# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email gxjin@fudan.edu.cn _publ_author_name 'Guo-Xin Jin' data_2c _database_code_depnum_ccdc_archive 'CCDC 818216' #TrackingRef '2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Cl2 O4 Ru2' _chemical_formula_weight 779.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.475(15) _cell_length_b 7.891(3) _cell_length_c 19.526(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.223(6) _cell_angle_gamma 90.00 _cell_volume 6078(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 618 _cell_measurement_theta_min 2.825 _cell_measurement_theta_max 19.741 _exptl_crystal_description prism _exptl_crystal_colour dark _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8686 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.23 _diffrn_reflns_number 12066 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.1976 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5328 _reflns_number_gt 2353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5328 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.663 _refine_ls_restrained_S_all 0.663 _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 Ru1 Ru 0.186339(14) 0.09904(7) 0.48096(3) 0.03654(18) Uani 1 1 d . . . Ru2 Ru 0.081732(15) 0.43796(8) 0.12173(3) 0.0417(2) Uani 1 1 d . . . O1 O 0.13735(10) 0.1182(5) 0.4462(2) 0.0376(12) Uani 1 1 d . . . O2 O 0.19844(10) 0.1949(5) 0.3867(2) 0.0394(13) Uani 1 1 d . . . O3 O 0.13073(10) 0.4039(6) 0.1546(2) 0.0476(13) Uani 1 1 d . . . O4 O 0.06966(10) 0.3416(5) 0.2152(2) 0.0391(12) Uani 1 1 d . . . Cl1 Cl 0.18117(4) 0.3927(2) 0.51281(9) 0.0569(5) Uani 1 1 d . . . Cl2 Cl 0.08344(5) 0.1445(2) 0.08892(10) 0.0682(7) Uani 1 1 d . . . C1 C 0.17832(18) 0.2402(8) 0.3366(3) 0.0304(17) Uani 1 1 d . . . C2 C 0.19563(18) 0.2979(9) 0.2766(4) 0.048(2) Uani 1 1 d . . . H2 H 0.2192 0.2975 0.2778 0.057 Uiso 1 1 calc R . . C3 C 0.17894(17) 0.3518(8) 0.2197(3) 0.043(2) Uani 1 1 d . . . H3 H 0.1913 0.3909 0.1834 0.052 Uiso 1 1 calc R . . C4 C 0.14280(17) 0.3513(8) 0.2127(3) 0.0345(18) Uani 1 1 d . . . C5 C 0.12442(16) 0.2921(8) 0.2701(3) 0.0269(17) Uani 1 1 d . . . C6 C 0.14259(16) 0.2363(7) 0.3321(3) 0.0240(16) Uani 1 1 d . . . C7 C 0.12432(17) 0.1714(7) 0.3878(3) 0.0288(17) Uani 1 1 d . . . C8 C 0.08720(16) 0.1635(7) 0.3815(3) 0.0258(16) Uani 1 1 d . . . C9 C 0.06961(16) 0.2260(8) 0.3246(3) 0.0266(17) Uani 1 1 d . . . C10 C 0.08854(17) 0.2910(8) 0.2662(3) 0.0299(17) Uani 1 1 d . . . C11 C 0.03459(17) 0.2253(9) 0.3218(3) 0.046(2) Uani 1 1 d . . . H11 H 0.0229 0.2722 0.2841 0.055 Uiso 1 1 calc R . . C12 C 0.01675(18) 0.1555(9) 0.3746(4) 0.053(2) Uani 1 1 d . . . H12 H -0.0068 0.1537 0.3726 0.064 Uiso 1 1 calc R . . C13 C 0.03447(18) 0.0895(10) 0.4296(3) 0.053(2) Uani 1 1 d . . . H13 H 0.0227 0.0426 0.4654 0.063 Uiso 1 1 calc R . . C14 C 0.06893(16) 0.0905(8) 0.4335(3) 0.0393(18) Uani 1 1 d . . . H14 H 0.0804 0.0421 0.4712 0.047 Uiso 1 1 calc R . . C15 C 0.2040(2) 0.0367(10) 0.5855(4) 0.052(2) Uani 1 1 d . . . C16 C 0.23183(17) 0.0462(9) 0.5411(4) 0.048(2) Uani 1 1 d . . . H16 H 0.2501 0.1172 0.5515 0.058 Uiso 1 1 calc R . . C17 C 0.23120(17) -0.0504(9) 0.4832(3) 0.043(2) Uani 1 1 d . . . H17 H 0.2496 -0.0455 0.4550 0.051 Uiso 1 1 calc R . . C18 C 0.2043(2) -0.1556(9) 0.4645(4) 0.043(2) Uani 1 1 d . . . C19 C 0.17690(18) -0.1616(8) 0.5044(4) 0.042(2) Uani 1 1 d . . . H19 H 0.1583 -0.2275 0.4910 0.050 Uiso 1 1 calc R . . C20 C 0.17653(18) -0.0673(10) 0.5667(4) 0.051(2) Uani 1 1 d . . . H20 H 0.1581 -0.0751 0.5948 0.061 Uiso 1 1 calc R . . C21 C 0.2032(2) 0.1507(11) 0.6484(3) 0.086(3) Uani 1 1 d . . . H21A H 0.1806 0.1931 0.6533 0.129 Uiso 1 1 calc R . . H21B H 0.2185 0.2440 0.6432 0.129 Uiso 1 1 calc R . . H21C H 0.2100 0.0869 0.6885 0.129 Uiso 1 1 calc R . . C22 C 0.20354(19) -0.2589(10) 0.3977(4) 0.057(2) Uani 1 1 d . . . H22 H 0.2076 -0.3772 0.4110 0.069 Uiso 1 1 calc R . . C23 C 0.2318(2) -0.2114(10) 0.3490(4) 0.090(3) Uani 1 1 d . . . H23A H 0.2306 -0.2843 0.3096 0.135 Uiso 1 1 calc R . . H23B H 0.2535 -0.2245 0.3724 0.135 Uiso 1 1 calc R . . H23C H 0.2290 -0.0958 0.3346 0.135 Uiso 1 1 calc R . . C24 C 0.1700(2) -0.2558(11) 0.3587(4) 0.094(3) Uani 1 1 d . . . H24A H 0.1526 -0.2974 0.3875 0.141 Uiso 1 1 calc R . . H24B H 0.1711 -0.3262 0.3188 0.141 Uiso 1 1 calc R . . H24C H 0.1647 -0.1416 0.3450 0.141 Uiso 1 1 calc R . . C25 C 0.0639(2) 0.5037(10) 0.0171(4) 0.060(2) Uani 1 1 d . . . C26 C 0.0925(2) 0.6027(11) 0.0369(4) 0.064(2) Uani 1 1 d . . . H26 H 0.1111 0.6060 0.0091 0.077 Uiso 1 1 calc R . . C27 C 0.0931(2) 0.6975(10) 0.0991(5) 0.060(3) Uani 1 1 d . . . H27 H 0.1122 0.7614 0.1108 0.072 Uiso 1 1 calc R . . C28 C 0.0667(3) 0.6983(10) 0.1422(5) 0.062(3) Uani 1 1 d . . . C29 C 0.0377(2) 0.6002(12) 0.1217(4) 0.065(3) Uani 1 1 d . . . H29 H 0.0190 0.5994 0.1493 0.077 Uiso 1 1 calc R . . C30 C 0.03673(19) 0.5066(10) 0.0622(5) 0.056(2) Uani 1 1 d . . . H30 H 0.0175 0.4429 0.0512 0.067 Uiso 1 1 calc R . . C31 C 0.0641(2) 0.4018(10) -0.0478(4) 0.105(4) Uani 1 1 d . . . H31A H 0.0545 0.4677 -0.0850 0.157 Uiso 1 1 calc R . . H31B H 0.0510 0.3005 -0.0425 0.157 Uiso 1 1 calc R . . H31C H 0.0870 0.3720 -0.0574 0.157 Uiso 1 1 calc R . . C32 C 0.0683(4) 0.7990(13) 0.2085(6) 0.115(4) Uani 1 1 d . . . H32 H 0.0611 0.9139 0.1958 0.137 Uiso 1 1 calc R . . C33 C 0.1038(3) 0.8177(15) 0.2380(6) 0.200(8) Uani 1 1 d . . . H33A H 0.1079 0.9342 0.2498 0.299 Uiso 1 1 calc R . . H33B H 0.1196 0.7824 0.2047 0.299 Uiso 1 1 calc R . . H33C H 0.1065 0.7487 0.2783 0.299 Uiso 1 1 calc R . . C34 C 0.0474(5) 0.7506(19) 0.2610(8) 0.290(12) Uani 1 1 d . . . H34A H 0.0606 0.7418 0.3032 0.434 Uiso 1 1 calc R . . H34B H 0.0373 0.6428 0.2501 0.434 Uiso 1 1 calc R . . H34C H 0.0300 0.8338 0.2659 0.434 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0298(4) 0.0446(4) 0.0348(4) 0.0116(3) -0.0041(3) 0.0015(3) Ru2 0.0404(4) 0.0511(4) 0.0331(4) 0.0093(3) -0.0056(3) 0.0023(3) O1 0.031(3) 0.049(3) 0.033(3) 0.017(2) 0.003(2) 0.002(2) O2 0.027(3) 0.062(3) 0.029(3) 0.017(2) 0.001(2) 0.000(2) O3 0.034(3) 0.076(4) 0.033(3) 0.018(3) 0.000(2) 0.002(3) O4 0.030(3) 0.057(3) 0.031(3) 0.007(2) -0.003(2) 0.006(2) Cl1 0.0501(13) 0.0484(13) 0.0720(14) 0.0003(11) -0.0012(10) -0.0003(11) Cl2 0.0949(18) 0.0550(14) 0.0541(14) -0.0039(11) -0.0054(12) 0.0115(12) C1 0.035(5) 0.027(4) 0.029(5) 0.008(3) 0.003(4) 0.006(3) C2 0.025(5) 0.059(6) 0.060(6) 0.012(4) 0.005(4) 0.001(4) C3 0.034(5) 0.065(6) 0.031(5) 0.016(4) 0.006(4) -0.001(4) C4 0.030(5) 0.040(5) 0.034(5) -0.002(4) 0.008(4) 0.002(4) C5 