) 0.0289(11) Uani 1 1 d . . . C47 C -0.2595(6) 1.0878(4) -0.2721(3) 0.0247(12) Uani 1 1 d . . . O9 O -0.0069(6) 0.5374(4) -0.0559(3) 0.0489(14) Uani 1 1 d . . . C9 C -0.5214(7) 0.8854(4) -0.1035(3) 0.0255(12) Uani 1 1 d . . . H9 H -0.5970 0.9354 -0.1145 0.031 Uiso 1 1 calc R . . N8 N 0.7340(6) 0.5821(4) 0.3459(2) 0.0289(11) Uani 1 1 d . . . C27 C 0.9853(7) 0.5655(5) 0.2278(3) 0.0298(13) Uani 1 1 d . . . H27 H 1.0532 0.5605 0.2578 0.036 Uiso 1 1 calc R . . O7 O 0.8345(7) 0.7479(4) 0.0469(3) 0.0566(16) Uani 1 1 d . . . C13 C 0.1350(7) 0.7808(4) -0.1481(3) 0.0242(11) Uani 1 1 d . . . C30 C 0.5124(7) 0.4874(4) 0.1745(3) 0.0256(12) Uani 1 1 d . . . H30 H 0.5276 0.5083 0.1345 0.031 Uiso 1 1 calc R . . C29 C 0.6196(7) 0.4939(4) 0.2146(3) 0.0244(11) Uani 1 1 d . . . C83 C 0.9703(7) 0.5351(5) 0.3961(3) 0.0287(13) Uani 1 1 d . . . C6 C -0.2995(6) 0.7380(4) -0.0698(3) 0.0238(11) Uani 1 1 d . . . H6 H -0.2223 0.6889 -0.0588 0.029 Uiso 1 1 calc R . . C31 C 0.3828(7) 0.4490(4) 0.1955(3) 0.0258(12) Uani 1 1 d . . . C78 C 0.8321(7) 0.6032(4) 0.3806(3) 0.0285(12) Uani 1 1 d . . . C23 C 0.7583(7) 0.5357(4) 0.1970(3) 0.0246(12) Uani 1 1 d . . . C5 C -0.2740(6) 0.8186(4) -0.1112(3) 0.0227(11) Uani 1 1 d . . . C12 C -0.0019(7) 0.7646(4) -0.1227(3) 0.0262(12) Uani 1 1 d . . . H12 H -0.0107 0.7085 -0.0956 0.031 Uiso 1 1 calc R . . C11 C -0.1267(7) 0.8317(4) -0.1374(3) 0.0241(11) Uani 1 1 d . . . C56 C 0.9551(7) 0.3077(5) 0.2795(3) 0.0313(13) Uani 1 1 d . . . H56 H 0.9842 0.3557 0.2497 0.038 Uiso 1 1 calc R . . C34 C 0.2692(7) 0.4385(5) 0.1516(3) 0.0292(13) Uani 1 1 d . . . C52 C 0.8170(8) 0.2590(5) 0.3640(3) 0.0326(14) Uani 1 1 d . . . C45 C -0.4320(8) 0.8548(4) -0.2508(3) 0.0316(13) Uani 1 1 d . . . H45 H -0.4548 0.8258 -0.2124 0.038 Uiso 1 1 calc R . . C71 C -0.5374(7) 1.0735(4) -0.2147(3) 0.0286(13) Uani 1 1 d . . . C14 C 0.1449(7) 0.8673(4) -0.1869(3) 0.0290(13) Uani 1 1 d . . . H14 H 0.2363 0.8819 -0.2035 0.035 Uiso 1 1 calc R . . C26 C 1.0207(7) 0.6116(5) 0.1709(3) 0.0296(13) Uani 1 1 d . . . H26 H 1.1123 0.6344 0.1629 0.036 Uiso 1 1 calc R . . C8 C -0.5516(7) 0.8062(4) -0.0614(3) 0.0254(12) Uani 1 1 d . . . H8 H -0.6459 0.8038 -0.0444 0.030 Uiso 1 1 calc R . . C72 C -0.6535(7) 1.0690(4) -0.2512(3) 0.0312(13) Uani 1 1 d . . . H72 H -0.6383 1.0282 -0.2742 0.037 Uiso 1 1 calc R . . C7 C -0.4395(6) 0.7307(4) -0.0449(2) 0.0224(11) Uani 1 1 d . . . C15 C 0.0158(7) 0.9305(4) -0.1999(3) 0.0278(12) Uani 1 1 d . . . H15 H 0.0226 0.9876 -0.2262 0.033 Uiso 1 1 calc R . . C16 C 0.2696(6) 0.7042(4) -0.1357(3) 0.0231(11) Uani 1 1 d . . . C19 C -0.4688(7) 0.6416(4) -0.0024(2) 0.0232(11) Uani 1 1 d . . . C24 C 0.7854(7) 0.5836(5) 0.1397(3) 0.0297(13) Uani 1 1 d . . . H24 H 0.7154 0.5891 0.1103 0.036 Uiso 1 1 calc R . . C33 C 0.4716(7) 0.4293(5) 0.2925(3) 0.0319(13) Uani 1 1 d . . . H33 H 0.4570 0.4095 0.3326 0.038 Uiso 1 1 calc R . . C32 C 0.3619(7) 0.4210(5) 0.2545(3) 0.0303(13) Uani 1 1 d . . . H32 H 0.2749 0.3965 0.2692 0.036 Uiso 1 1 calc R . . C58 C 0.7269(7) 0.2892(5) 0.4089(3) 0.0314(13) Uani 1 1 d . . . C69 C -0.1859(9) 1.0902(5) -0.1223(3) 0.0386(16) Uani 1 1 d . . . H69 H -0.1011 1.0483 -0.1238 0.046 Uiso 1 1 calc R . . C79 C 0.8025(8) 0.6836(5) 0.3992(3) 0.0357(14) Uani 1 1 d . . . H79 H 0.8697 0.6967 0.4240 0.043 Uiso 1 1 calc R . . C25 C 0.9165(7) 0.6229(5) 0.1264(3) 0.0307(13) Uani 1 1 d . . . C62 C 0.5939(9) 0.2628(6) 0.4987(3) 0.0419(17) Uani 1 1 d . . . H62 H 0.5525 0.2231 0.5302 0.050 Uiso 1 1 calc R . . C48 C -0.2032(7) 1.1719(5) -0.2768(3) 0.0355(15) Uani 1 1 d . . . H48 H -0.2002 1.1933 -0.2438 0.043 Uiso 1 1 calc R . . C85 C 1.1019(8) 0.3921(5) 0.3868(3) 0.0344(14) Uani 1 1 d . . . H85 H 1.1090 0.3407 0.3724 0.041 Uiso 1 1 calc R . . C84 C 0.9752(7) 0.4583(5) 0.3733(3) 0.0282(13) Uani 1 1 d . . . C37 C 0.9364(8) 0.6846(4) 0.0652(3) 0.0315(13) Uani 1 1 d . . . C68 C -0.1756(11) 1.1553(6) -0.0930(4) 0.050(2) Uani 1 1 d . . . H68 H -0.0844 1.1592 -0.0767 0.060 Uiso 1 1 calc R . . C60 C 0.6335(8) 0.4169(5) 0.4458(3) 0.0335(14) Uani 1 1 d . . . H60 H 0.6193 0.4796 0.4428 0.040 Uiso 1 1 calc R . . C61 C 0.5787(8) 0.3566(6) 0.4944(3) 0.0395(16) Uani 1 1 d . . . H61 H 0.5319 0.3790 0.5239 0.047 Uiso 1 1 calc R . . C70 C -0.5671(8) 1.1369(5) -0.1808(3) 0.0352(14) Uani 1 1 d . . . C80 C 0.6709(9) 0.7435(5) 0.3799(4) 0.0427(17) Uani 1 1 d . . . H80 H 0.6508 0.7982 0.3907 0.051 Uiso 1 1 calc R . . C63 C 0.6692(9) 0.2287(5) 0.4571(3) 0.0402(16) Uani 1 1 d . . . H63 H 0.6821 0.1657 0.4608 0.048 Uiso 1 1 calc R . . C86 C 1.2190(8) 0.4016(6) 0.4217(3) 0.0412(16) Uani 1 1 d . . . H86 H 1.3030 0.3567 0.4302 0.049 Uiso 1 1 calc R . . C88 C 1.0867(8) 0.5436(5) 0.4316(3) 0.0388(15) Uani 1 1 d . . . H88 H 1.0804 0.5939 0.4470 0.047 Uiso 1 1 calc R . . C65 C -0.4389(8) 1.1451(5) -0.1463(3) 0.0371(15) Uani 1 1 d . . . C87 C 1.2101(8) 0.4770(6) 0.4434(3) 0.0415(17) Uani 1 1 d . . . H87 H 1.2886 0.4829 0.4664 0.050 Uiso 1 1 calc R . . C41 C -0.3282(8) 0.9755(5) -0.3180(3) 0.0344(14) Uani 1 1 d . . . C81 C 0.5710(9) 0.7215(5) 0.3449(3) 0.0420(16) Uani 1 1 d . . . H81 H 0.4815 0.7601 0.3323 0.050 Uiso 1 1 calc R . . C55 C 1.0104(9) 0.2190(5) 0.2804(3) 0.0408(16) Uani 1 1 d . . . H55 H 1.0782 0.2071 0.2524 0.049 Uiso 1 1 calc R . . C49 C -0.1523(9) 1.2228(5) -0.3294(4) 0.047(2) Uani 1 1 d . . . H49 H -0.1151 1.2776 -0.3315 0.057 Uiso 1 1 calc R . . C46 C -0.2632(8) 1.0605(5) -0.3238(3) 0.0341(14) Uani 1 1 d . . . C82 C 0.6059(8) 0.6405(5) 0.3285(3) 0.0363(15) Uani 1 1 d . . . H82 H 0.5383 0.6258 0.3046 0.044 Uiso 1 1 calc R . . C73 C -0.7922(8) 1.1242(5) -0.2540(4) 0.0405(17) Uani 1 1 d . . . H73 H -0.8662 1.1202 -0.2795 0.049 Uiso 1 1 calc R . . C53 C 0.8667(10) 0.1668(5) 0.3663(3) 0.0451(18) Uani 1 1 d . . . H53 H 0.8354 0.1191 0.3958 0.054 Uiso 1 1 calc R . . C54 C 0.9644(11) 0.1485(6) 0.3232(4) 0.053(2) Uani 1 1 d . . . H54 H 0.9984 0.0878 0.3236 0.064 Uiso 1 1 calc R . . C50 C -0.1563(10) 1.1928(7) -0.3785(4) 0.053(2) Uani 1 1 d . . . H50 H -0.1230 1.2281 -0.4138 0.063 Uiso 1 1 calc R . . C67 C -0.3030(11) 1.2148(6) -0.0880(4) 0.055(2) Uani 1 1 d . . . H67 H -0.3000 1.2577 -0.0669 0.066 Uiso 1 1 calc R . . C42 C -0.3568(11) 0.9379(7) -0.3629(3) 0.053(2) Uani 1 1 d . . . H42 H -0.3296 0.9661 -0.4009 0.064 Uiso 1 1 calc R . . C44 C -0.4675(10) 0.8177(6) -0.2948(4) 0.050(2) Uani 1 1 d . . . H44 H -0.5182 0.7664 -0.2868 0.059 Uiso 1 1 calc R . . C74 C -0.8222(9) 1.1825(6) -0.2213(5) 0.056(2) Uani 1 1 d . . . H74 H -0.9165 1.2175 -0.2233 0.067 Uiso 1 1 calc R . . C66 C -0.4336(10) 1.2097(6) -0.1147(4) 0.052(2) Uani 1 1 d . . . H66 H -0.5199 1.2497 -0.1119 0.062 Uiso 1 1 calc R . . C51 C -0.2095(10) 1.1104(6) -0.3765(3) 0.0491(19) Uani 1 1 d . . . H51 H -0.2092 1.0892 -0.4096 0.059 Uiso 1 1 calc R . . C75 C -0.7070(10) 1.1907(6) -0.1829(5) 0.057(2) Uani 1 1 d . . . H75 H -0.7254 1.2312 -0.1598 0.068 Uiso 1 1 calc R . . C43 C -0.4245(13) 0.8597(7) -0.3519(4) 0.063(3) Uani 1 1 d . . . H43 H -0.4420 0.8345 -0.3822 0.076 Uiso 1 1 calc R . . O10 O 0.152(2) 0.9868(14) -0.0707(9) 0.206(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02251(13) 0.01492(12) 0.02201(13) -0.00138(9) -0.00086(9) -0.00110(9) Ir2 0.02434(13) 0.02795(14) 0.01687(12) -0.00548(9) -0.00318(9) -0.00295(9) Nd1 0.02964(18) 0.02070(16) 0.02022(16) -0.00148(12) -0.00202(13) -0.00591(13) O2 0.035(2) 0.021(2) 0.026(2) 0.0006(17) 0.0017(18) 0.0007(17) N6 0.017(2) 0.032(3) 0.019(2) -0.005(2) 0.0001(18) -0.0024(19) O3 0.033(2) 0.032(2) 0.027(2) 0.0030(19) 0.0013(18) 0.0060(19) O5 0.041(3) 0.056(3) 0.021(2) 0.006(2) -0.0107(19) -0.018(2) O8 0.046(3) 0.038(3) 0.036(3) -0.016(2) 0.018(2) -0.009(2) O1 0.033(2) 0.027(2) 0.038(2) -0.0036(19) 0.0032(19) -0.0141(18) N2 0.024(2) 0.022(2) 0.020(2) 0.0001(19) -0.0036(19) -0.0002(19) N5 0.029(3) 0.030(3) 0.019(2) -0.004(2) -0.0026(19) -0.006(2) N3 0.027(3) 0.023(2) 0.026(2) -0.005(2) 0.000(2) 0.000(2) O6 0.043(3) 0.061(3) 0.027(2) -0.009(2) 0.002(2) -0.027(3) N1 0.019(2) 0.021(2) 0.026(2) -0.0034(19) 0.0020(19) -0.0028(18) N7 0.034(3) 0.033(3) 0.021(2) -0.008(2) -0.005(2) -0.006(2) O4 0.032(2) 0.037(3) 0.044(3) 0.000(2) 0.012(2) 0.006(2) C59 0.023(3) 0.041(3) 0.011(2) -0.004(2) -0.004(2) -0.001(2) N4 0.031(3) 0.024(3) 0.029(3) -0.003(2) 0.004(2) -0.004(2) C47 0.021(3) 0.023(3) 0.024(3) 0.002(2) 0.000(2) 0.001(2) O9 0.032(3) 0.043(3) 0.076(4) -0.017(3) -0.008(3) -0.012(2) C9 0.024(3) 0.022(3) 0.025(3) 0.001(2) 0.001(2) 0.002(2) N8 0.030(3) 0.028(3) 0.027(3) -0.005(2) -0.003(2) -0.001(2) C27 0.026(3) 0.036(3) 0.027(3) -0.007(3) -0.006(2) -0.005(2) O7 0.058(4) 0.051(3) 0.043(3) 0.008(3) 0.006(3) 0.013(3) C13 0.025(3) 0.022(3) 0.022(3) -0.004(2) -0.001(2) 0.002(2) C30 0.025(3) 0.030(3) 0.022(3) -0.006(2) -0.004(2) -0.002(2) C29 0.024(3) 0.028(3) 0.020(3) -0.005(2) 0.000(2) -0.002(2) C83 0.029(3) 0.035(3) 0.022(3) -0.004(2) -0.001(2) -0.008(3) C6 0.021(3) 0.019(3) 0.027(3) 0.000(2) -0.002(2) -0.001(2) C31 0.026(3) 0.025(3) 0.024(3) -0.001(2) -0.005(2) -0.004(2) C78 0.032(3) 0.026(3) 0.025(3) -0.003(2) 0.003(2) -0.005(2) C23 0.026(3) 0.027(3) 0.021(3) -0.009(2) -0.001(2) -0.002(2) C5 0.023(3) 0.019(3) 0.024(3) -0.003(2) 0.001(2) -0.001(2) C12 0.028(3) 0.022(3) 0.025(3) 0.001(2) 0.001(2) -0.001(2) C11 0.028(3) 0.019(3) 0.022(3) -0.002(2) -0.001(2) -0.001(2) C56 0.034(3) 0.036(3) 0.026(3) -0.013(3) 0.001(3) -0.004(3) C34 0.033(3) 0.035(3) 0.019(3) -0.005(2) -0.006(2) -0.006(3) C52 0.038(3) 0.032(3) 0.028(3) -0.008(3) -0.004(3) -0.005(3) C45 0.036(3) 0.025(3) 0.036(3) -0.010(3) -0.003(3) -0.006(3) C71 0.025(3) 0.019(3) 0.035(3) 0.002(2) 0.005(2) -0.001(2) C14 0.026(3) 0.025(3) 0.033(3) -0.004(3) 0.003(2) -0.004(2) C26 0.026(3) 0.033(3) 0.027(3) -0.003(3) 0.001(2) -0.006(2) C8 0.024(3) 0.024(3) 0.027(3) -0.005(2) 0.003(2) -0.004(2) C72 0.024(3) 0.023(3) 0.041(4) 0.003(3) -0.004(3) -0.005(2) C7 0.024(3) 0.019(3) 0.022(3) -0.001(2) -0.001(2) -0.004(2) C15 0.031(3) 0.020(3) 0.029(3) -0.001(2) 0.000(2) -0.003(2) C16 0.023(3) 0.019(3) 0.022(3) -0.001(2) -0.001(2) 0.003(2) C19 0.029(3) 0.022(3) 0.019(3) -0.003(2) 0.000(2) -0.009(2) C24 0.026(3) 0.042(4) 0.020(3) -0.008(3) -0.002(2) -0.007(3) C33 0.030(3) 0.043(4) 0.022(3) -0.007(3) 0.002(2) -0.007(3) C32 0.026(3) 0.039(3) 0.025(3) -0.005(3) -0.005(2) -0.009(3) C58 0.033(3) 0.036(3) 0.025(3) -0.006(3) -0.001(3) -0.005(3) C69 0.055(4) 0.030(3) 0.031(3) -0.008(3) -0.010(3) -0.008(3) C79 0.042(4) 0.030(3) 0.037(4) -0.012(3) 0.003(3) -0.008(3) C25 0.031(3) 0.031(3) 0.027(3) -0.006(3) 0.000(3) -0.002(3) C62 0.041(4) 0.051(4) 0.026(3) 0.002(3) 0.004(3) -0.006(3) C48 0.029(3) 0.030(3) 0.039(4) 0.003(3) -0.008(3) -0.002(3) C85 0.033(3) 0.042(4) 0.027(3) -0.011(3) -0.007(3) 0.002(3) C84 0.033(3) 0.033(3) 0.019(3) -0.005(2) -0.003(2) -0.010(3) C37 0.039(4) 0.028(3) 0.028(3) -0.007(3) 0.000(3) -0.006(3) C68 0.066(5) 0.045(4) 0.044(4) -0.017(4) -0.007(4) -0.016(4) C60 0.039(4) 0.042(4) 0.020(3) -0.010(3) -0.001(3) -0.004(3) C61 0.039(4) 0.057(5) 0.022(3) -0.012(3) 0.004(3) -0.001(3) C70 0.031(3) 0.027(3) 0.047(4) -0.011(3) 0.006(3) -0.002(3) C80 0.049(4) 0.030(4) 0.050(4) -0.012(3) 0.011(3) -0.007(3) C63 0.047(4) 0.037(4) 0.031(3) 0.002(3) 0.000(3) -0.006(3) C86 0.029(3) 0.051(4) 0.042(4) -0.014(3) -0.012(3) 0.003(3) C88 0.040(4) 0.042(4) 0.037(4) -0.012(3) -0.007(3) -0.011(3) C65 