0.023(4) 0.032(4) 0.025(4) 0.002(3) -0.001(3) 0.003(3) C6 0.023(4) 0.027(4) 0.023(4) 0.007(3) 0.000(3) 0.003(3) C7 0.029(5) 0.025(4) 0.033(5) -0.005(3) 0.001(4) 0.001(3) C8 0.027(4) 0.022(4) 0.028(4) -0.004(3) 0.001(3) -0.002(3) C9 0.022(4) 0.038(4) 0.019(4) -0.005(3) -0.004(3) -0.002(3) C10 0.029(5) 0.031(4) 0.029(5) -0.001(3) -0.007(4) 0.008(3) C11 0.032(5) 0.066(6) 0.039(5) 0.004(4) -0.004(4) 0.002(4) C12 0.030(5) 0.081(7) 0.049(5) 0.001(5) 0.002(4) 0.000(4) C13 0.039(5) 0.084(6) 0.037(5) 0.015(5) 0.010(4) -0.004(5) C14 0.026(4) 0.062(5) 0.030(4) 0.006(4) 0.000(3) -0.007(4) C15 0.052(6) 0.059(6) 0.044(5) 0.008(4) -0.012(4) 0.006(5) C16 0.024(5) 0.064(6) 0.055(6) 0.017(5) -0.020(4) -0.010(4) C17 0.035(5) 0.062(6) 0.031(5) 0.016(4) 0.002(4) 0.004(4) C18 0.044(6) 0.044(5) 0.041(5) 0.011(4) 0.006(4) 0.009(4) C19 0.037(5) 0.043(5) 0.044(5) 0.013(4) -0.010(4) -0.013(4) C20 0.039(5) 0.066(6) 0.047(5) 0.036(5) -0.003(4) 0.000(5) C21 0.101(8) 0.115(8) 0.039(6) -0.005(5) -0.025(5) 0.003(6) C22 0.055(6) 0.048(6) 0.068(7) 0.014(5) 0.002(5) 0.014(4) C23 0.122(9) 0.078(7) 0.070(7) 0.007(5) 0.016(6) 0.030(6) C24 0.094(8) 0.109(8) 0.076(7) -0.036(6) -0.039(6) 0.033(6) C25 0.064(7) 0.064(6) 0.051(6) 0.021(5) -0.025(5) 0.000(5) C26 0.057(6) 0.076(7) 0.059(6) 0.036(6) 0.008(5) 0.011(5) C27 0.068(7) 0.048(6) 0.063(7) 0.012(5) -0.024(6) -0.013(5) C28 0.083(8) 0.047(6) 0.056(7) 0.008(5) 0.002(6) 0.026(6) C29 0.041(6) 0.099(8) 0.054(6) 0.021(6) 0.003(4) 0.026(6) C30 0.037(6) 0.067(6) 0.062(6) 0.028(5) -0.021(5) -0.015(4) C31 0.192(11) 0.091(8) 0.029(5) 0.004(5) -0.024(6) -0.021(7) C32 0.183(14) 0.072(8) 0.088(10) -0.018(7) 0.003(9) 0.041(8) C33 0.254(17) 0.183(14) 0.151(13) -0.119(11) -0.140(13) 0.114(13) C34 0.49(3) 0.205(19) 0.185(16) -0.121(14) 0.19(2) -0.110(19) _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 Ru1 O1 2.030(4) . ? Ru1 O2 2.063(4) . ? Ru1 C17 2.127(7) . ? Ru1 C19 2.143(6) . ? Ru1 C16 2.148(6) . ? Ru1 C18 2.159(7) . ? Ru1 C20 2.175(6) . ? Ru1 C15 2.186(7) . ? Ru1 Cl1 2.410(2) . ? Ru2 O3 2.032(4) . ? Ru2 O4 2.050(4) . ? Ru2 C27 2.146(7) . ? Ru2 C30 2.154(7) . ? Ru2 C29 2.158(7) . ? Ru2 C26 2.161(7) . ? Ru2 C28 2.179(8) . ? Ru2 C25 2.198(7) . ? Ru2 Cl2 2.404(2) . ? O1 C7 1.302(6) . ? O2 C1 1.287(7) . ? O3 C4 1.283(7) . ? O4 C10 1.284(6) . ? C1 C6 1.410(8) . ? C1 C2 1.452(8) . ? C2 C3 1.339(8) . ? C3 C4 1.428(8) . ? C4 C5 1.436(8) . ? C5 C10 1.416(8) . ? C5 C6 1.452(7) . ? C6 C7 1.424(8) . ? C7 C8 1.467(8) . ? C8 C9 1.379(8) . ? C8 C14 1.393(8) . ? C9 C11 1.382(8) . ? C9 C10 1.479(8) . ? C11 C12 1.385(8) . ? C12 C13 1.362(8) . ? C13 C14 1.359(8) . ? C15 C20 1.397(9) . ? C15 C16 1.428(9) . ? C15 C21 1.525(9) . ? C16 C17 1.363(8) . ? C17 C18 1.385(9) . ? C18 C19 1.359(8) . ? C18 C22 1.538(9) . ? C19 C20 1.427(9) . ? C22 C24 1.503(9) . ? C22 C23 1.540(9) . ? C25 C30 1.413(10) . ? C25 C26 1.417(10) . ? C25 C31 1.501(9) . ? C26 C27 1.426(10) . ? C27 C28 1.363(10) . ? C28 C29 1.426(10) . ? C28 C32 1.519(11) . ? C29 C30 1.377(10) . ? C32 C34 1.394(14) . ? C32 C33 1.499(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 O1 Ru1 O2 85.69(16) . . ? O1 Ru1 C17 146.1(3) . . ? O2 Ru1 C17 90.0(2) . . ? O1 Ru1 C19 88.4(2) . . ? O2 Ru1 C19 126.2(2) . . ? C17 Ru1 C19 67.4(3) . . ? O1 Ru1 C16 164.3(2) . . ? O2 Ru1 C16 109.9(2) . . ? C17 Ru1 C16 37.2(2) . . ? C19 Ru1 C16 81.1(3) . . ? O1 Ru1 C18 109.5(2) . . ? O2 Ru1 C18 96.9(2) . . ? C17 Ru1 C18 37.7(2) . . ? C19 Ru1 C18 36.8(2) . . ? C16 Ru1 C18 68.2(3) . . ? O1 Ru1 C20 96.1(2) . . ? O2 Ru1 C20 164.3(2) . . ? C17 Ru1 C20 79.8(3) . . ? C19 Ru1 C20 38.6(2) . . ? C16 Ru1 C20 68.4(3) . . ? C18 Ru1 C20 67.8(3) . . ? O1 Ru1 C15 126.4(3) . . ? O2 Ru1 C15 147.0(3) . . ? C17 Ru1 C15 67.7(3) . . ? C19 Ru1 C15 68.7(3) . . ? C16 Ru1 C15 38.5(2) . . ? C18 Ru1 C15 80.5(3) . . ? C20 Ru1 C15 37.4(2) . . ? O1 Ru1 Cl1 85.73(13) . . ? O2 Ru1 Cl1 84.40(13) . . ? C17 Ru1 Cl1 127.3(2) . . ? C19 Ru1 Cl1 148.3(2) . . ? C16 Ru1 Cl1 97.1(2) . . ? C18 Ru1 Cl1 164.8(2) . . ? C20 Ru1 Cl1 111.2(2) . . ? C15 Ru1 Cl1 90.2(2) . . ? O3 Ru2 O4 85.48(17) . . ? O3 Ru2 C27 89.3(3) . . ? O4 Ru2 C27 126.5(3) . . ? O3 Ru2 C30 163.5(3) . . ? O4 Ru2 C30 111.0(3) . . ? C27 Ru2 C30 79.8(3) . . ? O3 Ru2 C29 146.6(3) . . ? O4 Ru2 C29 90.3(2) . . ? C27 Ru2 C29 66.9(3) . . ? C30 Ru2 C29 37.2(3) . . ? O3 Ru2 C26 96.2(2) . . ? O4 Ru2 C26 164.8(3) . . ? C27 Ru2 C26 38.7(3) . . ? C30 Ru2 C26 67.5(3) . . ? C29 Ru2 C26 80.0(3) . . ? O3 Ru2 C28 109.2(3) . . ? O4 Ru2 C28 96.5(3) . . ? C27 Ru2 C28 36.7(3) . . ? C30 Ru2 C28 68.7(3) . . ? C29 Ru2 C28 38.4(3) . . ? C26 Ru2 C28 68.7(3) . . ? O3 Ru2 C25 126.3(3) . . ? O4 Ru2 C25 146.9(3) . . ? C27 Ru2 C25 69.2(3) . . ? C30 Ru2 C25 37.9(3) . . ? C29 Ru2 C25 68.3(3) . . ? C26 Ru2 C25 37.9(3) . . ? C28 Ru2 C25 82.4(3) . . ? O3 Ru2 Cl2 85.45(14) . . ? O4 Ru2 Cl2 83.67(13) . . ? C27 Ru2 Cl2 148.9(3) . . ? C30 Ru2 Cl2 97.4(2) . . ? C29 Ru2 Cl2 127.0(3) . . ? C26 Ru2 Cl2 111.5(3) . . ? C28 Ru2 Cl2 165.3(3) . . ? C25 Ru2 Cl2 89.5(2) . . ? C7 O1 Ru1 131.0(4) . . ? C1 O2 Ru1 128.5(4) . . ? C4 O3 Ru2 129.7(4) . . ? C10 O4 Ru2 131.1(4) . . ? O2 C1 C6 128.9(6) . . ? O2 C1 C2 113.9(6) . . ? C6 C1 C2 117.2(6) . . ? C3 C2 C1 122.5(7) . . ? C2 C3 C4 122.4(7) . . ? O3 C4 C3 114.8(6) . . ? O3 C4 C5 127.9(6) . . ? C3 C4 C5 117.4(6) . . ? C10 C5 C4 119.7(6) . . ? C10 C5 C6 120.2(5) . . ? C4 C5 C6 120.1(6) . . ? C1 C6 C7 119.7(6) . . ? C1 C6 C5 120.4(5) . . ? C7 C6 C5 119.9(6) . . ? O1 C7 C6 126.2(6) . . ? O1 C7 C8 114.8(6) . . ? C6 C7 C8 119.0(6) . . ? C9 C8 C14 118.5(6) . . ? C9 C8 C7 121.5(6) . . ? C14 C8 C7 120.0(6) . . ? C8 C9 C11 120.1(6) . . ? C8 C9 C10 119.5(6) . . ? C11 C9 C10 120.4(6) . . ? O4 C10 C5 126.1(6) . . ? O4 C10 C9 114.2(6) . . ? C5 C10 C9 119.7(6) . . ? C9 C11 C12 120.6(7) . . ? C13 C12 C11 118.6(7) . . ? C14 C13 C12 121.6(7) . . ? C13 C14 C8 120.5(6) . . ? C20 C15 C16 118.7(7) . . ? C20 C15 C21 121.2(8) . . ? C16 C15 C21 119.9(8) . . ? C20 C15 Ru1 70.9(4) . . ? C16 C15 Ru1 69.3(4) . . ? C21 C15 Ru1 127.2(5) . . ? C17 C16 C15 119.0(7) . . ? C17 C16 Ru1 70.6(4) . . ? C15 C16 Ru1 72.2(4) . . ? C16 C17 C18 122.9(7) . . ? C16 C17 Ru1 72.2(4) . . ? C18 C17 Ru1 72.4(4) . . ? C19 C18 C17 119.2(7) . . ? C19 C18 C22 118.6(7) . . ? C17 C18 C22 122.1(7) . . ? C19 C18 Ru1 70.9(4) . . ? C17 C18 Ru1 69.9(4) . . ? C22 C18 Ru1 128.6(5) . . ? C18 C19 C20 120.4(7) . . ? C18 C19 Ru1 72.2(4) . . ? C20 C19 Ru1 71.9(4) . . ? C15 C20 C19 119.7(7) . . ? C15 C20 Ru1 71.8(4) . . ? C19 C20 Ru1 69.5(4) . . ? C24 C22 C18 114.1(6) . . ? C24 C22 C23 