0.037(4) 0.029(3) 0.048(4) -0.015(3) 0.013(3) -0.005(3) C87 0.032(4) 0.059(5) 0.034(4) -0.012(3) -0.013(3) -0.008(3) C41 0.037(4) 0.037(4) 0.028(3) -0.007(3) -0.002(3) -0.003(3) C81 0.043(4) 0.033(4) 0.044(4) -0.004(3) 0.004(3) 0.002(3) C55 0.047(4) 0.044(4) 0.032(3) -0.018(3) 0.004(3) 0.003(3) C49 0.043(4) 0.036(4) 0.051(5) 0.015(3) -0.010(3) -0.017(3) C46 0.037(3) 0.027(3) 0.031(3) 0.001(3) -0.005(3) 0.001(3) C82 0.039(4) 0.036(4) 0.029(3) -0.003(3) -0.007(3) 0.000(3) C73 0.027(3) 0.031(3) 0.055(5) 0.003(3) -0.006(3) -0.004(3) C53 0.061(5) 0.035(4) 0.037(4) -0.008(3) 0.008(4) -0.004(3) C54 0.068(6) 0.037(4) 0.052(5) -0.017(4) 0.002(4) 0.012(4) C50 0.048(5) 0.061(5) 0.037(4) 0.014(4) 0.007(3) -0.021(4) C67 0.078(6) 0.048(5) 0.051(5) -0.031(4) 0.005(4) -0.014(4) C42 0.070(6) 0.063(5) 0.028(4) -0.011(4) 0.002(4) -0.015(4) C44 0.060(5) 0.042(4) 0.054(5) -0.020(4) -0.010(4) -0.013(4) C74 0.027(4) 0.035(4) 0.098(7) -0.011(4) 0.000(4) 0.008(3) C66 0.056(5) 0.042(4) 0.066(6) -0.030(4) 0.011(4) -0.007(4) C51 0.062(5) 0.051(5) 0.029(4) 0.000(3) 0.004(3) -0.012(4) C75 0.046(5) 0.039(4) 0.089(7) -0.029(5) 0.006(4) 0.004(4) C43 0.097(8) 0.062(6) 0.043(5) -0.027(4) -0.005(5) -0.025(5) _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 C47 2.003(6) . ? Ir1 C71 2.014(6) . ? Ir1 N4 2.040(5) . ? Ir1 N3 2.049(5) . ? Ir1 N2 2.133(5) . ? Ir1 N1 2.150(5) . ? Ir2 C59 1.992(6) . ? Ir2 C84 2.015(6) . ? Ir2 N7 2.044(6) . ? Ir2 N8 2.047(5) . ? Ir2 N6 2.129(5) . ? Ir2 N5 2.148(5) . ? Nd1 O5 2.365(4) . ? Nd1 O2 2.369(4) 2_565 ? Nd1 O3 2.376(5) . ? Nd1 O8 2.392(5) 1_455 ? Nd1 O9 2.406(5) . ? Nd1 O9 2.429(6) 2_565 ? Nd1 O1 2.443(4) 1_655 ? Nd1 Nd1 4.0829(7) 2_565 ? O2 C19 1.260(7) . ? O2 Nd1 2.369(4) 2_565 ? N6 C27 1.356(8) . ? N6 C23 1.360(7) . ? O3 C16 1.273(7) . ? O5 C34 1.242(8) . ? O8 C37 1.267(8) . ? O8 Nd1 2.392(5) 1_655 ? O1 C19 1.254(8) . ? O1 Nd1 2.443(4) 1_455 ? N2 C9 1.346(8) . ? N2 C5 1.365(7) . ? N5 C33 1.345(8) . ? N5 C29 1.351(8) . ? N3 C45 1.352(8) . ? N3 C41 1.377(8) . ? O6 C34 1.244(8) . ? N1 C15 1.333(8) . ? N1 C11 1.357(8) . ? N7 C52 1.350(9) . ? N7 C56 1.352(9) . ? O4 C16 1.230(8) . ? C59 C60 1.396(9) . ? C59 C58 1.423(9) . ? N4 C69 1.335(9) . ? N4 C65 1.370(9) . ? C47 C46 1.406(9) . ? C47 C48 1.415(9) . ? O9 Nd1 2.429(6) 2_565 ? C9 C8 1.395(8) . ? N8 C82 1.348(9) . ? N8 C78 1.350(8) . ? C27 C26 1.395(9) . ? O7 C37 1.224(9) . ? C13 C12 1.379(9) . ? C13 C14 1.398(9) . ? C13 C16 1.530(7) . ? C30 C31 1.393(9) . ? C30 C29 1.403(8) . ? C29 C23 1.475(8) . ? C83 C88 1.400(9) . ? C83 C84 1.413(9) . ? C83 C78 1.485(9) . ? C6 C7 1.382(8) . ? C6 C5 1.390(8) . ? C31 C32 1.367(9) . ? C31 C34 1.529(8) . ? C78 C79 1.402(9) . ? C23 C24 1.391(8) . ? C5 C11 1.464(8) . ? C12 C11 1.387(8) . ? C56 C55 1.366(10) . ? C52 C53 1.400(10) . ? C52 C58 1.460(10) . ? C45 C44 1.381(10) . ? C71 C72 1.392(9) . ? C71 C70 1.414(9) . ? C14 C15 1.382(9) . ? C26 C25 1.388(9) . ? C8 C7 1.391(8) . ? C72 C73 1.394(9) . ? C7 C19 1.504(8) . ? C24 C25 1.383(9) . ? C33 C32 1.394(9) . ? C58 C63 1.398(10) . ? C69 C68 1.373(10) . ? C79 C80 1.390(11) . ? C25 C37 1.522(9) . ? C62 C63 1.364(11) . ? C62 C61 1.391(12) . ? C48 C49 1.384(10) . ? C85 C84 1.391(9) . ? C85 C86 1.400(9) . ? C68 C67 1.381(13) . ? C60 C61 1.390(10) . ? C70 C75 1.395(10) . ? C70 C65 1.467(11) . ? C80 C81 1.372(12) . ? C86 C87 1.376(11) . ? C88 C87 1.371(11) . ? C65 C66 1.398(10) . ? C41 C42 1.388(10) . ? C41 C46 1.463(10) . ? C81 C82 1.386(11) . ? C55 C54 1.364(12) . ? C49 C50 1.369(13) . ? C46 C51 1.389(10) . ? C73 C74 1.329(13) . ? C53 C54 1.395(12) . ? C50 C51 1.391(13) . ? C67 C66 1.367(13) . ? C42 C43 1.369(13) . ? C44 C43 1.404(13) . ? C74 C75 1.435(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C47 Ir1 C71 89.2(2) . . ? C47 Ir1 N4 93.6(2) . . ? C71 Ir1 N4 81.1(2) . . ? C47 Ir1 N3 80.6(2) . . ? C71 Ir1 N3 92.3(2) . . ? N4 Ir1 N3 171.4(2) . . ? C47 Ir1 N2 171.8(2) . . ? C71 Ir1 N2 97.3(2) . . ? N4 Ir1 N2 92.3(2) . . ? N3 Ir1 N2 94.1(2) . . ? C47 Ir1 N1 96.7(2) . . ? C71 Ir1 N1 174.0(2) . . ? N4 Ir1 N1 97.2(2) . . ? N3 Ir1 N1 89.86(19) . . ? N2 Ir1 N1 76.93(18) . . ? C59 Ir2 C84 86.9(2) . . ? C59 Ir2 N7 80.5(2) . . ? C84 Ir2 N7 92.4(2) . . ? C59 Ir2 N8 93.8(2) . . ? C84 Ir2 N8 80.8(2) . . ? N7 Ir2 N8 171.4(2) . . ? C59 Ir2 N6 172.1(2) . . ? C84 Ir2 N6 100.2(2) . . ? N7 Ir2 N6 95.7(2) . . ? N8 Ir2 N6 90.7(2) . . ? C59 Ir2 N5 96.7(2) . . ? C84 Ir2 N5 176.3(2) . . ? N7 Ir2 N5 88.9(2) . . ? N8 Ir2 N5 98.3(2) . . ? N6 Ir2 N5 76.20(19) . . ? O5 Nd1 O2 80.07(18) . 2_565 ? O5 Nd1 O3 146.43(17) . . ? O2 Nd1 O3 88.02(15) 2_565 . ? O5 Nd1 O8 88.79(19) . 1_455 ? O2 Nd1 O8 168.83(17) 2_565 1_455 ? O3 Nd1 O8 101.01(17) . 1_455 ? O5 Nd1 O9 136.35(19) . . ? O2 Nd1 O9 95.55(18) 2_565 . ? O3 Nd1 O9 75.66(19) . . ? O8 Nd1 O9 93.07(19) 1_455 . ? O5 Nd1 O9 72.63(18) . 2_565 ? O2 Nd1 O9 96.86(17) 2_565 2_565 ? O3 Nd1 O9 140.41(18) . 2_565 ? O8 Nd1 O9 80.42(18) 1_455 2_565 ? O9 Nd1 O9 64.8(3) . 2_565 ? O5 Nd1 O1 75.83(16) . 1_655 ? O2 Nd1 O1 96.47(16) 2_565 1_655 ? O3 Nd1 O1 74.48(17) . 1_655 ? O8 Nd1 O1 79.87(17) 1_455 1_655 ? O9 Nd1 O1 147.29(18) . 1_655 ? O9 Nd1 O1 142.90(18) 2_565 1_655 ? O5 Nd1 Nd1 104.41(12) . 2_565 ? O2 Nd1 Nd1 97.35(11) 2_565 2_565 ? O3 Nd1 Nd1 108.20(12) . 2_565 ? O8 Nd1 Nd1 86.13(12) 1_455 2_565 ? O9 Nd1 Nd1 32.55(15) . 2_565 ? O9 Nd1 Nd1 32.22(14) 2_565 2_565 ? O1 Nd1 Nd1 166.00(11) 1_655 2_565 ? C19 O2 Nd1 149.8(4) . 2_565 ? C27 N6 C23 117.6(5) . . ? C27 N6 Ir2 125.9(4) . . ? C23 N6 Ir2 116.5(4) . . ? C16 O3 Nd1 159.5(4) . . ? C34 O5 Nd1 149.9(5) . . ? C37 O8 Nd1 142.9(4) . 1_655 ? C19 O1 Nd1 135.3(4) . 1_455 ? C9 N2 C5 118.9(5) . . ? C9 N2 Ir1 126.0(4) . . ? C5 N2 Ir1 114.7(4) . . ? C33 N5 C29 119.2(5) . . ? C33 N5 Ir2 124.4(4) . . ? C29 N5 Ir2 115.5(4) . . ? C45 N3 C41 120.0(6) . . ? C45 N3 Ir1 124.7(4) . . ? C41 N3 Ir1 115.1(4) . . ? C15 N1 C11 118.0(5) . . ? C15 N1 Ir1 127.2(4) . . ? C11 N1 Ir1 114.6(4) . . ? C52 N7 C56 119.3(6) . . ? C52 N7 Ir2 115.7(4) . . ? C56 N7 Ir2 124.7(5) . . ? C60 C59 C58 115.9(6) . . ? C60 C59 Ir2 129.4(5) . . ? C58 C59 Ir2 114.7(4) . . ? C69 N4 C65 119.4(6) . . ? C69 N4 Ir1 125.1(5) . . ? C65 N4 Ir1 115.3(5) . . ? C46 C47 C48 116.3(6) . . ? C46 C47 Ir1 115.1(5) . . ? C48 C47 Ir1 128.6(5) . . ? Nd1 O9 Nd1 115.2(3) . 2_565 ? N2 C9 C8 121.7(5) . . ? C82 N8 C78 118.7(6) . . ? C82 N8 Ir2 125.2(5) . . ? C78 N8 Ir2 116.0(4) . . ? N6 C27 C26 123.1(6) . . ? C12 C13 C14 118.1(5) . . ? C12 C13 C16 120.4(5) . . ? C14 C13 C16 121.5(5) . . ? C31 C30 C29 119.0(6) . . ? N5 C29 C30 121.2(6) . . ? N5 C29 C23 115.5(5) . . ? C30 C29 C23 123.2(5) . . ? C88 C83 C84 121.5(6) . . ? C88 C83 C78 123.5(6) . . ? C84 C83 C78 114.9(5) . . ? C7 C6 C5 120.0(5) . . ? C32 C31 C30 119.1(5) . . ? C32 C31 C34 122.0(6) . . ? C30 C31 C34 118.8(5) . . ? N8 C78 C79 121.3(6) . . ? N8 C78 C83 114.1(5) . . ? C79 C78 C83 124.6(6) . . ? N6 C23 C24 121.8(6) . . ? N6 C23 C29 115.0(5) . . ? C24 C23 C29 123.1(5) . . ? N2 C5 C6 121.2(5) . . ? N2 C5 C11 116.2(5) . . ? C6 C5 C11 122.5(5) . . ? C13 C12 C11 120.3(6) . . ? N1 C11 C12 121.4(6) . . ? N1 C11 C5 116.1(5) . . ? C12 C11 C5 122.5(5) . . ? N7 C56 C55 122.5(7) . . ? O5 C34 O6 127.1(6) . . ? O5 C34 C31 115.6(6) . . ? O6 C34 C31 117.3(5) . . ? N7 C52 C53 120.8(7) . . ? N7 C52 C58 114.6(6) . . ? C53 C52 C58 124.5(7) . . ? N3 C45 C44 122.2(7) . . ? C72 C71 C70 116.7(6) . . ? C72 C71 Ir1 129.5(5) . . ? C70 C71 Ir1 113.7(5) . . ? C15 C14 C13 118.4(6) . . ? C25 C26 C27 118.6(6) . . ? C7 C8 C9 119.6(5) . . ? C71 C72 C73 121.4(7) . . ? C6 C7 C8 118.5(5) . . ? C6 C7 C19 119.8(5) . . ? C8 C7 C19 121.7(5) . . ? N1 C15 C14 123.7(6) . . ? O4 C16 O3 127.2(5) . . ? O4 C16 C13 117.8(5) . . ? O3 C16 C13 115.1(5) . . ? O1 C19 O2 124.8(5) . . ? O1 C19 C7 117.1(5) . . ? O2 C19 C7 118.0(5) . . ? C25 C24 C23 120.0(6) . . ? N5 C33 C32 121.9(6) . . ? C31 C32 C33 119.6(6) . . ? C63 C58 C59 122.1(6) . . ? C63 C58 C52 123.6(7) . . ? C59 C58 C52 114.2(6) . . ? N4 C69 C68 122.8(8) . . ? C80 C79 C78 118.9(7) . . ? C24 C25 C26 118.8(6) . . ? C24 C25 C37 119.5(6) . . ? C26 C25 C37 121.5(6) . . ? C63 C62 C61 120.4(7) . . ? C49 C48 C47 121.3(7) . . ? C84 C85 C86 121.1(7) . . ? C85 C84 C83 117.2(6) . . ? C85 C84 Ir2 128.7(5) . . ? C83 C84 Ir2 114.1(5) . . ? O7 C37 O8 127.0(7) . . ? O7 C37 C25 115.9(6) . . ? O8 C37 C25 117.1(6) . . ? C69 C68 C67 118.9(8) . . ? C61 C60 C59 122.1(7) . . ? C60 C61 C62 119.9(6) . . ? C75 C70 C71 121.6(7) . . ? C75 C70 C65 123.1(7) . . ? C71 C70 C65 115.3(6) . . ? C81 C80 C79 119.5(7) . . ? C62 C63 C58 119.5(7) . . ? C87 C86 C85 120.2(7) . . ? C87 C88 C83 119.3(7) . . ? N4 C65 C66 119.1(7) . . ? N4 C65 C70 114.3(6) . . ? C66 C65 C70 126.5(7) . . ? C88 C87 C86 120.7(6) . . ? N3 C41 C42 119.4(7) . . ? N3 C41 C46 114.2(6) . . ? C42 C41 C46 126.4(7) . . ? C80 C81 C82 118.8(7) . . ? C54 C55 C56 118.8(7) . . ? C50 C49 C48 120.4(7) . . ? C51 C46 C47 122.6(7) . . ? C51 C46 C41 122.5(7) . . ? C47 C46 C41 114.9(6) . . ? N8 C82 C81 122.7(7) . . ? C74 C73 C72 122.3(7) . . ? C54 C53 C52 118.1(7) . . ? C55 C54 C53 120.4(7) . . ? C49 C50 C51 120.9(7) . . ? C66 C67 C68 118.9(7) . . ? C43 C42 C41 120.6(8) . . ? C45 C44 C43 117.9(7) . . ? C73 C74 C75 119.0(7) . . ? C67 C66 C65 120.8(8) . . ? C46 C51 C50 118.5(8) . . ? C70 C75 C74 119.0(8) . . ? C42 C43 C44 119.8(7) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 73.29 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 2.819 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.186 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.009 0.000 0.500 252 54 ' ' 2 0.500 0.000 0.000 78 30 ' ' 3 0.301 0.625 0.262 23 1 ' ' 4 0.699 0.375 0.738 23 1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 960741' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Ir-Er _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H44 Er Ir2 N8 O10' _chemical_formula_weight 1684.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 9.00246(19) _cell_length_b 15.2262(3) _cell_length_c 23.4324(5) _cell_angle_alpha 73.8380(18) _cell_angle_beta 89.0785(17) _cell_angle_gamma 83.0742(16) _cell_volume 3061.99(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15178 _cell_measurement_theta_min 3.8980 _cell_measurement_theta_max 73.0580 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 11.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54318 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28021 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 73.18 _reflns_number_total 11887 _reflns_number_gt 10483 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0545P)^2^+16.4460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11887 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.002 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 0.78176(3) 0.953339(18) 0.329079(10) 0.03127(8) Uani 1 1 d . . . Ir2 Ir -0.32015(3) 1.497831(15) -0.194056(11) 0.02979(8) Uani 1 1 d . . . Er3 Er 0.20140(7) 1.04492(3) 0.006820(17) 0.05682(15) Uani 1 1 d . . . O1 O 0.1604(7) 0.8806(6) 0.1740(2) 0.077(2) Uani 1 1 d . . . O2 O 0.2734(7) 0.9710(5) 0.0999(2) 0.0648(16) Uani 1 1 d . . . O3 O 0.3741(6) 1.2072(4) -0.1604(3) 0.0618(16) Uani 1 1 d . . . O4 O 0.2437(6) 1.1270(3) -0.0864(2) 0.0453(11) Uani 1 1 d . . . O5 O 0.8417(10) 1.2437(6) 0.0427(3) 0.088(2) Uani 1 1 d . . . O6 O 1.0651(8) 1.1524(4) 0.0396(3) 0.0680(18) Uani 1 1 d . . . O7 O -0.6028(7) 1.1293(4) 0.0180(2) 0.0567(14) Uani 1 1 d . . . O9 O -0.3668(7) 1.0681(3) 0.0111(2) 0.0572(14) Uani 1 1 d . . . N1 N -0.2872(7) 1.5782(4) -0.1394(3) 0.0455(14) Uani 1 1 d . . . N2 N -0.1133(5) 1.4084(3) -0.1724(2) 0.0332(11) Uani 1 1 d . . . N3 N -0.3794(6) 1.3883(3) -0.1212(2) 0.0324(10) Uani 1 1 d . . . N4 N -0.3689(6) 1.4341(3) -0.2569(2) 0.0345(11) Uani 1 1 d . . . N5 N 0.8551(6) 0.8235(4) 0.3241(2) 0.0367(11) Uani 1 1 d . . . N6 N 0.7248(6) 1.0789(4) 0.3458(2) 0.0395(12) Uani 1 1 d . . . N7 N 0.5910(6) 0.9557(4) 0.2746(2) 0.0364(11) Uani 1 1 d . . . N8 N 0.8496(6) 1.0221(3) 0.2416(2) 0.0322(10) Uani 1 1 d . . . C5 C -0.3352(9) 1.4773(5) -0.3133(3) 0.0470(16) Uani 1 1 d . . . C6 C -0.3720(13) 1.4416(7) -0.3597(4) 0.077(3) Uani 1 1 d . . . H6 H -0.3461 1.4700 -0.3984 0.092 Uiso 1 1 calc R . . C7 C -0.4455(14) 1.3654(8) -0.3483(5) 0.084(3) Uani 1 1 d . . . H7 H -0.4715 1.3425 -0.3792 0.100 Uiso 1 1 calc R . . C8 C -0.4814(11) 1.3222(6) -0.2902(4) 0.064(2) Uani 1 1 d . . . H8 H -0.5327 1.2706 -0.2815 0.077 Uiso 1 1 calc R . . C9 C -0.4388(8) 1.3578(5) -0.2461(4) 0.0467(16) Uani 1 1 d . . . H9 H -0.4592 1.3279 -0.2069 0.056 Uiso 1 1 calc R . . C10 C -0.2623(8) 1.5604(5) -0.3197(3) 0.0473(16) Uani 1 1 d . . . C11 C -0.2483(7) 1.5866(4) -0.2677(3) 0.0364(13) Uani 1 1 d . . . C12 C -0.1867(8) 1.6676(5) -0.2721(4) 0.0483(17) Uani 1 1 d . . . H12 H -0.1778 1.6875 -0.2384 0.058 Uiso 1 1 calc R . . C13 C -0.1383(10) 1.7189(6) -0.3262(4) 0.063(2) Uani 1 1 d . . . H13 H -0.0988 1.7733 -0.3283 0.076 Uiso 1 1 calc R . . C14 C -0.1474(11) 1.6909(7) -0.3767(4) 0.073(3) Uani 1 1 d . . . H14 H -0.1110 1.7249 -0.4124 0.088 Uiso 1 1 calc R . . C15 C -0.2111(11) 1.6118(7) -0.3740(4) 0.069(2) Uani 1 1 d . . . H15 H -0.2199 1.5927 -0.4081 0.082 Uiso 1 1 calc R . . C17 C -0.2724(7) 1.3146(4) -0.1051(3) 0.0324(12) Uani 1 1 d . . . C18 C -0.3017(8) 1.2329(4) -0.0658(3) 0.0381(14) Uani 1 1 d . . . H18 H -0.2270 1.1831 -0.0556 0.046 Uiso 1 1 calc R . . C19 C -0.4405(8) 1.2250(4) -0.0417(3) 0.0371(13) Uani 1 1 d . . . C20 C -0.5482(8) 1.3013(5) -0.0567(3) 0.0413(14) Uani 1 1 d . . . H20 H -0.6427 1.2982 -0.0401 0.050 Uiso 1 1 calc R . . C21 C -0.5140(7) 1.3823(4) -0.0965(3) 0.0392(14) Uani 1 1 d . . . H21 H -0.5863 1.4334 -0.1063 0.047 Uiso 1 1 calc R . . C23 C -0.1248(7) 1.3271(4) -0.1321(3) 0.0335(12) Uani 1 1 d . . . C24 C -0.0038(7) 1.2594(4) -0.1165(3) 0.0344(12) Uani 1 1 d . . . H24 H -0.0144 1.2042 -0.0881 0.041 Uiso 1 1 calc R . . C25 C 0.1331(7) 1.2737(4) -0.1432(3) 0.0342(12) Uani 1 1 d . . . C26 C 0.1465(7) 1.3586(5) -0.1835(3) 0.0421(15) Uani 1 1 d . . . H26 H 0.2379 1.3717 -0.2009 0.051 Uiso 1 1 calc R . . C27 C 0.0204(7) 1.4236(4) -0.1974(3) 0.0401(14) Uani 1 1 d . . . H27 H 0.0289 1.4800 -0.2250 0.048 Uiso 1 1 calc R . . C28 C 0.2641(7) 1.1965(4) -0.1296(3) 0.0379(14) Uani 1 1 d . . . C31 C -0.4744(9) 1.1329(4) -0.0009(3) 0.0430(16) Uani 1 1 d . . . C35 C 0.7507(7) 1.0287(4) 0.1969(3) 0.0327(12) Uani 1 1 d . . . C36 C 0.7812(8) 1.0740(5) 0.1384(3) 0.0453(16) Uani 1 1 d . . . H36 H 0.7130 1.0779 0.1081 0.054 Uiso 1 1 calc R . . C37 C 0.9138(9) 1.1133(6) 0.1252(3) 0.0548(19) Uani 1 1 d . . . C38 C 1.0156(8) 1.1015(6) 0.1706(3) 0.0490(17) Uani 1 1 d . . . H38 H 1.1090 1.1220 0.1626 0.059 Uiso 1 1 calc R . . C39 C 0.9780(8) 1.0592(5) 0.2277(3) 0.0421(14) Uani 1 1 d . . . H39 H 1.0447 1.0561 0.2583 0.051 Uiso 1 1 calc R . . C41 C 0.6091(7) 0.9885(4) 0.2150(3) 0.0322(12) Uani 1 1 d . . . C42 C 0.5024(7) 0.9816(4) 0.1751(3) 0.0361(13) Uani 1 1 d . . . H42 H 0.5166 1.0036 0.1345 0.043 Uiso 1 1 calc R . . C43 C 0.3751(7) 0.9420(4) 0.1957(3) 0.0352(13) Uani 1 1 d . . . C44 C 0.3557(7) 0.9124(5) 0.2569(3) 0.0407(14) Uani 1 1 d . . . H44 H 0.2697 0.8870 0.2722 0.049 Uiso 1 1 calc R . . C45 C 0.4651(8) 0.9213(5) 0.2941(3) 0.0433(15) Uani 1 1 d . . . H45 H 0.4505 0.9025 0.3349 0.052 Uiso 1 1 calc R . . C46 C 0.2588(8) 0.9293(6) 0.1536(3) 0.0466(17) Uani 1 1 d . . . C49 C 0.9401(11) 1.1769(6) 0.0628(4) 0.061(2) Uani 1 1 d . . . C52 C 0.7241(8) 0.7834(5) 0.4144(3) 0.0424(14) Uani 1 1 d . . . C53 C 0.6658(10) 0.7229(6) 0.4634(4) 0.0568(19) Uani 1 1 d . . . H53 H 0.6815 0.6597 0.4684 0.068 Uiso 1 1 calc R . . C54 C 0.5849(10) 0.7576(6) 0.5043(4) 0.062(2) Uani 1 1 d . . . H54 H 0.5449 0.7176 0.5367 0.074 Uiso 1 1 calc R . . C55 C 0.5627(8) 0.8507(6) 0.4977(3) 0.0519(18) Uani 1 1 d . . . H55 H 0.5105 0.8730 0.5263 0.062 Uiso 1 1 calc R . . C56 C 0.6177(8) 0.9117(5) 0.4485(3) 0.0424(14) Uani 1 1 d . . . H56 H 0.6002 0.9747 0.4441 0.051 Uiso 1 1 calc R . . C57 C 0.6988(7) 0.8796(4) 0.4056(3) 0.0340(12) Uani 1 1 d . . . C59 C 0.8165(9) 0.7536(5) 0.3699(3) 0.0454(15) Uani 1 1 d . . . C60 C 0.8732(11) 0.6628(6) 0.3733(4) 0.064(2) Uani 1 1 d . . . H60 H 0.8460 0.6146 0.4042 0.077 Uiso 1 1 calc R . . C61 C 0.9693(12) 0.6449(6) 0.3307(5) 0.071(3) Uani 1 1 d . . . H61 H 1.0063 0.5844 0.3325 0.086 Uiso 1 1 calc R . . C62 C 1.0106(10) 0.7161(6) 0.2856(4) 0.059(2) Uani 1 1 d . . . H62 H 1.0790 0.7049 0.2576 0.071 Uiso 1 1 calc R . . C63 C 0.9491(8) 0.8044(5) 0.2826(3) 0.0455(15) Uani 1 1 d . . . H63 H 0.9731 0.8525 0.2510 0.055 Uiso 1 1 calc R . . C65 C 0.8244(8) 1.1036(4) 0.3798(3) 0.0382(13) Uani 1 1 d . . . C66 C 0.7929(10) 1.1863(5) 0.3945(4) 0.0538(18) Uani 1 1 d . . . H66 H 0.8592 1.2025 0.4187 0.065 Uiso 1 1 calc R . . C67 C 0.6653(10) 1.2436(5) 0.3737(4) 0.059(2) Uani 1 1 d . . . H67 H 0.6461 1.2996 0.3827 0.071 Uiso 1 1 calc R . . C68 C 0.5647(10) 1.2182(6) 0.3391(4) 0.060(2) Uani 1 1 d . . . H68 H 0.4769 1.2564 0.3248 0.072 Uiso 1 1 calc R . . C69 C 0.5974(9) 1.1350(5) 0.3262(3) 0.0508(17) Uani 1 1 d . . . H69 H 0.5297 1.1171 0.3033 0.061 Uiso 1 1 calc R . . C70 C 0.9589(8) 1.0374(5) 0.3970(3) 0.0396(14) Uani 1 1 d . . . C71 C 0.9641(7) 0.9582(5) 0.3767(3) 0.0383(13) Uani 1 1 d . . . C72 C 1.0903(8) 0.8921(5) 0.3923(3) 0.0483(16) Uani 1 1 d . . . H72 H 1.0962 0.8390 0.3797 0.058 Uiso 1 1 calc R . . C73 C 1.2061(9) 0.9051(6) 0.4262(4) 0.057(2) Uani 1 1 d . . . H73 H 1.2891 0.8608 0.4361 0.068 Uiso 1 1 calc R . . C74 C 1.1989(10) 0.9833(6) 0.4453(4) 0.060(2) Uani 1 1 d . . . H74 H 1.2774 0.9917 0.4677 0.072 Uiso 1 1 calc R . . C75 C 1.0765(9) 1.0486(6) 0.4313(3) 0.0532(18) Uani 1 1 d . . . H75 H 1.0718 1.1008 0.4449 0.064 Uiso 1 1 calc R . . C77 C -0.4054(12) 1.6397(5) -0.1359(4) 0.063(2) Uani 1 1 d . . . C78 C -0.3900(17) 1.7034(7) -0.1039(6) 0.090(4) Uani 1 1 d . . . H78 H -0.4719 1.7448 -0.1002 0.108 Uiso 1 1 calc R . . C79 C -0.2576(19) 1.7052(8) -0.0786(6) 0.105(5) Uani 1 1 d . . . H79 H -0.2477 1.7488 -0.0583 0.126 Uiso 1 1 calc R . . C80 C -0.1381(15) 1.6431(9) -0.0824(5) 0.089(4) Uani 1 1 d . . . H80 H -0.0458 1.6439 -0.0654 0.107 Uiso 1 1 calc R . . C81 C -0.1584(13) 1.5783(7) -0.1127(4) 0.071(3) Uani 1 1 d . . . H81 H -0.0792 1.5338 -0.1143 0.085 Uiso 1 1 calc R . . C82 C -0.5380(11) 1.6363(5) -0.1692(4) 0.063(2) Uani 1 1 d . . . C83 C -0.5214(8) 1.5746(4) -0.2039(3) 0.0447(16) Uani 1 1 d . . . C84 C -0.6442(8) 1.5715(5) -0.2391(4) 0.058(2) Uani 1 1 d . . . H84 H -0.6352 1.5321 -0.2634 0.069 Uiso 1 1 calc R . . C85 C -0.7788(10) 1.6261(6) -0.2385(6) 0.079(3) Uani 1 1 d . . . H85 H -0.8590 1.6234 -0.2622 0.094 Uiso 1 1 calc R . . C86 C -0.7935(13) 1.6847(8) -0.2025(7) 0.107(5) Uani 1 1 d . . . H86 H -0.8842 1.7207 -0.2016 0.128 Uiso 1 1 calc R . . C87 C -0.6793(14) 1.6899(7) -0.1691(7) 0.093(4) Uani 1 1 d . . . H87 H -0.6915 1.7295 -0.1451 0.111 Uiso 1 1 calc R . . O8 O 0.0065(8) 0.9613(6) 0.0514(4) 0.093(2) Uani 1 1 d . . . O10 O 0.727(6) 0.462(2) 0.4822(14) 0.63(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 0.03129(14) 0.03814(14) 0.02391(12) -0.00664(10) -0.00473(9) -0.00647(10) Ir2 0.03076(13) 0.01968(11) 0.03475(14) -0.00055(9) 0.00127(9) -0.00354(9) Er3 0.1124(4) 0.0347(2) 0.02504(19) -0.00048(15) 0.0004(2) -0.0338(2) O1 0.070(4) 0.136(6) 0.038(3) -0.022(3) 0.005(3) -0.067(4) O2 0.056(3) 0.099(5) 0.028(2) 0.005(3) -0.011(2) -0.018(3) O3 0.053(3) 0.050(3) 0.066(4) 0.004(3) 0.020(3) 0.011(2) O4 0.051(3) 0.041(2) 0.033(2) 0.0016(19) 0.001(2) 0.008(2) O5 0.100(6) 0.086(5) 0.061(4) 0.007(4) -0.004(4) -0.005(4) O6 0.088(4) 0.077(4) 0.059(3) -0.041(3) 0.043(3) -0.042(3) O7 0.073(4) 0.054(3) 0.047(3) -0.007(2) 0.004(3) -0.041(3) O9 0.099(4) 0.031(2) 0.037(3) 0.004(2) -0.007(3) -0.020(3) N1 0.059(4) 0.035(3) 0.045(3) -0.009(2) 0.010(3) -0.021(3) N2 0.029(2) 0.023(2) 0.043(3) -0.003(2) -0.005(2) -0.0004(18) N3 0.034(3) 0.024(2) 0.035(3) 0.0007(19) 0.004(2) -0.0080(19) N4 0.034(3) 0.032(2) 0.037(3) -0.007(2) -0.002(2) -0.004(2) N5 0.039(3) 0.041(3) 0.031(3) -0.011(2) -0.002(2) -0.005(2) N6 0.046(3) 0.038(3) 0.031(3) -0.004(2) 0.002(2) -0.005(2) N7 0.038(3) 0.046(3) 0.025(2) -0.009(2) -0.007(2) -0.011(2) N8 0.031(2) 0.038(3) 0.029(2) -0.008(2) -0.0005(19) -0.008(2) C5 0.057(4) 0.046(4) 0.035(3) -0.005(3) -0.001(3) -0.010(3) C6 0.106(8) 0.085(7) 0.043(5) -0.016(4) 0.007(5) -0.036(6) C7 0.118(9) 0.084(7) 0.061(6) -0.032(5) -0.005(6) -0.037(7) C8 0.079(6) 0.052(5) 0.069(6) -0.025(4) -0.005(5) -0.021(4) C9 0.050(4) 0.036(3) 0.053(4) -0.008(3) 0.001(3) -0.012(3) C10 0.048(4) 0.042(4) 0.042(4) 0.004(3) 0.000(3) -0.006(3) C11 0.027(3) 0.029(3) 0.043(3) 0.005(2) 0.003(2) -0.001(2) C12 0.044(4) 0.037(3) 0.055(4) 0.005(3) -0.003(3) -0.011(3) C13 0.062(5) 0.045(4) 0.070(6) 0.014(4) -0.005(4) -0.026(4) C14 0.073(6) 0.073(6) 0.060(5) 0.014(5) 0.008(4) -0.034(5) C15 0.081(6) 0.072(6) 0.044(4) 0.003(4) 0.007(4) -0.022(5) C17 0.034(3) 0.029(3) 0.031(3) -0.002(2) -0.005(2) -0.006(2) C18 0.043(3) 0.026(3) 0.040(3) 0.002(2) -0.010(3) -0.009(2) C19 0.046(4) 0.030(3) 0.031(3) 0.002(2) -0.008(3) -0.014(3) C20 0.040(3) 0.043(3) 0.038(3) -0.001(3) 0.003(3) -0.014(3) C21 0.037(3) 0.034(3) 0.040(3) 0.002(3) 0.002(3) -0.008(2) C23 0.038(3) 0.026(3) 0.033(3) -0.003(2) -0.004(2) -0.007(2) C24 0.037(3) 0.027(3) 0.035(3) -0.003(2) -0.003(2) -0.001(2) C25 0.036(3) 0.031(3) 0.031(3) -0.004(2) -0.008(2) 0.003(2) C26 0.033(3) 0.040(3) 0.046(4) 0.000(3) 0.002(3) -0.003(3) C27 0.034(3) 0.030(3) 0.049(4) 0.002(3) 0.003(3) -0.005(2) C28 0.042(3) 0.032(3) 0.034(3) -0.004(2) -0.005(3) 0.007(3) C31 0.067(5) 0.034(3) 0.030(3) -0.002(3) -0.004(3) -0.027(3) C35 0.035(3) 0.036(3) 0.028(3) -0.010(2) 0.000(2) -0.003(2) C36 0.040(4) 0.065(4) 0.031(3) -0.012(3) -0.004(3) -0.006(3) C37 0.047(4) 0.080(6) 0.035(4) -0.009(4) 0.004(3) -0.017(4) C38 0.036(3) 0.066(5) 0.042(4) -0.007(3) 0.002(3) -0.014(3) C39 0.040(3) 0.048(4) 0.039(3) -0.012(3) -0.005(3) -0.011(3) C41 0.034(3) 0.034(3) 0.027(3) -0.005(2) -0.004(2) -0.004(2) C42 0.043(3) 0.040(3) 0.021(3) -0.001(2) -0.006(2) -0.003(3) C43 0.037(3) 0.040(3) 0.026(3) -0.002(2) -0.008(2) -0.008(2) C44 0.033(3) 0.056(4) 0.031(3) -0.005(3) 0.000(2) -0.012(3) C45 0.041(3) 0.060(4) 0.027(3) -0.005(3) -0.003(3) -0.013(3) C46 0.042(4) 0.071(5) 0.025(3) -0.008(3) -0.011(3) -0.015(3) C49 0.082(6) 0.054(5) 0.052(5) -0.015(4) 0.001(4) -0.026(4) C52 0.046(4) 0.045(4) 0.033(3) -0.006(3) 0.000(3) -0.007(3) C53 0.070(5) 0.048(4) 0.045(4) -0.002(3) 0.008(4) -0.006(4) C54 0.069(5) 0.063(5) 0.042(4) 0.002(4) 0.014(4) -0.006(4) C55 0.045(4) 0.070(5) 0.034(3) -0.008(3) 0.003(3) 0.004(3) C56 0.044(4) 