109.2(7) . . ? C18 C22 C23 113.8(7) . . ? C30 C25 C26 115.9(8) . . ? C30 C25 C31 124.4(9) . . ? C26 C25 C31 119.7(9) . . ? C30 C25 Ru2 69.4(4) . . ? C26 C25 Ru2 69.6(4) . . ? C31 C25 Ru2 130.2(5) . . ? C25 C26 C27 120.6(8) . . ? C25 C26 Ru2 72.5(4) . . ? C27 C26 Ru2 70.1(4) . . ? C28 C27 C26 122.7(8) . . ? C28 C27 Ru2 73.0(5) . . ? C26 C27 Ru2 71.2(4) . . ? C27 C28 C29 116.7(9) . . ? C27 C28 C32 121.4(11) . . ? C29 C28 C32 121.9(10) . . ? C27 C28 Ru2 70.3(5) . . ? C29 C28 Ru2 70.0(5) . . ? C32 C28 Ru2 130.3(6) . . ? C30 C29 C28 121.6(8) . . ? C30 C29 Ru2 71.2(4) . . ? C28 C29 Ru2 71.6(4) . . ? C29 C30 C25 122.5(8) . . ? C29 C30 Ru2 71.5(4) . . ? C25 C30 Ru2 72.7(4) . . ? C34 C32 C33 108.3(12) . . ? C34 C32 C28 118.5(12) . . ? C33 C32 C28 112.7(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.650 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.091 # Attachment '3a-CH2Cl2.cif' data_3a-1.53CH2Cl2-5.42H2O _database_code_depnum_ccdc_archive 'CCDC 818217' #TrackingRef '3a-CH2Cl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81.3 H93.44 Cl2.6 F12 Ir4 N4 O25.42 S4' _chemical_formula_weight 2750.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.764(5) _cell_length_b 13.320(5) _cell_length_c 16.760(6) _cell_angle_alpha 67.201(5) _cell_angle_beta 75.383(5) _cell_angle_gamma 77.627(6) _cell_volume 2520.0(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 816 _cell_measurement_theta_min 2.683 _cell_measurement_theta_max 22.378 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 5.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6084 _exptl_absorpt_correction_T_max 0.7331 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.44 _diffrn_reflns_number 10472 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1398 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8683 _reflns_number_gt 4435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8683 _refine_ls_number_parameters 659 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.22852(5) 0.20798(4) 1.25148(3) 0.0507(2) Uani 1 1 d . . . Ir2 Ir 0.27121(5) 0.47132(4) 0.70194(3) 0.0521(2) Uani 1 1 d . . . N1 N 0.0813(9) 0.3157(8) 1.2393(6) 0.042(3) Uani 1 1 d . . . N2 N -0.1195(8) 0.4432(8) 1.2598(6) 0.039(2) Uani 1 1 d . . . O1 O 0.2949(6) 0.3356(7) 1.1493(5) 0.049(2) Uani 1 1 d . . . O2 O 0.1899(7) 0.1652(7) 1.1576(5) 0.052(2) Uani 1 1 d . . . O3 O 0.2131(7) 0.3388(6) 0.8041(5) 0.047(2) Uani 1 1 d . A . O4 O 0.3177(7) 0.5095(7) 0.7961(5) 0.054(2) Uani 1 1 d . A . O5 O 0.6848(10) 0.0140(11) 0.4379(8) 0.123(5) Uani 1 1 d . . . O6 O 0.7124(10) 0.1815(10) 0.3166(10) 0.127(5) Uani 1 1 d . . . O7 O 0.8485(8) 0.0874(9) 0.3988(7) 0.087(3) Uani 1 1 d . . . O8 O 0.2731(13) 0.665(3) 0.294(3) 0.45(3) Uani 1 1 d . . . O9 O 0.203(3) 0.643(2) 0.1897(14) 0.35(2) Uani 1 1 d . . . O10 O 0.147(3) 0.5518(16) 0.3286(17) 0.34(2) Uani 1 1 d . . . F1 F 0.7399(14) -0.0054(13) 0.2648(9) 0.192(7) Uani 1 1 d . . . F2 F 0.8898(15) 0.0468(18) 0.2382(10) 0.242(10) Uani 1 1 d . . . F3 F 0.8459(13) -0.0995(14) 0.3497(15) 0.209(8) Uani 1 1 d . . . F4 F 0.109(3) 0.8418(17) 0.2379(14) 0.40(2) Uani 1 1 d . . . F5 F -0.0029(15) 0.7351(15) 0.2628(15) 0.241(9) Uani 1 1 d . . . F6 F 0.0566(16) 0.7443(15) 0.3655(11) 0.229(9) Uani 1 1 d . . . S1 S 0.7592(4) 0.0781(4) 0.3725(3) 0.0730(12) Uani 1 1 d . . . S2 S 0.1874(6) 0.6464(8) 0.2697(6) 0.153(3) Uani 1 1 d D . . C1 C 0.2972(9) 0.3664(10) 1.0654(8) 0.042(3) Uani 1 1 d . A . C2 C 0.2537(10) 0.3144(10) 1.0250(8) 0.044(3) Uani 1 1 d . . . C3 C 0.2097(10) 0.2131(10) 1.0727(8) 0.042(3) Uani 1 1 d . A . C4 C 0.1803(12) 0.1518(10) 1.0277(8) 0.055(4) Uani 1 1 d . . . C5 C 0.149(2) 0.0496(16) 1.0729(12) 0.078(8) Uani 0.711(9) 1 d P A 1 H5 H 0.1446 0.0204 1.1337 0.094 Uiso 0.711(9) 1 calc PR A 1 C6 C 0.125(3) -0.010(2) 1.0341(16) 0.120(11) Uani 0.711(9) 1 d P A 1 H6 H 0.1034 -0.0789 1.0665 0.145 Uiso 0.711(9) 1 calc PR A 1 C7 C 0.132(2) 0.036(2) 0.9421(15) 0.100(9) Uani 0.711(9) 1 d P A 1 H7 H 0.1185 -0.0061 0.9134 0.120 Uiso 0.711(9) 1 calc PR A 1 C8 C 0.1580(19) 0.1346(17) 0.8952(11) 0.072(7) Uani 0.711(9) 1 d P A 1 H8 H 0.1571 0.1643 0.8351 0.087 Uiso 0.711(9) 1 calc PR A 1 O13 O 0.4216(13) 0.7607(15) 0.9828(11) 0.107(6) Uani 0.711(9) 1 d P A 1 C5' C 0.348(3) 0.527(3) 1.065(3) 0.044(12) Uani 0.289(9) 1 d PDU A 2 H5' H 0.3323 0.4980 1.1258 0.053 Uiso 0.289(9) 1 calc PR A 2 C6' C 0.376(4) 0.635(3) 1.019(2) 0.060(14) Uani 0.289(9) 1 d PDU A 2 H6' H 0.3878 0.6766 1.0484 0.072 Uiso 0.289(9) 1 calc PR A 2 C7' C 0.386(3) 0.675(3) 0.926(2) 0.045(12) Uani 0.289(9) 1 d PDU A 2 H7' H 0.4001 0.7474 0.8947 0.054 Uiso 0.289(9) 1 calc PR A 2 C8' C 0.375(3) 0.611(3) 0.880(2) 0.042(12) Uani 0.289(9) 1 d PD A 2 H8' H 0.3847 0.6395 0.8186 0.051 Uiso 0.289(9) 1 calc PR A 2 C9 C 0.1871(11) 0.1952(10) 0.9369(8) 0.054(4) Uani 1 1 d . A . C10 C 0.2212(10) 0.3059(10) 0.8855(8) 0.047(3) Uani 1 1 d . . . C11 C 0.2591(10) 0.3622(10) 0.9267(7) 0.039(3) Uani 1 1 d . A . C12 C 0.3089(11) 0.4576(10) 0.8787(8) 0.049(3) Uani 1 1 d . . . C13 C 0.3502(11) 0.5113(11) 0.9232(9) 0.054(4) Uani 1 1 d . A . C14 C 0.3436(10) 0.4654(11) 1.0124(9) 0.050(3) Uani 1 1 d . . . C15 C 0.0760(10) 0.4158(11) 1.2365(8) 0.046(3) Uani 1 1 d . . . H15 H 0.1404 0.4443 1.2267 0.056 Uiso 1 1 calc R . . C16 C -0.0246(13) 0.4822(11) 1.2477(8) 0.058(4) Uani 1 1 d . . . H16 H -0.0259 0.5527 1.2469 0.069 Uiso 1 1 calc R . . C17 C -0.1142(11) 0.3455(12) 1.2560(8) 0.059(4) Uani 1 1 d . . . H17 H -0.1776 0.3182 1.2607 0.071 Uiso 1 1 calc R . . C18 C -0.0085(12) 0.2806(10) 1.2442(7) 0.049(3) Uani 1 1 d . . . H18 H -0.0049 0.2122 1.2400 0.059 Uiso 1 1 calc R . . C19 C 0.3133(18) 0.0557(14) 1.3164(12) 0.082(6) Uani 1 1 d . . . C20 C 0.2171(16) 0.0576(14) 1.3622(10) 0.073(5) Uani 1 1 d . . . C21 C 0.1938(16) 0.1417(14) 1.3934(8) 0.073(5) Uani 1 1 d . . . C22 C 0.2763(14) 0.2026(15) 1.3642(10) 0.065(4) Uani 1 1 d . . . C23 C 0.3613(15) 0.1453(18) 1.3183(10) 0.092(6) Uani 1 1 d . . . C24 C 0.372(2) -0.0197(19) 1.2753(13) 0.214(16) Uani 1 1 d . . . H24A H 0.4361 -0.0557 1.3006 0.321 Uiso 1 1 calc R . . H24B H 0.3939 0.0189 1.2133 0.321 Uiso 1 1 calc R . . H24C H 0.3269 -0.0734 1.2841 0.321 Uiso 1 1 calc R . . C25 C 0.1375(19) -0.0243(15) 1.3752(12) 0.144(9) Uani 1 1 d . . . H25A H 0.1754 -0.0784 1.3497 0.216 Uiso 1 1 calc R . . H25B H 0.0767 0.0152 1.3470 0.216 Uiso 1 1 calc R . . H25C H 0.1115 -0.0600 1.4370 0.216 Uiso 1 1 calc R . . C26 C 0.0761(15) 0.1686(17) 1.4462(10) 0.124(8) Uani 1 1 d . . . H26A H 0.0224 0.1478 1.4266 0.186 Uiso 1 1 calc R . . H26B