0.049(4) 0.036(3) -0.013(3) -0.003(3) -0.005(3) C57 0.028(3) 0.045(3) 0.029(3) -0.007(2) -0.006(2) -0.008(2) C59 0.053(4) 0.043(4) 0.039(4) -0.010(3) -0.003(3) -0.006(3) C60 0.085(6) 0.042(4) 0.062(5) -0.011(4) 0.012(5) -0.004(4) C61 0.085(7) 0.049(5) 0.078(6) -0.023(4) 0.011(5) 0.008(4) C62 0.064(5) 0.061(5) 0.055(5) -0.025(4) 0.010(4) 0.000(4) C63 0.047(4) 0.054(4) 0.041(4) -0.020(3) 0.003(3) -0.009(3) C65 0.044(3) 0.038(3) 0.033(3) -0.006(2) 0.005(3) -0.016(3) C66 0.066(5) 0.047(4) 0.052(4) -0.013(3) 0.013(4) -0.021(4) C67 0.071(5) 0.041(4) 0.063(5) -0.012(4) 0.021(4) -0.009(4) C68 0.055(5) 0.051(4) 0.063(5) -0.003(4) 0.009(4) 0.006(4) C69 0.051(4) 0.054(4) 0.043(4) -0.007(3) -0.006(3) -0.001(3) C70 0.046(4) 0.045(3) 0.030(3) -0.007(3) -0.001(3) -0.019(3) C71 0.035(3) 0.050(4) 0.030(3) -0.008(3) -0.003(2) -0.010(3) C72 0.047(4) 0.054(4) 0.046(4) -0.017(3) -0.008(3) -0.003(3) C73 0.039(4) 0.077(5) 0.051(4) -0.014(4) -0.017(3) 0.002(4) C74 0.051(4) 0.077(6) 0.054(5) -0.017(4) -0.021(4) -0.017(4) C75 0.058(5) 0.058(4) 0.049(4) -0.017(3) -0.006(3) -0.021(4) C77 0.093(7) 0.036(4) 0.064(5) -0.018(3) 0.033(5) -0.016(4) C78 0.134(11) 0.059(6) 0.094(8) -0.047(6) 0.033(8) -0.028(6) C79 0.175(15) 0.078(7) 0.095(9) -0.062(7) 0.062(9) -0.061(9) C80 0.113(9) 0.105(9) 0.073(7) -0.042(6) 0.011(6) -0.064(8) C81 0.091(7) 0.070(6) 0.066(6) -0.032(5) 0.002(5) -0.035(5) C82 0.069(5) 0.034(4) 0.078(6) -0.006(4) 0.024(5) -0.001(3) C83 0.043(4) 0.026(3) 0.056(4) 0.003(3) 0.013(3) -0.003(3) C84 0.040(4) 0.040(4) 0.077(6) 0.010(4) -0.002(4) -0.001(3) C85 0.038(4) 0.054(5) 0.118(9) 0.016(5) 0.001(5) -0.002(4) C86 0.055(6) 0.064(6) 0.176(14) -0.006(8) 0.034(8) 0.019(5) C87 0.074(7) 0.059(6) 0.138(11) -0.029(6) 0.029(7) 0.014(5) O8 0.065(4) 0.104(6) 0.123(7) -0.040(5) -0.002(4) -0.042(4) O10 1.14(11) 0.28(3) 0.28(3) 0.15(3) 0.08(5) 0.11(5) _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 C57 2.018(6) . ? Ir1 C71 2.019(6) . ? Ir1 N5 2.043(5) . ? Ir1 N6 2.060(6) . ? Ir1 N8 2.142(5) . ? Ir1 N7 2.147(5) . ? Ir2 C83 2.014(7) . ? Ir2 C11 2.025(6) . ? Ir2 N1 2.049(6) . ? Ir2 N4 2.054(5) . ? Ir2 N3 2.141(5) . ? Ir2 N2 2.148(5) . ? Er3 O2 2.225(5) . ? Er3 O6 2.227(6) 1_455 ? Er3 O4 2.247(4) . ? Er3 O9 2.263(6) 2_575 ? Er3 O8 2.352(7) . ? Er3 O7 2.361(5) 1_655 ? Er3 O8 2.360(7) 2_575 ? O1 C46 1.229(9) . ? O2 C46 1.254(8) . ? O3 C28 1.216(8) . ? O4 C28 1.273(8) . ? O5 C49 1.253(12) . ? O6 C49 1.301(11) . ? O6 Er3 2.227(6) 1_655 ? O7 C31 1.233(10) . ? O7 Er3 2.361(5) 1_455 ? O9 C31 1.271(10) . ? O9 Er3 2.263(6) 2_575 ? N1 C81 1.325(12) . ? N1 C77 1.348(11) . ? N2 C23 1.346(7) . ? N2 C27 1.347(8) . ? N3 C21 1.336(8) . ? N3 C17 1.358(8) . ? N4 C9 1.347(9) . ? N4 C5 1.352(9) . ? N5 C63 1.347(9) . ? N5 C59 1.360(9) . ? N6 C69 1.349(9) . ? N6 C65 1.359(9) . ? N7 C45 1.326(9) . ? N7 C41 1.361(8) . ? N8 C39 1.344(9) . ? N8 C35 1.359(8) . ? C5 C6 1.404(12) . ? C5 C10 1.465(11) . ? C6 C7 1.365(14) . ? C7 C8 1.388(14) . ? C8 C9 1.373(11) . ? C10 C11 1.396(11) . ? C10 C15 1.398(10) . ? C11 C12 1.389(10) . ? C12 C13 1.385(11) . ? C13 C14 1.372(15) . ? C14 C15 1.381(14) . ? C17 C18 1.378(8) . ? C17 C23 1.474(9) . ? C18 C19 1.367(10) . ? C19 C20 1.388(10) . ? C19 C31 1.525(8) . ? C20 C21 1.389(9) . ? C23 C24 1.384(8) . ? C24 C25 1.386(9) . ? C25 C26 1.390(9) . ? C25 C28 1.531(8) . ? C26 C27 1.391(9) . ? C35 C36 1.393(9) . ? C35 C41 1.485(9) . ? C36 C37 1.392(11) . ? C37 C38 1.374(11) . ? C37 C49 1.545(11) . ? C38 C39 1.371(10) . ? C41 C42 1.383(9) . ? C42 C43 1.377(9) . ? C43 C44 1.393(9) . ? C43 C46 1.515(8) . ? C44 C45 1.369(9) . ? C52 C53 1.397(10) . ? C52 C57 1.411(10) . ? C52 C59 1.460(10) . ? C53 C54 1.376(12) . ? C54 C55 1.372(12) . ? C55 C56 1.392(10) . ? C56 C57 1.395(9) . ? C59 C60 1.396(11) . ? C60 C61 1.372(13) . ? C61 C62 1.371(13) . ? C62 C63 1.374(11) . ? C65 C66 1.392(10) . ? C65 C70 1.463(10) . ? C66 C67 1.363(13) . ? C67 C68 1.382(14) . ? C68 C69 1.381(12) . ? C70 C75 1.395(10) . ? C70 C71 1.410(10) . ? C71 C72 1.403(10) . ? C72 C73 1.385(10) . ? C73 C74 1.379(13) . ? C74 C75 1.369(12) . ? C77 C78 1.400(13) . ? C77 C82 1.451(15) . ? C78 C79 1.35(2) . ? C79 C80 1.363(19) . ? C80 C81 1.396(13) . ? C82 C83 1.397(12) . ? C82 C87 1.427(13) . ? C83 C84 1.404(12) . ? C84 C85 1.387(12) . ? C85 C86 1.383(19) . ? C86 C87 1.32(2) . ? O8 Er3 2.360(7) 2_575 ? 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 C57 Ir1 C71 87.4(2) . . ? C57 Ir1 N5 80.6(2) . . ? C71 Ir1 N5 92.6(3) . . ? C57 Ir1 N6 94.8(2) . . ? C71 Ir1 N6 80.1(3) . . ? N5 Ir1 N6 171.6(2) . . ? C57 Ir1 N8 171.8(2) . . ? C71 Ir1 N8 100.0(2) . . ? N5 Ir1 N8 95.5(2) . . ? N6 Ir1 N8 90.0(2) . . ? C57 Ir1 N7 95.8(2) . . ? C71 Ir1 N7 176.5(2) . . ? N5 Ir1 N7 89.4(2) . . ? N6 Ir1 N7 98.2(2) . . ? N8 Ir1 N7 76.9(2) . . ? C83 Ir2 C11 90.0(2) . . ? C83 Ir2 N1 80.6(3) . . ? C11 Ir2 N1 94.5(3) . . ? C83 Ir2 N4 93.1(3) . . ? C11 Ir2 N4 80.2(2) . . ? N1 Ir2 N4 171.8(2) . . ? C83 Ir2 N3 96.3(2) . . ? C11 Ir2 N3 171.6(2) . . ? N1 Ir2 N3 92.1(2) . . ? N4 Ir2 N3 93.8(2) . . ? C83 Ir2 N2 172.9(2) . . ? C11 Ir2 N2 96.8(2) . . ? N1 Ir2 N2 96.7(2) . . ? N4 Ir2 N2 90.2(2) . . ? N3 Ir2 N2 77.19(19) . . ? O2 Er3 O6 89.4(3) . 1_455 ? O2 Er3 O4 152.8(2) . . ? O6 Er3 O4 100.2(2) 1_455 . ? O2 Er3 O9 81.1(2) . 2_575 ? O6 Er3 O9 169.3(2) 1_455 2_575 ? O4 Er3 O9 86.31(17) . 2_575 ? O2 Er3 O8 72.6(3) . . ? O6 Er3 O8 80.4(3) 1_455 . ? O4 Er3 O8 133.8(3) . . ? O9 Er3 O8 101.3(3) 2_575 . ? O2 Er3 O7 80.2(2) . 1_655 ? O6 Er3 O7 82.2(2) 1_455 1_655 ? O4 Er3 O7 76.04(19) . 1_655 ? O9 Er3 O7 91.2(2) 2_575 1_655 ? O8 Er3 O7 147.7(2) . 1_655 ? O2 Er3 O8 132.5(3) . 2_575 ? O6 Er3 O8 88.9(3) 1_455 2_575 ? O4 Er3 O8 73.5(2) . 2_575 ? O9 Er3 O8 101.2(3) 2_575 2_575 ? O8 Er3 O8 60.3(4) . 2_575 ? O7 Er3 O8 146.2(2) 1_655 2_575 ? C46 O2 Er3 157.1(5) . . ? C28 O4 Er3 159.0(5) . . ? C49 O6 Er3 147.1(5) . 1_655 ? C31 O7 Er3 134.0(5) . 1_455 ? C31 O9 Er3 155.9(5) . 2_575 ? C81 N1 C77 120.1(8) . . ? C81 N1 Ir2 125.0(6) . . ? C77 N1 Ir2 114.6(6) . . ? C23 N2 C27 118.5(5) . . ? C23 N2 Ir2 114.6(4) . . ? C27 N2 Ir2 126.7(4) . . ? C21 N3 C17 119.1(5) . . ? C21 N3 Ir2 126.1(4) . . ? C17 N3 Ir2 114.2(4) . . ? C9 N4 C5 119.4(6) . . ? C9 N4 Ir2 125.0(5) . . ? C5 N4 Ir2 115.5(5) . . ? C63 N5 C59 119.6(6) . . ? C63 N5 Ir1 124.4(5) . . ? C59 N5 Ir1 115.6(4) . . ? C69 N6 C65 119.9(6) . . ? C69 N6 Ir1 124.3(5) . . ? C65 N6 Ir1 115.8(4) . . ? C45 N7 C41 118.8(5) . . ? C45 N7 Ir1 125.4(4) . . ? C41 N7 Ir1 115.6(4) . . ? C39 N8 C35 118.3(5) . . ? C39 N8 Ir1 126.0(4) . . ? C35 N8 Ir1 115.6(4) . . ? N4 C5 C6 119.5(7) . . ? N4 C5 C10 114.5(6) . . ? C6 C5 C10 126.0(7) . . ? C7 C6 C5 120.4(9) . . ? C6 C7 C8 119.6(9) . . ? C9 C8 C7 117.9(8) . . ? N4 C9 C8 123.1(7) . . ? C11 C10 C15 121.3(8) . . ? C11 C10 C5 115.5(6) . . ? C15 C10 C5 123.2(8) . . ? C12 C11 C10 117.6(6) . . ? C12 C11 Ir2 128.3(6) . . ? C10 C11 Ir2 114.1(5) . . ? C13 C12 C11 120.7(8) . . ? C14 C13 C12 121.4(8) . . ? C13 C14 C15 119.2(8) . . ? C14 C15 C10 119.7(9) . . ? N3 C17 C18 121.4(6) . . ? N3 C17 C23 116.3(5) . . ? C18 C17 C23 122.3(6) . . ? C19 C18 C17 120.0(6) . . ? C18 C19 C20 118.5(6) . . ? C18 C19 C31 119.7(6) . . ? C20 C19 C31 121.8(6) . . ? C19 C20 C21 119.5(6) . . ? N3 C21 C20 121.4(6) . . ? N2 C23 C24 121.7(6) . . ? N2 C23 C17 116.4(5) . . ? C24 C23 C17 121.9(5) . . ? C23 C24 C25 120.1(5) . . ? C24 C25 C26 118.3(5) . . ? C24 C25 C28 120.4(5) . . ? C26 C25 C28 121.3(6) . . ? C27 C26 C25 118.6(6) . . ? N2 C27 C26 122.7(6) . . ? O3 C28 O4 127.3(6) . . ? O3 C28 C25 117.9(6) . . ? O4 C28 C25 114.9(6) . . ? O7 C31 O9 126.6(6) . . ? O7 C31 C19 116.7(7) . . ? O9 C31 C19 116.7(6) . . ? N8 C35 C36 120.7(6) . . ? N8 C35 C41 116.1(5) . . ? C36 C35 C41 123.2(6) . . ? C37 C36 C35 119.9(6) . . ? C38 C37 C36 118.3(7) . . ? C38 C37 C49 120.2(7) . . ? C36 C37 C49 121.2(7) . . ? C39 C38 C37 119.3(7) . . ? N8 C39 C38 123.2(6) . . ? N7 C41 C42 120.8(6) . . ? N7 C41 C35 115.4(5) . . ? C42 C41 C35 123.7(5) . . ? C43 C42 C41 120.0(5) . . ? C42 C43 C44 118.3(6) . . ? C42 C43 C46 121.6(5) . . ? C44 C43 C46 120.1(6) . . ? C45 C44 C43 119.1(6) . . ? N7 C45 C44 122.9(6) . . ? O1 C46 O2 125.9(7) . . ? O1 C46 C43 118.8(6) . . ? O2 C46 C43 115.2(6) . . ? O5 C49 O6 130.0(9) . . ? O5 C49 C37 116.6(9) . . ? O6 C49 C37 113.4(8) . . ? C53 C52 C57 121.1(7) . . ? C53 C52 C59 123.7(7) . . ? C57 C52 C59 115.2(6) . . ? C54 C53 C52 119.4(8) . . ? C55 C54 C53 120.7(7) . . ? C54 C55 C56 120.4(7) . . ? C55 C56 C57 120.8(7) . . ? C56 C57 C52 117.6(6) . . ? C56 C57 Ir1 128.4(5) . . ? C52 C57 Ir1 113.9(5) . . ? N5 C59 C60 119.7(7) . . ? N5 C59 C52 114.4(6) . . ? C60 C59 C52 125.7(7) . . ? C61 C60 C59 119.7(8) . . ? C60 C61 C62 119.9(8) . . ? C63 C62 C61 118.8(8) . . ? N5 C63 C62 122.1(7) . . ? N6 C65 C66 119.5(7) . . ? N6 C65 C70 114.2(6) . . ? C66 C65 C70 126.3(7) . . ? C67 C66 C65 120.4(8) . . ? C66 C67 C68 119.8(8) . . ? C67 C68 C69 118.6(8) . . ? N6 C69 C68 121.8(8) . . ? C75 C70 C71 120.3(7) . . ? C75 C70 C65 124.2(7) . . ? C71 C70 C65 115.4(6) . . ? C72 C71 C70 117.8(6) . . ? C72 C71 Ir1 127.7(5) . . ? C70 C71 Ir1 114.5(5) . . ? C73 C72 C71 120.8(7) . . ? C72 C73 C74 120.3(7) . . ? C75 C74 C73 120.3(7) . . ? C74 C75 C70 120.4(8) . . ? N1 C77 C78 119.1(11) . . ? N1 C77 C82 115.3(7) . . ? C78 C77 C82 125.5(10) . . ? C79 C78 C77 120.5(12) . . ? C80 C79 C78 120.1(10) . . ? C79 C80 C81 118.0(12) . . ? N1 C81 C80 122.1(11) . . ? C83 C82 C87 119.1(11) . . ? C83 C82 C77 115.4(7) . . ? C87 C82 C77 125.5(10) . . ? C82 C83 C84 117.8(7) . . ? C82 C83 Ir2 113.8(6) . . ? C84 C83 Ir2 128.3(6) . . ? C85 C84 C83 121.1(10) . . ? C86 C85 C84 119.8(11) . . ? C87 C86 C85 120.5(9) . . ? C86 C87 C82 121.6(12) . . ? Er3 O8 Er3 119.7(4) . 2_575 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 73.18 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 5.783 _refine_diff_density_min -5.106 _refine_diff_density_rms 0.153 _database_code_depnum_ccdc_archive 'CCDC 971016' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Ir-Gd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H44 Gd Ir2 N8 O10' _chemical_formula_weight 1674.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 8.9631(3) _cell_length_b 15.2186(5) _cell_length_c 23.6351(8) _cell_angle_alpha 73.861(3) _cell_angle_beta 88.732(3) _cell_angle_gamma 82.398(3) _cell_volume 3069.32(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10618 _cell_measurement_theta_min 3.877 _cell_measurement_theta_max 72.912 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1594 _exptl_absorpt_coefficient_mu 15.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44742 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23162 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 73.22 _reflns_number_total 11925 _reflns_number_gt 10298 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0736P)^2^+3.6908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11925 _refine_ls_number_parameters 797 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 0.82710(3) 0.500708(16) 1.197247(11) 0.02558(8) Uani 1 1 d . . . Ir2 Ir -0.28641(3) 1.043343(18) 0.672348(11) 0.02741(8) Uani 1 1 d . . . Gd3 Gd 0.30271(5) 0.95388(3) 0.995791(16) 0.03129(11) Uani 1 1 d . . . O1 O -0.3399(9) 0.7514(5) 0.9545(3) 0.0700(19) Uani 1 1 d . . . O2 O -0.5616(7) 0.8387(4) 0.9610(3) 0.0485(14) Uani 1 1 d . . . O3 O 0.3385(7) 1.1103(5) 0.8285(2) 0.0544(16) Uani 1 1 d . . . O4 O 0.2162(7) 1.0239(5) 0.9008(2) 0.0518(15) Uani 1 1 d . . . O5 O 0.1244(7) 0.7878(4) 1.1650(3) 0.0537(15) Uani 1 1 d . . . O6 O 0.2504(6) 0.8681(3) 1.0902(2) 0.0422(12) Uani 1 1 d . . . O7 O 1.1043(6) 0.8685(3) 0.9848(2) 0.0406(12) Uani 1 1 d . . . O8 O 0.8632(6) 0.9256(3) 0.9870(2) 0.0372(11) Uani 1 1 d . . . O9 O 0.4929(7) 1.0390(4) 0.9463(3) 0.0567(15) Uani 1 1 d . . . N1 N -0.3561(7) 1.1738(4) 0.6787(2) 0.0326(12) Uani 1 1 d . . . N2 N -0.2308(7) 0.9190(4) 0.6545(2) 0.0316(11) Uani 1 1 d . . . N3 N 0.8042(7) 0.4157(4) 1.1443(3) 0.0356(13) Uani 1 1 d . . . N4 N -0.3542(6) 0.9737(4) 0.7595(2) 0.0264(10) Uani 1 1 d . . . N5 N -0.0947(6) 1.0372(4) 0.7271(2) 0.0318(11) Uani 1 1 d . . . N6 N 0.6155(6) 0.5872(4) 1.1728(3) 0.0316(12) Uani 1 1 d . . . N7 N 0.8659(6) 0.5672(4) 1.2595(3) 0.0327(12) Uani 1 1 d . . . N8 N 0.8839(6) 0.6091(4) 1.1249(2) 0.0287(11) Uani 1 1 d . . . C5 C -0.2548(8) 0.9663(4) 0.8039(3) 0.0309(13) Uani 1 1 d . . . C6 C -0.2835(8) 0.9207(5) 0.8607(3) 0.0368(15) Uani 1 1 d . . . H6 H -0.2146 0.9159 0.8906 0.044 Uiso 1 1 calc R . . C7 C -0.4179(9) 0.8807(6) 0.8740(3) 0.0400(16) Uani 1 1 d . . . C8 C -0.5187(8) 0.8911(5) 0.8292(3) 0.0369(15) Uani 1 1 d . . . H8 H -0.6103 0.8680 0.8370 0.044 Uiso 1 1 calc R . . C9 C -0.4830(9) 0.9360(5) 0.7725(3) 0.0369(15) Uani 1 1 d . . . H9 H -0.5502 0.9406 0.7421 0.044 Uiso 1 1 calc R . . C11 C -0.1156(7) 1.0075(4) 0.7859(3) 0.0271(12) Uani 1 1 d . . . C12 C -0.0082(8) 1.0144(5) 0.8257(3) 0.0329(14) Uani 1 1 d . . . H12 H -0.0232 0.9929 0.8660 0.039 Uiso 1 1 calc R . . C13 C 0.1208(8) 1.0535(4) 0.8051(3) 0.0304(13) Uani 1 1 d . . . C14 C 0.1433(8) 1.0803(5) 0.7451(3) 0.0345(14) Uani 1 1 d . . . H14 H 0.2310 1.1040 0.7302 0.041 Uiso 1 1 calc R . . C15 C 0.0319(7) 1.0712(5) 0.7070(3) 0.0342(14) Uani 1 1 d . . . H15 H 0.0470 1.0894 0.6666 0.041 Uiso 1 1 calc R . . C16 C 0.2363(8) 1.0649(5) 0.8478(3) 0.0352(15) Uani 1 1 d . . . C19 C -0.4389(10) 0.8180(5) 0.9359(3) 0.0434(17) Uani 1 1 d . . . C23 C 0.7741(7) 0.6828(4) 1.1078(3) 0.0279(12) Uani 1 1 d . . . C24 C 0.8017(7) 0.7637(4) 1.0676(3) 0.0293(13) Uani 1 1 d . . . H24 H 0.7251 0.8130 1.0568 0.035 Uiso 1 1 calc R . . C25 C 0.9411(7) 0.7720(4) 1.0436(3) 0.0290(13) Uani 1 1 d . . . C26 C 1.0529(8) 0.6967(5) 1.0586(3) 0.0326(13) Uani 1 1 d . . . H26 H 1.1468 0.6993 1.0411 0.039 Uiso 1 1 calc R . . C27 C 1.0211(8) 0.6172(4) 1.1004(3) 0.0322(13) Uani 1 1 d . . . H27 H 1.0971 0.5677 1.1120 0.039 Uiso 1 1 calc R . . C29 C 0.6253(7) 0.6699(4) 1.1336(3) 0.0280(12) Uani 1 1 d . . . C30 C 0.5023(8) 0.7362(4) 1.1190(3) 0.0319(13) Uani 1 1 d . . . H30 H 0.5114 0.7918 1.0910 0.038 Uiso 1 1 calc R . . C31 C 0.3656(8) 0.7216(4) 1.1453(3) 0.0297(13) Uani 1 1 d . . . C32 C 0.3533(7) 0.6361(5) 1.1845(3) 0.0333(14) Uani 1 1 d . . . H32 H 0.2617 0.6225 1.2016 0.040 Uiso 1 1 calc R . . C33 C 0.4820(8) 0.5708(4) 1.1976(3) 0.0323(14) Uani 1 1 d . . . H33 H 0.4749 0.5140 1.2245 0.039 Uiso 1 1 calc R . . C34 C 0.2332(8) 0.7983(4) 1.1329(3) 0.0323(13) Uani 1 1 d . . . C37 C 0.9724(8) 0.8631(4) 1.0019(3) 0.0322(14) Uani 1 1 d . . . C40 C 0.8305(9) 0.5255(5) 1.3150(3) 0.0418(16) Uani 1 1 d . . . C41 C 0.8600(14) 0.5625(7) 1.3610(4) 0.065(3) Uani 1 1 d . . . H41 H 0.8322 0.5346 1.3993 0.078 Uiso 1 1 calc R . . C42 C 0.9304(15) 0.6403(8) 1.3491(4) 0.072(3) Uani 1 1 d . . . H42 H 0.9526 0.6649 1.3793 0.086 Uiso 1 1 calc R . . C43 C 0.9681(12) 0.6820(6) 1.2914(4) 0.057(2) Uani 1 1 d . . . H43 H 1.0171 0.7342 1.2826 0.068 Uiso 1 1 calc R . . C44 C 0.9324(9) 0.6453(5) 1.2482(3) 0.0402(16) Uani 1 1 d . . . H44 H 0.9543 0.6746 1.2094 0.048 Uiso 1 1 calc R . . C46 C 0.7626(8) 0.4407(5) 1.3213(3) 0.0383(16) Uani 1 1 d . . . C47 C 0.7550(7) 0.4126(4) 1.2697(3) 0.0338(14) Uani 1 1 d . . . C48 C 0.6991(9) 0.3297(5) 1.2741(4) 0.0438(18) Uani 1 1 d . . . H48 H 0.6948 0.3087 1.2408 0.053 Uiso 1 1 calc R . . C49 C 0.6498(10) 0.2781(6) 1.3279(4) 0.055(2) Uani 1 1 d . . . H49 H 0.6134 0.2228 1.3302 0.066 Uiso 1 1 calc R . . C50 C 0.6542(11) 0.3079(7) 1.3775(4) 0.064(3) Uani 1 1 d . . . H50 H 0.6196 0.2730 1.4129 0.077 Uiso 1 1 calc R . . C51 C 0.7099(11) 0.3898(7) 1.3750(4) 0.054(2) Uani 1 1 d . . . H51 H 0.7122 0.4105 1.4085 0.065 Uiso 1 1 calc R . . C52 C -0.2259(8) 1.2136(5) 0.5890(3) 0.0358(14) Uani 1 1 d . . . C53 C -0.2049(7) 1.1169(5) 0.5966(3) 0.0305(13) Uani 1 1 d . . . C54 C -0.1260(8) 1.0857(5) 0.5526(3) 0.0373(15) Uani 1 1 d . . . H54 H -0.1095 1.0227 0.5563 0.045 Uiso 1 1 calc R . . C55 C -0.0722(9) 1.1458(6) 0.5042(3) 0.0459(18) Uani 1 1 d . . . H55 H -0.0230 1.1233 0.4750 0.055 Uiso 1 1 calc R . . C56 C -0.0909(10) 1.2400(6) 0.4986(3) 0.050(2) Uani 1 1 d . . . H56 H -0.0515 1.2801 0.4663 0.060 Uiso 1 1 calc R . . C57 C -0.1670(10) 1.2735(6) 0.5403(4) 0.050(2) Uani 1 1 d . . . H57 H -0.1798 1.3365 0.5363 0.060 Uiso 1 1 calc R . . C59 C -0.3177(9) 1.2448(5) 0.6337(3) 0.0369(15) Uani 1 1 d . . . C60 C -0.3677(12) 1.3345(6) 0.6326(4) 0.053(2) Uani 1 1 d . . . H60 H -0.3361 1.3827 0.6032 0.063 Uiso 1 1 calc R . . C61 C -0.4648(12) 1.3533(6) 0.6752(4) 0.057(2) Uani 1 1 d . . . H61 H -0.5009 1.4140 0.6738 0.069 Uiso 1 1 calc R . . C62 C -0.5080(10) 1.2818(6) 0.7197(4) 0.052(2) Uani 1 1 d . . . H62 H -0.5735 1.2933 0.7487 0.062 Uiso 1 1 calc R . . C63 C -0.4516(9) 1.1926(5) 0.7202(3) 0.0385(15) Uani 1 1 d . . . H63 H -0.4802 1.1438 0.7500 0.046 Uiso 1 1 calc R . . C65 C 0.9313(11) 0.3554(5) 1.1429(4) 0.0487(19) Uani 1 1 d . . . C66 C 0.9243(14) 0.2893(7) 1.1131(5) 0.068(3) Uani 1 1 d . . . H66 H 1.0096 0.2483 1.1111 0.082 Uiso 1 1 calc R . . C67 C 0.7925(15) 0.2841(8) 1.0866(5) 0.076(3) Uani 1 1 d . . . H67 H 0.7878 0.2392 1.0671 0.091 Uiso 1 1 calc R . . C68 C 0.6663(14) 0.3464(7) 1.0890(5) 0.066(3) Uani 1 1 d . . . H68 H 0.5759 0.3445 1.0711 0.079 Uiso 1 1 calc R . . C69 C 0.6792(11) 0.4109(7) 1.1186(4) 0.055(2) Uani 1 1 d . . . H69 H 0.5953 0.4529 1.1206 0.066 Uiso 1 1 calc R . . C70 C 1.0599(9) 0.3623(5) 1.1772(4) 0.048(2) Uani 1 1 d . . . C71 C 1.0332(8) 0.4264(4) 1.2102(3) 0.0329(14) Uani 1 1 d . . . C72 C 1.1499(9) 0.4307(5) 1.2470(4) 0.0446(18) Uani 1 1 d . . . H72 H 1.1346 0.4711 1.2704 0.054 Uiso 1 1 calc R . . C73 C 1.2881(9) 0.3762(6) 1.2498(5) 0.059(3) Uani 1 1 d . . . H73 H 1.3639 0.3809 1.2746 0.071 Uiso 1 1 calc R . . C74 C 1.3132(11) 0.3160(7) 1.2164(6) 0.076(4) Uani 1 1 d . . . H74 H 1.4058 0.2797 1.2182 0.091 Uiso 1 1 calc R . . C75 C 1.2021(12) 0.3095(6) 1.1804(6) 0.070(3) Uani 1 1 d . . . H75 H 1.2205 0.2691 1.1571 0.084 Uiso 1 1 calc R . . C77 C -0.3310(8) 0.8965(5) 0.6193(3) 0.0344(14) Uani 1 1 d . . . C78 C -0.2999(10) 0.8158(5) 0.6029(3) 0.0430(17) Uani 1 1 d . . . H78 H -0.3678 0.8013 0.5788 0.052 Uiso 1 1 calc R . . C79 C -0.1704(10) 0.7570(5) 0.6217(4) 0.051(2) Uani 1 1 d . . . H79 H -0.1513 0.7022 0.6111 0.061 Uiso 1 1 calc R . . C80 C -0.0683(10) 0.7797(6) 0.6565(4) 0.050(2) Uani 1 1 d . . . H80 H 0.0215 0.7415 0.6691 0.060 Uiso 1 1 calc R . . C81 C -0.1039(9) 0.8606(5) 0.6720(3) 0.0415(16) Uani 1 1 d . . . H81 H -0.0363 0.8757 0.6960 0.050 Uiso 1 1 calc R . . C82 C -0.4638(8) 0.9649(5) 0.6036(3) 0.0340(14) Uani 1 1 d . . . C83 C -0.4712(8) 1.0419(5) 0.6254(3) 0.0318(14) Uani 1 1 d . . . C84 C -0.5973(9) 1.1095(6) 0.6107(3) 0.0440(17) Uani 1 1 d . . . H84 H -0.6031 1.1618 0.6240 0.053 Uiso 1 1 calc R . . C85 C -0.7133(9) 1.0985(6) 0.5764(3) 0.0470(18) Uani 1 1 d . . . H85 H -0.7967 1.1436 0.5672 0.056 Uiso 1 1 calc R . . C86 C -0.7074(10) 1.0226(7) 0.5558(4) 0.054(2) Uani 1 1 d . . . H86 H -0.7870 1.0162 0.5333 0.065 Uiso 1 1 calc R . . C87 C -0.5837(10) 0.9552(6) 0.5682(4) 0.0471(18) Uani 1 1 d . . . H87 H -0.5789 0.9041 0.5536 0.057 Uiso 1 1 calc R . . O10 O -0.288(5) 0.573(3) 1.0004(17) 0.43(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02522(14) 0.01848(12) 0.02923(14) -0.00068(9) 0.00194(9) -0.00241(9) Ir2 0.02696(14) 0.03351(15) 0.02007(13) -0.00464(10) -0.00279(9) -0.00344(10) Gd3 0.0421(2) 0.02747(19) 0.02217(18) 0.00069(14) -0.00362(15) -0.01282(16) O1 0.072(5) 0.067(4) 0.054(4) 0.001(3) 0.001(3) 0.011(4) O2 0.056(3) 0.047(3) 0.049(3) -0.021(2) 0.027(3) -0.021(3) O3 0.049(3) 0.086(4) 0.033(3) -0.011(3) -0.002(2) -0.037(3) O4 0.047(3) 0.075(4) 0.024(2) 0.006(2) -0.009(2) -0.016(3) O5 0.045(3) 0.043(3) 0.058(3) 0.004(3) 0.016(3) 0.010(2) O6 0.042(3) 0.036(3) 0.036(3) 0.007(2) 0.005(2) 0.003(2) O7 0.034(3) 0.037(3) 0.048(3) -0.002(2) 0.002(2) -0.019(2) O8 0.044(3) 0.028(2) 0.032(2) 0.0040(18) -0.001(2) -0.004(2) O9 0.044(3) 0.058(4) 0.070(4) -0.016(3) -0.004(3) -0.017(3) N1 0.032(3) 0.041(3) 0.025(2) -0.010(2) 0.000(2) -0.006(2) N2 0.034(3) 0.031(3) 0.026(3) -0.002(2) 0.000(2) -0.005(2) N3 0.040(3) 0.027(3) 0.040(3) -0.010(2) 0.008(3) -0.009(2) N4 0.018(2) 0.031(3) 0.029(2) -0.003(2) -0.0019(19) -0.010(2) N5 0.030(3) 0.040(3) 0.025(3) -0.007(2) -0.007(2) -0.006(2) N6 0.026(3) 0.021(2) 0.041(3) 0.001(2) -0.003(2) 0.002(2) N7 0.024(3) 0.028(3) 0.044(3) -0.005(2) 0.004(2) -0.007(2) N8 0.030(3) 0.028(3) 0.022(2) 0.000(2) 0.000(2) 0.002(2) C5 0.034(3) 0.030(3) 0.028(3) -0.008(2) -0.001(3) 0.002(3) C6 0.027(3) 0.055(4) 0.028(3) -0.011(3) -0.001(3) -0.003(3) C7 0.040(4) 0.053(4) 0.024(3) -0.005(3) 0.004(3) -0.004(3) C8 0.028(3) 0.049(4) 0.034(3) -0.010(3) 0.004(3) -0.010(3) C9 0.040(4) 0.043(4) 0.028(3) -0.010(3) -0.002(3) -0.005(3) C11 0.023(3) 0.031(3) 0.025(3) -0.004(2) -0.001(2) -0.004(2) C12 0.041(4) 0.034(3) 0.021(3) -0.003(2) -0.002(3) -0.007(3) C13 0.030(3) 0.031(3) 0.028(3) -0.001(2) -0.003(2) -0.009(3) C14 0.027(3) 0.045(4) 0.029(3) -0.004(3) -0.002(3) -0.010(3) C15 0.025(3) 0.051(4) 0.026(3) -0.006(3) -0.001(2) -0.010(3) C16 0.035(4) 0.044(4) 0.023(3) -0.003(3) -0.007(3) -0.004(3) C19 0.048(4) 0.042(4) 0.040(4) -0.010(3) -0.001(3) -0.009(3) C23 0.026(3) 0.025(3) 0.029(3) -0.002(2) -0.004(2) -0.001(2) C24 0.026(3) 0.026(3) 0.030(3) 0.003(2) -0.003(2) -0.005(2) C25 0.030(3) 0.024(3) 0.029(3) 0.001(2) -0.004(2) -0.005(2) C26 0.031(3) 0.035(3) 0.028(3) -0.003(3) 0.004(2) -0.006(3) C27 0.030(3) 0.025(3) 0.034(3) 0.001(2) -0.003(3) 0.004(2) C29 0.027(3) 0.025(3) 0.027(3) 0.002(2) -0.002(2) -0.003(2) C30 0.037(4) 0.026(3) 0.026(3) 0.003(2) 0.000(3) 0.000(3) C31 0.032(3) 0.031(3) 0.023(3) -0.004(2) -0.001(2) -0.002(3) C32 0.022(3) 0.034(3) 0.037(3) 0.001(3) 0.004(2) -0.003(3) C33 0.028(3) 0.026(3) 0.037(3) 0.002(3) 0.005(3) -0.007(3) C34 0.034(3) 0.029(3) 0.029(3) -0.003(2) 0.002(3) 0.003(3) C37 0.048(4) 0.024(3) 0.023(3) 0.000(2) -0.001(3) -0.013(3) C40 0.040(4) 0.043(4) 0.035(4) -0.002(3) 0.001(3) -0.001(3) C41 0.100(8) 0.064(6) 0.033(4) -0.015(4) -0.003(4) -0.018(6) C42 0.102(9) 0.079(7) 0.052(5) -0.034(5) -0.002(5) -0.039(7) C43 0.065(6) 0.050(5) 0.063(5) -0.020(4) -0.003(4) -0.024(4) C44 0.047(4) 0.027(3) 0.044(4) -0.006(3) 0.000(3) -0.002(3) C46 0.035(4) 0.032(3) 0.038(4) 0.007(3) 0.004(3) -0.006(3) C47 0.022(3) 0.028(3) 0.039(3) 0.007(3) 0.005(3) 0.001(2) C48 0.042(4) 0.033(4) 0.046(4) 0.009(3) -0.005(3) -0.009(3) C49 0.052(5) 0.045(4) 0.055(5) 0.014(4) -0.008(4) -0.021(4) C50 0.058(6) 0.065(6) 0.049(5) 0.024(4) 0.012(4) -0.021(5) C51 0.063(6) 0.063(5) 0.032(4) -0.002(4) 0.003(4) -0.015(4) C52 0.036(4) 0.041(4) 0.025(3) -0.002(3) -0.002(3) 