H 0.0614 0.2459 1.4361 0.186 Uiso 1 1 calc R . . H26C H 0.0734 0.1283 1.5081 0.186 Uiso 1 1 calc R . . C27 C 0.2771(15) 0.2988(16) 1.3884(11) 0.111(7) Uani 1 1 d . . . H27A H 0.2088 0.3457 1.3827 0.167 Uiso 1 1 calc R . . H27B H 0.3356 0.3390 1.3498 0.167 Uiso 1 1 calc R . . H27C H 0.2875 0.2738 1.4481 0.167 Uiso 1 1 calc R . . C28 C 0.4794(17) 0.181(2) 1.2745(14) 0.195(14) Uani 1 1 d . . . H28A H 0.4761 0.2584 1.2609 0.292 Uiso 1 1 calc R . . H28B H 0.5052 0.1645 1.2214 0.292 Uiso 1 1 calc R . . H28C H 0.5285 0.1414 1.3148 0.292 Uiso 1 1 calc R . . C29 C 0.4098(17) 0.5290(16) 0.5990(9) 0.093(6) Uani 1 1 d . . . C30 C 0.2984(14) 0.5685(14) 0.5654(8) 0.069(5) Uani 1 1 d . . . C31 C 0.2487(16) 0.4826(17) 0.5743(9) 0.076(5) Uani 1 1 d . . . C32 C 0.316(3) 0.3868(15) 0.6107(11) 0.142(12) Uani 1 1 d . . . C33 C 0.4176(15) 0.4077(19) 0.6305(11) 0.093(6) Uani 1 1 d . . . C34 C 0.4868(18) 0.586(2) 0.6107(14) 0.197(14) Uani 1 1 d . . . H34A H 0.4813 0.5701 0.6724 0.296 Uiso 1 1 calc R . . H34B H 0.4705 0.6632 0.5812 0.296 Uiso 1 1 calc R . . H34C H 0.5596 0.5607 0.5862 0.296 Uiso 1 1 calc R . . C35 C 0.2477(18) 0.6835(16) 0.5273(11) 0.157(11) Uani 1 1 d . . . H35A H 0.1767 0.6940 0.5620 0.235 Uiso 1 1 calc R . . H35B H 0.2409 0.6982 0.4679 0.235 Uiso 1 1 calc R . . H35C H 0.2928 0.7326 0.5273 0.235 Uiso 1 1 calc R . . C36 C 0.158(2) 0.486(2) 0.5426(13) 0.186(14) Uani 1 1 d . . . H36A H 0.1030 0.5430 0.5535 0.279 Uiso 1 1 calc R . . H36B H 0.1303 0.4165 0.5718 0.279 Uiso 1 1 calc R . . H36C H 0.1778 0.5002 0.4804 0.279 Uiso 1 1 calc R . . C37 C 0.274(3) 0.2746(15) 0.6308(13) 0.238(19) Uani 1 1 d . . . H37A H 0.3029 0.2499 0.5819 0.358 Uiso 1 1 calc R . . H37B H 0.1953 0.2854 0.6398 0.358 Uiso 1 1 calc R . . H37C H 0.2968 0.2204 0.6829 0.358 Uiso 1 1 calc R . . C38 C 0.490(2) 0.316(3) 0.6674(14) 0.28(2) Uani 1 1 d . . . H38A H 0.4588 0.2784 0.7275 0.417 Uiso 1 1 calc R . . H38B H 0.5573 0.3400 0.6653 0.417 Uiso 1 1 calc R . . H38C H 0.5050 0.2679 0.6347 0.417 Uiso 1 1 calc R . . C39 C 0.814(2) 0.006(2) 0.3039(19) 0.133(9) Uani 1 1 d U . . C40 C 0.0846(19) 0.748(2) 0.2859(19) 0.144(9) Uani 1 1 d DU . . C41 C 0.099(3) 0.676(3) 0.013(2) 0.17(2) Uani 0.65 1 d P . . H41A H 0.1560 0.6434 0.0474 0.199 Uiso 0.65 1 calc PR . . H41B H 0.0445 0.7201 0.0414 0.199 Uiso 0.65 1 calc PR . . Cl1 Cl 0.1532(15) 0.7583(9) -0.0869(10) 0.246(8) Uani 0.65 1 d P . . Cl2 Cl 0.0450(8) 0.5821(11) 0.0133(7) 0.167(5) Uani 0.65 1 d P . . O11 O 0.4914(9) 0.1160(10) 0.5365(8) 0.111(4) Uani 1 1 d . . . O12 O 0.5008(12) 0.8493(11) 0.0828(9) 0.138(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0614(4) 0.0496(4) 0.0387(3) -0.0129(3) -0.0220(3) 0.0077(3) Ir2 0.0609(4) 0.0496(4) 0.0344(3) -0.0118(3) -0.0066(3) 0.0074(3) N1 0.059(8) 0.040(7) 0.027(5) -0.013(5) -0.002(5) -0.010(6) N2 0.059(7) 0.019(5) 0.043(6) -0.010(5) -0.020(5) -0.002(5) O1 0.041(5) 0.063(6) 0.043(5) -0.015(4) -0.012(4) -0.008(4) O2 0.078(7) 0.049(6) 0.029(5) -0.013(4) -0.019(5) 0.000(5) O3 0.066(6) 0.044(5) 0.028(4) -0.018(4) -0.009(4) 0.014(4) O4 0.077(7) 0.049(6) 0.029(5) -0.013(4) -0.004(4) -0.003(5) O5 0.101(10) 0.137(11) 0.097(9) 0.002(8) 0.012(8) -0.062(9) O6 0.107(10) 0.076(9) 0.186(14) -0.004(9) -0.076(10) -0.010(8) O7 0.075(8) 0.089(8) 0.108(9) -0.031(7) -0.037(7) -0.018(6) O8 0.050(11) 0.65(6) 0.95(8) -0.60(6) -0.16(3) 0.035(19) O9 0.54(5) 0.45(4) 0.157(18) -0.22(2) 0.16(2) -0.29(4) O10 0.75(6) 0.110(15) 0.28(3) -0.114(17) -0.39(4) 0.13(2) F1 0.278(19) 0.216(16) 0.138(11) -0.097(11) 0.003(12) -0.130(15) F2 0.233(18) 0.41(3) 0.168(14) -0.199(17) 0.093(13) -0.19(2) F3 0.166(14) 0.158(14) 0.37(3) -0.162(17) -0.097(16) 0.029(12) F4 0.81(7) 0.20(2) 0.25(2) 0.027(18) -0.15(3) -0.31(3) F5 0.223(18) 0.210(18) 0.37(3) -0.153(18) -0.130(19) 0.006(14) F6 0.30(2) 0.26(2) 0.144(13) -0.114(14) -0.064(15) 0.039(16) S1 0.064(3) 0.077(3) 0.074(3) -0.020(2) -0.016(2) -0.008(2) S2 0.123(6) 0.203(9) 0.184(8) -0.132(7) -0.048(6) 0.019(6) C1 0.026(7) 0.052(9) 0.053(8) -0.019(7) -0.011(6) -0.007(6) C2 0.060(9) 0.031(7) 0.035(7) -0.010(6) -0.004(6) -0.002(7) C3 0.040(8) 0.038(8) 0.049(8) -0.023(6) -0.017(6) 0.020(6) C4 0.091(11) 0.040(8) 0.030(7) -0.002(6) -0.016(7) -0.015(8) C5 0.16(2) 0.049(13) 0.037(11) -0.009(10) -0.030(13) -0.047(14) C6 0.22(4) 0.077(19) 0.074(17) -0.014(15) -0.04(2) -0.06(2) C7 0.18(3) 0.070(18) 0.082(18) -0.034(15) -0.060(19) -0.019(18) C8 0.14(2) 0.051(14) 0.019(9) -0.010(9) -0.013(11) -0.006(13) O13 0.086(12) 0.151(17) 0.105(13) -0.075(12) -0.016(10) 0.000(11) C5' 0.022(17) 0.054(19) 0.059(19) -0.011(15) -0.015(14) -0.017(15) C6' 0.06(2) 0.07(2) 0.055(19) -0.033(16) -0.008(16) 0.004(16) C7' 0.029(18) 0.044(18) 0.048(18) -0.012(14) 0.003(14) 0.005(14) C8' 0.03(2) 0.07(3) 0.02(2) 0.00(2) -0.002(18) -0.02(2) C9 0.078(11) 0.042(8) 0.034(7) -0.005(6) -0.008(7) -0.008(7) C10 0.051(9) 0.034(8) 0.048(8) -0.017(6) 0.001(7) 0.005(6) C11 0.048(8) 0.039(8) 0.038(7) -0.021(6) -0.017(6) 0.006(6) C12 0.063(9) 0.042(8) 0.035(8) -0.011(6) -0.004(7) -0.006(7) C13 0.053(9) 0.041(9) 0.065(9) -0.006(7) -0.021(7) -0.013(7) C14 0.039(8) 0.047(8) 0.074(10) -0.022(8) -0.021(7) -0.013(7) C15 0.040(8) 0.054(9) 0.044(8) -0.017(7) -0.009(6) -0.005(7) C16 0.095(12) 0.044(9) 0.039(8) -0.019(6) -0.006(8) -0.020(9) C17 0.056(10) 0.079(12) 0.040(8) -0.028(7) -0.010(7) 0.013(8) C18 0.082(11) 0.038(8) 0.029(7) -0.011(6) -0.001(7) -0.021(8) C19 0.108(16) 0.066(12) 0.084(13) -0.050(10) -0.051(12) 0.051(11) C20 0.094(14) 0.063(12) 0.040(9) 0.002(8) -0.025(9) 0.012(11) C21 0.121(16) 0.055(11) 0.016(7) 0.006(7) -0.017(9) 0.012(11) C22 0.056(11) 0.075(12) 0.056(10) -0.010(9) -0.030(9) 0.004(10) C23 0.075(13) 0.120(17) 0.056(10) -0.006(10) -0.045(10) 0.028(12) C24 0.34(4) 0.17(2) 0.089(16) -0.061(16) -0.11(2) 0.16(3) C25 0.25(3) 0.079(14) 0.101(15) 0.017(12) -0.082(17) -0.049(17) C26 0.131(18) 0.16(2) 0.045(10) -0.010(11) -0.019(11) 0.002(15) C27 0.122(17) 0.122(18) 0.107(15) -0.035(13) -0.078(14) 0.006(13) C28 0.101(19) 0.35(4) 0.098(17) -0.03(2) -0.039(15) -0.03(2) C29 0.143(19) 0.094(15) 0.031(8) -0.026(9) 0.037(10) -0.048(13) C30 0.084(12) 0.077(12) 0.020(7) -0.008(7) 0.000(7) 0.011(10) C31 0.121(15) 0.079(13) 0.038(8) -0.018(9) 0.003(9) -0.059(12) C32 0.30(4) 0.051(12) 0.030(9) -0.022(9) 0.072(15) -0.044(18) C33 0.064(12) 0.111(18) 0.060(11) -0.017(11) 0.020(9) 0.018(12) C34 0.15(2) 0.37(4) 0.15(2) -0.17(2) 0.092(17) -0.20(3) C35 0.23(3) 0.13(2) 0.057(11) -0.033(12) -0.032(15) 0.080(19) C36 0.20(3) 0.33(4) 0.091(15) -0.09(2) -0.011(17) -0.14(3) C37 