0.001(3) C53 0.023(3) 0.046(4) 0.021(3) -0.005(3) -0.002(2) -0.006(3) C54 0.035(4) 0.047(4) 0.030(3) -0.013(3) 0.006(3) -0.002(3) C55 0.043(4) 0.060(5) 0.031(3) -0.010(3) 0.008(3) 0.000(4) C56 0.054(5) 0.053(5) 0.030(4) 0.008(3) 0.012(3) -0.005(4) C57 0.054(5) 0.044(4) 0.042(4) 0.007(3) 0.009(4) -0.006(4) C59 0.045(4) 0.035(3) 0.030(3) -0.006(3) -0.003(3) -0.005(3) C60 0.071(6) 0.035(4) 0.048(4) -0.010(3) 0.008(4) -0.002(4) C61 0.076(6) 0.039(4) 0.053(5) -0.013(4) -0.001(4) 0.010(4) C62 0.055(5) 0.060(5) 0.045(4) -0.029(4) 0.010(4) 0.005(4) C63 0.041(4) 0.044(4) 0.034(3) -0.016(3) -0.001(3) -0.006(3) C65 0.062(5) 0.037(4) 0.052(5) -0.019(3) 0.015(4) -0.013(4) C66 0.084(8) 0.046(5) 0.087(7) -0.038(5) 0.019(6) -0.011(5) C67 0.105(9) 0.067(7) 0.079(7) -0.049(6) 0.020(7) -0.037(7) C68 0.077(7) 0.060(6) 0.069(6) -0.022(5) 0.000(5) -0.027(5) C69 0.060(6) 0.056(5) 0.055(5) -0.020(4) -0.001(4) -0.020(4) C70 0.033(4) 0.031(4) 0.073(5) -0.010(4) 0.012(4) 0.008(3) C71 0.031(3) 0.024(3) 0.037(3) 0.004(2) 0.001(3) -0.009(3) C72 0.034(4) 0.031(3) 0.062(5) -0.004(3) 0.010(3) -0.001(3) C73 0.030(4) 0.041(4) 0.086(7) 0.015(4) 0.000(4) 0.000(3) C74 0.038(5) 0.046(5) 0.134(11) -0.016(6) 0.020(6) 0.007(4) C75 0.056(6) 0.040(5) 0.116(9) -0.028(5) 0.010(6) -0.001(4) C77 0.039(4) 0.032(3) 0.033(3) -0.009(3) 0.005(3) -0.011(3) C78 0.053(5) 0.038(4) 0.039(4) -0.010(3) 0.006(3) -0.014(3) C79 0.057(5) 0.033(4) 0.060(5) -0.011(3) 0.021(4) -0.003(3) C80 0.045(5) 0.038(4) 0.057(5) -0.002(3) 0.005(4) 0.005(3) C81 0.035(4) 0.047(4) 0.039(4) -0.007(3) -0.008(3) 0.001(3) C82 0.034(4) 0.041(4) 0.025(3) -0.004(3) 0.000(3) -0.010(3) C83 0.029(3) 0.040(3) 0.027(3) -0.006(3) -0.004(2) -0.014(3) C84 0.043(4) 0.053(4) 0.038(4) -0.016(3) -0.001(3) -0.007(3) C85 0.041(4) 0.057(5) 0.039(4) -0.010(3) -0.015(3) 0.005(4) C86 0.046(5) 0.073(6) 0.045(4) -0.015(4) -0.017(4) -0.010(4) C87 0.044(4) 0.052(5) 0.049(4) -0.016(4) -0.007(3) -0.014(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 C47 2.013(6) . ? Ir1 C71 2.017(7) . ? Ir1 N7 2.063(6) . ? Ir1 N3 2.065(6) . ? Ir1 N8 2.127(5) . ? Ir1 N6 2.151(5) . ? Ir2 C53 2.009(6) . ? Ir2 C83 2.020(6) . ? Ir2 N1 2.047(6) . ? Ir2 N2 2.048(6) . ? Ir2 N5 2.150(5) . ? Ir2 N4 2.153(5) . ? Gd3 O4 2.303(5) . ? Gd3 O8 2.325(5) 2_677 ? Gd3 O6 2.324(5) . ? Gd3 O2 2.330(6) 1_655 ? Gd3 O9 2.343(6) 2_677 ? Gd3 O9 2.367(6) . ? Gd3 O7 2.396(5) 1_455 ? Gd3 Gd3 4.0022(8) 2_677 ? O1 C19 1.241(11) . ? O2 C19 1.281(10) . ? O2 Gd3 2.330(6) 1_455 ? O3 C16 1.223(9) . ? O4 C16 1.257(8) . ? O5 C34 1.222(9) . ? O6 C34 1.269(8) . ? O7 C37 1.247(9) . ? O7 Gd3 2.396(5) 1_655 ? O8 C37 1.252(9) . ? O8 Gd3 2.325(5) 2_677 ? O9 Gd3 2.343(6) 2_677 ? N1 C63 1.352(9) . ? N1 C59 1.363(9) . ? N2 C81 1.343(10) . ? N2 C77 1.374(9) . ? N3 C69 1.306(11) . ? N3 C65 1.371(11) . ? N4 C9 1.349(9) . ? N4 C5 1.363(8) . ? N5 C15 1.332(8) . ? N5 C11 1.354(8) . ? N6 C33 1.343(8) . ? N6 C29 1.353(8) . ? N7 C40 1.340(9) . ? N7 C44 1.357(9) . ? N8 C27 1.353(9) . ? N8 C23 1.365(8) . ? C5 C6 1.366(9) . ? C5 C11 1.472(9) . ? C6 C7 1.411(10) . ? C7 C8 1.368(10) . ? C7 C19 1.532(10) . ? C8 C9 1.377(10) . ? C11 C12 1.395(9) . ? C12 C13 1.387(9) . ? C13 C14 1.380(9) . ? C13 C16 1.520(9) . ? C14 C15 1.405(9) . ? C23 C24 1.379(8) . ? C23 C29 1.468(9) . ? C24 C25 1.367(9) . ? C25 C26 1.389(10) . ? C25 C37 1.517(8) . ? C26 C27 1.391(9) . ? C29 C30 1.371(9) . ? C30 C31 1.378(9) . ? C31 C32 1.388(9) . ? C31 C34 1.522(9) . ? C32 C33 1.398(10) . ? C40 C41 1.402(12) . ? C40 C46 1.468(11) . ? C41 C42 1.372(14) . ? C42 C43 1.389(14) . ? C43 C44 1.356(12) . ? C46 C51 1.400(10) . ? C46 C47 1.404(11) . ? C47 C48 1.396(10) . ? C48 C49 1.394(11) . ? C49 C50 1.371(15) . ? C50 C51 1.390(14) . ? C52 C57 1.397(10) . ? C52 C53 1.420(10) . ? C52 C59 1.469(10) . ? C53 C54 1.399(9) . ? C54 C55 1.376(10) . ? C55 C56 1.390(13) . ? C56 C57 1.362(13) . ? C59 C60 1.372(11) . ? C60 C61 1.381(13) . ? C61 C62 1.377(13) . ? C62 C63 1.383(11) . ? C65 C66 1.388(12) . ? C65 C70 1.454(13) . ? C66 C67 1.371(18) . ? C67 C68 1.387(17) . ? C68 C69 1.373(13) . ? C70 C71 1.403(11) . ? C70 C75 1.406(13) . ? C71 C72 1.396(11) . ? C72 C73 1.388(11) . ? C73 C74 1.362(17) . ? C74 C75 1.354(18) . ? C77 C78 1.379(11) . ? C77 C82 1.454(11) . ? C78 C79 1.368(13) . ? C79 C80 1.382(14) . ? C80 C81 1.376(12) . ? C82 C83 1.398(10) . ? C82 C87 1.423(10) . ? C83 C84 1.402(11) . ? C84 C85 1.388(11) . ? C85 C86 1.367(13) . ? C86 C87 1.383(13) . ? 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 C47 Ir1 C71 89.6(3) . . ? C47 Ir1 N7 80.0(3) . . ? C71 Ir1 N7 92.4(3) . . ? C47 Ir1 N3 93.8(3) . . ? C71 Ir1 N3 81.0(3) . . ? N7 Ir1 N3 171.0(2) . . ? C47 Ir1 N8 171.6(2) . . ? C71 Ir1 N8 96.8(2) . . ? N7 Ir1 N8 94.3(2) . . ? N3 Ir1 N8 92.5(2) . . ? C47 Ir1 N6 97.0(2) . . ? C71 Ir1 N6 173.1(2) . . ? N7 Ir1 N6 90.8(2) . . ? N3 Ir1 N6 96.4(2) . . ? N8 Ir1 N6 76.8(2) . . ? C53 Ir2 C83 86.9(3) . . ? C53 Ir2 N1 80.4(3) . . ? C83 Ir2 N1 93.0(3) . . ? C53 Ir2 N2 94.5(3) . . ? C83 Ir2 N2 80.4(3) . . ? N1 Ir2 N2 171.9(2) . . ? C53 Ir2 N5 96.9(2) . . ? C83 Ir2 N5 176.0(2) . . ? N1 Ir2 N5 88.8(2) . . ? N2 Ir2 N5 98.1(2) . . ? C53 Ir2 N4 172.1(2) . . ? C83 Ir2 N4 100.2(2) . . ? N1 Ir2 N4 95.6(2) . . ? N2 Ir2 N4 90.2(2) . . ? N5 Ir2 N4 76.1(2) . . ? O4 Gd3 O8 81.0(2) . 2_677 ? O4 Gd3 O6 147.4(2) . . ? O8 Gd3 O6 87.19(17) 2_677 . ? O4 Gd3 O2 87.9(2) . 1_655 ? O8 Gd3 O2 168.0(2) 2_677 1_655 ? O6 Gd3 O2 100.01(19) . 1_655 ? O4 Gd3 O9 136.4(2) . 2_677 ? O8 Gd3 O9 99.1(2) 2_677 2_677 ? O6 Gd3 O9 75.3(2) . 2_677 ? O2 Gd3 O9 92.0(2) 1_655 2_677 ? O4 Gd3 O9 73.2(2) . . ? O8 Gd3 O9 99.1(2) 2_677 . ? O6 Gd3 O9 139.0(2) . . ? O2 Gd3 O9 81.7(2) 1_655 . ? O9 Gd3 O9 63.7(3) 2_677 . ? O4 Gd3 O7 76.52(19) . 1_455 ? O8 Gd3 O7 93.16(19) 2_677 1_455 ? O6 Gd3 O7 73.91(19) . 1_455 ? O2 Gd3 O7 79.9(2) 1_655 1_455 ? O9 Gd3 O7 146.2(2) 2_677 1_455 ? O9 Gd3 O7 144.9(2) . 1_455 ? O4 Gd3 Gd3 104.68(14) . 2_677 ? O8 Gd3 Gd3 100.77(13) 2_677 2_677 ? O6 Gd3 Gd3 107.36(15) . 2_677 ? O2 Gd3 Gd3 86.28(14) 1_655 2_677 ? O9 Gd3 Gd3 32.01(16) 2_677 2_677 ? O9 Gd3 Gd3 31.65(16) . 2_677 ? O7 Gd3 Gd3 166.05(14) 1_455 2_677 ? C19 O2 Gd3 143.4(5) . 1_455 ? C16 O4 Gd3 151.9(5) . . ? C34 O6 Gd3 159.3(5) . . ? C37 O7 Gd3 136.8(5) . 1_655 ? C37 O8 Gd3 151.7(5) . 2_677 ? Gd3 O9 Gd3 116.3(3) 2_677 . ? C63 N1 C59 119.2(6) . . ? C63 N1 Ir2 123.7(5) . . ? C59 N1 Ir2 116.6(5) . . ? C81 N2 C77 118.2(6) . . ? C81 N2 Ir2 125.8(5) . . ? C77 N2 Ir2 115.9(5) . . ? C69 N3 C65 121.1(7) . . ? C69 N3 Ir1 125.2(6) . . ? C65 N3 Ir1 113.4(5) . . ? C9 N4 C5 118.9(5) . . ? C9 N4 Ir2 125.3(4) . . ? C5 N4 Ir2 115.8(4) . . ? C15 N5 C11 119.5(5) . . ? C15 N5 Ir2 124.1(4) . . ? C11 N5 Ir2 115.8(4) . . ? C33 N6 C29 118.5(6) . . ? C33 N6 Ir1 126.1(4) . . ? C29 N6 Ir1 114.9(4) . . ? C40 N7 C44 119.5(7) . . ? C40 N7 Ir1 116.0(5) . . ? C44 N7 Ir1 124.3(5) . . ? C27 N8 C23 118.0(5) . . ? C27 N8 Ir1 126.6(4) . . ? C23 N8 Ir1 114.7(4) . . ? N4 C5 C6 120.9(6) . . ? N4 C5 C11 115.6(5) . . ? C6 C5 C11 123.4(6) . . ? C5 C6 C7 119.8(7) . . ? C8 C7 C6 118.6(6) . . ? C8 C7 C19 121.6(7) . . ? C6 C7 C19 119.4(7) . . ? C7 C8 C9 119.3(7) . . ? N4 C9 C8 122.4(7) . . ? N5 C11 C12 120.9(6) . . ? N5 C11 C5 115.6(6) . . ? C12 C11 C5 123.5(6) . . ? C13 C12 C11 119.9(6) . . ? C14 C13 C12 118.6(6) . . ? C14 C13 C16 120.7(6) . . ? C12 C13 C16 120.7(6) . . ? C13 C14 C15 119.0(6) . . ? N5 C15 C14 122.0(6) . . ? O3 C16 O4 126.4(7) . . ? O3 C16 C13 119.2(6) . . ? O4 C16 C13 114.4(6) . . ? O1 C19 O2 127.9(8) . . ? O1 C19 C7 116.7(8) . . ? O2 C19 C7 115.3(7) . . ? N8 C23 C24 121.4(6) . . ? N8 C23 C29 116.2(5) . . ? C24 C23 C29 122.3(6) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 119.1(6) . . ? C24 C25 C37 119.9(6) . . ? C26 C25 C37 121.0(6) . . ? C25 C26 C27 118.5(6) . . ? N8 C27 C26 122.5(6) . . ? N6 C29 C30 121.3(6) . . ? N6 C29 C23 115.7(6) . . ? C30 C29 C23 123.1(5) . . ? C29 C30 C31 121.0(6) . . ? C30 C31 C32 118.2(6) . . ? C30 C31 C34 120.7(6) . . ? C32 C31 C34 121.1(6) . . ? C31 C32 C33 118.4(6) . . ? N6 C33 C32 122.5(6) . . ? O5 C34 O6 126.9(7) . . ? O5 C34 C31 117.9(6) . . ? O6 C34 C31 115.2(6) . . ? O7 C37 O8 125.8(6) . . ? O7 C37 C25 116.9(6) . . ? O8 C37 C25 117.2(6) . . ? N7 C40 C41 120.5(7) . . ? N7 C40 C46 113.9(7) . . ? C41 C40 C46 125.6(7) . . ? C42 C41 C40 119.3(8) . . ? C41 C42 C43 119.4(8) . . ? C44 C43 C42 119.0(8) . . ? C43 C44 N7 122.3(7) . . ? C51 C46 C47 121.6(7) . . ? C51 C46 C40 122.8(8) . . ? C47 C46 C40 115.7(6) . . ? C48 C47 C46 117.9(6) . . ? C48 C47 Ir1 127.9(6) . . ? C46 C47 Ir1 114.2(5) . . ? C49 C48 C47 120.4(9) . . ? C50 C49 C48 120.9(8) . . ? C49 C50 C51 120.4(7) . . ? C50 C51 C46 118.8(9) . . ? C57 C52 C53 120.8(7) . . ? C57 C52 C59 123.6(7) . . ? C53 C52 C59 115.5(6) . . ? C54 C53 C52 116.8(6) . . ? C54 C53 Ir2 129.1(6) . . ? C52 C53 Ir2 114.0(5) . . ? C55 C54 C53 121.6(7) . . ? C54 C55 C56 120.4(7) . . ? C57 C56 C55 120.0(7) . . ? C56 C57 C52 120.4(8) . . ? N1 C59 C60 120.4(7) . . ? N1 C59 C52 113.1(6) . . ? C60 C59 C52 126.5(7) . . ? C59 C60 C61 120.1(8) . . ? C62 C61 C60 119.9(8) . . ? C63 C62 C61 118.2(8) . . ? N1 C63 C62 122.2(7) . . ? N3 C65 C66 118.3(9) . . ? N3 C65 C70 116.2(7) . . ? C66 C65 C70 125.4(9) . . ? C65 C66 C67 120.4(11) . . ? C68 C67 C66 119.5(9) . . ? C69 C68 C67 117.8(10) . . ? N3 C69 C68 122.9(10) . . ? C71 C70 C75 119.5(9) . . ? C71 C70 C65 115.0(7) . . ? C75 C70 C65 125.5(9) . . ? C72 C71 C70 117.1(7) . . ? C72 C71 Ir1 128.6(6) . . ? C70 C71 Ir1 114.3(5) . . ? C73 C72 C71 121.8(9) . . ? C74 C73 C72 120.3(10) . . ? C73 C74 C75 119.5(9) . . ? C74 C75 C70 121.8(10) . . ? N2 C77 C78 120.0(7) . . ? N2 C77 C82 112.8(6) . . ? C78 C77 C82 127.2(7) . . ? C79 C78 C77 120.8(8) . . ? C78 C79 C80 119.5(8) . . ? C81 C80 C79 117.8(8) . . ? N2 C81 C80 123.7(8) . . ? C83 C82 C87 120.2(7) . . ? C83 C82 C77 117.2(6) . . ? C87 C82 C77 122.6(7) . . ? C82 C83 C84 118.6(6) . . ? C82 C83 Ir2 113.5(5) . . ? C84 C83 Ir2 127.8(5) . . ? C85 C84 C83 120.2(8) . . ? C86 C85 C84 121.2(8) . . ? C85 C86 C87 120.4(8) . . ? C86 C87 C82 119.3(8) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 73.22 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 3.580 _refine_diff_density_min -3.819 _refine_diff_density_rms 0.157 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.006 0.500 0.500 249 42 ' ' 2 0.000 0.500 0.000 20 5 ' ' 3 0.202 0.877 0.736 23 1 ' ' 4 0.391 0.581 0.055 22 5 ' ' 5 0.609 0.419 0.945 22 5 ' ' 6 0.798 0.123 0.264 23 1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 971017' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Ir-Yb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H44 Ir2 N8 O10 Yb' _chemical_formula_weight 1690.6 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -7.2108 4.4329 '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 8.9717(3) _cell_length_b 15.1215(4) _cell_length_c 23.7174(6) _cell_angle_alpha 73.467(2) _cell_angle_beta 88.039(3) _cell_angle_gamma 81.392(3) _cell_volume 3049.73(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10496 _cell_measurement_theta_min 3.133 _cell_measurement_theta_max 72.914 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1582 _exptl_absorpt_coefficient_mu 11.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58412 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23295 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 73.38 _reflns_number_total 11812 _reflns_number_gt 10120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1417P)^2^+61.1198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11812 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2397 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.002 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 0.66524(5) 1.00251(3) 0.301912(18) 0.01482(16) Uani 1 1 d . . . Ir2 Ir -0.20330(5) 0.45495(3) 0.828306(19) 0.01947(16) Uani 1 1 d . . . Yb3 Yb 0.20173(15) 0.54303(7) 0.50891(5) 0.0711(4) Uani 1 1 d . . . O1 O 0.3907(11) 0.6296(5) 0.5131(4) 0.032(2) Uani 1 1 d . . . O2 O 0.6358(10) 0.5731(5) 0.5113(3) 0.0269(18) Uani 1 1 d . . . O3 O 1.2320(10) 0.6229(6) 0.4148(4) 0.0310(19) Uani 1 1 d . . . O4 O 1.3766(9) 0.7048(6) 0.3444(5) 0.036(2) Uani 1 1 d . . . O5 O 0.0697(11) 0.6616(6) 0.5371(4) 0.032(2) Uani 1 1 d . . . O6 O -0.1582(12) 0.7411(6) 0.5440(4) 0.038(2) Uani 1 1 d . . . O7 O -0.7040(11) 0.4775(7) 0.6009(4) 0.035(2) Uani 1 1 d . . . O9 O -0.8195(13) 0.3856(7) 0.6754(5) 0.044(2) Uani 1 1 d . . . O8 O 0.145(3) 0.981(2) 0.4312(11) 0.158(13) Uani 1 1 d . . . N1 N -0.3943(10) 0.4622(6) 0.7744(4) 0.0194(18) Uani 1 1 d . . . N2 N -0.1355(11) 0.3229(7) 0.8218(4) 0.0216(19) Uani 1 1 d . . . N3 N -0.1360(11) 0.5240(6) 0.7408(4) 0.0207(19) Uani 1 1 d . . . N4 N -0.2604(11) 0.5808(6) 0.8464(4) 0.0220(19) Uani 1 1 d . . . N5 N 0.6829(10) 1.0887(6) 0.3539(4) 0.0182(18) Uani 1 1 d . . . N6 N 0.6301(10) 0.9334(6) 0.2417(4) 0.0190(18) Uani 1 1 d . . . N7 N 0.6074(10) 0.8936(6) 0.3749(4) 0.0203(19) Uani 1 1 d . . . N8 N 0.8770(10) 0.9145(6) 0.3257(4) 0.0165(17) Uani 1 1 d . . . C5 C 0.7201(12) 0.8194(7) 0.3933(5) 0.021(2) Uani 1 1 d . . . C6 C 0.6925(12) 0.7386(8) 0.4334(5) 0.023(2) Uani 1 1 d . . . H6 H 0.7704 0.6890 0.4450 0.028 Uiso 1 1 calc R . . C7 C 0.5515(13) 0.7297(7) 0.4568(5) 0.018(2) Uani 1 1 d . . . C8 C 0.4380(12) 0.8063(8) 0.4405(5) 0.020(2) Uani 1 1 d . . . H8 H 0.3421 0.8031 0.4563 0.024 Uiso 1 1 calc R . . C9 C 0.4710(13) 0.8872(7) 0.4001(5) 0.020(2) Uani 1 1 d . . . H9 H 0.3963 0.9389 0.3901 0.024 Uiso 1 1 calc R . . C11 C 0.8682(13) 0.8322(8) 0.3672(5) 0.023(2) Uani 1 1 d . . . C12 C 0.9927(14) 0.7626(9) 0.3829(6) 0.033(3) Uani 1 1 d . . . H12 H 0.9825 0.7063 0.4107 0.040 Uiso 1 1 calc R . . C13 C 1.1277(13) 0.7767(8) 0.3580(5) 0.024(2) Uani 1 1 d . . . C14 C 1.1422(12) 0.8623(8) 0.3177(5) 0.022(2) Uani 1 1 d . . . H14 H 1.2350 0.8746 0.3011 0.026 Uiso 1 1 calc R . . C15 C 1.0157(12) 0.9281(7) 0.3031(5) 0.019(2) Uani 1 1 d . . . H15 H 1.0257 0.9852 0.2762 0.023 Uiso 1 1 calc R . . C16 C 1.2598(13) 0.6976(8) 0.3724(5) 0.023(2) Uani 1 1 d . . . C19 C 0.5237(14) 0.6373(7) 0.4972(5) 0.022(2) Uani 1 1 d . . . C23 C -0.1589(13) 0.6003(8) 0.8823(5) 0.024(2) Uani 1 1 d . . . C24 C -0.1902(13) 0.6837(8) 0.8983(5) 0.025(2) Uani 1 1 d . . . H24 H -0.1215 0.6985 0.9214 0.030 Uiso 1 1 calc R . . C25 C -0.3220(15) 0.7438(8) 0.8800(6) 0.030(3) Uani 1 1 d . . . H25 H -0.3439 0.7982 0.8915 0.036 Uiso 1 1 calc R . . C26 C -0.4217(14) 0.7220(8) 0.8440(5) 0.027(2) Uani 1 1 d . . . H26 H -0.5097 0.7625 0.8302 0.032 Uiso 1 1 calc R . . C27 C -0.3881(13) 0.6393(8) 0.8292(5) 0.023(2) Uani 1 1 d . . . H27 H -0.4568 0.6238 0.8064 0.027 Uiso 1 1 calc R . . C28 C -0.0253(13) 0.5314(8) 0.8974(5) 0.023(2) Uani 1 1 d . . . C29 C -0.0190(13) 0.4542(8) 0.8753(5) 0.023(2) Uani 1 1 d . . . C30 C 0.1084(14) 0.3857(9) 0.8897(6) 0.028(3) Uani 1 1 d . . . H30 H 0.1139 0.3328 0.8767 0.034 Uiso 1 1 calc R . . C31 C 0.2251(14) 0.3948(8) 0.9225(6) 0.028(3) Uani 1 1 d . . . H31 H 0.3097 0.3493 0.9302 0.034 Uiso 1 1 calc R . . C32 C 0.2184(15) 0.4711(10) 0.9445(6) 0.032(3) Uani 1 1 d . . . H32 H 0.2969 0.4767 0.9673 0.038 Uiso 1 1 calc R . . C33 C 0.0932(14) 0.5384(8) 0.9318(5) 0.028(2) Uani 1 1 d . . . H33 H 0.0873 0.5897 0.9464 0.034 Uiso 1 1 calc R . . C34 C 0.7297(14) 1.0621(8) 0.1776(5) 0.026(2) Uani 1 1 d . . . C35 C 0.7834(16) 1.1147(10) 0.1237(6) 0.036(3) Uani 1 1 d . . . H35 H 0.7801 1.0942 0.0904 0.044 Uiso 1 1 calc R . . C36 C 0.8382(15) 1.1923(10) 0.1197(6) 0.038(3) Uani 1 1 d . . . H36 H 0.8736 1.2258 0.0839 0.046 Uiso 1 1 calc R . . C37 C 0.8435(15) 1.2252(9) 0.1703(6) 0.035(3) Uani 1 1 d . . . H37 H 0.8799 1.2809 0.1670 0.043 Uiso 1 1 calc R . . C38 C 0.7948(13) 1.1747(8) 0.2240(6) 0.025(2) Uani 1 1 d . . . H38 H 0.8001 1.1960 0.2569 0.030 Uiso 1 1 calc R . . C39 C 0.7365(12) 1.0904(7) 0.2293(5) 0.021(2) Uani 1 1 d . . . C41 C 0.6648(14) 0.9772(8) 0.1849(5) 0.027(2) Uani 1 1 d . . . C42 C 0.633(2) 0.9403(10) 0.1393(6) 0.043(3) Uani 1 1 d . . . H42 H 0.6595 0.9686 0.1008 0.052 Uiso 1 1 calc R . . C43 C 0.561(2) 0.8588(11) 0.1528(7) 0.047(4) Uani 1 1 d . . . H43 H 0.5385 0.8337 0.1231 0.056 Uiso 1 1 calc R . . C44 C 0.5261(16) 0.8189(9) 0.2092(7) 0.037(3) Uani 1 1 d . . . H44 H 0.4768 0.7668 0.2184 0.044 Uiso 1 1 calc R . . C45 C 0.5634(13) 0.8553(7) 0.2534(6) 0.023(2) Uani 1 1 d . . . H45 H 0.5421 0.8254 0.2922 0.027 Uiso 1 1 calc R . . C47 C -0.2336(13) 0.5314(7) 0.6983(5) 0.021(2) Uani 1 1 d . . . C48 C -0.2071(15) 0.5781(7) 0.6395(5) 0.025(2) Uani 1 1 d . . . H48 H -0.2765 0.5827 0.6102 0.030 Uiso 1 1 calc R . . C49 C -0.0727(14) 0.6180(7) 0.6256(5) 0.023(2) Uani 1 1 d . . . C50 C 0.0273(14) 0.6069(8) 0.6703(5) 0.026(2) Uani 1 1 d . . . H50 H 0.1179 0.6307 0.6622 0.031 Uiso 1 1 calc R . . C51 C -0.0058(14) 0.5606(8) 0.7274(5) 0.026(2) Uani 1 1 d . . . H51 H 0.0628 0.5544 0.7573 0.031 Uiso 1 1 calc R . . C53 C -0.3723(13) 0.4917(7) 0.7158(5) 0.023(2) Uani 1 1 d . . . C54 C -0.4785(14) 0.4833(8) 0.6762(5) 0.024(2) Uani 1 1 d . . . H54 H -0.4614 0.5028 0.6360 0.028 Uiso 1 1 calc R . . C55 C -0.6086(13) 0.4462(7) 0.6968(5) 0.023(2) Uani 1 1 d . . . C56 C -0.6315(13) 0.4201(8) 0.7576(6) 0.027(2) Uani 1 1 d . . . H56 H -0.7198 0.3975 0.7728 0.032 Uiso 1 1 calc R . . C57 C -0.5241(13) 0.4278(8) 0.7948(5) 0.025(2) Uani 1 1 d . . . H57 H -0.5400 0.4090 0.8351 0.030 Uiso 1 1 calc R . . C58 C -0.7200(16) 0.4326(9) 0.6552(6) 0.032(3) Uani 1 1 d . . . C61 C -0.0562(15) 0.6796(8) 0.5636(5) 0.027(3) Uani 1 1 d . . . C65 C -0.1813(14) 0.2534(8) 0.8656(5) 0.025(2) Uani 1 1 d . . . C66 C -0.1332(15) 0.1600(9) 0.8667(6) 0.031(3) Uani 1 1 d . . . H66 H -0.1673 0.1119 0.8958 0.038 Uiso 1 1 calc R . . C67 C -0.0349(16) 0.1400(9) 0.8242(6) 0.033(3) Uani 1 1 d . . . H67 H -0.0028 0.0784 0.8246 0.039 Uiso 1 1 calc R . . C68 C 0.0147(15) 0.2116(9) 0.7816(6) 0.030(3) Uani 1 1 d . . . H68 H 0.0834 0.1991 0.7536 0.036 Uiso 1 1 calc R . . C69 C -0.0391(13) 0.3031(9) 0.7808(5) 0.025(2) Uani 1 1 d . . . H69 H -0.0078 0.3517 0.7513 0.030 Uiso 1 1 calc R . . C70 C -0.2728(13) 0.2845(8) 0.9110(5) 0.024(2) Uani 1 1 d . . . C71 C -0.2878(13) 0.3821(8) 0.9040(5) 0.022(2) Uani 1 1 d . . . C72 C -0.3623(12) 0.4146(9) 0.9485(5) 0.023(2) Uani 1 1 d . . . H72 H -0.3727 0.4778 0.9458 0.028 Uiso 1 1 calc R . . C73 C -0.4217(15) 0.3535(10) 0.9972(5) 0.031(3) Uani 1 1 d . . . H73 H -0.4684 0.3763 1.0269 0.038 Uiso 1 1 calc R . . C74 C -0.4113(15) 0.2602(10) 1.0013(6) 0.034(3) Uani 1 1 d . . . H74 H -0.4543 0.2206 1.0330 0.040 Uiso 1 1 calc R . . C75 C -0.3361(15) 0.2247(10) 0.9580(6) 0.034(3) Uani 1 1 d . . . H75 H -0.3286 0.1616 0.9607 0.041 Uiso 1 1 calc R . . C76 C 0.4278(14) 1.1423(8) 0.3220(6) 0.030(3) Uani 1 1 d . . . C77 C 0.2861(16) 1.1953(9) 0.3203(7) 0.040(3) Uani 1 1 d . . . H77 H 0.2670 1.2362 0.3433 0.048 Uiso 1 1 calc R . . C78 C 0.1730(15) 1.1869(9) 0.2842(8) 0.043(4) Uani 1 1 d . . . H78 H 0.0784 1.2223 0.2831 0.052 Uiso 1 1 calc R . . C79 C 0.2011(14) 1.1267(8) 0.2504(6) 0.032(3) Uani 1 1 d . . . H79 H 0.1258 1.1223 0.2257 0.038 Uiso 1 1 calc R . . C80 C 0.3412(12) 1.0719(8) 0.2525(6) 0.024(2) Uani 1 1 d . . . H80 H 0.3577 1.0312 0.2292 0.028 Uiso 1 1 calc R . . C81 C 0.4568(13) 1.0766(7) 0.2885(5) 0.023(2) Uani 1 1 d . . . C83 C 0.5541(15) 1.1510(8) 0.3557(6) 0.028(3) Uani 1 1 d . . . C84 C 0.5590(18) 1.2164(10) 0.3856(7) 0.039(3) Uani 1 1 d . . . H84 H 0.4728 1.2577 0.3880 0.047 Uiso 1 1 calc R . . C85 C 0.6935(18) 1.2210(10) 0.4123(6) 0.038(3) Uani 1 1 d . . . H85 H 0.6970 1.2648 0.4328 0.046 Uiso 1 1 calc R . . C86 C 0.8197(19) 1.1599(9) 0.4080(6) 0.038(3) Uani 1 1 d . . . H86 H 0.9117 1.1625 0.4239 0.046 Uiso 1 1 calc R . . C87 C 0.8045(15) 1.0935(8) 0.3787(5) 0.024(2) Uani 1 1 d . . . H87 H 0.8885 1.0500 0.3771 0.029 Uiso 1 1 calc R . . O11 O 0.0169(14) 0.4644(11) 0.5516(10) 0.108(8) 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 0.0135(2) 0.0073(2) 0.0197(2) 0.00209(16) 0.00225(16) -0.00118(16) Ir2 0.0191(3) 0.0168(3) 0.0182(3) -0.00024(18) 0.00554(18) 0.00054(18) Yb3 0.0978(9) 0.0406(5) 0.0727(7) -0.0144(5) 0.0431(6) -0.0160(5) O1 0.042(5) 0.012(4) 0.041(5) -0.003(3) 0.026(4) -0.011(3) O2 0.043(5) 0.011(4) 0.021(4) 0.002(3) 0.013(3) -0.002(3) O3 0.032(5) 0.022(4) 0.031(4) 0.001(3) -0.008(4) 0.005(4) O4 0.013(4) 0.026(4) 0.068(7) -0.016(4) -0.003(4) 0.003(3) O5 0.051(6) 0.017(4) 0.028(4) -0.004(3) 0.024(4) -0.011(4) O6 0.043(6) 0.025(5) 0.033(5) 0.008(4) 0.003(4) 0.002(4) O7 0.042(5) 0.034(5) 0.030(5) -0.010(4) 0.000(4) -0.004(4) O9 0.061(7) 0.040(6) 0.040(5) -0.019(5) 0.010(5) -0.025(5) O8 0.105(16) 0.24(3) 0.119(17) -0.10(2) -0.030(13) 0.099(19) N1 0.015(4) 0.016(4) 0.021(4) 0.001(3) 0.004(3) 0.004(3) N2 0.019(5) 0.020(5) 0.023(5) -0.002(4) 0.000(4) -0.002(4) N3 0.022(5) 0.018(4) 0.019(4) -0.004(4) 0.012(4) 0.003(4) N4 0.028(5) 0.018(4) 0.018(4) -0.002(4) 0.009(4) -0.003(4) N5 0.017(4) 0.008(4) 0.025(5) -0.001(3) 0.008(3) 0.002(3) N6 0.017(4) 0.013(4) 0.025(5) -0.003(4) 0.002(4) -0.003(3) N7 0.016(4) 0.013(4) 0.026(5) 0.005(4) 0.002(4) -0.005(3) N8 0.011(4) 0.012(4) 0.023(4) 0.001(3) -0.004(3) -0.001(3) C5 0.016(5) 0.015(5) 0.025(5) 0.005(4) -0.001(4) -0.003(4) C6 0.013(5) 0.026(6) 0.024(5) 0.004(4) -0.003(4) -0.002(4) C7 0.028(6) 0.007(4) 0.018(5) 0.000(4) 0.006(4) -0.005(4) C8 0.017(5) 0.018(5) 0.025(5) -0.006(4) 0.006(4) -0.004(4) C9 0.019(5) 0.013(5) 0.025(5) -0.001(4) 0.002(4) 0.000(4) C11 0.017(5) 0.015(5) 0.027(6) 0.009(4) 0.004(4) 0.002(4) C12 0.024(6) 0.019(6) 0.045(7) 0.012(5) 0.002(5) -0.007(5) C13 0.018(5) 0.016(5) 0.032(6) 0.002(4) -0.001(4) -0.003(4) C14 0.016(5) 0.025(6) 0.027(6) -0.011(5) 0.004(4) -0.007(4) C15 0.018(5) 0.006(4) 0.030(6) 0.000(4) 0.004(4) -0.003(4) C16 0.022(6) 0.016(5) 0.028(6) 0.000(4) -0.009(4) 0.000(4) C19 0.037(7) 0.009(5) 0.019(5) -0.003(4) 0.008(5) -0.005(4) C23 0.023(6) 0.026(6) 0.021(5) -0.004(4) 0.009(4) -0.010(5) C24 0.021(6) 0.022(6) 0.029(6) -0.001(5) 0.009(5) -0.007(4) C25 0.036(7) 0.014(5) 0.036(7) -0.002(5) 0.014(5) -0.005(5) C26 0.024(6) 0.018(5) 0.033(6) 0.000(5) 0.006(5) 0.000(4) C27 0.023(6) 0.020(5) 0.017(5) 0.004(4) 0.007(4) 0.004(4) C28 0.024(6) 0.018(5) 0.021(5) 0.003(4) 0.007(4) -0.005(4) C29 0.020(5) 0.020(5) 0.022(5) 0.006(4) 0.006(4) -0.002(4) C30 0.024(6) 0.024(6) 0.033(6) -0.007(5) -0.001(5) 0.006(5) C31 0.023(6) 0.022(6) 0.032(6) -0.001(5) 0.004(5) 0.006(5) C32 0.028(6) 0.036(7) 0.031(6) -0.008(5) 0.000(5) -0.008(5) C33 0.031(6) 0.022(6) 0.027(6) 0.000(5) 0.007(5) -0.007(5) C34 0.029(6) 0.018(5) 0.023(5) 0.006(4) -0.002(5) 0.002(5) C35 0.034(7) 0.041(8) 0.024(6) 0.005(5) 0.001(5) -0.002(6) C36 