0.52(5) 0.059(15) 0.088(16) -0.050(12) 0.06(2) -0.03(2) C38 0.20(3) 0.38(4) 0.089(16) -0.06(2) -0.013(17) 0.24(3) C39 0.116(15) 0.144(16) 0.180(18) -0.051(13) -0.048(13) -0.088(13) C40 0.155(17) 0.180(18) 0.122(15) -0.065(14) -0.028(14) -0.052(15) C41 0.07(2) 0.11(3) 0.17(4) 0.04(3) 0.04(2) 0.03(2) Cl1 0.41(2) 0.110(9) 0.269(16) -0.073(10) -0.202(17) 0.035(11) Cl2 0.096(8) 0.220(13) 0.116(7) -0.026(8) -0.008(6) 0.046(7) O11 0.091(9) 0.107(10) 0.139(11) -0.061(8) 0.000(8) -0.014(7) O12 0.163(13) 0.121(11) 0.114(11) -0.065(9) 0.008(10) 0.017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 O1 2.041(8) . ? Ir1 O2 2.062(7) . ? Ir1 C22 2.098(14) . ? Ir1 C19 2.101(14) . ? Ir1 N1 2.108(10) . ? Ir1 C23 2.109(14) . ? Ir1 C20 2.142(14) . ? Ir1 C21 2.154(13) . ? Ir2 O3 2.044(8) . ? Ir2 O4 2.079(8) . ? Ir2 N2 2.110(10) 2_567 ? Ir2 C30 2.128(12) . ? Ir2 C32 2.134(16) . ? Ir2 C33 2.150(16) . ? Ir2 C29 2.170(16) . ? Ir2 C31 2.173(15) . ? N1 C18 1.302(15) . ? N1 C15 1.303(15) . ? N2 C17 1.315(16) . ? N2 C16 1.357(16) . ? N2 Ir2 2.110(10) 2_567 ? O1 C1 1.298(13) . ? O2 C3 1.296(13) . ? O3 C10 1.285(13) . ? O4 C12 1.273(13) . ? O5 S1 1.388(10) . ? O6 S1 1.435(12) . ? O7 S1 1.365(9) . ? O8 S2 1.358(16) . ? O9 S2 1.322(19) . ? O10 S2 1.37(3) . ? F1 C39 1.34(2) . ? F2 C39 1.29(3) . ? F3 C39 1.35(3) . ? F4 C40 1.25(3) . ? F5 C40 1.34(2) . ? F6 C40 1.27(2) . ? S1 C39 1.70(3) . ? S2 C40 1.727(17) . ? C1 C2 1.400(16) . ? C1 C14 1.428(16) . ? C2 C3 1.428(16) . ? C2 C11 1.508(14) . ? C3 C4 1.457(17) . ? C4 C5 1.37(2) . ? C4 C9 1.390(15) . ? C5 C6 1.32(3) . ? C6 C7 1.41(3) . ? C7 C8 1.31(3) . ? C8 C9 1.41(2) . ? C5' C6' 1.41(2) . ? C5' C14 1.43(4) . ? C6' C7' 1.416(19) . ? C7' C8' 1.409(19) . ? C8' C13 1.31(4) . ? C9 C10 1.485(16) . ? C10 C11 1.414(16) . ? C11 C12 1.401(16) . ? C12 C13 1.456(17) . ? C13 C14 1.366(17) . ? C15 C16 1.409(18) . ? C17 C18 1.451(17) . ? C19 C20 1.27(2) . ? C19 C24 1.41(2) . ? C19 C23 1.47(2) . ? C20 C21 1.36(2) . ? C20 C25 1.56(2) . ? C21 C22 1.34(2) . ? C21 C26 1.59(2) . ? C22 C23 1.42(2) . ? C22 C27 1.49(2) . ? C23 C28 1.59(2) . ? C29 C34 1.45(2) . ? C29 C33 1.48(2) . ? C29 C30 1.57(2) . ? C30 C31 1.36(2) . ? C30 C35 1.48(2) . ? C31 C36 1.38(2) . ? C31 C32 1.39(3) . ? C32 C33 1.52(3) . ? C32 C37 1.58(3) . ? C33 C38 1.40(2) . ? C41 Cl2 1.54(4) . ? C41 Cl1 1.67(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ir1 O2 86.7(3) . . ? O1 Ir1 C22 106.3(6) . . ? O2 Ir1 C22 163.6(5) . . ? O1 Ir1 C19 126.3(7) . . ? O2 Ir1 C19 97.7(5) . . ? C22 Ir1 C19 66.6(6) . . ? O1 Ir1 N1 83.9(4) . . ? O2 Ir1 N1 84.1(4) . . ? C22 Ir1 N1 106.9(5) . . ? C19 Ir1 N1 149.7(7) . . ? O1 Ir1 C23 98.5(6) . . ? O2 Ir1 C23 129.9(7) . . ? C22 Ir1 C23 39.6(6) . . ? C19 Ir1 C23 40.8(7) . . ? N1 Ir1 C23 145.9(7) . . ? O1 Ir1 C20 160.1(6) . . ? O2 Ir1 C20 100.9(6) . . ? C22 Ir1 C20 63.6(7) . . ? C19 Ir1 C20 35.0(6) . . ? N1 Ir1 C20 114.9(6) . . ? C23 Ir1 C20 62.5(7) . . ? O1 Ir1 C21 141.0(6) . . ? O2 Ir1 C21 132.1(6) . . ? C22 Ir1 C21 36.8(6) . . ? C19 Ir1 C21 61.3(6) . . ? N1 Ir1 C21 95.2(5) . . ? C23 Ir1 C21 61.8(7) . . ? C20 Ir1 C21 36.9(6) . . ? O3 Ir2 O4 86.3(3) . . ? O3 Ir2 N2 84.2(3) . 2_567 ? O4 Ir2 N2 83.2(4) . 2_567 ? O3 Ir2 C30 150.8(6) . . ? O4 Ir2 C30 123.0(6) . . ? N2 Ir2 C30 98.1(5) 2_567 . ? O3 Ir2 C32 93.4(5) . . ? O4 Ir2 C32 146.9(10) . . ? N2 Ir2 C32 129.8(10) 2_567 . ? C30 Ir2 C32 62.7(6) . . ? O3 Ir2 C33 106.2(6) . . ? O4 Ir2 C33 107.0(7) . . ? N2 Ir2 C33 165.6(5) 2_567 . ? C30 Ir2 C33 68.0(6) . . ? C32 Ir2 C33 41.5(8) . . ? O3 Ir2 C29 145.1(6) . . ? O4 Ir2 C29 95.3(5) . . ? N2 Ir2 C29 130.7(6) 2_567 . ? C30 Ir2 C29 42.9(6) . . ? C32 Ir2 C29 66.9(8) . . ? C33 Ir2 C29 40.1(7) . . ? O3 Ir2 C31 113.8(5) . . ? O4 Ir2 C31 159.9(5) . . ? N2 Ir2 C31 98.6(6) 2_567 . ? C30 Ir2 C31 37.0(5) . . ? C32 Ir2 C31 37.6(8) . . ? C33 Ir2 C31 68.4(7) . . ? C29 Ir2 C31 68.3(6) . . ? C18 N1 C15 118.4(12) . . ? C18 N1 Ir1 120.8(9) . . ? C15 N1 Ir1 120.4(9) . . ? C17 N2 C16 118.3(12) . . ? C17 N2 Ir2 120.5(9) . 2_567 ? C16 N2 Ir2 120.9(9) . 2_567 ? C1 O1 Ir1 130.0(8) . . ? C3 O2 Ir1 128.3(8) . . ? C10 O3 Ir2 128.3(8) . . ? C12 O4 Ir2 129.4(8) . . ? O7 S1 O5 115.7(8) . . ? O7 S1 O6 112.5(7) . . ? O5 S1 O6 115.3(8) . . ? O7 S1 C39 102.8(9) . . ? O5 S1 C39 104.6(10) . . ? O6 S1 C39 104.0(12) . . ? O9 S2 O8 118(2) . . ? O9 S2 O10 107.9(15) . . ? O8 S2 O10 111(2) . . ? O9 S2 C40 112(2) . . ? O8 S2 C40 103.9(15) . . ? O10 S2 C40 103.2(18) . . ? O1 C1 C2 125.7(11) . . ? O1 C1 C14 115.3(11) . . ? C2 C1 C14 119.0(11) . . ? C1 C2 C3 122.5(11) . . ? C1 C2 C11 119.7(10) . . ? C3 C2 C11 117.7(10) . . ? O2 C3 C2 126.2(11) . . ? O2 C3 C4 112.2(11) . . ? C2 C3 C4 121.6(11) . . ? C5 C4 C9 118.5(13) . . ? C5 C4 C3 121.2(12) . . ? C9 C4 C3 120.3(11) . . ? C6 C5 C4 122.9(18) . . ? C5 C6 C7 118(2) . . ? C8 C7 C6 123(2) . . ? C7 C8 C9 119.0(16) . . ? C6' C5' C14 117(3) . . ? C5' C6' C7' 117(4) . . ? C8' C7' C6' 123(4) . . ? C13 C8' C7' 120(3) . . ? C4 C9 C8 119.1(13) . . ? C4 C9 C10 120.0(12) . . ? C8 C9 C10 120.8(12) . . ? O3 C10 C11 127.2(11) . . ? O3 C10 C9 112.5(11) . . ? C11 C10 C9 120.3(11) . . ? C12 C11 C10 122.3(11) . . ? C12 C11 C2 118.1(10) . . ? C10 C11 C2 119.5(10) . . ? O4 C12 C11 125.9(12) . . ? O4 C12 C13 113.2(11) . . ? C11 C12 C13 120.7(11) . . ? C8' C13 C14 120.9(19) . . ? C8' C13 C12 118.7(18) . . ? C14 C13 C12 119.2(11) . . ? C13 C14 C1 123.2(11) . . ? C13 C14 C5' 122.4(19) . . ? C1 C14 C5' 111.3(18) . . ? N1 C15 C16 122.0(12) . . ? N2 C16 C15 120.0(12) . . ? N2 C17 C18 119.4(13) . . ? N1 C18 C17 121.5(13) . . ? C20 C19 C24 130(3) . . ? C20 C19 C23 107.0(16) . . ? C24 C19 C23 123(2) . . ? C20 C19 Ir1 74.3(10) . . ? C24 C19 Ir1 124.4(12) . . ? C23 C19 Ir1 69.9(8) . . ? C19 C20 C21 110.8(18) . . ? C19 C20 C25 123(2) . . ? C21 C20 C25 126(2) . . ? C19 C20 Ir1 70.8(10) . . ? C21 C20 Ir1 72.0(9) . . ? C25 C20 Ir1 121.9(10) . . ? C22 C21 C20 111.5(17) . . ? C22 C21 C26 126.7(18) . . ? C20 C21 C26 121.3(19) . . ? C22 C21 Ir1 69.4(8) . . ? C20 C21 Ir1 71.1(8) . . ? C26 C21 Ir1 120.5(10) . . ? C21 C22 C23 104.5(18) . . ? C21 C22 C27 124.6(18) . . ? C23 C22 C27 130.4(18) . . ? C21 C22 Ir1 73.9(9) . . ? C23 C22 Ir1 70.6(9) . . ? C27 C22 Ir1 126.1(11) . . ? C22 C23 C19 105.8(16) . . ? C22 C23 C28 125(2) . . ? C19 C23 C28 129(2) . . ? C22 C23 Ir1 69.8(8) . . ? C19 C23 Ir1 69.3(9) . . ? C28 C23 Ir1 122.4(11) . . ? C34 C29 C33 123(2) . . ? C34 C29 C30 133(2) . . ? C33 C29 C30 103.1(15) . . ? C34 C29 Ir2 121.5(11) . . ? C33 C29 Ir2 69.2(8) . . ? C30 C29 Ir2 67.1(8) . . ? C31 C30 C35 120.9(19) . . ? C31 C30 C29 112.1(15) . . ? C35 C30 C29 127.0(19) . . ? C31 C30 Ir2 73.3(9) . . ? C35 C30 Ir2 124.7(11) . . ? C29 C30 Ir2 70.0(7) . . ? C30 C31 C36 128(2) . . ? C30 C31 C32 107.2(18) . . ? C36 C31 C32 124(2) . . ? C30 C31 Ir2 69.7(8) . . ? C36 C31 Ir2 132.8(14) . . ? C32 C31 Ir2 69.7(10) . . ? C31 C32 C33 113.1(16) . . ? C31 C32 C37 117(3) . . ? C33 C32 C37 130(3) . . ? C31 C32 Ir2 72.7(10) . . ? C33 C32 Ir2 69.8(10) . . ? C37 C32 Ir2 122.2(11) . . ? C38 C33 C29 138(3) . . ? C38 C33 C32 117(3) . . ? C29 C33 C32 104.4(16) . . ? C38 C33 Ir2 125.5(13) . . ? C29 C33 Ir2 70.7(10) . . ? C32 C33 Ir2 68.7(9) . . ? F2 C39 F1 103(2) . . ? F2 C39 F3 111(3) . . ? F1 C39 F3 100.8(18) . . ? F2 C39 S1 117.1(17) . . ? F1 C39 S1 113(2) . . ? F3 C39 S1 111(2) . . ? F4 C40 F6 109(2) . . ? F4 C40 F5 107(3) . . ? F6 C40 F5 107(2) . . ? F4 C40 S2 112(2) . . ? F6 C40 S2 114.1(19) . . ? F5 C40 S2 106.9(17) . . ? Cl2 C41 Cl1 116(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.588 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.170 # Attachment '3a-MeOH.cif' data_3a-2MeOH-4H2O _database_code_depnum_ccdc_archive 'CCDC 818218' #TrackingRef '3a-MeOH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H96 F12 Ir4 N4 O24 S4' _chemical_formula_weight 2670.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.935(3) _cell_length_b 17.652(3) _cell_length_c 16.044(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.882(2) _cell_angle_gamma 90.00 _cell_volume 4635.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8560 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.89 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 5.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4708 _exptl_absorpt_correction_T_max 0.6491 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.28 _diffrn_reflns_number 34352 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.96 _reflns_number_total 11069 _reflns_number_gt 7642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11069 _refine_ls_number_parameters 610 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.687103(15) 0.786238(16) 0.436764(17) 0.02574(10) Uani 1 1 d . . . Ir2 Ir 0.194070(16) 0.843360(16) 0.436863(18) 0.02612(10) Uani 1 1 d . . . N1 N 0.7072(3) 0.8999(3) 0.4768(5) 0.0324(15) Uani 1 1 d . . . N2 N 0.7575(3) 1.0470(4) 0.5283(4) 0.0277(13) Uani 1 1 d . . . O1 O 0.6175(3) 0.7793(3) 0.5253(3) 0.0304(11) Uani 1 1 d . . . O2 O 0.5836(3) 0.8307(3) 0.3544(3) 0.0280(11) Uani 1 1 d . . . O3 O 0.2621(3) 0.8536(3) 0.3472(3) 0.0302(11) Uani 1 1 d . . . O4 O 0.2992(3) 0.8086(3) 0.5219(3) 0.0311(11) Uani 1 1 d . . . O5 O 0.5993(7) 0.3097(5) 0.7191(6) 0.091(3) Uani 1 1 d . . . O6 O 0.7178(5) 0.3890(5) 0.7542(5) 0.079(2) Uani 1 1 d . . . O7 O 0.5846(5) 0.4369(5) 0.7547(5) 0.080(2) Uani 1 1 d . . . O8 O 0.0604(5) 0.0796(6) 0.2692(5) 0.090(3) Uani 1 1 d . . . O9 O 0.1897(5) 0.1066(5) 0.2417(5) 0.075(2) Uani 1 1 d . . . O10 O 0.0771(5) 0.1878(5) 0.1868(6) 0.077(2) Uani 1 1 d . . . S1 S 0.63039(17) 0.38379(15) 0.72254(16) 0.0535(6) Uani 1 1 d . . . S2 S 0.10365(16) 0.11454(18) 0.21494(18) 0.0620(7) Uani 1 1 d . . . F1 F 0.5350(5) 0.4053(7) 0.5711(5) 0.127(4) Uani 1 1 d . . . F2 F 0.6328(8) 0.4792(5) 0.6019(7) 0.151(5) Uani 1 1 d . . . F3 F 0.6521(6) 0.3670(6) 0.5681(5) 0.114(3) Uani 1 1 d . . . F4 F -0.0055(6) 0.0548(7) 0.0856(6) 0.135(4) Uani 1 1 d . . . F5 F 0.1095(6) 0.0808(6) 0.0554(5) 0.114(3) Uani 1 1 d . . . F6 F 0.0993(6) -0.0150(5) 0.1318(7) 0.127(3) Uani 1 1 d . . . C1 C 0.5394(4) 0.7859(4) 0.5096(5) 0.0262(15) Uani 1 1 d . . . C2 C 0.4834(4) 0.8150(4) 0.4356(4) 0.0257(14) Uani 1 1 d . . . C3 C 0.5100(4) 0.8362(4) 0.3619(4) 0.0238(14) Uani 1 1 d . . . C4 C 0.4507(4) 0.8669(4) 0.2853(4) 0.0249(14) Uani 1 1 d . . . C5 C 0.4785(5) 0.8960(4) 0.2155(5) 0.0339(17) Uani 1 1 d . . . H5 H 0.5339 0.8956 0.2177 0.041 Uiso 1 1 calc R . . C6 C 0.4226(5) 0.9251(5) 0.1442(5) 0.0368(18) Uani 1 1 d . . . H6 H 0.4404 0.9439 0.0980 0.044 Uiso 1 1 calc R . . C7 C 0.3396(5) 0.9261(5) 0.1413(5) 0.0384(18) Uani 1 1 d . . . H7 H 0.3019 0.9451 0.0931 0.046 Uiso 1 1 calc R . . C8 C 0.3134(5) 0.8985(4) 0.2114(5) 0.0320(16) Uani 1 1 d . . . H8 H 0.2580 0.8999 0.2095 0.038 Uiso 1 1 calc R . . C9 C 0.3679(4) 0.8692(4) 0.2837(5) 0.0309(16) Uani 1 1 d . . . C10 C 0.3402(4) 0.8462(4) 0.3589(4) 0.0242(14) Uani 1 1 d . . . C11 C 0.3969(4) 0.8219(4) 0.4346(4) 0.0240(14) Uani 1 1 d . . . C12 C 0.3714(4) 0.8013(4) 0.5086(5) 0.0252(14) Uani 1 1 d . . . C13 C 0.4297(5) 0.7688(4) 0.5817(5) 0.0316(16) Uani 1 1 d . . . H13 H 0.4122 0.7535 0.6295 0.038 Uiso 1 1 calc R . . C14 C 0.5083(4) 0.7602(4) 0.5822(5) 0.0284(15) Uani 1 1 d . . . H14 H 0.5439 0.7375 0.6295 0.034 Uiso 1 1 calc R . . C15 C 0.7369(5) 0.9179(4) 0.5618(5) 0.0351(17) Uani 1 1 d . . . H15 H 0.7405 0.8809 0.6039 0.042 Uiso 1 1 calc R . . C16 C 0.7614(4) 0.9909(4) 0.5851(5) 0.0307(16) Uani 1 1 d . . . H16 H 0.7817 1.0018 0.6434 0.037 Uiso 1 1 calc R . . C17 C 0.7260(5) 1.0278(4) 0.4451(5) 0.0328(17) Uani 1 1 d . . . H17 H 0.7205 1.0651 0.4031 0.039 Uiso 1 1 calc R . . C18 C 0.7018(5) 0.9557(4) 0.4200(5) 0.0334(17) Uani 1 1 d . . . H18 H 0.6810 0.9454 0.3616 0.040 Uiso 1 1 calc R . . C19 C 0.7443(4) 0.7478(4) 0.3409(5) 0.0301(16) Uani 1 1 d . . . C20 C 0.8064(4) 0.7680(5) 0.4159(5) 0.0319(16) Uani 1 1 d . . . C21 C 0.7969(5) 0.7234(5) 0.4867(5) 0.0341(17) Uani 1 1 d . . . C22 C 0.7329(5) 0.6728(4) 0.4557(6) 0.0367(18) Uani 1 1 d . . . C23 C 0.6973(5) 0.6858(4) 0.3657(5) 0.0359(18) Uani 1 1 d . . . C24 C 0.7299(6) 0.7797(5) 0.2510(5) 0.043(2) Uani 1 1 d . . . H24A H 0.7510 0.8304 0.2540 0.065 Uiso 1 1 calc R . . H24B H 0.6723 0.7803 0.2239 0.065 Uiso 1 1 calc R . . H24C H 0.7571 0.7486 0.2179 0.065 Uiso 1 1 calc R . . C25 C 0.8677(5) 0.8282(5) 0.4179(6) 0.045(2) Uani 1 1 d . . . H25A H 0.9161 0.8063 0.4073 0.067 Uiso 1 1 calc R . . H25B H 0.8810 0.8522 0.4735 0.067 Uiso 1 1 calc R . . H25C H 0.8457 0.8651 0.3742 0.067 Uiso 1 1 calc R . . C26 C 0.8550(6) 0.7227(6) 0.5754(6) 0.053(2) Uani 1 1 d . . . H26A H 0.8252 0.7131 0.6177 0.080 Uiso 1 1 calc R . . H26B H 0.8818 0.7710 0.5867 0.080 Uiso 1 1 calc R . . H26C H 0.8952 0.6837 0.5783 0.080 Uiso 1 1 calc R . . C27 C 0.7018(6) 0.6124(5) 0.5066(6) 0.048(2) Uani 1 1 d . . . H27A H 0.7382 0.5698 0.5157 0.072 Uiso 1 1 calc R . . H27B H 0.6482 0.5965 0.4751 0.072 Uiso 1 1 calc R . . H27C H 0.6992 0.6328 0.5613 0.072 Uiso 1 1 calc R . . C28 C 0.6280(6) 0.6458(5) 0.3047(6) 0.048(2) Uani 1 1 d . . . H28A H 0.6491 0.6133 0.2675 0.072 Uiso 1 1 calc R . . H28B