0.026(6) 0.042(8) 0.031(7) 0.016(6) 0.012(5) -0.011(6) C37 0.027(6) 0.023(6) 0.045(8) 0.013(5) -0.009(6) -0.010(5) C38 0.021(6) 0.012(5) 0.032(6) 0.012(4) -0.003(5) -0.005(4) C39 0.012(5) 0.011(5) 0.034(6) 0.005(4) -0.001(4) 0.001(4) C41 0.031(6) 0.024(6) 0.023(6) -0.002(5) 0.002(5) -0.002(5) C42 0.069(11) 0.031(7) 0.028(7) -0.003(6) -0.003(7) -0.011(7) C43 0.065(11) 0.043(8) 0.039(8) -0.023(7) -0.001(7) -0.008(7) C44 0.038(7) 0.018(6) 0.054(8) -0.010(6) -0.008(6) -0.001(5) C45 0.022(5) 0.010(5) 0.037(6) -0.008(4) 0.001(5) -0.003(4) C47 0.028(6) 0.011(5) 0.022(5) -0.004(4) 0.010(4) 0.002(4) C48 0.037(7) 0.011(5) 0.025(6) -0.005(4) 0.007(5) 0.000(4) C49 0.028(6) 0.011(5) 0.026(6) -0.005(4) 0.011(5) 0.002(4) C50 0.025(6) 0.022(6) 0.029(6) -0.006(5) 0.016(5) -0.004(5) C51 0.027(6) 0.021(6) 0.027(6) -0.005(5) 0.007(5) 0.000(5) C53 0.025(6) 0.009(5) 0.027(6) 0.000(4) 0.012(4) 0.006(4) C54 0.033(6) 0.018(5) 0.020(5) -0.006(4) 0.006(4) 0.000(4) C55 0.026(6) 0.011(5) 0.029(6) -0.004(4) 0.004(5) 0.008(4) C56 0.017(5) 0.025(6) 0.036(6) -0.008(5) 0.010(5) 0.002(4) C57 0.024(6) 0.023(6) 0.027(6) -0.005(5) 0.005(5) -0.001(4) C58 0.038(7) 0.029(6) 0.035(7) -0.021(5) 0.010(5) -0.004(5) C61 0.045(7) 0.017(5) 0.023(6) -0.006(4) 0.010(5) -0.014(5) C65 0.025(6) 0.020(5) 0.027(6) -0.003(4) -0.003(5) -0.001(4) C66 0.034(7) 0.021(6) 0.035(7) -0.001(5) 0.002(5) -0.004(5) C67 0.039(7) 0.018(6) 0.038(7) -0.007(5) 0.004(6) 0.001(5) C68 0.031(6) 0.025(6) 0.038(7) -0.017(5) -0.003(5) 0.005(5) C69 0.022(6) 0.026(6) 0.026(6) -0.006(5) 0.003(4) -0.001(5) C70 0.023(6) 0.016(5) 0.024(6) 0.007(4) 0.003(4) -0.001(4) C71 0.016(5) 0.024(6) 0.025(5) -0.007(5) 0.000(4) 0.002(4) C72 0.014(5) 0.031(6) 0.021(5) -0.004(5) 0.005(4) -0.002(4) C73 0.030(6) 0.044(7) 0.016(5) -0.004(5) 0.006(5) -0.002(5) C74 0.029(7) 0.038(7) 0.026(6) 0.004(5) 0.005(5) -0.006(5) C75 0.030(7) 0.030(7) 0.033(7) 0.005(5) 0.004(5) -0.003(5) C76 0.026(6) 0.014(5) 0.046(7) -0.003(5) 0.015(5) -0.007(4) C77 0.036(8) 0.016(6) 0.066(10) -0.012(6) 0.016(7) -0.003(5) C78 0.016(6) 0.021(6) 0.084(12) -0.002(7) 0.013(6) -0.004(5) C79 0.018(6) 0.014(5) 0.054(8) 0.007(5) 0.002(5) -0.005(4) C80 0.010(5) 0.013(5) 0.041(7) 0.005(4) -0.001(4) -0.003(4) C81 0.019(5) 0.009(5) 0.034(6) 0.002(4) 0.010(4) -0.007(4) C83 0.031(6) 0.018(5) 0.035(6) -0.004(5) 0.011(5) -0.010(5) C84 0.044(8) 0.028(7) 0.049(8) -0.015(6) 0.019(7) -0.008(6) C85 0.059(9) 0.030(7) 0.031(7) -0.017(6) 0.015(6) -0.010(6) C86 0.061(10) 0.027(7) 0.030(7) -0.007(5) 0.002(6) -0.016(6) C87 0.037(7) 0.013(5) 0.023(5) -0.007(4) 0.001(5) -0.002(5) O11 0.037(7) 0.095(11) 0.25(2) -0.137(15) 0.056(10) -0.041(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 C39 2.004(11) . ? Ir1 C81 2.016(11) . ? Ir1 N6 2.052(9) . ? Ir1 N5 2.058(9) . ? Ir1 N7 2.133(9) . ? Ir1 N8 2.142(8) . ? Ir2 C71 2.010(12) . ? Ir2 C29 2.022(12) . ? Ir2 N2 2.047(10) . ? Ir2 N4 2.057(9) . ? Ir2 N1 2.144(9) . ? Ir2 N3 2.151(9) . ? Yb3 O11 2.232(14) . ? Yb3 O3 2.245(9) 1_455 ? Yb3 O5 2.248(8) . ? Yb3 O2 2.259(8) 2_666 ? Yb3 O7 2.259(9) 1_655 ? Yb3 O1 2.313(9) . ? Yb3 O11 2.503(17) 2_566 ? Yb3 Yb3 4.099(3) 2_566 ? O1 C19 1.252(15) . ? O2 C19 1.269(15) . ? O2 Yb3 2.259(8) 2_666 ? O3 C16 1.331(15) . ? O3 Yb3 2.245(9) 1_655 ? O4 C16 1.223(16) . ? O5 C61 1.305(16) . ? O6 C61 1.202(16) . ? O7 C58 1.287(16) . ? O7 Yb3 2.259(9) 1_455 ? O9 C58 1.225(17) . ? N1 C53 1.350(15) . ? N1 C57 1.364(15) . ? N2 C69 1.347(15) . ? N2 C65 1.353(15) . ? N3 C47 1.327(16) . ? N3 C51 1.358(16) . ? N4 C27 1.336(15) . ? N4 C23 1.383(16) . ? N5 C87 1.278(16) . ? N5 C83 1.385(15) . ? N6 C45 1.357(14) . ? N6 C41 1.368(15) . ? N7 C9 1.348(15) . ? N7 C5 1.373(14) . ? N8 C15 1.359(14) . ? N8 C11 1.361(13) . ? C5 C6 1.367(15) . ? C5 C11 1.463(15) . ? C6 C7 1.374(16) . ? C7 C8 1.395(15) . ? C7 C19 1.503(13) . ? C8 C9 1.387(15) . ? C11 C12 1.396(17) . ? C12 C13 1.348(17) . ? C13 C14 1.395(16) . ? C13 C16 1.524(15) . ? C14 C15 1.375(16) . ? C23 C24 1.404(17) . ? C23 C28 1.447(17) . ? C24 C25 1.379(18) . ? C25 C26 1.393(19) . ? C26 C27 1.381(17) . ? C28 C33 1.397(18) . ? C28 C29 1.402(17) . ? C29 C30 1.402(16) . ? C30 C31 1.372(19) . ? C31 C32 1.388(19) . ? C32 C33 1.377(19) . ? C34 C35 1.413(17) . ? C34 C39 1.414(18) . ? C34 C41 1.452(17) . ? C35 C36 1.32(2) . ? C36 C37 1.43(2) . ? C37 C38 1.380(18) . ? C38 C39 1.420(15) . ? C41 C42 1.404(19) . ? C42 C43 1.43(2) . ? C43 C44 1.35(2) . ? C44 C45 1.389(18) . ? C47 C48 1.404(16) . ? C47 C53 1.458(17) . ? C48 C49 1.416(18) . ? C49 C50 1.371(18) . ? C49 C61 1.516(15) . ? C50 C51 1.379(17) . ? C53 C54 1.404(18) . ? C54 C55 1.385(17) . ? C55 C56 1.399(17) . ? C55 C58 1.504(18) . ? C56 C57 1.367(18) . ? C65 C66 1.407(17) . ? C65 C70 1.472(17) . ? C66 C67 1.384(19) . ? C67 C68 1.372(19) . ? C68 C69 1.391(17) . ? C70 C75 1.385(17) . ? C70 C71 1.424(16) . ? C71 C72 1.397(16) . ? C72 C73 1.403(17) . ? C73 C74 1.38(2) . ? C74 C75 1.40(2) . ? C76 C77 1.392(19) . ? C76 C81 1.431(17) . ? C76 C83 1.451(19) . ? C77 C78 1.39(2) . ? C78 C79 1.37(2) . ? C79 C80 1.393(16) . ? C80 C81 1.389(17) . ? C83 C84 1.377(19) . ? C84 C85 1.40(2) . ? C85 C86 1.37(2) . ? C86 C87 1.398(17) . ? O11 Yb3 2.503(17) 2_566 ? 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 C39 Ir1 C81 89.8(4) . . ? C39 Ir1 N6 80.7(4) . . ? C81 Ir1 N6 92.1(4) . . ? C39 Ir1 N5 94.0(4) . . ? C81 Ir1 N5 81.3(4) . . ? N6 Ir1 N5 171.6(4) . . ? C39 Ir1 N7 171.9(4) . . ? C81 Ir1 N7 96.1(4) . . ? N6 Ir1 N7 93.5(4) . . ? N5 Ir1 N7 92.4(4) . . ? C39 Ir1 N8 96.8(4) . . ? C81 Ir1 N8 173.3(4) . . ? N6 Ir1 N8 89.7(4) . . ? N5 Ir1 N8 97.5(3) . . ? N7 Ir1 N8 77.4(3) . . ? C71 Ir2 C29 87.1(4) . . ? C71 Ir2 N2 80.8(4) . . ? C29 Ir2 N2 93.6(4) . . ? C71 Ir2 N4 93.8(4) . . ? C29 Ir2 N4 80.4(4) . . ? N2 Ir2 N4 172.2(4) . . ? C71 Ir2 N1 96.1(4) . . ? C29 Ir2 N1 176.6(4) . . ? N2 Ir2 N1 87.9(4) . . ? N4 Ir2 N1 98.4(4) . . ? C71 Ir2 N3 171.3(4) . . ? C29 Ir2 N3 101.0(4) . . ? N2 Ir2 N3 95.1(4) . . ? N4 Ir2 N3 91.0(3) . . ? N1 Ir2 N3 75.9(4) . . ? O11 Yb3 O3 130.5(6) . 1_455 ? O11 Yb3 O5 84.4(4) . . ? O3 Yb3 O5 96.9(3) 1_455 . ? O11 Yb3 O2 100.3(4) . 2_666 ? O3 Yb3 O2 85.8(3) 1_455 2_666 ? O5 Yb3 O2 171.1(4) . 2_666 ? O11 Yb3 O7 79.0(6) . 1_655 ? O3 Yb3 O7 150.0(4) 1_455 1_655 ? O5 Yb3 O7 90.7(3) . 1_655 ? O2 Yb3 O7 82.9(3) 2_666 1_655 ? O11 Yb3 O1 150.6(5) . . ? O3 Yb3 O1 76.1(3) 1_455 . ? O5 Yb3 O1 79.3(3) . . ? O2 Yb3 O1 93.1(3) 2_666 . ? O7 Yb3 O1 76.9(4) 1_655 . ? O11 Yb3 O11 60.2(10) . 2_566 ? O3 Yb3 O11 70.3(5) 1_455 2_566 ? O5 Yb3 O11 90.8(4) . 2_566 ? O2 Yb3 O11 98.1(4) 2_666 2_566 ? O7 Yb3 O11 138.8(5) 1_655 2_566 ? O1 Yb3 O11 143.5(5) . 2_566 ? O11 Yb3 Yb3 32.0(6) . 2_566 ? O3 Yb3 Yb3 98.5(2) 1_455 2_566 ? O5 Yb3 Yb3 87.5(3) . 2_566 ? O2 Yb3 Yb3 100.6(2) 2_666 2_566 ? O7 Yb3 Yb3 110.8(3) 1_655 2_566 ? O1 Yb3 Yb3 164.9(2) . 2_566 ? O11 Yb3 Yb3 28.2(5) 2_566 2_566 ? C19 O1 Yb3 140.9(7) . . ? C19 O2 Yb3 150.7(8) . 2_666 ? C16 O3 Yb3 153.7(8) . 1_655 ? C61 O5 Yb3 139.1(7) . . ? C58 O7 Yb3 150.7(9) . 1_455 ? C53 N1 C57 119.2(10) . . ? C53 N1 Ir2 115.4(8) . . ? C57 N1 Ir2 124.7(8) . . ? C69 N2 C65 120.4(10) . . ? C69 N2 Ir2 123.7(8) . . ? C65 N2 Ir2 115.6(8) . . ? C47 N3 C51 119.7(10) . . ? C47 N3 Ir2 115.5(7) . . ? C51 N3 Ir2 124.8(8) . . ? C27 N4 C23 120.1(10) . . ? C27 N4 Ir2 125.0(8) . . ? C23 N4 Ir2 114.8(8) . . ? C87 N5 C83 120.1(10) . . ? C87 N5 Ir1 124.8(8) . . ? C83 N5 Ir1 114.7(8) . . ? C45 N6 C41 119.8(10) . . ? C45 N6 Ir1 125.0(8) . . ? C41 N6 Ir1 114.9(8) . . ? C9 N7 C5 118.3(9) . . ? C9 N7 Ir1 126.9(7) . . ? C5 N7 Ir1 114.5(7) . . ? C15 N8 C11 116.5(9) . . ? C15 N8 Ir1 128.8(7) . . ? C11 N8 Ir1 114.6(7) . . ? C6 C5 N7 121.0(10) . . ? C6 C5 C11 123.0(10) . . ? N7 C5 C11 116.0(9) . . ? C5 C6 C7 121.0(10) . . ? C6 C7 C8 118.5(10) . . ? C6 C7 C19 119.0(10) . . ? C8 C7 C19 122.5(10) . . ? C9 C8 C7 118.7(10) . . ? N7 C9 C8 122.3(10) . . ? N8 C11 C12 121.9(10) . . ? N8 C11 C5 116.5(9) . . ? C12 C11 C5 121.6(10) . . ? C13 C12 C11 120.1(11) . . ? C12 C13 C14 119.3(11) . . ? C12 C13 C16 119.5(10) . . ? C14 C13 C16 121.1(10) . . ? C15 C14 C13 118.2(10) . . ? N8 C15 C14 123.8(10) . . ? O4 C16 O3 125.6(11) . . ? O4 C16 C13 120.3(10) . . ? O3 C16 C13 114.1(10) . . ? O1 C19 O2 125.4(10) . . ? O1 C19 C7 116.9(10) . . ? O2 C19 C7 117.6(10) . . ? N4 C23 C24 118.9(11) . . ? N4 C23 C28 114.3(10) . . ? C24 C23 C28 126.8(11) . . ? C25 C24 C23 120.6(12) . . ? C24 C25 C26 119.0(11) . . ? C27 C26 C25 119.1(11) . . ? N4 C27 C26 122.3(12) . . ? C33 C28 C29 120.1(11) . . ? C33 C28 C23 123.7(11) . . ? C29 C28 C23 116.2(11) . . ? C30 C29 C28 117.5(11) . . ? C30 C29 Ir2 128.3(10) . . ? C28 C29 Ir2 114.2(8) . . ? C31 C30 C29 121.6(12) . . ? C30 C31 C32 120.8(11) . . ? C33 C32 C31 118.5(12) . . ? C32 C33 C28 121.5(12) . . ? C35 C34 C39 120.7(12) . . ? C35 C34 C41 124.1(12) . . ? C39 C34 C41 115.2(10) . . ? C36 C35 C34 121.1(14) . . ? C35 C36 C37 120.3(12) . . ? C38 C37 C36 120.2(12) . . ? C37 C38 C39 120.4(13) . . ? C34 C39 C38 117.2(11) . . ? C34 C39 Ir1 114.4(8) . . ? C38 C39 Ir1 128.3(10) . . ? N6 C41 C42 119.9(12) . . ? N6 C41 C34 114.6(10) . . ? C42 C41 C34 125.4(12) . . ? C41 C42 C43 119.2(13) . . ? C44 C43 C42 119.0(13) . . ? C43 C44 C45 120.3(13) . . ? N6 C45 C44 121.8(12) . . ? N3 C47 C48 121.6(11) . . ? N3 C47 C53 117.0(10) . . ? C48 C47 C53 121.4(11) . . ? C47 C48 C49 118.7(12) . . ? C50 C49 C48 118.0(11) . . ? C50 C49 C61 123.7(11) . . ? C48 C49 C61 117.9(11) . . ? C49 C50 C51 120.4(11) . . ? N3 C51 C50 121.5(12) . . ? N1 C53 C54 120.5(11) . . ? N1 C53 C47 115.2(11) . . ? C54 C53 C47 124.2(10) . . ? C55 C54 C53 120.3(10) . . ? C54 C55 C56 117.9(11) . . ? C54 C55 C58 120.9(11) . . ? C56 C55 C58 121.2(11) . . ? C57 C56 C55 120.0(11) . . ? N1 C57 C56 122.0(11) . . ? O9 C58 O7 126.6(13) . . ? O9 C58 C55 118.6(12) . . ? O7 C58 C55 114.6(12) . . ? O6 C61 O5 126.4(11) . . ? O6 C61 C49 117.3(11) . . ? O5 C61 C49 116.3(11) . . ? N2 C65 C66 119.6(11) . . ? N2 C65 C70 114.8(10) . . ? C66 C65 C70 125.5(11) . . ? C67 C66 C65 119.7(12) . . ? C68 C67 C66 119.6(11) . . ? C67 C68 C69 119.1(12) . . ? N2 C69 C68 121.5(11) . . ? C75 C70 C71 121.9(12) . . ? C75 C70 C65 123.7(11) . . ? C71 C70 C65 114.4(10) . . ? C72 C71 C70 117.0(11) . . ? C72 C71 Ir2 129.0(9) . . ? C70 C71 Ir2 114.0(8) . . ? C71 C72 C73 121.1(12) . . ? C74 C73 C72 120.5(12) . . ? C73 C74 C75 120.1(12) . . ? C70 C75 C74 119.3(13) . . ? C77 C76 C81 120.4(13) . . ? C77 C76 C83 123.4(12) . . ? C81 C76 C83 116.1(11) . . ? C78 C77 C76 120.1(13) . . ? C79 C78 C77 120.0(12) . . ? C78 C79 C80 120.7(13) . . ? C79 C80 C81 121.4(12) . . ? C80 C81 C76 117.3(11) . . ? C80 C81 Ir1 129.4(9) . . ? C76 C81 Ir1 113.3(9) . . ? C84 C83 N5 118.9(13) . . ? C84 C83 C76 126.7(13) . . ? N5 C83 C76 114.4(11) . . ? C83 C84 C85 120.2(13) . . ? C86 C85 C84 119.0(12) . . ? C85 C86 C87 117.3(14) . . ? N5 C87 C86 124.3(12) . . ? Yb3 O11 Yb3 119.8(10) . 2_566 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 73.38 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 4.871 _refine_diff_density_min -11.559 _refine_diff_density_rms 0.366 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.000 0.000 242 56 ' ' 2 0.500 0.000 0.500 76 35 ' ' 3 0.311 0.620 0.764 23 2 ' ' 4 0.688 0.380 0.236 23 2 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 971018'