H 0.5918 0.6824 0.2706 0.072 Uiso 1 1 calc R . . H28C H 0.5987 0.6159 0.3369 0.072 Uiso 1 1 calc R . . C29 C 0.0963(5) 0.8292(5) 0.4980(6) 0.041(2) Uani 1 1 d . . . C30 C 0.0676(4) 0.8723(5) 0.4168(5) 0.0348(17) Uani 1 1 d . . . C31 C 0.0783(5) 0.8253(5) 0.3469(5) 0.0378(18) Uani 1 1 d . . . C32 C 0.1113(5) 0.7553(5) 0.3832(7) 0.050(2) Uani 1 1 d . . . C33 C 0.1212(5) 0.7557(5) 0.4746(6) 0.044(2) Uani 1 1 d . . . C34 C 0.0924(6) 0.8566(7) 0.5836(6) 0.064(3) Uani 1 1 d . . . H34A H 0.0398 0.8449 0.5925 0.096 Uiso 1 1 calc R . . H34B H 0.1007 0.9104 0.5868 0.096 Uiso 1 1 calc R . . H34C H 0.1342 0.8322 0.6273 0.096 Uiso 1 1 calc R . . C35 C 0.0348(5) 0.9513(5) 0.4092(7) 0.051(2) Uani 1 1 d . . . H35A H 0.0541 0.9782 0.3663 0.076 Uiso 1 1 calc R . . H35B H 0.0532 0.9766 0.4638 0.076 Uiso 1 1 calc R . . H35C H -0.0238 0.9498 0.3927 0.076 Uiso 1 1 calc R . . C36 C 0.0569(6) 0.8464(8) 0.2543(6) 0.073(4) Uani 1 1 d . . . H36A H 0.0067 0.8220 0.2251 0.110 Uiso 1 1 calc R . . H36B H 0.0997 0.8304 0.2290 0.110 Uiso 1 1 calc R . . H36C H 0.0504 0.9003 0.2487 0.110 Uiso 1 1 calc R . . C37 C 0.1326(7) 0.6892(7) 0.3326(10) 0.086(5) Uani 1 1 d . . . H37A H 0.1679 0.6548 0.3714 0.129 Uiso 1 1 calc R . . H37B H 0.1598 0.7076 0.2911 0.129 Uiso 1 1 calc R . . H37C H 0.0834 0.6633 0.3033 0.129 Uiso 1 1 calc R . . C38 C 0.1572(7) 0.6963(6) 0.5383(8) 0.070(3) Uani 1 1 d . . . H38A H 0.1855 0.6600 0.5120 0.106 Uiso 1 1 calc R . . H38B H 0.1145 0.6714 0.5572 0.106 Uiso 1 1 calc R . . H38C H 0.1949 0.7191 0.5869 0.106 Uiso 1 1 calc R . . C39 C 0.6108(7) 0.4114(8) 0.6111(8) 0.072(3) Uani 1 1 d . . . C40 C 0.0772(10) 0.0569(10) 0.1182(9) 0.097(5) Uani 1 1 d . . . C41 C 0.4480(8) 0.4652(7) 0.8933(9) 0.075(3) Uani 1 1 d . . . O11 O 0.5292(7) 0.4754(6) 0.9003(6) 0.100(3) Uani 1 1 d . . . C42 C 0.1414(8) 0.4774(8) 0.2836(9) 0.080(4) Uani 1 1 d D . . H42A H 0.1733 0.4952 0.3385 0.120 Uiso 1 1 calc R . . H42B H 0.1249 0.4260 0.2890 0.120 Uiso 1 1 calc R . . H42C H 0.0938 0.5087 0.2644 0.120 Uiso 1 1 calc R . . O12 O 0.1883(7) 0.4808(6) 0.2236(7) 0.114(4) Uani 1 1 d D . . H12 H 0.245(5) 0.513(10) 0.259(5) 0.18(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01832(15) 0.02924(18) 0.03052(16) -0.00036(11) 0.00785(11) -0.00107(10) Ir2 0.01852(15) 0.02981(18) 0.03117(17) -0.00020(11) 0.00846(11) -0.00096(10) N1 0.019(3) 0.014(3) 0.071(5) -0.003(3) 0.024(3) -0.001(2) N2 0.019(3) 0.035(3) 0.029(3) 0.000(3) 0.005(2) 0.001(2) O1 0.017(2) 0.043(3) 0.031(3) 0.003(2) 0.005(2) 0.001(2) O2 0.019(2) 0.041(3) 0.027(2) -0.001(2) 0.011(2) -0.001(2) O3 0.014(2) 0.045(3) 0.032(3) 0.001(2) 0.006(2) 0.000(2) O4 0.022(3) 0.039(3) 0.036(3) 0.005(2) 0.014(2) 0.002(2) O5 0.138(9) 0.057(5) 0.072(5) 0.003(4) 0.018(6) -0.038(5) O6 0.048(4) 0.123(7) 0.060(5) -0.009(5) 0.007(4) 0.007(4) O7 0.078(6) 0.101(6) 0.069(5) -0.018(5) 0.034(4) 0.017(5) O8 0.078(6) 0.136(8) 0.057(5) 0.032(5) 0.019(4) -0.019(5) O9 0.049(4) 0.111(7) 0.059(4) 0.031(4) 0.003(4) -0.004(4) O10 0.080(6) 0.059(5) 0.102(6) 0.022(5) 0.040(5) 0.001(4) S1 0.0605(16) 0.0552(16) 0.0477(13) -0.0062(11) 0.0189(12) -0.0042(12) S2 0.0434(14) 0.080(2) 0.0619(16) 0.0314(14) 0.0124(12) -0.0067(12) F1 0.070(5) 0.227(11) 0.070(5) 0.016(6) -0.006(4) -0.005(6) F2 0.237(13) 0.091(7) 0.132(8) 0.020(6) 0.060(9) -0.064(8) F3 0.136(8) 0.164(8) 0.057(4) -0.010(5) 0.052(5) 0.013(6) F4 0.088(7) 0.193(10) 0.114(7) -0.020(7) 0.008(6) -0.067(7) F5 0.133(8) 0.138(8) 0.080(5) -0.001(5) 0.042(5) -0.053(6) F6 0.138(9) 0.082(6) 0.171(10) 0.010(6) 0.059(8) -0.011(6) C1 0.022(3) 0.022(4) 0.037(4) -0.007(3) 0.010(3) -0.001(3) C2 0.020(3) 0.028(4) 0.029(3) -0.002(3) 0.008(3) -0.003(3) C3 0.021(3) 0.024(4) 0.027(3) -0.003(3) 0.008(3) -0.003(3) C4 0.022(3) 0.025(4) 0.029(3) -0.002(3) 0.008(3) -0.004(3) C5 0.034(4) 0.042(5) 0.029(4) 0.001(3) 0.015(3) 0.001(3) C6 0.040(4) 0.040(5) 0.035(4) 0.003(3) 0.017(4) -0.003(3) C7 0.046(5) 0.040(5) 0.030(4) 0.005(3) 0.009(4) 0.002(4) C8 0.029(4) 0.033(4) 0.034(4) 0.005(3) 0.008(3) 0.001(3) C9 0.025(4) 0.028(4) 0.040(4) -0.001(3) 0.008(3) -0.003(3) C10 0.016(3) 0.027(4) 0.029(3) 0.000(3) 0.004(3) 0.001(2) C11 0.020(3) 0.024(4) 0.029(3) 0.003(3) 0.008(3) -0.001(3) C12 0.015(3) 0.026(4) 0.036(4) -0.003(3) 0.010(3) -0.002(3) C13 0.030(4) 0.043(4) 0.024(3) 0.004(3) 0.010(3) -0.005(3) C14 0.021(3) 0.037(4) 0.027(3) 0.002(3) 0.005(3) 0.007(3) C15 0.037(4) 0.029(4) 0.041(4) -0.001(3) 0.012(3) -0.004(3) C16 0.029(4) 0.035(4) 0.026(3) -0.001(3) 0.004(3) -0.002(3) C17 0.036(4) 0.032(4) 0.032(4) 0.009(3) 0.013(3) 0.012(3) C18 0.037(4) 0.033(4) 0.029(4) -0.006(3) 0.006(3) 0.000(3) C19 0.023(3) 0.040(5) 0.032(4) 0.003(3) 0.015(3) 0.005(3) C20 0.025(4) 0.040(4) 0.033(4) -0.003(3) 0.010(3) 0.004(3) C21 0.023(4) 0.040(5) 0.038(4) -0.002(3) 0.006(3) 0.010(3) C22 0.021(4) 0.031(4) 0.063(5) 0.001(4) 0.020(4) -0.003(3) C23 0.030(4) 0.026(4) 0.051(5) -0.008(4) 0.007(4) 0.003(3) C24 0.050(5) 0.050(5) 0.034(4) 0.007(4) 0.016(4) 0.007(4) C25 0.030(4) 0.051(5) 0.055(5) -0.006(4) 0.014(4) -0.012(4) C26 0.042(5) 0.072(7) 0.041(5) 0.008(4) 0.001(4) 0.017(5) C27 0.057(6) 0.040(5) 0.054(5) 0.008(4) 0.026(5) 0.000(4) C28 0.040(5) 0.046(5) 0.055(6) -0.019(4) 0.009(4) -0.016(4) C29 0.034(4) 0.046(5) 0.049(5) -0.004(4) 0.023(4) -0.009(4) C30 0.020(4) 0.037(4) 0.049(5) 0.004(4) 0.012(3) -0.001(3) C31 0.023(4) 0.048(5) 0.044(4) -0.006(4) 0.011(3) -0.013(3) C32 0.038(5) 0.039(5) 0.078(7) -0.009(5) 0.025(5) -0.006(4) C33 0.027(4) 0.035(5) 0.068(6) 0.019(4) 0.011(4) -0.008(3) C34 0.037(5) 0.120(10) 0.039(5) 0.000(6) 0.017(4) -0.004(5) C35 0.029(4) 0.044(5) 0.081(7) 0.004(5) 0.018(5) -0.001(4) C36 0.039(6) 0.140(11) 0.039(5) 0.001(6) 0.005(4) -0.021(6) C37 0.047(7) 0.072(8) 0.143(12) -0.064(8) 0.033(7) -0.014(6) C38 0.057(7) 0.057(7) 0.102(9) 0.035(6) 0.028(6) 0.005(5) C39 0.059(7) 0.097(10) 0.058(7) 0.013(6) 0.015(6) -0.018(6) C40 0.102(12) 0.108(12) 0.076(9) 0.027(8) 0.012(8) -0.051(9) C41 0.075(9) 0.061(8) 0.086(9) 0.008(6) 0.013(7) -0.010(6) O11 0.120(9) 0.108(8) 0.072(6) -0.005(5) 0.027(6) 0.001(6) C42 0.058(7) 0.097(10) 0.088(9) 0.001(7) 0.024(7) -0.006(7) O12 0.114(9) 0.124(9) 0.117(8) -0.066(7) 0.051(7) -0.033(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 O2 2.060(5) . ? Ir1 O1 2.069(5) . ? Ir1 N1 2.108(6) . ? Ir1 C19 2.128(7) . ? Ir1 C21 2.137(7) . ? Ir1 C23 2.139(8) . ? Ir1 C22 2.141(8) . ? Ir1 C20 2.156(7) . ? Ir2 O4 2.039(5) . ? Ir2 O3 2.069(5) . ? Ir2 N2 2.120(6) 3_676 ? Ir2 C32 2.122(9) . ? Ir2 C31 2.139(8) . ? Ir2 C30 2.144(7) . ? Ir2 C29 2.146(8) . ? Ir2 C33 2.159(7) . ? N1 C18 1.330(10) . ? N1 C15 1.364(10) . ? N2 C16 1.336(9) . ? N2 C17 1.347(10) . ? N2 Ir2 2.120(6) 3_676 ? O1 C1 1.285(8) . ? O2 C3 1.285(8) . ? O3 C10 1.293(8) . ? O4 C12 1.301(8) . ? O5 S1 1.405(8) . ? O6 S1 1.439(8) . ? O7 S1 1.397(8) . ? O8 S2 1.415(8) . ? O9 S2 1.417(8) . ? O10 S2 1.405(8) . ? S1 C39 1.800(12) . ? S2 C40 1.813(16) . ? F1 C39 1.284(13) . ? F2 C39 1.272(14) . ? F3 C39 1.353(15) . ? F4 C40 1.364(17) . ? F5 C40 1.333(15) . ? F6 C40 1.325(18) . ? C1 C2 1.412(10) . ? C1 C14 1.468(10) . ? C2 C3 1.420(9) . ? C2 C11 1.465(9) . ? C3 C4 1.476(10) . ? C4 C9 1.397(10) . ? C4 C5 1.417(9) . ? C5 C6 1.382(11) . ? C6 C7 1.395(11) . ? C7 C8 1.399(10) . ? C8 C9 1.384(10) . ? C9 C10 1.461(10) . ? C10 C11 1.408(9) . ? C11 C12 1.411(9) . ? C12 C13 1.444(10) . ? C13 C14 1.337(10) . ? C15 C16 1.376(10) . ? C17 C18 1.365(11) . ? C19 C20 1.425(11) . ? C19 C23 1.469(11) . ? C19 C24 1.508(10) . ? C20 C21 1.425(11) . ? C20 C25 1.480(11) . ? C21 C22 1.395(11) . ? C21 C26 1.507(11) . ? C22 C23 1.432(12) . ? C22 C27 1.517(11) . ? C23 C28 1.497(11) . ? C29 C33 1.443(12) . ? C29 C34 1.473(12) . ? C29 C30 1.479(12) . ? C30 C31 1.443(12) . ? C30 C35 1.493(12) . ? C31 C32 1.419(13) . ? C31 C36 1.484(13) . ? C32 C33 1.432(13) . ? C32 C37 1.516(13) . ? C33 C38 1.482(13) . ? C41 O11 1.362(16) . ? C42 O12 1.398(15) . ? 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 O2 Ir1 O1 85.47(19) . . ? O2 Ir1 N1 82.9(2) . . ? O1 Ir1 N1 85.6(2) . . ? O2 Ir1 C19 97.4(2) . . ? O1 Ir1 C19 157.3(3) . . ? N1 Ir1 C19 117.1(3) . . ? O2 Ir1 C21 162.5(3) . . ? O1 Ir1 C21 107.8(3) . . ? N1 Ir1 C21 108.9(3) . . ? C19 Ir1 C21 65.9(3) . . ? O2 Ir1 C23 98.4(3) . . ? O1 Ir1 C23 117.0(3) . . ? N1 Ir1 C23 157.4(3) . . ? C19 Ir1 C23 40.3(3) . . ? C21 Ir1 C23 65.7(3) . . ? O2 Ir1 C22 131.6(3) . . ? O1 Ir1 C22 95.5(3) . . ? N1 Ir1 C22 145.4(3) . . ? C19 Ir1 C22 65.7(3) . . ? C21 Ir1 C22 38.1(3) . . ? C23 Ir1 C22 39.1(3) . . ? O2 Ir1 C20 129.4(2) . . ? O1 Ir1 C20 145.1(3) . . ? N1 Ir1 C20 96.1(3) . . ? C19 Ir1 C20 38.9(3) . . ? C21 Ir1 C20 38.8(3) . . ? C23 Ir1 C20 65.6(3) . . ? C22 Ir1 C20 64.0(3) . . ? O4 Ir2 O3 86.86(19) . . ? O4 Ir2 N2 83.5(2) . 3_676 ? O3 Ir2 N2 81.8(2) . 3_676 ? O4 Ir2 C32 115.0(3) . . ? O3 Ir2 C32 102.1(3) . . ? N2 Ir2 C32 161.1(3) 3_676 . ? O4 Ir2 C31 153.9(3) . . ? O3 Ir2 C31 97.0(3) . . ? N2 Ir2 C31 122.6(3) 3_676 . ? C32 Ir2 C31 38.9(4) . . ? O4 Ir2 C30 147.0(3) . . ? O3 Ir2 C30 126.0(3) . . ? N2 Ir2 C30 97.2(3) 3_676 . ? C32 Ir2 C30 65.4(3) . . ? C31 Ir2 C30 39.4(3) . . ? O4 Ir2 C29 107.6(3) . . ? O3 Ir2 C29 164.0(3) . . ? N2 Ir2 C29 106.1(3) 3_676 . ? C32 Ir2 C29 66.0(3) . . ? C31 Ir2 C29 67.0(3) . . ? C30 Ir2 C29 40.3(3) . . ? O4 Ir2 C33 93.5(3) . . ? O3 Ir2 C33 135.9(3) . . ? N2 Ir2 C33 142.2(3) 3_676 . ? C32 Ir2 C33 39.1(4) . . ? C31 Ir2 C33 65.9(3) . . ? C30 Ir2 C33 65.9(3) . . ? C29 Ir2 C33 39.2(3) . . ? C18 N1 C15 117.1(6) . . ? C18 N1 Ir1 121.2(6) . . ? C15 N1 Ir1 121.0(5) . . ? C16 N2 C17 115.3(7) . . ? C16 N2 Ir2 123.3(5) . 3_676 ? C17 N2 Ir2 121.3(5) . 3_676 ? C1 O1 Ir1 126.8(5) . . ? C3 O2 Ir1 130.9(5) . . ? C10 O3 Ir2 128.3(5) . . ? C12 O4 Ir2 128.1(5) . . ? O7 S1 O5 113.6(6) . . ? O7 S1 O6 116.4(5) . . ? O5 S1 O6 114.4(6) . . ? O7 S1 C39 102.0(6) . . ? O5 S1 C39 104.0(6) . . ? O6 S1 C39 104.1(5) . . ? O10 S2 O8 115.2(6) . . ? O10 S2 O9 114.1(5) . . ? O8 S2 O9 115.2(5) . . ? O10 S2 C40 104.7(7) . . ? O8 S2 C40 103.2(6) . . ? O9 S2 C40 102.3(7) . . ? O1 C1 C2 129.2(7) . . ? O1 C1 C14 112.2(6) . . ? C2 C1 C14 118.6(6) . . ? C1 C2 C3 120.5(6) . . ? C1 C2 C11 119.6(6) . . ? C3 C2 C11 119.9(6) . . ? O2 C3 C2 125.4(6) . . ? O2 C3 C4 114.7(6) . . ? C2 C3 C4 119.8(6) . . ? C9 C4 C5 120.7(7) . . ? C9 C4 C3 119.4(6) . . ? C5 C4 C3 119.9(6) . . ? C6 C5 C4 119.5(7) . . ? C5 C6 C7 120.2(7) . . ? C6 C7 C8 119.6(7) . . ? C9 C8 C7 121.5(7) . . ? C8 C9 C4 118.5(7) . . ? C8 C9 C10 120.6(7) . . ? C4 C9 C10 120.8(7) . . ? O3 C10 C11 127.1(6) . . ? O3 C10 C9 112.6(6) . . ? C11 C10 C9 120.2(6) . . ? C10 C11 C12 121.0(6) . . ? C10 C11 C2 119.6(6) . . ? C12 C11 C2 119.3(6) . . ? O4 C12 C11 128.0(7) . . ? O4 C12 C13 112.4(6) . . ? C11 C12 C13 119.5(6) . . ? C14 C13 C12 121.4(7) . . ? C13 C14 C1 121.3(7) . . ? N1 C15 C16 119.8(7) . . ? N2 C16 C15 123.4(7) . . ? N2 C17 C18 122.7(7) . . ? N1 C18 C17 121.7(7) . . ? C20 C19 C23 106.9(6) . . ? C20 C19 C24 128.2(7) . . ? C23 C19 C24 124.9(7) . . ? C20 C19 Ir1 71.6(4) . . ? C23 C19 Ir1 70.3(4) . . ? C24 C19 Ir1 125.5(6) . . ? C21 C20 C19 109.0(7) . . ? C21 C20 C25 127.0(7) . . ? C19 C20 C25 124.0(7) . . ? C21 C20 Ir1 69.9(4) . . ? C19 C20 Ir1 69.5(4) . . ? C25 C20 Ir1 124.7(6) . . ? C22 C21 C20 107.8(7) . . ? C22 C21 C26 126.3(8) . . ? C20 C21 C26 125.2(8) . . ? C22 C21 Ir1 71.1(5) . . ? C20 C21 Ir1 71.3(4) . . ? C26 C21 Ir1 130.7(6) . . ? C21 C22 C23 110.2(7) . . ? C21 C22 C27 127.1(8) . . ? C23 C22 C27 122.7(7) . . ? C21 C22 Ir1 70.8(4) . . ? C23 C22 Ir1 70.4(4) . . ? C27 C22 Ir1 124.7(6) . . ? C22 C23 C19 106.0(6) . . ? C22 C23 C28 129.7(8) . . ? C19 C23 C28 124.2(8) . . ? C22 C23 Ir1 70.5(4) . . ? C19 C23 Ir1 69.5(4) . . ? C28 C23 Ir1 125.6(6) . . ? C33 C29 C34 128.6(9) . . ? C33 C29 C30 106.6(7) . . ? C34 C29 C30 124.7(9) . . ? C33 C29 Ir2 70.9(5) . . ? C34 C29 Ir2 127.8(7) . . ? C30 C29 Ir2 69.8(4) . . ? C31 C30 C29 108.1(7) . . ? C31 C30 C35 126.2(8) . . ? C29 C30 C35 125.7(8) . . ? C31 C30 Ir2 70.1(4) . . ? C29 C30 Ir2 69.9(4) . . ? C35 C30 Ir2 124.8(5) . . ? C32 C31 C30 107.3(8) . . ? C32 C31 C36 126.7(9) . . ? C30 C31 C36 126.0(9) . . ? C32 C31 Ir2 69.9(5) . . ? C30 C31 Ir2 70.5(4) . . ? C36 C31 Ir2 125.7(6) . . ? C31 C32 C33 110.2(8) . . ? C31 C32 C37 125.0(10) . . ? C33 C32 C37 124.8(10) . . ? C31 C32 Ir2 71.2(5) . . ? C33 C32 Ir2 71.9(5) . . ? C37 C32 Ir2 123.9(7) . . ? C32 C33 C29 107.9(7) . . ? C32 C33 C38 128.4(9) . . ? C29 C33 C38 123.5(9) . . ? C32 C33 Ir2 69.1(5) . . ? C29 C33 Ir2 69.9(4) . . ? C38 C33 Ir2 122.5(6) . . ? F2 C39 F1 107.8(13) . . ? F2 C39 F3 106.4(11) . . ? F1 C39 F3 106.1(11) . . ? F2 C39 S1 112.6(10) . . ? F1 C39 S1 112.3(8) . . ? F3 C39 S1 111.2(9) . . ? F6 C40 F5 106.0(15) . . ? F6 C40 F4 104.9(11) . . ? F5 C40 F4 107.4(12) . . ? F6 C40 S2 113.5(10) . . ? F5 C40 S2 114.2(9) . . ? F4 C40 S2 110.3(13) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.197 0.960 -0.029 16.8 -3.4 2 0.803 0.040 0.029 16.8 -4.0 3 0.197 0.540 0.471 16.8 -3.5 4 0.803 0.460 0.529 16.8 -4.1 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.623 _refine_diff_density_min -2.212 _refine_diff_density_rms 0.283